DATA USABILITY SUMMARY SPL LABORATORY REPORT … · These three types of reviews are discussed further in Sections 2.0, 3.0, and 4.0 of this Data Usability Summary (DUS) report, respectively.

DATA USABILITY SUMMARY

SPL LABORATORY

REPORT NUMBERS 07010444 AND 07010521

GENEVA INDUSTRIES

SHAW ENVIRONMENTAL, Inc. PROJECT NUMBER 124518

Prepared by

Shaw Environmental, Inc. 3010 Briarpark Drive, Suite 400

Houston, Texas 77042

January 29, 2007

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Appendix Not Included


SPL LABORATORY REPORT NUMBERS 07010444 AND 07010521

GENEVA INDUSTRIES

January 29, 2007

Approved by: Date: Diane Meyer, Project Chemist

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SPL LABORATORY REPORT NUMBERS 07010444 AND 07010521

GENEVA INDUSTRIES

TABLE OF CONTENTS

Page ACRONYMS AND ABBREVIATIONS ..........................................................................................v

1.0 INTRODUCTION............................................................................................................... 1-1

2.0 LABORATORY REVIEW CHECKLIST REVIEW CRITERIA ...................................... 2-1 2.1 Initial Calibration ....................................................................................................... 2-1 2.2 Initial and/ or Continuing Calibration Verification.................................................... 2-1 2.3 Internal Standard Data................................................................................................ 2-1 2.4 Dual Column Confirmation Results........................................................................... 2-1 2.5 ICP Interference Check Sample (ICS), Serial Dilution, and Post-Digestion Spike ... 2-1 2.6 Other Items Identified in the LRC Narrative ............................................................. 2-2

3.0 FIELD AND LABORATORY DATA PACKAGE REVIEW ........................................... 3-1 3.1 Holding Times............................................................................................................ 3-1 3.2 Blanks......................................................................................................................... 3-1 3.3 Surrogate Recoveries ................................................................................................. 3-1 3.4 Laboratory Control Sample (LCS) Results ................................................................ 3-2 3.5 Matrix Spike Sample Analysis................................................................................... 3-2 3.6 Duplicate Sample Analysis ........................................................................................ 3-2 3.7 Field Duplicate Results .............................................................................................. 3-2

4.0 VALIDATION REVIEW CRITERIA ................................................................................ 4-1

5.0 DATA REVIEW RESULTS............................................................................................... 5-1 5.1 Laboratory Data Package Review.............................................................................. 5-1

5.1.1 Review of the Laboratory Review Checklist ............................................... 5-1 5.1.2 Holding Times ............................................................................................. 5-1 5.1.3 Blanks .......................................................................................................... 5-2 5.1.4 Laboratory Control Sample Recovery ......................................................... 5-2 5.1.5 Matrix Spike/Matrix Spike Duplicate Recoveries ....................................... 5-2 5.1.6 Surrogate Recoveries ................................................................................... 5-2 5.1.7 Sample Duplicate Agreement ...................................................................... 5-2

5.2 Field Duplicate Result Agreement ............................................................................. 5-2

6.0 DATA VALIDATION RESULTS...................................................................................... 6-1

7.0 OVERALL ASSESSMENT................................................................................................ 7-1 7.1 Accuracy .................................................................................................................... 7-1 7.2 Precision..................................................................................................................... 7-1 7.3 Completeness ............................................................................................................. 7-1 7.4 Representativeness ..................................................................................................... 7-1

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TABLE OF CONTENTS (Continued)

Page

iv

7.5 Comparability............................................................................................................. 7-1 7.6 Sensitivity................................................................................................................... 7-2

8.0 DATA USABILITY RELATIVE TO PROJECT OBJECTIVES....................................... 8-1 8.1 Sample Quantitation Limits and Decision Criteria Comparison................................ 8-1 8.2 Effects of Potential Biases and Imprecision on Usability of the Data ....................... 8-2 8.3 Representativeness ..................................................................................................... 8-3

9.0 POTENTIAL ADDITIONAL DATA USES AND LIMITATIONS.................................. 9-1

10.0 CORRECTIVE ACTIONS AND WORKPLAN DEVIATIONS ..................................... 10-1

11.0 REJECTED DATA AND PROJECT CONSEQUENCES ............................................... 11-1

12.0 CONCLUSIONS............................................................................................................... 12-1 LIST OF TABLES Table 1-1 Sample Field and Laboratory ID Numbers ............................................................... 1-2 Table 1-2 Data Validation Qualifier Definitions....................................................................... 1-3 Table 1-3 Data Validation Qualifier Codes............................................................................... 1-4 Table 5-1 Sample and Associated QC Designations................................................................. 5-1 Table 5-2 Field Duplicate Comparison ..................................................................................... 5-3 Table 8-1 Sample Quantitation Limits and QAPP Decision Criteria Comparison ................... 8-2 APPENDICES APPENDIX A – Data Reporting Forms – SPL Laboratories Nos. 07010444 and 07010521 Including COC and Laboratory Review Checklist

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ACRONYMS AND ABBREVIATIONS BTEX benzene, toluene, ethyl benzene, and xylenes

COC chain of custody

GC gas chromatograph

LCS laboratory control sample

LCSD laboratory control sample duplicate

MQL method quantitation limit

MS matrix spike

MSD matrix spike duplicate

PCB polychlorinated biphenyl

QA quality assurance

QAPP Quality Assurance Project Plan

QC quality control

RPD relative percent difference

SOP Standard Operating Procedure

SQL sample quantitation limit

TCE trichloroethene

TCEQ Texas Commission on Environmental Quality

TOC total organic carbon

USEPA United States Environmental Protection Agency

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TCEQ Shaw Project No. 124518 Geneva Industries Federal Superfund Site January 2007

1-1

DATA USABILITY SUMMARY SPL LABORATORY

REPORT NUMBERS 07010444 AND 07010521 GENEVA INDUSTRIES

1.0 INTRODUCTION

This report contains the results of the data evaluation conducted for groundwater samples collected and analyzed as part of the site investigation at the Texas Commission on Environmental Quality (TCEQ), Geneva Industries for the Engineering Superfund Contract #5826-49221. Nine monitoring well samples, one field blank, one field duplicate, and two trip blanks were collected. These samples were analyzed by SPL Laboratories (Houston, Texas) in accordance with the approved site Quality Assurance Project Plan (QAPP) (200919.3) and the analytical methods specified for the analytes requested on the Chain of Custody (COC) documentation. The analytes requested for the groundwater samples were oil and grease, total organic carbon (TOC), benzene, toluene, ethyl benzene, and xylenes (BTEX) plus trichloroethene (TCE), total dissolved solids (TDS), and polychlorinated biphenyls (PCB). Table 1-1 provides a list of the samples collected, a laboratory sample number cross-reference, sample matrix, COC number, date collected, sample purpose, and analytical method performed for each sample. This DUS report includes a data review and a data validation for the PCB results and a data review for all results in accordance with Section D of the QAPP. The data were generated and reviewed in accordance with the site QAPP. The analytical results were reported in laboratory data packages 0701044 and 07010521. The data were evaluated against the quantitative acceptance limits given in the site QAPP for the data quality parameters of sensitivity, accuracy, precision, and completeness. The data were also evaluated for fulfillment of the qualitative data quality assurance parameters of representativeness and comparability as defined in the site QAPP. Appendix A contains the Laboratory Data Packages containing the Laboratory Review Checklist (LRC) and associated Exception Reports and the Required Reportable Data as specified in Element A.9.2 of the program QAPP and supporting data for validation. In accordance with the site QAPP, a review of the data was conducted independent of the laboratory. This review consisted of an evaluation of laboratory performance criteria from the Laboratory Review Checklist (LRC), an evaluation of the sample-specific criteria included in the laboratory data package in accordance with the site QAPP, and validation of calculations and data transcriptions using guidance from the February 1994 USEPA National Functional Guidelines for Inorganic Data Review (NFG) nd USEPA Contract Laboratory Program, National Functional Guidelines for Organic Data Review, (October 1999). The independent data review included three levels of data review. These three levels are summarized below. The first level of review consists of an evaluation of the laboratory performance criteria based on review of the LRC and associated Exceptions Reports. The laboratory performance parameters evaluated included: initial calibration procedures and results, continuing calibration procedures and results, interference check sample (ICS) analysis, post-digestion spike recoveries, ICP serial dilution, and other items identified as “supporting data” in the LRC. The second level of review consists of an evaluation of the sample-specific criteria included in the laboratory data package and an evaluation of the field data. The sample specific evaluation parameters include holding time, blank contamination, laboratory control sample analysis (LCS), and matrix spike (MS) and matrix spike duplicate (MSD) sample analyses. Field quality control samples were taken for comparison to project decision criteria.

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The third level of review consists of validation back to the raw data for evaluation of laboratory performance related to calculation, data transcriptions and chromatographic and spectrometric performance. Raw data were provided for the PCB fraction and a third level review was performed. These three types of reviews are discussed further in Sections 2.0, 3.0, and 4.0 of this Data Usability Summary (DUS) report, respectively. The results of the data review and validation are presented in Sections 5.0 and 6.0, respectively. An overall assessment of the data relative to the quantitative and qualitative data quality assurance parameters is provided in Section 7.0. Section 8.0 presents an evaluation of the quality and usability of the data in regards to project decisions.

Table 1-1 Sample Field and Laboratory ID Numbers

Field I.D. Lab Sample

Number

Matrix Date

Collected

Purpose Analytical Methods –

SW-846 MW-10 07010444-01 Water 1/9/07 Field sample Oil & Grease -1664

TOC – 415.1 PCB – 8082 BTEX, TCE – 8260B TDS – 160.1

MW-11 07010444-02 Water 1/10/07 Field sample Oil & Grease -1664 TOC – 415.1 PCB – 8082 BTEX, TCE – 8260B TDS – 160.1






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Table 1-1 Sample Field and Laboratory ID Numbers (continued)


Number

Matrix Date

Collected

Purpose Analytical Methods –

SW-846 MW-25 07010444-10 Water 1/9/07 Field sample Oil & Grease -1664

TOC – 415.1 PCB – 8082 BTEX, TCE – 8260B TDS – 160.1

WE-3 07010444-11 Water 1/10/07 Equipment blank BTEX, TCE – 8260B WT-3 07010444-12 Water 1/10/07 Trip blank BTEX, TCE – 8260B


WD-3 07010521-02 Water 1/11/07 Field duplicate of MW-26

Oil & Grease -1664 TOC – 415.1 PCB – 8082 BTEX, TCE – 8260B TDS – 160.1

WT-4 07010521-03 Water 1/11/07 Trip blank BTEX, TCE – 8260B a USEPA, 1997. Test Methods for Evaluating Solid Waste, Physical/Chemical Methods (SW-846), Update III. Office of Solid Waste and Emergency Response, Washington, D.C.

Following the specifications in the site QAPP related to the data validation process, the data were annotated with validation qualifiers (“U”, “J”, “UJ” and “R”) and associated bias codes on the analytical data sheets. Table 1-2 provides definitions of the data qualifiers and Table 1-3 lists and defines the data qualifiers and bias codes.

Table 1-2

Data Validation Qualifier Definitions

QUALIFIER DEFINITIONS U

Not detected: The analyte was analyzed for, but was not detected above the level of the associated value. The associate value is the sample quantitation limit (SQL).

J Estimated: The analyte was detected and positively identified. The associated numerical value is the approximate concentration of the analyte in the sample.

UJ Not detected, SQL is estimated: The analyte was analyzed for, but was not detected above the reported SQL. However, the reported SQL is an estimate and may be inaccurate or imprecise.

R Rejected: The data are unusable. (Note: The presence or absence of the analyte cannot be confirmed.)

.

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Table 1- 3 Data Validation Qualifier Codes

QUALIFIER CODE

DATA QUALITY CONDITION

RESULTING IN ASSIGNED QUALIFICATION General Use FB Field blank contamination FD Field duplicate evaluation criteria not met HT Holding time requirement was not met LCS Laboratory control sample evaluation criteria not met MB Method blank or preparation blank contamination RB Rinsate blank contamination TB Trip blank contamination SQL Sample quantitation limit exceeds decision criteria (for nondetects) Inorganic Methods CCB Continuing calibration blank contaminationCCV Continuing calibration verification evaluation criteria not met D Laboratory duplicate precision evaluation criteria not metDL Serial dilution results did not met evaluation criteriaICS Interference check sample evaluation criteria not metICV Initial calibration verification evaluation criteria not metMS Matrix spike recovery outside acceptance rangePDS Post-digestion spike recovery outside acceptance rangeMSA Method of standard additions correlation coefficient < 0.995 PB Preparation blankOrganic Methods CCAL Continuing calibration evaluation criteria not met ICAL Initial calibration evaluation criteria not met ID Target compound identification criteria not met IS Internal standard evaluation criteria not met MS/MSD Matrix spike/matrix spike duplicate accuracy and/or precision criteria not met SUR Surrogate recovery outside acceptance range TUNE Instrument performance (tuning) criteria not met P The detected concentration difference between the primary and secondary

column is greater than 25%. Bias Codes H

Bias in sample result likely to be high

L Bias in sample result likely to be low I Bias in sample result is indeterminate

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2.0 LABORATORY REVIEW CHECKLIST REVIEW CRITERIA

The data review by the analytical laboratory included a through review of laboratory and sample-specific performance criteria. Any results not meeting the QC acceptance criteria were documented by the laboratory in the Laboratory Review Checklist (LRC) and associated Exception Reports (Appendix A). The laboratory performance criteria evaluated from the LRC include: initial calibration procedures and results, continuing calibration procedures and results, ICP interference check sample, and other items identified in the LRC as potentially affecting the data. The sample specific criteria reviewed from the LRC include: ICP serial dilution and post-digestion spike recoveries. The subsections below discuss how each of the parameters was evaluated, as specified in the Superfund QAPP section B.5. If the Exception Report described a criterion not covered by the subsections below, the data were evaluated and qualified using guidance from the Functional Guidelines as applicable to the analytical method.

2.1 Initial Calibration

The Superfund Program QAPP (element B.5) contains the QC acceptance criteria for initial calibration for analytical methods required for the project. If the LRC indicated that the initial calibration for any analyte did not met the acceptance criteria, then the Exception Report was evaluated and all results for that given analyte associated with the initial calibration were qualified estimated (“J/UJ”) with a qualifier code of “ICAL” and a bias code of “I” for indeterminate direction of bias.

2.2 Initial and/ or Continuing Calibration Verification

The QAPP contains the QC acceptance criteria for initial and continuing calibration verification for each analytical method used in the project. If the LRC indicates that the initial or continuing calibration verification for any analyte did not meet the acceptance criteria, then all results for that given analyte associated with the initial or continuing calibration verification were qualified as estimated (“J/UJ”) with a qualifier of “ICV” or “CCV” for inorganics and “CCAL” for organics. If a direction of bias could be discerned, then the appropriate qualifier bias codes were assigned.

2.3 Internal Standard Data

Element B.5.1 contains the QC acceptance criteria for internal standard area counts and retention times for GC/MS organic analyses. If the LRC indicates that the internal standard area counts are below the lower acceptance limit, then results reported as not-detected, were qualified as estimated (“UJ”) and results reported as detected did not require qualification. If the exception report indicated that the internal standard area count was above the upper acceptance limit, then results reported as detected or as not-detected were qualified as estimated (“J/UJ”). A qualifier code of “IS” was applied.

2.4 Dual Column Confirmation Results

Dual column confirmation is not required for PCB analyses (B.5.1.6).

2.5 ICP Interference Check Sample (ICS), Serial Dilution, and Post-Digestion Spike

Metals were not required and these sections are not applicable.

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2.6 Other Items Identified in the LRC Narrative

Other items for which the laboratory may provide an Exception Report related to data not contained in the laboratory data package may include: tuning, system performance evaluation mixture analysis, internal standard area counts, Methods of Standard Additions, and method or SOP deviations. If an Exception Report describes a laboratory performance criterion not covered by the Superfund QAPP, the data should be evaluated and qualified using guidance from the Functional Guideline as applicable to the analytical method or professional judgment should be used.

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3.0 FIELD AND LABORATORY DATA PACKAGE REVIEW

The sample specific evaluation parameters include: holding times, blank contamination, laboratory control sample (LCS) analysis, matrix spike (MS), matrix spike duplicate (MSD), field duplicate results, and equipment rinsate blank results. The subsections below discuss how each of these sample specific parameters was evaluated. No field analytical data were collected during this phase of the project; all analytical data were generated by an off-site or fixed laboratory. Therefore, no field data review crieteria are specified in this data useability summary.

3.1 Holding Times

Holding times were calculated by computing the difference between the sample collection date found on the COC and the sample analysis date found on the sample test reports. The technical holding time specified in the QAPP for aqueous volatiles is 14 days until analyses. The technical holding time for PCB in water is 7 days for extraction and 40 days after extraction until analyses. For oil and grease, the holding time is 28 days, for TDS the holding times is 7 days, and the holding time for TOC is 28 days from collection. Results for analyses not performed within holding time limits were qualified as estimated (“J/UJ”).

3.2 Blanks

The results for field blanks, trip blanks, preparation blanks, and calibration blanks were reviewed. Sample results for analytes detected in an associated blank at concentrations less than five times the blank concentration were qualified as non-detect (“U”). Negative blank concentrations were evaluated for potential effects (bias low) on sample data when the absolute value of the negative concentration was greater than the analyte method quantitation limit. If the negative concentration in a blank may have produced more than a 25% effect on a reported sample results, the associated sample result was qualified as estimated (“J/UJ”). Preparation blanks are associated with all samples prepared with that sample. If contamination was noted in a continuing calibration blank, the samples preceding and following that blank were evaluated for potential effects.

3.3 Surrogate Recoveries

Results for the surrogate recoveries were compared to the organic QAPP Element D.1.1 acceptance range of 60 -140%. Results for analytes outside in the sample associated with surrogate recoveries outside the acceptance range were qualified as follows:

• If the surrogate is >140% all positive results for the associated analytes were qualified estimated (“J”) with a bias high; whereas non-detect results are acceptable without qualification. (For GC/MS semivolatiles two or more surrogates in either fraction shall be high).

• If the surrogate recovery is less than 60%, but greater than 10%, the associated analytes were qualified estimated (“J/UJ”) with bias low.

• If any surrogate is <10%, positive results shall be qualified estimated (“J”) with low bias and non-detects shall be qualified as unusable (“R”).

A qualifier code of “SUR” shall be assigned to all results qualified or rejected on the basis of surrogate recoveries.

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3.4 Laboratory Control Sample (LCS) Results

The LCS recoveries were compared to the organic QAPP acceptance criterion of 60 – 140% for PCB and volatiles. For the general chemistry analyses, the LCS recoveries were compared to the QAPP acceptance range of 70 – 130% for inorganic compounds. Positive results associated with LCS outside QC limits, but > 30% (inorganics) or > 10% (organics) were qualified as estimated (“J”); non-detects sample results associated LCS recoveries lower than the lower limit but above 30%(inorganics) or 10% (organics) were qualified “UJ”; and non-detect sample results associated with LCS recoveries greater than the upper limit did not require qualification. Sample results associated with a LCS recovery < 30% (inorganics) or <10% (organics) were considered to be unusable (“R”).

3.5 Matrix Spike Sample Analysis

The analyte recoveries for PCB and volatiles obtained for matrix spike analyses were compared to the organics acceptance range of 60-140% specified in the site QAPP for cases in which the native sample concentration was less than four times the spike concentration (as specific in the NFG). Data associated with MS or MSD recoveries outside the acceptance range follow the same criteria as the surrogate recoveries. In addition the relative percent difference (RPD) between the MS and MSD shall be compared to the acceptance criteria in Table D-1 of 40%. If the RPD exceeds 40%, the data shall be qualified as estimated (“J/UJ”). No qualification of associated samples in the batch or data package shall be performed on the basis of matrix spike recoveries alone. Professional judgment and consideration of other QC measure such as surrogate recoveries in conjunction with MS/MSD results, to determine the need for qualification of associated samples. For the inorganic parameter, the acceptance range is 70 – 130% for cases in which the native sample concentration was less than four times the spike concentration. If the matrix spike recovery was > 130%, suggesting a potential high bias, all positive results for that analyte in the data package were qualified as estimated (“J”) whereas non-detect results were considered to be acceptable for use without qualification. If the matrix spike recovery for an analyte was < 70% but > 30%, suggesting a potential low bias in reported results, positive and non-detect results were qualified as estimated (“J/UJ”). If the matrix spike recovery for an analyte was < 30%, positive sample results were qualified as estimated (“J”) whereas non-detect results were qualified as unusable (“R”).

3.6 Duplicate Sample Analysis

Results for the laboratory duplicate sample analyses were compared to the acceptance criteria in QAPP Element D.1.1. The RPD criterion of < 30% for inorganics and < 40% for organics was applied for cases in which both the sample and duplicate results were greater than five times the method quantitation limit. Otherwise, the absolute difference between the samples was compared to one times the greater sample quantitation limit for aqueous samples and two times greater sample quantitation limit for solid samples. If the duplicate results for an analyte did not satisfy the applicable evaluation criterion, results for that analyte in all associated samples were qualified as estimated (“J/UJ”).

3.7 Field Duplicate Results

Results for field duplicate sample analyses were compared to the following concentration-dependent acceptance criteria. The RPD criterion < 30% for aqueous samples, was applied for cases in which both the sample and duplicate results were greater than 5 times the method quantitation limit. Otherwise, the absolute difference between the sample results was compared to 2 times the greater sample quantitation (for aqueous samples). If the field duplicate results for an analyte did not satisfy the applicable criterion, results for that analyte in all associated samples were qualified (“J/UJ”).

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4.0 VALIDATION REVIEW CRITERIA

As specified in the QAPP, validation of project data is performed on ten percent of the project data package. In this case data validation was performed on the PCB data. Validation of analytical data package was performed following the protocol specified in the TCEQ QAPP. Data validation is implemented to provide a quality check on the laboratory system generating the data. The data validation process consisted of reviewing supplemental raw data supplied with the analytical data package. The supplemental raw data included the following:

• Initial calibration data for the method including all raw data for each calibration standard and the quantitation report for the calibration.

• Continuing calibration data for the method including raw data for the calibration standard and the quantitation report for the calibration.

• Instrument run logs documenting the laboratory analysis of the samples. • All raw data for each sample reported in the analytical data package. • Ten percent of the data were checked for transcription and calculation errors. No data used for

decision-making on the project was generated in the field.

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5.0 DATA REVIEW RESULTS

5.1 Laboratory Data Package Review

The samples reported in packages 07010444, 07010521, and the QC designations are listed in Table 5-1. Samples were analyzed for benzene, toluene, ethylbenzene, total xylenes, and trichloroethylene by gas chromatography/mass spectrometry (GC/MS), SW-846 method 8260B. Samples for PCB were analyzed by gas chromatography (GC), SW-846 method 8082. Also samples were analyzed for general chemistry parameters - total organic carbon by EPA method 415.1, Oil and Grease by EPA method 1664, and total dissolved solids by EPA method 160.1. The data packages were reviewed in accordance with the approved Superfund Site QAPP (200919.3)

Table 5-1 Sample and Associated QC Designations


Number

Matrix Date

Collected

QC Designation MW-10 07010444-01 Water 1/9/07 Field sample MW-11 07010444-02 Water 1/10/07 Field sample MW-17 07010444-03 Water 1/10/07 Field sample MW-8 07010444-06 Water 1/9/07 Field sample

MW-22 07010444-07 Water 1/10/07 Field sample MW-23 07010444-08 Water 1/9/07 Field sample MW-24 07010444-09 Water 1/9/07 Field sample MW-25 07010444-10 Water 1/9/07 Field sample WE-3 07010444-11 Water 1/10/07 Equipment blank WT-3 07010444-12 Water 1/10/07 Trip blank

MW-26 07010521-01 Water 1/11/07 Field sample WD-3 07010521-02 Water 1/11/07 Field duplicate of MW-26 WT-4 07010521-03 Water 1/11/07 Trip blank

5.1.1 Review of the Laboratory Review Checklist

Items identified in the LRC as outside of control limits for laboratory performance criteria were evaluated for data packages 07010444 and 07010521. The evaluation of laboratory performance criteria was conducted as summarized in Section 2.0 above and sample-specific criteria as summarized in Section 3.0 above. The COC was complete and contained the required information The actual methods used for sample analysis were based upon the COC. All samples arrived at the laboratory intact, on time, and within acceptable temperature range. A copy of the COC and cooler receipt form are included with the data package.

5.1.2 Holding Times

Holding times were calculated by computing the difference between the sample collection date found on the COC and the sample analysis date found on the sample test reports. The technical holding time specified in the TCEQ QAPP for PCB Aroclors is 7 days to extraction for water samples and 40 days to analyses. The holding time for volatiles is 14 days until analyses. The technical holding time for the

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following general chemistry parameters are: total organic carbon (TOC) is 28 days, total dissolved solids is 7 days, and oil and grease is 28 days. These samples were analyzed within the required holding time. No qualification of the data is required due to hold time violation.

5.1.3 Blanks

No target analytes were detected in the aqueous preparation blanks, equipment blank, and trip blanks. The continuing calibration blanks (CCB) bracketing the Geneva samples in SDG 0701044 contained TOC at 0.353mg/L and 0.425 mg/L. Samples < five times the CCB (up to 2.215 mg/L) were qualified “U” with validation code “CCB”. The affected samples, which were qualified “U”, were MW-17, MW-8, MW-22, MW-23, MW-24, and MW-25.

5.1.4 Laboratory Control Sample Recovery

The percent recoveries for the LCS for PCBs and volatiles were within the QAPP specified control limits of 60 - 140%. The general chemistry parameter recoveries were within the QAPP specified control limits of 70 – 130%. Therefore, no data qualification is required based on LCS recoveries, indicating that satisfactory levels of accuracy for analyses on a clean matrix were achieved.

5.1.5 Matrix Spike/Matrix Spike Duplicate Recoveries

The percent recoveries for the MS/MSD for volatiles and PCB were within the QAPP specified control limits of 60 - 140%. The general chemistry MS recoveries were within the 70 – 130% recovery. There was insufficient sample volume for a MSD for the oil and grease analyses. The laboratory analyzed a MS and a LCS/LCSD for precision. These recoveries were within the TCEQ guidelines. The relative percent difference (RPD) for the MS/MSD was within the QAPP limits of 30% for inorganics and 40% for organic analytes.

5.1.6 Surrogate Recoveries

The surrogates were within quality control limits of 60 – 140% for the volatile data. The surrogate decachlorobiphenyl was below the lower control limit of 60% for samples MW-26 (52%) and WD-3 (58%). The samples were non-detects for all aroclors and each aroclor was qualified “UJ-SUR-L” for these two samples.

5.1.7 Sample Duplicate Agreement

The sample duplicate analyses for TDS agreed within a RPD of 30%.

5.2 Field Duplicate Result Agreement

The field duplicates were evaluated using the criteria described in Section 3.7. Results for field duplicate sample analyses were compared to the following concentration-dependent acceptance criteria. The RPD criterion < 30% for aqueous samples was applied for cases in which both the sample and duplicate results were greater than 5 times the method quantitation limit (MQL). Otherwise, the absolute difference between the sample results was compared to 2 times the greater sample quantitation limit (SQL) for aqueous samples.

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Sample WD-3 was the field duplicate of MW-26. Table 5-2 shows the field duplicate comparison results. Only detected analytes were listed in Table 5-2. The remaining analytes are non-detects.

Table 5-2 Field Duplicate Comparison

Analyte MW-26result WD-3 result RPD % Qualifier Volatiles - µg/L Benzene 36 36 0 None Ethyl benzene 740 740 0 None Toluene 2 2 Dif =0 < 2SQL None Trichloroethene 150 150 0 None m,p-xylene 13 13 Dif = 0 < 2SQL None o-xylene 4 4 Dif = 0 < 2SQL None PCB – µg/L All aroclors Non detect Non-detect 0 None General chemistry – mg/L n-hexane extractable 2.1 2.2 Dif = 0.1 < 2 SQL None TDS 50,200 49,800 0.8% None TOC 4.56 5.06 Dif = 0.5 < 2SQL None None of the data was qualified based on field duplicate differences.

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6.0 DATA VALIDATION RESULTS

The laboratory appears to have an adequate QA system in place that is designed to ensure the accurate reporting of analytical results generated by the laboratory. The data packages were reviwed in accordance with the approved Superfund Site QAPP (200919.3). Data packages 07010444 and 07010521 provided a LRC which addressed all analytes of concern plus QC data to support a level II review. The contract required a level III data package (with raw data) for the PCB fraction. This validation report covers the additional supporting documentation provided for the PCB data. No transcription or calculation errors were found in the PCB data. All instances in which the analytical QC results fell outside the acceptance criteria were fully and correctly reported in the LRC. The initial calibration and continuing calibrations for the all analyses met the method acceptance criteria as specified in Section B5.1. The LRC was reviewed to indicate if any calibration nonconformance was present for the volatiles and inorganic parameters. Both the LRC and supplemental raw data were reviewed to verify that the PCB calibrations met QC criteria as summarized in Section 2.0 above. None of the data was qualified based on initial or continuing calibration exceptions. No additional qualifiers were added to the data based on data validation of the PCB fraction.

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7.0 OVERALL ASSESSMENT

The data reported in package 06011208 are considered acceptable for use (as qualified) in meeting project objectives. An overall assessment of each of the data quality assurance objectives is provided below.

7.1 Accuracy

Accuracy is defined as the degree of agreement of a measurement to an accepted reference or true value. Accuracy was measured as the percent recovery (%R) of an analyte in a reference standard or spiked sample. All calibration check standards, LCS, MS, MSD, and surrogate recoveries were within quality control limits, except the surrogates for PCB analyses. The surrogate decachlorobiphenyl was below the lower control limit of 60% for samples MW-26 (52%) and WD-3 (58%). The samples were non-detects for all aroclors and each aroclor was qualified “UJ-SUR-L” for these two samples. None of the data were rejected based on the LCS, MS, MSD or surrogate recovery and estimated data are considered acceptable. Therefore, the overall level of accuracy demonstrated by the analyses is considered acceptable.

7.2 Precision

Precision is defined as the agreement between a set of replicate measurements without assumption or knowledge of the true value. Precision of laboratory measurements was evaluated by the comparison of sample/sample duplicate results. The MS/MSD RPD was within quality control limits of 40% for organics and 30% for inorganic. As such, the overall level of precision demonstrated by the analyses is acceptable.

7.3 Completeness

No data was considered unusable for reconciliation with project objectives. Analytical completeness is defined as the ratio of the number of valid analytical results (valid analytical results include values qualified as estimated) to the total number of analytical results requested on samples submitted for analysis. The completeness goal for data packages 07010444 and 07010521 is 100%, which satisfies the site QAPP goal of 95% for aqueous samples.

7.4 Representativeness

Representativeness is the degree to which data accurately and precisely represents a characteristic of a population, parameter variations at a sampling point, or an environmental condition. Representativeness was evaluated by comparing the results obtained for the field duplicate sample pairs. Representativeness was maintained during the sampling event by conducting sampling in accordance with the QAPP and relevant Standard Operating Procedures (SOPs). The results of the field duplicate samples met the criteria in the Superfund QAPP for all parameters. This is another indication that representativeness was achieved during this sampling event.

7.5 Comparability

Comparability expresses the confidence with which one data set can be compared to another. Comparability can be related to accuracy and precision because these quantities are measures of data

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reliability. Data are comparable if collection techniques, measurement procedures, method and reporting are equivalent for the samples within a sample set. As the samples in this set and the other samples collected under the site QAPP were analyzed in accordance with the quality assurance and quality control measures prescribed in the site QAPP; and acceptable levels of overall accuracy and precision were attained, the data within this set are considered to be comparable to each other and to the other samples collected under the site QAPP.

7.6 Sensitivity

Sensitivity is evaluated in Section 8.1.

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8.0 DATA USABILITY RELATIVE TO PROJECT OBJECTIVES

The usability of the sample data relative to the intended end uses is discussed in this section. To facilitate the discussion, the project objectives and associated decisions for which sampling data are to be used as a data source are discussed. The groundwater sampling event is an annual sampling program for the Geneva Industries Federal Superfund Site. The samples were collected on January 9, 10, and 11, 2006 in accordance with the sample collection procedures contained in the site QAPP and include nine groundwater samples, one field duplicate sample, one equipment blank, and two trip blanks. The Geneva Industries Federal Superfund groundwater samples were collected to meet the following objective:

Objective: The purpose of the groundwater sampling event is to provide annual data to evaluate the groundwater contamination. The monitoring wells outside the slurry wall are monitored for PCBs and TCE. These concentrations are compared to the TRRP drinking water standards for residential property. These monitoring wells are MW-17, 11, 24, 26, 23, 8, 10, and 25.

In order to evaluate the usability of the data for making project decisions, the data must be reconciled with the project objectives and decision criteria. Only data considered to be valid (i.e., the quality of the data is known) as determined through data validation, may be considered for reconciliation with the project objectives. The reconciliation process begins with a comparison of the maximum sample quantitation limits obtained to the decision criteria. In general, for the data to be considered to be usable for making the project decisions, the sample quantitation limits obtained for each analyte must be less than or equal to the decision criteria. Non-detect results at sample quantitation limits which exceed decision criteria are not sufficient for making project decisions based on those criteria. Below in Section 8.1, the sample quantitation limits obtained are compared to the project decision criteria. After evaluating the usability of the data with respect to SQL obtained and project decision criteria, any potential biases and imprecision in results suggested by QC results must be assessed in order to evaluate the ultimate usability of the data for making decision. Potential biases and imprecision in analytical results and data usability are discussed in Section 8.2. Since multiple samples and a field duplicate were collected, these data can be used to evaluate the representativeness of the samples to the medium sampled. The results of this evaluation are discussed in Section 8.3.

8.1 Sample Quantitation Limits and Decision Criteria Comparison

The method quantitation limit (MQL) is the concentration of the lowest non-zero standard (adjusted for sample size and dilutions) in the laboratory’s initial calibration curve. Sample quantitation limit (SQL) represents the method detection limit for an analyte adjusted for sample size and dilutions. Table 8-1 below compares the MQL and SQL reported for each analyte to the decision criteria specified in the QAPP.

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Table 8-1 Sample Quantitation Limits and QAPP Decision Criteria Comparison

Tier 1 Groundwater PCLs for Residential/Organics

Analyte Lab MQL

(mg/L) QAPP MQL

(mg/L) Lab SQL (mg/L)

GW GW Ing2

(mg/L) Benzene 0.005 0.0004 0.0005 0.005

Ethyl benzene 0.005 0.001 0.00035 0.7 Toluene 0.005 0.001 0.00024 1.0

Total xylenes 0.005 0.005 0.00017 10 Trichloroethene 0.005 0.001 0.00025 0.005

PCB 0.001 0.0005 0.00010-0.00034 0.0005 All aqueous data are considered usable for meeting project objectives of sensitivity, as the SQL for each analyte is at or below the groundwater ingestion criteria. No data was reported as non-detects at elevated MQL/SQL based on qualification due to blank contamination or dilutions. The sample results for BTEX, TCE and PCB for monitoring wells MW-17, 11, 24, 26, 23, 22, 8, 10, and 25 were compared to the PCLs listed above. The sample results were non-detects for all samples, except MW-24 and MW-26. MW-24 contained TCE at 0.001 mg/L which is below the PCL. MW-26 exceeded the PCL for benzene (0.036 mg/L), ethyl benzene (0.740 mg/L), and trichloroethene (0.150 mg/L). The PCB results were non-detects (less than the SQL) for all samples.

8.2 Effects of Potential Biases and Imprecision on Usability of the Data

After evaluating the usability of the data with respect to sample quantitation limits obtained and project decision criteria, any potential biases and imprecision in results suggested by QC results must be assessed in order to evaluate the ultimate usability of the data making decisions. Potential biases and imprecision in analytical results are inferred from the results obtained for various types of quality control sample analyses. Potential bias and imprecision can result from the analytical system or the specific matrix analyzed. Quality control analyses that provide an indication of the potential bias and imprecision in the analytical system relative to the specific sample matrix include matrix spike analyses, post-digestion spiked analyses, laboratory duplicate analyses of field duplicate samples, and field duplicate analyses. Matrix spike samples are site-specific samples into which target analytes are spiked. As such, the percent recoveries obtained from the matrix spike analyses provide an indication of the potential biases of the analytical method on site-specific samples. Additionally, laboratory duplicate results provide an indication of the precision of the analyses on site-specific samples. There is no potential bias or imprecision for the results presented in this data package, except for the PBC data for samples MW-26 and WD-3. The PCB surrogate decachlorobiphenyl for these two samples were below 60% recovery. The sample results were all non-detects. With surrogate recovery of 52% (MW-26) and 58% (WD-3), the potential bias low is 48% and 42% respectively. The only impact is that the reporting limit for these two samples may be raised due to lower surrogate recovery. The second surrogate was within QC limits, suggesting that the potential bias is minimal.

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8.3 Representativeness

Representativeness is the degree to which data accurately and precisely represent a characteristic of a population, parameter variations at a sampling point, or an environmental condition. Sampling and analyses were conducted in compliance with the QAPP and relevant standard operating procedures (SOPs) in order to maintain representativeness. The results of the field duplicate samples met the criteria in the Superfund QAPP for all parameters. This is another indication that representativeness was achieved during this sampling event.

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9.0 POTENTIAL ADDITIONAL DATA USES AND LIMITATIONS

In addition to being used in making the decisions specified in the QAPP, the supplemental sample data generated may potentially have other end uses including risk assessment. The analytical data quality is generally considered sufficient for this additional potential end use, however, the magnitude of potential biases and imprecision discussed above must be considered. Prior to use in risk assessment, end users of the data should perform a data quality assessment relative to their specific risk assessment objectives and should perform an evaluation of whether the analytical data are sufficiently representative of the medium under evaluation. All data were validated in accordance with the provisions of the QAPP using guidance from the NFG for Inorganic Data Review (February 1994) and Organic Data Review (1999). The data validation is considered to meet the minimum requirements specified in USEPA’s Risk Assessment Guidance for Superfund (September, 1989) and those specified in USEPA’s Guidance for Data Usability in Risk Assessment (April, 1992). Data qualifiers were added as listed in Tables 1-2 and 1-3. As specified in DURA, data qualified as “U” (non-detectable) or “J” (estimated) should be used for risk assessment purposes. Section 8.2 above provides a detailed description of the magnitude and direction of potential bias associated with J-qualified data and should be useful to the risk assessor in evaluating the uncertainty associated with qualified results.

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10.0 CORRECTIVE ACTIONS AND WORKPLAN DEVIATIONS

No field or laboratory corrective actions were required during the course of the field investigation. No QAPP modifications were implemented.

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11.0 REJECTED DATA AND PROJECT CONSEQUENCES

None of the data was rejected during data validation. As a result, all data were considered to be usable for reconciliation with project objectives. As discussed in Sections 5 and 7, some results were qualified estimated based on a variety of minor QC problems. Section 8.2 discussed the direction and magnitude of the bias associated with the qualified results. After reconciliation of the data with project objective (by means of evaluating the data set relative to sample quantitation limits, the magnitude and direction of any potential biases, and representativeness), all results for the samples are considered to be suitable for making decision of whether individual analyte concentrations exceed the decision criteria specified in the QAPP.

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12.0 CONCLUSIONS

With the exception of limitations noted in Section 8.0, the data are considered to be usable for making project decisions. As described in Section 9.0, these data are also considered to be of sufficient analytical quality for a variety of other end uses including baseline risk assessment. For end uses of the data other than those for which decision criteria are specified in Section 8.0 the end user of the data should perform a data quality assessment relative to their specific end use objectives. This assessment should include an evaluation of whether the analytical data are sufficiently representative of the medium under evaluation for their specific data use.

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APPENDIX A

DATA REPORTING FORMS

SPL Laboratories Report Numbers 07010444 and 07010521

Including COC and Laboratory Review Checklist

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DATA USABILITY SUMMARY SPL LABORATORY REPORT … · These three types of reviews are discussed further in Sections 2.0, 3.0, and 4.0 of this Data Usability Summary (DUS) report, respectively.

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