m-c < onitroy mills landfill superfund site, troy, new hampshire tier ii organic data validation...

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SDMS DocID 000234888 Metcalf & Eddy 701rdm>«.iKM nmi> W.lkehi'ld MA 01 HBO 036.200100.0060.00005 M -a 1-241, ^oo r,i\ ~HI-24S-(>J 1 H \\v\\\ m-c < oni February 24, 2005 Christine Clark Regional Sample Control Center U.S. EPA Region I 11 Technology Drive North Chelmsford, Massachusetts 01863-2431 Re: Work Assignment No. 160-RICO-019M Case 0251M, SDG D05939 Woods Hole Group Environmental Laboratories, Raynham, Massachusetts Troy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945, DOS946, D05947, D05948, DOS949, D05950, D05951, D05952, D05953 (Field Duplicate Pairs: D05947/D05953) 1/Aqueous Equipment Blank/ D05954 1/Solid Performance Evaluation Sample/ D05939 Dear Ms. Clark: A Tier II data validation was performed by Metcalf & Eddy, Inc. (M&E) on the organic analytical data for nine soil samples (including one field duplicate), one equipment blank, and one performance evaluation (PE) sample collected by M&E from the Troy Mills Landfill Superfund Site in Troy, New Hampshire on December 14 and 15, 2004. The samples were analyzed for semivolatile organic compounds (S VOCs) through the Response Action Contract (RAC) Delivery of Analytical Services (DAS) program using the DAS Specification for the Analysis of Low Concentration TCL Semivolatile Organic Compounds in Solid Samples Including Those with High Moisture Content (D-148). M&E evaluated these data using the Region I, EPA-NE Data Validation Functional Guidelines for Evaluating Environmental Analyses, December 1996 criteria, modified as appropriate for the method. J \NE\WA160 Troy Mills Landfill\Data Vahdation\December 2004\DV Memos\sD05939_svocsim \<.pd AN At ( () M («Ml>\m

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Page 1: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

SDMS DocID 000234888

Metcalf amp Eddy 701 rdmgtlaquoiKM nmigt Wlkehild MA 01 HBO

036200100006000005 M -a 1-241 ^oo ri ~HI-24S-(gtJ1 H v m-c lt oni

February 24 2005

Christine Clark Regional Sample Control Center US EPA Region I 11 Technology Drive North Chelmsford Massachusetts 01863-2431

Re Work Assignment No 160-RICO-019M Case 0251M SDG D05939 Woods Hole Group Environmental Laboratories Raynham Massachusetts Troy Mills Landfill Superfund Site Troy New Hampshire Tier II Organic Data Validation

Semivolatiles

9Soils D05945 DOS946 D05947 D05948 DOS949 D05950 D05951 D05952 D05953 (Field Duplicate Pairs D05947D05953) 1Aqueous Equipment Blank D05954 1Solid Performance Evaluation Sample D05939

Dear Ms Clark

A Tier II data validation was performed by Metcalf amp Eddy Inc (MampE) on the organic analytical data for nine soil samples (including one field duplicate) one equipment blank and one performance evaluation (PE) sample collected by MampE from the Troy Mills Landfill Superfund Site in Troy New Hampshire on December 14 and 15 2004 The samples were analyzed for semivolatile organic compounds (S VOCs) through the Response Action Contract (RAC) Delivery of Analytical Services (DAS) program using the DAS Specification for the Analysis of Low Concentration TCL Semivolatile Organic Compounds in Solid Samples Including Those with High Moisture Content (D-148) MampE evaluated these data using the Region I EPA-NE Data Validation Functional Guidelines for Evaluating Environmental Analyses December 1996 criteria modified as appropriate for the method

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DV MemossD05939_svocsim ltpd

AN A t ( () M (laquoMlgtm

Ms Christine Clark Page 2 February 24 2005 Case 0251M SDG D05939

The Tier II validation for the SVOC data was based on an evaluation of the following parameters

bull Overall Evaluation of Data and Potential Usability Issues Data Completeness (CSF Audit)

bull Preservation and Technical Holding Times bull GCMS Instrument Performance Checks

bull Initial and Continuing Calibrations bull Blanks

bull Surrogate Spike Recoveries bull Internal Standards

bull Matrix SpikeMatrix Spike Duplicate (MSMSD) bull Field Duplicates

bull Sensitivity Check bull PE Sample ResultsAccuracy Check

NA bull Target Compound Identification bull Sample Quantitation and Reported Quantitation Limits

Tentatively Identified Compounds NA bull Semivolatile Cleanup NA bull System Performance

- All quality control criteria were met for this parameter NA - Not applicable to the analytical method or to a Tier II validation

Note Worksheets are not included for parameters that have met criteria or for criteria that are not applicable to a Tier II data validation

Copies of the field logbook and field sampling notes for this sample delivery group (SDG) may be found as an attachment to Case 0251M SDG D05916 which was previously submitted to the EPA

The following information was used to generate the Data Validation Memorandum attachments

Table I Recommendation Summary Table - summarizes validation recommendations Table II Overall Evaluation of Data - summarizes site DQOs and potential usability issues Table III Tentatively Identified Compound Summary Data Summary Tables - summarizes accepted qualified and rejected data

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossD05939_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 3 February 24 2005 Case 0251M SDG D05939

Overall Evaluation of Data and Potential Usability Issues

The following is a summary of the site DQOs (Data Quality Objectives)

bull To determine the nature and extent of contamination following the completion of two removal actions in order to perform human health and ecological risk assessments and thereby recommend a remedy to eliminate reduce or control risks to human health and the environment

The sample data were qualified as a result of sampling and analytical error Qualifications as a result of sampling error are summarized below

The positive results for benzaldehyde in soil samples D05945 D05946 D05949 D05950 D05951 and D05952 and for acetophenone in soil sample D05951 were flagged EB due to equipment blank contamination The end data user should consider that an indeterminate amount of sampling error may have affected these sample results The results are usable for project objectives These qualifications have a minor impact on data usability

Qualifications as a result of analytical error are summarized below

bull The positive and nondetect results for benzaldehyde hexachlorocyclopentadiene 24-dinitrophenol 46-dinitro-2-methylphenol atrazine and pentachlorophenol in all samples were qualified as estimated (J and UJ respectively) due to the percent relative standard deviation (RSD) exceedances in the initial calibration All results are usable for project objectives as estimated values and as nondetect results with estimated quantitation limits These qualifications have a minor impact on data usability

bull The positive and nondetect results for benzaldehyde and 33-dichlorobenzidine in all samples for hexachlorobutadiene 4-nitrophenol and hexachlorobenzene in samples D05948 D05949 and D05953 for hexachlorocyclopentadiene in samples D05954 D05948 D05949 and D05953 and for 24-dinitrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 were qualified as estimated (J and UJ respectively) due to the percent difference (D) exceedances in the continuing calibrations These results are usable for project objectives as estimated values and as nondetect results with estimated quantitation limits These qualifications have a minor impact on data usability

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DVMemossD05939_socsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 4 February 24 2005 Case 0251M SDG D05939

bull The positive di-n-butylphthalate result in equipment blank sample D05954 was qualified as estimated (J) due to the RSD exceedance in the initial calibration This result is usable for project objective as an estimated value Note that this result was also qualified as nondetect (U) due to method blank contamination Therefore the overall qualification for this result is estimated nondetect (UJ) These qualifications have a minor impact on data usability

bull The positive di-n-butylphthalate results in all soil samples were qualified as estimated (J) due to the D exceedance in the continuing calibration These results are usable for project objectives as estimated values Note that the di-nshybutylphthalate results in all soil samples were also qualified as nondetect (U) due to method blank contamination Therefore the overall qualification for these results is estimated nondetect (UJ) These qualifications have a minor impact on data usability

bull The positive result for di-n-butylphthalate in equipment blank sample D05954 was qualified as nondetect (U) at the reported value due to method blank contamination This result is usable for project objectives as a nondetect Note that this result was also qualified as estimated (J) due to calibration nonconformances and high recoveries in the low-level and high-level laboratory fortified blanks (LFBs) Therefore the overall qualification for this result is estimated nondetect (UJ) These qualifications have a minor impact on data usability

bull The positive result for bis(2-ethylhexyl)phthalate in equipment blank sample D05954 was qualified as nondetect (U) at the quantitation limit (QL) due to method blank contamination This result is usable for project objectives as a nondetect This qualification has a minor impact on data usability

bull The positive results for di-n-butylphthalate in all soil samples were qualified as nondetect (U) at the reported values due to method blank contamination These results are usable for project objectives as nondetects Note that the di-nshybutylphthalate results in all soil samples were also qualified as estimated (J) due to calibration nonconformances high recoveries in the low-level and high-level LFBs andor ion abundance ratio exceedances Therefore the overall qualification for these results is estimated nondetect (UJ) These qualifications have a minor impact on data usability

bull The positive results for bis(2-ethylhexyl)phthalate in samples D05950 D05951 and D05952 were qualified as nondetect (U) at the QL due to performance evaluation sample contamination These results are usable for project objectives as nondetects These qualifications have a minor impact on data usability

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DV MemossD05939_svocsim wpd MetcalfA Eddy Inc

Ms Christine Clark Page 5 February 24 2005 Case 0251M SDG D05939

bull The nondetect result for caprolactam in equipment blank sample D05954 was qualified as estimated (UJ) at the raised quantitation limit [equivalent to the concentration of the high-level LFB (4 ugL)] due to low recoveries in the low-level and high-level LFB analyses This result is usable for project objectives as a nondetect with a raised and estimated quantitation limit that may be biased low This qualification has a minor impact on data usability

bull The nondetect results for 4-nitrophenol 46-dinitro-2-methylphenol and pentachlorophenol in equipment blank sample D05954 were qualified as estimated (UJ) due to low recoveries in the low-level LFB analyses These results are usable for project objectives as nondetects with estimated quantitation limits that may be biased low These qualifications have a minor impact on data usability

bull The positive result for di-n-butylphthalate in equipment blank sample D05954 was qualified as estimated (J) due to high recoveries in the low-level and high-level LFB analyses This result is usable for project objectives as an estimated value that may be biased high Note that this result was also qualified as nondetect (U) due to method blank contamination Therefore the overall qualification for this result is estimated nondetect (UJ) These qualifications have a minor impact on data usability

bull The nondetect results for 24-dinitrophenol in all soil samples were qualified as estimated (UJ) at the raised quantitation limit [equivalent to the concentration of the high-level LFB (800 ugKg) and corrected for all preparation factors] due to low recoveries in the low-level and high-level LFB analyses These results are usable for project objectives as nondetects with raised and estimated quantitation limits that may be biased low These qualifications have a minor impact on data usability

bull The nondetect results for 24-dimethylphenol 4-nitrophenol 46-dinitro-2shymethylphenol pentachlorophenol and 33-dichlorobenzidine in all soil samples were qualified as estimated (UJ) due to low recoveries in the low-level LFB analyses These results are usable for project objectives as nondetects with estimated quantitation limits that may be biased low These qualifications have a minor impact on data usability

bull The nondetect results for 4-chloroaniline in all soil samples were qualified as estimated (UJ) due to low recoveries in the low-level and high-level LFB analyses These results are usable for project objectives as nondetects with estimated quantitation limits that maybe biased low These qualifications have a minor impact on data usability

J NEWA160 Troy Mills LandfiMData VahdationDecember 2004DV MemossD05939_svocsm pd Metcalfamp Eddy Inc

Ms Christine Clark Page 6 February 24 2005 Case 0251M SDG D05939

The positive results for di-n-butylphthalate in all soil samples were qualified as estimated (J) due to high recoveries in the low-level and high-level LFB analyses These results are usable for project objectives as estimated values that maybe biased high Note that the di-n-butylphthalate results in all soil samples were also qualified as nondetect (U) due to method blank contamination Therefore the overall qualification for these results is estimated nondetect (UJ) These qualifications have a minor impact on data usability

The positive results for benzo(b)fluoranthene in samples D05951 D05952 D05945 D05946 and D05949 were qualified as estimated (J) due to high recovery in the high-level LFB analyses These results are usable for project objectives as estimated values that may be biased high These qualifications have a minor impact on data usability

The nondetect result for caprolactam in equipment blank sample D05954 was qualified as estimated (UJ) due to the low recovery in the laboratory control sample (LCS) analysis This result is usable for project objectives as a nondetect with an estimated quantitation limit that may be biased low These qualifications have a minor impact on data usability

The nondetect results for benzaldehyde and 4-chloroaniline in all soil samples were qualified as estimated (UJ) due to low recoveries in the LCS analyses These results are usable for project objectives as nondetects with estimated quantitation limits that may be biased low These qualifications have a minor impact on data usability

The positive results for benzo(b)fluoranthene benzo(a)pyrene and indeno(l23shycd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 were qualified as estimated (J) due to the high recoveries in the LCS analyses These results are usable for project objectives as estimated values that may be biased high These qualifications have a minor impact on data usability

JNEWAI60 Troy Mills LandfillData ValidationDecember 2004DV MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 7 February 24 2005 Case 0251M SDG D05939

bull The following compounds in the samples listed below were qualified as estimated (J) due to uncertainty in the quantitation as a result of the exceeded ion abundance ratio criteria These results are usable for project objectives as estimated values Note that the results for di-n-butylphthalate in samples D05950 D05951 D05952 D05945 D05947 D05948 D05949 and D05953 were also qualified as nondetect (U) due to method blank contamination Therefore the overall qualification for these results is estimated nondetect (UJ) These qualifications have a minor impact on data usability

D05950 di-n-butylphthalate D05951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate indeno(l23-cd)pyrene D05946 indeno(l23-cd)pyrene DOS 947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate DOS 95 3 di-n-butylphthalate

Data Completeness (CSF Audit)

The following information was missing or incorrect in the data package This missing or incorrect information was requested from the laboratory on February 7 and 152005 A resubmittal response was received at MampE on February 18 2005 adequately addressing these issues

bull The method detection limit (MDL) study results for two selected ion monitoring (SIM) compounds (pentachlorophenol and di-n-butylphthalate) were missing from the data package

The Form I (TIC) for sample D05946 identified the TIC at 1246 as alphashycaryophyllene while the raw data reported this TIC as l6-octadien-3-ol 37shydimethyl- Clarification was requested

bull The Form I for sample D05949 reported 26-dinitrotoluene and fluoranthene while the quantitation report did not reflect these results The laboratory was asked to verify this discrepancy

bull A relative response factor for 46-dinitro-2-methylphenol was listed on the Form 6 for the initial calibration in association with the 05 ugml standard However this compound was not listed on the quantitation report in the raw data The laboratory was asked to verify this discrepancy

J NEWA16Q Troy Mills LandfillData VahdationDecember 2004DV MemossD05939_svocsim pd Metcalf amp Eddy Inc

Ms Christine Clark Page 8 February 24 2005 Case 0251M SDG D05939

Initial and Continuing Calibrations

Full Scan

The following table summarizes the initial calibration (1C) and continuing calibration (CC) results that failed to meet the relative response factor (RRF) criterion of ^005 andor RSD lt 30 in the 1C andor D lt 25 in the CC for all compounds

Calibration Date 1C CC CC CC 12505 12705 13105 2105

Compound RSD D D D

benzaldehyde 792 155 156 153

hexachlorobutadiene - - - 453

hexachlorocyc lopentadiene 488 448 - 360

24-dimtrophenol 337 - 25 8 -

4-nitrophenol - - - 467

hexachlorobenzene - - - 286

46-dimtro-2-methylphenol 450 - - -

atrazme 434 - - -

pentachlorophenol 384 - - -

33-dichlorobenzidme - 726 463 628

2-fluorophenol (surrogate) - - - 285

Associated samples All samples D05954 D05950 D05951 D05948RE D05952 D05945 D05949 D05946 D05947 D05953RE D05948 D05953 D05949DL

D05945DL D05946DL D05947DL D05948DL D05953DL

- - QC acceptance criteria were not exceeded for this compound

Actions RSD gt 30 Estimate (J and UJ respectively) positive and nondetect results D gt 25 Estimate (J and UJ respectively) positive and nondetect results

JNEWA160 Troy Mills LandftllData VahdationDecember 2004DV MemossD05939_socsim pd Metcalf amp Eddy Inc

Ms Christine Clark Page 9 February 24 2005 Case 0251M SDGD05939

The positive and nondetect results for benzaldehyde hexachlorocyclopentadiene 24-dinitrophenol 46-dinitro-2-methylphenol atrazine and pentachlorophenol in all samples were qualified as estimated (UJ) due to initial calibration RSD exceedances

The positive and nondetect results for benzaldehyde and 33-dichlorobenzidine in all samples for hexachlorobutadiene 4-nitrophenol and hexachlorobenzene in samples D05948RE D05949 and D05953RE for hexachlorocyclopentadiene in samples D05954 D05948RE D05949 and D05953RE and for 24-dinitrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 were qualified as estimated (J and UJ respectively) due to continuing calibration D exceedances

No validation actions were necessary for the calibration nonconformances associated with the dilution sample analyses or for the original analyses of samples D05948 and D05953 since the compounds listed in the table above were not reported from these analyses

No validation actions were necessary for the surrogate compound calibration nonconformance

SIM

The following table summarizes the 1C and CC results that failed to meet the RRF criterion of gt005 andor RSD lt 30 in the 1C andor D lt 25 in the CC for all compounds

Calibration Date 1C 12105 1C 2205 CC 2305

Compound RSD RSD D

pentachlorophenol 621 402 -

di-n-butyl phthalate 331 - 297

bis(2-ethylhexyl)phthalate 347 306

Associated samples D05954 all soil samples all soil samples

- - QC acceptance criteria were not exceeded for this compound

Actions RSD gt 30 Estimate (J and UJ respectively) positive and nondetect results D gt 25 Estimate (J and UJ respectively) positive and nondetect results

The positive di-n-butylphthalate result in equipment blank sample D05954 was qualified as estimated (J) due to the RSD exceedance in the initial calibration

The positive di-n-butylphthalate results in all soil samples were qualified as estimated (J) due to the D exceedance in the continuing calibration

J NE WA160 Troy Mills LandfillData Validation December 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 10 February 24 2005 Case 0251M SDG D05939

The pentachlorophenol and bis(2-ethylhexyl)phthalate results in all samples were reported from the full scan analyses therefore no data validation actions were required as a result of the calibration nonconformances

Blanks

Full Scan

Target compounds were detected as contaminants m the performance evaluation sample (PES) as well as the equipment and laboratory method blanks The highest concentration detected was used to qualify associated sample results The following table summarizes the blank actions as they apply to the samples

Compound Blank

Maximum Concentration

(units)

Blank Action

Level (units)

Quantitation Limit (units)

Affected SamplesActions

benzaldehyde D05954 (EB)

15 ugL NA 100 ugKg Qualify as EB in samples D05950 D05951D05952 D05945 D05946 and D05949

acetophenone D05954 (EB)

0 35 ugL NA 100 ugKg Qualify as EB in sample D05951

4-chloro-3shymethylphenol

D05954 (EB)

5 6 ugL NA 100 ugKg 4-Chloro-3shymethylphenol was not detected in all associated samples No actions were required

di-n-butylphthalate D05954 (EB)

049 ugL NA 100 ugKg Di-n-butylphthalate results were reported from the SIM analyses No actions were required

di-n-butylphthalate method 42 ugKg 420 ugKg 100 ugKg Di-n-butylphthalate results were reported from the SIM analyses No actions were required

bis(2shyethylhexyl)phthalate

method 0 68 ugL 6 8 ugL 1 0 ugL Qualify as nondetect (U) at the QL m equipment blank sample D05954

J NEWA160 Troy Mills LandfillData VahdatwnDecember 20Q4DVMemossD05939_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 11 February 24 2005 Case 0251M SDGD05939

Compound Blank

Maximum Concentration

(units)

Blank Action

Level (units)

Quantitation Limit (units)

bis(2shyethylhexyl)phthalate

PES 490 ugKg 4900 ugKg 100 ugKg

NA - Not applicable SIM - selected ion monitoring EB - equipment blank PES - performance evaluation sample

Sample results were qualified as follows

Affected SamplesActions

Qualify as nondetect (U) at the QL in samples 005950005951 and D05952

bull If sample result was gtQL and ltblank action level (BAL) the result was qualified as a nondetect (U) at the reported concentration

bull If the sample result was sQL and iBAL the results was qualified as a nondetect (U) at the QL bull If the sample result was gtBAL qualification of the data was not required bull If the sample result was nondetect qualification of the data was not required bull Positive results for compounds detected in the equipment blank are flagged with EB

SIM

Target compounds were detected in the laboratory method blanks The following table summarizes the blank actions as they apply to the samples

Compound

di-n-buty Iphthalate

bis(2-ethylhexyl)phthalate

di-n-butylphthalate

Blank Maximum Action Quantitation

Concentration Level Limit Blank (umts^ (units) (units)

method 120ngL 1200 ngL 100 ngL

method 760 ngL 7600 ngL 1600 ngL

method 49 ugKg 490^1^ 10 ugKg

Affected SamplesActions

Qualify as nondetect (U) at the reported value in sample D05954

Bis(2shyethylhexyl)phthalate results were reported from the full scan analyses No actions vere required

Qualify as nondetect (U) at the reported value in all soil samples

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossD05939_nocsirn vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 12 February 24 2005 Case 0251M SDGD05939

Blank Maximum Action Quantitation

Concentration Level Limit Affected Compound Blank (units) (units) (units) Samples Actions

bis(2-ethylhexyl)phthalate method 31 ugKg 3 10 ugKg 160 MgKg Bis(2shyethylhexyl)phthalate results were reported from the full scan analyses No actions were required

Sample results were qualified as follows bull If sample result was gtQL and ltBAL the result was qualified as a nondetect (U) at the reported

concentration bull If the sample result was sQL and ltBAL the results was qualified as a nondetect (U) at the QL bull If the sample result was gtBAL qualification of the data was not required bull If the sample result was nondetect qualification of the data was not required

Internal Standards

Full scan

The following table summarizes the internal standards (IS) that did not meet the acceptable area criteria

Sample ID Internal Standard IS Area Acceptable Range Action

D05948 perylene-d|2 394921 407622-1630486 Results not reported from this analysis

D05948RE chrysene-d2 1720979 350682-1402728 Sample results associated with this IS were either not detected or were reported from the dilution analysis No data validation actions required

D05953 perylene-d2 311034 407622-1630486 Results not reported from this analysis

D05953RE chrysene-dl2 1565496 350682-1402728 Sample results associated with this IS were either not detected or were reported from the dilution analysis No data validation actions required

SIM

Internal standards were within the acceptance criteria in all sample analyses

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DV MemossD05939_svocsim npd Metcalfamp Eddy Inc

Ms Christine Clark Page 13 February 24 2005 Case 0251M SDG D05939

Sensitivity Check

Full Scan

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F05 (low-level)

SW122104F04 (high-level)

Compound

caprolactam

24-dimtrophenol

4-mtrophenol

46-dmitro-2-methylphenol

pentachlorophenol

caprolactam

Recovery Action

0 Raise the quantitation limit to the concentration of the high-level LFB (4 ngL) and qualify as estimated (UJ) the nondetect caprolactam result in sample D05954

0 Since the QL for this compound is 4 |igL the high level LFB (spiked at 4 ugL) was used to evaluate this compound for sensitivity

38 Qualify as estimated (UJ) the nondetect 4shynitrophenol result in sample D05954

38 Qualify as estimated (UJ) the nondetect 46shydimtro-2-methylphenol result in sample D05954

36 Qualify as estimated (UJ) the nondetect pentachlorophenol result in sample D05954

27 Raise the quantitation limit to the concentration of the high-level LFB (4 ugL) and qualify as estimated (UJ) the nondetect caprolactam result in sample D05954

QL - quantitation limit LFB - laboratory fortified blank

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound

SS012805FL01 24-dimethylphenol (low-level)

4-chloroanihne

Action Recovery

26 Qualify as estimated (UJ) the nondetect 24shydimethylphenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shychloroamlme results in all soil samples

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossD05939j5vocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark February 24 2005

LFB

SS012805FL01 (low-level)

SS012805FH01 (high-level)

SIM

Compound

24-dimtrophenol

4-mtrophenol

4 6-dimtro-2-methylphenol

pentachlorophenol

33-dichlorobenzidme

4-chloroanilme

24-dimtrophenol

Page 14 Case 0251M SDG D05939

Action Recovery

0 Raise the quantitation limit to the concentration of the high-level LFB [800 ngKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shynitrophenol results in all soil samples

13 Qualify as estimated (UJ) the nondetect 46shydmitro-2-methylphenol results in all soil samples

32 Qualify as estimated (UJ) the nondetect pentachlorophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 33shydichlorobenzidme results in all soil samples

39 Qualify as estimated (UJ) the nondetect 4shychloroamhne results in all soil samples

21 Raise the quantitation limit to the concentration of the high-level LFB [800 ugKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F03 (low-level)

SW122104F04 (high-level)

Compound

pentachlorophenol

di-n-butylphthalate

bis(2-ethylhexyl)phthalate

di-n-butylphthalate

Recovery

0

327

622

131

Action

Pentachlorophenol was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

J NEWA160 Tro Mills LandfillData VahdationDecember 2004DVMemossD05939_socsim npd Metcalf amp Eddy Inc

Ms Christine Clark Page 15 February 24 2005 Case0251M SDGD05939

LFB Compound Action Recovery

SW122104F04 bis(2-ethylhexyl)phthalate 161 Bis(2-ethylhexyl)phthalate was reported from the (high-level) full scan analysis therefore no actions were

required

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound Action Recovery

SS012805FL02 di-n-butylphthalate 237 Qualify as estimated (J) the positive di-nshy(low-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 376 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 149 Since the QL for this compound is 160 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

indeno( 1 23-cd)pyrene 121 Since the QL for this compound is 1 60 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

SS012805FH02 di-n-butylphthalate 150 Qualify as estimated (J) the positive di-nshy(high-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 185 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 132 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D0595 1 D05952 D05945 D05946 and D05949

QL - quantitation limit

PE Sample ResultsAccuracy Check

PE Sample Results

Full Scan

A single-blind solid PE sample D05939 (PES number SS0491) was analyzed with this data set Eight compounds were scored as Within Limits 2-Chlorophenol acenaphthylene acenaphthene dibenzofuran fluorene anthracene fluoranthene benzo(a)anthracene and chrysene were scored as

J NEWA160 Troy Mills LandfillData VahdatwnDecember 2004DVMemossD05939_svocsim vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 16 February 24 2005 Case 0251M SDGD05939

Action High These compounds were not detected in any of the associated soil samples therefore no data validation actions were required Six compounds (naphthalene hexachlorobenzene phenanthrene pyrene and dibenz(ah)anthracene and benzo(ghi)perylene) were scored as Warning High two compounds (4-hydroxy-4-methyl-2-pentanone and 4-methyl-3-penten-2-one) were scored Non-spiked TIC and one compound (din-n-butylphthalate) was scored Less than CRQL No data validation action is required on the basis of the Warning High Non-spiked TIC and less than CRQL scores Bis(2-ethylhexyl)phthalate was scored as Contaminant This compound was also detected in the associated laboratory method blanks and consequently evaluated in the blank section of this memorandum (please see Blanks above)

Laboratory Control Sample (LCS) Results

Full Scan

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LCS Compound Recovery Action

SW122104L06 caprolactam 35 Qualify as estimated (UJ) the nondetectresult in sample D05954

caprolactam

atrazine 135 Atrazine was not detected in the associaNo actions were required

ted sample

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Recovery Action

SS012805L01 benzaldehyde 46 Qualify as estimated (J) the positive and (UJ) the nondetect benzaldehyde results in all soil samples

4-chloroanihne 35 Qualify as estimated (UJ) the nondetect 4shychloroaruhne results in all soil samples

SIM

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossDQ5939_svocstm vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 17 February 24 2005 Case 0251M SDGD05939

LCS Compound Action Recovery

SW122104L05 pentachlorophenol 194 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 123 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(a)pyrene 122 Benzo(a)pyrene was not detected in the associated sample No actions were required

mdeno( 1 2 3 -cd)pyrene 130 Indeno(l23-cd)pyrene was reported from the full scan analysis therefore no actions were required

dibenz(ah)anthracene 136 Dibenz(ah)anthracene was not detected in the associated sample No actions were required

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Action Recovery

SS012805L02 pentachlorophenol 126 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 142 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(b)fluoranthene 128 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D05951 D05952 D05945 D05946 and D05949

benzo(a)pyrene 121 Qualify as estimated (J) the positive benzo(a)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

mdeno( 1 23-cd)pyrene 129 Qualify as estimated (J) the positive indeno(l23shycd)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

dibenz(ah)anthracene 133 Dibenz(ah)anthracene was not detected in the associated samples No actions were required

J NE WA160 Troy Mills LandfillData Validation December 2004 D V MemossD0593 9_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 18 February 24 2005 Case 0251M SDG D05939

Compound Ouantitation and Reported Ouantitation Limits

Full Scan and SIM

Because of their high moisture content samples D05945 D05946 D05949 D05951 and D05952 were freeze-dried prior to extraction

The following table summarizes the SIM and full scan reporting when data existed for both full scan and SIM analyses Professional judgment was used to select specific analyses in order to report the lowest quantitation limit achievable and to report results with values within the calibration range

Compound Results reported from Full Scan Results reported from SIM

pentachlorophenol all samples none

di-n-butyl phthalate none all samples

benzo(a)anthracene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

bis(2-ethylhexyl)phthalate all samples none

benzo(b)fluoranthene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

benzo(a)pyrene none all samples

indeno(l23-cd)pyrene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

dibenz(ah)anthracene none all samples

Full Scan

The bis(2-ethylhexyl)phthalate results in the following samples were reported from the dilution analysis listed in parentheses since these results exceeded the calibration range in the undiluted analysis D05945 (5x) D05946 (20x) D05947 (20x) D05948 (20x) D05949 (5x) and D05953 (20x)

JNE WA160 Troy Mills LandfillData ValidationDecember 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 19 February 24 2005 Case 0251M SDGD05939

SIM

The following compounds in the samples listed below were qualified as estimated (J) due to uncertainty in the quantitation as a result of the exceeded ion abundance ratio criteria

D05950 di-n-butylphthalate DOS951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate indeno(l23-cd)pyrene D05946 indeno(l23-cd)pyrene DOS 947 di-n-butylphthalate DOS 948 di-n-butylphthalate DOS 949 di-n-butylphthalate D05953 di-n-butylphthalate

Tentatively Identified Compounds (TICs)

One TIC 4-hydroxy-4-methyl-2-pentanone was detected in all samples and is considered an aldol condensation product Consequently this TIC was not included on Table III Tentatively Identified Compound Summary for the affected samples

The following compound in the sample listed was reported twice in the affected sample For this sample this result was renamed to a more general identification since a compound cannot elute at multiple retention times The renamed TIC is described in the table below

Compound name as reported by the Compound name as renamed during data Affected sample laboratory validation

oleic acid unknown D05951

JNEWA160 Troy Mills LandflllData ValidationDecember 2004DV MemossD05939_svocsimwpd MetcalfA Eddy Inc

Ms Christine Clark Page 20 February 24 2005 Case 0251M SDG D05939

Please contact Ms Constance Lapite at (781) 224-6628 or at Constance lapite(am-ecom if you have any questions regarding this Tier II validation

Paula L DiMattei Data Validator

Deborah A Trwini ^mjrjat

Robert Shoemaker Project Chemist

bullgt pound^ampgtlt^ Constance D Lapite MampE RAC Lead Chemist

cc ^James Chow EPA Remedial Project Manager (DV memo and data summary tables) Karen Wedlock-Hunt MampE Project Manager (entire package) Robert Shoemaker Project Chemist (entire package) Troy Mills Landfill Project File WA No 160-RICO-019M (entire package)

Attachments ORDA Table I Recommendation Summary Table Table II Overall Evaluation of Data Table III Tentatively Identified Compound Summary Data Summary Tables Data Validation Worksheets PE Score Report Copy of non-CLP Analytical Method (MampE DAS Specification D-148) Copies of Telephone LogCommunications Forms Supporting Data for Reduced Payment Recommendations (not applicable) Copies of Field Sampling Notes (previously submitted) Copies of EPA-Approved Amendments not QAPjP or SAP (not applicable) CSF Completeness Evidence File Audit (DC-2 Form) DQO Summary Form

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DVMemossD05939_svocsim pd Metcatfamp Eddy Inc

REGION I EPA-NE ORGANIC REGIONAL DATA ASSESSMENT (ORDA)

CASE raquozjggtH _ SITE NAME TV

LAB NAME uoAlaquo Vlaquo- amp+ OF SAMPLESMATRIX

SDG Posirt_ VALIDATION CONTRACTOR

SOW CONTRACT p-rttll-- VALIDATORS NAME

EPA-NE DV TIER LEVEL JC_ DATE DP RECD BY EPA-NE

TPOPO ACTION _ FYI ^ DV COMPLETION DATE

ANALYTICAL DATA QUALITY SUMMARY tffpft^m t~

bullVGA SV-SM PestPCB 1 Preservation and Contractual Holding Times 2 GCMS GCECD Instrument Performance Check raquo 3 Initial Calibration laquo 4 Continuing Calibration o 5 Blanks ~ o 6 Surrogate Compounds raquo 7 Internal Standards o 8 Matrix SpikeMatrix Spike Duplicate ggt 9 Sensitivity Check 0 10 PE Samples-Accuracy Check 0 11 Target Compound Identification jpy 12 Compound Quantitation and Reported QLs o 13 Tentatively Identified Compounds o 14 Semivolatile CleanupPesticidePCB Cleanup ulaquor 15 Data Completeness 0 16 Overall Evaluation of Data laquo

o = Data had no problems or were qualified due to minor contractual problems m = Data were qualified due to major contractual problems z = Data were rejected as unusable due major contractual problems

ACTION ITEMS (z items)

AREAS OF CONCERN (m items)

COMMENTS

This form assesses the analytical data quality in terms of contractual compliance only It does not assess sampling errors andor non-contractual analytical issues that affect data quality

Check ACTION only if contractual defects resulted in reduced paymentdata rejection recommendations

Validator t ltiJSagt3gtlt -3 Date

INSTRUCTIONS ON REVERSE SIDE

1296

Table I Recommendation Summary

Soil Semivolatile Organic Analysis Troy Mills Landfill Superfund Site

Case0251M SDGD05939

Sample ID Matrix

D05945 SO

D05946 SO

D05947 SO (FD)

D05948 SO

D05949 SO

D05950 SO

D05951 SO

D05952 SO

D05953 SO (FD)

D05954 EB

EB shy Equipment Blank FD shy Field Duplicate SOshy Soil

Qualifier

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 11 13 14 15

2 Jl 3 4 7 8 9 10 13 15

A 2 jl 3 4 7 8 9 10 13 15

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 jl 3 4 7 8 9 10 13 15

A 2 3 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 Jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 13 15

^2 4 jl 2 3 5 6 7 12

A - Accept the data but qualify the positive results for benzaldehyde in samples D05945 D05946 D05949 D05950 D05951 and D05952 and for acetophenone in sample D05951 as (EB) due to equipment blank contamination

A2 - Accept the data but qualify the positive result for di-n-butylphthalate as nondetect (U) at the reported value due to laboratory method blank contamination

A5 - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to PE sample contamination

A - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to laboratory method blank contamination

J - Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde hexachlorocyclopentadiene 24shydmitrophenol 46-dmitro-2-methylphenol atrazine and pentachlorophenol due to initial calibration RSD exceedances

J2 Estimate (J) the positive result for di-n-butyl phthalate due to the initial calibration RSD exceedance

J3 Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde and 33-dichlorobenzidme in all samples for hexachlorobutadiene 4-mtrophenol and hexachlorobenzene m samples D05948 D05949 and D05953 for hexachlorocyclopentadiene m samples D05954 D05948 D05949 and D05953 and for 24shydimtrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 due to the continuing calibration D exceedances

J4 - Estimate (J) the positive results for di-n-butylphthalate in all soil samples due to continuing calibration exceedance

J5 - Estimate (UJ) the nondetect caprolactam result and raise the quantitation limit to 4 ugL (equivalent to the concentration of the high-level LFB) due to low low-level and high-level LFB recoveries This result may be biased low

J6 - Estimate (UJ) the nondetect results for 4-mtrophenol 46-dmitro-2-methylphenol and pentachlorophenol due to low low-level LFB recoveries These results may be biased low

J7 - Estimate (J) the positive result for di-n-butylphthalate due to high low-level and high-level LFB recoveries This result may be biased high

J8 - Estimate (UJ) the nondetect 24-dmitrophenol result and raise the quantitation limit to 800 ugKg (equivalent to the concentration of the high-level LFB and corrected for all preparation factors) due to low low-level and high-level LFB recoveries This result may be biased low

J9 - Estimate (UJ) the nondetect results for 24-dimethylphenol 4-mtrophenol 46-dimrro-2-methylphenol pentachlorophenol and 33-dichlorobenzidme due to low low-level LFB recoveries These results may be biased low

J10 - Estimate (UJ) the nondetect result 4-chIoroamlme due to low low-level and high-le el LFB recoveries This result may be biased low

J1 - Estimate (J) the positive result for benzo(b)fluoranthene due to high high-level LFB reco ery This result may be biased high

J12 - Estimate (UJ) the nondetect caprolactam result due to low LCS recovery This result may be biased low

J3 - Estimate (UJ) the nondetect benzaldehyde and 4-chloroamline results due to low LCS recoveries The results may be biased low

J14 - Estimate (J) the positive results for benzo(b)fluoranthene benzo(a)pyrene and mdeno(l23-cd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 due to high LCS recoveries The results may be biased high

J15 - Estimate (J) the positive results for the following compounds in the samples listed below due to uncertainty in the quantitation as a result of the exceeded ion abundance ration criteria

DOS 950 di-n-butylphthalate DOS 951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate mdeno(l23-cd)pyrene D05946 mdeno(l23-cd)pyrene D05947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate D05953 di-n-butylphthalate

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Page 2: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

Ms Christine Clark Page 2 February 24 2005 Case 0251M SDG D05939

The Tier II validation for the SVOC data was based on an evaluation of the following parameters

bull Overall Evaluation of Data and Potential Usability Issues Data Completeness (CSF Audit)

bull Preservation and Technical Holding Times bull GCMS Instrument Performance Checks

bull Initial and Continuing Calibrations bull Blanks

bull Surrogate Spike Recoveries bull Internal Standards

bull Matrix SpikeMatrix Spike Duplicate (MSMSD) bull Field Duplicates

bull Sensitivity Check bull PE Sample ResultsAccuracy Check

NA bull Target Compound Identification bull Sample Quantitation and Reported Quantitation Limits

Tentatively Identified Compounds NA bull Semivolatile Cleanup NA bull System Performance

- All quality control criteria were met for this parameter NA - Not applicable to the analytical method or to a Tier II validation

Note Worksheets are not included for parameters that have met criteria or for criteria that are not applicable to a Tier II data validation

Copies of the field logbook and field sampling notes for this sample delivery group (SDG) may be found as an attachment to Case 0251M SDG D05916 which was previously submitted to the EPA

The following information was used to generate the Data Validation Memorandum attachments

Table I Recommendation Summary Table - summarizes validation recommendations Table II Overall Evaluation of Data - summarizes site DQOs and potential usability issues Table III Tentatively Identified Compound Summary Data Summary Tables - summarizes accepted qualified and rejected data

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossD05939_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 3 February 24 2005 Case 0251M SDG D05939

Overall Evaluation of Data and Potential Usability Issues

The following is a summary of the site DQOs (Data Quality Objectives)

bull To determine the nature and extent of contamination following the completion of two removal actions in order to perform human health and ecological risk assessments and thereby recommend a remedy to eliminate reduce or control risks to human health and the environment

The sample data were qualified as a result of sampling and analytical error Qualifications as a result of sampling error are summarized below

The positive results for benzaldehyde in soil samples D05945 D05946 D05949 D05950 D05951 and D05952 and for acetophenone in soil sample D05951 were flagged EB due to equipment blank contamination The end data user should consider that an indeterminate amount of sampling error may have affected these sample results The results are usable for project objectives These qualifications have a minor impact on data usability

Qualifications as a result of analytical error are summarized below

bull The positive and nondetect results for benzaldehyde hexachlorocyclopentadiene 24-dinitrophenol 46-dinitro-2-methylphenol atrazine and pentachlorophenol in all samples were qualified as estimated (J and UJ respectively) due to the percent relative standard deviation (RSD) exceedances in the initial calibration All results are usable for project objectives as estimated values and as nondetect results with estimated quantitation limits These qualifications have a minor impact on data usability

bull The positive and nondetect results for benzaldehyde and 33-dichlorobenzidine in all samples for hexachlorobutadiene 4-nitrophenol and hexachlorobenzene in samples D05948 D05949 and D05953 for hexachlorocyclopentadiene in samples D05954 D05948 D05949 and D05953 and for 24-dinitrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 were qualified as estimated (J and UJ respectively) due to the percent difference (D) exceedances in the continuing calibrations These results are usable for project objectives as estimated values and as nondetect results with estimated quantitation limits These qualifications have a minor impact on data usability

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DVMemossD05939_socsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 4 February 24 2005 Case 0251M SDG D05939

bull The positive di-n-butylphthalate result in equipment blank sample D05954 was qualified as estimated (J) due to the RSD exceedance in the initial calibration This result is usable for project objective as an estimated value Note that this result was also qualified as nondetect (U) due to method blank contamination Therefore the overall qualification for this result is estimated nondetect (UJ) These qualifications have a minor impact on data usability

bull The positive di-n-butylphthalate results in all soil samples were qualified as estimated (J) due to the D exceedance in the continuing calibration These results are usable for project objectives as estimated values Note that the di-nshybutylphthalate results in all soil samples were also qualified as nondetect (U) due to method blank contamination Therefore the overall qualification for these results is estimated nondetect (UJ) These qualifications have a minor impact on data usability

bull The positive result for di-n-butylphthalate in equipment blank sample D05954 was qualified as nondetect (U) at the reported value due to method blank contamination This result is usable for project objectives as a nondetect Note that this result was also qualified as estimated (J) due to calibration nonconformances and high recoveries in the low-level and high-level laboratory fortified blanks (LFBs) Therefore the overall qualification for this result is estimated nondetect (UJ) These qualifications have a minor impact on data usability

bull The positive result for bis(2-ethylhexyl)phthalate in equipment blank sample D05954 was qualified as nondetect (U) at the quantitation limit (QL) due to method blank contamination This result is usable for project objectives as a nondetect This qualification has a minor impact on data usability

bull The positive results for di-n-butylphthalate in all soil samples were qualified as nondetect (U) at the reported values due to method blank contamination These results are usable for project objectives as nondetects Note that the di-nshybutylphthalate results in all soil samples were also qualified as estimated (J) due to calibration nonconformances high recoveries in the low-level and high-level LFBs andor ion abundance ratio exceedances Therefore the overall qualification for these results is estimated nondetect (UJ) These qualifications have a minor impact on data usability

bull The positive results for bis(2-ethylhexyl)phthalate in samples D05950 D05951 and D05952 were qualified as nondetect (U) at the QL due to performance evaluation sample contamination These results are usable for project objectives as nondetects These qualifications have a minor impact on data usability

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DV MemossD05939_svocsim wpd MetcalfA Eddy Inc

Ms Christine Clark Page 5 February 24 2005 Case 0251M SDG D05939

bull The nondetect result for caprolactam in equipment blank sample D05954 was qualified as estimated (UJ) at the raised quantitation limit [equivalent to the concentration of the high-level LFB (4 ugL)] due to low recoveries in the low-level and high-level LFB analyses This result is usable for project objectives as a nondetect with a raised and estimated quantitation limit that may be biased low This qualification has a minor impact on data usability

bull The nondetect results for 4-nitrophenol 46-dinitro-2-methylphenol and pentachlorophenol in equipment blank sample D05954 were qualified as estimated (UJ) due to low recoveries in the low-level LFB analyses These results are usable for project objectives as nondetects with estimated quantitation limits that may be biased low These qualifications have a minor impact on data usability

bull The positive result for di-n-butylphthalate in equipment blank sample D05954 was qualified as estimated (J) due to high recoveries in the low-level and high-level LFB analyses This result is usable for project objectives as an estimated value that may be biased high Note that this result was also qualified as nondetect (U) due to method blank contamination Therefore the overall qualification for this result is estimated nondetect (UJ) These qualifications have a minor impact on data usability

bull The nondetect results for 24-dinitrophenol in all soil samples were qualified as estimated (UJ) at the raised quantitation limit [equivalent to the concentration of the high-level LFB (800 ugKg) and corrected for all preparation factors] due to low recoveries in the low-level and high-level LFB analyses These results are usable for project objectives as nondetects with raised and estimated quantitation limits that may be biased low These qualifications have a minor impact on data usability

bull The nondetect results for 24-dimethylphenol 4-nitrophenol 46-dinitro-2shymethylphenol pentachlorophenol and 33-dichlorobenzidine in all soil samples were qualified as estimated (UJ) due to low recoveries in the low-level LFB analyses These results are usable for project objectives as nondetects with estimated quantitation limits that may be biased low These qualifications have a minor impact on data usability

bull The nondetect results for 4-chloroaniline in all soil samples were qualified as estimated (UJ) due to low recoveries in the low-level and high-level LFB analyses These results are usable for project objectives as nondetects with estimated quantitation limits that maybe biased low These qualifications have a minor impact on data usability

J NEWA160 Troy Mills LandfiMData VahdationDecember 2004DV MemossD05939_svocsm pd Metcalfamp Eddy Inc

Ms Christine Clark Page 6 February 24 2005 Case 0251M SDG D05939

The positive results for di-n-butylphthalate in all soil samples were qualified as estimated (J) due to high recoveries in the low-level and high-level LFB analyses These results are usable for project objectives as estimated values that maybe biased high Note that the di-n-butylphthalate results in all soil samples were also qualified as nondetect (U) due to method blank contamination Therefore the overall qualification for these results is estimated nondetect (UJ) These qualifications have a minor impact on data usability

The positive results for benzo(b)fluoranthene in samples D05951 D05952 D05945 D05946 and D05949 were qualified as estimated (J) due to high recovery in the high-level LFB analyses These results are usable for project objectives as estimated values that may be biased high These qualifications have a minor impact on data usability

The nondetect result for caprolactam in equipment blank sample D05954 was qualified as estimated (UJ) due to the low recovery in the laboratory control sample (LCS) analysis This result is usable for project objectives as a nondetect with an estimated quantitation limit that may be biased low These qualifications have a minor impact on data usability

The nondetect results for benzaldehyde and 4-chloroaniline in all soil samples were qualified as estimated (UJ) due to low recoveries in the LCS analyses These results are usable for project objectives as nondetects with estimated quantitation limits that may be biased low These qualifications have a minor impact on data usability

The positive results for benzo(b)fluoranthene benzo(a)pyrene and indeno(l23shycd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 were qualified as estimated (J) due to the high recoveries in the LCS analyses These results are usable for project objectives as estimated values that may be biased high These qualifications have a minor impact on data usability

JNEWAI60 Troy Mills LandfillData ValidationDecember 2004DV MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 7 February 24 2005 Case 0251M SDG D05939

bull The following compounds in the samples listed below were qualified as estimated (J) due to uncertainty in the quantitation as a result of the exceeded ion abundance ratio criteria These results are usable for project objectives as estimated values Note that the results for di-n-butylphthalate in samples D05950 D05951 D05952 D05945 D05947 D05948 D05949 and D05953 were also qualified as nondetect (U) due to method blank contamination Therefore the overall qualification for these results is estimated nondetect (UJ) These qualifications have a minor impact on data usability

D05950 di-n-butylphthalate D05951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate indeno(l23-cd)pyrene D05946 indeno(l23-cd)pyrene DOS 947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate DOS 95 3 di-n-butylphthalate

Data Completeness (CSF Audit)

The following information was missing or incorrect in the data package This missing or incorrect information was requested from the laboratory on February 7 and 152005 A resubmittal response was received at MampE on February 18 2005 adequately addressing these issues

bull The method detection limit (MDL) study results for two selected ion monitoring (SIM) compounds (pentachlorophenol and di-n-butylphthalate) were missing from the data package

The Form I (TIC) for sample D05946 identified the TIC at 1246 as alphashycaryophyllene while the raw data reported this TIC as l6-octadien-3-ol 37shydimethyl- Clarification was requested

bull The Form I for sample D05949 reported 26-dinitrotoluene and fluoranthene while the quantitation report did not reflect these results The laboratory was asked to verify this discrepancy

bull A relative response factor for 46-dinitro-2-methylphenol was listed on the Form 6 for the initial calibration in association with the 05 ugml standard However this compound was not listed on the quantitation report in the raw data The laboratory was asked to verify this discrepancy

J NEWA16Q Troy Mills LandfillData VahdationDecember 2004DV MemossD05939_svocsim pd Metcalf amp Eddy Inc

Ms Christine Clark Page 8 February 24 2005 Case 0251M SDG D05939

Initial and Continuing Calibrations

Full Scan

The following table summarizes the initial calibration (1C) and continuing calibration (CC) results that failed to meet the relative response factor (RRF) criterion of ^005 andor RSD lt 30 in the 1C andor D lt 25 in the CC for all compounds

Calibration Date 1C CC CC CC 12505 12705 13105 2105

Compound RSD D D D

benzaldehyde 792 155 156 153

hexachlorobutadiene - - - 453

hexachlorocyc lopentadiene 488 448 - 360

24-dimtrophenol 337 - 25 8 -

4-nitrophenol - - - 467

hexachlorobenzene - - - 286

46-dimtro-2-methylphenol 450 - - -

atrazme 434 - - -

pentachlorophenol 384 - - -

33-dichlorobenzidme - 726 463 628

2-fluorophenol (surrogate) - - - 285

Associated samples All samples D05954 D05950 D05951 D05948RE D05952 D05945 D05949 D05946 D05947 D05953RE D05948 D05953 D05949DL

D05945DL D05946DL D05947DL D05948DL D05953DL

- - QC acceptance criteria were not exceeded for this compound

Actions RSD gt 30 Estimate (J and UJ respectively) positive and nondetect results D gt 25 Estimate (J and UJ respectively) positive and nondetect results

JNEWA160 Troy Mills LandftllData VahdationDecember 2004DV MemossD05939_socsim pd Metcalf amp Eddy Inc

Ms Christine Clark Page 9 February 24 2005 Case 0251M SDGD05939

The positive and nondetect results for benzaldehyde hexachlorocyclopentadiene 24-dinitrophenol 46-dinitro-2-methylphenol atrazine and pentachlorophenol in all samples were qualified as estimated (UJ) due to initial calibration RSD exceedances

The positive and nondetect results for benzaldehyde and 33-dichlorobenzidine in all samples for hexachlorobutadiene 4-nitrophenol and hexachlorobenzene in samples D05948RE D05949 and D05953RE for hexachlorocyclopentadiene in samples D05954 D05948RE D05949 and D05953RE and for 24-dinitrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 were qualified as estimated (J and UJ respectively) due to continuing calibration D exceedances

No validation actions were necessary for the calibration nonconformances associated with the dilution sample analyses or for the original analyses of samples D05948 and D05953 since the compounds listed in the table above were not reported from these analyses

No validation actions were necessary for the surrogate compound calibration nonconformance

SIM

The following table summarizes the 1C and CC results that failed to meet the RRF criterion of gt005 andor RSD lt 30 in the 1C andor D lt 25 in the CC for all compounds

Calibration Date 1C 12105 1C 2205 CC 2305

Compound RSD RSD D

pentachlorophenol 621 402 -

di-n-butyl phthalate 331 - 297

bis(2-ethylhexyl)phthalate 347 306

Associated samples D05954 all soil samples all soil samples

- - QC acceptance criteria were not exceeded for this compound

Actions RSD gt 30 Estimate (J and UJ respectively) positive and nondetect results D gt 25 Estimate (J and UJ respectively) positive and nondetect results

The positive di-n-butylphthalate result in equipment blank sample D05954 was qualified as estimated (J) due to the RSD exceedance in the initial calibration

The positive di-n-butylphthalate results in all soil samples were qualified as estimated (J) due to the D exceedance in the continuing calibration

J NE WA160 Troy Mills LandfillData Validation December 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 10 February 24 2005 Case 0251M SDG D05939

The pentachlorophenol and bis(2-ethylhexyl)phthalate results in all samples were reported from the full scan analyses therefore no data validation actions were required as a result of the calibration nonconformances

Blanks

Full Scan

Target compounds were detected as contaminants m the performance evaluation sample (PES) as well as the equipment and laboratory method blanks The highest concentration detected was used to qualify associated sample results The following table summarizes the blank actions as they apply to the samples

Compound Blank

Maximum Concentration

(units)

Blank Action

Level (units)

Quantitation Limit (units)

Affected SamplesActions

benzaldehyde D05954 (EB)

15 ugL NA 100 ugKg Qualify as EB in samples D05950 D05951D05952 D05945 D05946 and D05949

acetophenone D05954 (EB)

0 35 ugL NA 100 ugKg Qualify as EB in sample D05951

4-chloro-3shymethylphenol

D05954 (EB)

5 6 ugL NA 100 ugKg 4-Chloro-3shymethylphenol was not detected in all associated samples No actions were required

di-n-butylphthalate D05954 (EB)

049 ugL NA 100 ugKg Di-n-butylphthalate results were reported from the SIM analyses No actions were required

di-n-butylphthalate method 42 ugKg 420 ugKg 100 ugKg Di-n-butylphthalate results were reported from the SIM analyses No actions were required

bis(2shyethylhexyl)phthalate

method 0 68 ugL 6 8 ugL 1 0 ugL Qualify as nondetect (U) at the QL m equipment blank sample D05954

J NEWA160 Troy Mills LandfillData VahdatwnDecember 20Q4DVMemossD05939_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 11 February 24 2005 Case 0251M SDGD05939

Compound Blank

Maximum Concentration

(units)

Blank Action

Level (units)

Quantitation Limit (units)

bis(2shyethylhexyl)phthalate

PES 490 ugKg 4900 ugKg 100 ugKg

NA - Not applicable SIM - selected ion monitoring EB - equipment blank PES - performance evaluation sample

Sample results were qualified as follows

Affected SamplesActions

Qualify as nondetect (U) at the QL in samples 005950005951 and D05952

bull If sample result was gtQL and ltblank action level (BAL) the result was qualified as a nondetect (U) at the reported concentration

bull If the sample result was sQL and iBAL the results was qualified as a nondetect (U) at the QL bull If the sample result was gtBAL qualification of the data was not required bull If the sample result was nondetect qualification of the data was not required bull Positive results for compounds detected in the equipment blank are flagged with EB

SIM

Target compounds were detected in the laboratory method blanks The following table summarizes the blank actions as they apply to the samples

Compound

di-n-buty Iphthalate

bis(2-ethylhexyl)phthalate

di-n-butylphthalate

Blank Maximum Action Quantitation

Concentration Level Limit Blank (umts^ (units) (units)

method 120ngL 1200 ngL 100 ngL

method 760 ngL 7600 ngL 1600 ngL

method 49 ugKg 490^1^ 10 ugKg

Affected SamplesActions

Qualify as nondetect (U) at the reported value in sample D05954

Bis(2shyethylhexyl)phthalate results were reported from the full scan analyses No actions vere required

Qualify as nondetect (U) at the reported value in all soil samples

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossD05939_nocsirn vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 12 February 24 2005 Case 0251M SDGD05939

Blank Maximum Action Quantitation

Concentration Level Limit Affected Compound Blank (units) (units) (units) Samples Actions

bis(2-ethylhexyl)phthalate method 31 ugKg 3 10 ugKg 160 MgKg Bis(2shyethylhexyl)phthalate results were reported from the full scan analyses No actions were required

Sample results were qualified as follows bull If sample result was gtQL and ltBAL the result was qualified as a nondetect (U) at the reported

concentration bull If the sample result was sQL and ltBAL the results was qualified as a nondetect (U) at the QL bull If the sample result was gtBAL qualification of the data was not required bull If the sample result was nondetect qualification of the data was not required

Internal Standards

Full scan

The following table summarizes the internal standards (IS) that did not meet the acceptable area criteria

Sample ID Internal Standard IS Area Acceptable Range Action

D05948 perylene-d|2 394921 407622-1630486 Results not reported from this analysis

D05948RE chrysene-d2 1720979 350682-1402728 Sample results associated with this IS were either not detected or were reported from the dilution analysis No data validation actions required

D05953 perylene-d2 311034 407622-1630486 Results not reported from this analysis

D05953RE chrysene-dl2 1565496 350682-1402728 Sample results associated with this IS were either not detected or were reported from the dilution analysis No data validation actions required

SIM

Internal standards were within the acceptance criteria in all sample analyses

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DV MemossD05939_svocsim npd Metcalfamp Eddy Inc

Ms Christine Clark Page 13 February 24 2005 Case 0251M SDG D05939

Sensitivity Check

Full Scan

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F05 (low-level)

SW122104F04 (high-level)

Compound

caprolactam

24-dimtrophenol

4-mtrophenol

46-dmitro-2-methylphenol

pentachlorophenol

caprolactam

Recovery Action

0 Raise the quantitation limit to the concentration of the high-level LFB (4 ngL) and qualify as estimated (UJ) the nondetect caprolactam result in sample D05954

0 Since the QL for this compound is 4 |igL the high level LFB (spiked at 4 ugL) was used to evaluate this compound for sensitivity

38 Qualify as estimated (UJ) the nondetect 4shynitrophenol result in sample D05954

38 Qualify as estimated (UJ) the nondetect 46shydimtro-2-methylphenol result in sample D05954

36 Qualify as estimated (UJ) the nondetect pentachlorophenol result in sample D05954

27 Raise the quantitation limit to the concentration of the high-level LFB (4 ugL) and qualify as estimated (UJ) the nondetect caprolactam result in sample D05954

QL - quantitation limit LFB - laboratory fortified blank

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound

SS012805FL01 24-dimethylphenol (low-level)

4-chloroanihne

Action Recovery

26 Qualify as estimated (UJ) the nondetect 24shydimethylphenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shychloroamlme results in all soil samples

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossD05939j5vocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark February 24 2005

LFB

SS012805FL01 (low-level)

SS012805FH01 (high-level)

SIM

Compound

24-dimtrophenol

4-mtrophenol

4 6-dimtro-2-methylphenol

pentachlorophenol

33-dichlorobenzidme

4-chloroanilme

24-dimtrophenol

Page 14 Case 0251M SDG D05939

Action Recovery

0 Raise the quantitation limit to the concentration of the high-level LFB [800 ngKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shynitrophenol results in all soil samples

13 Qualify as estimated (UJ) the nondetect 46shydmitro-2-methylphenol results in all soil samples

32 Qualify as estimated (UJ) the nondetect pentachlorophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 33shydichlorobenzidme results in all soil samples

39 Qualify as estimated (UJ) the nondetect 4shychloroamhne results in all soil samples

21 Raise the quantitation limit to the concentration of the high-level LFB [800 ugKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F03 (low-level)

SW122104F04 (high-level)

Compound

pentachlorophenol

di-n-butylphthalate

bis(2-ethylhexyl)phthalate

di-n-butylphthalate

Recovery

0

327

622

131

Action

Pentachlorophenol was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

J NEWA160 Tro Mills LandfillData VahdationDecember 2004DVMemossD05939_socsim npd Metcalf amp Eddy Inc

Ms Christine Clark Page 15 February 24 2005 Case0251M SDGD05939

LFB Compound Action Recovery

SW122104F04 bis(2-ethylhexyl)phthalate 161 Bis(2-ethylhexyl)phthalate was reported from the (high-level) full scan analysis therefore no actions were

required

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound Action Recovery

SS012805FL02 di-n-butylphthalate 237 Qualify as estimated (J) the positive di-nshy(low-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 376 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 149 Since the QL for this compound is 160 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

indeno( 1 23-cd)pyrene 121 Since the QL for this compound is 1 60 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

SS012805FH02 di-n-butylphthalate 150 Qualify as estimated (J) the positive di-nshy(high-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 185 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 132 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D0595 1 D05952 D05945 D05946 and D05949

QL - quantitation limit

PE Sample ResultsAccuracy Check

PE Sample Results

Full Scan

A single-blind solid PE sample D05939 (PES number SS0491) was analyzed with this data set Eight compounds were scored as Within Limits 2-Chlorophenol acenaphthylene acenaphthene dibenzofuran fluorene anthracene fluoranthene benzo(a)anthracene and chrysene were scored as

J NEWA160 Troy Mills LandfillData VahdatwnDecember 2004DVMemossD05939_svocsim vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 16 February 24 2005 Case 0251M SDGD05939

Action High These compounds were not detected in any of the associated soil samples therefore no data validation actions were required Six compounds (naphthalene hexachlorobenzene phenanthrene pyrene and dibenz(ah)anthracene and benzo(ghi)perylene) were scored as Warning High two compounds (4-hydroxy-4-methyl-2-pentanone and 4-methyl-3-penten-2-one) were scored Non-spiked TIC and one compound (din-n-butylphthalate) was scored Less than CRQL No data validation action is required on the basis of the Warning High Non-spiked TIC and less than CRQL scores Bis(2-ethylhexyl)phthalate was scored as Contaminant This compound was also detected in the associated laboratory method blanks and consequently evaluated in the blank section of this memorandum (please see Blanks above)

Laboratory Control Sample (LCS) Results

Full Scan

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LCS Compound Recovery Action

SW122104L06 caprolactam 35 Qualify as estimated (UJ) the nondetectresult in sample D05954

caprolactam

atrazine 135 Atrazine was not detected in the associaNo actions were required

ted sample

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Recovery Action

SS012805L01 benzaldehyde 46 Qualify as estimated (J) the positive and (UJ) the nondetect benzaldehyde results in all soil samples

4-chloroanihne 35 Qualify as estimated (UJ) the nondetect 4shychloroaruhne results in all soil samples

SIM

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossDQ5939_svocstm vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 17 February 24 2005 Case 0251M SDGD05939

LCS Compound Action Recovery

SW122104L05 pentachlorophenol 194 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 123 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(a)pyrene 122 Benzo(a)pyrene was not detected in the associated sample No actions were required

mdeno( 1 2 3 -cd)pyrene 130 Indeno(l23-cd)pyrene was reported from the full scan analysis therefore no actions were required

dibenz(ah)anthracene 136 Dibenz(ah)anthracene was not detected in the associated sample No actions were required

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Action Recovery

SS012805L02 pentachlorophenol 126 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 142 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(b)fluoranthene 128 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D05951 D05952 D05945 D05946 and D05949

benzo(a)pyrene 121 Qualify as estimated (J) the positive benzo(a)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

mdeno( 1 23-cd)pyrene 129 Qualify as estimated (J) the positive indeno(l23shycd)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

dibenz(ah)anthracene 133 Dibenz(ah)anthracene was not detected in the associated samples No actions were required

J NE WA160 Troy Mills LandfillData Validation December 2004 D V MemossD0593 9_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 18 February 24 2005 Case 0251M SDG D05939

Compound Ouantitation and Reported Ouantitation Limits

Full Scan and SIM

Because of their high moisture content samples D05945 D05946 D05949 D05951 and D05952 were freeze-dried prior to extraction

The following table summarizes the SIM and full scan reporting when data existed for both full scan and SIM analyses Professional judgment was used to select specific analyses in order to report the lowest quantitation limit achievable and to report results with values within the calibration range

Compound Results reported from Full Scan Results reported from SIM

pentachlorophenol all samples none

di-n-butyl phthalate none all samples

benzo(a)anthracene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

bis(2-ethylhexyl)phthalate all samples none

benzo(b)fluoranthene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

benzo(a)pyrene none all samples

indeno(l23-cd)pyrene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

dibenz(ah)anthracene none all samples

Full Scan

The bis(2-ethylhexyl)phthalate results in the following samples were reported from the dilution analysis listed in parentheses since these results exceeded the calibration range in the undiluted analysis D05945 (5x) D05946 (20x) D05947 (20x) D05948 (20x) D05949 (5x) and D05953 (20x)

JNE WA160 Troy Mills LandfillData ValidationDecember 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 19 February 24 2005 Case 0251M SDGD05939

SIM

The following compounds in the samples listed below were qualified as estimated (J) due to uncertainty in the quantitation as a result of the exceeded ion abundance ratio criteria

D05950 di-n-butylphthalate DOS951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate indeno(l23-cd)pyrene D05946 indeno(l23-cd)pyrene DOS 947 di-n-butylphthalate DOS 948 di-n-butylphthalate DOS 949 di-n-butylphthalate D05953 di-n-butylphthalate

Tentatively Identified Compounds (TICs)

One TIC 4-hydroxy-4-methyl-2-pentanone was detected in all samples and is considered an aldol condensation product Consequently this TIC was not included on Table III Tentatively Identified Compound Summary for the affected samples

The following compound in the sample listed was reported twice in the affected sample For this sample this result was renamed to a more general identification since a compound cannot elute at multiple retention times The renamed TIC is described in the table below

Compound name as reported by the Compound name as renamed during data Affected sample laboratory validation

oleic acid unknown D05951

JNEWA160 Troy Mills LandflllData ValidationDecember 2004DV MemossD05939_svocsimwpd MetcalfA Eddy Inc

Ms Christine Clark Page 20 February 24 2005 Case 0251M SDG D05939

Please contact Ms Constance Lapite at (781) 224-6628 or at Constance lapite(am-ecom if you have any questions regarding this Tier II validation

Paula L DiMattei Data Validator

Deborah A Trwini ^mjrjat

Robert Shoemaker Project Chemist

bullgt pound^ampgtlt^ Constance D Lapite MampE RAC Lead Chemist

cc ^James Chow EPA Remedial Project Manager (DV memo and data summary tables) Karen Wedlock-Hunt MampE Project Manager (entire package) Robert Shoemaker Project Chemist (entire package) Troy Mills Landfill Project File WA No 160-RICO-019M (entire package)

Attachments ORDA Table I Recommendation Summary Table Table II Overall Evaluation of Data Table III Tentatively Identified Compound Summary Data Summary Tables Data Validation Worksheets PE Score Report Copy of non-CLP Analytical Method (MampE DAS Specification D-148) Copies of Telephone LogCommunications Forms Supporting Data for Reduced Payment Recommendations (not applicable) Copies of Field Sampling Notes (previously submitted) Copies of EPA-Approved Amendments not QAPjP or SAP (not applicable) CSF Completeness Evidence File Audit (DC-2 Form) DQO Summary Form

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DVMemossD05939_svocsim pd Metcatfamp Eddy Inc

REGION I EPA-NE ORGANIC REGIONAL DATA ASSESSMENT (ORDA)

CASE raquozjggtH _ SITE NAME TV

LAB NAME uoAlaquo Vlaquo- amp+ OF SAMPLESMATRIX

SDG Posirt_ VALIDATION CONTRACTOR

SOW CONTRACT p-rttll-- VALIDATORS NAME

EPA-NE DV TIER LEVEL JC_ DATE DP RECD BY EPA-NE

TPOPO ACTION _ FYI ^ DV COMPLETION DATE

ANALYTICAL DATA QUALITY SUMMARY tffpft^m t~

bullVGA SV-SM PestPCB 1 Preservation and Contractual Holding Times 2 GCMS GCECD Instrument Performance Check raquo 3 Initial Calibration laquo 4 Continuing Calibration o 5 Blanks ~ o 6 Surrogate Compounds raquo 7 Internal Standards o 8 Matrix SpikeMatrix Spike Duplicate ggt 9 Sensitivity Check 0 10 PE Samples-Accuracy Check 0 11 Target Compound Identification jpy 12 Compound Quantitation and Reported QLs o 13 Tentatively Identified Compounds o 14 Semivolatile CleanupPesticidePCB Cleanup ulaquor 15 Data Completeness 0 16 Overall Evaluation of Data laquo

o = Data had no problems or were qualified due to minor contractual problems m = Data were qualified due to major contractual problems z = Data were rejected as unusable due major contractual problems

ACTION ITEMS (z items)

AREAS OF CONCERN (m items)

COMMENTS

This form assesses the analytical data quality in terms of contractual compliance only It does not assess sampling errors andor non-contractual analytical issues that affect data quality

Check ACTION only if contractual defects resulted in reduced paymentdata rejection recommendations

Validator t ltiJSagt3gtlt -3 Date

INSTRUCTIONS ON REVERSE SIDE

1296

Table I Recommendation Summary

Soil Semivolatile Organic Analysis Troy Mills Landfill Superfund Site

Case0251M SDGD05939

Sample ID Matrix

D05945 SO

D05946 SO

D05947 SO (FD)

D05948 SO

D05949 SO

D05950 SO

D05951 SO

D05952 SO

D05953 SO (FD)

D05954 EB

EB shy Equipment Blank FD shy Field Duplicate SOshy Soil

Qualifier

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 11 13 14 15

2 Jl 3 4 7 8 9 10 13 15

A 2 jl 3 4 7 8 9 10 13 15

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 jl 3 4 7 8 9 10 13 15

A 2 3 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 Jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 13 15

^2 4 jl 2 3 5 6 7 12

A - Accept the data but qualify the positive results for benzaldehyde in samples D05945 D05946 D05949 D05950 D05951 and D05952 and for acetophenone in sample D05951 as (EB) due to equipment blank contamination

A2 - Accept the data but qualify the positive result for di-n-butylphthalate as nondetect (U) at the reported value due to laboratory method blank contamination

A5 - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to PE sample contamination

A - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to laboratory method blank contamination

J - Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde hexachlorocyclopentadiene 24shydmitrophenol 46-dmitro-2-methylphenol atrazine and pentachlorophenol due to initial calibration RSD exceedances

J2 Estimate (J) the positive result for di-n-butyl phthalate due to the initial calibration RSD exceedance

J3 Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde and 33-dichlorobenzidme in all samples for hexachlorobutadiene 4-mtrophenol and hexachlorobenzene m samples D05948 D05949 and D05953 for hexachlorocyclopentadiene m samples D05954 D05948 D05949 and D05953 and for 24shydimtrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 due to the continuing calibration D exceedances

J4 - Estimate (J) the positive results for di-n-butylphthalate in all soil samples due to continuing calibration exceedance

J5 - Estimate (UJ) the nondetect caprolactam result and raise the quantitation limit to 4 ugL (equivalent to the concentration of the high-level LFB) due to low low-level and high-level LFB recoveries This result may be biased low

J6 - Estimate (UJ) the nondetect results for 4-mtrophenol 46-dmitro-2-methylphenol and pentachlorophenol due to low low-level LFB recoveries These results may be biased low

J7 - Estimate (J) the positive result for di-n-butylphthalate due to high low-level and high-level LFB recoveries This result may be biased high

J8 - Estimate (UJ) the nondetect 24-dmitrophenol result and raise the quantitation limit to 800 ugKg (equivalent to the concentration of the high-level LFB and corrected for all preparation factors) due to low low-level and high-level LFB recoveries This result may be biased low

J9 - Estimate (UJ) the nondetect results for 24-dimethylphenol 4-mtrophenol 46-dimrro-2-methylphenol pentachlorophenol and 33-dichlorobenzidme due to low low-level LFB recoveries These results may be biased low

J10 - Estimate (UJ) the nondetect result 4-chIoroamlme due to low low-level and high-le el LFB recoveries This result may be biased low

J1 - Estimate (J) the positive result for benzo(b)fluoranthene due to high high-level LFB reco ery This result may be biased high

J12 - Estimate (UJ) the nondetect caprolactam result due to low LCS recovery This result may be biased low

J3 - Estimate (UJ) the nondetect benzaldehyde and 4-chloroamline results due to low LCS recoveries The results may be biased low

J14 - Estimate (J) the positive results for benzo(b)fluoranthene benzo(a)pyrene and mdeno(l23-cd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 due to high LCS recoveries The results may be biased high

J15 - Estimate (J) the positive results for the following compounds in the samples listed below due to uncertainty in the quantitation as a result of the exceeded ion abundance ration criteria

DOS 950 di-n-butylphthalate DOS 951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate mdeno(l23-cd)pyrene D05946 mdeno(l23-cd)pyrene D05947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate D05953 di-n-butylphthalate

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Page 3: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

Ms Christine Clark Page 3 February 24 2005 Case 0251M SDG D05939

Overall Evaluation of Data and Potential Usability Issues

The following is a summary of the site DQOs (Data Quality Objectives)

bull To determine the nature and extent of contamination following the completion of two removal actions in order to perform human health and ecological risk assessments and thereby recommend a remedy to eliminate reduce or control risks to human health and the environment

The sample data were qualified as a result of sampling and analytical error Qualifications as a result of sampling error are summarized below

The positive results for benzaldehyde in soil samples D05945 D05946 D05949 D05950 D05951 and D05952 and for acetophenone in soil sample D05951 were flagged EB due to equipment blank contamination The end data user should consider that an indeterminate amount of sampling error may have affected these sample results The results are usable for project objectives These qualifications have a minor impact on data usability

Qualifications as a result of analytical error are summarized below

bull The positive and nondetect results for benzaldehyde hexachlorocyclopentadiene 24-dinitrophenol 46-dinitro-2-methylphenol atrazine and pentachlorophenol in all samples were qualified as estimated (J and UJ respectively) due to the percent relative standard deviation (RSD) exceedances in the initial calibration All results are usable for project objectives as estimated values and as nondetect results with estimated quantitation limits These qualifications have a minor impact on data usability

bull The positive and nondetect results for benzaldehyde and 33-dichlorobenzidine in all samples for hexachlorobutadiene 4-nitrophenol and hexachlorobenzene in samples D05948 D05949 and D05953 for hexachlorocyclopentadiene in samples D05954 D05948 D05949 and D05953 and for 24-dinitrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 were qualified as estimated (J and UJ respectively) due to the percent difference (D) exceedances in the continuing calibrations These results are usable for project objectives as estimated values and as nondetect results with estimated quantitation limits These qualifications have a minor impact on data usability

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DVMemossD05939_socsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 4 February 24 2005 Case 0251M SDG D05939

bull The positive di-n-butylphthalate result in equipment blank sample D05954 was qualified as estimated (J) due to the RSD exceedance in the initial calibration This result is usable for project objective as an estimated value Note that this result was also qualified as nondetect (U) due to method blank contamination Therefore the overall qualification for this result is estimated nondetect (UJ) These qualifications have a minor impact on data usability

bull The positive di-n-butylphthalate results in all soil samples were qualified as estimated (J) due to the D exceedance in the continuing calibration These results are usable for project objectives as estimated values Note that the di-nshybutylphthalate results in all soil samples were also qualified as nondetect (U) due to method blank contamination Therefore the overall qualification for these results is estimated nondetect (UJ) These qualifications have a minor impact on data usability

bull The positive result for di-n-butylphthalate in equipment blank sample D05954 was qualified as nondetect (U) at the reported value due to method blank contamination This result is usable for project objectives as a nondetect Note that this result was also qualified as estimated (J) due to calibration nonconformances and high recoveries in the low-level and high-level laboratory fortified blanks (LFBs) Therefore the overall qualification for this result is estimated nondetect (UJ) These qualifications have a minor impact on data usability

bull The positive result for bis(2-ethylhexyl)phthalate in equipment blank sample D05954 was qualified as nondetect (U) at the quantitation limit (QL) due to method blank contamination This result is usable for project objectives as a nondetect This qualification has a minor impact on data usability

bull The positive results for di-n-butylphthalate in all soil samples were qualified as nondetect (U) at the reported values due to method blank contamination These results are usable for project objectives as nondetects Note that the di-nshybutylphthalate results in all soil samples were also qualified as estimated (J) due to calibration nonconformances high recoveries in the low-level and high-level LFBs andor ion abundance ratio exceedances Therefore the overall qualification for these results is estimated nondetect (UJ) These qualifications have a minor impact on data usability

bull The positive results for bis(2-ethylhexyl)phthalate in samples D05950 D05951 and D05952 were qualified as nondetect (U) at the QL due to performance evaluation sample contamination These results are usable for project objectives as nondetects These qualifications have a minor impact on data usability

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DV MemossD05939_svocsim wpd MetcalfA Eddy Inc

Ms Christine Clark Page 5 February 24 2005 Case 0251M SDG D05939

bull The nondetect result for caprolactam in equipment blank sample D05954 was qualified as estimated (UJ) at the raised quantitation limit [equivalent to the concentration of the high-level LFB (4 ugL)] due to low recoveries in the low-level and high-level LFB analyses This result is usable for project objectives as a nondetect with a raised and estimated quantitation limit that may be biased low This qualification has a minor impact on data usability

bull The nondetect results for 4-nitrophenol 46-dinitro-2-methylphenol and pentachlorophenol in equipment blank sample D05954 were qualified as estimated (UJ) due to low recoveries in the low-level LFB analyses These results are usable for project objectives as nondetects with estimated quantitation limits that may be biased low These qualifications have a minor impact on data usability

bull The positive result for di-n-butylphthalate in equipment blank sample D05954 was qualified as estimated (J) due to high recoveries in the low-level and high-level LFB analyses This result is usable for project objectives as an estimated value that may be biased high Note that this result was also qualified as nondetect (U) due to method blank contamination Therefore the overall qualification for this result is estimated nondetect (UJ) These qualifications have a minor impact on data usability

bull The nondetect results for 24-dinitrophenol in all soil samples were qualified as estimated (UJ) at the raised quantitation limit [equivalent to the concentration of the high-level LFB (800 ugKg) and corrected for all preparation factors] due to low recoveries in the low-level and high-level LFB analyses These results are usable for project objectives as nondetects with raised and estimated quantitation limits that may be biased low These qualifications have a minor impact on data usability

bull The nondetect results for 24-dimethylphenol 4-nitrophenol 46-dinitro-2shymethylphenol pentachlorophenol and 33-dichlorobenzidine in all soil samples were qualified as estimated (UJ) due to low recoveries in the low-level LFB analyses These results are usable for project objectives as nondetects with estimated quantitation limits that may be biased low These qualifications have a minor impact on data usability

bull The nondetect results for 4-chloroaniline in all soil samples were qualified as estimated (UJ) due to low recoveries in the low-level and high-level LFB analyses These results are usable for project objectives as nondetects with estimated quantitation limits that maybe biased low These qualifications have a minor impact on data usability

J NEWA160 Troy Mills LandfiMData VahdationDecember 2004DV MemossD05939_svocsm pd Metcalfamp Eddy Inc

Ms Christine Clark Page 6 February 24 2005 Case 0251M SDG D05939

The positive results for di-n-butylphthalate in all soil samples were qualified as estimated (J) due to high recoveries in the low-level and high-level LFB analyses These results are usable for project objectives as estimated values that maybe biased high Note that the di-n-butylphthalate results in all soil samples were also qualified as nondetect (U) due to method blank contamination Therefore the overall qualification for these results is estimated nondetect (UJ) These qualifications have a minor impact on data usability

The positive results for benzo(b)fluoranthene in samples D05951 D05952 D05945 D05946 and D05949 were qualified as estimated (J) due to high recovery in the high-level LFB analyses These results are usable for project objectives as estimated values that may be biased high These qualifications have a minor impact on data usability

The nondetect result for caprolactam in equipment blank sample D05954 was qualified as estimated (UJ) due to the low recovery in the laboratory control sample (LCS) analysis This result is usable for project objectives as a nondetect with an estimated quantitation limit that may be biased low These qualifications have a minor impact on data usability

The nondetect results for benzaldehyde and 4-chloroaniline in all soil samples were qualified as estimated (UJ) due to low recoveries in the LCS analyses These results are usable for project objectives as nondetects with estimated quantitation limits that may be biased low These qualifications have a minor impact on data usability

The positive results for benzo(b)fluoranthene benzo(a)pyrene and indeno(l23shycd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 were qualified as estimated (J) due to the high recoveries in the LCS analyses These results are usable for project objectives as estimated values that may be biased high These qualifications have a minor impact on data usability

JNEWAI60 Troy Mills LandfillData ValidationDecember 2004DV MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 7 February 24 2005 Case 0251M SDG D05939

bull The following compounds in the samples listed below were qualified as estimated (J) due to uncertainty in the quantitation as a result of the exceeded ion abundance ratio criteria These results are usable for project objectives as estimated values Note that the results for di-n-butylphthalate in samples D05950 D05951 D05952 D05945 D05947 D05948 D05949 and D05953 were also qualified as nondetect (U) due to method blank contamination Therefore the overall qualification for these results is estimated nondetect (UJ) These qualifications have a minor impact on data usability

D05950 di-n-butylphthalate D05951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate indeno(l23-cd)pyrene D05946 indeno(l23-cd)pyrene DOS 947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate DOS 95 3 di-n-butylphthalate

Data Completeness (CSF Audit)

The following information was missing or incorrect in the data package This missing or incorrect information was requested from the laboratory on February 7 and 152005 A resubmittal response was received at MampE on February 18 2005 adequately addressing these issues

bull The method detection limit (MDL) study results for two selected ion monitoring (SIM) compounds (pentachlorophenol and di-n-butylphthalate) were missing from the data package

The Form I (TIC) for sample D05946 identified the TIC at 1246 as alphashycaryophyllene while the raw data reported this TIC as l6-octadien-3-ol 37shydimethyl- Clarification was requested

bull The Form I for sample D05949 reported 26-dinitrotoluene and fluoranthene while the quantitation report did not reflect these results The laboratory was asked to verify this discrepancy

bull A relative response factor for 46-dinitro-2-methylphenol was listed on the Form 6 for the initial calibration in association with the 05 ugml standard However this compound was not listed on the quantitation report in the raw data The laboratory was asked to verify this discrepancy

J NEWA16Q Troy Mills LandfillData VahdationDecember 2004DV MemossD05939_svocsim pd Metcalf amp Eddy Inc

Ms Christine Clark Page 8 February 24 2005 Case 0251M SDG D05939

Initial and Continuing Calibrations

Full Scan

The following table summarizes the initial calibration (1C) and continuing calibration (CC) results that failed to meet the relative response factor (RRF) criterion of ^005 andor RSD lt 30 in the 1C andor D lt 25 in the CC for all compounds

Calibration Date 1C CC CC CC 12505 12705 13105 2105

Compound RSD D D D

benzaldehyde 792 155 156 153

hexachlorobutadiene - - - 453

hexachlorocyc lopentadiene 488 448 - 360

24-dimtrophenol 337 - 25 8 -

4-nitrophenol - - - 467

hexachlorobenzene - - - 286

46-dimtro-2-methylphenol 450 - - -

atrazme 434 - - -

pentachlorophenol 384 - - -

33-dichlorobenzidme - 726 463 628

2-fluorophenol (surrogate) - - - 285

Associated samples All samples D05954 D05950 D05951 D05948RE D05952 D05945 D05949 D05946 D05947 D05953RE D05948 D05953 D05949DL

D05945DL D05946DL D05947DL D05948DL D05953DL

- - QC acceptance criteria were not exceeded for this compound

Actions RSD gt 30 Estimate (J and UJ respectively) positive and nondetect results D gt 25 Estimate (J and UJ respectively) positive and nondetect results

JNEWA160 Troy Mills LandftllData VahdationDecember 2004DV MemossD05939_socsim pd Metcalf amp Eddy Inc

Ms Christine Clark Page 9 February 24 2005 Case 0251M SDGD05939

The positive and nondetect results for benzaldehyde hexachlorocyclopentadiene 24-dinitrophenol 46-dinitro-2-methylphenol atrazine and pentachlorophenol in all samples were qualified as estimated (UJ) due to initial calibration RSD exceedances

The positive and nondetect results for benzaldehyde and 33-dichlorobenzidine in all samples for hexachlorobutadiene 4-nitrophenol and hexachlorobenzene in samples D05948RE D05949 and D05953RE for hexachlorocyclopentadiene in samples D05954 D05948RE D05949 and D05953RE and for 24-dinitrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 were qualified as estimated (J and UJ respectively) due to continuing calibration D exceedances

No validation actions were necessary for the calibration nonconformances associated with the dilution sample analyses or for the original analyses of samples D05948 and D05953 since the compounds listed in the table above were not reported from these analyses

No validation actions were necessary for the surrogate compound calibration nonconformance

SIM

The following table summarizes the 1C and CC results that failed to meet the RRF criterion of gt005 andor RSD lt 30 in the 1C andor D lt 25 in the CC for all compounds

Calibration Date 1C 12105 1C 2205 CC 2305

Compound RSD RSD D

pentachlorophenol 621 402 -

di-n-butyl phthalate 331 - 297

bis(2-ethylhexyl)phthalate 347 306

Associated samples D05954 all soil samples all soil samples

- - QC acceptance criteria were not exceeded for this compound

Actions RSD gt 30 Estimate (J and UJ respectively) positive and nondetect results D gt 25 Estimate (J and UJ respectively) positive and nondetect results

The positive di-n-butylphthalate result in equipment blank sample D05954 was qualified as estimated (J) due to the RSD exceedance in the initial calibration

The positive di-n-butylphthalate results in all soil samples were qualified as estimated (J) due to the D exceedance in the continuing calibration

J NE WA160 Troy Mills LandfillData Validation December 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 10 February 24 2005 Case 0251M SDG D05939

The pentachlorophenol and bis(2-ethylhexyl)phthalate results in all samples were reported from the full scan analyses therefore no data validation actions were required as a result of the calibration nonconformances

Blanks

Full Scan

Target compounds were detected as contaminants m the performance evaluation sample (PES) as well as the equipment and laboratory method blanks The highest concentration detected was used to qualify associated sample results The following table summarizes the blank actions as they apply to the samples

Compound Blank

Maximum Concentration

(units)

Blank Action

Level (units)

Quantitation Limit (units)

Affected SamplesActions

benzaldehyde D05954 (EB)

15 ugL NA 100 ugKg Qualify as EB in samples D05950 D05951D05952 D05945 D05946 and D05949

acetophenone D05954 (EB)

0 35 ugL NA 100 ugKg Qualify as EB in sample D05951

4-chloro-3shymethylphenol

D05954 (EB)

5 6 ugL NA 100 ugKg 4-Chloro-3shymethylphenol was not detected in all associated samples No actions were required

di-n-butylphthalate D05954 (EB)

049 ugL NA 100 ugKg Di-n-butylphthalate results were reported from the SIM analyses No actions were required

di-n-butylphthalate method 42 ugKg 420 ugKg 100 ugKg Di-n-butylphthalate results were reported from the SIM analyses No actions were required

bis(2shyethylhexyl)phthalate

method 0 68 ugL 6 8 ugL 1 0 ugL Qualify as nondetect (U) at the QL m equipment blank sample D05954

J NEWA160 Troy Mills LandfillData VahdatwnDecember 20Q4DVMemossD05939_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 11 February 24 2005 Case 0251M SDGD05939

Compound Blank

Maximum Concentration

(units)

Blank Action

Level (units)

Quantitation Limit (units)

bis(2shyethylhexyl)phthalate

PES 490 ugKg 4900 ugKg 100 ugKg

NA - Not applicable SIM - selected ion monitoring EB - equipment blank PES - performance evaluation sample

Sample results were qualified as follows

Affected SamplesActions

Qualify as nondetect (U) at the QL in samples 005950005951 and D05952

bull If sample result was gtQL and ltblank action level (BAL) the result was qualified as a nondetect (U) at the reported concentration

bull If the sample result was sQL and iBAL the results was qualified as a nondetect (U) at the QL bull If the sample result was gtBAL qualification of the data was not required bull If the sample result was nondetect qualification of the data was not required bull Positive results for compounds detected in the equipment blank are flagged with EB

SIM

Target compounds were detected in the laboratory method blanks The following table summarizes the blank actions as they apply to the samples

Compound

di-n-buty Iphthalate

bis(2-ethylhexyl)phthalate

di-n-butylphthalate

Blank Maximum Action Quantitation

Concentration Level Limit Blank (umts^ (units) (units)

method 120ngL 1200 ngL 100 ngL

method 760 ngL 7600 ngL 1600 ngL

method 49 ugKg 490^1^ 10 ugKg

Affected SamplesActions

Qualify as nondetect (U) at the reported value in sample D05954

Bis(2shyethylhexyl)phthalate results were reported from the full scan analyses No actions vere required

Qualify as nondetect (U) at the reported value in all soil samples

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossD05939_nocsirn vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 12 February 24 2005 Case 0251M SDGD05939

Blank Maximum Action Quantitation

Concentration Level Limit Affected Compound Blank (units) (units) (units) Samples Actions

bis(2-ethylhexyl)phthalate method 31 ugKg 3 10 ugKg 160 MgKg Bis(2shyethylhexyl)phthalate results were reported from the full scan analyses No actions were required

Sample results were qualified as follows bull If sample result was gtQL and ltBAL the result was qualified as a nondetect (U) at the reported

concentration bull If the sample result was sQL and ltBAL the results was qualified as a nondetect (U) at the QL bull If the sample result was gtBAL qualification of the data was not required bull If the sample result was nondetect qualification of the data was not required

Internal Standards

Full scan

The following table summarizes the internal standards (IS) that did not meet the acceptable area criteria

Sample ID Internal Standard IS Area Acceptable Range Action

D05948 perylene-d|2 394921 407622-1630486 Results not reported from this analysis

D05948RE chrysene-d2 1720979 350682-1402728 Sample results associated with this IS were either not detected or were reported from the dilution analysis No data validation actions required

D05953 perylene-d2 311034 407622-1630486 Results not reported from this analysis

D05953RE chrysene-dl2 1565496 350682-1402728 Sample results associated with this IS were either not detected or were reported from the dilution analysis No data validation actions required

SIM

Internal standards were within the acceptance criteria in all sample analyses

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DV MemossD05939_svocsim npd Metcalfamp Eddy Inc

Ms Christine Clark Page 13 February 24 2005 Case 0251M SDG D05939

Sensitivity Check

Full Scan

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F05 (low-level)

SW122104F04 (high-level)

Compound

caprolactam

24-dimtrophenol

4-mtrophenol

46-dmitro-2-methylphenol

pentachlorophenol

caprolactam

Recovery Action

0 Raise the quantitation limit to the concentration of the high-level LFB (4 ngL) and qualify as estimated (UJ) the nondetect caprolactam result in sample D05954

0 Since the QL for this compound is 4 |igL the high level LFB (spiked at 4 ugL) was used to evaluate this compound for sensitivity

38 Qualify as estimated (UJ) the nondetect 4shynitrophenol result in sample D05954

38 Qualify as estimated (UJ) the nondetect 46shydimtro-2-methylphenol result in sample D05954

36 Qualify as estimated (UJ) the nondetect pentachlorophenol result in sample D05954

27 Raise the quantitation limit to the concentration of the high-level LFB (4 ugL) and qualify as estimated (UJ) the nondetect caprolactam result in sample D05954

QL - quantitation limit LFB - laboratory fortified blank

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound

SS012805FL01 24-dimethylphenol (low-level)

4-chloroanihne

Action Recovery

26 Qualify as estimated (UJ) the nondetect 24shydimethylphenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shychloroamlme results in all soil samples

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossD05939j5vocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark February 24 2005

LFB

SS012805FL01 (low-level)

SS012805FH01 (high-level)

SIM

Compound

24-dimtrophenol

4-mtrophenol

4 6-dimtro-2-methylphenol

pentachlorophenol

33-dichlorobenzidme

4-chloroanilme

24-dimtrophenol

Page 14 Case 0251M SDG D05939

Action Recovery

0 Raise the quantitation limit to the concentration of the high-level LFB [800 ngKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shynitrophenol results in all soil samples

13 Qualify as estimated (UJ) the nondetect 46shydmitro-2-methylphenol results in all soil samples

32 Qualify as estimated (UJ) the nondetect pentachlorophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 33shydichlorobenzidme results in all soil samples

39 Qualify as estimated (UJ) the nondetect 4shychloroamhne results in all soil samples

21 Raise the quantitation limit to the concentration of the high-level LFB [800 ugKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F03 (low-level)

SW122104F04 (high-level)

Compound

pentachlorophenol

di-n-butylphthalate

bis(2-ethylhexyl)phthalate

di-n-butylphthalate

Recovery

0

327

622

131

Action

Pentachlorophenol was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

J NEWA160 Tro Mills LandfillData VahdationDecember 2004DVMemossD05939_socsim npd Metcalf amp Eddy Inc

Ms Christine Clark Page 15 February 24 2005 Case0251M SDGD05939

LFB Compound Action Recovery

SW122104F04 bis(2-ethylhexyl)phthalate 161 Bis(2-ethylhexyl)phthalate was reported from the (high-level) full scan analysis therefore no actions were

required

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound Action Recovery

SS012805FL02 di-n-butylphthalate 237 Qualify as estimated (J) the positive di-nshy(low-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 376 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 149 Since the QL for this compound is 160 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

indeno( 1 23-cd)pyrene 121 Since the QL for this compound is 1 60 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

SS012805FH02 di-n-butylphthalate 150 Qualify as estimated (J) the positive di-nshy(high-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 185 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 132 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D0595 1 D05952 D05945 D05946 and D05949

QL - quantitation limit

PE Sample ResultsAccuracy Check

PE Sample Results

Full Scan

A single-blind solid PE sample D05939 (PES number SS0491) was analyzed with this data set Eight compounds were scored as Within Limits 2-Chlorophenol acenaphthylene acenaphthene dibenzofuran fluorene anthracene fluoranthene benzo(a)anthracene and chrysene were scored as

J NEWA160 Troy Mills LandfillData VahdatwnDecember 2004DVMemossD05939_svocsim vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 16 February 24 2005 Case 0251M SDGD05939

Action High These compounds were not detected in any of the associated soil samples therefore no data validation actions were required Six compounds (naphthalene hexachlorobenzene phenanthrene pyrene and dibenz(ah)anthracene and benzo(ghi)perylene) were scored as Warning High two compounds (4-hydroxy-4-methyl-2-pentanone and 4-methyl-3-penten-2-one) were scored Non-spiked TIC and one compound (din-n-butylphthalate) was scored Less than CRQL No data validation action is required on the basis of the Warning High Non-spiked TIC and less than CRQL scores Bis(2-ethylhexyl)phthalate was scored as Contaminant This compound was also detected in the associated laboratory method blanks and consequently evaluated in the blank section of this memorandum (please see Blanks above)

Laboratory Control Sample (LCS) Results

Full Scan

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LCS Compound Recovery Action

SW122104L06 caprolactam 35 Qualify as estimated (UJ) the nondetectresult in sample D05954

caprolactam

atrazine 135 Atrazine was not detected in the associaNo actions were required

ted sample

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Recovery Action

SS012805L01 benzaldehyde 46 Qualify as estimated (J) the positive and (UJ) the nondetect benzaldehyde results in all soil samples

4-chloroanihne 35 Qualify as estimated (UJ) the nondetect 4shychloroaruhne results in all soil samples

SIM

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossDQ5939_svocstm vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 17 February 24 2005 Case 0251M SDGD05939

LCS Compound Action Recovery

SW122104L05 pentachlorophenol 194 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 123 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(a)pyrene 122 Benzo(a)pyrene was not detected in the associated sample No actions were required

mdeno( 1 2 3 -cd)pyrene 130 Indeno(l23-cd)pyrene was reported from the full scan analysis therefore no actions were required

dibenz(ah)anthracene 136 Dibenz(ah)anthracene was not detected in the associated sample No actions were required

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Action Recovery

SS012805L02 pentachlorophenol 126 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 142 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(b)fluoranthene 128 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D05951 D05952 D05945 D05946 and D05949

benzo(a)pyrene 121 Qualify as estimated (J) the positive benzo(a)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

mdeno( 1 23-cd)pyrene 129 Qualify as estimated (J) the positive indeno(l23shycd)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

dibenz(ah)anthracene 133 Dibenz(ah)anthracene was not detected in the associated samples No actions were required

J NE WA160 Troy Mills LandfillData Validation December 2004 D V MemossD0593 9_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 18 February 24 2005 Case 0251M SDG D05939

Compound Ouantitation and Reported Ouantitation Limits

Full Scan and SIM

Because of their high moisture content samples D05945 D05946 D05949 D05951 and D05952 were freeze-dried prior to extraction

The following table summarizes the SIM and full scan reporting when data existed for both full scan and SIM analyses Professional judgment was used to select specific analyses in order to report the lowest quantitation limit achievable and to report results with values within the calibration range

Compound Results reported from Full Scan Results reported from SIM

pentachlorophenol all samples none

di-n-butyl phthalate none all samples

benzo(a)anthracene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

bis(2-ethylhexyl)phthalate all samples none

benzo(b)fluoranthene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

benzo(a)pyrene none all samples

indeno(l23-cd)pyrene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

dibenz(ah)anthracene none all samples

Full Scan

The bis(2-ethylhexyl)phthalate results in the following samples were reported from the dilution analysis listed in parentheses since these results exceeded the calibration range in the undiluted analysis D05945 (5x) D05946 (20x) D05947 (20x) D05948 (20x) D05949 (5x) and D05953 (20x)

JNE WA160 Troy Mills LandfillData ValidationDecember 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 19 February 24 2005 Case 0251M SDGD05939

SIM

The following compounds in the samples listed below were qualified as estimated (J) due to uncertainty in the quantitation as a result of the exceeded ion abundance ratio criteria

D05950 di-n-butylphthalate DOS951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate indeno(l23-cd)pyrene D05946 indeno(l23-cd)pyrene DOS 947 di-n-butylphthalate DOS 948 di-n-butylphthalate DOS 949 di-n-butylphthalate D05953 di-n-butylphthalate

Tentatively Identified Compounds (TICs)

One TIC 4-hydroxy-4-methyl-2-pentanone was detected in all samples and is considered an aldol condensation product Consequently this TIC was not included on Table III Tentatively Identified Compound Summary for the affected samples

The following compound in the sample listed was reported twice in the affected sample For this sample this result was renamed to a more general identification since a compound cannot elute at multiple retention times The renamed TIC is described in the table below

Compound name as reported by the Compound name as renamed during data Affected sample laboratory validation

oleic acid unknown D05951

JNEWA160 Troy Mills LandflllData ValidationDecember 2004DV MemossD05939_svocsimwpd MetcalfA Eddy Inc

Ms Christine Clark Page 20 February 24 2005 Case 0251M SDG D05939

Please contact Ms Constance Lapite at (781) 224-6628 or at Constance lapite(am-ecom if you have any questions regarding this Tier II validation

Paula L DiMattei Data Validator

Deborah A Trwini ^mjrjat

Robert Shoemaker Project Chemist

bullgt pound^ampgtlt^ Constance D Lapite MampE RAC Lead Chemist

cc ^James Chow EPA Remedial Project Manager (DV memo and data summary tables) Karen Wedlock-Hunt MampE Project Manager (entire package) Robert Shoemaker Project Chemist (entire package) Troy Mills Landfill Project File WA No 160-RICO-019M (entire package)

Attachments ORDA Table I Recommendation Summary Table Table II Overall Evaluation of Data Table III Tentatively Identified Compound Summary Data Summary Tables Data Validation Worksheets PE Score Report Copy of non-CLP Analytical Method (MampE DAS Specification D-148) Copies of Telephone LogCommunications Forms Supporting Data for Reduced Payment Recommendations (not applicable) Copies of Field Sampling Notes (previously submitted) Copies of EPA-Approved Amendments not QAPjP or SAP (not applicable) CSF Completeness Evidence File Audit (DC-2 Form) DQO Summary Form

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DVMemossD05939_svocsim pd Metcatfamp Eddy Inc

REGION I EPA-NE ORGANIC REGIONAL DATA ASSESSMENT (ORDA)

CASE raquozjggtH _ SITE NAME TV

LAB NAME uoAlaquo Vlaquo- amp+ OF SAMPLESMATRIX

SDG Posirt_ VALIDATION CONTRACTOR

SOW CONTRACT p-rttll-- VALIDATORS NAME

EPA-NE DV TIER LEVEL JC_ DATE DP RECD BY EPA-NE

TPOPO ACTION _ FYI ^ DV COMPLETION DATE

ANALYTICAL DATA QUALITY SUMMARY tffpft^m t~

bullVGA SV-SM PestPCB 1 Preservation and Contractual Holding Times 2 GCMS GCECD Instrument Performance Check raquo 3 Initial Calibration laquo 4 Continuing Calibration o 5 Blanks ~ o 6 Surrogate Compounds raquo 7 Internal Standards o 8 Matrix SpikeMatrix Spike Duplicate ggt 9 Sensitivity Check 0 10 PE Samples-Accuracy Check 0 11 Target Compound Identification jpy 12 Compound Quantitation and Reported QLs o 13 Tentatively Identified Compounds o 14 Semivolatile CleanupPesticidePCB Cleanup ulaquor 15 Data Completeness 0 16 Overall Evaluation of Data laquo

o = Data had no problems or were qualified due to minor contractual problems m = Data were qualified due to major contractual problems z = Data were rejected as unusable due major contractual problems

ACTION ITEMS (z items)

AREAS OF CONCERN (m items)

COMMENTS

This form assesses the analytical data quality in terms of contractual compliance only It does not assess sampling errors andor non-contractual analytical issues that affect data quality

Check ACTION only if contractual defects resulted in reduced paymentdata rejection recommendations

Validator t ltiJSagt3gtlt -3 Date

INSTRUCTIONS ON REVERSE SIDE

1296

Table I Recommendation Summary

Soil Semivolatile Organic Analysis Troy Mills Landfill Superfund Site

Case0251M SDGD05939

Sample ID Matrix

D05945 SO

D05946 SO

D05947 SO (FD)

D05948 SO

D05949 SO

D05950 SO

D05951 SO

D05952 SO

D05953 SO (FD)

D05954 EB

EB shy Equipment Blank FD shy Field Duplicate SOshy Soil

Qualifier

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 11 13 14 15

2 Jl 3 4 7 8 9 10 13 15

A 2 jl 3 4 7 8 9 10 13 15

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 jl 3 4 7 8 9 10 13 15

A 2 3 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 Jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 13 15

^2 4 jl 2 3 5 6 7 12

A - Accept the data but qualify the positive results for benzaldehyde in samples D05945 D05946 D05949 D05950 D05951 and D05952 and for acetophenone in sample D05951 as (EB) due to equipment blank contamination

A2 - Accept the data but qualify the positive result for di-n-butylphthalate as nondetect (U) at the reported value due to laboratory method blank contamination

A5 - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to PE sample contamination

A - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to laboratory method blank contamination

J - Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde hexachlorocyclopentadiene 24shydmitrophenol 46-dmitro-2-methylphenol atrazine and pentachlorophenol due to initial calibration RSD exceedances

J2 Estimate (J) the positive result for di-n-butyl phthalate due to the initial calibration RSD exceedance

J3 Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde and 33-dichlorobenzidme in all samples for hexachlorobutadiene 4-mtrophenol and hexachlorobenzene m samples D05948 D05949 and D05953 for hexachlorocyclopentadiene m samples D05954 D05948 D05949 and D05953 and for 24shydimtrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 due to the continuing calibration D exceedances

J4 - Estimate (J) the positive results for di-n-butylphthalate in all soil samples due to continuing calibration exceedance

J5 - Estimate (UJ) the nondetect caprolactam result and raise the quantitation limit to 4 ugL (equivalent to the concentration of the high-level LFB) due to low low-level and high-level LFB recoveries This result may be biased low

J6 - Estimate (UJ) the nondetect results for 4-mtrophenol 46-dmitro-2-methylphenol and pentachlorophenol due to low low-level LFB recoveries These results may be biased low

J7 - Estimate (J) the positive result for di-n-butylphthalate due to high low-level and high-level LFB recoveries This result may be biased high

J8 - Estimate (UJ) the nondetect 24-dmitrophenol result and raise the quantitation limit to 800 ugKg (equivalent to the concentration of the high-level LFB and corrected for all preparation factors) due to low low-level and high-level LFB recoveries This result may be biased low

J9 - Estimate (UJ) the nondetect results for 24-dimethylphenol 4-mtrophenol 46-dimrro-2-methylphenol pentachlorophenol and 33-dichlorobenzidme due to low low-level LFB recoveries These results may be biased low

J10 - Estimate (UJ) the nondetect result 4-chIoroamlme due to low low-level and high-le el LFB recoveries This result may be biased low

J1 - Estimate (J) the positive result for benzo(b)fluoranthene due to high high-level LFB reco ery This result may be biased high

J12 - Estimate (UJ) the nondetect caprolactam result due to low LCS recovery This result may be biased low

J3 - Estimate (UJ) the nondetect benzaldehyde and 4-chloroamline results due to low LCS recoveries The results may be biased low

J14 - Estimate (J) the positive results for benzo(b)fluoranthene benzo(a)pyrene and mdeno(l23-cd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 due to high LCS recoveries The results may be biased high

J15 - Estimate (J) the positive results for the following compounds in the samples listed below due to uncertainty in the quantitation as a result of the exceeded ion abundance ration criteria

DOS 950 di-n-butylphthalate DOS 951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate mdeno(l23-cd)pyrene D05946 mdeno(l23-cd)pyrene D05947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate D05953 di-n-butylphthalate

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Page 4: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

Ms Christine Clark Page 4 February 24 2005 Case 0251M SDG D05939

bull The positive di-n-butylphthalate result in equipment blank sample D05954 was qualified as estimated (J) due to the RSD exceedance in the initial calibration This result is usable for project objective as an estimated value Note that this result was also qualified as nondetect (U) due to method blank contamination Therefore the overall qualification for this result is estimated nondetect (UJ) These qualifications have a minor impact on data usability

bull The positive di-n-butylphthalate results in all soil samples were qualified as estimated (J) due to the D exceedance in the continuing calibration These results are usable for project objectives as estimated values Note that the di-nshybutylphthalate results in all soil samples were also qualified as nondetect (U) due to method blank contamination Therefore the overall qualification for these results is estimated nondetect (UJ) These qualifications have a minor impact on data usability

bull The positive result for di-n-butylphthalate in equipment blank sample D05954 was qualified as nondetect (U) at the reported value due to method blank contamination This result is usable for project objectives as a nondetect Note that this result was also qualified as estimated (J) due to calibration nonconformances and high recoveries in the low-level and high-level laboratory fortified blanks (LFBs) Therefore the overall qualification for this result is estimated nondetect (UJ) These qualifications have a minor impact on data usability

bull The positive result for bis(2-ethylhexyl)phthalate in equipment blank sample D05954 was qualified as nondetect (U) at the quantitation limit (QL) due to method blank contamination This result is usable for project objectives as a nondetect This qualification has a minor impact on data usability

bull The positive results for di-n-butylphthalate in all soil samples were qualified as nondetect (U) at the reported values due to method blank contamination These results are usable for project objectives as nondetects Note that the di-nshybutylphthalate results in all soil samples were also qualified as estimated (J) due to calibration nonconformances high recoveries in the low-level and high-level LFBs andor ion abundance ratio exceedances Therefore the overall qualification for these results is estimated nondetect (UJ) These qualifications have a minor impact on data usability

bull The positive results for bis(2-ethylhexyl)phthalate in samples D05950 D05951 and D05952 were qualified as nondetect (U) at the QL due to performance evaluation sample contamination These results are usable for project objectives as nondetects These qualifications have a minor impact on data usability

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DV MemossD05939_svocsim wpd MetcalfA Eddy Inc

Ms Christine Clark Page 5 February 24 2005 Case 0251M SDG D05939

bull The nondetect result for caprolactam in equipment blank sample D05954 was qualified as estimated (UJ) at the raised quantitation limit [equivalent to the concentration of the high-level LFB (4 ugL)] due to low recoveries in the low-level and high-level LFB analyses This result is usable for project objectives as a nondetect with a raised and estimated quantitation limit that may be biased low This qualification has a minor impact on data usability

bull The nondetect results for 4-nitrophenol 46-dinitro-2-methylphenol and pentachlorophenol in equipment blank sample D05954 were qualified as estimated (UJ) due to low recoveries in the low-level LFB analyses These results are usable for project objectives as nondetects with estimated quantitation limits that may be biased low These qualifications have a minor impact on data usability

bull The positive result for di-n-butylphthalate in equipment blank sample D05954 was qualified as estimated (J) due to high recoveries in the low-level and high-level LFB analyses This result is usable for project objectives as an estimated value that may be biased high Note that this result was also qualified as nondetect (U) due to method blank contamination Therefore the overall qualification for this result is estimated nondetect (UJ) These qualifications have a minor impact on data usability

bull The nondetect results for 24-dinitrophenol in all soil samples were qualified as estimated (UJ) at the raised quantitation limit [equivalent to the concentration of the high-level LFB (800 ugKg) and corrected for all preparation factors] due to low recoveries in the low-level and high-level LFB analyses These results are usable for project objectives as nondetects with raised and estimated quantitation limits that may be biased low These qualifications have a minor impact on data usability

bull The nondetect results for 24-dimethylphenol 4-nitrophenol 46-dinitro-2shymethylphenol pentachlorophenol and 33-dichlorobenzidine in all soil samples were qualified as estimated (UJ) due to low recoveries in the low-level LFB analyses These results are usable for project objectives as nondetects with estimated quantitation limits that may be biased low These qualifications have a minor impact on data usability

bull The nondetect results for 4-chloroaniline in all soil samples were qualified as estimated (UJ) due to low recoveries in the low-level and high-level LFB analyses These results are usable for project objectives as nondetects with estimated quantitation limits that maybe biased low These qualifications have a minor impact on data usability

J NEWA160 Troy Mills LandfiMData VahdationDecember 2004DV MemossD05939_svocsm pd Metcalfamp Eddy Inc

Ms Christine Clark Page 6 February 24 2005 Case 0251M SDG D05939

The positive results for di-n-butylphthalate in all soil samples were qualified as estimated (J) due to high recoveries in the low-level and high-level LFB analyses These results are usable for project objectives as estimated values that maybe biased high Note that the di-n-butylphthalate results in all soil samples were also qualified as nondetect (U) due to method blank contamination Therefore the overall qualification for these results is estimated nondetect (UJ) These qualifications have a minor impact on data usability

The positive results for benzo(b)fluoranthene in samples D05951 D05952 D05945 D05946 and D05949 were qualified as estimated (J) due to high recovery in the high-level LFB analyses These results are usable for project objectives as estimated values that may be biased high These qualifications have a minor impact on data usability

The nondetect result for caprolactam in equipment blank sample D05954 was qualified as estimated (UJ) due to the low recovery in the laboratory control sample (LCS) analysis This result is usable for project objectives as a nondetect with an estimated quantitation limit that may be biased low These qualifications have a minor impact on data usability

The nondetect results for benzaldehyde and 4-chloroaniline in all soil samples were qualified as estimated (UJ) due to low recoveries in the LCS analyses These results are usable for project objectives as nondetects with estimated quantitation limits that may be biased low These qualifications have a minor impact on data usability

The positive results for benzo(b)fluoranthene benzo(a)pyrene and indeno(l23shycd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 were qualified as estimated (J) due to the high recoveries in the LCS analyses These results are usable for project objectives as estimated values that may be biased high These qualifications have a minor impact on data usability

JNEWAI60 Troy Mills LandfillData ValidationDecember 2004DV MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 7 February 24 2005 Case 0251M SDG D05939

bull The following compounds in the samples listed below were qualified as estimated (J) due to uncertainty in the quantitation as a result of the exceeded ion abundance ratio criteria These results are usable for project objectives as estimated values Note that the results for di-n-butylphthalate in samples D05950 D05951 D05952 D05945 D05947 D05948 D05949 and D05953 were also qualified as nondetect (U) due to method blank contamination Therefore the overall qualification for these results is estimated nondetect (UJ) These qualifications have a minor impact on data usability

D05950 di-n-butylphthalate D05951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate indeno(l23-cd)pyrene D05946 indeno(l23-cd)pyrene DOS 947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate DOS 95 3 di-n-butylphthalate

Data Completeness (CSF Audit)

The following information was missing or incorrect in the data package This missing or incorrect information was requested from the laboratory on February 7 and 152005 A resubmittal response was received at MampE on February 18 2005 adequately addressing these issues

bull The method detection limit (MDL) study results for two selected ion monitoring (SIM) compounds (pentachlorophenol and di-n-butylphthalate) were missing from the data package

The Form I (TIC) for sample D05946 identified the TIC at 1246 as alphashycaryophyllene while the raw data reported this TIC as l6-octadien-3-ol 37shydimethyl- Clarification was requested

bull The Form I for sample D05949 reported 26-dinitrotoluene and fluoranthene while the quantitation report did not reflect these results The laboratory was asked to verify this discrepancy

bull A relative response factor for 46-dinitro-2-methylphenol was listed on the Form 6 for the initial calibration in association with the 05 ugml standard However this compound was not listed on the quantitation report in the raw data The laboratory was asked to verify this discrepancy

J NEWA16Q Troy Mills LandfillData VahdationDecember 2004DV MemossD05939_svocsim pd Metcalf amp Eddy Inc

Ms Christine Clark Page 8 February 24 2005 Case 0251M SDG D05939

Initial and Continuing Calibrations

Full Scan

The following table summarizes the initial calibration (1C) and continuing calibration (CC) results that failed to meet the relative response factor (RRF) criterion of ^005 andor RSD lt 30 in the 1C andor D lt 25 in the CC for all compounds

Calibration Date 1C CC CC CC 12505 12705 13105 2105

Compound RSD D D D

benzaldehyde 792 155 156 153

hexachlorobutadiene - - - 453

hexachlorocyc lopentadiene 488 448 - 360

24-dimtrophenol 337 - 25 8 -

4-nitrophenol - - - 467

hexachlorobenzene - - - 286

46-dimtro-2-methylphenol 450 - - -

atrazme 434 - - -

pentachlorophenol 384 - - -

33-dichlorobenzidme - 726 463 628

2-fluorophenol (surrogate) - - - 285

Associated samples All samples D05954 D05950 D05951 D05948RE D05952 D05945 D05949 D05946 D05947 D05953RE D05948 D05953 D05949DL

D05945DL D05946DL D05947DL D05948DL D05953DL

- - QC acceptance criteria were not exceeded for this compound

Actions RSD gt 30 Estimate (J and UJ respectively) positive and nondetect results D gt 25 Estimate (J and UJ respectively) positive and nondetect results

JNEWA160 Troy Mills LandftllData VahdationDecember 2004DV MemossD05939_socsim pd Metcalf amp Eddy Inc

Ms Christine Clark Page 9 February 24 2005 Case 0251M SDGD05939

The positive and nondetect results for benzaldehyde hexachlorocyclopentadiene 24-dinitrophenol 46-dinitro-2-methylphenol atrazine and pentachlorophenol in all samples were qualified as estimated (UJ) due to initial calibration RSD exceedances

The positive and nondetect results for benzaldehyde and 33-dichlorobenzidine in all samples for hexachlorobutadiene 4-nitrophenol and hexachlorobenzene in samples D05948RE D05949 and D05953RE for hexachlorocyclopentadiene in samples D05954 D05948RE D05949 and D05953RE and for 24-dinitrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 were qualified as estimated (J and UJ respectively) due to continuing calibration D exceedances

No validation actions were necessary for the calibration nonconformances associated with the dilution sample analyses or for the original analyses of samples D05948 and D05953 since the compounds listed in the table above were not reported from these analyses

No validation actions were necessary for the surrogate compound calibration nonconformance

SIM

The following table summarizes the 1C and CC results that failed to meet the RRF criterion of gt005 andor RSD lt 30 in the 1C andor D lt 25 in the CC for all compounds

Calibration Date 1C 12105 1C 2205 CC 2305

Compound RSD RSD D

pentachlorophenol 621 402 -

di-n-butyl phthalate 331 - 297

bis(2-ethylhexyl)phthalate 347 306

Associated samples D05954 all soil samples all soil samples

- - QC acceptance criteria were not exceeded for this compound

Actions RSD gt 30 Estimate (J and UJ respectively) positive and nondetect results D gt 25 Estimate (J and UJ respectively) positive and nondetect results

The positive di-n-butylphthalate result in equipment blank sample D05954 was qualified as estimated (J) due to the RSD exceedance in the initial calibration

The positive di-n-butylphthalate results in all soil samples were qualified as estimated (J) due to the D exceedance in the continuing calibration

J NE WA160 Troy Mills LandfillData Validation December 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 10 February 24 2005 Case 0251M SDG D05939

The pentachlorophenol and bis(2-ethylhexyl)phthalate results in all samples were reported from the full scan analyses therefore no data validation actions were required as a result of the calibration nonconformances

Blanks

Full Scan

Target compounds were detected as contaminants m the performance evaluation sample (PES) as well as the equipment and laboratory method blanks The highest concentration detected was used to qualify associated sample results The following table summarizes the blank actions as they apply to the samples

Compound Blank

Maximum Concentration

(units)

Blank Action

Level (units)

Quantitation Limit (units)

Affected SamplesActions

benzaldehyde D05954 (EB)

15 ugL NA 100 ugKg Qualify as EB in samples D05950 D05951D05952 D05945 D05946 and D05949

acetophenone D05954 (EB)

0 35 ugL NA 100 ugKg Qualify as EB in sample D05951

4-chloro-3shymethylphenol

D05954 (EB)

5 6 ugL NA 100 ugKg 4-Chloro-3shymethylphenol was not detected in all associated samples No actions were required

di-n-butylphthalate D05954 (EB)

049 ugL NA 100 ugKg Di-n-butylphthalate results were reported from the SIM analyses No actions were required

di-n-butylphthalate method 42 ugKg 420 ugKg 100 ugKg Di-n-butylphthalate results were reported from the SIM analyses No actions were required

bis(2shyethylhexyl)phthalate

method 0 68 ugL 6 8 ugL 1 0 ugL Qualify as nondetect (U) at the QL m equipment blank sample D05954

J NEWA160 Troy Mills LandfillData VahdatwnDecember 20Q4DVMemossD05939_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 11 February 24 2005 Case 0251M SDGD05939

Compound Blank

Maximum Concentration

(units)

Blank Action

Level (units)

Quantitation Limit (units)

bis(2shyethylhexyl)phthalate

PES 490 ugKg 4900 ugKg 100 ugKg

NA - Not applicable SIM - selected ion monitoring EB - equipment blank PES - performance evaluation sample

Sample results were qualified as follows

Affected SamplesActions

Qualify as nondetect (U) at the QL in samples 005950005951 and D05952

bull If sample result was gtQL and ltblank action level (BAL) the result was qualified as a nondetect (U) at the reported concentration

bull If the sample result was sQL and iBAL the results was qualified as a nondetect (U) at the QL bull If the sample result was gtBAL qualification of the data was not required bull If the sample result was nondetect qualification of the data was not required bull Positive results for compounds detected in the equipment blank are flagged with EB

SIM

Target compounds were detected in the laboratory method blanks The following table summarizes the blank actions as they apply to the samples

Compound

di-n-buty Iphthalate

bis(2-ethylhexyl)phthalate

di-n-butylphthalate

Blank Maximum Action Quantitation

Concentration Level Limit Blank (umts^ (units) (units)

method 120ngL 1200 ngL 100 ngL

method 760 ngL 7600 ngL 1600 ngL

method 49 ugKg 490^1^ 10 ugKg

Affected SamplesActions

Qualify as nondetect (U) at the reported value in sample D05954

Bis(2shyethylhexyl)phthalate results were reported from the full scan analyses No actions vere required

Qualify as nondetect (U) at the reported value in all soil samples

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossD05939_nocsirn vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 12 February 24 2005 Case 0251M SDGD05939

Blank Maximum Action Quantitation

Concentration Level Limit Affected Compound Blank (units) (units) (units) Samples Actions

bis(2-ethylhexyl)phthalate method 31 ugKg 3 10 ugKg 160 MgKg Bis(2shyethylhexyl)phthalate results were reported from the full scan analyses No actions were required

Sample results were qualified as follows bull If sample result was gtQL and ltBAL the result was qualified as a nondetect (U) at the reported

concentration bull If the sample result was sQL and ltBAL the results was qualified as a nondetect (U) at the QL bull If the sample result was gtBAL qualification of the data was not required bull If the sample result was nondetect qualification of the data was not required

Internal Standards

Full scan

The following table summarizes the internal standards (IS) that did not meet the acceptable area criteria

Sample ID Internal Standard IS Area Acceptable Range Action

D05948 perylene-d|2 394921 407622-1630486 Results not reported from this analysis

D05948RE chrysene-d2 1720979 350682-1402728 Sample results associated with this IS were either not detected or were reported from the dilution analysis No data validation actions required

D05953 perylene-d2 311034 407622-1630486 Results not reported from this analysis

D05953RE chrysene-dl2 1565496 350682-1402728 Sample results associated with this IS were either not detected or were reported from the dilution analysis No data validation actions required

SIM

Internal standards were within the acceptance criteria in all sample analyses

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DV MemossD05939_svocsim npd Metcalfamp Eddy Inc

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Sensitivity Check

Full Scan

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F05 (low-level)

SW122104F04 (high-level)

Compound

caprolactam

24-dimtrophenol

4-mtrophenol

46-dmitro-2-methylphenol

pentachlorophenol

caprolactam

Recovery Action

0 Raise the quantitation limit to the concentration of the high-level LFB (4 ngL) and qualify as estimated (UJ) the nondetect caprolactam result in sample D05954

0 Since the QL for this compound is 4 |igL the high level LFB (spiked at 4 ugL) was used to evaluate this compound for sensitivity

38 Qualify as estimated (UJ) the nondetect 4shynitrophenol result in sample D05954

38 Qualify as estimated (UJ) the nondetect 46shydimtro-2-methylphenol result in sample D05954

36 Qualify as estimated (UJ) the nondetect pentachlorophenol result in sample D05954

27 Raise the quantitation limit to the concentration of the high-level LFB (4 ugL) and qualify as estimated (UJ) the nondetect caprolactam result in sample D05954

QL - quantitation limit LFB - laboratory fortified blank

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound

SS012805FL01 24-dimethylphenol (low-level)

4-chloroanihne

Action Recovery

26 Qualify as estimated (UJ) the nondetect 24shydimethylphenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shychloroamlme results in all soil samples

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossD05939j5vocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark February 24 2005

LFB

SS012805FL01 (low-level)

SS012805FH01 (high-level)

SIM

Compound

24-dimtrophenol

4-mtrophenol

4 6-dimtro-2-methylphenol

pentachlorophenol

33-dichlorobenzidme

4-chloroanilme

24-dimtrophenol

Page 14 Case 0251M SDG D05939

Action Recovery

0 Raise the quantitation limit to the concentration of the high-level LFB [800 ngKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shynitrophenol results in all soil samples

13 Qualify as estimated (UJ) the nondetect 46shydmitro-2-methylphenol results in all soil samples

32 Qualify as estimated (UJ) the nondetect pentachlorophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 33shydichlorobenzidme results in all soil samples

39 Qualify as estimated (UJ) the nondetect 4shychloroamhne results in all soil samples

21 Raise the quantitation limit to the concentration of the high-level LFB [800 ugKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F03 (low-level)

SW122104F04 (high-level)

Compound

pentachlorophenol

di-n-butylphthalate

bis(2-ethylhexyl)phthalate

di-n-butylphthalate

Recovery

0

327

622

131

Action

Pentachlorophenol was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

J NEWA160 Tro Mills LandfillData VahdationDecember 2004DVMemossD05939_socsim npd Metcalf amp Eddy Inc

Ms Christine Clark Page 15 February 24 2005 Case0251M SDGD05939

LFB Compound Action Recovery

SW122104F04 bis(2-ethylhexyl)phthalate 161 Bis(2-ethylhexyl)phthalate was reported from the (high-level) full scan analysis therefore no actions were

required

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound Action Recovery

SS012805FL02 di-n-butylphthalate 237 Qualify as estimated (J) the positive di-nshy(low-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 376 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 149 Since the QL for this compound is 160 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

indeno( 1 23-cd)pyrene 121 Since the QL for this compound is 1 60 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

SS012805FH02 di-n-butylphthalate 150 Qualify as estimated (J) the positive di-nshy(high-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 185 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 132 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D0595 1 D05952 D05945 D05946 and D05949

QL - quantitation limit

PE Sample ResultsAccuracy Check

PE Sample Results

Full Scan

A single-blind solid PE sample D05939 (PES number SS0491) was analyzed with this data set Eight compounds were scored as Within Limits 2-Chlorophenol acenaphthylene acenaphthene dibenzofuran fluorene anthracene fluoranthene benzo(a)anthracene and chrysene were scored as

J NEWA160 Troy Mills LandfillData VahdatwnDecember 2004DVMemossD05939_svocsim vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 16 February 24 2005 Case 0251M SDGD05939

Action High These compounds were not detected in any of the associated soil samples therefore no data validation actions were required Six compounds (naphthalene hexachlorobenzene phenanthrene pyrene and dibenz(ah)anthracene and benzo(ghi)perylene) were scored as Warning High two compounds (4-hydroxy-4-methyl-2-pentanone and 4-methyl-3-penten-2-one) were scored Non-spiked TIC and one compound (din-n-butylphthalate) was scored Less than CRQL No data validation action is required on the basis of the Warning High Non-spiked TIC and less than CRQL scores Bis(2-ethylhexyl)phthalate was scored as Contaminant This compound was also detected in the associated laboratory method blanks and consequently evaluated in the blank section of this memorandum (please see Blanks above)

Laboratory Control Sample (LCS) Results

Full Scan

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LCS Compound Recovery Action

SW122104L06 caprolactam 35 Qualify as estimated (UJ) the nondetectresult in sample D05954

caprolactam

atrazine 135 Atrazine was not detected in the associaNo actions were required

ted sample

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Recovery Action

SS012805L01 benzaldehyde 46 Qualify as estimated (J) the positive and (UJ) the nondetect benzaldehyde results in all soil samples

4-chloroanihne 35 Qualify as estimated (UJ) the nondetect 4shychloroaruhne results in all soil samples

SIM

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossDQ5939_svocstm vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 17 February 24 2005 Case 0251M SDGD05939

LCS Compound Action Recovery

SW122104L05 pentachlorophenol 194 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 123 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(a)pyrene 122 Benzo(a)pyrene was not detected in the associated sample No actions were required

mdeno( 1 2 3 -cd)pyrene 130 Indeno(l23-cd)pyrene was reported from the full scan analysis therefore no actions were required

dibenz(ah)anthracene 136 Dibenz(ah)anthracene was not detected in the associated sample No actions were required

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Action Recovery

SS012805L02 pentachlorophenol 126 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 142 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(b)fluoranthene 128 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D05951 D05952 D05945 D05946 and D05949

benzo(a)pyrene 121 Qualify as estimated (J) the positive benzo(a)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

mdeno( 1 23-cd)pyrene 129 Qualify as estimated (J) the positive indeno(l23shycd)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

dibenz(ah)anthracene 133 Dibenz(ah)anthracene was not detected in the associated samples No actions were required

J NE WA160 Troy Mills LandfillData Validation December 2004 D V MemossD0593 9_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 18 February 24 2005 Case 0251M SDG D05939

Compound Ouantitation and Reported Ouantitation Limits

Full Scan and SIM

Because of their high moisture content samples D05945 D05946 D05949 D05951 and D05952 were freeze-dried prior to extraction

The following table summarizes the SIM and full scan reporting when data existed for both full scan and SIM analyses Professional judgment was used to select specific analyses in order to report the lowest quantitation limit achievable and to report results with values within the calibration range

Compound Results reported from Full Scan Results reported from SIM

pentachlorophenol all samples none

di-n-butyl phthalate none all samples

benzo(a)anthracene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

bis(2-ethylhexyl)phthalate all samples none

benzo(b)fluoranthene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

benzo(a)pyrene none all samples

indeno(l23-cd)pyrene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

dibenz(ah)anthracene none all samples

Full Scan

The bis(2-ethylhexyl)phthalate results in the following samples were reported from the dilution analysis listed in parentheses since these results exceeded the calibration range in the undiluted analysis D05945 (5x) D05946 (20x) D05947 (20x) D05948 (20x) D05949 (5x) and D05953 (20x)

JNE WA160 Troy Mills LandfillData ValidationDecember 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 19 February 24 2005 Case 0251M SDGD05939

SIM

The following compounds in the samples listed below were qualified as estimated (J) due to uncertainty in the quantitation as a result of the exceeded ion abundance ratio criteria

D05950 di-n-butylphthalate DOS951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate indeno(l23-cd)pyrene D05946 indeno(l23-cd)pyrene DOS 947 di-n-butylphthalate DOS 948 di-n-butylphthalate DOS 949 di-n-butylphthalate D05953 di-n-butylphthalate

Tentatively Identified Compounds (TICs)

One TIC 4-hydroxy-4-methyl-2-pentanone was detected in all samples and is considered an aldol condensation product Consequently this TIC was not included on Table III Tentatively Identified Compound Summary for the affected samples

The following compound in the sample listed was reported twice in the affected sample For this sample this result was renamed to a more general identification since a compound cannot elute at multiple retention times The renamed TIC is described in the table below

Compound name as reported by the Compound name as renamed during data Affected sample laboratory validation

oleic acid unknown D05951

JNEWA160 Troy Mills LandflllData ValidationDecember 2004DV MemossD05939_svocsimwpd MetcalfA Eddy Inc

Ms Christine Clark Page 20 February 24 2005 Case 0251M SDG D05939

Please contact Ms Constance Lapite at (781) 224-6628 or at Constance lapite(am-ecom if you have any questions regarding this Tier II validation

Paula L DiMattei Data Validator

Deborah A Trwini ^mjrjat

Robert Shoemaker Project Chemist

bullgt pound^ampgtlt^ Constance D Lapite MampE RAC Lead Chemist

cc ^James Chow EPA Remedial Project Manager (DV memo and data summary tables) Karen Wedlock-Hunt MampE Project Manager (entire package) Robert Shoemaker Project Chemist (entire package) Troy Mills Landfill Project File WA No 160-RICO-019M (entire package)

Attachments ORDA Table I Recommendation Summary Table Table II Overall Evaluation of Data Table III Tentatively Identified Compound Summary Data Summary Tables Data Validation Worksheets PE Score Report Copy of non-CLP Analytical Method (MampE DAS Specification D-148) Copies of Telephone LogCommunications Forms Supporting Data for Reduced Payment Recommendations (not applicable) Copies of Field Sampling Notes (previously submitted) Copies of EPA-Approved Amendments not QAPjP or SAP (not applicable) CSF Completeness Evidence File Audit (DC-2 Form) DQO Summary Form

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DVMemossD05939_svocsim pd Metcatfamp Eddy Inc

REGION I EPA-NE ORGANIC REGIONAL DATA ASSESSMENT (ORDA)

CASE raquozjggtH _ SITE NAME TV

LAB NAME uoAlaquo Vlaquo- amp+ OF SAMPLESMATRIX

SDG Posirt_ VALIDATION CONTRACTOR

SOW CONTRACT p-rttll-- VALIDATORS NAME

EPA-NE DV TIER LEVEL JC_ DATE DP RECD BY EPA-NE

TPOPO ACTION _ FYI ^ DV COMPLETION DATE

ANALYTICAL DATA QUALITY SUMMARY tffpft^m t~

bullVGA SV-SM PestPCB 1 Preservation and Contractual Holding Times 2 GCMS GCECD Instrument Performance Check raquo 3 Initial Calibration laquo 4 Continuing Calibration o 5 Blanks ~ o 6 Surrogate Compounds raquo 7 Internal Standards o 8 Matrix SpikeMatrix Spike Duplicate ggt 9 Sensitivity Check 0 10 PE Samples-Accuracy Check 0 11 Target Compound Identification jpy 12 Compound Quantitation and Reported QLs o 13 Tentatively Identified Compounds o 14 Semivolatile CleanupPesticidePCB Cleanup ulaquor 15 Data Completeness 0 16 Overall Evaluation of Data laquo

o = Data had no problems or were qualified due to minor contractual problems m = Data were qualified due to major contractual problems z = Data were rejected as unusable due major contractual problems

ACTION ITEMS (z items)

AREAS OF CONCERN (m items)

COMMENTS

This form assesses the analytical data quality in terms of contractual compliance only It does not assess sampling errors andor non-contractual analytical issues that affect data quality

Check ACTION only if contractual defects resulted in reduced paymentdata rejection recommendations

Validator t ltiJSagt3gtlt -3 Date

INSTRUCTIONS ON REVERSE SIDE

1296

Table I Recommendation Summary

Soil Semivolatile Organic Analysis Troy Mills Landfill Superfund Site

Case0251M SDGD05939

Sample ID Matrix

D05945 SO

D05946 SO

D05947 SO (FD)

D05948 SO

D05949 SO

D05950 SO

D05951 SO

D05952 SO

D05953 SO (FD)

D05954 EB

EB shy Equipment Blank FD shy Field Duplicate SOshy Soil

Qualifier

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 11 13 14 15

2 Jl 3 4 7 8 9 10 13 15

A 2 jl 3 4 7 8 9 10 13 15

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 jl 3 4 7 8 9 10 13 15

A 2 3 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 Jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 13 15

^2 4 jl 2 3 5 6 7 12

A - Accept the data but qualify the positive results for benzaldehyde in samples D05945 D05946 D05949 D05950 D05951 and D05952 and for acetophenone in sample D05951 as (EB) due to equipment blank contamination

A2 - Accept the data but qualify the positive result for di-n-butylphthalate as nondetect (U) at the reported value due to laboratory method blank contamination

A5 - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to PE sample contamination

A - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to laboratory method blank contamination

J - Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde hexachlorocyclopentadiene 24shydmitrophenol 46-dmitro-2-methylphenol atrazine and pentachlorophenol due to initial calibration RSD exceedances

J2 Estimate (J) the positive result for di-n-butyl phthalate due to the initial calibration RSD exceedance

J3 Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde and 33-dichlorobenzidme in all samples for hexachlorobutadiene 4-mtrophenol and hexachlorobenzene m samples D05948 D05949 and D05953 for hexachlorocyclopentadiene m samples D05954 D05948 D05949 and D05953 and for 24shydimtrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 due to the continuing calibration D exceedances

J4 - Estimate (J) the positive results for di-n-butylphthalate in all soil samples due to continuing calibration exceedance

J5 - Estimate (UJ) the nondetect caprolactam result and raise the quantitation limit to 4 ugL (equivalent to the concentration of the high-level LFB) due to low low-level and high-level LFB recoveries This result may be biased low

J6 - Estimate (UJ) the nondetect results for 4-mtrophenol 46-dmitro-2-methylphenol and pentachlorophenol due to low low-level LFB recoveries These results may be biased low

J7 - Estimate (J) the positive result for di-n-butylphthalate due to high low-level and high-level LFB recoveries This result may be biased high

J8 - Estimate (UJ) the nondetect 24-dmitrophenol result and raise the quantitation limit to 800 ugKg (equivalent to the concentration of the high-level LFB and corrected for all preparation factors) due to low low-level and high-level LFB recoveries This result may be biased low

J9 - Estimate (UJ) the nondetect results for 24-dimethylphenol 4-mtrophenol 46-dimrro-2-methylphenol pentachlorophenol and 33-dichlorobenzidme due to low low-level LFB recoveries These results may be biased low

J10 - Estimate (UJ) the nondetect result 4-chIoroamlme due to low low-level and high-le el LFB recoveries This result may be biased low

J1 - Estimate (J) the positive result for benzo(b)fluoranthene due to high high-level LFB reco ery This result may be biased high

J12 - Estimate (UJ) the nondetect caprolactam result due to low LCS recovery This result may be biased low

J3 - Estimate (UJ) the nondetect benzaldehyde and 4-chloroamline results due to low LCS recoveries The results may be biased low

J14 - Estimate (J) the positive results for benzo(b)fluoranthene benzo(a)pyrene and mdeno(l23-cd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 due to high LCS recoveries The results may be biased high

J15 - Estimate (J) the positive results for the following compounds in the samples listed below due to uncertainty in the quantitation as a result of the exceeded ion abundance ration criteria

DOS 950 di-n-butylphthalate DOS 951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate mdeno(l23-cd)pyrene D05946 mdeno(l23-cd)pyrene D05947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate D05953 di-n-butylphthalate

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Page 5: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

Ms Christine Clark Page 5 February 24 2005 Case 0251M SDG D05939

bull The nondetect result for caprolactam in equipment blank sample D05954 was qualified as estimated (UJ) at the raised quantitation limit [equivalent to the concentration of the high-level LFB (4 ugL)] due to low recoveries in the low-level and high-level LFB analyses This result is usable for project objectives as a nondetect with a raised and estimated quantitation limit that may be biased low This qualification has a minor impact on data usability

bull The nondetect results for 4-nitrophenol 46-dinitro-2-methylphenol and pentachlorophenol in equipment blank sample D05954 were qualified as estimated (UJ) due to low recoveries in the low-level LFB analyses These results are usable for project objectives as nondetects with estimated quantitation limits that may be biased low These qualifications have a minor impact on data usability

bull The positive result for di-n-butylphthalate in equipment blank sample D05954 was qualified as estimated (J) due to high recoveries in the low-level and high-level LFB analyses This result is usable for project objectives as an estimated value that may be biased high Note that this result was also qualified as nondetect (U) due to method blank contamination Therefore the overall qualification for this result is estimated nondetect (UJ) These qualifications have a minor impact on data usability

bull The nondetect results for 24-dinitrophenol in all soil samples were qualified as estimated (UJ) at the raised quantitation limit [equivalent to the concentration of the high-level LFB (800 ugKg) and corrected for all preparation factors] due to low recoveries in the low-level and high-level LFB analyses These results are usable for project objectives as nondetects with raised and estimated quantitation limits that may be biased low These qualifications have a minor impact on data usability

bull The nondetect results for 24-dimethylphenol 4-nitrophenol 46-dinitro-2shymethylphenol pentachlorophenol and 33-dichlorobenzidine in all soil samples were qualified as estimated (UJ) due to low recoveries in the low-level LFB analyses These results are usable for project objectives as nondetects with estimated quantitation limits that may be biased low These qualifications have a minor impact on data usability

bull The nondetect results for 4-chloroaniline in all soil samples were qualified as estimated (UJ) due to low recoveries in the low-level and high-level LFB analyses These results are usable for project objectives as nondetects with estimated quantitation limits that maybe biased low These qualifications have a minor impact on data usability

J NEWA160 Troy Mills LandfiMData VahdationDecember 2004DV MemossD05939_svocsm pd Metcalfamp Eddy Inc

Ms Christine Clark Page 6 February 24 2005 Case 0251M SDG D05939

The positive results for di-n-butylphthalate in all soil samples were qualified as estimated (J) due to high recoveries in the low-level and high-level LFB analyses These results are usable for project objectives as estimated values that maybe biased high Note that the di-n-butylphthalate results in all soil samples were also qualified as nondetect (U) due to method blank contamination Therefore the overall qualification for these results is estimated nondetect (UJ) These qualifications have a minor impact on data usability

The positive results for benzo(b)fluoranthene in samples D05951 D05952 D05945 D05946 and D05949 were qualified as estimated (J) due to high recovery in the high-level LFB analyses These results are usable for project objectives as estimated values that may be biased high These qualifications have a minor impact on data usability

The nondetect result for caprolactam in equipment blank sample D05954 was qualified as estimated (UJ) due to the low recovery in the laboratory control sample (LCS) analysis This result is usable for project objectives as a nondetect with an estimated quantitation limit that may be biased low These qualifications have a minor impact on data usability

The nondetect results for benzaldehyde and 4-chloroaniline in all soil samples were qualified as estimated (UJ) due to low recoveries in the LCS analyses These results are usable for project objectives as nondetects with estimated quantitation limits that may be biased low These qualifications have a minor impact on data usability

The positive results for benzo(b)fluoranthene benzo(a)pyrene and indeno(l23shycd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 were qualified as estimated (J) due to the high recoveries in the LCS analyses These results are usable for project objectives as estimated values that may be biased high These qualifications have a minor impact on data usability

JNEWAI60 Troy Mills LandfillData ValidationDecember 2004DV MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 7 February 24 2005 Case 0251M SDG D05939

bull The following compounds in the samples listed below were qualified as estimated (J) due to uncertainty in the quantitation as a result of the exceeded ion abundance ratio criteria These results are usable for project objectives as estimated values Note that the results for di-n-butylphthalate in samples D05950 D05951 D05952 D05945 D05947 D05948 D05949 and D05953 were also qualified as nondetect (U) due to method blank contamination Therefore the overall qualification for these results is estimated nondetect (UJ) These qualifications have a minor impact on data usability

D05950 di-n-butylphthalate D05951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate indeno(l23-cd)pyrene D05946 indeno(l23-cd)pyrene DOS 947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate DOS 95 3 di-n-butylphthalate

Data Completeness (CSF Audit)

The following information was missing or incorrect in the data package This missing or incorrect information was requested from the laboratory on February 7 and 152005 A resubmittal response was received at MampE on February 18 2005 adequately addressing these issues

bull The method detection limit (MDL) study results for two selected ion monitoring (SIM) compounds (pentachlorophenol and di-n-butylphthalate) were missing from the data package

The Form I (TIC) for sample D05946 identified the TIC at 1246 as alphashycaryophyllene while the raw data reported this TIC as l6-octadien-3-ol 37shydimethyl- Clarification was requested

bull The Form I for sample D05949 reported 26-dinitrotoluene and fluoranthene while the quantitation report did not reflect these results The laboratory was asked to verify this discrepancy

bull A relative response factor for 46-dinitro-2-methylphenol was listed on the Form 6 for the initial calibration in association with the 05 ugml standard However this compound was not listed on the quantitation report in the raw data The laboratory was asked to verify this discrepancy

J NEWA16Q Troy Mills LandfillData VahdationDecember 2004DV MemossD05939_svocsim pd Metcalf amp Eddy Inc

Ms Christine Clark Page 8 February 24 2005 Case 0251M SDG D05939

Initial and Continuing Calibrations

Full Scan

The following table summarizes the initial calibration (1C) and continuing calibration (CC) results that failed to meet the relative response factor (RRF) criterion of ^005 andor RSD lt 30 in the 1C andor D lt 25 in the CC for all compounds

Calibration Date 1C CC CC CC 12505 12705 13105 2105

Compound RSD D D D

benzaldehyde 792 155 156 153

hexachlorobutadiene - - - 453

hexachlorocyc lopentadiene 488 448 - 360

24-dimtrophenol 337 - 25 8 -

4-nitrophenol - - - 467

hexachlorobenzene - - - 286

46-dimtro-2-methylphenol 450 - - -

atrazme 434 - - -

pentachlorophenol 384 - - -

33-dichlorobenzidme - 726 463 628

2-fluorophenol (surrogate) - - - 285

Associated samples All samples D05954 D05950 D05951 D05948RE D05952 D05945 D05949 D05946 D05947 D05953RE D05948 D05953 D05949DL

D05945DL D05946DL D05947DL D05948DL D05953DL

- - QC acceptance criteria were not exceeded for this compound

Actions RSD gt 30 Estimate (J and UJ respectively) positive and nondetect results D gt 25 Estimate (J and UJ respectively) positive and nondetect results

JNEWA160 Troy Mills LandftllData VahdationDecember 2004DV MemossD05939_socsim pd Metcalf amp Eddy Inc

Ms Christine Clark Page 9 February 24 2005 Case 0251M SDGD05939

The positive and nondetect results for benzaldehyde hexachlorocyclopentadiene 24-dinitrophenol 46-dinitro-2-methylphenol atrazine and pentachlorophenol in all samples were qualified as estimated (UJ) due to initial calibration RSD exceedances

The positive and nondetect results for benzaldehyde and 33-dichlorobenzidine in all samples for hexachlorobutadiene 4-nitrophenol and hexachlorobenzene in samples D05948RE D05949 and D05953RE for hexachlorocyclopentadiene in samples D05954 D05948RE D05949 and D05953RE and for 24-dinitrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 were qualified as estimated (J and UJ respectively) due to continuing calibration D exceedances

No validation actions were necessary for the calibration nonconformances associated with the dilution sample analyses or for the original analyses of samples D05948 and D05953 since the compounds listed in the table above were not reported from these analyses

No validation actions were necessary for the surrogate compound calibration nonconformance

SIM

The following table summarizes the 1C and CC results that failed to meet the RRF criterion of gt005 andor RSD lt 30 in the 1C andor D lt 25 in the CC for all compounds

Calibration Date 1C 12105 1C 2205 CC 2305

Compound RSD RSD D

pentachlorophenol 621 402 -

di-n-butyl phthalate 331 - 297

bis(2-ethylhexyl)phthalate 347 306

Associated samples D05954 all soil samples all soil samples

- - QC acceptance criteria were not exceeded for this compound

Actions RSD gt 30 Estimate (J and UJ respectively) positive and nondetect results D gt 25 Estimate (J and UJ respectively) positive and nondetect results

The positive di-n-butylphthalate result in equipment blank sample D05954 was qualified as estimated (J) due to the RSD exceedance in the initial calibration

The positive di-n-butylphthalate results in all soil samples were qualified as estimated (J) due to the D exceedance in the continuing calibration

J NE WA160 Troy Mills LandfillData Validation December 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 10 February 24 2005 Case 0251M SDG D05939

The pentachlorophenol and bis(2-ethylhexyl)phthalate results in all samples were reported from the full scan analyses therefore no data validation actions were required as a result of the calibration nonconformances

Blanks

Full Scan

Target compounds were detected as contaminants m the performance evaluation sample (PES) as well as the equipment and laboratory method blanks The highest concentration detected was used to qualify associated sample results The following table summarizes the blank actions as they apply to the samples

Compound Blank

Maximum Concentration

(units)

Blank Action

Level (units)

Quantitation Limit (units)

Affected SamplesActions

benzaldehyde D05954 (EB)

15 ugL NA 100 ugKg Qualify as EB in samples D05950 D05951D05952 D05945 D05946 and D05949

acetophenone D05954 (EB)

0 35 ugL NA 100 ugKg Qualify as EB in sample D05951

4-chloro-3shymethylphenol

D05954 (EB)

5 6 ugL NA 100 ugKg 4-Chloro-3shymethylphenol was not detected in all associated samples No actions were required

di-n-butylphthalate D05954 (EB)

049 ugL NA 100 ugKg Di-n-butylphthalate results were reported from the SIM analyses No actions were required

di-n-butylphthalate method 42 ugKg 420 ugKg 100 ugKg Di-n-butylphthalate results were reported from the SIM analyses No actions were required

bis(2shyethylhexyl)phthalate

method 0 68 ugL 6 8 ugL 1 0 ugL Qualify as nondetect (U) at the QL m equipment blank sample D05954

J NEWA160 Troy Mills LandfillData VahdatwnDecember 20Q4DVMemossD05939_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 11 February 24 2005 Case 0251M SDGD05939

Compound Blank

Maximum Concentration

(units)

Blank Action

Level (units)

Quantitation Limit (units)

bis(2shyethylhexyl)phthalate

PES 490 ugKg 4900 ugKg 100 ugKg

NA - Not applicable SIM - selected ion monitoring EB - equipment blank PES - performance evaluation sample

Sample results were qualified as follows

Affected SamplesActions

Qualify as nondetect (U) at the QL in samples 005950005951 and D05952

bull If sample result was gtQL and ltblank action level (BAL) the result was qualified as a nondetect (U) at the reported concentration

bull If the sample result was sQL and iBAL the results was qualified as a nondetect (U) at the QL bull If the sample result was gtBAL qualification of the data was not required bull If the sample result was nondetect qualification of the data was not required bull Positive results for compounds detected in the equipment blank are flagged with EB

SIM

Target compounds were detected in the laboratory method blanks The following table summarizes the blank actions as they apply to the samples

Compound

di-n-buty Iphthalate

bis(2-ethylhexyl)phthalate

di-n-butylphthalate

Blank Maximum Action Quantitation

Concentration Level Limit Blank (umts^ (units) (units)

method 120ngL 1200 ngL 100 ngL

method 760 ngL 7600 ngL 1600 ngL

method 49 ugKg 490^1^ 10 ugKg

Affected SamplesActions

Qualify as nondetect (U) at the reported value in sample D05954

Bis(2shyethylhexyl)phthalate results were reported from the full scan analyses No actions vere required

Qualify as nondetect (U) at the reported value in all soil samples

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossD05939_nocsirn vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 12 February 24 2005 Case 0251M SDGD05939

Blank Maximum Action Quantitation

Concentration Level Limit Affected Compound Blank (units) (units) (units) Samples Actions

bis(2-ethylhexyl)phthalate method 31 ugKg 3 10 ugKg 160 MgKg Bis(2shyethylhexyl)phthalate results were reported from the full scan analyses No actions were required

Sample results were qualified as follows bull If sample result was gtQL and ltBAL the result was qualified as a nondetect (U) at the reported

concentration bull If the sample result was sQL and ltBAL the results was qualified as a nondetect (U) at the QL bull If the sample result was gtBAL qualification of the data was not required bull If the sample result was nondetect qualification of the data was not required

Internal Standards

Full scan

The following table summarizes the internal standards (IS) that did not meet the acceptable area criteria

Sample ID Internal Standard IS Area Acceptable Range Action

D05948 perylene-d|2 394921 407622-1630486 Results not reported from this analysis

D05948RE chrysene-d2 1720979 350682-1402728 Sample results associated with this IS were either not detected or were reported from the dilution analysis No data validation actions required

D05953 perylene-d2 311034 407622-1630486 Results not reported from this analysis

D05953RE chrysene-dl2 1565496 350682-1402728 Sample results associated with this IS were either not detected or were reported from the dilution analysis No data validation actions required

SIM

Internal standards were within the acceptance criteria in all sample analyses

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DV MemossD05939_svocsim npd Metcalfamp Eddy Inc

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Sensitivity Check

Full Scan

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F05 (low-level)

SW122104F04 (high-level)

Compound

caprolactam

24-dimtrophenol

4-mtrophenol

46-dmitro-2-methylphenol

pentachlorophenol

caprolactam

Recovery Action

0 Raise the quantitation limit to the concentration of the high-level LFB (4 ngL) and qualify as estimated (UJ) the nondetect caprolactam result in sample D05954

0 Since the QL for this compound is 4 |igL the high level LFB (spiked at 4 ugL) was used to evaluate this compound for sensitivity

38 Qualify as estimated (UJ) the nondetect 4shynitrophenol result in sample D05954

38 Qualify as estimated (UJ) the nondetect 46shydimtro-2-methylphenol result in sample D05954

36 Qualify as estimated (UJ) the nondetect pentachlorophenol result in sample D05954

27 Raise the quantitation limit to the concentration of the high-level LFB (4 ugL) and qualify as estimated (UJ) the nondetect caprolactam result in sample D05954

QL - quantitation limit LFB - laboratory fortified blank

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound

SS012805FL01 24-dimethylphenol (low-level)

4-chloroanihne

Action Recovery

26 Qualify as estimated (UJ) the nondetect 24shydimethylphenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shychloroamlme results in all soil samples

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossD05939j5vocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark February 24 2005

LFB

SS012805FL01 (low-level)

SS012805FH01 (high-level)

SIM

Compound

24-dimtrophenol

4-mtrophenol

4 6-dimtro-2-methylphenol

pentachlorophenol

33-dichlorobenzidme

4-chloroanilme

24-dimtrophenol

Page 14 Case 0251M SDG D05939

Action Recovery

0 Raise the quantitation limit to the concentration of the high-level LFB [800 ngKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shynitrophenol results in all soil samples

13 Qualify as estimated (UJ) the nondetect 46shydmitro-2-methylphenol results in all soil samples

32 Qualify as estimated (UJ) the nondetect pentachlorophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 33shydichlorobenzidme results in all soil samples

39 Qualify as estimated (UJ) the nondetect 4shychloroamhne results in all soil samples

21 Raise the quantitation limit to the concentration of the high-level LFB [800 ugKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F03 (low-level)

SW122104F04 (high-level)

Compound

pentachlorophenol

di-n-butylphthalate

bis(2-ethylhexyl)phthalate

di-n-butylphthalate

Recovery

0

327

622

131

Action

Pentachlorophenol was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

J NEWA160 Tro Mills LandfillData VahdationDecember 2004DVMemossD05939_socsim npd Metcalf amp Eddy Inc

Ms Christine Clark Page 15 February 24 2005 Case0251M SDGD05939

LFB Compound Action Recovery

SW122104F04 bis(2-ethylhexyl)phthalate 161 Bis(2-ethylhexyl)phthalate was reported from the (high-level) full scan analysis therefore no actions were

required

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound Action Recovery

SS012805FL02 di-n-butylphthalate 237 Qualify as estimated (J) the positive di-nshy(low-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 376 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 149 Since the QL for this compound is 160 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

indeno( 1 23-cd)pyrene 121 Since the QL for this compound is 1 60 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

SS012805FH02 di-n-butylphthalate 150 Qualify as estimated (J) the positive di-nshy(high-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 185 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 132 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D0595 1 D05952 D05945 D05946 and D05949

QL - quantitation limit

PE Sample ResultsAccuracy Check

PE Sample Results

Full Scan

A single-blind solid PE sample D05939 (PES number SS0491) was analyzed with this data set Eight compounds were scored as Within Limits 2-Chlorophenol acenaphthylene acenaphthene dibenzofuran fluorene anthracene fluoranthene benzo(a)anthracene and chrysene were scored as

J NEWA160 Troy Mills LandfillData VahdatwnDecember 2004DVMemossD05939_svocsim vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 16 February 24 2005 Case 0251M SDGD05939

Action High These compounds were not detected in any of the associated soil samples therefore no data validation actions were required Six compounds (naphthalene hexachlorobenzene phenanthrene pyrene and dibenz(ah)anthracene and benzo(ghi)perylene) were scored as Warning High two compounds (4-hydroxy-4-methyl-2-pentanone and 4-methyl-3-penten-2-one) were scored Non-spiked TIC and one compound (din-n-butylphthalate) was scored Less than CRQL No data validation action is required on the basis of the Warning High Non-spiked TIC and less than CRQL scores Bis(2-ethylhexyl)phthalate was scored as Contaminant This compound was also detected in the associated laboratory method blanks and consequently evaluated in the blank section of this memorandum (please see Blanks above)

Laboratory Control Sample (LCS) Results

Full Scan

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LCS Compound Recovery Action

SW122104L06 caprolactam 35 Qualify as estimated (UJ) the nondetectresult in sample D05954

caprolactam

atrazine 135 Atrazine was not detected in the associaNo actions were required

ted sample

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Recovery Action

SS012805L01 benzaldehyde 46 Qualify as estimated (J) the positive and (UJ) the nondetect benzaldehyde results in all soil samples

4-chloroanihne 35 Qualify as estimated (UJ) the nondetect 4shychloroaruhne results in all soil samples

SIM

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossDQ5939_svocstm vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 17 February 24 2005 Case 0251M SDGD05939

LCS Compound Action Recovery

SW122104L05 pentachlorophenol 194 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 123 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(a)pyrene 122 Benzo(a)pyrene was not detected in the associated sample No actions were required

mdeno( 1 2 3 -cd)pyrene 130 Indeno(l23-cd)pyrene was reported from the full scan analysis therefore no actions were required

dibenz(ah)anthracene 136 Dibenz(ah)anthracene was not detected in the associated sample No actions were required

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Action Recovery

SS012805L02 pentachlorophenol 126 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 142 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(b)fluoranthene 128 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D05951 D05952 D05945 D05946 and D05949

benzo(a)pyrene 121 Qualify as estimated (J) the positive benzo(a)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

mdeno( 1 23-cd)pyrene 129 Qualify as estimated (J) the positive indeno(l23shycd)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

dibenz(ah)anthracene 133 Dibenz(ah)anthracene was not detected in the associated samples No actions were required

J NE WA160 Troy Mills LandfillData Validation December 2004 D V MemossD0593 9_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 18 February 24 2005 Case 0251M SDG D05939

Compound Ouantitation and Reported Ouantitation Limits

Full Scan and SIM

Because of their high moisture content samples D05945 D05946 D05949 D05951 and D05952 were freeze-dried prior to extraction

The following table summarizes the SIM and full scan reporting when data existed for both full scan and SIM analyses Professional judgment was used to select specific analyses in order to report the lowest quantitation limit achievable and to report results with values within the calibration range

Compound Results reported from Full Scan Results reported from SIM

pentachlorophenol all samples none

di-n-butyl phthalate none all samples

benzo(a)anthracene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

bis(2-ethylhexyl)phthalate all samples none

benzo(b)fluoranthene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

benzo(a)pyrene none all samples

indeno(l23-cd)pyrene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

dibenz(ah)anthracene none all samples

Full Scan

The bis(2-ethylhexyl)phthalate results in the following samples were reported from the dilution analysis listed in parentheses since these results exceeded the calibration range in the undiluted analysis D05945 (5x) D05946 (20x) D05947 (20x) D05948 (20x) D05949 (5x) and D05953 (20x)

JNE WA160 Troy Mills LandfillData ValidationDecember 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 19 February 24 2005 Case 0251M SDGD05939

SIM

The following compounds in the samples listed below were qualified as estimated (J) due to uncertainty in the quantitation as a result of the exceeded ion abundance ratio criteria

D05950 di-n-butylphthalate DOS951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate indeno(l23-cd)pyrene D05946 indeno(l23-cd)pyrene DOS 947 di-n-butylphthalate DOS 948 di-n-butylphthalate DOS 949 di-n-butylphthalate D05953 di-n-butylphthalate

Tentatively Identified Compounds (TICs)

One TIC 4-hydroxy-4-methyl-2-pentanone was detected in all samples and is considered an aldol condensation product Consequently this TIC was not included on Table III Tentatively Identified Compound Summary for the affected samples

The following compound in the sample listed was reported twice in the affected sample For this sample this result was renamed to a more general identification since a compound cannot elute at multiple retention times The renamed TIC is described in the table below

Compound name as reported by the Compound name as renamed during data Affected sample laboratory validation

oleic acid unknown D05951

JNEWA160 Troy Mills LandflllData ValidationDecember 2004DV MemossD05939_svocsimwpd MetcalfA Eddy Inc

Ms Christine Clark Page 20 February 24 2005 Case 0251M SDG D05939

Please contact Ms Constance Lapite at (781) 224-6628 or at Constance lapite(am-ecom if you have any questions regarding this Tier II validation

Paula L DiMattei Data Validator

Deborah A Trwini ^mjrjat

Robert Shoemaker Project Chemist

bullgt pound^ampgtlt^ Constance D Lapite MampE RAC Lead Chemist

cc ^James Chow EPA Remedial Project Manager (DV memo and data summary tables) Karen Wedlock-Hunt MampE Project Manager (entire package) Robert Shoemaker Project Chemist (entire package) Troy Mills Landfill Project File WA No 160-RICO-019M (entire package)

Attachments ORDA Table I Recommendation Summary Table Table II Overall Evaluation of Data Table III Tentatively Identified Compound Summary Data Summary Tables Data Validation Worksheets PE Score Report Copy of non-CLP Analytical Method (MampE DAS Specification D-148) Copies of Telephone LogCommunications Forms Supporting Data for Reduced Payment Recommendations (not applicable) Copies of Field Sampling Notes (previously submitted) Copies of EPA-Approved Amendments not QAPjP or SAP (not applicable) CSF Completeness Evidence File Audit (DC-2 Form) DQO Summary Form

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DVMemossD05939_svocsim pd Metcatfamp Eddy Inc

REGION I EPA-NE ORGANIC REGIONAL DATA ASSESSMENT (ORDA)

CASE raquozjggtH _ SITE NAME TV

LAB NAME uoAlaquo Vlaquo- amp+ OF SAMPLESMATRIX

SDG Posirt_ VALIDATION CONTRACTOR

SOW CONTRACT p-rttll-- VALIDATORS NAME

EPA-NE DV TIER LEVEL JC_ DATE DP RECD BY EPA-NE

TPOPO ACTION _ FYI ^ DV COMPLETION DATE

ANALYTICAL DATA QUALITY SUMMARY tffpft^m t~

bullVGA SV-SM PestPCB 1 Preservation and Contractual Holding Times 2 GCMS GCECD Instrument Performance Check raquo 3 Initial Calibration laquo 4 Continuing Calibration o 5 Blanks ~ o 6 Surrogate Compounds raquo 7 Internal Standards o 8 Matrix SpikeMatrix Spike Duplicate ggt 9 Sensitivity Check 0 10 PE Samples-Accuracy Check 0 11 Target Compound Identification jpy 12 Compound Quantitation and Reported QLs o 13 Tentatively Identified Compounds o 14 Semivolatile CleanupPesticidePCB Cleanup ulaquor 15 Data Completeness 0 16 Overall Evaluation of Data laquo

o = Data had no problems or were qualified due to minor contractual problems m = Data were qualified due to major contractual problems z = Data were rejected as unusable due major contractual problems

ACTION ITEMS (z items)

AREAS OF CONCERN (m items)

COMMENTS

This form assesses the analytical data quality in terms of contractual compliance only It does not assess sampling errors andor non-contractual analytical issues that affect data quality

Check ACTION only if contractual defects resulted in reduced paymentdata rejection recommendations

Validator t ltiJSagt3gtlt -3 Date

INSTRUCTIONS ON REVERSE SIDE

1296

Table I Recommendation Summary

Soil Semivolatile Organic Analysis Troy Mills Landfill Superfund Site

Case0251M SDGD05939

Sample ID Matrix

D05945 SO

D05946 SO

D05947 SO (FD)

D05948 SO

D05949 SO

D05950 SO

D05951 SO

D05952 SO

D05953 SO (FD)

D05954 EB

EB shy Equipment Blank FD shy Field Duplicate SOshy Soil

Qualifier

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 11 13 14 15

2 Jl 3 4 7 8 9 10 13 15

A 2 jl 3 4 7 8 9 10 13 15

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 jl 3 4 7 8 9 10 13 15

A 2 3 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 Jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 13 15

^2 4 jl 2 3 5 6 7 12

A - Accept the data but qualify the positive results for benzaldehyde in samples D05945 D05946 D05949 D05950 D05951 and D05952 and for acetophenone in sample D05951 as (EB) due to equipment blank contamination

A2 - Accept the data but qualify the positive result for di-n-butylphthalate as nondetect (U) at the reported value due to laboratory method blank contamination

A5 - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to PE sample contamination

A - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to laboratory method blank contamination

J - Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde hexachlorocyclopentadiene 24shydmitrophenol 46-dmitro-2-methylphenol atrazine and pentachlorophenol due to initial calibration RSD exceedances

J2 Estimate (J) the positive result for di-n-butyl phthalate due to the initial calibration RSD exceedance

J3 Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde and 33-dichlorobenzidme in all samples for hexachlorobutadiene 4-mtrophenol and hexachlorobenzene m samples D05948 D05949 and D05953 for hexachlorocyclopentadiene m samples D05954 D05948 D05949 and D05953 and for 24shydimtrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 due to the continuing calibration D exceedances

J4 - Estimate (J) the positive results for di-n-butylphthalate in all soil samples due to continuing calibration exceedance

J5 - Estimate (UJ) the nondetect caprolactam result and raise the quantitation limit to 4 ugL (equivalent to the concentration of the high-level LFB) due to low low-level and high-level LFB recoveries This result may be biased low

J6 - Estimate (UJ) the nondetect results for 4-mtrophenol 46-dmitro-2-methylphenol and pentachlorophenol due to low low-level LFB recoveries These results may be biased low

J7 - Estimate (J) the positive result for di-n-butylphthalate due to high low-level and high-level LFB recoveries This result may be biased high

J8 - Estimate (UJ) the nondetect 24-dmitrophenol result and raise the quantitation limit to 800 ugKg (equivalent to the concentration of the high-level LFB and corrected for all preparation factors) due to low low-level and high-level LFB recoveries This result may be biased low

J9 - Estimate (UJ) the nondetect results for 24-dimethylphenol 4-mtrophenol 46-dimrro-2-methylphenol pentachlorophenol and 33-dichlorobenzidme due to low low-level LFB recoveries These results may be biased low

J10 - Estimate (UJ) the nondetect result 4-chIoroamlme due to low low-level and high-le el LFB recoveries This result may be biased low

J1 - Estimate (J) the positive result for benzo(b)fluoranthene due to high high-level LFB reco ery This result may be biased high

J12 - Estimate (UJ) the nondetect caprolactam result due to low LCS recovery This result may be biased low

J3 - Estimate (UJ) the nondetect benzaldehyde and 4-chloroamline results due to low LCS recoveries The results may be biased low

J14 - Estimate (J) the positive results for benzo(b)fluoranthene benzo(a)pyrene and mdeno(l23-cd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 due to high LCS recoveries The results may be biased high

J15 - Estimate (J) the positive results for the following compounds in the samples listed below due to uncertainty in the quantitation as a result of the exceeded ion abundance ration criteria

DOS 950 di-n-butylphthalate DOS 951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate mdeno(l23-cd)pyrene D05946 mdeno(l23-cd)pyrene D05947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate D05953 di-n-butylphthalate

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Page 6: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

Ms Christine Clark Page 6 February 24 2005 Case 0251M SDG D05939

The positive results for di-n-butylphthalate in all soil samples were qualified as estimated (J) due to high recoveries in the low-level and high-level LFB analyses These results are usable for project objectives as estimated values that maybe biased high Note that the di-n-butylphthalate results in all soil samples were also qualified as nondetect (U) due to method blank contamination Therefore the overall qualification for these results is estimated nondetect (UJ) These qualifications have a minor impact on data usability

The positive results for benzo(b)fluoranthene in samples D05951 D05952 D05945 D05946 and D05949 were qualified as estimated (J) due to high recovery in the high-level LFB analyses These results are usable for project objectives as estimated values that may be biased high These qualifications have a minor impact on data usability

The nondetect result for caprolactam in equipment blank sample D05954 was qualified as estimated (UJ) due to the low recovery in the laboratory control sample (LCS) analysis This result is usable for project objectives as a nondetect with an estimated quantitation limit that may be biased low These qualifications have a minor impact on data usability

The nondetect results for benzaldehyde and 4-chloroaniline in all soil samples were qualified as estimated (UJ) due to low recoveries in the LCS analyses These results are usable for project objectives as nondetects with estimated quantitation limits that may be biased low These qualifications have a minor impact on data usability

The positive results for benzo(b)fluoranthene benzo(a)pyrene and indeno(l23shycd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 were qualified as estimated (J) due to the high recoveries in the LCS analyses These results are usable for project objectives as estimated values that may be biased high These qualifications have a minor impact on data usability

JNEWAI60 Troy Mills LandfillData ValidationDecember 2004DV MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 7 February 24 2005 Case 0251M SDG D05939

bull The following compounds in the samples listed below were qualified as estimated (J) due to uncertainty in the quantitation as a result of the exceeded ion abundance ratio criteria These results are usable for project objectives as estimated values Note that the results for di-n-butylphthalate in samples D05950 D05951 D05952 D05945 D05947 D05948 D05949 and D05953 were also qualified as nondetect (U) due to method blank contamination Therefore the overall qualification for these results is estimated nondetect (UJ) These qualifications have a minor impact on data usability

D05950 di-n-butylphthalate D05951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate indeno(l23-cd)pyrene D05946 indeno(l23-cd)pyrene DOS 947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate DOS 95 3 di-n-butylphthalate

Data Completeness (CSF Audit)

The following information was missing or incorrect in the data package This missing or incorrect information was requested from the laboratory on February 7 and 152005 A resubmittal response was received at MampE on February 18 2005 adequately addressing these issues

bull The method detection limit (MDL) study results for two selected ion monitoring (SIM) compounds (pentachlorophenol and di-n-butylphthalate) were missing from the data package

The Form I (TIC) for sample D05946 identified the TIC at 1246 as alphashycaryophyllene while the raw data reported this TIC as l6-octadien-3-ol 37shydimethyl- Clarification was requested

bull The Form I for sample D05949 reported 26-dinitrotoluene and fluoranthene while the quantitation report did not reflect these results The laboratory was asked to verify this discrepancy

bull A relative response factor for 46-dinitro-2-methylphenol was listed on the Form 6 for the initial calibration in association with the 05 ugml standard However this compound was not listed on the quantitation report in the raw data The laboratory was asked to verify this discrepancy

J NEWA16Q Troy Mills LandfillData VahdationDecember 2004DV MemossD05939_svocsim pd Metcalf amp Eddy Inc

Ms Christine Clark Page 8 February 24 2005 Case 0251M SDG D05939

Initial and Continuing Calibrations

Full Scan

The following table summarizes the initial calibration (1C) and continuing calibration (CC) results that failed to meet the relative response factor (RRF) criterion of ^005 andor RSD lt 30 in the 1C andor D lt 25 in the CC for all compounds

Calibration Date 1C CC CC CC 12505 12705 13105 2105

Compound RSD D D D

benzaldehyde 792 155 156 153

hexachlorobutadiene - - - 453

hexachlorocyc lopentadiene 488 448 - 360

24-dimtrophenol 337 - 25 8 -

4-nitrophenol - - - 467

hexachlorobenzene - - - 286

46-dimtro-2-methylphenol 450 - - -

atrazme 434 - - -

pentachlorophenol 384 - - -

33-dichlorobenzidme - 726 463 628

2-fluorophenol (surrogate) - - - 285

Associated samples All samples D05954 D05950 D05951 D05948RE D05952 D05945 D05949 D05946 D05947 D05953RE D05948 D05953 D05949DL

D05945DL D05946DL D05947DL D05948DL D05953DL

- - QC acceptance criteria were not exceeded for this compound

Actions RSD gt 30 Estimate (J and UJ respectively) positive and nondetect results D gt 25 Estimate (J and UJ respectively) positive and nondetect results

JNEWA160 Troy Mills LandftllData VahdationDecember 2004DV MemossD05939_socsim pd Metcalf amp Eddy Inc

Ms Christine Clark Page 9 February 24 2005 Case 0251M SDGD05939

The positive and nondetect results for benzaldehyde hexachlorocyclopentadiene 24-dinitrophenol 46-dinitro-2-methylphenol atrazine and pentachlorophenol in all samples were qualified as estimated (UJ) due to initial calibration RSD exceedances

The positive and nondetect results for benzaldehyde and 33-dichlorobenzidine in all samples for hexachlorobutadiene 4-nitrophenol and hexachlorobenzene in samples D05948RE D05949 and D05953RE for hexachlorocyclopentadiene in samples D05954 D05948RE D05949 and D05953RE and for 24-dinitrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 were qualified as estimated (J and UJ respectively) due to continuing calibration D exceedances

No validation actions were necessary for the calibration nonconformances associated with the dilution sample analyses or for the original analyses of samples D05948 and D05953 since the compounds listed in the table above were not reported from these analyses

No validation actions were necessary for the surrogate compound calibration nonconformance

SIM

The following table summarizes the 1C and CC results that failed to meet the RRF criterion of gt005 andor RSD lt 30 in the 1C andor D lt 25 in the CC for all compounds

Calibration Date 1C 12105 1C 2205 CC 2305

Compound RSD RSD D

pentachlorophenol 621 402 -

di-n-butyl phthalate 331 - 297

bis(2-ethylhexyl)phthalate 347 306

Associated samples D05954 all soil samples all soil samples

- - QC acceptance criteria were not exceeded for this compound

Actions RSD gt 30 Estimate (J and UJ respectively) positive and nondetect results D gt 25 Estimate (J and UJ respectively) positive and nondetect results

The positive di-n-butylphthalate result in equipment blank sample D05954 was qualified as estimated (J) due to the RSD exceedance in the initial calibration

The positive di-n-butylphthalate results in all soil samples were qualified as estimated (J) due to the D exceedance in the continuing calibration

J NE WA160 Troy Mills LandfillData Validation December 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 10 February 24 2005 Case 0251M SDG D05939

The pentachlorophenol and bis(2-ethylhexyl)phthalate results in all samples were reported from the full scan analyses therefore no data validation actions were required as a result of the calibration nonconformances

Blanks

Full Scan

Target compounds were detected as contaminants m the performance evaluation sample (PES) as well as the equipment and laboratory method blanks The highest concentration detected was used to qualify associated sample results The following table summarizes the blank actions as they apply to the samples

Compound Blank

Maximum Concentration

(units)

Blank Action

Level (units)

Quantitation Limit (units)

Affected SamplesActions

benzaldehyde D05954 (EB)

15 ugL NA 100 ugKg Qualify as EB in samples D05950 D05951D05952 D05945 D05946 and D05949

acetophenone D05954 (EB)

0 35 ugL NA 100 ugKg Qualify as EB in sample D05951

4-chloro-3shymethylphenol

D05954 (EB)

5 6 ugL NA 100 ugKg 4-Chloro-3shymethylphenol was not detected in all associated samples No actions were required

di-n-butylphthalate D05954 (EB)

049 ugL NA 100 ugKg Di-n-butylphthalate results were reported from the SIM analyses No actions were required

di-n-butylphthalate method 42 ugKg 420 ugKg 100 ugKg Di-n-butylphthalate results were reported from the SIM analyses No actions were required

bis(2shyethylhexyl)phthalate

method 0 68 ugL 6 8 ugL 1 0 ugL Qualify as nondetect (U) at the QL m equipment blank sample D05954

J NEWA160 Troy Mills LandfillData VahdatwnDecember 20Q4DVMemossD05939_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 11 February 24 2005 Case 0251M SDGD05939

Compound Blank

Maximum Concentration

(units)

Blank Action

Level (units)

Quantitation Limit (units)

bis(2shyethylhexyl)phthalate

PES 490 ugKg 4900 ugKg 100 ugKg

NA - Not applicable SIM - selected ion monitoring EB - equipment blank PES - performance evaluation sample

Sample results were qualified as follows

Affected SamplesActions

Qualify as nondetect (U) at the QL in samples 005950005951 and D05952

bull If sample result was gtQL and ltblank action level (BAL) the result was qualified as a nondetect (U) at the reported concentration

bull If the sample result was sQL and iBAL the results was qualified as a nondetect (U) at the QL bull If the sample result was gtBAL qualification of the data was not required bull If the sample result was nondetect qualification of the data was not required bull Positive results for compounds detected in the equipment blank are flagged with EB

SIM

Target compounds were detected in the laboratory method blanks The following table summarizes the blank actions as they apply to the samples

Compound

di-n-buty Iphthalate

bis(2-ethylhexyl)phthalate

di-n-butylphthalate

Blank Maximum Action Quantitation

Concentration Level Limit Blank (umts^ (units) (units)

method 120ngL 1200 ngL 100 ngL

method 760 ngL 7600 ngL 1600 ngL

method 49 ugKg 490^1^ 10 ugKg

Affected SamplesActions

Qualify as nondetect (U) at the reported value in sample D05954

Bis(2shyethylhexyl)phthalate results were reported from the full scan analyses No actions vere required

Qualify as nondetect (U) at the reported value in all soil samples

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossD05939_nocsirn vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 12 February 24 2005 Case 0251M SDGD05939

Blank Maximum Action Quantitation

Concentration Level Limit Affected Compound Blank (units) (units) (units) Samples Actions

bis(2-ethylhexyl)phthalate method 31 ugKg 3 10 ugKg 160 MgKg Bis(2shyethylhexyl)phthalate results were reported from the full scan analyses No actions were required

Sample results were qualified as follows bull If sample result was gtQL and ltBAL the result was qualified as a nondetect (U) at the reported

concentration bull If the sample result was sQL and ltBAL the results was qualified as a nondetect (U) at the QL bull If the sample result was gtBAL qualification of the data was not required bull If the sample result was nondetect qualification of the data was not required

Internal Standards

Full scan

The following table summarizes the internal standards (IS) that did not meet the acceptable area criteria

Sample ID Internal Standard IS Area Acceptable Range Action

D05948 perylene-d|2 394921 407622-1630486 Results not reported from this analysis

D05948RE chrysene-d2 1720979 350682-1402728 Sample results associated with this IS were either not detected or were reported from the dilution analysis No data validation actions required

D05953 perylene-d2 311034 407622-1630486 Results not reported from this analysis

D05953RE chrysene-dl2 1565496 350682-1402728 Sample results associated with this IS were either not detected or were reported from the dilution analysis No data validation actions required

SIM

Internal standards were within the acceptance criteria in all sample analyses

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DV MemossD05939_svocsim npd Metcalfamp Eddy Inc

Ms Christine Clark Page 13 February 24 2005 Case 0251M SDG D05939

Sensitivity Check

Full Scan

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F05 (low-level)

SW122104F04 (high-level)

Compound

caprolactam

24-dimtrophenol

4-mtrophenol

46-dmitro-2-methylphenol

pentachlorophenol

caprolactam

Recovery Action

0 Raise the quantitation limit to the concentration of the high-level LFB (4 ngL) and qualify as estimated (UJ) the nondetect caprolactam result in sample D05954

0 Since the QL for this compound is 4 |igL the high level LFB (spiked at 4 ugL) was used to evaluate this compound for sensitivity

38 Qualify as estimated (UJ) the nondetect 4shynitrophenol result in sample D05954

38 Qualify as estimated (UJ) the nondetect 46shydimtro-2-methylphenol result in sample D05954

36 Qualify as estimated (UJ) the nondetect pentachlorophenol result in sample D05954

27 Raise the quantitation limit to the concentration of the high-level LFB (4 ugL) and qualify as estimated (UJ) the nondetect caprolactam result in sample D05954

QL - quantitation limit LFB - laboratory fortified blank

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound

SS012805FL01 24-dimethylphenol (low-level)

4-chloroanihne

Action Recovery

26 Qualify as estimated (UJ) the nondetect 24shydimethylphenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shychloroamlme results in all soil samples

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossD05939j5vocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark February 24 2005

LFB

SS012805FL01 (low-level)

SS012805FH01 (high-level)

SIM

Compound

24-dimtrophenol

4-mtrophenol

4 6-dimtro-2-methylphenol

pentachlorophenol

33-dichlorobenzidme

4-chloroanilme

24-dimtrophenol

Page 14 Case 0251M SDG D05939

Action Recovery

0 Raise the quantitation limit to the concentration of the high-level LFB [800 ngKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shynitrophenol results in all soil samples

13 Qualify as estimated (UJ) the nondetect 46shydmitro-2-methylphenol results in all soil samples

32 Qualify as estimated (UJ) the nondetect pentachlorophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 33shydichlorobenzidme results in all soil samples

39 Qualify as estimated (UJ) the nondetect 4shychloroamhne results in all soil samples

21 Raise the quantitation limit to the concentration of the high-level LFB [800 ugKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F03 (low-level)

SW122104F04 (high-level)

Compound

pentachlorophenol

di-n-butylphthalate

bis(2-ethylhexyl)phthalate

di-n-butylphthalate

Recovery

0

327

622

131

Action

Pentachlorophenol was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

J NEWA160 Tro Mills LandfillData VahdationDecember 2004DVMemossD05939_socsim npd Metcalf amp Eddy Inc

Ms Christine Clark Page 15 February 24 2005 Case0251M SDGD05939

LFB Compound Action Recovery

SW122104F04 bis(2-ethylhexyl)phthalate 161 Bis(2-ethylhexyl)phthalate was reported from the (high-level) full scan analysis therefore no actions were

required

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound Action Recovery

SS012805FL02 di-n-butylphthalate 237 Qualify as estimated (J) the positive di-nshy(low-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 376 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 149 Since the QL for this compound is 160 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

indeno( 1 23-cd)pyrene 121 Since the QL for this compound is 1 60 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

SS012805FH02 di-n-butylphthalate 150 Qualify as estimated (J) the positive di-nshy(high-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 185 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 132 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D0595 1 D05952 D05945 D05946 and D05949

QL - quantitation limit

PE Sample ResultsAccuracy Check

PE Sample Results

Full Scan

A single-blind solid PE sample D05939 (PES number SS0491) was analyzed with this data set Eight compounds were scored as Within Limits 2-Chlorophenol acenaphthylene acenaphthene dibenzofuran fluorene anthracene fluoranthene benzo(a)anthracene and chrysene were scored as

J NEWA160 Troy Mills LandfillData VahdatwnDecember 2004DVMemossD05939_svocsim vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 16 February 24 2005 Case 0251M SDGD05939

Action High These compounds were not detected in any of the associated soil samples therefore no data validation actions were required Six compounds (naphthalene hexachlorobenzene phenanthrene pyrene and dibenz(ah)anthracene and benzo(ghi)perylene) were scored as Warning High two compounds (4-hydroxy-4-methyl-2-pentanone and 4-methyl-3-penten-2-one) were scored Non-spiked TIC and one compound (din-n-butylphthalate) was scored Less than CRQL No data validation action is required on the basis of the Warning High Non-spiked TIC and less than CRQL scores Bis(2-ethylhexyl)phthalate was scored as Contaminant This compound was also detected in the associated laboratory method blanks and consequently evaluated in the blank section of this memorandum (please see Blanks above)

Laboratory Control Sample (LCS) Results

Full Scan

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LCS Compound Recovery Action

SW122104L06 caprolactam 35 Qualify as estimated (UJ) the nondetectresult in sample D05954

caprolactam

atrazine 135 Atrazine was not detected in the associaNo actions were required

ted sample

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Recovery Action

SS012805L01 benzaldehyde 46 Qualify as estimated (J) the positive and (UJ) the nondetect benzaldehyde results in all soil samples

4-chloroanihne 35 Qualify as estimated (UJ) the nondetect 4shychloroaruhne results in all soil samples

SIM

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossDQ5939_svocstm vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 17 February 24 2005 Case 0251M SDGD05939

LCS Compound Action Recovery

SW122104L05 pentachlorophenol 194 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 123 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(a)pyrene 122 Benzo(a)pyrene was not detected in the associated sample No actions were required

mdeno( 1 2 3 -cd)pyrene 130 Indeno(l23-cd)pyrene was reported from the full scan analysis therefore no actions were required

dibenz(ah)anthracene 136 Dibenz(ah)anthracene was not detected in the associated sample No actions were required

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Action Recovery

SS012805L02 pentachlorophenol 126 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 142 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(b)fluoranthene 128 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D05951 D05952 D05945 D05946 and D05949

benzo(a)pyrene 121 Qualify as estimated (J) the positive benzo(a)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

mdeno( 1 23-cd)pyrene 129 Qualify as estimated (J) the positive indeno(l23shycd)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

dibenz(ah)anthracene 133 Dibenz(ah)anthracene was not detected in the associated samples No actions were required

J NE WA160 Troy Mills LandfillData Validation December 2004 D V MemossD0593 9_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 18 February 24 2005 Case 0251M SDG D05939

Compound Ouantitation and Reported Ouantitation Limits

Full Scan and SIM

Because of their high moisture content samples D05945 D05946 D05949 D05951 and D05952 were freeze-dried prior to extraction

The following table summarizes the SIM and full scan reporting when data existed for both full scan and SIM analyses Professional judgment was used to select specific analyses in order to report the lowest quantitation limit achievable and to report results with values within the calibration range

Compound Results reported from Full Scan Results reported from SIM

pentachlorophenol all samples none

di-n-butyl phthalate none all samples

benzo(a)anthracene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

bis(2-ethylhexyl)phthalate all samples none

benzo(b)fluoranthene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

benzo(a)pyrene none all samples

indeno(l23-cd)pyrene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

dibenz(ah)anthracene none all samples

Full Scan

The bis(2-ethylhexyl)phthalate results in the following samples were reported from the dilution analysis listed in parentheses since these results exceeded the calibration range in the undiluted analysis D05945 (5x) D05946 (20x) D05947 (20x) D05948 (20x) D05949 (5x) and D05953 (20x)

JNE WA160 Troy Mills LandfillData ValidationDecember 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 19 February 24 2005 Case 0251M SDGD05939

SIM

The following compounds in the samples listed below were qualified as estimated (J) due to uncertainty in the quantitation as a result of the exceeded ion abundance ratio criteria

D05950 di-n-butylphthalate DOS951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate indeno(l23-cd)pyrene D05946 indeno(l23-cd)pyrene DOS 947 di-n-butylphthalate DOS 948 di-n-butylphthalate DOS 949 di-n-butylphthalate D05953 di-n-butylphthalate

Tentatively Identified Compounds (TICs)

One TIC 4-hydroxy-4-methyl-2-pentanone was detected in all samples and is considered an aldol condensation product Consequently this TIC was not included on Table III Tentatively Identified Compound Summary for the affected samples

The following compound in the sample listed was reported twice in the affected sample For this sample this result was renamed to a more general identification since a compound cannot elute at multiple retention times The renamed TIC is described in the table below

Compound name as reported by the Compound name as renamed during data Affected sample laboratory validation

oleic acid unknown D05951

JNEWA160 Troy Mills LandflllData ValidationDecember 2004DV MemossD05939_svocsimwpd MetcalfA Eddy Inc

Ms Christine Clark Page 20 February 24 2005 Case 0251M SDG D05939

Please contact Ms Constance Lapite at (781) 224-6628 or at Constance lapite(am-ecom if you have any questions regarding this Tier II validation

Paula L DiMattei Data Validator

Deborah A Trwini ^mjrjat

Robert Shoemaker Project Chemist

bullgt pound^ampgtlt^ Constance D Lapite MampE RAC Lead Chemist

cc ^James Chow EPA Remedial Project Manager (DV memo and data summary tables) Karen Wedlock-Hunt MampE Project Manager (entire package) Robert Shoemaker Project Chemist (entire package) Troy Mills Landfill Project File WA No 160-RICO-019M (entire package)

Attachments ORDA Table I Recommendation Summary Table Table II Overall Evaluation of Data Table III Tentatively Identified Compound Summary Data Summary Tables Data Validation Worksheets PE Score Report Copy of non-CLP Analytical Method (MampE DAS Specification D-148) Copies of Telephone LogCommunications Forms Supporting Data for Reduced Payment Recommendations (not applicable) Copies of Field Sampling Notes (previously submitted) Copies of EPA-Approved Amendments not QAPjP or SAP (not applicable) CSF Completeness Evidence File Audit (DC-2 Form) DQO Summary Form

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DVMemossD05939_svocsim pd Metcatfamp Eddy Inc

REGION I EPA-NE ORGANIC REGIONAL DATA ASSESSMENT (ORDA)

CASE raquozjggtH _ SITE NAME TV

LAB NAME uoAlaquo Vlaquo- amp+ OF SAMPLESMATRIX

SDG Posirt_ VALIDATION CONTRACTOR

SOW CONTRACT p-rttll-- VALIDATORS NAME

EPA-NE DV TIER LEVEL JC_ DATE DP RECD BY EPA-NE

TPOPO ACTION _ FYI ^ DV COMPLETION DATE

ANALYTICAL DATA QUALITY SUMMARY tffpft^m t~

bullVGA SV-SM PestPCB 1 Preservation and Contractual Holding Times 2 GCMS GCECD Instrument Performance Check raquo 3 Initial Calibration laquo 4 Continuing Calibration o 5 Blanks ~ o 6 Surrogate Compounds raquo 7 Internal Standards o 8 Matrix SpikeMatrix Spike Duplicate ggt 9 Sensitivity Check 0 10 PE Samples-Accuracy Check 0 11 Target Compound Identification jpy 12 Compound Quantitation and Reported QLs o 13 Tentatively Identified Compounds o 14 Semivolatile CleanupPesticidePCB Cleanup ulaquor 15 Data Completeness 0 16 Overall Evaluation of Data laquo

o = Data had no problems or were qualified due to minor contractual problems m = Data were qualified due to major contractual problems z = Data were rejected as unusable due major contractual problems

ACTION ITEMS (z items)

AREAS OF CONCERN (m items)

COMMENTS

This form assesses the analytical data quality in terms of contractual compliance only It does not assess sampling errors andor non-contractual analytical issues that affect data quality

Check ACTION only if contractual defects resulted in reduced paymentdata rejection recommendations

Validator t ltiJSagt3gtlt -3 Date

INSTRUCTIONS ON REVERSE SIDE

1296

Table I Recommendation Summary

Soil Semivolatile Organic Analysis Troy Mills Landfill Superfund Site

Case0251M SDGD05939

Sample ID Matrix

D05945 SO

D05946 SO

D05947 SO (FD)

D05948 SO

D05949 SO

D05950 SO

D05951 SO

D05952 SO

D05953 SO (FD)

D05954 EB

EB shy Equipment Blank FD shy Field Duplicate SOshy Soil

Qualifier

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 11 13 14 15

2 Jl 3 4 7 8 9 10 13 15

A 2 jl 3 4 7 8 9 10 13 15

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 jl 3 4 7 8 9 10 13 15

A 2 3 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 Jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 13 15

^2 4 jl 2 3 5 6 7 12

A - Accept the data but qualify the positive results for benzaldehyde in samples D05945 D05946 D05949 D05950 D05951 and D05952 and for acetophenone in sample D05951 as (EB) due to equipment blank contamination

A2 - Accept the data but qualify the positive result for di-n-butylphthalate as nondetect (U) at the reported value due to laboratory method blank contamination

A5 - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to PE sample contamination

A - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to laboratory method blank contamination

J - Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde hexachlorocyclopentadiene 24shydmitrophenol 46-dmitro-2-methylphenol atrazine and pentachlorophenol due to initial calibration RSD exceedances

J2 Estimate (J) the positive result for di-n-butyl phthalate due to the initial calibration RSD exceedance

J3 Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde and 33-dichlorobenzidme in all samples for hexachlorobutadiene 4-mtrophenol and hexachlorobenzene m samples D05948 D05949 and D05953 for hexachlorocyclopentadiene m samples D05954 D05948 D05949 and D05953 and for 24shydimtrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 due to the continuing calibration D exceedances

J4 - Estimate (J) the positive results for di-n-butylphthalate in all soil samples due to continuing calibration exceedance

J5 - Estimate (UJ) the nondetect caprolactam result and raise the quantitation limit to 4 ugL (equivalent to the concentration of the high-level LFB) due to low low-level and high-level LFB recoveries This result may be biased low

J6 - Estimate (UJ) the nondetect results for 4-mtrophenol 46-dmitro-2-methylphenol and pentachlorophenol due to low low-level LFB recoveries These results may be biased low

J7 - Estimate (J) the positive result for di-n-butylphthalate due to high low-level and high-level LFB recoveries This result may be biased high

J8 - Estimate (UJ) the nondetect 24-dmitrophenol result and raise the quantitation limit to 800 ugKg (equivalent to the concentration of the high-level LFB and corrected for all preparation factors) due to low low-level and high-level LFB recoveries This result may be biased low

J9 - Estimate (UJ) the nondetect results for 24-dimethylphenol 4-mtrophenol 46-dimrro-2-methylphenol pentachlorophenol and 33-dichlorobenzidme due to low low-level LFB recoveries These results may be biased low

J10 - Estimate (UJ) the nondetect result 4-chIoroamlme due to low low-level and high-le el LFB recoveries This result may be biased low

J1 - Estimate (J) the positive result for benzo(b)fluoranthene due to high high-level LFB reco ery This result may be biased high

J12 - Estimate (UJ) the nondetect caprolactam result due to low LCS recovery This result may be biased low

J3 - Estimate (UJ) the nondetect benzaldehyde and 4-chloroamline results due to low LCS recoveries The results may be biased low

J14 - Estimate (J) the positive results for benzo(b)fluoranthene benzo(a)pyrene and mdeno(l23-cd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 due to high LCS recoveries The results may be biased high

J15 - Estimate (J) the positive results for the following compounds in the samples listed below due to uncertainty in the quantitation as a result of the exceeded ion abundance ration criteria

DOS 950 di-n-butylphthalate DOS 951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate mdeno(l23-cd)pyrene D05946 mdeno(l23-cd)pyrene D05947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate D05953 di-n-butylphthalate

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Page 7: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

Ms Christine Clark Page 7 February 24 2005 Case 0251M SDG D05939

bull The following compounds in the samples listed below were qualified as estimated (J) due to uncertainty in the quantitation as a result of the exceeded ion abundance ratio criteria These results are usable for project objectives as estimated values Note that the results for di-n-butylphthalate in samples D05950 D05951 D05952 D05945 D05947 D05948 D05949 and D05953 were also qualified as nondetect (U) due to method blank contamination Therefore the overall qualification for these results is estimated nondetect (UJ) These qualifications have a minor impact on data usability

D05950 di-n-butylphthalate D05951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate indeno(l23-cd)pyrene D05946 indeno(l23-cd)pyrene DOS 947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate DOS 95 3 di-n-butylphthalate

Data Completeness (CSF Audit)

The following information was missing or incorrect in the data package This missing or incorrect information was requested from the laboratory on February 7 and 152005 A resubmittal response was received at MampE on February 18 2005 adequately addressing these issues

bull The method detection limit (MDL) study results for two selected ion monitoring (SIM) compounds (pentachlorophenol and di-n-butylphthalate) were missing from the data package

The Form I (TIC) for sample D05946 identified the TIC at 1246 as alphashycaryophyllene while the raw data reported this TIC as l6-octadien-3-ol 37shydimethyl- Clarification was requested

bull The Form I for sample D05949 reported 26-dinitrotoluene and fluoranthene while the quantitation report did not reflect these results The laboratory was asked to verify this discrepancy

bull A relative response factor for 46-dinitro-2-methylphenol was listed on the Form 6 for the initial calibration in association with the 05 ugml standard However this compound was not listed on the quantitation report in the raw data The laboratory was asked to verify this discrepancy

J NEWA16Q Troy Mills LandfillData VahdationDecember 2004DV MemossD05939_svocsim pd Metcalf amp Eddy Inc

Ms Christine Clark Page 8 February 24 2005 Case 0251M SDG D05939

Initial and Continuing Calibrations

Full Scan

The following table summarizes the initial calibration (1C) and continuing calibration (CC) results that failed to meet the relative response factor (RRF) criterion of ^005 andor RSD lt 30 in the 1C andor D lt 25 in the CC for all compounds

Calibration Date 1C CC CC CC 12505 12705 13105 2105

Compound RSD D D D

benzaldehyde 792 155 156 153

hexachlorobutadiene - - - 453

hexachlorocyc lopentadiene 488 448 - 360

24-dimtrophenol 337 - 25 8 -

4-nitrophenol - - - 467

hexachlorobenzene - - - 286

46-dimtro-2-methylphenol 450 - - -

atrazme 434 - - -

pentachlorophenol 384 - - -

33-dichlorobenzidme - 726 463 628

2-fluorophenol (surrogate) - - - 285

Associated samples All samples D05954 D05950 D05951 D05948RE D05952 D05945 D05949 D05946 D05947 D05953RE D05948 D05953 D05949DL

D05945DL D05946DL D05947DL D05948DL D05953DL

- - QC acceptance criteria were not exceeded for this compound

Actions RSD gt 30 Estimate (J and UJ respectively) positive and nondetect results D gt 25 Estimate (J and UJ respectively) positive and nondetect results

JNEWA160 Troy Mills LandftllData VahdationDecember 2004DV MemossD05939_socsim pd Metcalf amp Eddy Inc

Ms Christine Clark Page 9 February 24 2005 Case 0251M SDGD05939

The positive and nondetect results for benzaldehyde hexachlorocyclopentadiene 24-dinitrophenol 46-dinitro-2-methylphenol atrazine and pentachlorophenol in all samples were qualified as estimated (UJ) due to initial calibration RSD exceedances

The positive and nondetect results for benzaldehyde and 33-dichlorobenzidine in all samples for hexachlorobutadiene 4-nitrophenol and hexachlorobenzene in samples D05948RE D05949 and D05953RE for hexachlorocyclopentadiene in samples D05954 D05948RE D05949 and D05953RE and for 24-dinitrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 were qualified as estimated (J and UJ respectively) due to continuing calibration D exceedances

No validation actions were necessary for the calibration nonconformances associated with the dilution sample analyses or for the original analyses of samples D05948 and D05953 since the compounds listed in the table above were not reported from these analyses

No validation actions were necessary for the surrogate compound calibration nonconformance

SIM

The following table summarizes the 1C and CC results that failed to meet the RRF criterion of gt005 andor RSD lt 30 in the 1C andor D lt 25 in the CC for all compounds

Calibration Date 1C 12105 1C 2205 CC 2305

Compound RSD RSD D

pentachlorophenol 621 402 -

di-n-butyl phthalate 331 - 297

bis(2-ethylhexyl)phthalate 347 306

Associated samples D05954 all soil samples all soil samples

- - QC acceptance criteria were not exceeded for this compound

Actions RSD gt 30 Estimate (J and UJ respectively) positive and nondetect results D gt 25 Estimate (J and UJ respectively) positive and nondetect results

The positive di-n-butylphthalate result in equipment blank sample D05954 was qualified as estimated (J) due to the RSD exceedance in the initial calibration

The positive di-n-butylphthalate results in all soil samples were qualified as estimated (J) due to the D exceedance in the continuing calibration

J NE WA160 Troy Mills LandfillData Validation December 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 10 February 24 2005 Case 0251M SDG D05939

The pentachlorophenol and bis(2-ethylhexyl)phthalate results in all samples were reported from the full scan analyses therefore no data validation actions were required as a result of the calibration nonconformances

Blanks

Full Scan

Target compounds were detected as contaminants m the performance evaluation sample (PES) as well as the equipment and laboratory method blanks The highest concentration detected was used to qualify associated sample results The following table summarizes the blank actions as they apply to the samples

Compound Blank

Maximum Concentration

(units)

Blank Action

Level (units)

Quantitation Limit (units)

Affected SamplesActions

benzaldehyde D05954 (EB)

15 ugL NA 100 ugKg Qualify as EB in samples D05950 D05951D05952 D05945 D05946 and D05949

acetophenone D05954 (EB)

0 35 ugL NA 100 ugKg Qualify as EB in sample D05951

4-chloro-3shymethylphenol

D05954 (EB)

5 6 ugL NA 100 ugKg 4-Chloro-3shymethylphenol was not detected in all associated samples No actions were required

di-n-butylphthalate D05954 (EB)

049 ugL NA 100 ugKg Di-n-butylphthalate results were reported from the SIM analyses No actions were required

di-n-butylphthalate method 42 ugKg 420 ugKg 100 ugKg Di-n-butylphthalate results were reported from the SIM analyses No actions were required

bis(2shyethylhexyl)phthalate

method 0 68 ugL 6 8 ugL 1 0 ugL Qualify as nondetect (U) at the QL m equipment blank sample D05954

J NEWA160 Troy Mills LandfillData VahdatwnDecember 20Q4DVMemossD05939_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 11 February 24 2005 Case 0251M SDGD05939

Compound Blank

Maximum Concentration

(units)

Blank Action

Level (units)

Quantitation Limit (units)

bis(2shyethylhexyl)phthalate

PES 490 ugKg 4900 ugKg 100 ugKg

NA - Not applicable SIM - selected ion monitoring EB - equipment blank PES - performance evaluation sample

Sample results were qualified as follows

Affected SamplesActions

Qualify as nondetect (U) at the QL in samples 005950005951 and D05952

bull If sample result was gtQL and ltblank action level (BAL) the result was qualified as a nondetect (U) at the reported concentration

bull If the sample result was sQL and iBAL the results was qualified as a nondetect (U) at the QL bull If the sample result was gtBAL qualification of the data was not required bull If the sample result was nondetect qualification of the data was not required bull Positive results for compounds detected in the equipment blank are flagged with EB

SIM

Target compounds were detected in the laboratory method blanks The following table summarizes the blank actions as they apply to the samples

Compound

di-n-buty Iphthalate

bis(2-ethylhexyl)phthalate

di-n-butylphthalate

Blank Maximum Action Quantitation

Concentration Level Limit Blank (umts^ (units) (units)

method 120ngL 1200 ngL 100 ngL

method 760 ngL 7600 ngL 1600 ngL

method 49 ugKg 490^1^ 10 ugKg

Affected SamplesActions

Qualify as nondetect (U) at the reported value in sample D05954

Bis(2shyethylhexyl)phthalate results were reported from the full scan analyses No actions vere required

Qualify as nondetect (U) at the reported value in all soil samples

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossD05939_nocsirn vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 12 February 24 2005 Case 0251M SDGD05939

Blank Maximum Action Quantitation

Concentration Level Limit Affected Compound Blank (units) (units) (units) Samples Actions

bis(2-ethylhexyl)phthalate method 31 ugKg 3 10 ugKg 160 MgKg Bis(2shyethylhexyl)phthalate results were reported from the full scan analyses No actions were required

Sample results were qualified as follows bull If sample result was gtQL and ltBAL the result was qualified as a nondetect (U) at the reported

concentration bull If the sample result was sQL and ltBAL the results was qualified as a nondetect (U) at the QL bull If the sample result was gtBAL qualification of the data was not required bull If the sample result was nondetect qualification of the data was not required

Internal Standards

Full scan

The following table summarizes the internal standards (IS) that did not meet the acceptable area criteria

Sample ID Internal Standard IS Area Acceptable Range Action

D05948 perylene-d|2 394921 407622-1630486 Results not reported from this analysis

D05948RE chrysene-d2 1720979 350682-1402728 Sample results associated with this IS were either not detected or were reported from the dilution analysis No data validation actions required

D05953 perylene-d2 311034 407622-1630486 Results not reported from this analysis

D05953RE chrysene-dl2 1565496 350682-1402728 Sample results associated with this IS were either not detected or were reported from the dilution analysis No data validation actions required

SIM

Internal standards were within the acceptance criteria in all sample analyses

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DV MemossD05939_svocsim npd Metcalfamp Eddy Inc

Ms Christine Clark Page 13 February 24 2005 Case 0251M SDG D05939

Sensitivity Check

Full Scan

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F05 (low-level)

SW122104F04 (high-level)

Compound

caprolactam

24-dimtrophenol

4-mtrophenol

46-dmitro-2-methylphenol

pentachlorophenol

caprolactam

Recovery Action

0 Raise the quantitation limit to the concentration of the high-level LFB (4 ngL) and qualify as estimated (UJ) the nondetect caprolactam result in sample D05954

0 Since the QL for this compound is 4 |igL the high level LFB (spiked at 4 ugL) was used to evaluate this compound for sensitivity

38 Qualify as estimated (UJ) the nondetect 4shynitrophenol result in sample D05954

38 Qualify as estimated (UJ) the nondetect 46shydimtro-2-methylphenol result in sample D05954

36 Qualify as estimated (UJ) the nondetect pentachlorophenol result in sample D05954

27 Raise the quantitation limit to the concentration of the high-level LFB (4 ugL) and qualify as estimated (UJ) the nondetect caprolactam result in sample D05954

QL - quantitation limit LFB - laboratory fortified blank

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound

SS012805FL01 24-dimethylphenol (low-level)

4-chloroanihne

Action Recovery

26 Qualify as estimated (UJ) the nondetect 24shydimethylphenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shychloroamlme results in all soil samples

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossD05939j5vocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark February 24 2005

LFB

SS012805FL01 (low-level)

SS012805FH01 (high-level)

SIM

Compound

24-dimtrophenol

4-mtrophenol

4 6-dimtro-2-methylphenol

pentachlorophenol

33-dichlorobenzidme

4-chloroanilme

24-dimtrophenol

Page 14 Case 0251M SDG D05939

Action Recovery

0 Raise the quantitation limit to the concentration of the high-level LFB [800 ngKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shynitrophenol results in all soil samples

13 Qualify as estimated (UJ) the nondetect 46shydmitro-2-methylphenol results in all soil samples

32 Qualify as estimated (UJ) the nondetect pentachlorophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 33shydichlorobenzidme results in all soil samples

39 Qualify as estimated (UJ) the nondetect 4shychloroamhne results in all soil samples

21 Raise the quantitation limit to the concentration of the high-level LFB [800 ugKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F03 (low-level)

SW122104F04 (high-level)

Compound

pentachlorophenol

di-n-butylphthalate

bis(2-ethylhexyl)phthalate

di-n-butylphthalate

Recovery

0

327

622

131

Action

Pentachlorophenol was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

J NEWA160 Tro Mills LandfillData VahdationDecember 2004DVMemossD05939_socsim npd Metcalf amp Eddy Inc

Ms Christine Clark Page 15 February 24 2005 Case0251M SDGD05939

LFB Compound Action Recovery

SW122104F04 bis(2-ethylhexyl)phthalate 161 Bis(2-ethylhexyl)phthalate was reported from the (high-level) full scan analysis therefore no actions were

required

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound Action Recovery

SS012805FL02 di-n-butylphthalate 237 Qualify as estimated (J) the positive di-nshy(low-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 376 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 149 Since the QL for this compound is 160 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

indeno( 1 23-cd)pyrene 121 Since the QL for this compound is 1 60 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

SS012805FH02 di-n-butylphthalate 150 Qualify as estimated (J) the positive di-nshy(high-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 185 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 132 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D0595 1 D05952 D05945 D05946 and D05949

QL - quantitation limit

PE Sample ResultsAccuracy Check

PE Sample Results

Full Scan

A single-blind solid PE sample D05939 (PES number SS0491) was analyzed with this data set Eight compounds were scored as Within Limits 2-Chlorophenol acenaphthylene acenaphthene dibenzofuran fluorene anthracene fluoranthene benzo(a)anthracene and chrysene were scored as

J NEWA160 Troy Mills LandfillData VahdatwnDecember 2004DVMemossD05939_svocsim vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 16 February 24 2005 Case 0251M SDGD05939

Action High These compounds were not detected in any of the associated soil samples therefore no data validation actions were required Six compounds (naphthalene hexachlorobenzene phenanthrene pyrene and dibenz(ah)anthracene and benzo(ghi)perylene) were scored as Warning High two compounds (4-hydroxy-4-methyl-2-pentanone and 4-methyl-3-penten-2-one) were scored Non-spiked TIC and one compound (din-n-butylphthalate) was scored Less than CRQL No data validation action is required on the basis of the Warning High Non-spiked TIC and less than CRQL scores Bis(2-ethylhexyl)phthalate was scored as Contaminant This compound was also detected in the associated laboratory method blanks and consequently evaluated in the blank section of this memorandum (please see Blanks above)

Laboratory Control Sample (LCS) Results

Full Scan

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LCS Compound Recovery Action

SW122104L06 caprolactam 35 Qualify as estimated (UJ) the nondetectresult in sample D05954

caprolactam

atrazine 135 Atrazine was not detected in the associaNo actions were required

ted sample

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Recovery Action

SS012805L01 benzaldehyde 46 Qualify as estimated (J) the positive and (UJ) the nondetect benzaldehyde results in all soil samples

4-chloroanihne 35 Qualify as estimated (UJ) the nondetect 4shychloroaruhne results in all soil samples

SIM

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossDQ5939_svocstm vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 17 February 24 2005 Case 0251M SDGD05939

LCS Compound Action Recovery

SW122104L05 pentachlorophenol 194 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 123 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(a)pyrene 122 Benzo(a)pyrene was not detected in the associated sample No actions were required

mdeno( 1 2 3 -cd)pyrene 130 Indeno(l23-cd)pyrene was reported from the full scan analysis therefore no actions were required

dibenz(ah)anthracene 136 Dibenz(ah)anthracene was not detected in the associated sample No actions were required

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Action Recovery

SS012805L02 pentachlorophenol 126 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 142 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(b)fluoranthene 128 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D05951 D05952 D05945 D05946 and D05949

benzo(a)pyrene 121 Qualify as estimated (J) the positive benzo(a)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

mdeno( 1 23-cd)pyrene 129 Qualify as estimated (J) the positive indeno(l23shycd)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

dibenz(ah)anthracene 133 Dibenz(ah)anthracene was not detected in the associated samples No actions were required

J NE WA160 Troy Mills LandfillData Validation December 2004 D V MemossD0593 9_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 18 February 24 2005 Case 0251M SDG D05939

Compound Ouantitation and Reported Ouantitation Limits

Full Scan and SIM

Because of their high moisture content samples D05945 D05946 D05949 D05951 and D05952 were freeze-dried prior to extraction

The following table summarizes the SIM and full scan reporting when data existed for both full scan and SIM analyses Professional judgment was used to select specific analyses in order to report the lowest quantitation limit achievable and to report results with values within the calibration range

Compound Results reported from Full Scan Results reported from SIM

pentachlorophenol all samples none

di-n-butyl phthalate none all samples

benzo(a)anthracene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

bis(2-ethylhexyl)phthalate all samples none

benzo(b)fluoranthene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

benzo(a)pyrene none all samples

indeno(l23-cd)pyrene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

dibenz(ah)anthracene none all samples

Full Scan

The bis(2-ethylhexyl)phthalate results in the following samples were reported from the dilution analysis listed in parentheses since these results exceeded the calibration range in the undiluted analysis D05945 (5x) D05946 (20x) D05947 (20x) D05948 (20x) D05949 (5x) and D05953 (20x)

JNE WA160 Troy Mills LandfillData ValidationDecember 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 19 February 24 2005 Case 0251M SDGD05939

SIM

The following compounds in the samples listed below were qualified as estimated (J) due to uncertainty in the quantitation as a result of the exceeded ion abundance ratio criteria

D05950 di-n-butylphthalate DOS951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate indeno(l23-cd)pyrene D05946 indeno(l23-cd)pyrene DOS 947 di-n-butylphthalate DOS 948 di-n-butylphthalate DOS 949 di-n-butylphthalate D05953 di-n-butylphthalate

Tentatively Identified Compounds (TICs)

One TIC 4-hydroxy-4-methyl-2-pentanone was detected in all samples and is considered an aldol condensation product Consequently this TIC was not included on Table III Tentatively Identified Compound Summary for the affected samples

The following compound in the sample listed was reported twice in the affected sample For this sample this result was renamed to a more general identification since a compound cannot elute at multiple retention times The renamed TIC is described in the table below

Compound name as reported by the Compound name as renamed during data Affected sample laboratory validation

oleic acid unknown D05951

JNEWA160 Troy Mills LandflllData ValidationDecember 2004DV MemossD05939_svocsimwpd MetcalfA Eddy Inc

Ms Christine Clark Page 20 February 24 2005 Case 0251M SDG D05939

Please contact Ms Constance Lapite at (781) 224-6628 or at Constance lapite(am-ecom if you have any questions regarding this Tier II validation

Paula L DiMattei Data Validator

Deborah A Trwini ^mjrjat

Robert Shoemaker Project Chemist

bullgt pound^ampgtlt^ Constance D Lapite MampE RAC Lead Chemist

cc ^James Chow EPA Remedial Project Manager (DV memo and data summary tables) Karen Wedlock-Hunt MampE Project Manager (entire package) Robert Shoemaker Project Chemist (entire package) Troy Mills Landfill Project File WA No 160-RICO-019M (entire package)

Attachments ORDA Table I Recommendation Summary Table Table II Overall Evaluation of Data Table III Tentatively Identified Compound Summary Data Summary Tables Data Validation Worksheets PE Score Report Copy of non-CLP Analytical Method (MampE DAS Specification D-148) Copies of Telephone LogCommunications Forms Supporting Data for Reduced Payment Recommendations (not applicable) Copies of Field Sampling Notes (previously submitted) Copies of EPA-Approved Amendments not QAPjP or SAP (not applicable) CSF Completeness Evidence File Audit (DC-2 Form) DQO Summary Form

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DVMemossD05939_svocsim pd Metcatfamp Eddy Inc

REGION I EPA-NE ORGANIC REGIONAL DATA ASSESSMENT (ORDA)

CASE raquozjggtH _ SITE NAME TV

LAB NAME uoAlaquo Vlaquo- amp+ OF SAMPLESMATRIX

SDG Posirt_ VALIDATION CONTRACTOR

SOW CONTRACT p-rttll-- VALIDATORS NAME

EPA-NE DV TIER LEVEL JC_ DATE DP RECD BY EPA-NE

TPOPO ACTION _ FYI ^ DV COMPLETION DATE

ANALYTICAL DATA QUALITY SUMMARY tffpft^m t~

bullVGA SV-SM PestPCB 1 Preservation and Contractual Holding Times 2 GCMS GCECD Instrument Performance Check raquo 3 Initial Calibration laquo 4 Continuing Calibration o 5 Blanks ~ o 6 Surrogate Compounds raquo 7 Internal Standards o 8 Matrix SpikeMatrix Spike Duplicate ggt 9 Sensitivity Check 0 10 PE Samples-Accuracy Check 0 11 Target Compound Identification jpy 12 Compound Quantitation and Reported QLs o 13 Tentatively Identified Compounds o 14 Semivolatile CleanupPesticidePCB Cleanup ulaquor 15 Data Completeness 0 16 Overall Evaluation of Data laquo

o = Data had no problems or were qualified due to minor contractual problems m = Data were qualified due to major contractual problems z = Data were rejected as unusable due major contractual problems

ACTION ITEMS (z items)

AREAS OF CONCERN (m items)

COMMENTS

This form assesses the analytical data quality in terms of contractual compliance only It does not assess sampling errors andor non-contractual analytical issues that affect data quality

Check ACTION only if contractual defects resulted in reduced paymentdata rejection recommendations

Validator t ltiJSagt3gtlt -3 Date

INSTRUCTIONS ON REVERSE SIDE

1296

Table I Recommendation Summary

Soil Semivolatile Organic Analysis Troy Mills Landfill Superfund Site

Case0251M SDGD05939

Sample ID Matrix

D05945 SO

D05946 SO

D05947 SO (FD)

D05948 SO

D05949 SO

D05950 SO

D05951 SO

D05952 SO

D05953 SO (FD)

D05954 EB

EB shy Equipment Blank FD shy Field Duplicate SOshy Soil

Qualifier

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 11 13 14 15

2 Jl 3 4 7 8 9 10 13 15

A 2 jl 3 4 7 8 9 10 13 15

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 jl 3 4 7 8 9 10 13 15

A 2 3 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 Jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 13 15

^2 4 jl 2 3 5 6 7 12

A - Accept the data but qualify the positive results for benzaldehyde in samples D05945 D05946 D05949 D05950 D05951 and D05952 and for acetophenone in sample D05951 as (EB) due to equipment blank contamination

A2 - Accept the data but qualify the positive result for di-n-butylphthalate as nondetect (U) at the reported value due to laboratory method blank contamination

A5 - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to PE sample contamination

A - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to laboratory method blank contamination

J - Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde hexachlorocyclopentadiene 24shydmitrophenol 46-dmitro-2-methylphenol atrazine and pentachlorophenol due to initial calibration RSD exceedances

J2 Estimate (J) the positive result for di-n-butyl phthalate due to the initial calibration RSD exceedance

J3 Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde and 33-dichlorobenzidme in all samples for hexachlorobutadiene 4-mtrophenol and hexachlorobenzene m samples D05948 D05949 and D05953 for hexachlorocyclopentadiene m samples D05954 D05948 D05949 and D05953 and for 24shydimtrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 due to the continuing calibration D exceedances

J4 - Estimate (J) the positive results for di-n-butylphthalate in all soil samples due to continuing calibration exceedance

J5 - Estimate (UJ) the nondetect caprolactam result and raise the quantitation limit to 4 ugL (equivalent to the concentration of the high-level LFB) due to low low-level and high-level LFB recoveries This result may be biased low

J6 - Estimate (UJ) the nondetect results for 4-mtrophenol 46-dmitro-2-methylphenol and pentachlorophenol due to low low-level LFB recoveries These results may be biased low

J7 - Estimate (J) the positive result for di-n-butylphthalate due to high low-level and high-level LFB recoveries This result may be biased high

J8 - Estimate (UJ) the nondetect 24-dmitrophenol result and raise the quantitation limit to 800 ugKg (equivalent to the concentration of the high-level LFB and corrected for all preparation factors) due to low low-level and high-level LFB recoveries This result may be biased low

J9 - Estimate (UJ) the nondetect results for 24-dimethylphenol 4-mtrophenol 46-dimrro-2-methylphenol pentachlorophenol and 33-dichlorobenzidme due to low low-level LFB recoveries These results may be biased low

J10 - Estimate (UJ) the nondetect result 4-chIoroamlme due to low low-level and high-le el LFB recoveries This result may be biased low

J1 - Estimate (J) the positive result for benzo(b)fluoranthene due to high high-level LFB reco ery This result may be biased high

J12 - Estimate (UJ) the nondetect caprolactam result due to low LCS recovery This result may be biased low

J3 - Estimate (UJ) the nondetect benzaldehyde and 4-chloroamline results due to low LCS recoveries The results may be biased low

J14 - Estimate (J) the positive results for benzo(b)fluoranthene benzo(a)pyrene and mdeno(l23-cd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 due to high LCS recoveries The results may be biased high

J15 - Estimate (J) the positive results for the following compounds in the samples listed below due to uncertainty in the quantitation as a result of the exceeded ion abundance ration criteria

DOS 950 di-n-butylphthalate DOS 951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate mdeno(l23-cd)pyrene D05946 mdeno(l23-cd)pyrene D05947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate D05953 di-n-butylphthalate

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Page 8: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

Ms Christine Clark Page 8 February 24 2005 Case 0251M SDG D05939

Initial and Continuing Calibrations

Full Scan

The following table summarizes the initial calibration (1C) and continuing calibration (CC) results that failed to meet the relative response factor (RRF) criterion of ^005 andor RSD lt 30 in the 1C andor D lt 25 in the CC for all compounds

Calibration Date 1C CC CC CC 12505 12705 13105 2105

Compound RSD D D D

benzaldehyde 792 155 156 153

hexachlorobutadiene - - - 453

hexachlorocyc lopentadiene 488 448 - 360

24-dimtrophenol 337 - 25 8 -

4-nitrophenol - - - 467

hexachlorobenzene - - - 286

46-dimtro-2-methylphenol 450 - - -

atrazme 434 - - -

pentachlorophenol 384 - - -

33-dichlorobenzidme - 726 463 628

2-fluorophenol (surrogate) - - - 285

Associated samples All samples D05954 D05950 D05951 D05948RE D05952 D05945 D05949 D05946 D05947 D05953RE D05948 D05953 D05949DL

D05945DL D05946DL D05947DL D05948DL D05953DL

- - QC acceptance criteria were not exceeded for this compound

Actions RSD gt 30 Estimate (J and UJ respectively) positive and nondetect results D gt 25 Estimate (J and UJ respectively) positive and nondetect results

JNEWA160 Troy Mills LandftllData VahdationDecember 2004DV MemossD05939_socsim pd Metcalf amp Eddy Inc

Ms Christine Clark Page 9 February 24 2005 Case 0251M SDGD05939

The positive and nondetect results for benzaldehyde hexachlorocyclopentadiene 24-dinitrophenol 46-dinitro-2-methylphenol atrazine and pentachlorophenol in all samples were qualified as estimated (UJ) due to initial calibration RSD exceedances

The positive and nondetect results for benzaldehyde and 33-dichlorobenzidine in all samples for hexachlorobutadiene 4-nitrophenol and hexachlorobenzene in samples D05948RE D05949 and D05953RE for hexachlorocyclopentadiene in samples D05954 D05948RE D05949 and D05953RE and for 24-dinitrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 were qualified as estimated (J and UJ respectively) due to continuing calibration D exceedances

No validation actions were necessary for the calibration nonconformances associated with the dilution sample analyses or for the original analyses of samples D05948 and D05953 since the compounds listed in the table above were not reported from these analyses

No validation actions were necessary for the surrogate compound calibration nonconformance

SIM

The following table summarizes the 1C and CC results that failed to meet the RRF criterion of gt005 andor RSD lt 30 in the 1C andor D lt 25 in the CC for all compounds

Calibration Date 1C 12105 1C 2205 CC 2305

Compound RSD RSD D

pentachlorophenol 621 402 -

di-n-butyl phthalate 331 - 297

bis(2-ethylhexyl)phthalate 347 306

Associated samples D05954 all soil samples all soil samples

- - QC acceptance criteria were not exceeded for this compound

Actions RSD gt 30 Estimate (J and UJ respectively) positive and nondetect results D gt 25 Estimate (J and UJ respectively) positive and nondetect results

The positive di-n-butylphthalate result in equipment blank sample D05954 was qualified as estimated (J) due to the RSD exceedance in the initial calibration

The positive di-n-butylphthalate results in all soil samples were qualified as estimated (J) due to the D exceedance in the continuing calibration

J NE WA160 Troy Mills LandfillData Validation December 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 10 February 24 2005 Case 0251M SDG D05939

The pentachlorophenol and bis(2-ethylhexyl)phthalate results in all samples were reported from the full scan analyses therefore no data validation actions were required as a result of the calibration nonconformances

Blanks

Full Scan

Target compounds were detected as contaminants m the performance evaluation sample (PES) as well as the equipment and laboratory method blanks The highest concentration detected was used to qualify associated sample results The following table summarizes the blank actions as they apply to the samples

Compound Blank

Maximum Concentration

(units)

Blank Action

Level (units)

Quantitation Limit (units)

Affected SamplesActions

benzaldehyde D05954 (EB)

15 ugL NA 100 ugKg Qualify as EB in samples D05950 D05951D05952 D05945 D05946 and D05949

acetophenone D05954 (EB)

0 35 ugL NA 100 ugKg Qualify as EB in sample D05951

4-chloro-3shymethylphenol

D05954 (EB)

5 6 ugL NA 100 ugKg 4-Chloro-3shymethylphenol was not detected in all associated samples No actions were required

di-n-butylphthalate D05954 (EB)

049 ugL NA 100 ugKg Di-n-butylphthalate results were reported from the SIM analyses No actions were required

di-n-butylphthalate method 42 ugKg 420 ugKg 100 ugKg Di-n-butylphthalate results were reported from the SIM analyses No actions were required

bis(2shyethylhexyl)phthalate

method 0 68 ugL 6 8 ugL 1 0 ugL Qualify as nondetect (U) at the QL m equipment blank sample D05954

J NEWA160 Troy Mills LandfillData VahdatwnDecember 20Q4DVMemossD05939_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 11 February 24 2005 Case 0251M SDGD05939

Compound Blank

Maximum Concentration

(units)

Blank Action

Level (units)

Quantitation Limit (units)

bis(2shyethylhexyl)phthalate

PES 490 ugKg 4900 ugKg 100 ugKg

NA - Not applicable SIM - selected ion monitoring EB - equipment blank PES - performance evaluation sample

Sample results were qualified as follows

Affected SamplesActions

Qualify as nondetect (U) at the QL in samples 005950005951 and D05952

bull If sample result was gtQL and ltblank action level (BAL) the result was qualified as a nondetect (U) at the reported concentration

bull If the sample result was sQL and iBAL the results was qualified as a nondetect (U) at the QL bull If the sample result was gtBAL qualification of the data was not required bull If the sample result was nondetect qualification of the data was not required bull Positive results for compounds detected in the equipment blank are flagged with EB

SIM

Target compounds were detected in the laboratory method blanks The following table summarizes the blank actions as they apply to the samples

Compound

di-n-buty Iphthalate

bis(2-ethylhexyl)phthalate

di-n-butylphthalate

Blank Maximum Action Quantitation

Concentration Level Limit Blank (umts^ (units) (units)

method 120ngL 1200 ngL 100 ngL

method 760 ngL 7600 ngL 1600 ngL

method 49 ugKg 490^1^ 10 ugKg

Affected SamplesActions

Qualify as nondetect (U) at the reported value in sample D05954

Bis(2shyethylhexyl)phthalate results were reported from the full scan analyses No actions vere required

Qualify as nondetect (U) at the reported value in all soil samples

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossD05939_nocsirn vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 12 February 24 2005 Case 0251M SDGD05939

Blank Maximum Action Quantitation

Concentration Level Limit Affected Compound Blank (units) (units) (units) Samples Actions

bis(2-ethylhexyl)phthalate method 31 ugKg 3 10 ugKg 160 MgKg Bis(2shyethylhexyl)phthalate results were reported from the full scan analyses No actions were required

Sample results were qualified as follows bull If sample result was gtQL and ltBAL the result was qualified as a nondetect (U) at the reported

concentration bull If the sample result was sQL and ltBAL the results was qualified as a nondetect (U) at the QL bull If the sample result was gtBAL qualification of the data was not required bull If the sample result was nondetect qualification of the data was not required

Internal Standards

Full scan

The following table summarizes the internal standards (IS) that did not meet the acceptable area criteria

Sample ID Internal Standard IS Area Acceptable Range Action

D05948 perylene-d|2 394921 407622-1630486 Results not reported from this analysis

D05948RE chrysene-d2 1720979 350682-1402728 Sample results associated with this IS were either not detected or were reported from the dilution analysis No data validation actions required

D05953 perylene-d2 311034 407622-1630486 Results not reported from this analysis

D05953RE chrysene-dl2 1565496 350682-1402728 Sample results associated with this IS were either not detected or were reported from the dilution analysis No data validation actions required

SIM

Internal standards were within the acceptance criteria in all sample analyses

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DV MemossD05939_svocsim npd Metcalfamp Eddy Inc

Ms Christine Clark Page 13 February 24 2005 Case 0251M SDG D05939

Sensitivity Check

Full Scan

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F05 (low-level)

SW122104F04 (high-level)

Compound

caprolactam

24-dimtrophenol

4-mtrophenol

46-dmitro-2-methylphenol

pentachlorophenol

caprolactam

Recovery Action

0 Raise the quantitation limit to the concentration of the high-level LFB (4 ngL) and qualify as estimated (UJ) the nondetect caprolactam result in sample D05954

0 Since the QL for this compound is 4 |igL the high level LFB (spiked at 4 ugL) was used to evaluate this compound for sensitivity

38 Qualify as estimated (UJ) the nondetect 4shynitrophenol result in sample D05954

38 Qualify as estimated (UJ) the nondetect 46shydimtro-2-methylphenol result in sample D05954

36 Qualify as estimated (UJ) the nondetect pentachlorophenol result in sample D05954

27 Raise the quantitation limit to the concentration of the high-level LFB (4 ugL) and qualify as estimated (UJ) the nondetect caprolactam result in sample D05954

QL - quantitation limit LFB - laboratory fortified blank

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound

SS012805FL01 24-dimethylphenol (low-level)

4-chloroanihne

Action Recovery

26 Qualify as estimated (UJ) the nondetect 24shydimethylphenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shychloroamlme results in all soil samples

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossD05939j5vocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark February 24 2005

LFB

SS012805FL01 (low-level)

SS012805FH01 (high-level)

SIM

Compound

24-dimtrophenol

4-mtrophenol

4 6-dimtro-2-methylphenol

pentachlorophenol

33-dichlorobenzidme

4-chloroanilme

24-dimtrophenol

Page 14 Case 0251M SDG D05939

Action Recovery

0 Raise the quantitation limit to the concentration of the high-level LFB [800 ngKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shynitrophenol results in all soil samples

13 Qualify as estimated (UJ) the nondetect 46shydmitro-2-methylphenol results in all soil samples

32 Qualify as estimated (UJ) the nondetect pentachlorophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 33shydichlorobenzidme results in all soil samples

39 Qualify as estimated (UJ) the nondetect 4shychloroamhne results in all soil samples

21 Raise the quantitation limit to the concentration of the high-level LFB [800 ugKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F03 (low-level)

SW122104F04 (high-level)

Compound

pentachlorophenol

di-n-butylphthalate

bis(2-ethylhexyl)phthalate

di-n-butylphthalate

Recovery

0

327

622

131

Action

Pentachlorophenol was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

J NEWA160 Tro Mills LandfillData VahdationDecember 2004DVMemossD05939_socsim npd Metcalf amp Eddy Inc

Ms Christine Clark Page 15 February 24 2005 Case0251M SDGD05939

LFB Compound Action Recovery

SW122104F04 bis(2-ethylhexyl)phthalate 161 Bis(2-ethylhexyl)phthalate was reported from the (high-level) full scan analysis therefore no actions were

required

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound Action Recovery

SS012805FL02 di-n-butylphthalate 237 Qualify as estimated (J) the positive di-nshy(low-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 376 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 149 Since the QL for this compound is 160 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

indeno( 1 23-cd)pyrene 121 Since the QL for this compound is 1 60 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

SS012805FH02 di-n-butylphthalate 150 Qualify as estimated (J) the positive di-nshy(high-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 185 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 132 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D0595 1 D05952 D05945 D05946 and D05949

QL - quantitation limit

PE Sample ResultsAccuracy Check

PE Sample Results

Full Scan

A single-blind solid PE sample D05939 (PES number SS0491) was analyzed with this data set Eight compounds were scored as Within Limits 2-Chlorophenol acenaphthylene acenaphthene dibenzofuran fluorene anthracene fluoranthene benzo(a)anthracene and chrysene were scored as

J NEWA160 Troy Mills LandfillData VahdatwnDecember 2004DVMemossD05939_svocsim vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 16 February 24 2005 Case 0251M SDGD05939

Action High These compounds were not detected in any of the associated soil samples therefore no data validation actions were required Six compounds (naphthalene hexachlorobenzene phenanthrene pyrene and dibenz(ah)anthracene and benzo(ghi)perylene) were scored as Warning High two compounds (4-hydroxy-4-methyl-2-pentanone and 4-methyl-3-penten-2-one) were scored Non-spiked TIC and one compound (din-n-butylphthalate) was scored Less than CRQL No data validation action is required on the basis of the Warning High Non-spiked TIC and less than CRQL scores Bis(2-ethylhexyl)phthalate was scored as Contaminant This compound was also detected in the associated laboratory method blanks and consequently evaluated in the blank section of this memorandum (please see Blanks above)

Laboratory Control Sample (LCS) Results

Full Scan

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LCS Compound Recovery Action

SW122104L06 caprolactam 35 Qualify as estimated (UJ) the nondetectresult in sample D05954

caprolactam

atrazine 135 Atrazine was not detected in the associaNo actions were required

ted sample

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Recovery Action

SS012805L01 benzaldehyde 46 Qualify as estimated (J) the positive and (UJ) the nondetect benzaldehyde results in all soil samples

4-chloroanihne 35 Qualify as estimated (UJ) the nondetect 4shychloroaruhne results in all soil samples

SIM

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossDQ5939_svocstm vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 17 February 24 2005 Case 0251M SDGD05939

LCS Compound Action Recovery

SW122104L05 pentachlorophenol 194 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 123 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(a)pyrene 122 Benzo(a)pyrene was not detected in the associated sample No actions were required

mdeno( 1 2 3 -cd)pyrene 130 Indeno(l23-cd)pyrene was reported from the full scan analysis therefore no actions were required

dibenz(ah)anthracene 136 Dibenz(ah)anthracene was not detected in the associated sample No actions were required

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Action Recovery

SS012805L02 pentachlorophenol 126 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 142 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(b)fluoranthene 128 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D05951 D05952 D05945 D05946 and D05949

benzo(a)pyrene 121 Qualify as estimated (J) the positive benzo(a)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

mdeno( 1 23-cd)pyrene 129 Qualify as estimated (J) the positive indeno(l23shycd)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

dibenz(ah)anthracene 133 Dibenz(ah)anthracene was not detected in the associated samples No actions were required

J NE WA160 Troy Mills LandfillData Validation December 2004 D V MemossD0593 9_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 18 February 24 2005 Case 0251M SDG D05939

Compound Ouantitation and Reported Ouantitation Limits

Full Scan and SIM

Because of their high moisture content samples D05945 D05946 D05949 D05951 and D05952 were freeze-dried prior to extraction

The following table summarizes the SIM and full scan reporting when data existed for both full scan and SIM analyses Professional judgment was used to select specific analyses in order to report the lowest quantitation limit achievable and to report results with values within the calibration range

Compound Results reported from Full Scan Results reported from SIM

pentachlorophenol all samples none

di-n-butyl phthalate none all samples

benzo(a)anthracene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

bis(2-ethylhexyl)phthalate all samples none

benzo(b)fluoranthene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

benzo(a)pyrene none all samples

indeno(l23-cd)pyrene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

dibenz(ah)anthracene none all samples

Full Scan

The bis(2-ethylhexyl)phthalate results in the following samples were reported from the dilution analysis listed in parentheses since these results exceeded the calibration range in the undiluted analysis D05945 (5x) D05946 (20x) D05947 (20x) D05948 (20x) D05949 (5x) and D05953 (20x)

JNE WA160 Troy Mills LandfillData ValidationDecember 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 19 February 24 2005 Case 0251M SDGD05939

SIM

The following compounds in the samples listed below were qualified as estimated (J) due to uncertainty in the quantitation as a result of the exceeded ion abundance ratio criteria

D05950 di-n-butylphthalate DOS951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate indeno(l23-cd)pyrene D05946 indeno(l23-cd)pyrene DOS 947 di-n-butylphthalate DOS 948 di-n-butylphthalate DOS 949 di-n-butylphthalate D05953 di-n-butylphthalate

Tentatively Identified Compounds (TICs)

One TIC 4-hydroxy-4-methyl-2-pentanone was detected in all samples and is considered an aldol condensation product Consequently this TIC was not included on Table III Tentatively Identified Compound Summary for the affected samples

The following compound in the sample listed was reported twice in the affected sample For this sample this result was renamed to a more general identification since a compound cannot elute at multiple retention times The renamed TIC is described in the table below

Compound name as reported by the Compound name as renamed during data Affected sample laboratory validation

oleic acid unknown D05951

JNEWA160 Troy Mills LandflllData ValidationDecember 2004DV MemossD05939_svocsimwpd MetcalfA Eddy Inc

Ms Christine Clark Page 20 February 24 2005 Case 0251M SDG D05939

Please contact Ms Constance Lapite at (781) 224-6628 or at Constance lapite(am-ecom if you have any questions regarding this Tier II validation

Paula L DiMattei Data Validator

Deborah A Trwini ^mjrjat

Robert Shoemaker Project Chemist

bullgt pound^ampgtlt^ Constance D Lapite MampE RAC Lead Chemist

cc ^James Chow EPA Remedial Project Manager (DV memo and data summary tables) Karen Wedlock-Hunt MampE Project Manager (entire package) Robert Shoemaker Project Chemist (entire package) Troy Mills Landfill Project File WA No 160-RICO-019M (entire package)

Attachments ORDA Table I Recommendation Summary Table Table II Overall Evaluation of Data Table III Tentatively Identified Compound Summary Data Summary Tables Data Validation Worksheets PE Score Report Copy of non-CLP Analytical Method (MampE DAS Specification D-148) Copies of Telephone LogCommunications Forms Supporting Data for Reduced Payment Recommendations (not applicable) Copies of Field Sampling Notes (previously submitted) Copies of EPA-Approved Amendments not QAPjP or SAP (not applicable) CSF Completeness Evidence File Audit (DC-2 Form) DQO Summary Form

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DVMemossD05939_svocsim pd Metcatfamp Eddy Inc

REGION I EPA-NE ORGANIC REGIONAL DATA ASSESSMENT (ORDA)

CASE raquozjggtH _ SITE NAME TV

LAB NAME uoAlaquo Vlaquo- amp+ OF SAMPLESMATRIX

SDG Posirt_ VALIDATION CONTRACTOR

SOW CONTRACT p-rttll-- VALIDATORS NAME

EPA-NE DV TIER LEVEL JC_ DATE DP RECD BY EPA-NE

TPOPO ACTION _ FYI ^ DV COMPLETION DATE

ANALYTICAL DATA QUALITY SUMMARY tffpft^m t~

bullVGA SV-SM PestPCB 1 Preservation and Contractual Holding Times 2 GCMS GCECD Instrument Performance Check raquo 3 Initial Calibration laquo 4 Continuing Calibration o 5 Blanks ~ o 6 Surrogate Compounds raquo 7 Internal Standards o 8 Matrix SpikeMatrix Spike Duplicate ggt 9 Sensitivity Check 0 10 PE Samples-Accuracy Check 0 11 Target Compound Identification jpy 12 Compound Quantitation and Reported QLs o 13 Tentatively Identified Compounds o 14 Semivolatile CleanupPesticidePCB Cleanup ulaquor 15 Data Completeness 0 16 Overall Evaluation of Data laquo

o = Data had no problems or were qualified due to minor contractual problems m = Data were qualified due to major contractual problems z = Data were rejected as unusable due major contractual problems

ACTION ITEMS (z items)

AREAS OF CONCERN (m items)

COMMENTS

This form assesses the analytical data quality in terms of contractual compliance only It does not assess sampling errors andor non-contractual analytical issues that affect data quality

Check ACTION only if contractual defects resulted in reduced paymentdata rejection recommendations

Validator t ltiJSagt3gtlt -3 Date

INSTRUCTIONS ON REVERSE SIDE

1296

Table I Recommendation Summary

Soil Semivolatile Organic Analysis Troy Mills Landfill Superfund Site

Case0251M SDGD05939

Sample ID Matrix

D05945 SO

D05946 SO

D05947 SO (FD)

D05948 SO

D05949 SO

D05950 SO

D05951 SO

D05952 SO

D05953 SO (FD)

D05954 EB

EB shy Equipment Blank FD shy Field Duplicate SOshy Soil

Qualifier

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 11 13 14 15

2 Jl 3 4 7 8 9 10 13 15

A 2 jl 3 4 7 8 9 10 13 15

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 jl 3 4 7 8 9 10 13 15

A 2 3 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 Jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 13 15

^2 4 jl 2 3 5 6 7 12

A - Accept the data but qualify the positive results for benzaldehyde in samples D05945 D05946 D05949 D05950 D05951 and D05952 and for acetophenone in sample D05951 as (EB) due to equipment blank contamination

A2 - Accept the data but qualify the positive result for di-n-butylphthalate as nondetect (U) at the reported value due to laboratory method blank contamination

A5 - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to PE sample contamination

A - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to laboratory method blank contamination

J - Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde hexachlorocyclopentadiene 24shydmitrophenol 46-dmitro-2-methylphenol atrazine and pentachlorophenol due to initial calibration RSD exceedances

J2 Estimate (J) the positive result for di-n-butyl phthalate due to the initial calibration RSD exceedance

J3 Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde and 33-dichlorobenzidme in all samples for hexachlorobutadiene 4-mtrophenol and hexachlorobenzene m samples D05948 D05949 and D05953 for hexachlorocyclopentadiene m samples D05954 D05948 D05949 and D05953 and for 24shydimtrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 due to the continuing calibration D exceedances

J4 - Estimate (J) the positive results for di-n-butylphthalate in all soil samples due to continuing calibration exceedance

J5 - Estimate (UJ) the nondetect caprolactam result and raise the quantitation limit to 4 ugL (equivalent to the concentration of the high-level LFB) due to low low-level and high-level LFB recoveries This result may be biased low

J6 - Estimate (UJ) the nondetect results for 4-mtrophenol 46-dmitro-2-methylphenol and pentachlorophenol due to low low-level LFB recoveries These results may be biased low

J7 - Estimate (J) the positive result for di-n-butylphthalate due to high low-level and high-level LFB recoveries This result may be biased high

J8 - Estimate (UJ) the nondetect 24-dmitrophenol result and raise the quantitation limit to 800 ugKg (equivalent to the concentration of the high-level LFB and corrected for all preparation factors) due to low low-level and high-level LFB recoveries This result may be biased low

J9 - Estimate (UJ) the nondetect results for 24-dimethylphenol 4-mtrophenol 46-dimrro-2-methylphenol pentachlorophenol and 33-dichlorobenzidme due to low low-level LFB recoveries These results may be biased low

J10 - Estimate (UJ) the nondetect result 4-chIoroamlme due to low low-level and high-le el LFB recoveries This result may be biased low

J1 - Estimate (J) the positive result for benzo(b)fluoranthene due to high high-level LFB reco ery This result may be biased high

J12 - Estimate (UJ) the nondetect caprolactam result due to low LCS recovery This result may be biased low

J3 - Estimate (UJ) the nondetect benzaldehyde and 4-chloroamline results due to low LCS recoveries The results may be biased low

J14 - Estimate (J) the positive results for benzo(b)fluoranthene benzo(a)pyrene and mdeno(l23-cd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 due to high LCS recoveries The results may be biased high

J15 - Estimate (J) the positive results for the following compounds in the samples listed below due to uncertainty in the quantitation as a result of the exceeded ion abundance ration criteria

DOS 950 di-n-butylphthalate DOS 951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate mdeno(l23-cd)pyrene D05946 mdeno(l23-cd)pyrene D05947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate D05953 di-n-butylphthalate

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Page 9: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

Ms Christine Clark Page 9 February 24 2005 Case 0251M SDGD05939

The positive and nondetect results for benzaldehyde hexachlorocyclopentadiene 24-dinitrophenol 46-dinitro-2-methylphenol atrazine and pentachlorophenol in all samples were qualified as estimated (UJ) due to initial calibration RSD exceedances

The positive and nondetect results for benzaldehyde and 33-dichlorobenzidine in all samples for hexachlorobutadiene 4-nitrophenol and hexachlorobenzene in samples D05948RE D05949 and D05953RE for hexachlorocyclopentadiene in samples D05954 D05948RE D05949 and D05953RE and for 24-dinitrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 were qualified as estimated (J and UJ respectively) due to continuing calibration D exceedances

No validation actions were necessary for the calibration nonconformances associated with the dilution sample analyses or for the original analyses of samples D05948 and D05953 since the compounds listed in the table above were not reported from these analyses

No validation actions were necessary for the surrogate compound calibration nonconformance

SIM

The following table summarizes the 1C and CC results that failed to meet the RRF criterion of gt005 andor RSD lt 30 in the 1C andor D lt 25 in the CC for all compounds

Calibration Date 1C 12105 1C 2205 CC 2305

Compound RSD RSD D

pentachlorophenol 621 402 -

di-n-butyl phthalate 331 - 297

bis(2-ethylhexyl)phthalate 347 306

Associated samples D05954 all soil samples all soil samples

- - QC acceptance criteria were not exceeded for this compound

Actions RSD gt 30 Estimate (J and UJ respectively) positive and nondetect results D gt 25 Estimate (J and UJ respectively) positive and nondetect results

The positive di-n-butylphthalate result in equipment blank sample D05954 was qualified as estimated (J) due to the RSD exceedance in the initial calibration

The positive di-n-butylphthalate results in all soil samples were qualified as estimated (J) due to the D exceedance in the continuing calibration

J NE WA160 Troy Mills LandfillData Validation December 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 10 February 24 2005 Case 0251M SDG D05939

The pentachlorophenol and bis(2-ethylhexyl)phthalate results in all samples were reported from the full scan analyses therefore no data validation actions were required as a result of the calibration nonconformances

Blanks

Full Scan

Target compounds were detected as contaminants m the performance evaluation sample (PES) as well as the equipment and laboratory method blanks The highest concentration detected was used to qualify associated sample results The following table summarizes the blank actions as they apply to the samples

Compound Blank

Maximum Concentration

(units)

Blank Action

Level (units)

Quantitation Limit (units)

Affected SamplesActions

benzaldehyde D05954 (EB)

15 ugL NA 100 ugKg Qualify as EB in samples D05950 D05951D05952 D05945 D05946 and D05949

acetophenone D05954 (EB)

0 35 ugL NA 100 ugKg Qualify as EB in sample D05951

4-chloro-3shymethylphenol

D05954 (EB)

5 6 ugL NA 100 ugKg 4-Chloro-3shymethylphenol was not detected in all associated samples No actions were required

di-n-butylphthalate D05954 (EB)

049 ugL NA 100 ugKg Di-n-butylphthalate results were reported from the SIM analyses No actions were required

di-n-butylphthalate method 42 ugKg 420 ugKg 100 ugKg Di-n-butylphthalate results were reported from the SIM analyses No actions were required

bis(2shyethylhexyl)phthalate

method 0 68 ugL 6 8 ugL 1 0 ugL Qualify as nondetect (U) at the QL m equipment blank sample D05954

J NEWA160 Troy Mills LandfillData VahdatwnDecember 20Q4DVMemossD05939_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 11 February 24 2005 Case 0251M SDGD05939

Compound Blank

Maximum Concentration

(units)

Blank Action

Level (units)

Quantitation Limit (units)

bis(2shyethylhexyl)phthalate

PES 490 ugKg 4900 ugKg 100 ugKg

NA - Not applicable SIM - selected ion monitoring EB - equipment blank PES - performance evaluation sample

Sample results were qualified as follows

Affected SamplesActions

Qualify as nondetect (U) at the QL in samples 005950005951 and D05952

bull If sample result was gtQL and ltblank action level (BAL) the result was qualified as a nondetect (U) at the reported concentration

bull If the sample result was sQL and iBAL the results was qualified as a nondetect (U) at the QL bull If the sample result was gtBAL qualification of the data was not required bull If the sample result was nondetect qualification of the data was not required bull Positive results for compounds detected in the equipment blank are flagged with EB

SIM

Target compounds were detected in the laboratory method blanks The following table summarizes the blank actions as they apply to the samples

Compound

di-n-buty Iphthalate

bis(2-ethylhexyl)phthalate

di-n-butylphthalate

Blank Maximum Action Quantitation

Concentration Level Limit Blank (umts^ (units) (units)

method 120ngL 1200 ngL 100 ngL

method 760 ngL 7600 ngL 1600 ngL

method 49 ugKg 490^1^ 10 ugKg

Affected SamplesActions

Qualify as nondetect (U) at the reported value in sample D05954

Bis(2shyethylhexyl)phthalate results were reported from the full scan analyses No actions vere required

Qualify as nondetect (U) at the reported value in all soil samples

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossD05939_nocsirn vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 12 February 24 2005 Case 0251M SDGD05939

Blank Maximum Action Quantitation

Concentration Level Limit Affected Compound Blank (units) (units) (units) Samples Actions

bis(2-ethylhexyl)phthalate method 31 ugKg 3 10 ugKg 160 MgKg Bis(2shyethylhexyl)phthalate results were reported from the full scan analyses No actions were required

Sample results were qualified as follows bull If sample result was gtQL and ltBAL the result was qualified as a nondetect (U) at the reported

concentration bull If the sample result was sQL and ltBAL the results was qualified as a nondetect (U) at the QL bull If the sample result was gtBAL qualification of the data was not required bull If the sample result was nondetect qualification of the data was not required

Internal Standards

Full scan

The following table summarizes the internal standards (IS) that did not meet the acceptable area criteria

Sample ID Internal Standard IS Area Acceptable Range Action

D05948 perylene-d|2 394921 407622-1630486 Results not reported from this analysis

D05948RE chrysene-d2 1720979 350682-1402728 Sample results associated with this IS were either not detected or were reported from the dilution analysis No data validation actions required

D05953 perylene-d2 311034 407622-1630486 Results not reported from this analysis

D05953RE chrysene-dl2 1565496 350682-1402728 Sample results associated with this IS were either not detected or were reported from the dilution analysis No data validation actions required

SIM

Internal standards were within the acceptance criteria in all sample analyses

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DV MemossD05939_svocsim npd Metcalfamp Eddy Inc

Ms Christine Clark Page 13 February 24 2005 Case 0251M SDG D05939

Sensitivity Check

Full Scan

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F05 (low-level)

SW122104F04 (high-level)

Compound

caprolactam

24-dimtrophenol

4-mtrophenol

46-dmitro-2-methylphenol

pentachlorophenol

caprolactam

Recovery Action

0 Raise the quantitation limit to the concentration of the high-level LFB (4 ngL) and qualify as estimated (UJ) the nondetect caprolactam result in sample D05954

0 Since the QL for this compound is 4 |igL the high level LFB (spiked at 4 ugL) was used to evaluate this compound for sensitivity

38 Qualify as estimated (UJ) the nondetect 4shynitrophenol result in sample D05954

38 Qualify as estimated (UJ) the nondetect 46shydimtro-2-methylphenol result in sample D05954

36 Qualify as estimated (UJ) the nondetect pentachlorophenol result in sample D05954

27 Raise the quantitation limit to the concentration of the high-level LFB (4 ugL) and qualify as estimated (UJ) the nondetect caprolactam result in sample D05954

QL - quantitation limit LFB - laboratory fortified blank

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound

SS012805FL01 24-dimethylphenol (low-level)

4-chloroanihne

Action Recovery

26 Qualify as estimated (UJ) the nondetect 24shydimethylphenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shychloroamlme results in all soil samples

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossD05939j5vocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark February 24 2005

LFB

SS012805FL01 (low-level)

SS012805FH01 (high-level)

SIM

Compound

24-dimtrophenol

4-mtrophenol

4 6-dimtro-2-methylphenol

pentachlorophenol

33-dichlorobenzidme

4-chloroanilme

24-dimtrophenol

Page 14 Case 0251M SDG D05939

Action Recovery

0 Raise the quantitation limit to the concentration of the high-level LFB [800 ngKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shynitrophenol results in all soil samples

13 Qualify as estimated (UJ) the nondetect 46shydmitro-2-methylphenol results in all soil samples

32 Qualify as estimated (UJ) the nondetect pentachlorophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 33shydichlorobenzidme results in all soil samples

39 Qualify as estimated (UJ) the nondetect 4shychloroamhne results in all soil samples

21 Raise the quantitation limit to the concentration of the high-level LFB [800 ugKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F03 (low-level)

SW122104F04 (high-level)

Compound

pentachlorophenol

di-n-butylphthalate

bis(2-ethylhexyl)phthalate

di-n-butylphthalate

Recovery

0

327

622

131

Action

Pentachlorophenol was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

J NEWA160 Tro Mills LandfillData VahdationDecember 2004DVMemossD05939_socsim npd Metcalf amp Eddy Inc

Ms Christine Clark Page 15 February 24 2005 Case0251M SDGD05939

LFB Compound Action Recovery

SW122104F04 bis(2-ethylhexyl)phthalate 161 Bis(2-ethylhexyl)phthalate was reported from the (high-level) full scan analysis therefore no actions were

required

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound Action Recovery

SS012805FL02 di-n-butylphthalate 237 Qualify as estimated (J) the positive di-nshy(low-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 376 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 149 Since the QL for this compound is 160 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

indeno( 1 23-cd)pyrene 121 Since the QL for this compound is 1 60 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

SS012805FH02 di-n-butylphthalate 150 Qualify as estimated (J) the positive di-nshy(high-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 185 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 132 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D0595 1 D05952 D05945 D05946 and D05949

QL - quantitation limit

PE Sample ResultsAccuracy Check

PE Sample Results

Full Scan

A single-blind solid PE sample D05939 (PES number SS0491) was analyzed with this data set Eight compounds were scored as Within Limits 2-Chlorophenol acenaphthylene acenaphthene dibenzofuran fluorene anthracene fluoranthene benzo(a)anthracene and chrysene were scored as

J NEWA160 Troy Mills LandfillData VahdatwnDecember 2004DVMemossD05939_svocsim vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 16 February 24 2005 Case 0251M SDGD05939

Action High These compounds were not detected in any of the associated soil samples therefore no data validation actions were required Six compounds (naphthalene hexachlorobenzene phenanthrene pyrene and dibenz(ah)anthracene and benzo(ghi)perylene) were scored as Warning High two compounds (4-hydroxy-4-methyl-2-pentanone and 4-methyl-3-penten-2-one) were scored Non-spiked TIC and one compound (din-n-butylphthalate) was scored Less than CRQL No data validation action is required on the basis of the Warning High Non-spiked TIC and less than CRQL scores Bis(2-ethylhexyl)phthalate was scored as Contaminant This compound was also detected in the associated laboratory method blanks and consequently evaluated in the blank section of this memorandum (please see Blanks above)

Laboratory Control Sample (LCS) Results

Full Scan

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LCS Compound Recovery Action

SW122104L06 caprolactam 35 Qualify as estimated (UJ) the nondetectresult in sample D05954

caprolactam

atrazine 135 Atrazine was not detected in the associaNo actions were required

ted sample

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Recovery Action

SS012805L01 benzaldehyde 46 Qualify as estimated (J) the positive and (UJ) the nondetect benzaldehyde results in all soil samples

4-chloroanihne 35 Qualify as estimated (UJ) the nondetect 4shychloroaruhne results in all soil samples

SIM

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossDQ5939_svocstm vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 17 February 24 2005 Case 0251M SDGD05939

LCS Compound Action Recovery

SW122104L05 pentachlorophenol 194 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 123 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(a)pyrene 122 Benzo(a)pyrene was not detected in the associated sample No actions were required

mdeno( 1 2 3 -cd)pyrene 130 Indeno(l23-cd)pyrene was reported from the full scan analysis therefore no actions were required

dibenz(ah)anthracene 136 Dibenz(ah)anthracene was not detected in the associated sample No actions were required

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Action Recovery

SS012805L02 pentachlorophenol 126 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 142 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(b)fluoranthene 128 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D05951 D05952 D05945 D05946 and D05949

benzo(a)pyrene 121 Qualify as estimated (J) the positive benzo(a)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

mdeno( 1 23-cd)pyrene 129 Qualify as estimated (J) the positive indeno(l23shycd)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

dibenz(ah)anthracene 133 Dibenz(ah)anthracene was not detected in the associated samples No actions were required

J NE WA160 Troy Mills LandfillData Validation December 2004 D V MemossD0593 9_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 18 February 24 2005 Case 0251M SDG D05939

Compound Ouantitation and Reported Ouantitation Limits

Full Scan and SIM

Because of their high moisture content samples D05945 D05946 D05949 D05951 and D05952 were freeze-dried prior to extraction

The following table summarizes the SIM and full scan reporting when data existed for both full scan and SIM analyses Professional judgment was used to select specific analyses in order to report the lowest quantitation limit achievable and to report results with values within the calibration range

Compound Results reported from Full Scan Results reported from SIM

pentachlorophenol all samples none

di-n-butyl phthalate none all samples

benzo(a)anthracene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

bis(2-ethylhexyl)phthalate all samples none

benzo(b)fluoranthene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

benzo(a)pyrene none all samples

indeno(l23-cd)pyrene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

dibenz(ah)anthracene none all samples

Full Scan

The bis(2-ethylhexyl)phthalate results in the following samples were reported from the dilution analysis listed in parentheses since these results exceeded the calibration range in the undiluted analysis D05945 (5x) D05946 (20x) D05947 (20x) D05948 (20x) D05949 (5x) and D05953 (20x)

JNE WA160 Troy Mills LandfillData ValidationDecember 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 19 February 24 2005 Case 0251M SDGD05939

SIM

The following compounds in the samples listed below were qualified as estimated (J) due to uncertainty in the quantitation as a result of the exceeded ion abundance ratio criteria

D05950 di-n-butylphthalate DOS951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate indeno(l23-cd)pyrene D05946 indeno(l23-cd)pyrene DOS 947 di-n-butylphthalate DOS 948 di-n-butylphthalate DOS 949 di-n-butylphthalate D05953 di-n-butylphthalate

Tentatively Identified Compounds (TICs)

One TIC 4-hydroxy-4-methyl-2-pentanone was detected in all samples and is considered an aldol condensation product Consequently this TIC was not included on Table III Tentatively Identified Compound Summary for the affected samples

The following compound in the sample listed was reported twice in the affected sample For this sample this result was renamed to a more general identification since a compound cannot elute at multiple retention times The renamed TIC is described in the table below

Compound name as reported by the Compound name as renamed during data Affected sample laboratory validation

oleic acid unknown D05951

JNEWA160 Troy Mills LandflllData ValidationDecember 2004DV MemossD05939_svocsimwpd MetcalfA Eddy Inc

Ms Christine Clark Page 20 February 24 2005 Case 0251M SDG D05939

Please contact Ms Constance Lapite at (781) 224-6628 or at Constance lapite(am-ecom if you have any questions regarding this Tier II validation

Paula L DiMattei Data Validator

Deborah A Trwini ^mjrjat

Robert Shoemaker Project Chemist

bullgt pound^ampgtlt^ Constance D Lapite MampE RAC Lead Chemist

cc ^James Chow EPA Remedial Project Manager (DV memo and data summary tables) Karen Wedlock-Hunt MampE Project Manager (entire package) Robert Shoemaker Project Chemist (entire package) Troy Mills Landfill Project File WA No 160-RICO-019M (entire package)

Attachments ORDA Table I Recommendation Summary Table Table II Overall Evaluation of Data Table III Tentatively Identified Compound Summary Data Summary Tables Data Validation Worksheets PE Score Report Copy of non-CLP Analytical Method (MampE DAS Specification D-148) Copies of Telephone LogCommunications Forms Supporting Data for Reduced Payment Recommendations (not applicable) Copies of Field Sampling Notes (previously submitted) Copies of EPA-Approved Amendments not QAPjP or SAP (not applicable) CSF Completeness Evidence File Audit (DC-2 Form) DQO Summary Form

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DVMemossD05939_svocsim pd Metcatfamp Eddy Inc

REGION I EPA-NE ORGANIC REGIONAL DATA ASSESSMENT (ORDA)

CASE raquozjggtH _ SITE NAME TV

LAB NAME uoAlaquo Vlaquo- amp+ OF SAMPLESMATRIX

SDG Posirt_ VALIDATION CONTRACTOR

SOW CONTRACT p-rttll-- VALIDATORS NAME

EPA-NE DV TIER LEVEL JC_ DATE DP RECD BY EPA-NE

TPOPO ACTION _ FYI ^ DV COMPLETION DATE

ANALYTICAL DATA QUALITY SUMMARY tffpft^m t~

bullVGA SV-SM PestPCB 1 Preservation and Contractual Holding Times 2 GCMS GCECD Instrument Performance Check raquo 3 Initial Calibration laquo 4 Continuing Calibration o 5 Blanks ~ o 6 Surrogate Compounds raquo 7 Internal Standards o 8 Matrix SpikeMatrix Spike Duplicate ggt 9 Sensitivity Check 0 10 PE Samples-Accuracy Check 0 11 Target Compound Identification jpy 12 Compound Quantitation and Reported QLs o 13 Tentatively Identified Compounds o 14 Semivolatile CleanupPesticidePCB Cleanup ulaquor 15 Data Completeness 0 16 Overall Evaluation of Data laquo

o = Data had no problems or were qualified due to minor contractual problems m = Data were qualified due to major contractual problems z = Data were rejected as unusable due major contractual problems

ACTION ITEMS (z items)

AREAS OF CONCERN (m items)

COMMENTS

This form assesses the analytical data quality in terms of contractual compliance only It does not assess sampling errors andor non-contractual analytical issues that affect data quality

Check ACTION only if contractual defects resulted in reduced paymentdata rejection recommendations

Validator t ltiJSagt3gtlt -3 Date

INSTRUCTIONS ON REVERSE SIDE

1296

Table I Recommendation Summary

Soil Semivolatile Organic Analysis Troy Mills Landfill Superfund Site

Case0251M SDGD05939

Sample ID Matrix

D05945 SO

D05946 SO

D05947 SO (FD)

D05948 SO

D05949 SO

D05950 SO

D05951 SO

D05952 SO

D05953 SO (FD)

D05954 EB

EB shy Equipment Blank FD shy Field Duplicate SOshy Soil

Qualifier

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 11 13 14 15

2 Jl 3 4 7 8 9 10 13 15

A 2 jl 3 4 7 8 9 10 13 15

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 jl 3 4 7 8 9 10 13 15

A 2 3 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 Jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 13 15

^2 4 jl 2 3 5 6 7 12

A - Accept the data but qualify the positive results for benzaldehyde in samples D05945 D05946 D05949 D05950 D05951 and D05952 and for acetophenone in sample D05951 as (EB) due to equipment blank contamination

A2 - Accept the data but qualify the positive result for di-n-butylphthalate as nondetect (U) at the reported value due to laboratory method blank contamination

A5 - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to PE sample contamination

A - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to laboratory method blank contamination

J - Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde hexachlorocyclopentadiene 24shydmitrophenol 46-dmitro-2-methylphenol atrazine and pentachlorophenol due to initial calibration RSD exceedances

J2 Estimate (J) the positive result for di-n-butyl phthalate due to the initial calibration RSD exceedance

J3 Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde and 33-dichlorobenzidme in all samples for hexachlorobutadiene 4-mtrophenol and hexachlorobenzene m samples D05948 D05949 and D05953 for hexachlorocyclopentadiene m samples D05954 D05948 D05949 and D05953 and for 24shydimtrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 due to the continuing calibration D exceedances

J4 - Estimate (J) the positive results for di-n-butylphthalate in all soil samples due to continuing calibration exceedance

J5 - Estimate (UJ) the nondetect caprolactam result and raise the quantitation limit to 4 ugL (equivalent to the concentration of the high-level LFB) due to low low-level and high-level LFB recoveries This result may be biased low

J6 - Estimate (UJ) the nondetect results for 4-mtrophenol 46-dmitro-2-methylphenol and pentachlorophenol due to low low-level LFB recoveries These results may be biased low

J7 - Estimate (J) the positive result for di-n-butylphthalate due to high low-level and high-level LFB recoveries This result may be biased high

J8 - Estimate (UJ) the nondetect 24-dmitrophenol result and raise the quantitation limit to 800 ugKg (equivalent to the concentration of the high-level LFB and corrected for all preparation factors) due to low low-level and high-level LFB recoveries This result may be biased low

J9 - Estimate (UJ) the nondetect results for 24-dimethylphenol 4-mtrophenol 46-dimrro-2-methylphenol pentachlorophenol and 33-dichlorobenzidme due to low low-level LFB recoveries These results may be biased low

J10 - Estimate (UJ) the nondetect result 4-chIoroamlme due to low low-level and high-le el LFB recoveries This result may be biased low

J1 - Estimate (J) the positive result for benzo(b)fluoranthene due to high high-level LFB reco ery This result may be biased high

J12 - Estimate (UJ) the nondetect caprolactam result due to low LCS recovery This result may be biased low

J3 - Estimate (UJ) the nondetect benzaldehyde and 4-chloroamline results due to low LCS recoveries The results may be biased low

J14 - Estimate (J) the positive results for benzo(b)fluoranthene benzo(a)pyrene and mdeno(l23-cd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 due to high LCS recoveries The results may be biased high

J15 - Estimate (J) the positive results for the following compounds in the samples listed below due to uncertainty in the quantitation as a result of the exceeded ion abundance ration criteria

DOS 950 di-n-butylphthalate DOS 951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate mdeno(l23-cd)pyrene D05946 mdeno(l23-cd)pyrene D05947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate D05953 di-n-butylphthalate

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Page 10: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

Ms Christine Clark Page 10 February 24 2005 Case 0251M SDG D05939

The pentachlorophenol and bis(2-ethylhexyl)phthalate results in all samples were reported from the full scan analyses therefore no data validation actions were required as a result of the calibration nonconformances

Blanks

Full Scan

Target compounds were detected as contaminants m the performance evaluation sample (PES) as well as the equipment and laboratory method blanks The highest concentration detected was used to qualify associated sample results The following table summarizes the blank actions as they apply to the samples

Compound Blank

Maximum Concentration

(units)

Blank Action

Level (units)

Quantitation Limit (units)

Affected SamplesActions

benzaldehyde D05954 (EB)

15 ugL NA 100 ugKg Qualify as EB in samples D05950 D05951D05952 D05945 D05946 and D05949

acetophenone D05954 (EB)

0 35 ugL NA 100 ugKg Qualify as EB in sample D05951

4-chloro-3shymethylphenol

D05954 (EB)

5 6 ugL NA 100 ugKg 4-Chloro-3shymethylphenol was not detected in all associated samples No actions were required

di-n-butylphthalate D05954 (EB)

049 ugL NA 100 ugKg Di-n-butylphthalate results were reported from the SIM analyses No actions were required

di-n-butylphthalate method 42 ugKg 420 ugKg 100 ugKg Di-n-butylphthalate results were reported from the SIM analyses No actions were required

bis(2shyethylhexyl)phthalate

method 0 68 ugL 6 8 ugL 1 0 ugL Qualify as nondetect (U) at the QL m equipment blank sample D05954

J NEWA160 Troy Mills LandfillData VahdatwnDecember 20Q4DVMemossD05939_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 11 February 24 2005 Case 0251M SDGD05939

Compound Blank

Maximum Concentration

(units)

Blank Action

Level (units)

Quantitation Limit (units)

bis(2shyethylhexyl)phthalate

PES 490 ugKg 4900 ugKg 100 ugKg

NA - Not applicable SIM - selected ion monitoring EB - equipment blank PES - performance evaluation sample

Sample results were qualified as follows

Affected SamplesActions

Qualify as nondetect (U) at the QL in samples 005950005951 and D05952

bull If sample result was gtQL and ltblank action level (BAL) the result was qualified as a nondetect (U) at the reported concentration

bull If the sample result was sQL and iBAL the results was qualified as a nondetect (U) at the QL bull If the sample result was gtBAL qualification of the data was not required bull If the sample result was nondetect qualification of the data was not required bull Positive results for compounds detected in the equipment blank are flagged with EB

SIM

Target compounds were detected in the laboratory method blanks The following table summarizes the blank actions as they apply to the samples

Compound

di-n-buty Iphthalate

bis(2-ethylhexyl)phthalate

di-n-butylphthalate

Blank Maximum Action Quantitation

Concentration Level Limit Blank (umts^ (units) (units)

method 120ngL 1200 ngL 100 ngL

method 760 ngL 7600 ngL 1600 ngL

method 49 ugKg 490^1^ 10 ugKg

Affected SamplesActions

Qualify as nondetect (U) at the reported value in sample D05954

Bis(2shyethylhexyl)phthalate results were reported from the full scan analyses No actions vere required

Qualify as nondetect (U) at the reported value in all soil samples

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossD05939_nocsirn vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 12 February 24 2005 Case 0251M SDGD05939

Blank Maximum Action Quantitation

Concentration Level Limit Affected Compound Blank (units) (units) (units) Samples Actions

bis(2-ethylhexyl)phthalate method 31 ugKg 3 10 ugKg 160 MgKg Bis(2shyethylhexyl)phthalate results were reported from the full scan analyses No actions were required

Sample results were qualified as follows bull If sample result was gtQL and ltBAL the result was qualified as a nondetect (U) at the reported

concentration bull If the sample result was sQL and ltBAL the results was qualified as a nondetect (U) at the QL bull If the sample result was gtBAL qualification of the data was not required bull If the sample result was nondetect qualification of the data was not required

Internal Standards

Full scan

The following table summarizes the internal standards (IS) that did not meet the acceptable area criteria

Sample ID Internal Standard IS Area Acceptable Range Action

D05948 perylene-d|2 394921 407622-1630486 Results not reported from this analysis

D05948RE chrysene-d2 1720979 350682-1402728 Sample results associated with this IS were either not detected or were reported from the dilution analysis No data validation actions required

D05953 perylene-d2 311034 407622-1630486 Results not reported from this analysis

D05953RE chrysene-dl2 1565496 350682-1402728 Sample results associated with this IS were either not detected or were reported from the dilution analysis No data validation actions required

SIM

Internal standards were within the acceptance criteria in all sample analyses

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DV MemossD05939_svocsim npd Metcalfamp Eddy Inc

Ms Christine Clark Page 13 February 24 2005 Case 0251M SDG D05939

Sensitivity Check

Full Scan

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F05 (low-level)

SW122104F04 (high-level)

Compound

caprolactam

24-dimtrophenol

4-mtrophenol

46-dmitro-2-methylphenol

pentachlorophenol

caprolactam

Recovery Action

0 Raise the quantitation limit to the concentration of the high-level LFB (4 ngL) and qualify as estimated (UJ) the nondetect caprolactam result in sample D05954

0 Since the QL for this compound is 4 |igL the high level LFB (spiked at 4 ugL) was used to evaluate this compound for sensitivity

38 Qualify as estimated (UJ) the nondetect 4shynitrophenol result in sample D05954

38 Qualify as estimated (UJ) the nondetect 46shydimtro-2-methylphenol result in sample D05954

36 Qualify as estimated (UJ) the nondetect pentachlorophenol result in sample D05954

27 Raise the quantitation limit to the concentration of the high-level LFB (4 ugL) and qualify as estimated (UJ) the nondetect caprolactam result in sample D05954

QL - quantitation limit LFB - laboratory fortified blank

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound

SS012805FL01 24-dimethylphenol (low-level)

4-chloroanihne

Action Recovery

26 Qualify as estimated (UJ) the nondetect 24shydimethylphenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shychloroamlme results in all soil samples

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossD05939j5vocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark February 24 2005

LFB

SS012805FL01 (low-level)

SS012805FH01 (high-level)

SIM

Compound

24-dimtrophenol

4-mtrophenol

4 6-dimtro-2-methylphenol

pentachlorophenol

33-dichlorobenzidme

4-chloroanilme

24-dimtrophenol

Page 14 Case 0251M SDG D05939

Action Recovery

0 Raise the quantitation limit to the concentration of the high-level LFB [800 ngKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shynitrophenol results in all soil samples

13 Qualify as estimated (UJ) the nondetect 46shydmitro-2-methylphenol results in all soil samples

32 Qualify as estimated (UJ) the nondetect pentachlorophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 33shydichlorobenzidme results in all soil samples

39 Qualify as estimated (UJ) the nondetect 4shychloroamhne results in all soil samples

21 Raise the quantitation limit to the concentration of the high-level LFB [800 ugKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F03 (low-level)

SW122104F04 (high-level)

Compound

pentachlorophenol

di-n-butylphthalate

bis(2-ethylhexyl)phthalate

di-n-butylphthalate

Recovery

0

327

622

131

Action

Pentachlorophenol was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

J NEWA160 Tro Mills LandfillData VahdationDecember 2004DVMemossD05939_socsim npd Metcalf amp Eddy Inc

Ms Christine Clark Page 15 February 24 2005 Case0251M SDGD05939

LFB Compound Action Recovery

SW122104F04 bis(2-ethylhexyl)phthalate 161 Bis(2-ethylhexyl)phthalate was reported from the (high-level) full scan analysis therefore no actions were

required

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound Action Recovery

SS012805FL02 di-n-butylphthalate 237 Qualify as estimated (J) the positive di-nshy(low-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 376 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 149 Since the QL for this compound is 160 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

indeno( 1 23-cd)pyrene 121 Since the QL for this compound is 1 60 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

SS012805FH02 di-n-butylphthalate 150 Qualify as estimated (J) the positive di-nshy(high-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 185 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 132 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D0595 1 D05952 D05945 D05946 and D05949

QL - quantitation limit

PE Sample ResultsAccuracy Check

PE Sample Results

Full Scan

A single-blind solid PE sample D05939 (PES number SS0491) was analyzed with this data set Eight compounds were scored as Within Limits 2-Chlorophenol acenaphthylene acenaphthene dibenzofuran fluorene anthracene fluoranthene benzo(a)anthracene and chrysene were scored as

J NEWA160 Troy Mills LandfillData VahdatwnDecember 2004DVMemossD05939_svocsim vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 16 February 24 2005 Case 0251M SDGD05939

Action High These compounds were not detected in any of the associated soil samples therefore no data validation actions were required Six compounds (naphthalene hexachlorobenzene phenanthrene pyrene and dibenz(ah)anthracene and benzo(ghi)perylene) were scored as Warning High two compounds (4-hydroxy-4-methyl-2-pentanone and 4-methyl-3-penten-2-one) were scored Non-spiked TIC and one compound (din-n-butylphthalate) was scored Less than CRQL No data validation action is required on the basis of the Warning High Non-spiked TIC and less than CRQL scores Bis(2-ethylhexyl)phthalate was scored as Contaminant This compound was also detected in the associated laboratory method blanks and consequently evaluated in the blank section of this memorandum (please see Blanks above)

Laboratory Control Sample (LCS) Results

Full Scan

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LCS Compound Recovery Action

SW122104L06 caprolactam 35 Qualify as estimated (UJ) the nondetectresult in sample D05954

caprolactam

atrazine 135 Atrazine was not detected in the associaNo actions were required

ted sample

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Recovery Action

SS012805L01 benzaldehyde 46 Qualify as estimated (J) the positive and (UJ) the nondetect benzaldehyde results in all soil samples

4-chloroanihne 35 Qualify as estimated (UJ) the nondetect 4shychloroaruhne results in all soil samples

SIM

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossDQ5939_svocstm vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 17 February 24 2005 Case 0251M SDGD05939

LCS Compound Action Recovery

SW122104L05 pentachlorophenol 194 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 123 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(a)pyrene 122 Benzo(a)pyrene was not detected in the associated sample No actions were required

mdeno( 1 2 3 -cd)pyrene 130 Indeno(l23-cd)pyrene was reported from the full scan analysis therefore no actions were required

dibenz(ah)anthracene 136 Dibenz(ah)anthracene was not detected in the associated sample No actions were required

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Action Recovery

SS012805L02 pentachlorophenol 126 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 142 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(b)fluoranthene 128 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D05951 D05952 D05945 D05946 and D05949

benzo(a)pyrene 121 Qualify as estimated (J) the positive benzo(a)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

mdeno( 1 23-cd)pyrene 129 Qualify as estimated (J) the positive indeno(l23shycd)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

dibenz(ah)anthracene 133 Dibenz(ah)anthracene was not detected in the associated samples No actions were required

J NE WA160 Troy Mills LandfillData Validation December 2004 D V MemossD0593 9_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 18 February 24 2005 Case 0251M SDG D05939

Compound Ouantitation and Reported Ouantitation Limits

Full Scan and SIM

Because of their high moisture content samples D05945 D05946 D05949 D05951 and D05952 were freeze-dried prior to extraction

The following table summarizes the SIM and full scan reporting when data existed for both full scan and SIM analyses Professional judgment was used to select specific analyses in order to report the lowest quantitation limit achievable and to report results with values within the calibration range

Compound Results reported from Full Scan Results reported from SIM

pentachlorophenol all samples none

di-n-butyl phthalate none all samples

benzo(a)anthracene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

bis(2-ethylhexyl)phthalate all samples none

benzo(b)fluoranthene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

benzo(a)pyrene none all samples

indeno(l23-cd)pyrene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

dibenz(ah)anthracene none all samples

Full Scan

The bis(2-ethylhexyl)phthalate results in the following samples were reported from the dilution analysis listed in parentheses since these results exceeded the calibration range in the undiluted analysis D05945 (5x) D05946 (20x) D05947 (20x) D05948 (20x) D05949 (5x) and D05953 (20x)

JNE WA160 Troy Mills LandfillData ValidationDecember 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 19 February 24 2005 Case 0251M SDGD05939

SIM

The following compounds in the samples listed below were qualified as estimated (J) due to uncertainty in the quantitation as a result of the exceeded ion abundance ratio criteria

D05950 di-n-butylphthalate DOS951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate indeno(l23-cd)pyrene D05946 indeno(l23-cd)pyrene DOS 947 di-n-butylphthalate DOS 948 di-n-butylphthalate DOS 949 di-n-butylphthalate D05953 di-n-butylphthalate

Tentatively Identified Compounds (TICs)

One TIC 4-hydroxy-4-methyl-2-pentanone was detected in all samples and is considered an aldol condensation product Consequently this TIC was not included on Table III Tentatively Identified Compound Summary for the affected samples

The following compound in the sample listed was reported twice in the affected sample For this sample this result was renamed to a more general identification since a compound cannot elute at multiple retention times The renamed TIC is described in the table below

Compound name as reported by the Compound name as renamed during data Affected sample laboratory validation

oleic acid unknown D05951

JNEWA160 Troy Mills LandflllData ValidationDecember 2004DV MemossD05939_svocsimwpd MetcalfA Eddy Inc

Ms Christine Clark Page 20 February 24 2005 Case 0251M SDG D05939

Please contact Ms Constance Lapite at (781) 224-6628 or at Constance lapite(am-ecom if you have any questions regarding this Tier II validation

Paula L DiMattei Data Validator

Deborah A Trwini ^mjrjat

Robert Shoemaker Project Chemist

bullgt pound^ampgtlt^ Constance D Lapite MampE RAC Lead Chemist

cc ^James Chow EPA Remedial Project Manager (DV memo and data summary tables) Karen Wedlock-Hunt MampE Project Manager (entire package) Robert Shoemaker Project Chemist (entire package) Troy Mills Landfill Project File WA No 160-RICO-019M (entire package)

Attachments ORDA Table I Recommendation Summary Table Table II Overall Evaluation of Data Table III Tentatively Identified Compound Summary Data Summary Tables Data Validation Worksheets PE Score Report Copy of non-CLP Analytical Method (MampE DAS Specification D-148) Copies of Telephone LogCommunications Forms Supporting Data for Reduced Payment Recommendations (not applicable) Copies of Field Sampling Notes (previously submitted) Copies of EPA-Approved Amendments not QAPjP or SAP (not applicable) CSF Completeness Evidence File Audit (DC-2 Form) DQO Summary Form

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DVMemossD05939_svocsim pd Metcatfamp Eddy Inc

REGION I EPA-NE ORGANIC REGIONAL DATA ASSESSMENT (ORDA)

CASE raquozjggtH _ SITE NAME TV

LAB NAME uoAlaquo Vlaquo- amp+ OF SAMPLESMATRIX

SDG Posirt_ VALIDATION CONTRACTOR

SOW CONTRACT p-rttll-- VALIDATORS NAME

EPA-NE DV TIER LEVEL JC_ DATE DP RECD BY EPA-NE

TPOPO ACTION _ FYI ^ DV COMPLETION DATE

ANALYTICAL DATA QUALITY SUMMARY tffpft^m t~

bullVGA SV-SM PestPCB 1 Preservation and Contractual Holding Times 2 GCMS GCECD Instrument Performance Check raquo 3 Initial Calibration laquo 4 Continuing Calibration o 5 Blanks ~ o 6 Surrogate Compounds raquo 7 Internal Standards o 8 Matrix SpikeMatrix Spike Duplicate ggt 9 Sensitivity Check 0 10 PE Samples-Accuracy Check 0 11 Target Compound Identification jpy 12 Compound Quantitation and Reported QLs o 13 Tentatively Identified Compounds o 14 Semivolatile CleanupPesticidePCB Cleanup ulaquor 15 Data Completeness 0 16 Overall Evaluation of Data laquo

o = Data had no problems or were qualified due to minor contractual problems m = Data were qualified due to major contractual problems z = Data were rejected as unusable due major contractual problems

ACTION ITEMS (z items)

AREAS OF CONCERN (m items)

COMMENTS

This form assesses the analytical data quality in terms of contractual compliance only It does not assess sampling errors andor non-contractual analytical issues that affect data quality

Check ACTION only if contractual defects resulted in reduced paymentdata rejection recommendations

Validator t ltiJSagt3gtlt -3 Date

INSTRUCTIONS ON REVERSE SIDE

1296

Table I Recommendation Summary

Soil Semivolatile Organic Analysis Troy Mills Landfill Superfund Site

Case0251M SDGD05939

Sample ID Matrix

D05945 SO

D05946 SO

D05947 SO (FD)

D05948 SO

D05949 SO

D05950 SO

D05951 SO

D05952 SO

D05953 SO (FD)

D05954 EB

EB shy Equipment Blank FD shy Field Duplicate SOshy Soil

Qualifier

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 11 13 14 15

2 Jl 3 4 7 8 9 10 13 15

A 2 jl 3 4 7 8 9 10 13 15

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 jl 3 4 7 8 9 10 13 15

A 2 3 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 Jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 13 15

^2 4 jl 2 3 5 6 7 12

A - Accept the data but qualify the positive results for benzaldehyde in samples D05945 D05946 D05949 D05950 D05951 and D05952 and for acetophenone in sample D05951 as (EB) due to equipment blank contamination

A2 - Accept the data but qualify the positive result for di-n-butylphthalate as nondetect (U) at the reported value due to laboratory method blank contamination

A5 - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to PE sample contamination

A - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to laboratory method blank contamination

J - Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde hexachlorocyclopentadiene 24shydmitrophenol 46-dmitro-2-methylphenol atrazine and pentachlorophenol due to initial calibration RSD exceedances

J2 Estimate (J) the positive result for di-n-butyl phthalate due to the initial calibration RSD exceedance

J3 Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde and 33-dichlorobenzidme in all samples for hexachlorobutadiene 4-mtrophenol and hexachlorobenzene m samples D05948 D05949 and D05953 for hexachlorocyclopentadiene m samples D05954 D05948 D05949 and D05953 and for 24shydimtrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 due to the continuing calibration D exceedances

J4 - Estimate (J) the positive results for di-n-butylphthalate in all soil samples due to continuing calibration exceedance

J5 - Estimate (UJ) the nondetect caprolactam result and raise the quantitation limit to 4 ugL (equivalent to the concentration of the high-level LFB) due to low low-level and high-level LFB recoveries This result may be biased low

J6 - Estimate (UJ) the nondetect results for 4-mtrophenol 46-dmitro-2-methylphenol and pentachlorophenol due to low low-level LFB recoveries These results may be biased low

J7 - Estimate (J) the positive result for di-n-butylphthalate due to high low-level and high-level LFB recoveries This result may be biased high

J8 - Estimate (UJ) the nondetect 24-dmitrophenol result and raise the quantitation limit to 800 ugKg (equivalent to the concentration of the high-level LFB and corrected for all preparation factors) due to low low-level and high-level LFB recoveries This result may be biased low

J9 - Estimate (UJ) the nondetect results for 24-dimethylphenol 4-mtrophenol 46-dimrro-2-methylphenol pentachlorophenol and 33-dichlorobenzidme due to low low-level LFB recoveries These results may be biased low

J10 - Estimate (UJ) the nondetect result 4-chIoroamlme due to low low-level and high-le el LFB recoveries This result may be biased low

J1 - Estimate (J) the positive result for benzo(b)fluoranthene due to high high-level LFB reco ery This result may be biased high

J12 - Estimate (UJ) the nondetect caprolactam result due to low LCS recovery This result may be biased low

J3 - Estimate (UJ) the nondetect benzaldehyde and 4-chloroamline results due to low LCS recoveries The results may be biased low

J14 - Estimate (J) the positive results for benzo(b)fluoranthene benzo(a)pyrene and mdeno(l23-cd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 due to high LCS recoveries The results may be biased high

J15 - Estimate (J) the positive results for the following compounds in the samples listed below due to uncertainty in the quantitation as a result of the exceeded ion abundance ration criteria

DOS 950 di-n-butylphthalate DOS 951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate mdeno(l23-cd)pyrene D05946 mdeno(l23-cd)pyrene D05947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate D05953 di-n-butylphthalate

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Page 11: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

Ms Christine Clark Page 11 February 24 2005 Case 0251M SDGD05939

Compound Blank

Maximum Concentration

(units)

Blank Action

Level (units)

Quantitation Limit (units)

bis(2shyethylhexyl)phthalate

PES 490 ugKg 4900 ugKg 100 ugKg

NA - Not applicable SIM - selected ion monitoring EB - equipment blank PES - performance evaluation sample

Sample results were qualified as follows

Affected SamplesActions

Qualify as nondetect (U) at the QL in samples 005950005951 and D05952

bull If sample result was gtQL and ltblank action level (BAL) the result was qualified as a nondetect (U) at the reported concentration

bull If the sample result was sQL and iBAL the results was qualified as a nondetect (U) at the QL bull If the sample result was gtBAL qualification of the data was not required bull If the sample result was nondetect qualification of the data was not required bull Positive results for compounds detected in the equipment blank are flagged with EB

SIM

Target compounds were detected in the laboratory method blanks The following table summarizes the blank actions as they apply to the samples

Compound

di-n-buty Iphthalate

bis(2-ethylhexyl)phthalate

di-n-butylphthalate

Blank Maximum Action Quantitation

Concentration Level Limit Blank (umts^ (units) (units)

method 120ngL 1200 ngL 100 ngL

method 760 ngL 7600 ngL 1600 ngL

method 49 ugKg 490^1^ 10 ugKg

Affected SamplesActions

Qualify as nondetect (U) at the reported value in sample D05954

Bis(2shyethylhexyl)phthalate results were reported from the full scan analyses No actions vere required

Qualify as nondetect (U) at the reported value in all soil samples

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossD05939_nocsirn vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 12 February 24 2005 Case 0251M SDGD05939

Blank Maximum Action Quantitation

Concentration Level Limit Affected Compound Blank (units) (units) (units) Samples Actions

bis(2-ethylhexyl)phthalate method 31 ugKg 3 10 ugKg 160 MgKg Bis(2shyethylhexyl)phthalate results were reported from the full scan analyses No actions were required

Sample results were qualified as follows bull If sample result was gtQL and ltBAL the result was qualified as a nondetect (U) at the reported

concentration bull If the sample result was sQL and ltBAL the results was qualified as a nondetect (U) at the QL bull If the sample result was gtBAL qualification of the data was not required bull If the sample result was nondetect qualification of the data was not required

Internal Standards

Full scan

The following table summarizes the internal standards (IS) that did not meet the acceptable area criteria

Sample ID Internal Standard IS Area Acceptable Range Action

D05948 perylene-d|2 394921 407622-1630486 Results not reported from this analysis

D05948RE chrysene-d2 1720979 350682-1402728 Sample results associated with this IS were either not detected or were reported from the dilution analysis No data validation actions required

D05953 perylene-d2 311034 407622-1630486 Results not reported from this analysis

D05953RE chrysene-dl2 1565496 350682-1402728 Sample results associated with this IS were either not detected or were reported from the dilution analysis No data validation actions required

SIM

Internal standards were within the acceptance criteria in all sample analyses

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DV MemossD05939_svocsim npd Metcalfamp Eddy Inc

Ms Christine Clark Page 13 February 24 2005 Case 0251M SDG D05939

Sensitivity Check

Full Scan

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F05 (low-level)

SW122104F04 (high-level)

Compound

caprolactam

24-dimtrophenol

4-mtrophenol

46-dmitro-2-methylphenol

pentachlorophenol

caprolactam

Recovery Action

0 Raise the quantitation limit to the concentration of the high-level LFB (4 ngL) and qualify as estimated (UJ) the nondetect caprolactam result in sample D05954

0 Since the QL for this compound is 4 |igL the high level LFB (spiked at 4 ugL) was used to evaluate this compound for sensitivity

38 Qualify as estimated (UJ) the nondetect 4shynitrophenol result in sample D05954

38 Qualify as estimated (UJ) the nondetect 46shydimtro-2-methylphenol result in sample D05954

36 Qualify as estimated (UJ) the nondetect pentachlorophenol result in sample D05954

27 Raise the quantitation limit to the concentration of the high-level LFB (4 ugL) and qualify as estimated (UJ) the nondetect caprolactam result in sample D05954

QL - quantitation limit LFB - laboratory fortified blank

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound

SS012805FL01 24-dimethylphenol (low-level)

4-chloroanihne

Action Recovery

26 Qualify as estimated (UJ) the nondetect 24shydimethylphenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shychloroamlme results in all soil samples

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossD05939j5vocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark February 24 2005

LFB

SS012805FL01 (low-level)

SS012805FH01 (high-level)

SIM

Compound

24-dimtrophenol

4-mtrophenol

4 6-dimtro-2-methylphenol

pentachlorophenol

33-dichlorobenzidme

4-chloroanilme

24-dimtrophenol

Page 14 Case 0251M SDG D05939

Action Recovery

0 Raise the quantitation limit to the concentration of the high-level LFB [800 ngKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shynitrophenol results in all soil samples

13 Qualify as estimated (UJ) the nondetect 46shydmitro-2-methylphenol results in all soil samples

32 Qualify as estimated (UJ) the nondetect pentachlorophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 33shydichlorobenzidme results in all soil samples

39 Qualify as estimated (UJ) the nondetect 4shychloroamhne results in all soil samples

21 Raise the quantitation limit to the concentration of the high-level LFB [800 ugKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F03 (low-level)

SW122104F04 (high-level)

Compound

pentachlorophenol

di-n-butylphthalate

bis(2-ethylhexyl)phthalate

di-n-butylphthalate

Recovery

0

327

622

131

Action

Pentachlorophenol was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

J NEWA160 Tro Mills LandfillData VahdationDecember 2004DVMemossD05939_socsim npd Metcalf amp Eddy Inc

Ms Christine Clark Page 15 February 24 2005 Case0251M SDGD05939

LFB Compound Action Recovery

SW122104F04 bis(2-ethylhexyl)phthalate 161 Bis(2-ethylhexyl)phthalate was reported from the (high-level) full scan analysis therefore no actions were

required

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound Action Recovery

SS012805FL02 di-n-butylphthalate 237 Qualify as estimated (J) the positive di-nshy(low-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 376 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 149 Since the QL for this compound is 160 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

indeno( 1 23-cd)pyrene 121 Since the QL for this compound is 1 60 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

SS012805FH02 di-n-butylphthalate 150 Qualify as estimated (J) the positive di-nshy(high-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 185 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 132 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D0595 1 D05952 D05945 D05946 and D05949

QL - quantitation limit

PE Sample ResultsAccuracy Check

PE Sample Results

Full Scan

A single-blind solid PE sample D05939 (PES number SS0491) was analyzed with this data set Eight compounds were scored as Within Limits 2-Chlorophenol acenaphthylene acenaphthene dibenzofuran fluorene anthracene fluoranthene benzo(a)anthracene and chrysene were scored as

J NEWA160 Troy Mills LandfillData VahdatwnDecember 2004DVMemossD05939_svocsim vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 16 February 24 2005 Case 0251M SDGD05939

Action High These compounds were not detected in any of the associated soil samples therefore no data validation actions were required Six compounds (naphthalene hexachlorobenzene phenanthrene pyrene and dibenz(ah)anthracene and benzo(ghi)perylene) were scored as Warning High two compounds (4-hydroxy-4-methyl-2-pentanone and 4-methyl-3-penten-2-one) were scored Non-spiked TIC and one compound (din-n-butylphthalate) was scored Less than CRQL No data validation action is required on the basis of the Warning High Non-spiked TIC and less than CRQL scores Bis(2-ethylhexyl)phthalate was scored as Contaminant This compound was also detected in the associated laboratory method blanks and consequently evaluated in the blank section of this memorandum (please see Blanks above)

Laboratory Control Sample (LCS) Results

Full Scan

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LCS Compound Recovery Action

SW122104L06 caprolactam 35 Qualify as estimated (UJ) the nondetectresult in sample D05954

caprolactam

atrazine 135 Atrazine was not detected in the associaNo actions were required

ted sample

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Recovery Action

SS012805L01 benzaldehyde 46 Qualify as estimated (J) the positive and (UJ) the nondetect benzaldehyde results in all soil samples

4-chloroanihne 35 Qualify as estimated (UJ) the nondetect 4shychloroaruhne results in all soil samples

SIM

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossDQ5939_svocstm vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 17 February 24 2005 Case 0251M SDGD05939

LCS Compound Action Recovery

SW122104L05 pentachlorophenol 194 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 123 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(a)pyrene 122 Benzo(a)pyrene was not detected in the associated sample No actions were required

mdeno( 1 2 3 -cd)pyrene 130 Indeno(l23-cd)pyrene was reported from the full scan analysis therefore no actions were required

dibenz(ah)anthracene 136 Dibenz(ah)anthracene was not detected in the associated sample No actions were required

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Action Recovery

SS012805L02 pentachlorophenol 126 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 142 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(b)fluoranthene 128 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D05951 D05952 D05945 D05946 and D05949

benzo(a)pyrene 121 Qualify as estimated (J) the positive benzo(a)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

mdeno( 1 23-cd)pyrene 129 Qualify as estimated (J) the positive indeno(l23shycd)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

dibenz(ah)anthracene 133 Dibenz(ah)anthracene was not detected in the associated samples No actions were required

J NE WA160 Troy Mills LandfillData Validation December 2004 D V MemossD0593 9_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 18 February 24 2005 Case 0251M SDG D05939

Compound Ouantitation and Reported Ouantitation Limits

Full Scan and SIM

Because of their high moisture content samples D05945 D05946 D05949 D05951 and D05952 were freeze-dried prior to extraction

The following table summarizes the SIM and full scan reporting when data existed for both full scan and SIM analyses Professional judgment was used to select specific analyses in order to report the lowest quantitation limit achievable and to report results with values within the calibration range

Compound Results reported from Full Scan Results reported from SIM

pentachlorophenol all samples none

di-n-butyl phthalate none all samples

benzo(a)anthracene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

bis(2-ethylhexyl)phthalate all samples none

benzo(b)fluoranthene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

benzo(a)pyrene none all samples

indeno(l23-cd)pyrene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

dibenz(ah)anthracene none all samples

Full Scan

The bis(2-ethylhexyl)phthalate results in the following samples were reported from the dilution analysis listed in parentheses since these results exceeded the calibration range in the undiluted analysis D05945 (5x) D05946 (20x) D05947 (20x) D05948 (20x) D05949 (5x) and D05953 (20x)

JNE WA160 Troy Mills LandfillData ValidationDecember 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 19 February 24 2005 Case 0251M SDGD05939

SIM

The following compounds in the samples listed below were qualified as estimated (J) due to uncertainty in the quantitation as a result of the exceeded ion abundance ratio criteria

D05950 di-n-butylphthalate DOS951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate indeno(l23-cd)pyrene D05946 indeno(l23-cd)pyrene DOS 947 di-n-butylphthalate DOS 948 di-n-butylphthalate DOS 949 di-n-butylphthalate D05953 di-n-butylphthalate

Tentatively Identified Compounds (TICs)

One TIC 4-hydroxy-4-methyl-2-pentanone was detected in all samples and is considered an aldol condensation product Consequently this TIC was not included on Table III Tentatively Identified Compound Summary for the affected samples

The following compound in the sample listed was reported twice in the affected sample For this sample this result was renamed to a more general identification since a compound cannot elute at multiple retention times The renamed TIC is described in the table below

Compound name as reported by the Compound name as renamed during data Affected sample laboratory validation

oleic acid unknown D05951

JNEWA160 Troy Mills LandflllData ValidationDecember 2004DV MemossD05939_svocsimwpd MetcalfA Eddy Inc

Ms Christine Clark Page 20 February 24 2005 Case 0251M SDG D05939

Please contact Ms Constance Lapite at (781) 224-6628 or at Constance lapite(am-ecom if you have any questions regarding this Tier II validation

Paula L DiMattei Data Validator

Deborah A Trwini ^mjrjat

Robert Shoemaker Project Chemist

bullgt pound^ampgtlt^ Constance D Lapite MampE RAC Lead Chemist

cc ^James Chow EPA Remedial Project Manager (DV memo and data summary tables) Karen Wedlock-Hunt MampE Project Manager (entire package) Robert Shoemaker Project Chemist (entire package) Troy Mills Landfill Project File WA No 160-RICO-019M (entire package)

Attachments ORDA Table I Recommendation Summary Table Table II Overall Evaluation of Data Table III Tentatively Identified Compound Summary Data Summary Tables Data Validation Worksheets PE Score Report Copy of non-CLP Analytical Method (MampE DAS Specification D-148) Copies of Telephone LogCommunications Forms Supporting Data for Reduced Payment Recommendations (not applicable) Copies of Field Sampling Notes (previously submitted) Copies of EPA-Approved Amendments not QAPjP or SAP (not applicable) CSF Completeness Evidence File Audit (DC-2 Form) DQO Summary Form

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DVMemossD05939_svocsim pd Metcatfamp Eddy Inc

REGION I EPA-NE ORGANIC REGIONAL DATA ASSESSMENT (ORDA)

CASE raquozjggtH _ SITE NAME TV

LAB NAME uoAlaquo Vlaquo- amp+ OF SAMPLESMATRIX

SDG Posirt_ VALIDATION CONTRACTOR

SOW CONTRACT p-rttll-- VALIDATORS NAME

EPA-NE DV TIER LEVEL JC_ DATE DP RECD BY EPA-NE

TPOPO ACTION _ FYI ^ DV COMPLETION DATE

ANALYTICAL DATA QUALITY SUMMARY tffpft^m t~

bullVGA SV-SM PestPCB 1 Preservation and Contractual Holding Times 2 GCMS GCECD Instrument Performance Check raquo 3 Initial Calibration laquo 4 Continuing Calibration o 5 Blanks ~ o 6 Surrogate Compounds raquo 7 Internal Standards o 8 Matrix SpikeMatrix Spike Duplicate ggt 9 Sensitivity Check 0 10 PE Samples-Accuracy Check 0 11 Target Compound Identification jpy 12 Compound Quantitation and Reported QLs o 13 Tentatively Identified Compounds o 14 Semivolatile CleanupPesticidePCB Cleanup ulaquor 15 Data Completeness 0 16 Overall Evaluation of Data laquo

o = Data had no problems or were qualified due to minor contractual problems m = Data were qualified due to major contractual problems z = Data were rejected as unusable due major contractual problems

ACTION ITEMS (z items)

AREAS OF CONCERN (m items)

COMMENTS

This form assesses the analytical data quality in terms of contractual compliance only It does not assess sampling errors andor non-contractual analytical issues that affect data quality

Check ACTION only if contractual defects resulted in reduced paymentdata rejection recommendations

Validator t ltiJSagt3gtlt -3 Date

INSTRUCTIONS ON REVERSE SIDE

1296

Table I Recommendation Summary

Soil Semivolatile Organic Analysis Troy Mills Landfill Superfund Site

Case0251M SDGD05939

Sample ID Matrix

D05945 SO

D05946 SO

D05947 SO (FD)

D05948 SO

D05949 SO

D05950 SO

D05951 SO

D05952 SO

D05953 SO (FD)

D05954 EB

EB shy Equipment Blank FD shy Field Duplicate SOshy Soil

Qualifier

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 11 13 14 15

2 Jl 3 4 7 8 9 10 13 15

A 2 jl 3 4 7 8 9 10 13 15

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 jl 3 4 7 8 9 10 13 15

A 2 3 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 Jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 13 15

^2 4 jl 2 3 5 6 7 12

A - Accept the data but qualify the positive results for benzaldehyde in samples D05945 D05946 D05949 D05950 D05951 and D05952 and for acetophenone in sample D05951 as (EB) due to equipment blank contamination

A2 - Accept the data but qualify the positive result for di-n-butylphthalate as nondetect (U) at the reported value due to laboratory method blank contamination

A5 - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to PE sample contamination

A - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to laboratory method blank contamination

J - Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde hexachlorocyclopentadiene 24shydmitrophenol 46-dmitro-2-methylphenol atrazine and pentachlorophenol due to initial calibration RSD exceedances

J2 Estimate (J) the positive result for di-n-butyl phthalate due to the initial calibration RSD exceedance

J3 Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde and 33-dichlorobenzidme in all samples for hexachlorobutadiene 4-mtrophenol and hexachlorobenzene m samples D05948 D05949 and D05953 for hexachlorocyclopentadiene m samples D05954 D05948 D05949 and D05953 and for 24shydimtrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 due to the continuing calibration D exceedances

J4 - Estimate (J) the positive results for di-n-butylphthalate in all soil samples due to continuing calibration exceedance

J5 - Estimate (UJ) the nondetect caprolactam result and raise the quantitation limit to 4 ugL (equivalent to the concentration of the high-level LFB) due to low low-level and high-level LFB recoveries This result may be biased low

J6 - Estimate (UJ) the nondetect results for 4-mtrophenol 46-dmitro-2-methylphenol and pentachlorophenol due to low low-level LFB recoveries These results may be biased low

J7 - Estimate (J) the positive result for di-n-butylphthalate due to high low-level and high-level LFB recoveries This result may be biased high

J8 - Estimate (UJ) the nondetect 24-dmitrophenol result and raise the quantitation limit to 800 ugKg (equivalent to the concentration of the high-level LFB and corrected for all preparation factors) due to low low-level and high-level LFB recoveries This result may be biased low

J9 - Estimate (UJ) the nondetect results for 24-dimethylphenol 4-mtrophenol 46-dimrro-2-methylphenol pentachlorophenol and 33-dichlorobenzidme due to low low-level LFB recoveries These results may be biased low

J10 - Estimate (UJ) the nondetect result 4-chIoroamlme due to low low-level and high-le el LFB recoveries This result may be biased low

J1 - Estimate (J) the positive result for benzo(b)fluoranthene due to high high-level LFB reco ery This result may be biased high

J12 - Estimate (UJ) the nondetect caprolactam result due to low LCS recovery This result may be biased low

J3 - Estimate (UJ) the nondetect benzaldehyde and 4-chloroamline results due to low LCS recoveries The results may be biased low

J14 - Estimate (J) the positive results for benzo(b)fluoranthene benzo(a)pyrene and mdeno(l23-cd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 due to high LCS recoveries The results may be biased high

J15 - Estimate (J) the positive results for the following compounds in the samples listed below due to uncertainty in the quantitation as a result of the exceeded ion abundance ration criteria

DOS 950 di-n-butylphthalate DOS 951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate mdeno(l23-cd)pyrene D05946 mdeno(l23-cd)pyrene D05947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate D05953 di-n-butylphthalate

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Page 12: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

Ms Christine Clark Page 12 February 24 2005 Case 0251M SDGD05939

Blank Maximum Action Quantitation

Concentration Level Limit Affected Compound Blank (units) (units) (units) Samples Actions

bis(2-ethylhexyl)phthalate method 31 ugKg 3 10 ugKg 160 MgKg Bis(2shyethylhexyl)phthalate results were reported from the full scan analyses No actions were required

Sample results were qualified as follows bull If sample result was gtQL and ltBAL the result was qualified as a nondetect (U) at the reported

concentration bull If the sample result was sQL and ltBAL the results was qualified as a nondetect (U) at the QL bull If the sample result was gtBAL qualification of the data was not required bull If the sample result was nondetect qualification of the data was not required

Internal Standards

Full scan

The following table summarizes the internal standards (IS) that did not meet the acceptable area criteria

Sample ID Internal Standard IS Area Acceptable Range Action

D05948 perylene-d|2 394921 407622-1630486 Results not reported from this analysis

D05948RE chrysene-d2 1720979 350682-1402728 Sample results associated with this IS were either not detected or were reported from the dilution analysis No data validation actions required

D05953 perylene-d2 311034 407622-1630486 Results not reported from this analysis

D05953RE chrysene-dl2 1565496 350682-1402728 Sample results associated with this IS were either not detected or were reported from the dilution analysis No data validation actions required

SIM

Internal standards were within the acceptance criteria in all sample analyses

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DV MemossD05939_svocsim npd Metcalfamp Eddy Inc

Ms Christine Clark Page 13 February 24 2005 Case 0251M SDG D05939

Sensitivity Check

Full Scan

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F05 (low-level)

SW122104F04 (high-level)

Compound

caprolactam

24-dimtrophenol

4-mtrophenol

46-dmitro-2-methylphenol

pentachlorophenol

caprolactam

Recovery Action

0 Raise the quantitation limit to the concentration of the high-level LFB (4 ngL) and qualify as estimated (UJ) the nondetect caprolactam result in sample D05954

0 Since the QL for this compound is 4 |igL the high level LFB (spiked at 4 ugL) was used to evaluate this compound for sensitivity

38 Qualify as estimated (UJ) the nondetect 4shynitrophenol result in sample D05954

38 Qualify as estimated (UJ) the nondetect 46shydimtro-2-methylphenol result in sample D05954

36 Qualify as estimated (UJ) the nondetect pentachlorophenol result in sample D05954

27 Raise the quantitation limit to the concentration of the high-level LFB (4 ugL) and qualify as estimated (UJ) the nondetect caprolactam result in sample D05954

QL - quantitation limit LFB - laboratory fortified blank

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound

SS012805FL01 24-dimethylphenol (low-level)

4-chloroanihne

Action Recovery

26 Qualify as estimated (UJ) the nondetect 24shydimethylphenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shychloroamlme results in all soil samples

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossD05939j5vocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark February 24 2005

LFB

SS012805FL01 (low-level)

SS012805FH01 (high-level)

SIM

Compound

24-dimtrophenol

4-mtrophenol

4 6-dimtro-2-methylphenol

pentachlorophenol

33-dichlorobenzidme

4-chloroanilme

24-dimtrophenol

Page 14 Case 0251M SDG D05939

Action Recovery

0 Raise the quantitation limit to the concentration of the high-level LFB [800 ngKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shynitrophenol results in all soil samples

13 Qualify as estimated (UJ) the nondetect 46shydmitro-2-methylphenol results in all soil samples

32 Qualify as estimated (UJ) the nondetect pentachlorophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 33shydichlorobenzidme results in all soil samples

39 Qualify as estimated (UJ) the nondetect 4shychloroamhne results in all soil samples

21 Raise the quantitation limit to the concentration of the high-level LFB [800 ugKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F03 (low-level)

SW122104F04 (high-level)

Compound

pentachlorophenol

di-n-butylphthalate

bis(2-ethylhexyl)phthalate

di-n-butylphthalate

Recovery

0

327

622

131

Action

Pentachlorophenol was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

J NEWA160 Tro Mills LandfillData VahdationDecember 2004DVMemossD05939_socsim npd Metcalf amp Eddy Inc

Ms Christine Clark Page 15 February 24 2005 Case0251M SDGD05939

LFB Compound Action Recovery

SW122104F04 bis(2-ethylhexyl)phthalate 161 Bis(2-ethylhexyl)phthalate was reported from the (high-level) full scan analysis therefore no actions were

required

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound Action Recovery

SS012805FL02 di-n-butylphthalate 237 Qualify as estimated (J) the positive di-nshy(low-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 376 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 149 Since the QL for this compound is 160 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

indeno( 1 23-cd)pyrene 121 Since the QL for this compound is 1 60 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

SS012805FH02 di-n-butylphthalate 150 Qualify as estimated (J) the positive di-nshy(high-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 185 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 132 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D0595 1 D05952 D05945 D05946 and D05949

QL - quantitation limit

PE Sample ResultsAccuracy Check

PE Sample Results

Full Scan

A single-blind solid PE sample D05939 (PES number SS0491) was analyzed with this data set Eight compounds were scored as Within Limits 2-Chlorophenol acenaphthylene acenaphthene dibenzofuran fluorene anthracene fluoranthene benzo(a)anthracene and chrysene were scored as

J NEWA160 Troy Mills LandfillData VahdatwnDecember 2004DVMemossD05939_svocsim vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 16 February 24 2005 Case 0251M SDGD05939

Action High These compounds were not detected in any of the associated soil samples therefore no data validation actions were required Six compounds (naphthalene hexachlorobenzene phenanthrene pyrene and dibenz(ah)anthracene and benzo(ghi)perylene) were scored as Warning High two compounds (4-hydroxy-4-methyl-2-pentanone and 4-methyl-3-penten-2-one) were scored Non-spiked TIC and one compound (din-n-butylphthalate) was scored Less than CRQL No data validation action is required on the basis of the Warning High Non-spiked TIC and less than CRQL scores Bis(2-ethylhexyl)phthalate was scored as Contaminant This compound was also detected in the associated laboratory method blanks and consequently evaluated in the blank section of this memorandum (please see Blanks above)

Laboratory Control Sample (LCS) Results

Full Scan

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LCS Compound Recovery Action

SW122104L06 caprolactam 35 Qualify as estimated (UJ) the nondetectresult in sample D05954

caprolactam

atrazine 135 Atrazine was not detected in the associaNo actions were required

ted sample

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Recovery Action

SS012805L01 benzaldehyde 46 Qualify as estimated (J) the positive and (UJ) the nondetect benzaldehyde results in all soil samples

4-chloroanihne 35 Qualify as estimated (UJ) the nondetect 4shychloroaruhne results in all soil samples

SIM

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossDQ5939_svocstm vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 17 February 24 2005 Case 0251M SDGD05939

LCS Compound Action Recovery

SW122104L05 pentachlorophenol 194 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 123 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(a)pyrene 122 Benzo(a)pyrene was not detected in the associated sample No actions were required

mdeno( 1 2 3 -cd)pyrene 130 Indeno(l23-cd)pyrene was reported from the full scan analysis therefore no actions were required

dibenz(ah)anthracene 136 Dibenz(ah)anthracene was not detected in the associated sample No actions were required

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Action Recovery

SS012805L02 pentachlorophenol 126 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 142 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(b)fluoranthene 128 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D05951 D05952 D05945 D05946 and D05949

benzo(a)pyrene 121 Qualify as estimated (J) the positive benzo(a)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

mdeno( 1 23-cd)pyrene 129 Qualify as estimated (J) the positive indeno(l23shycd)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

dibenz(ah)anthracene 133 Dibenz(ah)anthracene was not detected in the associated samples No actions were required

J NE WA160 Troy Mills LandfillData Validation December 2004 D V MemossD0593 9_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 18 February 24 2005 Case 0251M SDG D05939

Compound Ouantitation and Reported Ouantitation Limits

Full Scan and SIM

Because of their high moisture content samples D05945 D05946 D05949 D05951 and D05952 were freeze-dried prior to extraction

The following table summarizes the SIM and full scan reporting when data existed for both full scan and SIM analyses Professional judgment was used to select specific analyses in order to report the lowest quantitation limit achievable and to report results with values within the calibration range

Compound Results reported from Full Scan Results reported from SIM

pentachlorophenol all samples none

di-n-butyl phthalate none all samples

benzo(a)anthracene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

bis(2-ethylhexyl)phthalate all samples none

benzo(b)fluoranthene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

benzo(a)pyrene none all samples

indeno(l23-cd)pyrene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

dibenz(ah)anthracene none all samples

Full Scan

The bis(2-ethylhexyl)phthalate results in the following samples were reported from the dilution analysis listed in parentheses since these results exceeded the calibration range in the undiluted analysis D05945 (5x) D05946 (20x) D05947 (20x) D05948 (20x) D05949 (5x) and D05953 (20x)

JNE WA160 Troy Mills LandfillData ValidationDecember 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 19 February 24 2005 Case 0251M SDGD05939

SIM

The following compounds in the samples listed below were qualified as estimated (J) due to uncertainty in the quantitation as a result of the exceeded ion abundance ratio criteria

D05950 di-n-butylphthalate DOS951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate indeno(l23-cd)pyrene D05946 indeno(l23-cd)pyrene DOS 947 di-n-butylphthalate DOS 948 di-n-butylphthalate DOS 949 di-n-butylphthalate D05953 di-n-butylphthalate

Tentatively Identified Compounds (TICs)

One TIC 4-hydroxy-4-methyl-2-pentanone was detected in all samples and is considered an aldol condensation product Consequently this TIC was not included on Table III Tentatively Identified Compound Summary for the affected samples

The following compound in the sample listed was reported twice in the affected sample For this sample this result was renamed to a more general identification since a compound cannot elute at multiple retention times The renamed TIC is described in the table below

Compound name as reported by the Compound name as renamed during data Affected sample laboratory validation

oleic acid unknown D05951

JNEWA160 Troy Mills LandflllData ValidationDecember 2004DV MemossD05939_svocsimwpd MetcalfA Eddy Inc

Ms Christine Clark Page 20 February 24 2005 Case 0251M SDG D05939

Please contact Ms Constance Lapite at (781) 224-6628 or at Constance lapite(am-ecom if you have any questions regarding this Tier II validation

Paula L DiMattei Data Validator

Deborah A Trwini ^mjrjat

Robert Shoemaker Project Chemist

bullgt pound^ampgtlt^ Constance D Lapite MampE RAC Lead Chemist

cc ^James Chow EPA Remedial Project Manager (DV memo and data summary tables) Karen Wedlock-Hunt MampE Project Manager (entire package) Robert Shoemaker Project Chemist (entire package) Troy Mills Landfill Project File WA No 160-RICO-019M (entire package)

Attachments ORDA Table I Recommendation Summary Table Table II Overall Evaluation of Data Table III Tentatively Identified Compound Summary Data Summary Tables Data Validation Worksheets PE Score Report Copy of non-CLP Analytical Method (MampE DAS Specification D-148) Copies of Telephone LogCommunications Forms Supporting Data for Reduced Payment Recommendations (not applicable) Copies of Field Sampling Notes (previously submitted) Copies of EPA-Approved Amendments not QAPjP or SAP (not applicable) CSF Completeness Evidence File Audit (DC-2 Form) DQO Summary Form

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DVMemossD05939_svocsim pd Metcatfamp Eddy Inc

REGION I EPA-NE ORGANIC REGIONAL DATA ASSESSMENT (ORDA)

CASE raquozjggtH _ SITE NAME TV

LAB NAME uoAlaquo Vlaquo- amp+ OF SAMPLESMATRIX

SDG Posirt_ VALIDATION CONTRACTOR

SOW CONTRACT p-rttll-- VALIDATORS NAME

EPA-NE DV TIER LEVEL JC_ DATE DP RECD BY EPA-NE

TPOPO ACTION _ FYI ^ DV COMPLETION DATE

ANALYTICAL DATA QUALITY SUMMARY tffpft^m t~

bullVGA SV-SM PestPCB 1 Preservation and Contractual Holding Times 2 GCMS GCECD Instrument Performance Check raquo 3 Initial Calibration laquo 4 Continuing Calibration o 5 Blanks ~ o 6 Surrogate Compounds raquo 7 Internal Standards o 8 Matrix SpikeMatrix Spike Duplicate ggt 9 Sensitivity Check 0 10 PE Samples-Accuracy Check 0 11 Target Compound Identification jpy 12 Compound Quantitation and Reported QLs o 13 Tentatively Identified Compounds o 14 Semivolatile CleanupPesticidePCB Cleanup ulaquor 15 Data Completeness 0 16 Overall Evaluation of Data laquo

o = Data had no problems or were qualified due to minor contractual problems m = Data were qualified due to major contractual problems z = Data were rejected as unusable due major contractual problems

ACTION ITEMS (z items)

AREAS OF CONCERN (m items)

COMMENTS

This form assesses the analytical data quality in terms of contractual compliance only It does not assess sampling errors andor non-contractual analytical issues that affect data quality

Check ACTION only if contractual defects resulted in reduced paymentdata rejection recommendations

Validator t ltiJSagt3gtlt -3 Date

INSTRUCTIONS ON REVERSE SIDE

1296

Table I Recommendation Summary

Soil Semivolatile Organic Analysis Troy Mills Landfill Superfund Site

Case0251M SDGD05939

Sample ID Matrix

D05945 SO

D05946 SO

D05947 SO (FD)

D05948 SO

D05949 SO

D05950 SO

D05951 SO

D05952 SO

D05953 SO (FD)

D05954 EB

EB shy Equipment Blank FD shy Field Duplicate SOshy Soil

Qualifier

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 11 13 14 15

2 Jl 3 4 7 8 9 10 13 15

A 2 jl 3 4 7 8 9 10 13 15

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 jl 3 4 7 8 9 10 13 15

A 2 3 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 Jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 13 15

^2 4 jl 2 3 5 6 7 12

A - Accept the data but qualify the positive results for benzaldehyde in samples D05945 D05946 D05949 D05950 D05951 and D05952 and for acetophenone in sample D05951 as (EB) due to equipment blank contamination

A2 - Accept the data but qualify the positive result for di-n-butylphthalate as nondetect (U) at the reported value due to laboratory method blank contamination

A5 - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to PE sample contamination

A - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to laboratory method blank contamination

J - Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde hexachlorocyclopentadiene 24shydmitrophenol 46-dmitro-2-methylphenol atrazine and pentachlorophenol due to initial calibration RSD exceedances

J2 Estimate (J) the positive result for di-n-butyl phthalate due to the initial calibration RSD exceedance

J3 Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde and 33-dichlorobenzidme in all samples for hexachlorobutadiene 4-mtrophenol and hexachlorobenzene m samples D05948 D05949 and D05953 for hexachlorocyclopentadiene m samples D05954 D05948 D05949 and D05953 and for 24shydimtrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 due to the continuing calibration D exceedances

J4 - Estimate (J) the positive results for di-n-butylphthalate in all soil samples due to continuing calibration exceedance

J5 - Estimate (UJ) the nondetect caprolactam result and raise the quantitation limit to 4 ugL (equivalent to the concentration of the high-level LFB) due to low low-level and high-level LFB recoveries This result may be biased low

J6 - Estimate (UJ) the nondetect results for 4-mtrophenol 46-dmitro-2-methylphenol and pentachlorophenol due to low low-level LFB recoveries These results may be biased low

J7 - Estimate (J) the positive result for di-n-butylphthalate due to high low-level and high-level LFB recoveries This result may be biased high

J8 - Estimate (UJ) the nondetect 24-dmitrophenol result and raise the quantitation limit to 800 ugKg (equivalent to the concentration of the high-level LFB and corrected for all preparation factors) due to low low-level and high-level LFB recoveries This result may be biased low

J9 - Estimate (UJ) the nondetect results for 24-dimethylphenol 4-mtrophenol 46-dimrro-2-methylphenol pentachlorophenol and 33-dichlorobenzidme due to low low-level LFB recoveries These results may be biased low

J10 - Estimate (UJ) the nondetect result 4-chIoroamlme due to low low-level and high-le el LFB recoveries This result may be biased low

J1 - Estimate (J) the positive result for benzo(b)fluoranthene due to high high-level LFB reco ery This result may be biased high

J12 - Estimate (UJ) the nondetect caprolactam result due to low LCS recovery This result may be biased low

J3 - Estimate (UJ) the nondetect benzaldehyde and 4-chloroamline results due to low LCS recoveries The results may be biased low

J14 - Estimate (J) the positive results for benzo(b)fluoranthene benzo(a)pyrene and mdeno(l23-cd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 due to high LCS recoveries The results may be biased high

J15 - Estimate (J) the positive results for the following compounds in the samples listed below due to uncertainty in the quantitation as a result of the exceeded ion abundance ration criteria

DOS 950 di-n-butylphthalate DOS 951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate mdeno(l23-cd)pyrene D05946 mdeno(l23-cd)pyrene D05947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate D05953 di-n-butylphthalate

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Page 13: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

Ms Christine Clark Page 13 February 24 2005 Case 0251M SDG D05939

Sensitivity Check

Full Scan

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F05 (low-level)

SW122104F04 (high-level)

Compound

caprolactam

24-dimtrophenol

4-mtrophenol

46-dmitro-2-methylphenol

pentachlorophenol

caprolactam

Recovery Action

0 Raise the quantitation limit to the concentration of the high-level LFB (4 ngL) and qualify as estimated (UJ) the nondetect caprolactam result in sample D05954

0 Since the QL for this compound is 4 |igL the high level LFB (spiked at 4 ugL) was used to evaluate this compound for sensitivity

38 Qualify as estimated (UJ) the nondetect 4shynitrophenol result in sample D05954

38 Qualify as estimated (UJ) the nondetect 46shydimtro-2-methylphenol result in sample D05954

36 Qualify as estimated (UJ) the nondetect pentachlorophenol result in sample D05954

27 Raise the quantitation limit to the concentration of the high-level LFB (4 ugL) and qualify as estimated (UJ) the nondetect caprolactam result in sample D05954

QL - quantitation limit LFB - laboratory fortified blank

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound

SS012805FL01 24-dimethylphenol (low-level)

4-chloroanihne

Action Recovery

26 Qualify as estimated (UJ) the nondetect 24shydimethylphenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shychloroamlme results in all soil samples

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossD05939j5vocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark February 24 2005

LFB

SS012805FL01 (low-level)

SS012805FH01 (high-level)

SIM

Compound

24-dimtrophenol

4-mtrophenol

4 6-dimtro-2-methylphenol

pentachlorophenol

33-dichlorobenzidme

4-chloroanilme

24-dimtrophenol

Page 14 Case 0251M SDG D05939

Action Recovery

0 Raise the quantitation limit to the concentration of the high-level LFB [800 ngKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shynitrophenol results in all soil samples

13 Qualify as estimated (UJ) the nondetect 46shydmitro-2-methylphenol results in all soil samples

32 Qualify as estimated (UJ) the nondetect pentachlorophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 33shydichlorobenzidme results in all soil samples

39 Qualify as estimated (UJ) the nondetect 4shychloroamhne results in all soil samples

21 Raise the quantitation limit to the concentration of the high-level LFB [800 ugKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F03 (low-level)

SW122104F04 (high-level)

Compound

pentachlorophenol

di-n-butylphthalate

bis(2-ethylhexyl)phthalate

di-n-butylphthalate

Recovery

0

327

622

131

Action

Pentachlorophenol was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

J NEWA160 Tro Mills LandfillData VahdationDecember 2004DVMemossD05939_socsim npd Metcalf amp Eddy Inc

Ms Christine Clark Page 15 February 24 2005 Case0251M SDGD05939

LFB Compound Action Recovery

SW122104F04 bis(2-ethylhexyl)phthalate 161 Bis(2-ethylhexyl)phthalate was reported from the (high-level) full scan analysis therefore no actions were

required

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound Action Recovery

SS012805FL02 di-n-butylphthalate 237 Qualify as estimated (J) the positive di-nshy(low-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 376 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 149 Since the QL for this compound is 160 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

indeno( 1 23-cd)pyrene 121 Since the QL for this compound is 1 60 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

SS012805FH02 di-n-butylphthalate 150 Qualify as estimated (J) the positive di-nshy(high-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 185 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 132 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D0595 1 D05952 D05945 D05946 and D05949

QL - quantitation limit

PE Sample ResultsAccuracy Check

PE Sample Results

Full Scan

A single-blind solid PE sample D05939 (PES number SS0491) was analyzed with this data set Eight compounds were scored as Within Limits 2-Chlorophenol acenaphthylene acenaphthene dibenzofuran fluorene anthracene fluoranthene benzo(a)anthracene and chrysene were scored as

J NEWA160 Troy Mills LandfillData VahdatwnDecember 2004DVMemossD05939_svocsim vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 16 February 24 2005 Case 0251M SDGD05939

Action High These compounds were not detected in any of the associated soil samples therefore no data validation actions were required Six compounds (naphthalene hexachlorobenzene phenanthrene pyrene and dibenz(ah)anthracene and benzo(ghi)perylene) were scored as Warning High two compounds (4-hydroxy-4-methyl-2-pentanone and 4-methyl-3-penten-2-one) were scored Non-spiked TIC and one compound (din-n-butylphthalate) was scored Less than CRQL No data validation action is required on the basis of the Warning High Non-spiked TIC and less than CRQL scores Bis(2-ethylhexyl)phthalate was scored as Contaminant This compound was also detected in the associated laboratory method blanks and consequently evaluated in the blank section of this memorandum (please see Blanks above)

Laboratory Control Sample (LCS) Results

Full Scan

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LCS Compound Recovery Action

SW122104L06 caprolactam 35 Qualify as estimated (UJ) the nondetectresult in sample D05954

caprolactam

atrazine 135 Atrazine was not detected in the associaNo actions were required

ted sample

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Recovery Action

SS012805L01 benzaldehyde 46 Qualify as estimated (J) the positive and (UJ) the nondetect benzaldehyde results in all soil samples

4-chloroanihne 35 Qualify as estimated (UJ) the nondetect 4shychloroaruhne results in all soil samples

SIM

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossDQ5939_svocstm vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 17 February 24 2005 Case 0251M SDGD05939

LCS Compound Action Recovery

SW122104L05 pentachlorophenol 194 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 123 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(a)pyrene 122 Benzo(a)pyrene was not detected in the associated sample No actions were required

mdeno( 1 2 3 -cd)pyrene 130 Indeno(l23-cd)pyrene was reported from the full scan analysis therefore no actions were required

dibenz(ah)anthracene 136 Dibenz(ah)anthracene was not detected in the associated sample No actions were required

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Action Recovery

SS012805L02 pentachlorophenol 126 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 142 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(b)fluoranthene 128 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D05951 D05952 D05945 D05946 and D05949

benzo(a)pyrene 121 Qualify as estimated (J) the positive benzo(a)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

mdeno( 1 23-cd)pyrene 129 Qualify as estimated (J) the positive indeno(l23shycd)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

dibenz(ah)anthracene 133 Dibenz(ah)anthracene was not detected in the associated samples No actions were required

J NE WA160 Troy Mills LandfillData Validation December 2004 D V MemossD0593 9_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 18 February 24 2005 Case 0251M SDG D05939

Compound Ouantitation and Reported Ouantitation Limits

Full Scan and SIM

Because of their high moisture content samples D05945 D05946 D05949 D05951 and D05952 were freeze-dried prior to extraction

The following table summarizes the SIM and full scan reporting when data existed for both full scan and SIM analyses Professional judgment was used to select specific analyses in order to report the lowest quantitation limit achievable and to report results with values within the calibration range

Compound Results reported from Full Scan Results reported from SIM

pentachlorophenol all samples none

di-n-butyl phthalate none all samples

benzo(a)anthracene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

bis(2-ethylhexyl)phthalate all samples none

benzo(b)fluoranthene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

benzo(a)pyrene none all samples

indeno(l23-cd)pyrene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

dibenz(ah)anthracene none all samples

Full Scan

The bis(2-ethylhexyl)phthalate results in the following samples were reported from the dilution analysis listed in parentheses since these results exceeded the calibration range in the undiluted analysis D05945 (5x) D05946 (20x) D05947 (20x) D05948 (20x) D05949 (5x) and D05953 (20x)

JNE WA160 Troy Mills LandfillData ValidationDecember 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 19 February 24 2005 Case 0251M SDGD05939

SIM

The following compounds in the samples listed below were qualified as estimated (J) due to uncertainty in the quantitation as a result of the exceeded ion abundance ratio criteria

D05950 di-n-butylphthalate DOS951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate indeno(l23-cd)pyrene D05946 indeno(l23-cd)pyrene DOS 947 di-n-butylphthalate DOS 948 di-n-butylphthalate DOS 949 di-n-butylphthalate D05953 di-n-butylphthalate

Tentatively Identified Compounds (TICs)

One TIC 4-hydroxy-4-methyl-2-pentanone was detected in all samples and is considered an aldol condensation product Consequently this TIC was not included on Table III Tentatively Identified Compound Summary for the affected samples

The following compound in the sample listed was reported twice in the affected sample For this sample this result was renamed to a more general identification since a compound cannot elute at multiple retention times The renamed TIC is described in the table below

Compound name as reported by the Compound name as renamed during data Affected sample laboratory validation

oleic acid unknown D05951

JNEWA160 Troy Mills LandflllData ValidationDecember 2004DV MemossD05939_svocsimwpd MetcalfA Eddy Inc

Ms Christine Clark Page 20 February 24 2005 Case 0251M SDG D05939

Please contact Ms Constance Lapite at (781) 224-6628 or at Constance lapite(am-ecom if you have any questions regarding this Tier II validation

Paula L DiMattei Data Validator

Deborah A Trwini ^mjrjat

Robert Shoemaker Project Chemist

bullgt pound^ampgtlt^ Constance D Lapite MampE RAC Lead Chemist

cc ^James Chow EPA Remedial Project Manager (DV memo and data summary tables) Karen Wedlock-Hunt MampE Project Manager (entire package) Robert Shoemaker Project Chemist (entire package) Troy Mills Landfill Project File WA No 160-RICO-019M (entire package)

Attachments ORDA Table I Recommendation Summary Table Table II Overall Evaluation of Data Table III Tentatively Identified Compound Summary Data Summary Tables Data Validation Worksheets PE Score Report Copy of non-CLP Analytical Method (MampE DAS Specification D-148) Copies of Telephone LogCommunications Forms Supporting Data for Reduced Payment Recommendations (not applicable) Copies of Field Sampling Notes (previously submitted) Copies of EPA-Approved Amendments not QAPjP or SAP (not applicable) CSF Completeness Evidence File Audit (DC-2 Form) DQO Summary Form

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DVMemossD05939_svocsim pd Metcatfamp Eddy Inc

REGION I EPA-NE ORGANIC REGIONAL DATA ASSESSMENT (ORDA)

CASE raquozjggtH _ SITE NAME TV

LAB NAME uoAlaquo Vlaquo- amp+ OF SAMPLESMATRIX

SDG Posirt_ VALIDATION CONTRACTOR

SOW CONTRACT p-rttll-- VALIDATORS NAME

EPA-NE DV TIER LEVEL JC_ DATE DP RECD BY EPA-NE

TPOPO ACTION _ FYI ^ DV COMPLETION DATE

ANALYTICAL DATA QUALITY SUMMARY tffpft^m t~

bullVGA SV-SM PestPCB 1 Preservation and Contractual Holding Times 2 GCMS GCECD Instrument Performance Check raquo 3 Initial Calibration laquo 4 Continuing Calibration o 5 Blanks ~ o 6 Surrogate Compounds raquo 7 Internal Standards o 8 Matrix SpikeMatrix Spike Duplicate ggt 9 Sensitivity Check 0 10 PE Samples-Accuracy Check 0 11 Target Compound Identification jpy 12 Compound Quantitation and Reported QLs o 13 Tentatively Identified Compounds o 14 Semivolatile CleanupPesticidePCB Cleanup ulaquor 15 Data Completeness 0 16 Overall Evaluation of Data laquo

o = Data had no problems or were qualified due to minor contractual problems m = Data were qualified due to major contractual problems z = Data were rejected as unusable due major contractual problems

ACTION ITEMS (z items)

AREAS OF CONCERN (m items)

COMMENTS

This form assesses the analytical data quality in terms of contractual compliance only It does not assess sampling errors andor non-contractual analytical issues that affect data quality

Check ACTION only if contractual defects resulted in reduced paymentdata rejection recommendations

Validator t ltiJSagt3gtlt -3 Date

INSTRUCTIONS ON REVERSE SIDE

1296

Table I Recommendation Summary

Soil Semivolatile Organic Analysis Troy Mills Landfill Superfund Site

Case0251M SDGD05939

Sample ID Matrix

D05945 SO

D05946 SO

D05947 SO (FD)

D05948 SO

D05949 SO

D05950 SO

D05951 SO

D05952 SO

D05953 SO (FD)

D05954 EB

EB shy Equipment Blank FD shy Field Duplicate SOshy Soil

Qualifier

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 11 13 14 15

2 Jl 3 4 7 8 9 10 13 15

A 2 jl 3 4 7 8 9 10 13 15

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 jl 3 4 7 8 9 10 13 15

A 2 3 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 Jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 13 15

^2 4 jl 2 3 5 6 7 12

A - Accept the data but qualify the positive results for benzaldehyde in samples D05945 D05946 D05949 D05950 D05951 and D05952 and for acetophenone in sample D05951 as (EB) due to equipment blank contamination

A2 - Accept the data but qualify the positive result for di-n-butylphthalate as nondetect (U) at the reported value due to laboratory method blank contamination

A5 - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to PE sample contamination

A - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to laboratory method blank contamination

J - Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde hexachlorocyclopentadiene 24shydmitrophenol 46-dmitro-2-methylphenol atrazine and pentachlorophenol due to initial calibration RSD exceedances

J2 Estimate (J) the positive result for di-n-butyl phthalate due to the initial calibration RSD exceedance

J3 Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde and 33-dichlorobenzidme in all samples for hexachlorobutadiene 4-mtrophenol and hexachlorobenzene m samples D05948 D05949 and D05953 for hexachlorocyclopentadiene m samples D05954 D05948 D05949 and D05953 and for 24shydimtrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 due to the continuing calibration D exceedances

J4 - Estimate (J) the positive results for di-n-butylphthalate in all soil samples due to continuing calibration exceedance

J5 - Estimate (UJ) the nondetect caprolactam result and raise the quantitation limit to 4 ugL (equivalent to the concentration of the high-level LFB) due to low low-level and high-level LFB recoveries This result may be biased low

J6 - Estimate (UJ) the nondetect results for 4-mtrophenol 46-dmitro-2-methylphenol and pentachlorophenol due to low low-level LFB recoveries These results may be biased low

J7 - Estimate (J) the positive result for di-n-butylphthalate due to high low-level and high-level LFB recoveries This result may be biased high

J8 - Estimate (UJ) the nondetect 24-dmitrophenol result and raise the quantitation limit to 800 ugKg (equivalent to the concentration of the high-level LFB and corrected for all preparation factors) due to low low-level and high-level LFB recoveries This result may be biased low

J9 - Estimate (UJ) the nondetect results for 24-dimethylphenol 4-mtrophenol 46-dimrro-2-methylphenol pentachlorophenol and 33-dichlorobenzidme due to low low-level LFB recoveries These results may be biased low

J10 - Estimate (UJ) the nondetect result 4-chIoroamlme due to low low-level and high-le el LFB recoveries This result may be biased low

J1 - Estimate (J) the positive result for benzo(b)fluoranthene due to high high-level LFB reco ery This result may be biased high

J12 - Estimate (UJ) the nondetect caprolactam result due to low LCS recovery This result may be biased low

J3 - Estimate (UJ) the nondetect benzaldehyde and 4-chloroamline results due to low LCS recoveries The results may be biased low

J14 - Estimate (J) the positive results for benzo(b)fluoranthene benzo(a)pyrene and mdeno(l23-cd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 due to high LCS recoveries The results may be biased high

J15 - Estimate (J) the positive results for the following compounds in the samples listed below due to uncertainty in the quantitation as a result of the exceeded ion abundance ration criteria

DOS 950 di-n-butylphthalate DOS 951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate mdeno(l23-cd)pyrene D05946 mdeno(l23-cd)pyrene D05947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate D05953 di-n-butylphthalate

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Page 14: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

Ms Christine Clark February 24 2005

LFB

SS012805FL01 (low-level)

SS012805FH01 (high-level)

SIM

Compound

24-dimtrophenol

4-mtrophenol

4 6-dimtro-2-methylphenol

pentachlorophenol

33-dichlorobenzidme

4-chloroanilme

24-dimtrophenol

Page 14 Case 0251M SDG D05939

Action Recovery

0 Raise the quantitation limit to the concentration of the high-level LFB [800 ngKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 4shynitrophenol results in all soil samples

13 Qualify as estimated (UJ) the nondetect 46shydmitro-2-methylphenol results in all soil samples

32 Qualify as estimated (UJ) the nondetect pentachlorophenol results in all soil samples

35 Qualify as estimated (UJ) the nondetect 33shydichlorobenzidme results in all soil samples

39 Qualify as estimated (UJ) the nondetect 4shychloroamhne results in all soil samples

21 Raise the quantitation limit to the concentration of the high-level LFB [800 ugKg (corrected for all preparation factors)] and qualify as estimated (UJ) the nondetect 24-dimtrophenol results in all soil samples

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LFB

SW122104F03 (low-level)

SW122104F04 (high-level)

Compound

pentachlorophenol

di-n-butylphthalate

bis(2-ethylhexyl)phthalate

di-n-butylphthalate

Recovery

0

327

622

131

Action

Pentachlorophenol was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

Qualify as estimated (J) the positive di-nshybutylphthalate result in sample D05954

J NEWA160 Tro Mills LandfillData VahdationDecember 2004DVMemossD05939_socsim npd Metcalf amp Eddy Inc

Ms Christine Clark Page 15 February 24 2005 Case0251M SDGD05939

LFB Compound Action Recovery

SW122104F04 bis(2-ethylhexyl)phthalate 161 Bis(2-ethylhexyl)phthalate was reported from the (high-level) full scan analysis therefore no actions were

required

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound Action Recovery

SS012805FL02 di-n-butylphthalate 237 Qualify as estimated (J) the positive di-nshy(low-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 376 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 149 Since the QL for this compound is 160 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

indeno( 1 23-cd)pyrene 121 Since the QL for this compound is 1 60 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

SS012805FH02 di-n-butylphthalate 150 Qualify as estimated (J) the positive di-nshy(high-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 185 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 132 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D0595 1 D05952 D05945 D05946 and D05949

QL - quantitation limit

PE Sample ResultsAccuracy Check

PE Sample Results

Full Scan

A single-blind solid PE sample D05939 (PES number SS0491) was analyzed with this data set Eight compounds were scored as Within Limits 2-Chlorophenol acenaphthylene acenaphthene dibenzofuran fluorene anthracene fluoranthene benzo(a)anthracene and chrysene were scored as

J NEWA160 Troy Mills LandfillData VahdatwnDecember 2004DVMemossD05939_svocsim vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 16 February 24 2005 Case 0251M SDGD05939

Action High These compounds were not detected in any of the associated soil samples therefore no data validation actions were required Six compounds (naphthalene hexachlorobenzene phenanthrene pyrene and dibenz(ah)anthracene and benzo(ghi)perylene) were scored as Warning High two compounds (4-hydroxy-4-methyl-2-pentanone and 4-methyl-3-penten-2-one) were scored Non-spiked TIC and one compound (din-n-butylphthalate) was scored Less than CRQL No data validation action is required on the basis of the Warning High Non-spiked TIC and less than CRQL scores Bis(2-ethylhexyl)phthalate was scored as Contaminant This compound was also detected in the associated laboratory method blanks and consequently evaluated in the blank section of this memorandum (please see Blanks above)

Laboratory Control Sample (LCS) Results

Full Scan

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LCS Compound Recovery Action

SW122104L06 caprolactam 35 Qualify as estimated (UJ) the nondetectresult in sample D05954

caprolactam

atrazine 135 Atrazine was not detected in the associaNo actions were required

ted sample

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Recovery Action

SS012805L01 benzaldehyde 46 Qualify as estimated (J) the positive and (UJ) the nondetect benzaldehyde results in all soil samples

4-chloroanihne 35 Qualify as estimated (UJ) the nondetect 4shychloroaruhne results in all soil samples

SIM

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossDQ5939_svocstm vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 17 February 24 2005 Case 0251M SDGD05939

LCS Compound Action Recovery

SW122104L05 pentachlorophenol 194 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 123 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(a)pyrene 122 Benzo(a)pyrene was not detected in the associated sample No actions were required

mdeno( 1 2 3 -cd)pyrene 130 Indeno(l23-cd)pyrene was reported from the full scan analysis therefore no actions were required

dibenz(ah)anthracene 136 Dibenz(ah)anthracene was not detected in the associated sample No actions were required

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Action Recovery

SS012805L02 pentachlorophenol 126 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 142 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(b)fluoranthene 128 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D05951 D05952 D05945 D05946 and D05949

benzo(a)pyrene 121 Qualify as estimated (J) the positive benzo(a)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

mdeno( 1 23-cd)pyrene 129 Qualify as estimated (J) the positive indeno(l23shycd)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

dibenz(ah)anthracene 133 Dibenz(ah)anthracene was not detected in the associated samples No actions were required

J NE WA160 Troy Mills LandfillData Validation December 2004 D V MemossD0593 9_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 18 February 24 2005 Case 0251M SDG D05939

Compound Ouantitation and Reported Ouantitation Limits

Full Scan and SIM

Because of their high moisture content samples D05945 D05946 D05949 D05951 and D05952 were freeze-dried prior to extraction

The following table summarizes the SIM and full scan reporting when data existed for both full scan and SIM analyses Professional judgment was used to select specific analyses in order to report the lowest quantitation limit achievable and to report results with values within the calibration range

Compound Results reported from Full Scan Results reported from SIM

pentachlorophenol all samples none

di-n-butyl phthalate none all samples

benzo(a)anthracene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

bis(2-ethylhexyl)phthalate all samples none

benzo(b)fluoranthene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

benzo(a)pyrene none all samples

indeno(l23-cd)pyrene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

dibenz(ah)anthracene none all samples

Full Scan

The bis(2-ethylhexyl)phthalate results in the following samples were reported from the dilution analysis listed in parentheses since these results exceeded the calibration range in the undiluted analysis D05945 (5x) D05946 (20x) D05947 (20x) D05948 (20x) D05949 (5x) and D05953 (20x)

JNE WA160 Troy Mills LandfillData ValidationDecember 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 19 February 24 2005 Case 0251M SDGD05939

SIM

The following compounds in the samples listed below were qualified as estimated (J) due to uncertainty in the quantitation as a result of the exceeded ion abundance ratio criteria

D05950 di-n-butylphthalate DOS951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate indeno(l23-cd)pyrene D05946 indeno(l23-cd)pyrene DOS 947 di-n-butylphthalate DOS 948 di-n-butylphthalate DOS 949 di-n-butylphthalate D05953 di-n-butylphthalate

Tentatively Identified Compounds (TICs)

One TIC 4-hydroxy-4-methyl-2-pentanone was detected in all samples and is considered an aldol condensation product Consequently this TIC was not included on Table III Tentatively Identified Compound Summary for the affected samples

The following compound in the sample listed was reported twice in the affected sample For this sample this result was renamed to a more general identification since a compound cannot elute at multiple retention times The renamed TIC is described in the table below

Compound name as reported by the Compound name as renamed during data Affected sample laboratory validation

oleic acid unknown D05951

JNEWA160 Troy Mills LandflllData ValidationDecember 2004DV MemossD05939_svocsimwpd MetcalfA Eddy Inc

Ms Christine Clark Page 20 February 24 2005 Case 0251M SDG D05939

Please contact Ms Constance Lapite at (781) 224-6628 or at Constance lapite(am-ecom if you have any questions regarding this Tier II validation

Paula L DiMattei Data Validator

Deborah A Trwini ^mjrjat

Robert Shoemaker Project Chemist

bullgt pound^ampgtlt^ Constance D Lapite MampE RAC Lead Chemist

cc ^James Chow EPA Remedial Project Manager (DV memo and data summary tables) Karen Wedlock-Hunt MampE Project Manager (entire package) Robert Shoemaker Project Chemist (entire package) Troy Mills Landfill Project File WA No 160-RICO-019M (entire package)

Attachments ORDA Table I Recommendation Summary Table Table II Overall Evaluation of Data Table III Tentatively Identified Compound Summary Data Summary Tables Data Validation Worksheets PE Score Report Copy of non-CLP Analytical Method (MampE DAS Specification D-148) Copies of Telephone LogCommunications Forms Supporting Data for Reduced Payment Recommendations (not applicable) Copies of Field Sampling Notes (previously submitted) Copies of EPA-Approved Amendments not QAPjP or SAP (not applicable) CSF Completeness Evidence File Audit (DC-2 Form) DQO Summary Form

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DVMemossD05939_svocsim pd Metcatfamp Eddy Inc

REGION I EPA-NE ORGANIC REGIONAL DATA ASSESSMENT (ORDA)

CASE raquozjggtH _ SITE NAME TV

LAB NAME uoAlaquo Vlaquo- amp+ OF SAMPLESMATRIX

SDG Posirt_ VALIDATION CONTRACTOR

SOW CONTRACT p-rttll-- VALIDATORS NAME

EPA-NE DV TIER LEVEL JC_ DATE DP RECD BY EPA-NE

TPOPO ACTION _ FYI ^ DV COMPLETION DATE

ANALYTICAL DATA QUALITY SUMMARY tffpft^m t~

bullVGA SV-SM PestPCB 1 Preservation and Contractual Holding Times 2 GCMS GCECD Instrument Performance Check raquo 3 Initial Calibration laquo 4 Continuing Calibration o 5 Blanks ~ o 6 Surrogate Compounds raquo 7 Internal Standards o 8 Matrix SpikeMatrix Spike Duplicate ggt 9 Sensitivity Check 0 10 PE Samples-Accuracy Check 0 11 Target Compound Identification jpy 12 Compound Quantitation and Reported QLs o 13 Tentatively Identified Compounds o 14 Semivolatile CleanupPesticidePCB Cleanup ulaquor 15 Data Completeness 0 16 Overall Evaluation of Data laquo

o = Data had no problems or were qualified due to minor contractual problems m = Data were qualified due to major contractual problems z = Data were rejected as unusable due major contractual problems

ACTION ITEMS (z items)

AREAS OF CONCERN (m items)

COMMENTS

This form assesses the analytical data quality in terms of contractual compliance only It does not assess sampling errors andor non-contractual analytical issues that affect data quality

Check ACTION only if contractual defects resulted in reduced paymentdata rejection recommendations

Validator t ltiJSagt3gtlt -3 Date

INSTRUCTIONS ON REVERSE SIDE

1296

Table I Recommendation Summary

Soil Semivolatile Organic Analysis Troy Mills Landfill Superfund Site

Case0251M SDGD05939

Sample ID Matrix

D05945 SO

D05946 SO

D05947 SO (FD)

D05948 SO

D05949 SO

D05950 SO

D05951 SO

D05952 SO

D05953 SO (FD)

D05954 EB

EB shy Equipment Blank FD shy Field Duplicate SOshy Soil

Qualifier

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 11 13 14 15

2 Jl 3 4 7 8 9 10 13 15

A 2 jl 3 4 7 8 9 10 13 15

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 jl 3 4 7 8 9 10 13 15

A 2 3 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 Jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 13 15

^2 4 jl 2 3 5 6 7 12

A - Accept the data but qualify the positive results for benzaldehyde in samples D05945 D05946 D05949 D05950 D05951 and D05952 and for acetophenone in sample D05951 as (EB) due to equipment blank contamination

A2 - Accept the data but qualify the positive result for di-n-butylphthalate as nondetect (U) at the reported value due to laboratory method blank contamination

A5 - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to PE sample contamination

A - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to laboratory method blank contamination

J - Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde hexachlorocyclopentadiene 24shydmitrophenol 46-dmitro-2-methylphenol atrazine and pentachlorophenol due to initial calibration RSD exceedances

J2 Estimate (J) the positive result for di-n-butyl phthalate due to the initial calibration RSD exceedance

J3 Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde and 33-dichlorobenzidme in all samples for hexachlorobutadiene 4-mtrophenol and hexachlorobenzene m samples D05948 D05949 and D05953 for hexachlorocyclopentadiene m samples D05954 D05948 D05949 and D05953 and for 24shydimtrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 due to the continuing calibration D exceedances

J4 - Estimate (J) the positive results for di-n-butylphthalate in all soil samples due to continuing calibration exceedance

J5 - Estimate (UJ) the nondetect caprolactam result and raise the quantitation limit to 4 ugL (equivalent to the concentration of the high-level LFB) due to low low-level and high-level LFB recoveries This result may be biased low

J6 - Estimate (UJ) the nondetect results for 4-mtrophenol 46-dmitro-2-methylphenol and pentachlorophenol due to low low-level LFB recoveries These results may be biased low

J7 - Estimate (J) the positive result for di-n-butylphthalate due to high low-level and high-level LFB recoveries This result may be biased high

J8 - Estimate (UJ) the nondetect 24-dmitrophenol result and raise the quantitation limit to 800 ugKg (equivalent to the concentration of the high-level LFB and corrected for all preparation factors) due to low low-level and high-level LFB recoveries This result may be biased low

J9 - Estimate (UJ) the nondetect results for 24-dimethylphenol 4-mtrophenol 46-dimrro-2-methylphenol pentachlorophenol and 33-dichlorobenzidme due to low low-level LFB recoveries These results may be biased low

J10 - Estimate (UJ) the nondetect result 4-chIoroamlme due to low low-level and high-le el LFB recoveries This result may be biased low

J1 - Estimate (J) the positive result for benzo(b)fluoranthene due to high high-level LFB reco ery This result may be biased high

J12 - Estimate (UJ) the nondetect caprolactam result due to low LCS recovery This result may be biased low

J3 - Estimate (UJ) the nondetect benzaldehyde and 4-chloroamline results due to low LCS recoveries The results may be biased low

J14 - Estimate (J) the positive results for benzo(b)fluoranthene benzo(a)pyrene and mdeno(l23-cd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 due to high LCS recoveries The results may be biased high

J15 - Estimate (J) the positive results for the following compounds in the samples listed below due to uncertainty in the quantitation as a result of the exceeded ion abundance ration criteria

DOS 950 di-n-butylphthalate DOS 951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate mdeno(l23-cd)pyrene D05946 mdeno(l23-cd)pyrene D05947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate D05953 di-n-butylphthalate

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Page 15: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

Ms Christine Clark Page 15 February 24 2005 Case0251M SDGD05939

LFB Compound Action Recovery

SW122104F04 bis(2-ethylhexyl)phthalate 161 Bis(2-ethylhexyl)phthalate was reported from the (high-level) full scan analysis therefore no actions were

required

The following table summarizes the LFB recoveries outside the 40-120 criteria in association with all soil samples in this data set and the validation actions taken

LFB Compound Action Recovery

SS012805FL02 di-n-butylphthalate 237 Qualify as estimated (J) the positive di-nshy(low-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 376 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 149 Since the QL for this compound is 160 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

indeno( 1 23-cd)pyrene 121 Since the QL for this compound is 1 60 ugKg the high level LFB (spiked at 50 ugKg) was used to evaluate this compound for sensitivity

SS012805FH02 di-n-butylphthalate 150 Qualify as estimated (J) the positive di-nshy(high-level) butylphthalate results in all soil samples

bis(2-ethylhexyl)phthalate 185 All bis(2-ethylhexyl)phthalate results were reported from full scan analysis therefore no actions were required

benzo(b)fluoranthene 132 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D0595 1 D05952 D05945 D05946 and D05949

QL - quantitation limit

PE Sample ResultsAccuracy Check

PE Sample Results

Full Scan

A single-blind solid PE sample D05939 (PES number SS0491) was analyzed with this data set Eight compounds were scored as Within Limits 2-Chlorophenol acenaphthylene acenaphthene dibenzofuran fluorene anthracene fluoranthene benzo(a)anthracene and chrysene were scored as

J NEWA160 Troy Mills LandfillData VahdatwnDecember 2004DVMemossD05939_svocsim vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 16 February 24 2005 Case 0251M SDGD05939

Action High These compounds were not detected in any of the associated soil samples therefore no data validation actions were required Six compounds (naphthalene hexachlorobenzene phenanthrene pyrene and dibenz(ah)anthracene and benzo(ghi)perylene) were scored as Warning High two compounds (4-hydroxy-4-methyl-2-pentanone and 4-methyl-3-penten-2-one) were scored Non-spiked TIC and one compound (din-n-butylphthalate) was scored Less than CRQL No data validation action is required on the basis of the Warning High Non-spiked TIC and less than CRQL scores Bis(2-ethylhexyl)phthalate was scored as Contaminant This compound was also detected in the associated laboratory method blanks and consequently evaluated in the blank section of this memorandum (please see Blanks above)

Laboratory Control Sample (LCS) Results

Full Scan

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LCS Compound Recovery Action

SW122104L06 caprolactam 35 Qualify as estimated (UJ) the nondetectresult in sample D05954

caprolactam

atrazine 135 Atrazine was not detected in the associaNo actions were required

ted sample

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Recovery Action

SS012805L01 benzaldehyde 46 Qualify as estimated (J) the positive and (UJ) the nondetect benzaldehyde results in all soil samples

4-chloroanihne 35 Qualify as estimated (UJ) the nondetect 4shychloroaruhne results in all soil samples

SIM

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossDQ5939_svocstm vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 17 February 24 2005 Case 0251M SDGD05939

LCS Compound Action Recovery

SW122104L05 pentachlorophenol 194 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 123 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(a)pyrene 122 Benzo(a)pyrene was not detected in the associated sample No actions were required

mdeno( 1 2 3 -cd)pyrene 130 Indeno(l23-cd)pyrene was reported from the full scan analysis therefore no actions were required

dibenz(ah)anthracene 136 Dibenz(ah)anthracene was not detected in the associated sample No actions were required

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Action Recovery

SS012805L02 pentachlorophenol 126 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 142 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(b)fluoranthene 128 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D05951 D05952 D05945 D05946 and D05949

benzo(a)pyrene 121 Qualify as estimated (J) the positive benzo(a)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

mdeno( 1 23-cd)pyrene 129 Qualify as estimated (J) the positive indeno(l23shycd)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

dibenz(ah)anthracene 133 Dibenz(ah)anthracene was not detected in the associated samples No actions were required

J NE WA160 Troy Mills LandfillData Validation December 2004 D V MemossD0593 9_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 18 February 24 2005 Case 0251M SDG D05939

Compound Ouantitation and Reported Ouantitation Limits

Full Scan and SIM

Because of their high moisture content samples D05945 D05946 D05949 D05951 and D05952 were freeze-dried prior to extraction

The following table summarizes the SIM and full scan reporting when data existed for both full scan and SIM analyses Professional judgment was used to select specific analyses in order to report the lowest quantitation limit achievable and to report results with values within the calibration range

Compound Results reported from Full Scan Results reported from SIM

pentachlorophenol all samples none

di-n-butyl phthalate none all samples

benzo(a)anthracene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

bis(2-ethylhexyl)phthalate all samples none

benzo(b)fluoranthene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

benzo(a)pyrene none all samples

indeno(l23-cd)pyrene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

dibenz(ah)anthracene none all samples

Full Scan

The bis(2-ethylhexyl)phthalate results in the following samples were reported from the dilution analysis listed in parentheses since these results exceeded the calibration range in the undiluted analysis D05945 (5x) D05946 (20x) D05947 (20x) D05948 (20x) D05949 (5x) and D05953 (20x)

JNE WA160 Troy Mills LandfillData ValidationDecember 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 19 February 24 2005 Case 0251M SDGD05939

SIM

The following compounds in the samples listed below were qualified as estimated (J) due to uncertainty in the quantitation as a result of the exceeded ion abundance ratio criteria

D05950 di-n-butylphthalate DOS951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate indeno(l23-cd)pyrene D05946 indeno(l23-cd)pyrene DOS 947 di-n-butylphthalate DOS 948 di-n-butylphthalate DOS 949 di-n-butylphthalate D05953 di-n-butylphthalate

Tentatively Identified Compounds (TICs)

One TIC 4-hydroxy-4-methyl-2-pentanone was detected in all samples and is considered an aldol condensation product Consequently this TIC was not included on Table III Tentatively Identified Compound Summary for the affected samples

The following compound in the sample listed was reported twice in the affected sample For this sample this result was renamed to a more general identification since a compound cannot elute at multiple retention times The renamed TIC is described in the table below

Compound name as reported by the Compound name as renamed during data Affected sample laboratory validation

oleic acid unknown D05951

JNEWA160 Troy Mills LandflllData ValidationDecember 2004DV MemossD05939_svocsimwpd MetcalfA Eddy Inc

Ms Christine Clark Page 20 February 24 2005 Case 0251M SDG D05939

Please contact Ms Constance Lapite at (781) 224-6628 or at Constance lapite(am-ecom if you have any questions regarding this Tier II validation

Paula L DiMattei Data Validator

Deborah A Trwini ^mjrjat

Robert Shoemaker Project Chemist

bullgt pound^ampgtlt^ Constance D Lapite MampE RAC Lead Chemist

cc ^James Chow EPA Remedial Project Manager (DV memo and data summary tables) Karen Wedlock-Hunt MampE Project Manager (entire package) Robert Shoemaker Project Chemist (entire package) Troy Mills Landfill Project File WA No 160-RICO-019M (entire package)

Attachments ORDA Table I Recommendation Summary Table Table II Overall Evaluation of Data Table III Tentatively Identified Compound Summary Data Summary Tables Data Validation Worksheets PE Score Report Copy of non-CLP Analytical Method (MampE DAS Specification D-148) Copies of Telephone LogCommunications Forms Supporting Data for Reduced Payment Recommendations (not applicable) Copies of Field Sampling Notes (previously submitted) Copies of EPA-Approved Amendments not QAPjP or SAP (not applicable) CSF Completeness Evidence File Audit (DC-2 Form) DQO Summary Form

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DVMemossD05939_svocsim pd Metcatfamp Eddy Inc

REGION I EPA-NE ORGANIC REGIONAL DATA ASSESSMENT (ORDA)

CASE raquozjggtH _ SITE NAME TV

LAB NAME uoAlaquo Vlaquo- amp+ OF SAMPLESMATRIX

SDG Posirt_ VALIDATION CONTRACTOR

SOW CONTRACT p-rttll-- VALIDATORS NAME

EPA-NE DV TIER LEVEL JC_ DATE DP RECD BY EPA-NE

TPOPO ACTION _ FYI ^ DV COMPLETION DATE

ANALYTICAL DATA QUALITY SUMMARY tffpft^m t~

bullVGA SV-SM PestPCB 1 Preservation and Contractual Holding Times 2 GCMS GCECD Instrument Performance Check raquo 3 Initial Calibration laquo 4 Continuing Calibration o 5 Blanks ~ o 6 Surrogate Compounds raquo 7 Internal Standards o 8 Matrix SpikeMatrix Spike Duplicate ggt 9 Sensitivity Check 0 10 PE Samples-Accuracy Check 0 11 Target Compound Identification jpy 12 Compound Quantitation and Reported QLs o 13 Tentatively Identified Compounds o 14 Semivolatile CleanupPesticidePCB Cleanup ulaquor 15 Data Completeness 0 16 Overall Evaluation of Data laquo

o = Data had no problems or were qualified due to minor contractual problems m = Data were qualified due to major contractual problems z = Data were rejected as unusable due major contractual problems

ACTION ITEMS (z items)

AREAS OF CONCERN (m items)

COMMENTS

This form assesses the analytical data quality in terms of contractual compliance only It does not assess sampling errors andor non-contractual analytical issues that affect data quality

Check ACTION only if contractual defects resulted in reduced paymentdata rejection recommendations

Validator t ltiJSagt3gtlt -3 Date

INSTRUCTIONS ON REVERSE SIDE

1296

Table I Recommendation Summary

Soil Semivolatile Organic Analysis Troy Mills Landfill Superfund Site

Case0251M SDGD05939

Sample ID Matrix

D05945 SO

D05946 SO

D05947 SO (FD)

D05948 SO

D05949 SO

D05950 SO

D05951 SO

D05952 SO

D05953 SO (FD)

D05954 EB

EB shy Equipment Blank FD shy Field Duplicate SOshy Soil

Qualifier

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 11 13 14 15

2 Jl 3 4 7 8 9 10 13 15

A 2 jl 3 4 7 8 9 10 13 15

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 jl 3 4 7 8 9 10 13 15

A 2 3 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 Jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 13 15

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A - Accept the data but qualify the positive results for benzaldehyde in samples D05945 D05946 D05949 D05950 D05951 and D05952 and for acetophenone in sample D05951 as (EB) due to equipment blank contamination

A2 - Accept the data but qualify the positive result for di-n-butylphthalate as nondetect (U) at the reported value due to laboratory method blank contamination

A5 - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to PE sample contamination

A - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to laboratory method blank contamination

J - Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde hexachlorocyclopentadiene 24shydmitrophenol 46-dmitro-2-methylphenol atrazine and pentachlorophenol due to initial calibration RSD exceedances

J2 Estimate (J) the positive result for di-n-butyl phthalate due to the initial calibration RSD exceedance

J3 Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde and 33-dichlorobenzidme in all samples for hexachlorobutadiene 4-mtrophenol and hexachlorobenzene m samples D05948 D05949 and D05953 for hexachlorocyclopentadiene m samples D05954 D05948 D05949 and D05953 and for 24shydimtrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 due to the continuing calibration D exceedances

J4 - Estimate (J) the positive results for di-n-butylphthalate in all soil samples due to continuing calibration exceedance

J5 - Estimate (UJ) the nondetect caprolactam result and raise the quantitation limit to 4 ugL (equivalent to the concentration of the high-level LFB) due to low low-level and high-level LFB recoveries This result may be biased low

J6 - Estimate (UJ) the nondetect results for 4-mtrophenol 46-dmitro-2-methylphenol and pentachlorophenol due to low low-level LFB recoveries These results may be biased low

J7 - Estimate (J) the positive result for di-n-butylphthalate due to high low-level and high-level LFB recoveries This result may be biased high

J8 - Estimate (UJ) the nondetect 24-dmitrophenol result and raise the quantitation limit to 800 ugKg (equivalent to the concentration of the high-level LFB and corrected for all preparation factors) due to low low-level and high-level LFB recoveries This result may be biased low

J9 - Estimate (UJ) the nondetect results for 24-dimethylphenol 4-mtrophenol 46-dimrro-2-methylphenol pentachlorophenol and 33-dichlorobenzidme due to low low-level LFB recoveries These results may be biased low

J10 - Estimate (UJ) the nondetect result 4-chIoroamlme due to low low-level and high-le el LFB recoveries This result may be biased low

J1 - Estimate (J) the positive result for benzo(b)fluoranthene due to high high-level LFB reco ery This result may be biased high

J12 - Estimate (UJ) the nondetect caprolactam result due to low LCS recovery This result may be biased low

J3 - Estimate (UJ) the nondetect benzaldehyde and 4-chloroamline results due to low LCS recoveries The results may be biased low

J14 - Estimate (J) the positive results for benzo(b)fluoranthene benzo(a)pyrene and mdeno(l23-cd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 due to high LCS recoveries The results may be biased high

J15 - Estimate (J) the positive results for the following compounds in the samples listed below due to uncertainty in the quantitation as a result of the exceeded ion abundance ration criteria

DOS 950 di-n-butylphthalate DOS 951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate mdeno(l23-cd)pyrene D05946 mdeno(l23-cd)pyrene D05947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate D05953 di-n-butylphthalate

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Page 16: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

Ms Christine Clark Page 16 February 24 2005 Case 0251M SDGD05939

Action High These compounds were not detected in any of the associated soil samples therefore no data validation actions were required Six compounds (naphthalene hexachlorobenzene phenanthrene pyrene and dibenz(ah)anthracene and benzo(ghi)perylene) were scored as Warning High two compounds (4-hydroxy-4-methyl-2-pentanone and 4-methyl-3-penten-2-one) were scored Non-spiked TIC and one compound (din-n-butylphthalate) was scored Less than CRQL No data validation action is required on the basis of the Warning High Non-spiked TIC and less than CRQL scores Bis(2-ethylhexyl)phthalate was scored as Contaminant This compound was also detected in the associated laboratory method blanks and consequently evaluated in the blank section of this memorandum (please see Blanks above)

Laboratory Control Sample (LCS) Results

Full Scan

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

LCS Compound Recovery Action

SW122104L06 caprolactam 35 Qualify as estimated (UJ) the nondetectresult in sample D05954

caprolactam

atrazine 135 Atrazine was not detected in the associaNo actions were required

ted sample

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Recovery Action

SS012805L01 benzaldehyde 46 Qualify as estimated (J) the positive and (UJ) the nondetect benzaldehyde results in all soil samples

4-chloroanihne 35 Qualify as estimated (UJ) the nondetect 4shychloroaruhne results in all soil samples

SIM

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with equipment blank sample D05954 and the validation actions taken

J NEWA160 Troy Mills LandfillData VahdationDecember 2004DVMemossDQ5939_svocstm vpd Metcalfamp Eddy Inc

Ms Christine Clark Page 17 February 24 2005 Case 0251M SDGD05939

LCS Compound Action Recovery

SW122104L05 pentachlorophenol 194 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 123 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(a)pyrene 122 Benzo(a)pyrene was not detected in the associated sample No actions were required

mdeno( 1 2 3 -cd)pyrene 130 Indeno(l23-cd)pyrene was reported from the full scan analysis therefore no actions were required

dibenz(ah)anthracene 136 Dibenz(ah)anthracene was not detected in the associated sample No actions were required

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Action Recovery

SS012805L02 pentachlorophenol 126 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 142 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(b)fluoranthene 128 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D05951 D05952 D05945 D05946 and D05949

benzo(a)pyrene 121 Qualify as estimated (J) the positive benzo(a)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

mdeno( 1 23-cd)pyrene 129 Qualify as estimated (J) the positive indeno(l23shycd)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

dibenz(ah)anthracene 133 Dibenz(ah)anthracene was not detected in the associated samples No actions were required

J NE WA160 Troy Mills LandfillData Validation December 2004 D V MemossD0593 9_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 18 February 24 2005 Case 0251M SDG D05939

Compound Ouantitation and Reported Ouantitation Limits

Full Scan and SIM

Because of their high moisture content samples D05945 D05946 D05949 D05951 and D05952 were freeze-dried prior to extraction

The following table summarizes the SIM and full scan reporting when data existed for both full scan and SIM analyses Professional judgment was used to select specific analyses in order to report the lowest quantitation limit achievable and to report results with values within the calibration range

Compound Results reported from Full Scan Results reported from SIM

pentachlorophenol all samples none

di-n-butyl phthalate none all samples

benzo(a)anthracene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

bis(2-ethylhexyl)phthalate all samples none

benzo(b)fluoranthene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

benzo(a)pyrene none all samples

indeno(l23-cd)pyrene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

dibenz(ah)anthracene none all samples

Full Scan

The bis(2-ethylhexyl)phthalate results in the following samples were reported from the dilution analysis listed in parentheses since these results exceeded the calibration range in the undiluted analysis D05945 (5x) D05946 (20x) D05947 (20x) D05948 (20x) D05949 (5x) and D05953 (20x)

JNE WA160 Troy Mills LandfillData ValidationDecember 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 19 February 24 2005 Case 0251M SDGD05939

SIM

The following compounds in the samples listed below were qualified as estimated (J) due to uncertainty in the quantitation as a result of the exceeded ion abundance ratio criteria

D05950 di-n-butylphthalate DOS951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate indeno(l23-cd)pyrene D05946 indeno(l23-cd)pyrene DOS 947 di-n-butylphthalate DOS 948 di-n-butylphthalate DOS 949 di-n-butylphthalate D05953 di-n-butylphthalate

Tentatively Identified Compounds (TICs)

One TIC 4-hydroxy-4-methyl-2-pentanone was detected in all samples and is considered an aldol condensation product Consequently this TIC was not included on Table III Tentatively Identified Compound Summary for the affected samples

The following compound in the sample listed was reported twice in the affected sample For this sample this result was renamed to a more general identification since a compound cannot elute at multiple retention times The renamed TIC is described in the table below

Compound name as reported by the Compound name as renamed during data Affected sample laboratory validation

oleic acid unknown D05951

JNEWA160 Troy Mills LandflllData ValidationDecember 2004DV MemossD05939_svocsimwpd MetcalfA Eddy Inc

Ms Christine Clark Page 20 February 24 2005 Case 0251M SDG D05939

Please contact Ms Constance Lapite at (781) 224-6628 or at Constance lapite(am-ecom if you have any questions regarding this Tier II validation

Paula L DiMattei Data Validator

Deborah A Trwini ^mjrjat

Robert Shoemaker Project Chemist

bullgt pound^ampgtlt^ Constance D Lapite MampE RAC Lead Chemist

cc ^James Chow EPA Remedial Project Manager (DV memo and data summary tables) Karen Wedlock-Hunt MampE Project Manager (entire package) Robert Shoemaker Project Chemist (entire package) Troy Mills Landfill Project File WA No 160-RICO-019M (entire package)

Attachments ORDA Table I Recommendation Summary Table Table II Overall Evaluation of Data Table III Tentatively Identified Compound Summary Data Summary Tables Data Validation Worksheets PE Score Report Copy of non-CLP Analytical Method (MampE DAS Specification D-148) Copies of Telephone LogCommunications Forms Supporting Data for Reduced Payment Recommendations (not applicable) Copies of Field Sampling Notes (previously submitted) Copies of EPA-Approved Amendments not QAPjP or SAP (not applicable) CSF Completeness Evidence File Audit (DC-2 Form) DQO Summary Form

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DVMemossD05939_svocsim pd Metcatfamp Eddy Inc

REGION I EPA-NE ORGANIC REGIONAL DATA ASSESSMENT (ORDA)

CASE raquozjggtH _ SITE NAME TV

LAB NAME uoAlaquo Vlaquo- amp+ OF SAMPLESMATRIX

SDG Posirt_ VALIDATION CONTRACTOR

SOW CONTRACT p-rttll-- VALIDATORS NAME

EPA-NE DV TIER LEVEL JC_ DATE DP RECD BY EPA-NE

TPOPO ACTION _ FYI ^ DV COMPLETION DATE

ANALYTICAL DATA QUALITY SUMMARY tffpft^m t~

bullVGA SV-SM PestPCB 1 Preservation and Contractual Holding Times 2 GCMS GCECD Instrument Performance Check raquo 3 Initial Calibration laquo 4 Continuing Calibration o 5 Blanks ~ o 6 Surrogate Compounds raquo 7 Internal Standards o 8 Matrix SpikeMatrix Spike Duplicate ggt 9 Sensitivity Check 0 10 PE Samples-Accuracy Check 0 11 Target Compound Identification jpy 12 Compound Quantitation and Reported QLs o 13 Tentatively Identified Compounds o 14 Semivolatile CleanupPesticidePCB Cleanup ulaquor 15 Data Completeness 0 16 Overall Evaluation of Data laquo

o = Data had no problems or were qualified due to minor contractual problems m = Data were qualified due to major contractual problems z = Data were rejected as unusable due major contractual problems

ACTION ITEMS (z items)

AREAS OF CONCERN (m items)

COMMENTS

This form assesses the analytical data quality in terms of contractual compliance only It does not assess sampling errors andor non-contractual analytical issues that affect data quality

Check ACTION only if contractual defects resulted in reduced paymentdata rejection recommendations

Validator t ltiJSagt3gtlt -3 Date

INSTRUCTIONS ON REVERSE SIDE

1296

Table I Recommendation Summary

Soil Semivolatile Organic Analysis Troy Mills Landfill Superfund Site

Case0251M SDGD05939

Sample ID Matrix

D05945 SO

D05946 SO

D05947 SO (FD)

D05948 SO

D05949 SO

D05950 SO

D05951 SO

D05952 SO

D05953 SO (FD)

D05954 EB

EB shy Equipment Blank FD shy Field Duplicate SOshy Soil

Qualifier

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 11 13 14 15

2 Jl 3 4 7 8 9 10 13 15

A 2 jl 3 4 7 8 9 10 13 15

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 jl 3 4 7 8 9 10 13 15

A 2 3 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 Jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 13 15

^2 4 jl 2 3 5 6 7 12

A - Accept the data but qualify the positive results for benzaldehyde in samples D05945 D05946 D05949 D05950 D05951 and D05952 and for acetophenone in sample D05951 as (EB) due to equipment blank contamination

A2 - Accept the data but qualify the positive result for di-n-butylphthalate as nondetect (U) at the reported value due to laboratory method blank contamination

A5 - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to PE sample contamination

A - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to laboratory method blank contamination

J - Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde hexachlorocyclopentadiene 24shydmitrophenol 46-dmitro-2-methylphenol atrazine and pentachlorophenol due to initial calibration RSD exceedances

J2 Estimate (J) the positive result for di-n-butyl phthalate due to the initial calibration RSD exceedance

J3 Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde and 33-dichlorobenzidme in all samples for hexachlorobutadiene 4-mtrophenol and hexachlorobenzene m samples D05948 D05949 and D05953 for hexachlorocyclopentadiene m samples D05954 D05948 D05949 and D05953 and for 24shydimtrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 due to the continuing calibration D exceedances

J4 - Estimate (J) the positive results for di-n-butylphthalate in all soil samples due to continuing calibration exceedance

J5 - Estimate (UJ) the nondetect caprolactam result and raise the quantitation limit to 4 ugL (equivalent to the concentration of the high-level LFB) due to low low-level and high-level LFB recoveries This result may be biased low

J6 - Estimate (UJ) the nondetect results for 4-mtrophenol 46-dmitro-2-methylphenol and pentachlorophenol due to low low-level LFB recoveries These results may be biased low

J7 - Estimate (J) the positive result for di-n-butylphthalate due to high low-level and high-level LFB recoveries This result may be biased high

J8 - Estimate (UJ) the nondetect 24-dmitrophenol result and raise the quantitation limit to 800 ugKg (equivalent to the concentration of the high-level LFB and corrected for all preparation factors) due to low low-level and high-level LFB recoveries This result may be biased low

J9 - Estimate (UJ) the nondetect results for 24-dimethylphenol 4-mtrophenol 46-dimrro-2-methylphenol pentachlorophenol and 33-dichlorobenzidme due to low low-level LFB recoveries These results may be biased low

J10 - Estimate (UJ) the nondetect result 4-chIoroamlme due to low low-level and high-le el LFB recoveries This result may be biased low

J1 - Estimate (J) the positive result for benzo(b)fluoranthene due to high high-level LFB reco ery This result may be biased high

J12 - Estimate (UJ) the nondetect caprolactam result due to low LCS recovery This result may be biased low

J3 - Estimate (UJ) the nondetect benzaldehyde and 4-chloroamline results due to low LCS recoveries The results may be biased low

J14 - Estimate (J) the positive results for benzo(b)fluoranthene benzo(a)pyrene and mdeno(l23-cd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 due to high LCS recoveries The results may be biased high

J15 - Estimate (J) the positive results for the following compounds in the samples listed below due to uncertainty in the quantitation as a result of the exceeded ion abundance ration criteria

DOS 950 di-n-butylphthalate DOS 951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate mdeno(l23-cd)pyrene D05946 mdeno(l23-cd)pyrene D05947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate D05953 di-n-butylphthalate

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Page 17: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

Ms Christine Clark Page 17 February 24 2005 Case 0251M SDGD05939

LCS Compound Action Recovery

SW122104L05 pentachlorophenol 194 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 123 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(a)pyrene 122 Benzo(a)pyrene was not detected in the associated sample No actions were required

mdeno( 1 2 3 -cd)pyrene 130 Indeno(l23-cd)pyrene was reported from the full scan analysis therefore no actions were required

dibenz(ah)anthracene 136 Dibenz(ah)anthracene was not detected in the associated sample No actions were required

The following table summarizes the LCS recoveries outside the 50-120 criteria in association with all soil samples in this data set and the validation actions taken

LCS Compound Action Recovery

SS012805L02 pentachlorophenol 126 Pentachlorophenol was reported from the full scan analysis therefore no actions were required

bis(2-ethylhexyl)phthalate 142 Bis(2-ethylhexyl)phthalate was reported from the full scan analysis therefore no actions were required

benzo(b)fluoranthene 128 Qualify as estimated (J) the positive benzo(b)fluoranthene result in samples D05951 D05952 D05945 D05946 and D05949

benzo(a)pyrene 121 Qualify as estimated (J) the positive benzo(a)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

mdeno( 1 23-cd)pyrene 129 Qualify as estimated (J) the positive indeno(l23shycd)pyrene result in samples D05951 D05952 D05945 D05946 and D05949

dibenz(ah)anthracene 133 Dibenz(ah)anthracene was not detected in the associated samples No actions were required

J NE WA160 Troy Mills LandfillData Validation December 2004 D V MemossD0593 9_svocsim pd Metcalfamp Eddy Inc

Ms Christine Clark Page 18 February 24 2005 Case 0251M SDG D05939

Compound Ouantitation and Reported Ouantitation Limits

Full Scan and SIM

Because of their high moisture content samples D05945 D05946 D05949 D05951 and D05952 were freeze-dried prior to extraction

The following table summarizes the SIM and full scan reporting when data existed for both full scan and SIM analyses Professional judgment was used to select specific analyses in order to report the lowest quantitation limit achievable and to report results with values within the calibration range

Compound Results reported from Full Scan Results reported from SIM

pentachlorophenol all samples none

di-n-butyl phthalate none all samples

benzo(a)anthracene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

bis(2-ethylhexyl)phthalate all samples none

benzo(b)fluoranthene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

benzo(a)pyrene none all samples

indeno(l23-cd)pyrene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

dibenz(ah)anthracene none all samples

Full Scan

The bis(2-ethylhexyl)phthalate results in the following samples were reported from the dilution analysis listed in parentheses since these results exceeded the calibration range in the undiluted analysis D05945 (5x) D05946 (20x) D05947 (20x) D05948 (20x) D05949 (5x) and D05953 (20x)

JNE WA160 Troy Mills LandfillData ValidationDecember 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 19 February 24 2005 Case 0251M SDGD05939

SIM

The following compounds in the samples listed below were qualified as estimated (J) due to uncertainty in the quantitation as a result of the exceeded ion abundance ratio criteria

D05950 di-n-butylphthalate DOS951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate indeno(l23-cd)pyrene D05946 indeno(l23-cd)pyrene DOS 947 di-n-butylphthalate DOS 948 di-n-butylphthalate DOS 949 di-n-butylphthalate D05953 di-n-butylphthalate

Tentatively Identified Compounds (TICs)

One TIC 4-hydroxy-4-methyl-2-pentanone was detected in all samples and is considered an aldol condensation product Consequently this TIC was not included on Table III Tentatively Identified Compound Summary for the affected samples

The following compound in the sample listed was reported twice in the affected sample For this sample this result was renamed to a more general identification since a compound cannot elute at multiple retention times The renamed TIC is described in the table below

Compound name as reported by the Compound name as renamed during data Affected sample laboratory validation

oleic acid unknown D05951

JNEWA160 Troy Mills LandflllData ValidationDecember 2004DV MemossD05939_svocsimwpd MetcalfA Eddy Inc

Ms Christine Clark Page 20 February 24 2005 Case 0251M SDG D05939

Please contact Ms Constance Lapite at (781) 224-6628 or at Constance lapite(am-ecom if you have any questions regarding this Tier II validation

Paula L DiMattei Data Validator

Deborah A Trwini ^mjrjat

Robert Shoemaker Project Chemist

bullgt pound^ampgtlt^ Constance D Lapite MampE RAC Lead Chemist

cc ^James Chow EPA Remedial Project Manager (DV memo and data summary tables) Karen Wedlock-Hunt MampE Project Manager (entire package) Robert Shoemaker Project Chemist (entire package) Troy Mills Landfill Project File WA No 160-RICO-019M (entire package)

Attachments ORDA Table I Recommendation Summary Table Table II Overall Evaluation of Data Table III Tentatively Identified Compound Summary Data Summary Tables Data Validation Worksheets PE Score Report Copy of non-CLP Analytical Method (MampE DAS Specification D-148) Copies of Telephone LogCommunications Forms Supporting Data for Reduced Payment Recommendations (not applicable) Copies of Field Sampling Notes (previously submitted) Copies of EPA-Approved Amendments not QAPjP or SAP (not applicable) CSF Completeness Evidence File Audit (DC-2 Form) DQO Summary Form

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DVMemossD05939_svocsim pd Metcatfamp Eddy Inc

REGION I EPA-NE ORGANIC REGIONAL DATA ASSESSMENT (ORDA)

CASE raquozjggtH _ SITE NAME TV

LAB NAME uoAlaquo Vlaquo- amp+ OF SAMPLESMATRIX

SDG Posirt_ VALIDATION CONTRACTOR

SOW CONTRACT p-rttll-- VALIDATORS NAME

EPA-NE DV TIER LEVEL JC_ DATE DP RECD BY EPA-NE

TPOPO ACTION _ FYI ^ DV COMPLETION DATE

ANALYTICAL DATA QUALITY SUMMARY tffpft^m t~

bullVGA SV-SM PestPCB 1 Preservation and Contractual Holding Times 2 GCMS GCECD Instrument Performance Check raquo 3 Initial Calibration laquo 4 Continuing Calibration o 5 Blanks ~ o 6 Surrogate Compounds raquo 7 Internal Standards o 8 Matrix SpikeMatrix Spike Duplicate ggt 9 Sensitivity Check 0 10 PE Samples-Accuracy Check 0 11 Target Compound Identification jpy 12 Compound Quantitation and Reported QLs o 13 Tentatively Identified Compounds o 14 Semivolatile CleanupPesticidePCB Cleanup ulaquor 15 Data Completeness 0 16 Overall Evaluation of Data laquo

o = Data had no problems or were qualified due to minor contractual problems m = Data were qualified due to major contractual problems z = Data were rejected as unusable due major contractual problems

ACTION ITEMS (z items)

AREAS OF CONCERN (m items)

COMMENTS

This form assesses the analytical data quality in terms of contractual compliance only It does not assess sampling errors andor non-contractual analytical issues that affect data quality

Check ACTION only if contractual defects resulted in reduced paymentdata rejection recommendations

Validator t ltiJSagt3gtlt -3 Date

INSTRUCTIONS ON REVERSE SIDE

1296

Table I Recommendation Summary

Soil Semivolatile Organic Analysis Troy Mills Landfill Superfund Site

Case0251M SDGD05939

Sample ID Matrix

D05945 SO

D05946 SO

D05947 SO (FD)

D05948 SO

D05949 SO

D05950 SO

D05951 SO

D05952 SO

D05953 SO (FD)

D05954 EB

EB shy Equipment Blank FD shy Field Duplicate SOshy Soil

Qualifier

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 11 13 14 15

2 Jl 3 4 7 8 9 10 13 15

A 2 jl 3 4 7 8 9 10 13 15

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 jl 3 4 7 8 9 10 13 15

A 2 3 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 Jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 13 15

^2 4 jl 2 3 5 6 7 12

A - Accept the data but qualify the positive results for benzaldehyde in samples D05945 D05946 D05949 D05950 D05951 and D05952 and for acetophenone in sample D05951 as (EB) due to equipment blank contamination

A2 - Accept the data but qualify the positive result for di-n-butylphthalate as nondetect (U) at the reported value due to laboratory method blank contamination

A5 - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to PE sample contamination

A - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to laboratory method blank contamination

J - Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde hexachlorocyclopentadiene 24shydmitrophenol 46-dmitro-2-methylphenol atrazine and pentachlorophenol due to initial calibration RSD exceedances

J2 Estimate (J) the positive result for di-n-butyl phthalate due to the initial calibration RSD exceedance

J3 Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde and 33-dichlorobenzidme in all samples for hexachlorobutadiene 4-mtrophenol and hexachlorobenzene m samples D05948 D05949 and D05953 for hexachlorocyclopentadiene m samples D05954 D05948 D05949 and D05953 and for 24shydimtrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 due to the continuing calibration D exceedances

J4 - Estimate (J) the positive results for di-n-butylphthalate in all soil samples due to continuing calibration exceedance

J5 - Estimate (UJ) the nondetect caprolactam result and raise the quantitation limit to 4 ugL (equivalent to the concentration of the high-level LFB) due to low low-level and high-level LFB recoveries This result may be biased low

J6 - Estimate (UJ) the nondetect results for 4-mtrophenol 46-dmitro-2-methylphenol and pentachlorophenol due to low low-level LFB recoveries These results may be biased low

J7 - Estimate (J) the positive result for di-n-butylphthalate due to high low-level and high-level LFB recoveries This result may be biased high

J8 - Estimate (UJ) the nondetect 24-dmitrophenol result and raise the quantitation limit to 800 ugKg (equivalent to the concentration of the high-level LFB and corrected for all preparation factors) due to low low-level and high-level LFB recoveries This result may be biased low

J9 - Estimate (UJ) the nondetect results for 24-dimethylphenol 4-mtrophenol 46-dimrro-2-methylphenol pentachlorophenol and 33-dichlorobenzidme due to low low-level LFB recoveries These results may be biased low

J10 - Estimate (UJ) the nondetect result 4-chIoroamlme due to low low-level and high-le el LFB recoveries This result may be biased low

J1 - Estimate (J) the positive result for benzo(b)fluoranthene due to high high-level LFB reco ery This result may be biased high

J12 - Estimate (UJ) the nondetect caprolactam result due to low LCS recovery This result may be biased low

J3 - Estimate (UJ) the nondetect benzaldehyde and 4-chloroamline results due to low LCS recoveries The results may be biased low

J14 - Estimate (J) the positive results for benzo(b)fluoranthene benzo(a)pyrene and mdeno(l23-cd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 due to high LCS recoveries The results may be biased high

J15 - Estimate (J) the positive results for the following compounds in the samples listed below due to uncertainty in the quantitation as a result of the exceeded ion abundance ration criteria

DOS 950 di-n-butylphthalate DOS 951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate mdeno(l23-cd)pyrene D05946 mdeno(l23-cd)pyrene D05947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate D05953 di-n-butylphthalate

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Page 18: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

Ms Christine Clark Page 18 February 24 2005 Case 0251M SDG D05939

Compound Ouantitation and Reported Ouantitation Limits

Full Scan and SIM

Because of their high moisture content samples D05945 D05946 D05949 D05951 and D05952 were freeze-dried prior to extraction

The following table summarizes the SIM and full scan reporting when data existed for both full scan and SIM analyses Professional judgment was used to select specific analyses in order to report the lowest quantitation limit achievable and to report results with values within the calibration range

Compound Results reported from Full Scan Results reported from SIM

pentachlorophenol all samples none

di-n-butyl phthalate none all samples

benzo(a)anthracene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

bis(2-ethylhexyl)phthalate all samples none

benzo(b)fluoranthene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

benzo(a)pyrene none all samples

indeno(l23-cd)pyrene D05947 D05948 D05950 D05945 D05946 D05949 D05953 D05954 D05951D05952

dibenz(ah)anthracene none all samples

Full Scan

The bis(2-ethylhexyl)phthalate results in the following samples were reported from the dilution analysis listed in parentheses since these results exceeded the calibration range in the undiluted analysis D05945 (5x) D05946 (20x) D05947 (20x) D05948 (20x) D05949 (5x) and D05953 (20x)

JNE WA160 Troy Mills LandfillData ValidationDecember 2004D V MemossD05939_svocsim wpd Metcalfamp Eddy Inc

Ms Christine Clark Page 19 February 24 2005 Case 0251M SDGD05939

SIM

The following compounds in the samples listed below were qualified as estimated (J) due to uncertainty in the quantitation as a result of the exceeded ion abundance ratio criteria

D05950 di-n-butylphthalate DOS951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate indeno(l23-cd)pyrene D05946 indeno(l23-cd)pyrene DOS 947 di-n-butylphthalate DOS 948 di-n-butylphthalate DOS 949 di-n-butylphthalate D05953 di-n-butylphthalate

Tentatively Identified Compounds (TICs)

One TIC 4-hydroxy-4-methyl-2-pentanone was detected in all samples and is considered an aldol condensation product Consequently this TIC was not included on Table III Tentatively Identified Compound Summary for the affected samples

The following compound in the sample listed was reported twice in the affected sample For this sample this result was renamed to a more general identification since a compound cannot elute at multiple retention times The renamed TIC is described in the table below

Compound name as reported by the Compound name as renamed during data Affected sample laboratory validation

oleic acid unknown D05951

JNEWA160 Troy Mills LandflllData ValidationDecember 2004DV MemossD05939_svocsimwpd MetcalfA Eddy Inc

Ms Christine Clark Page 20 February 24 2005 Case 0251M SDG D05939

Please contact Ms Constance Lapite at (781) 224-6628 or at Constance lapite(am-ecom if you have any questions regarding this Tier II validation

Paula L DiMattei Data Validator

Deborah A Trwini ^mjrjat

Robert Shoemaker Project Chemist

bullgt pound^ampgtlt^ Constance D Lapite MampE RAC Lead Chemist

cc ^James Chow EPA Remedial Project Manager (DV memo and data summary tables) Karen Wedlock-Hunt MampE Project Manager (entire package) Robert Shoemaker Project Chemist (entire package) Troy Mills Landfill Project File WA No 160-RICO-019M (entire package)

Attachments ORDA Table I Recommendation Summary Table Table II Overall Evaluation of Data Table III Tentatively Identified Compound Summary Data Summary Tables Data Validation Worksheets PE Score Report Copy of non-CLP Analytical Method (MampE DAS Specification D-148) Copies of Telephone LogCommunications Forms Supporting Data for Reduced Payment Recommendations (not applicable) Copies of Field Sampling Notes (previously submitted) Copies of EPA-Approved Amendments not QAPjP or SAP (not applicable) CSF Completeness Evidence File Audit (DC-2 Form) DQO Summary Form

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DVMemossD05939_svocsim pd Metcatfamp Eddy Inc

REGION I EPA-NE ORGANIC REGIONAL DATA ASSESSMENT (ORDA)

CASE raquozjggtH _ SITE NAME TV

LAB NAME uoAlaquo Vlaquo- amp+ OF SAMPLESMATRIX

SDG Posirt_ VALIDATION CONTRACTOR

SOW CONTRACT p-rttll-- VALIDATORS NAME

EPA-NE DV TIER LEVEL JC_ DATE DP RECD BY EPA-NE

TPOPO ACTION _ FYI ^ DV COMPLETION DATE

ANALYTICAL DATA QUALITY SUMMARY tffpft^m t~

bullVGA SV-SM PestPCB 1 Preservation and Contractual Holding Times 2 GCMS GCECD Instrument Performance Check raquo 3 Initial Calibration laquo 4 Continuing Calibration o 5 Blanks ~ o 6 Surrogate Compounds raquo 7 Internal Standards o 8 Matrix SpikeMatrix Spike Duplicate ggt 9 Sensitivity Check 0 10 PE Samples-Accuracy Check 0 11 Target Compound Identification jpy 12 Compound Quantitation and Reported QLs o 13 Tentatively Identified Compounds o 14 Semivolatile CleanupPesticidePCB Cleanup ulaquor 15 Data Completeness 0 16 Overall Evaluation of Data laquo

o = Data had no problems or were qualified due to minor contractual problems m = Data were qualified due to major contractual problems z = Data were rejected as unusable due major contractual problems

ACTION ITEMS (z items)

AREAS OF CONCERN (m items)

COMMENTS

This form assesses the analytical data quality in terms of contractual compliance only It does not assess sampling errors andor non-contractual analytical issues that affect data quality

Check ACTION only if contractual defects resulted in reduced paymentdata rejection recommendations

Validator t ltiJSagt3gtlt -3 Date

INSTRUCTIONS ON REVERSE SIDE

1296

Table I Recommendation Summary

Soil Semivolatile Organic Analysis Troy Mills Landfill Superfund Site

Case0251M SDGD05939

Sample ID Matrix

D05945 SO

D05946 SO

D05947 SO (FD)

D05948 SO

D05949 SO

D05950 SO

D05951 SO

D05952 SO

D05953 SO (FD)

D05954 EB

EB shy Equipment Blank FD shy Field Duplicate SOshy Soil

Qualifier

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 11 13 14 15

2 Jl 3 4 7 8 9 10 13 15

A 2 jl 3 4 7 8 9 10 13 15

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 jl 3 4 7 8 9 10 13 15

A 2 3 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 Jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 13 15

^2 4 jl 2 3 5 6 7 12

A - Accept the data but qualify the positive results for benzaldehyde in samples D05945 D05946 D05949 D05950 D05951 and D05952 and for acetophenone in sample D05951 as (EB) due to equipment blank contamination

A2 - Accept the data but qualify the positive result for di-n-butylphthalate as nondetect (U) at the reported value due to laboratory method blank contamination

A5 - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to PE sample contamination

A - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to laboratory method blank contamination

J - Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde hexachlorocyclopentadiene 24shydmitrophenol 46-dmitro-2-methylphenol atrazine and pentachlorophenol due to initial calibration RSD exceedances

J2 Estimate (J) the positive result for di-n-butyl phthalate due to the initial calibration RSD exceedance

J3 Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde and 33-dichlorobenzidme in all samples for hexachlorobutadiene 4-mtrophenol and hexachlorobenzene m samples D05948 D05949 and D05953 for hexachlorocyclopentadiene m samples D05954 D05948 D05949 and D05953 and for 24shydimtrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 due to the continuing calibration D exceedances

J4 - Estimate (J) the positive results for di-n-butylphthalate in all soil samples due to continuing calibration exceedance

J5 - Estimate (UJ) the nondetect caprolactam result and raise the quantitation limit to 4 ugL (equivalent to the concentration of the high-level LFB) due to low low-level and high-level LFB recoveries This result may be biased low

J6 - Estimate (UJ) the nondetect results for 4-mtrophenol 46-dmitro-2-methylphenol and pentachlorophenol due to low low-level LFB recoveries These results may be biased low

J7 - Estimate (J) the positive result for di-n-butylphthalate due to high low-level and high-level LFB recoveries This result may be biased high

J8 - Estimate (UJ) the nondetect 24-dmitrophenol result and raise the quantitation limit to 800 ugKg (equivalent to the concentration of the high-level LFB and corrected for all preparation factors) due to low low-level and high-level LFB recoveries This result may be biased low

J9 - Estimate (UJ) the nondetect results for 24-dimethylphenol 4-mtrophenol 46-dimrro-2-methylphenol pentachlorophenol and 33-dichlorobenzidme due to low low-level LFB recoveries These results may be biased low

J10 - Estimate (UJ) the nondetect result 4-chIoroamlme due to low low-level and high-le el LFB recoveries This result may be biased low

J1 - Estimate (J) the positive result for benzo(b)fluoranthene due to high high-level LFB reco ery This result may be biased high

J12 - Estimate (UJ) the nondetect caprolactam result due to low LCS recovery This result may be biased low

J3 - Estimate (UJ) the nondetect benzaldehyde and 4-chloroamline results due to low LCS recoveries The results may be biased low

J14 - Estimate (J) the positive results for benzo(b)fluoranthene benzo(a)pyrene and mdeno(l23-cd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 due to high LCS recoveries The results may be biased high

J15 - Estimate (J) the positive results for the following compounds in the samples listed below due to uncertainty in the quantitation as a result of the exceeded ion abundance ration criteria

DOS 950 di-n-butylphthalate DOS 951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate mdeno(l23-cd)pyrene D05946 mdeno(l23-cd)pyrene D05947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate D05953 di-n-butylphthalate

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Page 19: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

Ms Christine Clark Page 19 February 24 2005 Case 0251M SDGD05939

SIM

The following compounds in the samples listed below were qualified as estimated (J) due to uncertainty in the quantitation as a result of the exceeded ion abundance ratio criteria

D05950 di-n-butylphthalate DOS951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate indeno(l23-cd)pyrene D05946 indeno(l23-cd)pyrene DOS 947 di-n-butylphthalate DOS 948 di-n-butylphthalate DOS 949 di-n-butylphthalate D05953 di-n-butylphthalate

Tentatively Identified Compounds (TICs)

One TIC 4-hydroxy-4-methyl-2-pentanone was detected in all samples and is considered an aldol condensation product Consequently this TIC was not included on Table III Tentatively Identified Compound Summary for the affected samples

The following compound in the sample listed was reported twice in the affected sample For this sample this result was renamed to a more general identification since a compound cannot elute at multiple retention times The renamed TIC is described in the table below

Compound name as reported by the Compound name as renamed during data Affected sample laboratory validation

oleic acid unknown D05951

JNEWA160 Troy Mills LandflllData ValidationDecember 2004DV MemossD05939_svocsimwpd MetcalfA Eddy Inc

Ms Christine Clark Page 20 February 24 2005 Case 0251M SDG D05939

Please contact Ms Constance Lapite at (781) 224-6628 or at Constance lapite(am-ecom if you have any questions regarding this Tier II validation

Paula L DiMattei Data Validator

Deborah A Trwini ^mjrjat

Robert Shoemaker Project Chemist

bullgt pound^ampgtlt^ Constance D Lapite MampE RAC Lead Chemist

cc ^James Chow EPA Remedial Project Manager (DV memo and data summary tables) Karen Wedlock-Hunt MampE Project Manager (entire package) Robert Shoemaker Project Chemist (entire package) Troy Mills Landfill Project File WA No 160-RICO-019M (entire package)

Attachments ORDA Table I Recommendation Summary Table Table II Overall Evaluation of Data Table III Tentatively Identified Compound Summary Data Summary Tables Data Validation Worksheets PE Score Report Copy of non-CLP Analytical Method (MampE DAS Specification D-148) Copies of Telephone LogCommunications Forms Supporting Data for Reduced Payment Recommendations (not applicable) Copies of Field Sampling Notes (previously submitted) Copies of EPA-Approved Amendments not QAPjP or SAP (not applicable) CSF Completeness Evidence File Audit (DC-2 Form) DQO Summary Form

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DVMemossD05939_svocsim pd Metcatfamp Eddy Inc

REGION I EPA-NE ORGANIC REGIONAL DATA ASSESSMENT (ORDA)

CASE raquozjggtH _ SITE NAME TV

LAB NAME uoAlaquo Vlaquo- amp+ OF SAMPLESMATRIX

SDG Posirt_ VALIDATION CONTRACTOR

SOW CONTRACT p-rttll-- VALIDATORS NAME

EPA-NE DV TIER LEVEL JC_ DATE DP RECD BY EPA-NE

TPOPO ACTION _ FYI ^ DV COMPLETION DATE

ANALYTICAL DATA QUALITY SUMMARY tffpft^m t~

bullVGA SV-SM PestPCB 1 Preservation and Contractual Holding Times 2 GCMS GCECD Instrument Performance Check raquo 3 Initial Calibration laquo 4 Continuing Calibration o 5 Blanks ~ o 6 Surrogate Compounds raquo 7 Internal Standards o 8 Matrix SpikeMatrix Spike Duplicate ggt 9 Sensitivity Check 0 10 PE Samples-Accuracy Check 0 11 Target Compound Identification jpy 12 Compound Quantitation and Reported QLs o 13 Tentatively Identified Compounds o 14 Semivolatile CleanupPesticidePCB Cleanup ulaquor 15 Data Completeness 0 16 Overall Evaluation of Data laquo

o = Data had no problems or were qualified due to minor contractual problems m = Data were qualified due to major contractual problems z = Data were rejected as unusable due major contractual problems

ACTION ITEMS (z items)

AREAS OF CONCERN (m items)

COMMENTS

This form assesses the analytical data quality in terms of contractual compliance only It does not assess sampling errors andor non-contractual analytical issues that affect data quality

Check ACTION only if contractual defects resulted in reduced paymentdata rejection recommendations

Validator t ltiJSagt3gtlt -3 Date

INSTRUCTIONS ON REVERSE SIDE

1296

Table I Recommendation Summary

Soil Semivolatile Organic Analysis Troy Mills Landfill Superfund Site

Case0251M SDGD05939

Sample ID Matrix

D05945 SO

D05946 SO

D05947 SO (FD)

D05948 SO

D05949 SO

D05950 SO

D05951 SO

D05952 SO

D05953 SO (FD)

D05954 EB

EB shy Equipment Blank FD shy Field Duplicate SOshy Soil

Qualifier

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 11 13 14 15

2 Jl 3 4 7 8 9 10 13 15

A 2 jl 3 4 7 8 9 10 13 15

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 jl 3 4 7 8 9 10 13 15

A 2 3 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 Jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 13 15

^2 4 jl 2 3 5 6 7 12

A - Accept the data but qualify the positive results for benzaldehyde in samples D05945 D05946 D05949 D05950 D05951 and D05952 and for acetophenone in sample D05951 as (EB) due to equipment blank contamination

A2 - Accept the data but qualify the positive result for di-n-butylphthalate as nondetect (U) at the reported value due to laboratory method blank contamination

A5 - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to PE sample contamination

A - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to laboratory method blank contamination

J - Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde hexachlorocyclopentadiene 24shydmitrophenol 46-dmitro-2-methylphenol atrazine and pentachlorophenol due to initial calibration RSD exceedances

J2 Estimate (J) the positive result for di-n-butyl phthalate due to the initial calibration RSD exceedance

J3 Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde and 33-dichlorobenzidme in all samples for hexachlorobutadiene 4-mtrophenol and hexachlorobenzene m samples D05948 D05949 and D05953 for hexachlorocyclopentadiene m samples D05954 D05948 D05949 and D05953 and for 24shydimtrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 due to the continuing calibration D exceedances

J4 - Estimate (J) the positive results for di-n-butylphthalate in all soil samples due to continuing calibration exceedance

J5 - Estimate (UJ) the nondetect caprolactam result and raise the quantitation limit to 4 ugL (equivalent to the concentration of the high-level LFB) due to low low-level and high-level LFB recoveries This result may be biased low

J6 - Estimate (UJ) the nondetect results for 4-mtrophenol 46-dmitro-2-methylphenol and pentachlorophenol due to low low-level LFB recoveries These results may be biased low

J7 - Estimate (J) the positive result for di-n-butylphthalate due to high low-level and high-level LFB recoveries This result may be biased high

J8 - Estimate (UJ) the nondetect 24-dmitrophenol result and raise the quantitation limit to 800 ugKg (equivalent to the concentration of the high-level LFB and corrected for all preparation factors) due to low low-level and high-level LFB recoveries This result may be biased low

J9 - Estimate (UJ) the nondetect results for 24-dimethylphenol 4-mtrophenol 46-dimrro-2-methylphenol pentachlorophenol and 33-dichlorobenzidme due to low low-level LFB recoveries These results may be biased low

J10 - Estimate (UJ) the nondetect result 4-chIoroamlme due to low low-level and high-le el LFB recoveries This result may be biased low

J1 - Estimate (J) the positive result for benzo(b)fluoranthene due to high high-level LFB reco ery This result may be biased high

J12 - Estimate (UJ) the nondetect caprolactam result due to low LCS recovery This result may be biased low

J3 - Estimate (UJ) the nondetect benzaldehyde and 4-chloroamline results due to low LCS recoveries The results may be biased low

J14 - Estimate (J) the positive results for benzo(b)fluoranthene benzo(a)pyrene and mdeno(l23-cd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 due to high LCS recoveries The results may be biased high

J15 - Estimate (J) the positive results for the following compounds in the samples listed below due to uncertainty in the quantitation as a result of the exceeded ion abundance ration criteria

DOS 950 di-n-butylphthalate DOS 951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate mdeno(l23-cd)pyrene D05946 mdeno(l23-cd)pyrene D05947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate D05953 di-n-butylphthalate

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Page 20: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

Ms Christine Clark Page 20 February 24 2005 Case 0251M SDG D05939

Please contact Ms Constance Lapite at (781) 224-6628 or at Constance lapite(am-ecom if you have any questions regarding this Tier II validation

Paula L DiMattei Data Validator

Deborah A Trwini ^mjrjat

Robert Shoemaker Project Chemist

bullgt pound^ampgtlt^ Constance D Lapite MampE RAC Lead Chemist

cc ^James Chow EPA Remedial Project Manager (DV memo and data summary tables) Karen Wedlock-Hunt MampE Project Manager (entire package) Robert Shoemaker Project Chemist (entire package) Troy Mills Landfill Project File WA No 160-RICO-019M (entire package)

Attachments ORDA Table I Recommendation Summary Table Table II Overall Evaluation of Data Table III Tentatively Identified Compound Summary Data Summary Tables Data Validation Worksheets PE Score Report Copy of non-CLP Analytical Method (MampE DAS Specification D-148) Copies of Telephone LogCommunications Forms Supporting Data for Reduced Payment Recommendations (not applicable) Copies of Field Sampling Notes (previously submitted) Copies of EPA-Approved Amendments not QAPjP or SAP (not applicable) CSF Completeness Evidence File Audit (DC-2 Form) DQO Summary Form

J NEWA160 Troy Mills LandfillData ValidatwnDecember 2004DVMemossD05939_svocsim pd Metcatfamp Eddy Inc

REGION I EPA-NE ORGANIC REGIONAL DATA ASSESSMENT (ORDA)

CASE raquozjggtH _ SITE NAME TV

LAB NAME uoAlaquo Vlaquo- amp+ OF SAMPLESMATRIX

SDG Posirt_ VALIDATION CONTRACTOR

SOW CONTRACT p-rttll-- VALIDATORS NAME

EPA-NE DV TIER LEVEL JC_ DATE DP RECD BY EPA-NE

TPOPO ACTION _ FYI ^ DV COMPLETION DATE

ANALYTICAL DATA QUALITY SUMMARY tffpft^m t~

bullVGA SV-SM PestPCB 1 Preservation and Contractual Holding Times 2 GCMS GCECD Instrument Performance Check raquo 3 Initial Calibration laquo 4 Continuing Calibration o 5 Blanks ~ o 6 Surrogate Compounds raquo 7 Internal Standards o 8 Matrix SpikeMatrix Spike Duplicate ggt 9 Sensitivity Check 0 10 PE Samples-Accuracy Check 0 11 Target Compound Identification jpy 12 Compound Quantitation and Reported QLs o 13 Tentatively Identified Compounds o 14 Semivolatile CleanupPesticidePCB Cleanup ulaquor 15 Data Completeness 0 16 Overall Evaluation of Data laquo

o = Data had no problems or were qualified due to minor contractual problems m = Data were qualified due to major contractual problems z = Data were rejected as unusable due major contractual problems

ACTION ITEMS (z items)

AREAS OF CONCERN (m items)

COMMENTS

This form assesses the analytical data quality in terms of contractual compliance only It does not assess sampling errors andor non-contractual analytical issues that affect data quality

Check ACTION only if contractual defects resulted in reduced paymentdata rejection recommendations

Validator t ltiJSagt3gtlt -3 Date

INSTRUCTIONS ON REVERSE SIDE

1296

Table I Recommendation Summary

Soil Semivolatile Organic Analysis Troy Mills Landfill Superfund Site

Case0251M SDGD05939

Sample ID Matrix

D05945 SO

D05946 SO

D05947 SO (FD)

D05948 SO

D05949 SO

D05950 SO

D05951 SO

D05952 SO

D05953 SO (FD)

D05954 EB

EB shy Equipment Blank FD shy Field Duplicate SOshy Soil

Qualifier

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 11 13 14 15

2 Jl 3 4 7 8 9 10 13 15

A 2 jl 3 4 7 8 9 10 13 15

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 jl 3 4 7 8 9 10 13 15

A 2 3 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 Jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 13 15

^2 4 jl 2 3 5 6 7 12

A - Accept the data but qualify the positive results for benzaldehyde in samples D05945 D05946 D05949 D05950 D05951 and D05952 and for acetophenone in sample D05951 as (EB) due to equipment blank contamination

A2 - Accept the data but qualify the positive result for di-n-butylphthalate as nondetect (U) at the reported value due to laboratory method blank contamination

A5 - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to PE sample contamination

A - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to laboratory method blank contamination

J - Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde hexachlorocyclopentadiene 24shydmitrophenol 46-dmitro-2-methylphenol atrazine and pentachlorophenol due to initial calibration RSD exceedances

J2 Estimate (J) the positive result for di-n-butyl phthalate due to the initial calibration RSD exceedance

J3 Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde and 33-dichlorobenzidme in all samples for hexachlorobutadiene 4-mtrophenol and hexachlorobenzene m samples D05948 D05949 and D05953 for hexachlorocyclopentadiene m samples D05954 D05948 D05949 and D05953 and for 24shydimtrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 due to the continuing calibration D exceedances

J4 - Estimate (J) the positive results for di-n-butylphthalate in all soil samples due to continuing calibration exceedance

J5 - Estimate (UJ) the nondetect caprolactam result and raise the quantitation limit to 4 ugL (equivalent to the concentration of the high-level LFB) due to low low-level and high-level LFB recoveries This result may be biased low

J6 - Estimate (UJ) the nondetect results for 4-mtrophenol 46-dmitro-2-methylphenol and pentachlorophenol due to low low-level LFB recoveries These results may be biased low

J7 - Estimate (J) the positive result for di-n-butylphthalate due to high low-level and high-level LFB recoveries This result may be biased high

J8 - Estimate (UJ) the nondetect 24-dmitrophenol result and raise the quantitation limit to 800 ugKg (equivalent to the concentration of the high-level LFB and corrected for all preparation factors) due to low low-level and high-level LFB recoveries This result may be biased low

J9 - Estimate (UJ) the nondetect results for 24-dimethylphenol 4-mtrophenol 46-dimrro-2-methylphenol pentachlorophenol and 33-dichlorobenzidme due to low low-level LFB recoveries These results may be biased low

J10 - Estimate (UJ) the nondetect result 4-chIoroamlme due to low low-level and high-le el LFB recoveries This result may be biased low

J1 - Estimate (J) the positive result for benzo(b)fluoranthene due to high high-level LFB reco ery This result may be biased high

J12 - Estimate (UJ) the nondetect caprolactam result due to low LCS recovery This result may be biased low

J3 - Estimate (UJ) the nondetect benzaldehyde and 4-chloroamline results due to low LCS recoveries The results may be biased low

J14 - Estimate (J) the positive results for benzo(b)fluoranthene benzo(a)pyrene and mdeno(l23-cd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 due to high LCS recoveries The results may be biased high

J15 - Estimate (J) the positive results for the following compounds in the samples listed below due to uncertainty in the quantitation as a result of the exceeded ion abundance ration criteria

DOS 950 di-n-butylphthalate DOS 951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate mdeno(l23-cd)pyrene D05946 mdeno(l23-cd)pyrene D05947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate D05953 di-n-butylphthalate

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Page 21: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

REGION I EPA-NE ORGANIC REGIONAL DATA ASSESSMENT (ORDA)

CASE raquozjggtH _ SITE NAME TV

LAB NAME uoAlaquo Vlaquo- amp+ OF SAMPLESMATRIX

SDG Posirt_ VALIDATION CONTRACTOR

SOW CONTRACT p-rttll-- VALIDATORS NAME

EPA-NE DV TIER LEVEL JC_ DATE DP RECD BY EPA-NE

TPOPO ACTION _ FYI ^ DV COMPLETION DATE

ANALYTICAL DATA QUALITY SUMMARY tffpft^m t~

bullVGA SV-SM PestPCB 1 Preservation and Contractual Holding Times 2 GCMS GCECD Instrument Performance Check raquo 3 Initial Calibration laquo 4 Continuing Calibration o 5 Blanks ~ o 6 Surrogate Compounds raquo 7 Internal Standards o 8 Matrix SpikeMatrix Spike Duplicate ggt 9 Sensitivity Check 0 10 PE Samples-Accuracy Check 0 11 Target Compound Identification jpy 12 Compound Quantitation and Reported QLs o 13 Tentatively Identified Compounds o 14 Semivolatile CleanupPesticidePCB Cleanup ulaquor 15 Data Completeness 0 16 Overall Evaluation of Data laquo

o = Data had no problems or were qualified due to minor contractual problems m = Data were qualified due to major contractual problems z = Data were rejected as unusable due major contractual problems

ACTION ITEMS (z items)

AREAS OF CONCERN (m items)

COMMENTS

This form assesses the analytical data quality in terms of contractual compliance only It does not assess sampling errors andor non-contractual analytical issues that affect data quality

Check ACTION only if contractual defects resulted in reduced paymentdata rejection recommendations

Validator t ltiJSagt3gtlt -3 Date

INSTRUCTIONS ON REVERSE SIDE

1296

Table I Recommendation Summary

Soil Semivolatile Organic Analysis Troy Mills Landfill Superfund Site

Case0251M SDGD05939

Sample ID Matrix

D05945 SO

D05946 SO

D05947 SO (FD)

D05948 SO

D05949 SO

D05950 SO

D05951 SO

D05952 SO

D05953 SO (FD)

D05954 EB

EB shy Equipment Blank FD shy Field Duplicate SOshy Soil

Qualifier

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 11 13 14 15

2 Jl 3 4 7 8 9 10 13 15

A 2 jl 3 4 7 8 9 10 13 15

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 jl 3 4 7 8 9 10 13 15

A 2 3 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 Jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 13 15

^2 4 jl 2 3 5 6 7 12

A - Accept the data but qualify the positive results for benzaldehyde in samples D05945 D05946 D05949 D05950 D05951 and D05952 and for acetophenone in sample D05951 as (EB) due to equipment blank contamination

A2 - Accept the data but qualify the positive result for di-n-butylphthalate as nondetect (U) at the reported value due to laboratory method blank contamination

A5 - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to PE sample contamination

A - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to laboratory method blank contamination

J - Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde hexachlorocyclopentadiene 24shydmitrophenol 46-dmitro-2-methylphenol atrazine and pentachlorophenol due to initial calibration RSD exceedances

J2 Estimate (J) the positive result for di-n-butyl phthalate due to the initial calibration RSD exceedance

J3 Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde and 33-dichlorobenzidme in all samples for hexachlorobutadiene 4-mtrophenol and hexachlorobenzene m samples D05948 D05949 and D05953 for hexachlorocyclopentadiene m samples D05954 D05948 D05949 and D05953 and for 24shydimtrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 due to the continuing calibration D exceedances

J4 - Estimate (J) the positive results for di-n-butylphthalate in all soil samples due to continuing calibration exceedance

J5 - Estimate (UJ) the nondetect caprolactam result and raise the quantitation limit to 4 ugL (equivalent to the concentration of the high-level LFB) due to low low-level and high-level LFB recoveries This result may be biased low

J6 - Estimate (UJ) the nondetect results for 4-mtrophenol 46-dmitro-2-methylphenol and pentachlorophenol due to low low-level LFB recoveries These results may be biased low

J7 - Estimate (J) the positive result for di-n-butylphthalate due to high low-level and high-level LFB recoveries This result may be biased high

J8 - Estimate (UJ) the nondetect 24-dmitrophenol result and raise the quantitation limit to 800 ugKg (equivalent to the concentration of the high-level LFB and corrected for all preparation factors) due to low low-level and high-level LFB recoveries This result may be biased low

J9 - Estimate (UJ) the nondetect results for 24-dimethylphenol 4-mtrophenol 46-dimrro-2-methylphenol pentachlorophenol and 33-dichlorobenzidme due to low low-level LFB recoveries These results may be biased low

J10 - Estimate (UJ) the nondetect result 4-chIoroamlme due to low low-level and high-le el LFB recoveries This result may be biased low

J1 - Estimate (J) the positive result for benzo(b)fluoranthene due to high high-level LFB reco ery This result may be biased high

J12 - Estimate (UJ) the nondetect caprolactam result due to low LCS recovery This result may be biased low

J3 - Estimate (UJ) the nondetect benzaldehyde and 4-chloroamline results due to low LCS recoveries The results may be biased low

J14 - Estimate (J) the positive results for benzo(b)fluoranthene benzo(a)pyrene and mdeno(l23-cd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 due to high LCS recoveries The results may be biased high

J15 - Estimate (J) the positive results for the following compounds in the samples listed below due to uncertainty in the quantitation as a result of the exceeded ion abundance ration criteria

DOS 950 di-n-butylphthalate DOS 951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate mdeno(l23-cd)pyrene D05946 mdeno(l23-cd)pyrene D05947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate D05953 di-n-butylphthalate

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Page 22: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

Table I Recommendation Summary

Soil Semivolatile Organic Analysis Troy Mills Landfill Superfund Site

Case0251M SDGD05939

Sample ID Matrix

D05945 SO

D05946 SO

D05947 SO (FD)

D05948 SO

D05949 SO

D05950 SO

D05951 SO

D05952 SO

D05953 SO (FD)

D05954 EB

EB shy Equipment Blank FD shy Field Duplicate SOshy Soil

Qualifier

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 11 13 14 15

2 Jl 3 4 7 8 9 10 13 15

A 2 jl 3 4 7 8 9 10 13 15

A 1 2 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 jl 3 4 7 8 9 10 13 15

A 2 3 jl 3 4 7 8 9 10 11 13 14 15

A 1 2 3 Jl 3 4 7 8 9 10 11 13 14 15

A 2 jl 3 4 7 8 9 10 13 15

^2 4 jl 2 3 5 6 7 12

A - Accept the data but qualify the positive results for benzaldehyde in samples D05945 D05946 D05949 D05950 D05951 and D05952 and for acetophenone in sample D05951 as (EB) due to equipment blank contamination

A2 - Accept the data but qualify the positive result for di-n-butylphthalate as nondetect (U) at the reported value due to laboratory method blank contamination

A5 - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to PE sample contamination

A - Accept the data but qualify the positive result for bis(2-ethylhexyl)phthalate as nondetect (U) at the QL due to laboratory method blank contamination

J - Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde hexachlorocyclopentadiene 24shydmitrophenol 46-dmitro-2-methylphenol atrazine and pentachlorophenol due to initial calibration RSD exceedances

J2 Estimate (J) the positive result for di-n-butyl phthalate due to the initial calibration RSD exceedance

J3 Estimate (J) the positive and (UJ) the nondetect results for benzaldehyde and 33-dichlorobenzidme in all samples for hexachlorobutadiene 4-mtrophenol and hexachlorobenzene m samples D05948 D05949 and D05953 for hexachlorocyclopentadiene m samples D05954 D05948 D05949 and D05953 and for 24shydimtrophenol in samples D05950 D05951 D05952 D05945 D05946 and D05947 due to the continuing calibration D exceedances

J4 - Estimate (J) the positive results for di-n-butylphthalate in all soil samples due to continuing calibration exceedance

J5 - Estimate (UJ) the nondetect caprolactam result and raise the quantitation limit to 4 ugL (equivalent to the concentration of the high-level LFB) due to low low-level and high-level LFB recoveries This result may be biased low

J6 - Estimate (UJ) the nondetect results for 4-mtrophenol 46-dmitro-2-methylphenol and pentachlorophenol due to low low-level LFB recoveries These results may be biased low

J7 - Estimate (J) the positive result for di-n-butylphthalate due to high low-level and high-level LFB recoveries This result may be biased high

J8 - Estimate (UJ) the nondetect 24-dmitrophenol result and raise the quantitation limit to 800 ugKg (equivalent to the concentration of the high-level LFB and corrected for all preparation factors) due to low low-level and high-level LFB recoveries This result may be biased low

J9 - Estimate (UJ) the nondetect results for 24-dimethylphenol 4-mtrophenol 46-dimrro-2-methylphenol pentachlorophenol and 33-dichlorobenzidme due to low low-level LFB recoveries These results may be biased low

J10 - Estimate (UJ) the nondetect result 4-chIoroamlme due to low low-level and high-le el LFB recoveries This result may be biased low

J1 - Estimate (J) the positive result for benzo(b)fluoranthene due to high high-level LFB reco ery This result may be biased high

J12 - Estimate (UJ) the nondetect caprolactam result due to low LCS recovery This result may be biased low

J3 - Estimate (UJ) the nondetect benzaldehyde and 4-chloroamline results due to low LCS recoveries The results may be biased low

J14 - Estimate (J) the positive results for benzo(b)fluoranthene benzo(a)pyrene and mdeno(l23-cd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 due to high LCS recoveries The results may be biased high

J15 - Estimate (J) the positive results for the following compounds in the samples listed below due to uncertainty in the quantitation as a result of the exceeded ion abundance ration criteria

DOS 950 di-n-butylphthalate DOS 951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate mdeno(l23-cd)pyrene D05946 mdeno(l23-cd)pyrene D05947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate D05953 di-n-butylphthalate

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Page 23: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

J5 - Estimate (UJ) the nondetect caprolactam result and raise the quantitation limit to 4 ugL (equivalent to the concentration of the high-level LFB) due to low low-level and high-level LFB recoveries This result may be biased low

J6 - Estimate (UJ) the nondetect results for 4-mtrophenol 46-dmitro-2-methylphenol and pentachlorophenol due to low low-level LFB recoveries These results may be biased low

J7 - Estimate (J) the positive result for di-n-butylphthalate due to high low-level and high-level LFB recoveries This result may be biased high

J8 - Estimate (UJ) the nondetect 24-dmitrophenol result and raise the quantitation limit to 800 ugKg (equivalent to the concentration of the high-level LFB and corrected for all preparation factors) due to low low-level and high-level LFB recoveries This result may be biased low

J9 - Estimate (UJ) the nondetect results for 24-dimethylphenol 4-mtrophenol 46-dimrro-2-methylphenol pentachlorophenol and 33-dichlorobenzidme due to low low-level LFB recoveries These results may be biased low

J10 - Estimate (UJ) the nondetect result 4-chIoroamlme due to low low-level and high-le el LFB recoveries This result may be biased low

J1 - Estimate (J) the positive result for benzo(b)fluoranthene due to high high-level LFB reco ery This result may be biased high

J12 - Estimate (UJ) the nondetect caprolactam result due to low LCS recovery This result may be biased low

J3 - Estimate (UJ) the nondetect benzaldehyde and 4-chloroamline results due to low LCS recoveries The results may be biased low

J14 - Estimate (J) the positive results for benzo(b)fluoranthene benzo(a)pyrene and mdeno(l23-cd)pyrene in samples D05951 D05952 D05945 D05946 and D05949 due to high LCS recoveries The results may be biased high

J15 - Estimate (J) the positive results for the following compounds in the samples listed below due to uncertainty in the quantitation as a result of the exceeded ion abundance ration criteria

DOS 950 di-n-butylphthalate DOS 951 di-n-butylphthalate benzo(a)pyrene D05952 di-n-butylphthalate benzo(a)pyrene D05945 di-n-butylphthalate mdeno(l23-cd)pyrene D05946 mdeno(l23-cd)pyrene D05947 di-n-butylphthalate D05948 di-n-butylphthalate D05949 di-n-butylphthalate D05953 di-n-butylphthalate

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Page 24: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

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Page 27: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

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Page 28: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

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t bull m O1shyo o o _ poundj lt amp So laquo-bull ^ Mg DO

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Page 35: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

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Page 38: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

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Page 40: m-c < oniTroy Mills Landfill Superfund Site, Troy, New Hampshire Tier II Organic Data Validation Semivolatiles: 9/Soils/ D05945 DOS946, D05947, , D05948 DOS949, D05950, …

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