surveillance and monitoring branch

STANDARD OPERATING PROCEDURE

Title: Attachment 2 - CLP Data Assessment Checklist(GC and GC/MS Analyses)

Page of

Date:SFP - 5 19S6Number: HW-4Revision:

SURVEILLANCE AND MONITORING BRANCH REVIEW

Project Name/Site :__H_

Case Number; ? 3 ?D Q

E Lt

Type Investigation (Circle One): CRemediall Site Other

Contract Mo.:

Laboratory ; L

Sample Identification Numbers:

Aqueous:_ _ __________

-/ "ZtuW ^3

Superfund Account No.:_

Comments:

Oo

vo00

STAN 5 C ATING PROCEDURE s 5 of 32

Date: SEP • 'J '9-5^ Number: HW-4Title: Attachment 1 - CLP Data Assessment Checklist Revision:

(GC and GC/MS Analysis)

CONTRACTOR AND MONITORING MANAGEMENT BRANCH REVIEW

PART I: Contractor and Preliminary Review

1.0 Data Completeness and Deliverables TJ6S NO N/A

1.1 Are any deliverables missing? __ I__1 *

1.2 Has FIT Preliminary Review included with package? t__1 __ J^

1.3 Was SMO CCS checklist included with package? I__] __ _i£L

CONTRACTOR ACTION: If incomplete, list any missing dataon the Missing Data Tracking Form(Attachment 3).

I. COYER LETTER/NARRATIVE

2.0 Cover Letter/Case Narrative

2.1 Is the Narrative or Cover Letter present? t__.] __ __•-*.—--2.2 Are the following items contained in the Narrative

or Cover Letter:

a Case Number and/or SAS Number [__1 __ ——

b. Contract Number [__] __ ——

II. QC SCMMART

3.0 Surrogate Percent Recovery Summaries (Form II)

* 3.1 Are the Surrogate Percent Recovery Summaries presentfor each of the following matrix:

a. Hater (__1 —— -i— 3K

b. Soil t__1 —— ie^Lo

• 3.2 Are all the samples listed on the Surrogate Percent ^Recovery Summaries for each of the following matrix:

a. Hater I__1 —— —— to./

b. Soil I__1 ——

STANF ^ 0' \TING PROCEDURE ' » 6 of 32

Date: SEP - 5 1936Title: Attachment 1 - CLP Data Assessment Checklist Number: HW-4

(GC and GC/HS Analysis) Part I: Revision:^- Contractor and Preliminary Review

YES NO N/A

* 3.3 Were outliers marked correctly with an asterisk? [__] __ \S

CONTRACTOR ACTION: Circle all outliers in red.

* 3.4 Were two or more BN surrogates outside of contract specifications /(or one surrogate less than 10% recovery) for any samples? __ [__1 __

Blanks? __ t__1 iX

If yes, were samples reanalyzed? [___] __ Y

Were blanks reanalyzed? [__] __ S

MMB ACTION: If initial analysis and reanalysis both havetwo or more surrogates outside of contractspecifications (or one surrogate less than 10%recovery) for samples or blanks, reject allquantitation results, including detection limits.

fitf* 3-5 Were two. more acid surrogates outside of contract specifications *(or one surrogate less than 10% recovery) for any samples? __ [_J __

Blanks? __ t__1 j^L.

If yes, were samples reanalyzed? [__] __ __

Were blanks reanalyzed? [__1 __ __

MMB ACTION: If initial analysis and reanalysis both havetwo or more surrogates outside of contractspecifications (or one surrogate less than 10%recovery) for samples or blanks, reject allquantitation results, including detection limits.

* 3.6 Was one or more VOA surrogates outside of contract /specifications for any samples? .__ t__J *

Blanks? __ I__1 ±/.

If yes, were samples reanalyzed? [___1 __ */

Were blanks reanalyzed? t__J __ J__«.

MMB ACTION: If initial analysis and reanalysis both haveone or more surrogates outside of contract *••specifications (or one surrogate less than 10% orecovery) for samples or blanks, reject all °quantitation results, including detection limits.

STANL Ol iTING PROCKDORB of 32

'••tie: Attachment 1 - CLP Data Assessaent Checklist(GC and GC/MS Analysis) Part Z:Contractor and Preliminary Review

Date: SF? - = 1226Number: HH-4Revision :

* 3.7 Was pesticides surrogate outside of contract specifi-cations for any samples?

Blanks?

MNB ACTION: If yes, for saaples use professional judg-ment to determine acceptability of data.

4.0 Matrix Spikes

4.1 Is the Matrix Spike Duplicate/Recovery Form Present(Form III)?

4.2 Here matrix spikes analyzed at the required frequencyfor: Hater?

4.2.1 For each set in a case or for every 20 samples isone sample spiked in duplicate?

4.3 Form III

4.3.1 How many spikes are outside of recovery limits?

VOA's?

B/N?

Acids?

Pesticides?

PCBs?

4.3.2 How many RPD's for matrix spike and matrix spikeduplicates are outside of accepted limits?

VOA'S?

B/N?

Acids?

Pesticides?

PCBs?

YJB NO N/A

f\JLoCt<A(A AiM\£J} k

i*

Matrix '• f,sl-^MW^^^^^^B •• M^^^™*™

fJ/ft i out of 10

A///3 t out of 12

K//fi i out of 10

out of 12

N/A

Matrix

i out of 5

» of 6

N/A too

STAND* OP .TING PROCEDURE Pi 9 Of 32

Date: SFP • 5 1986*vcle: Attachment 1 - CLP Data Assessment Checklist Number: HW-4

^ (GC and GC/MS Analysis) Part I: Revision:Contractor and Preliminary Review

YES NO N/A

* 6.2 Do any field/trip blanks have positive results for:VOA's? __ t__1

B/N? __ t__1

Acids? __ [__1 ^

Pesticides? __ [__1

PCBs? __ [__1

CONTRACTOR ACTION: Prepare a list of the samples associatedwith each of the contaminated and/ormissing method blanks (attach a separatesheet).

MMB ACTION: For common VOA blank contaminants found (e.g.methylene chloride, acetone, toluene and 2-butanone)reject (red-line) all associated positive resultspresent at less than 10 times the blank contami-nant levels; for all other contaminants reject

*-—- (red-line) when all associated positive resultsare present at less than 5 times the blank conta-minant levels. Do not reject any values reportedwith a "U" (detection limit values).

Blanks for B/N/Aa and pesticides/PCBs must containless than 5X the CRDL of any phthalate ester andless than the CRDL of any other MSL compound.

7.0 GC/MS Tuning and Mass Calibration Forms (Form V)

7.1 Are the GC/MS Tuning and Mass Calibration forms presentfor the following:

7.1.1 Bromofluorobenzene (BFB) l__J __

7.1.2 Decaf1uorotriphenylphosphine (DFTPP) I__1 __

CONTRACTOR ACTION: List any missing GC/MS Tuning and Mas*Calibration Form on the Missing DataTracking Form.

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STAND ' 0T \TING PROCEDURE r 11 of 32

.. , Datas SFP • 5 1986Title: Attachment 1 - CLP Data Assessment Checklist Number: HW-4

(GC and GC/MS Analysis) Part I: Revision:_ Contractor and Preliminary Review

YES NO N/A

CONTRACTOR ACTION: If no, please list the missingspectrum and listings on HissingData Tracking Form.

7.2.5 Are there any transcription errors in going frommass lists to the GC/MS Tuning and Calibrationforms? (Check 10% of values) __ [__] __

7.2.6 Eave the appropriate number of S M MM figures(3) been reported? (Check 10% of data) [__] __ __

CONTRACTOR ACTION: If no, make necessary corrections.

7.2.7 Are there any calculation errors in the tuningratios? (For example, the ratios of M/Z 199/198and 443/442 for DFT*P.) Check 10% of the values

BFB (VOAs)? __ [__] __

DFTPP (NVOAs)? __ C__] __

CONTRACTOR ACTION: Recalculate, make necessarycorrections.

8.0 Is the Cross Reference Table present? [__] __ __

III SAMPLE DATA

*9.0 Are the Traffic Report Forms present for all samples? [__] __ _UC

CONTRACTOR ACTION: List missing Traffic Reports on MissingData Tracking Form.

10.0 Organic Analysis Data

• 10.1 Are the foui- (4) 0»ganla Xi>oijets Omle Blunts•MM: Pesticides and Tentatively tis«itfi«a UJIapuiiuAe)present for each of the following.

a. Samples and/or fractions as appropriate [ \S\ __ ——

b. Matrix spikes and matrix spite duplicate* [ i^l __ —— ^X »

c. Blanks tJ_J __ —— oo

CONTRACTOR ACTION: List Missing Data Sheets on Missing *~*Data Tracking Form.

STAND. Of HNG PROCEDURE

Title: Attachment 1 - CLP Data Assessment Checklist(GC and GC/MS Analysis) Part I:Contractor and Preliminary Review

P. 13 of 32

Date: SFP - 5 198SNumber: HW-4Revision:

YES NO N/A

CONTRACTOR ACTION: If no, list the missing numbers onthe Missing Data Tracking Form.

12.0 Holding Times

* 12.1 Have any holding times been exceeded for:

a. Volatiles

Aqueous (7 days)?

Soil/Sediment (10 days)?

b.-NVOA's and Pesticides/PCBs:

Aqueous (5 days to extraction, 40 days afterextraction)

Soil/Sediment (10 days to extraction, 40 daysafter extraction)

CONTRACTOR ACTION: List the samples and their respective~" fractions with exceedances below.

(Attach additional sheets ifnecessary.)

Table of Holding Time Exceedances

SampleSample Matrix Fraction(s)

[__]

t__1

du«*

DateSampled

Date LabReceived

DateExtracted

DateAnalyzed

MMB ACTION: If these holding times are exceeded, red-line all values on the data sheet(including detection limits) indicatingrejection.

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fSTAND; as TING PROCEDURE p is of 32

Date: ™ ' 5 **Title: Attachment 1 - CLP Data Assessment Checklist Number: HW-4

(GC and GC/MS Analysis) Part I: Revision:-—- Contractor and Preliminary Review

res NO N/A

15.3 Are the GC Screen Chromatograms present for thesamples and blanks? [__1

CONTRACTOR ACTION: List any missing data on the MissingData Tracking Form.

16.0 Standards Data (GC/MS)

* 16.1 Are the Reconstructed Ion Chromatograms, Data SystemPrintouts (Quant, list), and work sheet calculationspresent for the following:

a. Semi-volatiles (initial and continuing calibrations) [__]

b. Volatiles (initial and continuing calibrations) [__]

CONTRACTOR ACTION: List missing RICs, Quant, lists andwork sheet calculations on MissingData Tracking Form.

_ .6.2 GC/MS Initial Calibration Data Sheets (Form VI)

* 16.2.1 Are the Initial Calibration Data Sheets present andcompletely filled out for all compounds for thefollowing fractions:

a. Semi-volatiles [__1

b. Volatiles [__J

CONTRACTOR ACTION: List missing RICs, Quant, listsand work sheet calculations onMissing Data Tracking Form.

* 16.3 RF Stability

* 16.3.1 Are response factors stable over the concentrationrange of the calibration? (RSD for non-CCC com-pounds <50%) [__1

CONTRACTOR ACTION: Circle all outliers in red.oo

K>Ovo

STAND; >PERATING PROCEDURE page 17 of 32Date: SFP - 5 1986

Title: Attachment 1 - CLP Data Assessment Checklist Number: HW-4(GC and GC/MS Analysis) Part I: Revision:

"~-." Contractor and Preliminary Review

YES NO N/A

* 17.3 Are the volatile data within the specified limits /presented on Form VT? [__] __ *

* 17.4 Are the Base/Neutral data within the specified limits xpresented in Form VI? [__] __ _•_

* 17.5 Are the Acid data within the specified limitspresented in Form VI? [__] __ iX


MMB ACTION: For the volatile fraction, if the combinedtotal of CCC's and SPCC's outside theacceptance limits is 5 or greater, rejectthe entire fraction of all samples run.For the acid fraction, the above applieswith a combined total of 3 or greater SPCC'sand CCC's. For the base/neutral fraction,the above applies with a combined total of5 SPCC's and CCC's. If there are notenough compounds outside of acceptance to

^_ reject entire fractions, then reject thoseindividual compounds for samples run within12 hours of the calibration which have eitherCCC or SPCC values out of acceptance.

18.0 GC/MS Continuing Calibration

18.1 Calibration Check Sheets (Form VII)

18.1.1 Are the Calibration Check Sheets present andcompletely filled out for all compounds for thefollowing fractions:

a. semi-volatiles t__1 _ _ ——

b. volatile* I__1 —— ——

CONTRACTOR ACTION: List missing calibration check 3sheets on Missing Data Tracking *Form.

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STAND. OPERATING PROCEDURE Page 19 of 32

Dates S F P - 5 1 9 8 6Title: Attachment 1 - CLP Data Assessment Checklist Number: HW-4

(GC and GC/MS Analysis) Part Z: Revision:^. Contractor and Preliminary Review

YES NO N/A

• 18.5.2 How many CCC' s have a greater than 00» HOD for responsefactors: Number of Instrument

Outliers ID/Date

VOAs?

Base/Neutrals?

Acids?

CONTRACTOR ACTION: Circle all outliers in red. Listbelow the dates of continuing cali-brations with outliers, and theassociated samples.

MMB ACTION: For the volatile fraction, if the combinedtotal of CCC's and SPCC's outside theacceptance limits is 5 or greater, rejectthe entire fraction of all samples run.For the acid fraction, the above applieswith a combined total of 3 or greater SPCC'sand CCC's. For the base/neutral fraction,the above applies with a combined total of5 SPCC's and CCC's. If there are notenough compounds outside of acceptance toreject entire fractions, then reject thoseindividual compounds for samples run within12 hoars of the calibration which have eitherCCC or SPCC values out of acceptance.

18.5.3 Are any transcription/calculation errors found inreporting %D values between initial calibration RPsand continuing calibration RFs? __ t __ 1

CONTRACTOR ACTION: Circle errors in red and make anynecessary corrections

Ul

' STAND* OPERATING PROCEDURE Page 21 of 32

. ' D«te: SFP - 5 1986• Title: Attachment 1 - CLP Data Assessment Checklist Number: HW-4

(GC and GC/MS Analysis) Part I: Revision:Contractor and Preliminary Review

YKS NO N/A

20.0 GC Performance and Calibration

* 20.1 DOT Retention Time check - Z> DOT retention time onpacked columns greater than or equal to 12 minutes? /(Form IX) [ j/3 __ __

CONTRACTOR ACTION: Circle DOT retention times on packedcolumns <12 minutes in red.

20.2 Analytical Sequence - Form VIII

20.2.1 Have all standards been run within required timeframes? [ __ ] __ __

MMB ACTION: If no/ use professional judgment todetermine severity of effects ondata, and accept or reject the dataaccordingly.

20.2.2 Has the proper sequence of standards and samplesbeen followed? [ __ ] __ __

MMB ACTION: If no, use professional judgment to""•"' determine severity of effects on data,

and accept or reject the dataaccordingly.

* 20.3 DDT/Endrin Degradation Check (Form VIII) - Has the /total percent breakdown for DDT/Endrin exceeded 20%? __ Li£J ——


MMB ACTION:

1) If DDT breakdown is greater than 20%:

a. all quantitative results for DOT should berejected (red-lined);

b. qualitative and quantitative results for ODDand DDE should be rejected; and,

c. all other pesticides/PCB results should beinspected closely for acceptability.

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STAND OPERATING PROCEDURE Page 23 of 32

„,. , Date: $EP - 5 1986Title: Attachment 1 - CLP Data Assessment Checklist Number: HW-4

(GC and GC/MS Analysis) Part I: Revision:Contractor and Preliminary Review

YKS NO N/A


MMB ACTION: If no, all associated positive resultsshould be rejected (red-lined).

20.6 Continuing Calibration

20.6.1 Are the alternating standards' calibration factorswithin 15% of each other and within 15% of resultsat beginning of the 12 hour period (20% for bothof above for non-quantitation mix)?

Quantitation Mix I__1 __ __

Non-Quantitative Mix [__] __ __

20.6.2 If no, were analyses repeated as required bycontract? [__] __ __

20.6.3 Were repeats within contract limits? [__J __ __


MMB ACTION: If quantitation standards were outsideof contract limits, reject all associatedpositive results. If non-quantitationstandards were outside of contract limits,use professional judgment to determineacceptability of data.

21.0 Package Copies

21.1 Are all the xeroxing of readable quality? [__J __ ——

CONTRACTOR ACTION: If not, list appropriate page numberson Missing Data Tracking Form.

ro

STAND; OPERATING PROCBOURB

Title: Attachment 1 - CLP Data Assessment Checklist(GC and GC/MS Analysis)PART II: MMB Review

Page 24 of 32

Date: SFP - 5 1986Number: HW-4Revision:

>•*——Type of Review (Circle One): Total (T); Targeted Element (TB)j Significant Element USE),If TE Review, which samples were initially chosen? JT£" £HJ^LUD Jf, DCT^OJlLL/Tftl fxJj Jfi

1.0 Data Completeness and Deliverables

1.1 Have all the missing deliverables been received andadded to the data package.

MKB ACTION: Note any missing data and its effect onreviewing the package under conclusionssection contract problems/non-compliance.

I CASE NARRATIVE

2.0 Cover Letter/Case Narrative

2.1 Are the Case Number and/or SAS Number, ContractNumber and Superfund Account Number correct?

YES NO N/A

II QC SUMMARY RESULTS

#3.0 Surrogate Spikes

3.1 Here any transcription/calculation errors foundbetween raw data and Surrogate Per Cent RecoveryForm?

MMB ACTION: Make any necessary corrections, andnote errors under Conclusions.

* 3.2 Were the appropriate actions designated MMB ACTIONParagraph 3 in Part I taken?

4.0 Matrix Spikes

* 4.1 Has Matrix Spike data used in conjunction with otherQC criteria in determining the acceptability ofreported data? L_J —

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K>M00

STAND; OPERATING PROCEDURE

Title: Attachment 1 - CLP Data Assessment Checklist(GC and GC/HS Analysis) Part I:PART II: MKB Review

5.0 Blanks

* 5.1 Chromatography - review the blank raw data - chromato-grams, RICs, quan reports or data system printouts andspectra. Is chromatographic performance for eachinstrument acceptable?

MMB ACTION: Use professional judgment to determinethe extent of the problem.

6.0 Contamination (Reagent Blank Summary - Form IV)

6.1 Check transcription and'recalculate 10% of hits wherepossible. Are there any errors?

MMB ACTION: Make corrections where necessary.

7.0 GC/MS Tuning and Mass Calibration

• 7.1 Are the spectra of the mass calibration compoundsacceptable?

^- MMB ACTION: Use professional judgment to determinewhether associated data should beaccepted, qualified, or rejected.

8.0 Cross Reference Table

8.1 If a cross-reference table is missing, are the sampleruns clearly labeled and not confusing to the reviewer?

Page 25 of 32

DM, SFP ' 5Number: HH-4Revision:

YES NO N/A

t__1

III SAMPLE DATA PACKAGE

9.0 Traffic Report

9.1 Do the Traffic Reports indicate any problems withsample receipt, condition of samples or specialnotations affecting the quality of the data?

MMB ACTION: Use professional judgment inevaluating any effect on the qualityof the data.

vo

STANDA. OPERATING PROCEDURE Page 27 of 32

^ SFP - 5 1986Title: Attachment 1 - CLP Data Assessoent Checklist Number: HW-4

(GC and GC/MS Analysis) Revision:PART II: MMB Review

11.1.5 Check 10% of all positive values. Were any errorsfound in: Transcriptions?

Yjs NO N/A

Calculations? __ I__1

MMB ACTION: Make any necessary corrections andnote errors under Conclusions.

11.2 Tentative ID - Non-HSL Compounds

11.2.1 Are all ions present in the reference mass spectrumwith a relative intensity greater than 10% presentin the sample mass spectrum? [__] __

11.2.2 Do relative intensities specified above agree with-in 20% between the sample and reference spectra? [__1 __

11.2.3 Are molecular ions present in reference spectrumpresent in sample spectrum? [__] __

11.2.4 Are all non-HSL compounds classified as tentativelyidentified reported with estimated quantitation

-—- and detection limits? [__1 __

MMB ACTION: Use professional judgment to determineacceptability of data. If data isconsidered to be unacceptable. thetentative ID should be changed to"unknown".

.2.0 Holding Times

* 12.1 Have all associated sample data which have exceededholding times been red-lined on the data sheet (in-cluding detection limits) indicating rejection? [__] __ __£.

.3.0 GC Evaluation

* 13.1 Do chromatograms and data system printouts confirmretention times, retention time windows, and re- sported values (Form I)? t_y\ __ ——

* 13.2 Do positive identifications have proper dissimilar /column analysis? LJ J __ ——

toto

STANt OPERATING PROCEDURE Page 29 of 32

Dat.: SFP • 5 1986Title: Attachment 1 - OJ? Data Assessment Checklist »»ber: HW-4

(GC and OC/MS Analysis) Revision:_.- PART II: NMB Review

YES HO N/A

16.0 GC/MS Initial Calibration

* 16.1 If initial calibration raw data is provided, is chroma- stographic performance acceptable for each instrument? [__] __ *

MMB ACTION: List exceptions under Conclusions. Dseprofessional judgment to determine effecton data. Acceptance or rejection shouldnot be based solely on this factor, butshould be determined in conjunction withother criteria.

16.2 RF Stability

* 16.2.1 Are response factors stable over the concentrationrange of the calibration? (RSD for non-CCC compounds /<50%) [__1 __ _±_

MMB ACTION: Use professional judgment to determineeffect on data. Acceptance or rejectionshould not be based solely on this factor,but should be determined in conjuctionwith other criteria.

16.3 Transcription and Calculation

16.3.1 Are any transcription/calculation errors found inthe reporting of response factors (RF) for SPCCs?(Check 10% of values) __ I__1 ——

MMB ACTION: Make any necessary corrections. Ifchanges were made, see Action under16.2.1.

17.0 Check Compounds - (SFCC and CCC)

* 17.1 Have all associated sample data which have exceeded thecombined SPCC and CCC's (see NMB Action Section 17.4Part I) been red-lined on the data sheet indicatingrejection? I__1 ——

I

STAHDA. OPERATING PROCEDURE P*9« 31 of 32

' 5 1986oat.:Title: Attachment 1 - CLP Data Assessment Checklist Ht»ber: HW-4

(GC and GC/MS Analysis) Revision:— PART II: HUB Review

YES MO N/A

20.4 Were calibration factors calculated and transposedcorrectly (check 10% of calibration factors)? [__1 __ __

MMB ACTION: Make any necessary corrections, andreapply criteria in 20.3 and 20.4above. Note errors under Conclusions.

20.5 Do chromatograms and printouts verify data as re-ported on the Pesticide Evaluation StandardsSummary (Form VTII)? I__1 __ ——

20.6 Were calibration factors calculated and trans-posed correctly (check 10% of calibration factors)? [__1 __ ——

MMB ACTION: Make any necessary corrections, andreapply criteria in 20.5 and 20.6above. Note errors under Conclusions.

N)K>Ul

STA> 0 OPERATING PROCEDURE Page 32 of 32

Date iT. . m^ Number: HH-4Title: Attachment 2 - CLP Data Assessment Checklist Revision:

(GC and GC/MS Analysis)

21.0 Conclusions: (NOTE: Reviewers must red-line unacceptable data on sample datasheets; red-line data does not imply the compound is not present) Only the 1MBreviewer has the authority to red-line unacceptable data.

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21.2 Contract Problems/Non-compliance

21.3 Contractor Review Problems/Errors

Reviewer's Signature: ^ln^>u nfy. rtJktLA^j ________ Patmi 2//7/P7 ^

Verified By: s^jh~iSt-*^ fost<~^______________ Date: "f/fl/l/ ti

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