O'Reilly, Talbot & Okun Associates, Inc. Letter of Transmittal

O'Reilly, Talbot & Okun Associates, Inc. 293 Bridge Street; Suite 500 Springfield, Massachusetts 01103

DATE:

JOB NO.:

4/16/99

267-02-01

(413) 788-8830 fax (413) 788-8830 VIA: Hcl |x| Regular mail

To Chip Crocetti [ | Overnight (Monday)

Other Sanborn, Head & Associates

6 Garvins Falls Road, Suite 1 s. i • • • i i u u l Record*Cemci

Concord, NH 03301-5174

Telephone No.: 603-229-1900 liM

ATTACHED PLEASE FIND THE FOLLOWING:

NO. COPIES DATE DESCRIPTION

4/15/99 Inorganic Validation Memo, SDG BW223

4/5/99 Reissued Page 1 of Inorganic Validation Memo, SDG BW214

4/6/99 Reissued Page 1 of Inorganic Validation Memo, SDG BW215

Please replace previously submitted page 1's with reissued versions. Previous versions were incorrectly dated 1998.

| | As requested

| x | For your use

[~~] For review and comment. Comments dueby:_

NOTES:

COPY TO: DiLorenzo, Ives, Vorhees, Bickford (text & tables only) SIGNED: Valerie Watanabe D. Szaro (w/all attachments)

EnvironmentalSafetyHealthGeotechnicsT

O'Reilly, Talbot & Okun <— *SBSB£B3& -* 293 Bridge street [ A S S O C I A T E S ] I

•!• Suite 500

Springfield, MA 01103

Tel 413 788 6222

Fax 413 788 8830

April 6, 1999 *

File No. 267-02-01 Email ofnce@oto-env com

Mr. Charles Crocetti

Sanborn, Head & Associates ^ ' U v r i u n d Records Center 6 Garvins Falls Road, Suite 1 ^ ! i' i- _ Concord, New Hampshire 03301-5 174 ' •< i \K.

Re: SDG BW215 NHDES Laboratory Beede Waste Oil/Cash Energy Site Inorganic Data Validation

Metals / 177 Groundwater / AE-2, AE-10, AE-11D, AE-12, AE-14, AE-17D, AE-18S, RFW-1, RFW-2, SH-2I, SH-10I, SH-17I, SH-32, SH-33, SH-34, SH-37, OW-215 (Field Duplicate Pair 7 AE-12 and OW-215)

1 7 Aqueous Equipment Blank / OW-215A 2 7 Aqueous PES 7 PL989 (metals) and HG979307 (mercury)

Water Quality Parameters 7 11 Groundwater 7 AE-2, AE-10, AE-11D, AE-12, AE-14, AE-17D, AE-18S, SH-2I, SH-10I, SH-17I, OW-215 (Field Duplicate Pair 7 SH-19S and OW-214)

1 7 Aqueous Equipment Blank 7 OW-215A 1 7 Aqueous PES7 PC836 (nitrate)

Dear Mr. Crocetti:

This memo covers the Tier II validation of metals data in sample delivery group (SDG) BW215. This SDG is comprised of 17 groundwater samples, one aqueous equipment blank and three aqueous performance evaluation samples (PES). Groundwater samples were collected from the Beede Waste Oil/Cash Energy Site by Sanborn Head & Associates, Inc. with assistance from the New Hampshire Department of Environmental Services (NHDES) field staff. Copies of field sampling notes were provided with the BW215 organics validation memo dated July 23, 1998.

These samples were analyzed by the NHDES laboratory. Each of the samples was analyzed for a suite of 16 metals; eleven samples were analyzed for an expanded suite of 22 metals and water quality parameters. Analytical standard operating procedures (SOPs) for these methods were included in the November 1997 Quality Assurance Project Plan (QAPP), and were also provided as attachments to the BW210 inorganic validation memo dated March 29, 1999.

Tier H. data validation was performed by O'Reilly, Talbot & Okun Associates, Inc. (OTO). The Region I Laboratory Data Validation Functional Guidelines for Evaluating Inorganic Analyses dated February 1989 was used as the primary guidance source. Available sections

Rev.l

EnvironmentalSafetyHealthGeotechnicc O'Reilly, Talbot & Okun *— OJQEQSE^ —> 293 B^ street

[ A S S O C I A T E S ] I i- Suite 500

Springfield, MA 01103

Tel 413 788 6222

Fax 413 788 8830

April 5, 1999 Email office@oto-envcom

File No. 267-02-01

Mr. Charles Crocetti Sanborn, Head & Associates Superiund Record 6 Garvins Falls Road, Suite 1 S ' )

I,f: , - ­HRl' X KConcord, New Hampshire 03301-5174 ------O H i L K -

Re: SDGBW214 NHDES Laboratory Beede Waste Oil/Cash Energy Site Inorganic Data Validation

Metals / 177 Groundwater / SH-2D, SH-10D, SH-13D, SH-14D, SH-16D, SH-17D, SH-18D, SH-19D, SH-19I, SH-19S, SH-24D, SH-24I, SH-24S, SH-25D, SH-25I, SH-25S, OW-214 (Field Duplicate Pair / SH-19S and OW-214)

1 / Aqueous Equipment Blank / OW-214A 2 / Aqueous PES / PN617 (metals) and HG979222 (mercury)

Water Quality Parameters / 10 Groundwater / SH-2D, SH-10D, SH-13D, SH-14D, SH-16D, SH-17D, SH-18D, SH-24D, SH-24I, SH-24S

1 / Aqueous Equipment Blank / OW-214A 1 / Aqueous PES / PA 196 (nitrate)

Dear Mr. Crocetti:

This memo covers the Tier II validation of metals data in sample delivery group (SDG) BW214. This SDG is comprised of 17 groundwater samples, one aqueous equipment blank and three aqueous performance evaluation samples (PES). Groundwater samples were collected from the Beede Waste Oil/Cash Energy Site by Sanborn Head & Associates, Inc. with assistance from the New Hampshire Department of Environmental Services (NHDES) field staff. Copies of field sampling notes were provided with the BW214 organics validation memo dated July 20, 1998.

These samples were analyzed by the NHDES laboratory. Each of the 17 samples was analyzed for a suite of 16 metals; 10 samples were also analyzed for water quality parameters. Analytical standard operating procedures (SOPs) for these methods were included in the November 1997 Quality Assurance Project Plan (QAPP), and were also provided as attachments to the BW210 inorganic validation memo dated March 29, 1999.

Tier II data validation was performed by O'Reilly, Talbot & Okun Associates, Inc. (OTO). The Region I Laboratory Data Validation Functional Guidelines for Evaluating Inorganic Analyses dated February 1989 was used as the primary guidance source. Available sections of the newer Region I EPA-New England Data Validation Functional Guidelines for

Rev.l

EnvironmentalSafetyHealthGeotechnic T

O'Reilly, Talbot & Okun <— ^iUNUiUS^—>• 293 Bndge street [ A S S O C I A T E S ] I

4- Suite 500

Springfield, MA 01103

Tel 413 788 6222

April 15, 1999 pax 4i3 788 saso File No. 267-02-01 E m a i l office@oto env com

Mr. Charles Crocetti Sanborn, Head & Associates

'"' L • 1u:>d H f6 Garvins Falls Road, Suite 1 Si j iConcord, New Hampshire 03301-5174

nf \ r \ K Re: SDGBW223

NHDES Laboratory Beede Waste Oil/Cash Energy Site Inorganic Data Validation

> H ( h R . ~

Metals and WQ Parameters 14 / Groundwater / AE-8, AE-9, AE-11S, AE-16, BR-25, BR-28, SH-5S,

SH-6S, SH-7S, SH-10S, SH-22R, SH-53S, WS-1, OW-223 (Field DupHcate Pair / AE-9 & OW-223)

2 / Aqueous Equipment Blanks / OW-223A-P and OW-223A-R 3 / Aq. PES / 0013265 (metals), HG9801091 (mercury), PB531 (nitrate)

Dear Mr. Crocetti:

This memo covers the Tier n validation of metals data in sample delivery group (SDG) BW223. This SDG is comprised of 14 groundwater samples, one aqueous equipment blank and three aqueous performance evaluation samples (PES). Groundwater samples were collected from the Beede Waste Oil/Cash Energy Site by Sanborn Head & Associates, Inc. (SHA). Copies of field sampling notes were provided with the BW223 organics validation memo dated July 9, 1998.

These samples were analyzed by the New Hampshire Department of Environmental Services (NHDES) laboratory. Each of the 14 samples was analyzed for water quality parameters. Three samples and one blank were analyzed for a suite of 16 metals; the other 11 samples and blank were analyzed for an abbreviated list of minerals. Analytical standard operating procedures (SOPs) for the methods were included in the November 1997 Quality Assurance Project Plan (QAPP), and were also provided as attachments to the BW210 inorganic validation memo dated March 29, 1999.

Tier n data validation was performed by O'Reilly, Talbot & Okun Associates, Inc. (OTO). The Region I Laboratory Data Validation Functional Guidelines for Evaluating Inorganic Analyses dated February 1989 was used as the primary guidance source. Available sections of the newer Region I EPA-New England Data Validation Functional Guidelines for Evaluating Environmental Analyses (December 1996) were used in assessing performance evaluation sample results and for general formatting information. Inorganic validation sections of that document have not yet been issued. Project specific criteria were used for some parameters. Analytical and validation criteria are summarized on the Table 6 and 8 series of the QAPP, which were also provided as attachments to the BW210 inorganic validation memo dated March 29, 1999.

T BW223 Inorganic Data Validation; Page 2 O'Reilly, Talbot & Okun

[ A S S O C I A T E S ] I

Tier n validation generally does not include review of raw data. In this case, however, review of raw data was required to obtain/confirm information for some parameters. The NHDES laboratory is not equipped to generate reporting forms like those required for the Contract Laboratory Program (CLP). Their QC summary tables are manually generated and do not provide the same information as CLP forms in all cases. Partial Tier III review was conducted to locate and/or verify results as necessary. A CADRE review was not performed.

This data package was evaluated based on the following parameters:

- Overall evaluation of data and potential usability issues; * - Data completeness; * - Holding times;

- Initial and continuing calibration; - Blanks;

* - ICP interference check sample results; - Matrix spike results/lab duplicates; - Field duplicates;

* - Lab control sample results; - Furnace atomic absorption results;

* - Serial dilution results; - Detection limit check; - Performance evaluation samples; and - Sample results 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 data and validation recommendations.

Overall Evaluation of Data and Potential Usability Issues

These data are intended for use in site characterization and risk assessment. Target quantitation limits for groundwaters were based on US Environmental Protection Agency Maximum Contaminant Levels (MCLs) for drinking water, and New Hampshire GW-1 groundwater criteria, as summarized on Table C.6 of the Work Plan (attached with DQO form). The desired quantitation limits were met for these samples.

Several analytes had calibration checks that did not meet criteria. Associated sample results are usable, but have been estimated to indicate uncertainty in quantitation.

TKN was detected in an equipment blank. Sample concentrations within five times the blank result have been converted to nondetects due to the possibility of false positives. The

T BW223 Inorganic Data Validation; Page 3 O'Reilly, Talbot & Okun <— aoauaaffi —>

[ A S S O C I A T E S ] I

field duplicates for TKN showed high variability. Other analytes in the field duplicates had acceptable precision, suggesting the TKN may have been due to contamination which occurred during sample collection or handling.

Nitrate, o-phosphate and chloride have been estimated in some samples due to matrix spike results which indicate possible low bias. Concentrations of other constituents in the samples may interfere with these analyses.

Antimony results were estimated due to variable instrument response at the low requested detection limit. Antimony was run by the method of standard additions. Analytical curves were not linear, due in large part to poor response at the low end of the curve. Antimony was nondetect in samples. Those results are usable but estimated.

The quantitation limit for mercury was increased from the reported value of 0.5 ug/1 to 1.0 ug/1 in the groundwater samples. The lab's method detection limit (MDL) study reported an MDL of 0.6 ug/1. Recoveries for the quantitation limit standard were low, indicating response at 0.5 ug/1 is variable. The elevated quantitation limit is still below the drinking water standard, therefore data usability has not been significantly impacted.

The following sections provide further information on this sample delivery group.

Holding Times

The nitrate and o-phosphate 48 hour holding times were exceeded for seven of the original samples submitted. The lab notified SHA, and replacement samples were collected. Replacement samples were identified with an "R" suffix. Holding times were met for these replacements. Results are reported for samples analyzed within holding time. No validation action was required on this item.

Initial and Continuing Calibrations

The QAPP requires analysis of continuing calibration checks after every 10 samples for most inorganic parameters. This was generally performed. However, ICP sequences sometimes included 11 runs prior to the calibration check. Standards and QC sample results indicate instrument response was stable in these instances, therefore sample data were not affected by this deviation. The laboratory should perform calibration checks at the appropriate frequency to document on-going instrument response.

Several analytes had calibration checks which did not meet recovery criteria. These calibrations and actions taken on associated samples are summarized below. Low recoveries indicate potential low bias in sample data, therefore associated detects and nondetects are estimated. High recoveries indicate potential high bias; nondetects are acceptable in this circumstance. When the quantitation limit standard varied by more than 20% from true, results below 3 times the quantitation limit were estimated Q/UJ) due to variable response at the low end of the calibration range.

T BW223 Inorganic Data Validation; Page 4 iMnraaani O'Reilly, Talbot & Okun

[ A S S O C I A T E S ]

Analyte Cal. Standard Action Affected Samples Recoveries

Beryllium 80%, 87% J detects/UJ nondetects SH-22R, SH-53S, WS-1, OW-223A-R

<i 51% (QL) J detects/UJ nondetects SH-22R, SH-53S, WS-1, below 3*QL (raw) OW-223A-R

Lead 114.5% J detects none; samples were nondetect

Mercury 32% QL raised; see Detection SH-22R, SH-53S, WS-1, Limit section OW-223A-R

Nickel 71% (QL) J detects/UJ nondetects SH-22R, SH-53S, WS-1, below 3*QL (raw) OW-223A-R

Nitrate 93% J detects/UJ nondetects SH-22R, SH-53S, WS-1

Potassium 49% (QL) J detects/UJ nondetects AE-11S, SH-5S, OW-223A-R below 3*QL (raw)

Thallium 130% (QL) J detects/UJ nondetects SH-22R, SH-53S, WS-1, below 3*QL (raw) OW-223A-R

Notes: "QL" indicates lowest standard, at quantitation limit. If not specified, standard was a midrange continuing calibration check.

There were no reportable concentrations of target analytes in lab blanks. Two equipment blanks were submitted with the SDG: OW-223A-P, which was collected with a peristaltic pump, and OW-223A-R, which was collected with a Redi-Flo submersible pump. TKN was reported in one equipment blank, OW-223A-R. Three of the samples in this SDG were collected with the Redi-flo pump: SH-22R, SH-53S and WS-1. Equipment blank OW-223A-R would usually be applicable only to those three samples. However, in this case, professional judgment was used to apply actions to all samples in this SDG. Field duplicate results (discussed in a later section) were acceptable for all analytes except TKN. This suggests TKN may be a contaminant in those samples as well, and they were collected with the peristaltic pump. Based on this information, blank actions were applied to TKN results in all samples, not just those collected with the Redi-flo pump. Results less than five times the blank concentration are considered nondetects due to possible false positives, and sample-specific quantitation limits raised to the detected value, as shown below.

Analyte Cone, in Equip. Action Affected Samples Blank

TKN 0.2 mg/1 Report results below 1.0 BR-28, SH-5S, mg/1 (raw) as nondetects SH-10S, WS-1, ("U"); elevate quantitation OW-223 limits to detected values

T BW223 Inorganic Data Validation; Page 5 KIHI.I«:II:II O'Reilly, Talbot & Okun

[ A S S O C I A T E S ]

Matrix Spike Results/Lab Duplicates

Lab precision and accuracy was assessed by means of a matrix spike/matrix spike duplicate pair (MS/MSD). Cadmium had a nigh recovery (185%) in one of the matrix spike samples. As a result, cadmium was analyzed by the method of standard additions (MSA) in this SDG. No action was taken on cadmium matrix spike results because MSA accounts for matrix effects in individual samples.

Other metals had acceptable recoveries and duplicate precision in the MS/MSD. The water quality parameters nitrate, o-phosphate and chloride had acceptable precision, but did not meet recovery criteria. Noncompliant results and actions taken on associated samples are summarized below. In some instances an MS/MSD pair was run on each date of analysis instead of just once per 20 samples. Action has been applied to samples analyzed on the same date in this situation.

Analyte Sample Recoveries Action Affected Samples

o-Phosphate SH-6S 38%, 46% J detects/UJ BR-25, BR-28, SH-6S, SH-10S nondetects

Nitrate AE-16 81%, 85% J detects/UJ BR-25, BR-28, SH-6S, SH-10S nondetects

ct OW-223 75%, 75% J detects/UJ AE-8, AE-9, AE-11S, AE-16, nondetects SH-5S, SH-7S, OW-223,

OW-223A-P, OW-223A-R

Chloride SH-22R 77%, 73% J detects/UJ SH-22R, SH-53S, WS-1 nondetects

The lab narrative indicates low nitrate recoveries are due to colored samples, which produce positive interference with nitrite results. Subtraction of high-biased nitrite concentration from the combined result yields a low-biased nitrate result. Additionally, the combined result may be low due to the presence of petroleum and high iron concentrations, which can cause poor column efficiency. Due to the prevalence of these issues with nitrate analysis, nitrate results for all of the samples in this SDG are considered estimates.

A post-digest spike (PDS) was performed for the ICP elements. Iron and magnesium recoveries fell below the acceptance range of 75-125%. However, in each case, the native (unspiked) sample concentration was more than five times the spike level. Results of the PDS were therefore accepted, as a spike cannot be reliably detected in the presence of an overwhelming sample concentration.

Field Duplicates

The field duplicates were submitted to the lab single-blind, identified as samples AE-9 and OW-223. Metals results showed acceptable precision. The TKN results had an unacceptably high relative percent difference (67%; the acceptance criterion is <30%).

I BW223 Inorganic Data Validation; Page6 O'Reilly, Talbot & Okun <— ammaaau —>

[ A S S O C I A T E S ] I

TKN detections in all groundwater samples in this SDG are therefore estimated to indicate sampling and/or analytical uncertainty. The acceptable precision observed for other analytes indicates the TKN variability is isolated, and may be due to either analytical error or contamination introduced during collection/handling.

Furnace Atomic Absorption Results

The graphite furnace atomic absorption (GFAA) method used for these analyses does not require duplicate injections for each run. However, the laboratory performed them for some runs, therefore duplicate injection results were assessed. This is a Tier III activity, as it requires a review of raw instrument printout to locate duplicate results and relative percent differences (RPDs). Duplicate injection RPDs were acceptable for results above the quantitation limit.

Cadmium and antimony were analyzed by the method of standard additions (MSA) due to unacceptable matrix spike recoveries. Matrix spike results were not reported due to use of MSA, which accounts for the individual sample matrix by creating a calibration curve within the sample digestate. Linearity of the MSA curve is acceptable if the correlation coefficient is _>0.995. Correlation coefficients for cadmium did not meet that criterion in two instances: once in a calibration check and once in the PES. No action is taken on either of those runs, as validation actions apply only to sample data.

Antimony MSA curves were not linear, and the lab inappropriately dropped standards from midrange to achieve acceptable correlation coefficients in the four samples analyzed (supporting raw data attached). Additionally, the lowest spike addition (6 ug/1) was frequently indistinguishable from the unspiked sample. The spike concentration corresponds to 3 ug/1 antimony in the samples, which were run at 2X concentration. The lab's reported detection limit was 6 ug/1. The lowest standard addition that was reliably detected was 10 ug/1, which corresponds to 5 ug/1 in samples. The reported quantitation limit of 6 ug/1 was therefore used, but estimated due to analytical variability at low concentrations. Antimony was nondetect in the four samples analyzed (SH-22R, SH-53S, WS-1 and OW-223A-R); those results have been flagged "UJ".

The sample result pages listed the method reference for copper as "200.9", which is a GFAA method. Copper was analyzed by ICP, not GFAA. This was confirmed with the laboratory to be an error (correspondence attached). The reference should be corrected to "200.7" on each sample result sheet.

Serial Dilution Results

The ICP serial dilutions for this SDG met criteria. NHDES inadvertently used a draft version of QAPP Table 6m which listed "RPD" as the means of assessing serial dilutions, rather than "%D" as was correctly listed in the 11/97 QAPP. The correct calculation was made by the validator; project criteria were met for this parameter. NHDES will include the correct calculation in future submittals.

T BW223 Inorganic Data Validation; Page 7 O'Reilly, Talbot & Okun <— ^maas

[ A S S O C I A T E S ] I

Detection Limit Results

Method detection limit (MDL) studies were submitted as part of laboratory prequalification for this project, and were not included in the data packages. The study for mercury in aqueous samples reported an MDL of 0.6 ug/1. The samples in this SDG were reported down to 0.5 ug/1. The low standard (0.5 ug/1) dropped to a reading of 0.16 ug/1 at the end of the run sequence. This indicates possible low bias or false negative results for samples. Due to analytical uncertainty at the low reported level, the quantitation limit for mercury has been raised from 0.5 to 1.0 ug/1 in this SDG.

Performance Evaluation Samples

Three aqueous performance evaluation sample (PES) were submitted with this SDG: 0013265 for GFAA and ICP metals; HG9801091 for mercury and PB531 for nitrate. PES score reports from EPA are attached.

Mercury and the seven metals targets metals in PES 0013265 scored within limits, indicating good analytical accuracy for metals. Nitrate scored warning low, indicating sample results may be slightly low-biased. Per Region I guidance, no validation action is taken on warning scores.

Sample Results and Reported Quantitation Limits

Iron and manganese analyses were requested on both a total and dissolved basis. Original result sheets from the lab had a note in the "Client's Comments" section which indicated "DISS. METALS" on what appeared to be the total metals results for three samples (AE-8, AE-11S and SH-5S). The lab checked their records and corrected those sheets to indicate "TOTAL METALS" (correspondence attached).

Several samples had iron and/or manganese results which exceeded the upper limit of the initial calibration. However, a high concentration standard identified as "High Analyte" in the data package was analyzed separately. Results for that standard indicate the linear ranges for iron and manganese extend above the measured sample concentrations. Sample results are therefore considered acceptable and were not qualified based on exceeding the initial calibration range.

The lab was inconsistent in their use of significant figures, reporting up to three figures on analytical result sheets. The validator reduced the number of significant figures to two in these instances.

BW223 Inorganic Data Validation; Page 8 MIilMflKI O'Reilly, Talbot & Okun <­

[ A S S O C I A T E S ]

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

Very truly yours,

Valerie "Data V

;s D. Okun .cipal

cc: D. Szaro/EPA QA (with all attachments) W. Ives/NHDES Site Manager (memo + tables only) J. DiLorenzo/EPA Site Manager (memo + tables only) P. Bickford/NHDES Lab (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 Table Data Validation Worksheets PES Score Reports (3) Communication/Phone Logs Supporting Raw Data CSF Audit (DC-2 Form) DQO Summary Form with attached Table C.6 from Work Plan

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