addendum to sampling and analysis plan · for this residential well samplin roungd (roun 6)d , it...

EPA Contract No. 68-W9-0036 ^r Q EPA Work Assignment No. 18-ILA5 /

EPA Project Officer: Diane Kelley EPA Remedial Project Manager: David Newton

ADDENDUM TO SAMPLING AND ANALYSIS PLAN

FOR

REMEDIAL INVESTIGATION/ FEASIBILITY STUDY

Rose Hill Regional Landfill Superfund Site South Kingstown, Rhode Island

September 1993

Prepared by:

An Air & Water Technologies Company

TABLE OF CONTENTS

page

1.0 INTRODUCTION 1

2.0 SAMPLING EQUIPMENT AND PROCEDURES 5

2.1 EQUIPMENT 5 2.2 SAMPLING PROCEDURE 5 2.3 DOCUMENTATION 6

3.0 SAMPLE HANDLING FOR ANALYSIS 7

3.1 SAMPLE PRESERVATION 7

3.1.1. Volatile Organic Analysis 7 3.1.2 Metals Analyses 9 3.1.3 Cyanide Analyses 9

3.2 SAMPLE CUSTODY 10

3.3. DOCUMENTATION 10

3.4 FIELD TESTING EQUIPMENT 10

4.0 SPECIAL ANALYTICAL SERVICES 11

TABLES

TABLE 1

TABLE 2

TABLE 3

RESIDENTIAL WELLS AND ANALYSES

NUMBER OF SAMPLES AND ANALYSES

SAMPLE CONTAINERS, PRESERVATION REQUIREMENTS, AND HOLDING TIMES FOR AQUEOUS SAMPLES

PAGE

3

4

FIGURES

FIGURE 1 RESIDENTIAL WELL LOCATIONS

11

1.0 INTRODUCTION

The purpose of this addendum to the Sampling and Analysis Plan for the Rose Hill Regional

Landfill Superfund Site is to collect tap water samples from eight residential wells to confirm

sampling results of previous sampling rounds conducted as part of the Remedial Investigation

(RI). Antimony was detected in some residential wells during the RI field investigation, which

was completed in April of 1992. On July 17, 1992, the Maximum Contaminant Level (MCL)

for antimony was lowered to 6 /*g/L. The contract required detection limit (CRQL) for

antimony of 60 jig/L, using the Routine Analytical Services (RAS) method of inductively

coupled plasma (ICP), exceeds the MCL of 6 fj.g/L. Therefore, a Special Analytical Services

(SAS) method for low concentration of antimony was written with a CRQL of 5 jtg/L. Thus,

results of this sampling round will be used to determine if the concentration of antimony exceeds

the MCL in any of the residential wells. Antimony results from the RAS analyses (ICP) will

be used for comparison purposes with previous sampling rounds. In addition, since volatile

organics were detected in residential well, RES #7, and a water soluble organic compound was

detected in residential well, RES #8, those wells will also be sampled.

For this residential well sampling round (Round 6), it is planned that tap water will be collected

from eight of the residential wells shown on Figure 1. Seven residential wells (RES #1, #5, #6,

#7, #8, #9, and #10) will be sampled for Target Analyte List (TAL) metals (filtered and

unfiltered), and antimony (filtered and unfiltered); one residential well (RES #7) for volatile

organics (524.2); one residential well (RES #8) for water soluble organics; and one residential

well RES #11 for volatile organics (524.2), Target Compound List (TCL) semi-volatile organics,

TCL pesticides/PCBs, water soluble organics, cyanide, TAL metals (filtered and unfiltered), and

antimony (filtered and unfiltered) as described in Table 1. The number of samples to be

collected and the associated quality control (QC) samples are described in Table 2.

For residents identified as using a filtration system, well samples will be collected following the

filtration system. Wells will be sampled via a spigot or tap. The type of filtration system in

use, if any, will be documented in the field log book.

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2.0 SAMPLING EQUIPMENT AND PROCEDURES

2.1 EQUIPMENT

The sampling equipment to be used is a follows:

• Sample containers

• Required Sample Preservatives

• Disposable polystyrene cups for collection of field monitoring aliquot

• pH meter

• Conductivity meter

• Thermometer

• Standard pH buffer solutions of pH 4.0, 7.0 and 10.0

• KC1 calibration standard solutions

• Filtration apparatus, 0.45 micron filters, glass fiber prefilter

• HPLC water for collection of all QC samples

2.2 SAMPLING PROCEDURE

Homeowners will be contacted for permission to sample and their requests with respect to the

sampling schedule will be adhered to, as much as possible. A well sampling worksheet will be

completed for each well sampled.

The following procedures will be used for well sampling.

1) The wells will be purged for 15 minutes prior to sampling at a flow rate of approximately 5 gallons per minute.

2) During purging, an aliquot will be collected every 5 minutes for pH, temperature and conductivity measurements. Purging will continue, until

pH, temperature, and conductivity readings have stabilized to within 10%. However, purging time will not exceed 30 minutes.

3) Obtain water samples immediately after purging, by filling sample containers directly from the spigot or tap.

4) Samples collected for volatile organics must contain no air bubbles in the VOA vial after it is capped; ensure this by turning the vial upside down and tapping it lightly. Filter dissolved metals and antimony using decontaminated filtration apparatus (see Section 9 of the Final Field Sampling Plan of May 1991 for Decontamination Procedures). Fill all other containers to the shoulder.

5) Immediately label and tag, preserve if necessary, ice, and log samples into a field log book.

6) Collect final sample aliquot in a disposable container and immediately measure and record the pH, temperature, and conductivity of the sample.

7) Use HPLC water for the collection of all trip blanks, bottle blanks, and equipment blanks.

Note: Tap water for equipment decontamination will be procured from the hydrant at the corner of Rose Hill Road and the Site owner's driveway (this was the source of tap water for the previous sampling rounds).

2.3 DOCUMENTATION

Include at a minimum the following information on well sampling sheets or log book. Refer to

Section 3.3 for more information regarding documentation.

• weather, date, and time of sample collection

• description of sample location (outside spigot, inside tap, etc.)

• temperature, pH, and conductivity readings

• time well purged and flow rate

• description of filtration apparatus, if present

3.0 SAMPLE HANDLING FOR ANALYSIS

3.1 SAMPLE PRESERVATION

All samples will be preserved immediately following collection. Table 3 summarizes the sample

containers, preservation requirements, and holding times for the aqueous samples based on the

analytical methods being performed. The following procedures will be used for testing and

preserving samples collected in the field for volatile organics, metals, and cyanide analyses.

These procedures will also be applied to all aqueous QC samples that are generated in the field.

3.1.1 Volatile Organic Analyses

At each sampling location, 40 ml of the aqueous sample is pretested for the presence of

oxidizing agents and to determine the amount of 1:1 hydrochloric acid (HC1) needed to bring

the pH to less than 2. Prior to the addition of HC1, the sample is tested for the presence of

oxidizing agents by placing a few drops of sample onto potassium iodide (Kl)-starch paper. A

blue color change on the Kl-starch paper indicates the presence of oxidizing agents. This must

be noted on the appropriate chain of custodies (COCs), although no treatment of the sample for

oxidizing agents is necessary.

After testing for oxidizing agents, pH test paper is used to determine the amount of HC1 needed

to lower the pH of the test aliquot to pH < 2. The number of drops of 1:1 HC1 needed to lower

the pH of the test aliquot will then be added to each sample vial, prior to collection of the

sample. If bubbles are created during the addition of the acid to the test aliquot, then carbonates

are likely to be present and the associated samples must not be preserved. In this case, it must

be noted on the chain of custody that the preservative was not added. In order to meet the

required holding time for unpreserved volatile organic samples, the analysis must be completed

in seven days.

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3.1.2 Metal Analyses

Aqueous samples for TAL metals and antimony analyses are preserved to a pH less than 2 with

the addition of concentrated nitric acid (HNO3). Preservation is performed following collection

of the sample into the container. A few drops of acid (start with approximately 1 ml) are added

into the sample container, the container is closed and is gently agitated. To check the pH, a few

drops of the preserved sample are removed from the container and checked with pH paper to

ensure that the pH is less than 2. This procedure is repeated until the sample reaches a pH of

less than 2.

3.1.3 Cyanide analyses

Aqueous samples for cyanide analysis are preserved by raising the pH to a pH > 12 with the

addition of concentrated sodium hydroxide (NaOH). Preservation is performed following

collection of the sample into the container and pretesting the sample as described below.

Prior to preserving the sample with NaOH and ascorbic acid, the sample is tested for the

presence of sulfides by placing a few drops of sample onto lead-acetate paper. A darkening of

the lead-acetate indicates the presence of sulfides. This must be noted on the appropriate COCs,

although no treatment of the sample for sulfides is necessary. After testing for sulfides, the

sample is tested for the presence of oxidizing agents by placing a few drops of the sample onto

Kl-starch paper. A blue color change indicates the presence of oxidizing agents and the need

for treatment with ascorbic acid. Add approximately 0.6 grams of ascorbic acid to the sample

to treat for the presence of oxidizing agents and retest with Kl-starch paper until no color

changes are observed. A few drops of NaOH (start with approximately 1 ml) is then added to

the sample container, the container is closed and gently agitated. To check the pH, a few drops

of the preserved sample are removed from the container and checked with pH paper to ensure

the pH is greater than 12. This procedure is repeated until the sample pH exceeds 12.

3.2 SAMPLE CUSTODY

Refer to section 10.2 (Sample Custody) of the Final Field Sampling Plan for the Rose Hill

Regional Landfill of May 1991, except use newest version of the traffic reports for RAS and

SAS and attach the appropriate SAS SDG Nos. to bottles submitted for SAS analyses.

3.3 DOCUMENTATION

Refer to portions of Section 10.3 (Documentation) of the Final Field Sampling Plan for the Rose

Hill Regional Landfill of May 1991 related to groundwater sampling.

3.4 FIELD TESTING EQUIPMENT

Refer to Sections 12.1.2 and 12.1.3 of the Final Field Sampling Plan of May 1991 for

calibration procedures for the pH meter and conductivity meters.

10

4.0 SPECIAL ANALYTICAL SERVICES

The SASs for antimony and water soluble organics are attached.

11

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U.S. Environmental Protection Agency SAS No. CLP Sample Management Office P.O. Box 818 - Alexandria, Virginia 22313 _ Phone: 703/557-2490 - FTS/557-2490

Region I, CLP-DPO, SAS Approval Date

SPECIAL ANALYTICAL SERVICES

Client Request

X Regional Transmittal Telephone Request

A. EPA Region/Client: REGION I/METCA1^? & BPDY/ARCS

B. RSCC Representative: Alvce Lee

C. Telephone Number (61T> S73-S76S

D. Date of Request: August 25. 1993

E. Site Name: Rose Hill Regional Landfill

Please provide below description of your request for Special Analytical Services under the Contract Laboratory Program. In order to most efficiently obtain laboratory capability for your request, please address the following considerations, if applicable. Incomplete or erroneous information may result in a delay in the processing of your request. Please continue response on additional sheets, or attach supplementary information as needed.

1. General description of analytical service requested:

Analysis of water samples for antimony following Supcrfund Analytical Methods for Low Concentration Water for Inorganics Analysis, 10/91, Statement of Work IFB-ILCO2.0

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2. Definition and number of work units involved (specify whether whole samples or fractions; whether organics or inorganics; whether aqueous or soil and sediments; and whether low, medium or high concentration):

Fourteen (14) groundwater water samples to be analyzed for antimony. All samples ^^ will be low concentration.

One Performance Evaluation ampule for analysis according to instructions provided.

3. Purpose of analysis (specify whether Superfund (enforcement or remedial action), RCRA, NPDES, etc.):

Superfund Remedial Investigation.

4. Estimated date(s) of collection:

September 20 - 24, 1993.

5. Estimated date(s) and method of shipment:

September 20 - 24, 1993.

Shipment by overnight express delivery. Saturday deliveries may be necessary.

6. Number of days analysis and data required after laboratory receipt of samples:

Data receipt within 35 days after laboratory receipt of last sample.

Deliver data to:

Overnight Delivery Regular Mail

Heidi Horahan Heidi Horahan USEPA Region I JFK Federal Building 90 Canal Street HPC - CAN 7 Boston, MA 02114 Boston, MA 02203-2211

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7. Analytical protocol required (attach copy if other than a protocol currently used in this program):

Follow Superfund Analytical Methods for Low Concentration Water for Inorganics Analysis, 10/91, SOW IFB-ILCO2.0

8. Special technical instructions (if outside protocol requirements, specify compound names, CAS numbers, detection limits, etc.):

None.

9. Analytical results required (if known, specify format for data sheets, QA/QC reports, Chain-of-Custody documentation, etc.) If not completed, format of results will be left to program discretion.

Follow all requirements of SOW IFB-ILCO2.0

Deliverables must be supplied according to SMO's Basic Ordering Agreement (BOA). Forms DC-1 and DC-2 must be included. Data packages must be delivered to the Region under custody seal.

10. Other (use additional sheets or attach supplementary information, as needed):

11. Name of sampling/shipping contact: P. Svetaka

Phone: (617) 246-5200, x-4629

12. Data Requirements

Reporting Parameter Limit

Follow requirements of SOW EFB-ILCO2.0

13. OC Requirements

Audits Frequency Corrective Required Audits Limits Actions

Follow requirements of SOW IFB-ELCO2.0

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14. Action Required if Limits are Exceeded

Contact SMO first. Contact P. Svetaka, M&E Interim Lead Chemist, (617) 246-5200, x-4629.

Please return this request to the Sample Management Office as soon as possible to expedite processing of your request for special analytical services. Should you have any questions or need any assistance, please contact your Regional representative at the Sample Management Office.

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HUG Z7 '33 i d : 1 0 FROM M E UKEFIELD TO PHGE.032

EDDY

31993 Page 1 of 14

SAS NoU.S. Environmental Protection Agency -CLP Sample Management Office P.O. Box 818 - Alexandria, Virginia 22313 Phone: 703/557-2490 - FTS/557-2490

f Region I, CLP-DPO, SAS Approval Date

SPECIAL ANALYTICAL SERVICES

Client Request

Regional Transmittal Telephone Request

A. EPA Region/Client: I/Metcalf & Eddv

B. RSCC Representative: Heidi Horahao_

C. Telephone Number: (6\T> 573-5765

D. Date of Request: August 23. 1993

E. Site Name: Rose Hill South Kingstown. R.I.

Please provide below description of your request for Special Analytical Services under the Contract Laboratory Program. In order to most efficiently obtain laboratory capability for your request, please address the following considerations, if applicable. Incomplete or erroneous information may result in a delay in the processing of your request. Please continue response on additional sheets, or attach supplementary information as needed.

1. General description of analytical service requested:

Water soluble organic compounds including N,N-dimethylfonnamide presented in Attachment I using direct injection with a nitrogen phosphorous detector (NPD).

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Method based on SW846, Method 8015. The use of a confirmation column is required for all positive results.

Part I of the SAS is: The laboratory is required to submit along with their SAS bid a MDL study or a fortified blank, or an initial calibration performed within the previous six months (See Special Technical Instructions Attachment H#l). Either submittal must meet the criteria required in the Special Technical Instructions before award of Part n of the SAS, the analysis of samples.

2. Definition and number of work units involved (specify whether whole samples or fractions; whether organics or inorganics; whether aqueous or soil and sediments; and whether low, medium or high concentration):

Approximately 4 groundwater samples for low level organics analysis.

3. Purpose of analysis (specify whether Superfund (enforcement or remedial action), RCRA, NPDES, etc.):

Superfund RI/FS (enforcement)

4. Estimated date(s) of collection:

There will be 1 round of sampling from 9/20/93 to 9/24/93.

5. Estimated date(s) and method of shipment:

Samples will be shipped Federal Express Priority Overnight delivery. Samples will be sent in one shipment. Saturday delivery may be required.

6. Number of days analysis and data required after laboratory receipt of samples:

Samples must be analyzed within 14 days of sample receipt. All data required 35 days after sample receipt. Data must be provided after each round.

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Deliver data to:

Overnight Delivery

Heidi HorahanUSEPA Region I90 Canal StreetBoston, MA 02114

Regular Mail

Heidi Horahan JFK Federal Building

HPC-CAN 7 Boston, MA 02203-2211

7. Analytical protocol required (attach copy if other than a protocol currently used in this program):

"Test Methods for Evaluating Solid Waste" EPA SW-846 3rd Edition 1986 Method 8015, Modified as in Attachment n.

8. Special technical instructions (if outside protocol requirements, specify compound names, CAS numbers, detection limits, etc.):

Specific analytes to be included in each analysis and required quantitation limits are presented in Attachment I. The quantitation limits are presented as goals. If for any reason the laboratory cannot reach the limits present for any parameter except N,N,dimethylformamide, they may present those values prior to the award of Part n of the SAS. The MDL for N,N,dimethylformamide must be met. Special technical instructions are in Attachment n.

9. Analytical results required (if known, specify format for data sheets, QA/QC reports, Chain-of-Custody documentation, etc.) If not completed, format of results will be left to program discretion.

See Attachment m.

10. Other (use additional sheets or attach supplementary information, as needed):

11. Name of sampling/shipping contact:

Name: Jay Best, Deb Simone, Al Clancy Phone: (617)246-5200

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12. Data Requirements

See Attachment I for compound list, CAS numbers and detection limits

13. OC Requirements

Audits Required

Frequency of Audits

Corrective Actions

Part I - Prior to the Award of SAS

Laboratory Fortified Blanks

Prior to the award of SAS

70%-130% for each analyte

Criteria must be met prior to the awards of SAS

or

Method Detection Limit Study

Prior to the award of SAS

Detection Limits must meet or exceed the quantitation limits listed in Attachment I

Criteria must be met prior to the award of SAS

or

Initial Calibration Prior to the award of SAS

%RSD<25% Criteria must be met prior to the award of SAS

Part n - After Successful completion of Part I

Method Blanks

Prior to the analysis of any samples, then after each sample or standard analyzed

Compounds detected must be less than Vi the required quantitation Limit

Locate source of contamination, correct problem and reanalyze all samples since last acceptable method blank

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13. OC Requirements (Continued)

Audits Required

MS/MSD

Initial Calibration

Continuing Calibration

Surrogate spike (dimethyl) acetamide 0.5 mg/1)

Frequency of Audits

One per sample batch (10 samples or less)

See Attachment

Once every 8 hours and after the last sample each 8 hour period

Each Sample, blank, standard and matrix spike

Limits

70%-130% recovery

RSD <_ 25%

RPD < 25%

Area must be 50%-100% of associated standard.

Surrogates must be within retention time window determined in item 8 of Attachment n and within 30 sec. of the surrogate retention time in the continuing calibration.

Corrective Actions

Reanalyze. If still out, flag non-compliant data with an asterisk (*).

Criteria must be met before analysis of blanks and samples.

Perform another initial calibration and reanalyze all samples analyzed since the last continuing calibration within limits.

Rerun sample and report both values. Flag noncompliant values with an asterisk (*)

Rerun samples, blanks, or spikes which do not meet the surrogate retention time window, until they are in compliance

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13. OC Requirements (Continued)

Audits Required

Frequency of Audits

Corrective Actions

Laboratory Fortified Blank

Daily before the analysis of any samples

Percent recovery must be within 70-130% for each analyte samples

Criteria must be met prior to the analysis of standards and

14. Action Required if Limits are Exceeded

First contact SMO, then Contact A. Beliveau - Lead Chemist Metcalf & Eddy (617)246-5200 X4433 or J. Best (617)246-5200 X4411

Please return this request to the Sample Management Office as soon as possible to expedite processing of your request for special analytical services. Should you have any questions or need any assistance, please contact your Regional representative at the Sample Management Office.

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ATTACHMENT I SPECIAL TECHNICAL INSTRUCTIONS

Compound CAS Number Required Quantitation Limit Qig/L)

N.N-dimethylformamide 68-12-2 50 ethyl carbamate 51-79-6 50 ethyl urethane (N-ethyl, ethyl

ester carbamic acid) 623-78-9 50 Acrylonitrile 107-13-1 50

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ATTACHMENT H SPECIAL TECHNICAL INSTRUCTIONS

1. Part I of the SAS will be to generate and submit one of the following proofs of laboratory capability:

a. The MDL study must be performed on the Attachment I compounds by analyzing a 250 /*g/L concentration standard at a minimum of seven times. The MDL Study must be performed in accordance with the Title 40 Code of Federal Regulations Part 136, Appendix B. The MDL study is acceptable if performed within six months prior to bid acceptance. MDL's for each analyte are required to be less than or equal to those identified in Attachment I.

b. A laboratory fortified blank will be analyzed containing all of the compounds listed in Attachment I at a concentration equal to the RQL in Attachment I. For each analyte the percent recovery must be between 70-130%. Acceptable criteria must be met prior to bid acceptance and daily prior to sample analysis.

c. An initial calibration meeting the criteria indicated in item 6 of the special technical instructions and QC Section B.

d. One of these three that has been conducted during the past 6 months.

e. Upon receipt of one of the three above items and upon acceptance by M&E of the analytical requirements, samples will be shipped to the laboratory for analysis of Part H of the SAS.

2. Samples and standards will be analyzed by direct aqueous injection. The primary column must be a 30 meter by 0.53 mm ID capillary carbowax column. An injection volume of 2 ul is suggested. Larger volumes may be used to achieve the required detection limit provided significant column degradation does not result. The same injection volume should be used for all analysis standards and blanks. This volume must be reported on the Form I's.

3. The detector used will be a nitrogen/phosphorous thennoionic detector (NPD). The chromatographic column and conditions that must be used are specified below. They are the same for both the primary and confirmation columns except that the final hold may be eliminated in the confirmation column provided all compounds of interest have eluted.

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Primary Column: Carbowax 30m x .53mm 1.0 urn film Confirmation Column: Nukol 30m x .53mm 1.0 urn film

Initial Temperature: 50°C Initial Hold: 0.5 minutes Ramp Rate: 6°C/minute Final Temperature: 150°C Final Hold: 4.0 minutes Detector Temperature: 300°C Injector Temperature: 225 °C

Carrier gas flow rates should be adjusted such that the DMF retention time is greater than 3 minutes.

4. Specific analytes to be included in each standard and required quantitation limits are presented in Attachment I.

5. Each sample, standard, and blank must contain an surrogate spike of dimethyl acetamide at a concentration of 0.5 ppm. A retention time window for the surrogate must be established as required by Item 8. The surrogate retention time must fall within this window for all samples, blanks and spikes. The surrogate retention time of all blanks and samples must also fall within 30 seconds of its associated continuing calibration.

6. The CG is calibrated using a five-point external calibration containing all analytes (Attachment I). This must be analyzed prior to analysis of blanks and samples. The midrange calibration mixtures of aqueous standards must provide a minimum of a half scale response for all compounds of interest. The lowest standard must produce a peak that is well defined and can be easily quantitated. This response must be at an attenuation setting capable of achieving well defined symmetrical peaks. One of the standards must be at a concentration near or at the required quantitation limit and the others at concentrations that correspond to the expected range of concentrations found in real samples or should define the working range of the detector. This must be performed on each quantitation column and each instrument at the beginning of the analytical episode and each time a new column is installed.

Response factors must be calculated for each of the five calibration points for each analyte listed in Attachment 1. An average response factor (RF) and a percent relative standard deviation (% RSD) must be calculated in the same manner as required by Form VI of the SOW (OLM01.8) for RAS organics. The % RSD for all compounds must be less than 25 percent or another five-point calibration is required.

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7. A continuing calibration must be performed every 8 hours and at the end of each 8 hour period of analysis. The continuing calibration concentration should be chosen to provide approximately half scale response for all compounds of interest. A relative percent difference (RPD) must be calculated in the same manner required by the SOW (OLM01.8) for RAS organics. If the RPD is greater than 25 percent for any compound then another initial calibration must be performed, and all samples analyzed since the last continuing calibration within limits must be reanalyzed.

8. Retention time windows must be determined prior to the use of any instrument or column. If a new column is installed retention time windows must be reestablished.

Before establishing windows, make sure the GC system is within optimum operating conditions. Make three injections of all single component standard mixtures. Injection should be made over at least a 72-hour period. If the injections are made over a period less than 72 hours then the retention time window may be too small.

Calculate the standard deviation of the three absolute retention times for each single component standard. Plus or minus three times the standard deviation of the absolute retention times for each standard will be used to define the retention time window; however, the experience of the analyst should weigh heavily in the interpretation of chromatograms.

In those cases where the standard deviation for a particular standard is zero, the laboratory must substitute the standard deviation of a close eluting, similar compound to develop a valid retention time window.

9. Matrix spike and matrix spike duplicate analysis shall be performed using all of the compounds listed on Attachment I. The spike shall be added prior to any sample dilution. A concentration shall be chosen that provides for an approximately half scale instrument response, but is at least 50 percent of the concentration detected in the unspiked sample.

10. A confirmation analysis of all positive results must be performed. The confirmation column must be able to separate N,N-dimethylformamide from all other compounds of interest.

Initial and continuing calibrations must be performed on the confirmation column. Either column may be used for quantisation provided that the criteria described in #6 are met.

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11. In the event that 2 or more compounds can not be resolved on either the quantitation column or the confirmation column, then SMO and M&E must be notified.

12. Large carryover problems are experienced with this method. Therefore, it is required that a method blank be analyzed prior to each sample analysis. This blank must meet the requirements listed in the QC requirements. (Compounds must be less than 1/2 the required quantitation limit.)

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ATTACHMENT HI

DELIVERABLES

• The MDL study data must be in tabular form with raw data provided including standard deviation, percent RSD, concentration of standard and MDL. The laboratory fortified blank must be in tabular form as in RAS Form IV modified for the Attachment I list of compound. The initial calibration must be as in RAS Form VI VOA modified for the attachment I list of compounds.

• The data package deliverable should resemble as closely as possible the SOW (OLM01.8) for RAS analysis of pesticides/PCBs. Delivery forms provided in CLP RAS SOWs must be modified to include all Attachment I compounds. The data qualifier used in the SOW must be applied to the data provided.

• A case narrative must be provided describing the procedure performed by the laboratory for any deviations from this SAS. Problems encountered during analysis must be discussed as well as any factors influencing the data quality. The sample SAS request, SAS packing list and chain of custody forms must be included. All signed and dated sample tags and shipping air bills must be provided. Describe GC columns and detectors.

• Any procedural details which have been left to the laboratory to specify must be described. These include but are not limited to:

• Injection volumes (must be reported on Form I's beneath the dilution factor)

• Concentration of calibration standards • MS/MSD spike concentrations • Column used for quantitation • Retention time windows • Detection limits • Dilutions

• An example calculation must be provided for each method of analysis (if more than one method is used) for positive results and detection limit values reported.

• All telephone logs generated must be included.

• The data package must be paginated.

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• The data package must include:

1. Run log or instrument log for standards and samples.

2. Raw data for blanks, standards, samples and QC check samples.

3. Chromatograms from both quantitation and confirmation.

4. Instrument quantitation sheets.

5. Date and time of analysis labeled on instrument quantitation sheet.

6. The sample results must be summarized on the appropriate Form I modified for the Attachment I compounds.

7. The calibration results reported in tabulated format like RAS Forms VI and modified for the Attachment I list of compounds. The relative response factors and percent relative standard deviation must be calculated for each day's calibration. The concentration of the standards analyzed and the raw data must be provided.

8. Tabulated initial five point calibration results, average response factor and % RSD must use RAS form VI modified for the compounds of interest. Continuing calibration results, and percent difference must use RAS Form Vn modified for the compounds of interest.

9. The method blanks and associated samples must be summarized using RAS Form IV.

10. The matrix spike/matrix spike duplicate results must be reported on Form in VOA modified to include compounds presented in special technical instructions.

11. All raw data from single compound standards runs used to determine retention time windows must be provided.

12. A standard chromatogram which has all of the peaks labeled with the compounds listed in Attachment I.

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13. Results of surrogate spike areas must be summarized using RAS Form VTUD modified for the compounds of interest.

NOTE: Raw data includes the associated instrument printouts. The concentration of all standards analyzed with the amount injected must be included.

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addendum to sampling and analysis plan · for this residential well samplin roungd (roun 6)d , it...

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