O'Reilly, Talbot & Okun Environmental • Safety • Health • Geotechnical Engineering

Associates, Inc.

June 22, 1998 File No. 267-02-01

BREAKS Mr. Charles Crocetti OTHER-Sanborn, Head & Associates 6 Garvins Falls Road, Suite 1 Concord, New Hampshire 03301-5174

Re: SDG BW227 NHDES Laboratory Beede Waste Oil/Cash Energy Site Organic Data Validation

Volatiles: 197 Soils / TP-127/139; TP-136 to TP-145; TP-147; P9-10; P9-13 to P9-15; PI 1-1; PI 1-2; OW-227 (Field Duplicate Pair/Pi 1-1 and OW-227)

2 / Aqueous Trip Blanks / TB042298 and TB042898 1 / Aqueous Equipment Blank / OW-227A 1 / Aqueous PES/VO1959

Dear Mr. Crocetti:

A Tier II data validation was performed on the volatile organic analytical data for 19 low level soil samples, three aqueous blanks and one aqueous PE sample which together comprise SDG BW227. These samples were collected from the Beede Waste Oil/Cash Energy Site by Sanborn, Head & Associates. Copies of field sampling notes are attached.

The samples were analyzed by the New Hampshire Department of Environmental Services (NHDES) Laboratory using EPA Method 8260A consistent with the project Work Plan and QAPP, both dated November 1997. The analytical SOP (No. 10.57e, Rev. 0, 6/19/97) was provided in the QAPP and was attached to the validation memo for BW219 (4/6/98) for reference.

Tier II data validation was performed using the Region I. EPA-NE Data Validation Functional Guidelines for Evaluating Environmental Analyses, December 1996, and project specific criteria (attached). A partial Tier III review was conducted on laboratory method blanks to assess the possible presence of compounds below quantitation limits. A CADRE review was not performed on these data.

The data were evaluated based on the following parameters:

• Overall evaluation of data and potential usability issues; * • Data completeness (CSF audit); * • Preservation and technical holding times;

293 Bridge Street • Suite 500 • Springfield, Massachusetts 01103 Phone (413) 788-6222 • Fax (413) 788-8830 • E-Mailoto413@aol.com

BW227 Data Validation. Page 2O'Reilly, Talbot & Okun

Associates, Inc. * • GC/MS instrument performance check (tuning);

• Initial and continuing calibration; • Blanks; • Surrogate compounds; • Internal Standards;

* • Matrix spike/matrix spike duplicate; * • Field duplicates; * • Sensitivity check;

• PE Samples/Accuracy Check; and • Compound quantitation and reported quantitation limits.

* Indicates all criteria were met for this parameter.

The following information is provided in attachments to this data validation memorandum:

Table 1: Recommendation Summary Table - summarizes validation recommendations.

Table 2: Overall Evaluation of Data - summarizes site DQOs and potential usability issues.

Table 3: Data Summary Table - summarizes accepted, qualified and rejected data, including tentatively identified compounds (TICs).

Overall Evaluation of Data and Potential Usability Issues

This soil data is intended for use in assessment of human health and ecological risks, nature and extent of contamination, and remedial alternatives. Four of the soils were run as medium level samples. The elevated quantitation limits which result from medium level analysis may affect data usability for undetected compounds.

The primary concern in this SDG is analytical error due to incomplete purging at the heavy end of the run. This resulted in low level blank contamination, carryover and poor internal standard recoveries for the less volatile analytes. Aqueous samples and medium level soils, which are extracted into methanol and then purged, generally had acceptable IS results. Sample matrix may therefore be affecting results. The data is largely useable, although some analytes and quantitation limits have been estimated (J-flagged). Low concentrations of four target analytes and one tentatively identified compound have been changed to "U" values based on their presence in blanks.

The following sections provide further information on this data package.

Initial and Continuing Calibration

This project has expanded criteria for relative response factors (RRFs) for four compounds, as shown on the attached tables from the QAPP. Four target analytes failed to meet criteria in initial and/or continuing calibrations. These compounds, the affected samples and validation actions are summarized below. When an analyte failed due to a high initial calibration relative standard

BW227 Data Validation. Page 3O'Reilly, Talbot & Okun

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deviation (%RSD) or continuing calibration percent difference (%D), data were estimated due to uncertainty in results.

Calibration Compound Failing Action Affected Samples Value

4/13/98 Acetone 33.3%RSD J(+),UJ(-) TP-127/139, Low Soil ICal TP-136to 139, 141

to 145, 147;P9-10, 13, 14, 15 (and reruns)

4/30/98 Dichlorodifluoromethane 26.2 %D J(+),UJ(-) trip blanks (3) and Aqueous CCal 2-Butanone RRF 0.009 None* equip, blank

sec-Butylbenzene 27 %D J(+), UJ (-) (OW-227A)

n-Butylbenzene 31.2%D J(+),UJ(-) 5/5/98 Acetone 27.7 %D J(+),UJ(-) TP-140; Aqueous CCal n-Butylbenzene 28.7 %D J(+),UJ(-) Pll-1; (applies to 1 ,2,4-Trichlorobenzene 35.5 %D J(+),UJ(-) Pll-2RE;and medium soils) 1 ,2,3-Trichlorobenzene 37 %D J(+),UJ(-) OW-227

5/4/98 Naphthalene 33.6%D J(+),UJ(-) TP-143RE;TP-145; Soil CCal TP-147;P9-10. 13,

14, and 15RE Notes: (+) indicates detected values, (-) indicates nondetect results. *Results would normally be rejected if nondetect. Since the only affected samples are blanks and the analyte is not present in samples, there is no reason to suspect false negatives in this case. Professional judgment used to accept data.

Blanks

The trip blanks, bottle blanks and method blanks associated with these samples did not contain reportable levels of VOCs. The equipment blank contained 3 ug/1 chloroform. Chloroform was not detected in samples, therefore no action is taken based on that detection. The equipment blank was prepared with water provided by the laboratory. The source of the chloroform has not been identified.

Based on the results of past laboratory blanks, a partial Tier III validation was conducted to assess the presence of compounds near/below the quantitation limit. Previous SDGs have had carryover, particularly in the blank and first sample run after the calibration check in each sequence. The data package narrative states that carryover probably occurred in this SDG. A comparison of blank chromatograms from previous SDGs shows a similar carryover pattern occurring (raw data attached). Two samples analyzed after calibration checks were reported to contain low levels of analytes which are believed to be carryover. Blank results and validation actions are summarized below.

Compounds Below QL in Blanks Action

1 ,2,4-Trichlorobenzene, Hexachlorobutadiene, "IT detects in TP-127/139 and Naphthalene and 1,2,3-Trichlorobenzene TB-143RE; raise QLs to reported values

BW227 Data Validation, Page 4O'Reilly, Talbot & Okun

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Samples TP-138, P9-10, P9-13 and P9-14 also contained naphthalene. Those detections have been left unqualified due to the following reasons:

The samples did not follow calibration checks or high level samples in the run sequence; The naphthalene peak was significantly above the baseline; and

• The chromatograms had a hydrocarbon pattern suggesting the presence of petroleum, of which naphthalene is a natural constituent.

Surrogate Compounds

One medium level and six low level soil samples had surrogate recoveries above the upper QC limit. In the low level soils, high surrogate recoveries were accompanied by low internal standards (IS), which falsely inflated results. Surrogate results are summarized below. Internal standard results are discussed in the next section.

Sample Failing % Recovery % Recovery Action

Surrogate* (original run) (rerun) (+) Detects Nondetects

TP-127/139 SI 139 J A

S2 126 145

TP-136 S2 121 123 J A

TP-138 S2 123 J A

TP-139 SI 122 J A

S2 128 127

TP-142 S2 123 J A

TP-143 S2 129 121 J A

TP-145 S2 121 125 J A

P9-15 S2 122 122 J A

Pll-2 S3 126 119 J A

* Sl=Dibromofluoromethane, limits 80-120%. S2=l,2-Dichloroethane-d4, limits 80-120%. S3=Toluene-d8, limits 81-117%. A blank space indicates value was acceptable.

Internal Standards

Eight of the fifteen low soils had one or more internal standard (IS) which failed. Each of these samples was reanalyzed and again displayed poor internal standard results. Results were poorest for 1,4-dichlorobenzene-d4 (IS-3), against which the last third of the analytes are quantitated. Results of compounds quantitated with these internal standards may be biased high or low.

No trend was evident in internal standard recoveries. Internal standards met criteria in aqueous samples, medium level soils, calibration standards and blanks. This suggests some component of matrix effect. Matrix spike/matrix spike duplicate results and field duplicate results were good,

BW227 Data Validation, Page 5O'Reilly, Talbot & Okun

Associates, Inc. although none of the MS/MSD analytes are quantitated against IS-3. The following table summarizes outlying IS results and applicable validation actions.

Sample IS-1 %Recovery Action IS-2 %Recovery Action IS-3 %Recovery Action (Fluorobenzene) (Chlorobenzene-d5) (l,4-Dichlorobenzene-d4)

(+)/(-)* (+)/(-)* (+>/<-)*

TP-127/139 36 J/UJ 31 J/UJ 19 J/R

TP-127/139RE 25 J/UJ 27 J/UJ 17 J/R

TP-136 37 J/UJ

TP-136RE 35 J/UJ

TP-138 47 J/UJ

TP-138RE 42 J/UJ

TP-139 28 J/UJ

TP-139RE 28 J/UJ

TP-142 48 J/UJ

TP-142RE 39 J/UJ

TP-143 32 J/UJ

TP-143RE 41 J/UJ

TP-145 33 J/UJ

TP-145RE 35 J/UJ

P9-15 32 J/UJ

P9-15RE 36 J/UJ

A blank space indicates the recovery was acceptable. * Actions apply only to those compounds quantitated with the out-of-specification internal standard. (+) indicates action for positive detections; (-) indicates nondetects. Nondetects are estimated when the IS recovery is between 20 and 50%, and rejected when the recovery is <20%.

Poor internal standard results have been observed in past soil SDGs from this site. As indicated in their narrative and in verbal correspondence, the laboratory has attempted various means of improving recoveries.

Samples with poor recoveries were reanalyzed, therefore two sets of analytical data are available. Internal standard (IS) and surrogate spike (SS) results were reviewed to determine which analyses should be recommended for use. In most cases one run had better recoveries than the other, and was selected for use. In cases where IS and SS recoveries were similar in the two runs, use of the original run is recommended due to the shorter hold time and unopened state of the sample jar at that time. Recommendations for use and rationale are provided in the table below.

BW227 Data Validation, Paee 6O'Reilly, Talbot & Okun

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Sample No. Use Original or Rerun? Rationale TP- 127/1 39 Original Better IS and SS recoveries TP-136 Original Better IS and SS recoveries TP-138 Original Better IS and SS recoveries TP-139 Rerun SS recovery better: IS results same in both TP-142 Original Better IS and SS recoveries TP-143 Rerun Better IS and SS recoveries TP-145 Original IS slightly worse, SS slightly better: use first run P9-15 Rerun IS recovery better; SS results same in both Notes: IS=Intemal Standard; SS=Surrogate Spike

Table 3 summarizes the data which is recommended for use.

PE Sample/Accuracy Check

The performance evaluation sample (PES) for this SDG contained 13 target analytes, seven of which scored within limits. There were also two nontarget compounds which were correctly identified in the tentatively identified compound report. Five targets scored warning low. There was no trend to the compound class or elution time of those analytes. Per Region I guidance, no action is taken on warning scores. One compound scored action high. That compound (1,2-dichloropropane) was not detected in the samples, therefore no action was taken based on PES scores.

Compound Quantisation and Reported Quantitation Limits

Sample TP-137 contained 1,2,4-trimethylbenzene at a concentration exceeding the upper calibration limit in its undiluted run. The sample was reanalyzed at an effective dilution of 5 to get this analyte on scale. Dilution raised quantitation limits for the other analytes correspondingly. Use of the lower quantitation limits is desirable. It is recommended that the undiluted run be used for all analytes except 1,2,4-trimethylbenzene, which should be reported from the diluted run for TP-137.

Quantitation limit requirements for soil samples were based primarily on NHDES S-l soil standards, as shown on Table C.12 of the 11/97 Work Plan (copy attached with the DQO summary form). DQOs were achieved for soils run as low level samples. The four samples which required medium level analysis exceeded DQOs for up to 22 target analytes each. The end user should assess the impact of elevated quantitation limits for samples PI 1-1, PI 1-2, TP-140 and OW-227.

The laboratory reported results on two sets of forms in this SDG: standard Form I's and signed result reports on DES letterhead. The soil quantitation limits for three compounds (vinyl chloride, chloromethane and bromomethane) are different on the two sets of reports. The laboratory was contacted to confirm which was the correct set. The Form I's have the correct

O'Reilly, TalbQt & Okun BW227 Data Validation, Page 7

Associates, Inc. quantitation limits, as supported by the 5/98 MDL study. The reports on DES letterhead have elevated quantitation limits for three compounds due to a software error, and should not be used.

Please feel free to contact me at (413) 788-6222 if you have any questions regarding this validation.

Very truly yours,

O'Reilly, Talbot & Okun Associates, Inc.

Valerie D. Watanabe Data Validator

es D. Okun rincipal

cc: D. Szaro/EPA QA (with all attachments) W. Ives/NHDES Site Manager (memo + tables only) J. DiLorenzo/EPA Site Manager (memo + tables only) D. Vorhees/Menzie-Cura (memo + tables only)

Attachments: Table 1: Recommendation Summary Table Table 2: Overall Evaluation of Data Table 3: Data Summary Tables (includes TICs) Data Validation Worksheets PES Score Report Communication/Phone Logs Method Blank Raw Data Field Sampling Notes Project Validation Criteria (QAPP Tables 6b and 8b) CSF Audit (DC-2 Form) DQO Summary Form

O'Reilly, Talbot & Okun

Associates, Inc.

BW227 Data Validation, Page 8

TABLE 1 Recommendation Summary Table

VOLATILE ORGANIC ANALYSIS (8260A) Beede Waste Oil/Cash Energy Site

SDG BW227

Sample Number

TP-127/139 (use original run)

TP-136 (use original run)

TP-137

TP-138 (use original run)

TP-139 (use rerun)

TP-140

TP-141

TP-142 (use original run)

TP-143 (use rerun)

TP-144

TP-145 (use original run)

TP-147

P9-10

P9-13

P9-14

P9-15 (use rerun)

Pll-1

PI 1-2

OW-227

OW-227A

TB042298

TB042898

TB SOIL

Matrix

Soil

Soil

Soil

Soil

Soil

Soil

Soil

Soil

Soil

Soil

Soil

Soil

Soil

Soil

Soil

Soil

Soil

Soil

Soil

Aq. /Equip blank

Aq./Trip blank

Aq./Trip blank

AqVTrip blank

Recommended Qualifiers

I1 5 6 7' - - J/R1 U1

Jl.5,6

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J3

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J1'4

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J3

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D - Sample was reanalyzed at dilution to get high concentration on scale. Use undiluted run for analytes which were within calibration range; use diluted run 1,2,4-trimethylbenzene only.

J1 - High relative standard deviation for acetone in initial calibration. J detects and UJ nondetects due to analytical variability.

J2 - High percent difference for dichlorodifluoromethane, sec-butylbenzene and n-butylbenzene in continuing calibration-. J detects and UJ nondetects due to analytical variability.

BW227 Data Validation. Pase 9O'Reilly, Talbot & Okun

Associates, Inc. J3 ­ High percent difference for acetone, n-butylbenzene, 1,2,4-trichlorobenzene and

1,2,3-trichlorobenzene in continuing calibration. J detects and UJ nondetects due to analytical variability.

J4 ­ High percent difference for naphthalene in continuing calibration. J detects and UJ nondetects due to analytical variability.

J5 ­ Surrogate recovery(ies) exceeded QC limits. J positive target detections and accept nondetects due to possible high bias. May be associated with low internal standard recoveries; check for additional validation action based on IS.

J6 ­ Internal standard recovery low. Use original run. J detects and UJ nondetects for compounds quantitated using l,4-dichlorobenzene-d4. Results may be biased high or low

J7 ­ Internal standards low; J detects and UJ nondetects for compounds quantitated using fluorobenzene and chlorobenzene-d5. Results may be biased high or low

J/R' - Internal standard below 20%; J detects and reject nondetects for compounds quantitated using l,4-dichlorobenzene-d4. Potential for high or low bias, false negatives.

U' - Report naphthalene, hexachlorobutadiene, 1,2,3-trichlorobenzene, and 1,2,4-trichlorobenzene as nondetect due to presence in method blank; elevate quantitation limit to reported concentration.

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