Appendices_Final_2007_SBM_Road_Data_Evaluation_Report.pdf

APPENDIX D

D CH2M HILL Data Quality Summary for Sulphur Bank Mine Road Soil Sampling, April and May 2007

D.1 Introduction CH2M HILL collected soil samples from April 12 through May 29, 2007, for the Sulphur Bank Mine Road soil sampling effort. Samples were collected and analyzed using field-portable x-ray fluorescence and laboratory methods. The investigation was conducted on and adjacent to Sulphur Bank Mine Road to determine whether mine-related waste is present in the soil. This data quality summary report focuses on the laboratory data.

The laboratory samples were analyzed in accordance with the Quality Assurance Project Plan for Sulphur Bank Mercury Mine Superfund Site, Clearlake Oaks, California (QAPP) (CH2M HILL, 2005a). The QAPP presents specific policies, organization, functions, and quality assurance/quality control activities associated with generating and assessing the analytical data.

D.2 Analytical Data Two hundred and ninety-five native environmental samples and 24 field duplicates were collected for laboratory analysis. The samples were divided into 25 sample delivery groups by the laboratory. The samples were analyzed for mercury and arsenic by Contract Laboratory Program (CLP) Method ILM05.3. The analyses were performed by Bonner Analytical Testing Co., in Hattiesburg, Mississippi. Samples were collected and shipped by overnight carrier to the laboratory for analysis.

All data were validated by the U.S. Environmental Protection Agency (EPA), Region 9 Environmental Services Assistance Team. Analytical data reporting and validation proce-dures were performed in accordance with CLP guidelines for the review of inorganic data (EPA, 2004). Fifty percent of all samples received a Tier 1B equivalent validation. The Tier 1B validation reports are included in Attachment D1 (on the attached CD-ROM).

Fifty percent of the samples for each of the analyses performed received a Tier 3 validation review. The Tier 3 validation reports are included in Attachment D2 (on the attached

COD-ROM).

D.3 Overall Assessment The data are 100 percent complete. The number and severity of quality control issues or field procedure problems were minimal considering the size of the data set. Out of approxi-mately 640 normal and field duplicate data points, 131 detected results (approximately 20 percent) and one nondetect result (approximately 0.2 percent) were qualified as

RDD/073030016 (NLH3629.DOC) D-1

APPENDIX D

CH2M HILL DATA QUALITY SUMMARY FOR SULPHUR BANK MINE ROAD SOIL SAMPLING, APRIL AND MAY 2007 estimated. These results and the overall completeness of the sampling effort show that the goals for the project were met and that the quality of the analytical program and labora-tories is sufficient to meet the project data quality objectives.

D.4 Data Management The data management system was designed to assure the usability and integrity of data through a series of procedures and quality control checks that began at the field site and carried through to the generation of data. These data included both the analytical chemical data and information from field activities. Both the chemical data and the field activity information were recorded and managed in the relational database in accordance with the guidelines established in the QAPP and in the Data Management Plan for Sulphur Bank Mercury Mine Superfund Site, Clearlake Oaks, California (CH2M HILL, 2005b).

SBMM sampling activity logs and laboratory analytical data are maintained in a project database or in project files, as appropriate. Data were collected and stored in a manner consistent with the requirements outlined in the QAPP and the data management plan (CH2M HILL, 2005b). The data include but are not limited to the following:

• Field data including the following:

− Daily field progress reports − Field worksheets − Daily field notebooks − Sample collection logs − Chain-of-custody forms

• Laboratory data received in electronic comma-delimited American Standard Code for Information Interchange (ASCII) format.

• Validated data for Tier 1B and Tier 3, delivered by EPA Region 9 Environmental Services Assistance Team as Microsoft® Excel spreadsheets that included sample results and validation qualifiers. Final validation data flags were assigned by the EPA validators and applied to the database by CH2M HILL.

The laboratory data files, validated data files, and electronic data are stored in project files and project local area network hard drives in the CH2M HILL office in Redding, California.

The original field data forms are also stored in the CH2M HILL office in Redding.

Laboratories are required to archive the analytical data in accordance with the QAPP.

D.5 References CH2M HILL. 2005a. Quality Assurance Project Plan for Sulphur Bank Mercury Mine Superfund Site, Clearlake Oaks, California. June.

CH2M HILL. 2005b. Data Management Plan for Sulphur Bank Mercury Mine Superfund Site, Clearlake Oaks, California. May.

U.S. Environmental Protection Agency (EPA). 2004. Contract Laboratory Program National Functional Guidelines for Inorganic Data Review.

D-2 RDD/073030016 (NLH3629.DOC)

00105071-8203/36281/MY39Z9T1A.xls

ANALYTICAL RESULTS Page 1 of 1 Case No. : 36281 SDG No. : MY39Z9 Table 1A

Site : SULPHUR BANK MERCURY MINE Lab : BONNER ANALYTICAL TESTING CO. (BONNER)

Reviewer : Stan Kott, ESAT/LDC QUALIFIED DATA Analysis Type : Low Concentration Soil Samples Date : July 30, 2007 Concentration in mg/kg (Dry Weight) for Total Arsenic and Total Mercury

Station Location : RA88SBa0507 RA88SBc0507 RA188SBc0507 RA88SBd0509 RA89SBb0507 RA89SBc0507 Sample ID : MY3A00 MY3A01 D1 MY3A02 D1 MY3A03 MY3BC8 MY3BC9

Collection Date : 5/21/2007 5/21/2007 5/21/2007 5/21/2007 5/21/2007 5/21/2007

PARAMETER Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com

ARSENIC 35.7 J B 3.8 J B 3.7 J B 6.2 J B 3.2 J B 1.3U J B

MERCURY 92.4 J A 2.8 J AC 0.68 J AC 1.4 J A 6.1 J A 2.2 J A

Percent Solids 89.9% 92.7% 94.4% 93.6% 94.9% 79.9%

Station Location : RA90SBa0507 RA90SBb0507 RA91SBa0507 RA91SBb0507 RA92SBa0507 RA92SBb0507 Sample ID : MY3BD0 MY3BD1 MY3BD2 MY3BD3 MY3BD4 MY3BD5

Collection Date : 5/21/2007 5/21/2007 5/21/2007 5/21/2007 5/21/2007 5/21/2007

PARAMETER Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com

ARSENIC 3.8 J B 1.2 J B 9.8 J B 3.0 J B 3.5 J B 2.6 J B

MERCURY 15.2 J A 0.91 J A 20.6 J A 8.7 J A 11.5 J A 3.3 J A

Percent Solids 93.3% 92.3% 89.2% 93.7% 92.0% 88.9%

Station Location : RA93SBa0507 RA93SBe0507 RA93SBf0507 RA94SBb0507 RA94SBc0507 RA94SBe0507 Sample ID : MY3BD6 MY3BD7 MY3BD8 MY3BD9 MY3BE0 MY3BE1

Collection Date : 5/21/2007 5/21/2007 5/21/2007 5/21/2007 5/21/2007 5/21/2007

PARAMETER Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com

ARSENIC 12.7 J B 6.4 J B 4.3 J B 3.4 J B 5.2 J B 4.2 J B

MERCURY 54.3 J A 2.7 J A 9.2 J A 6.2 J A 9.8 J A 12.7 J A

Percent Solids 82.5% 94.0% 88.1% 90.1% 88.2% 88.5%

Station Location : RA95SBa0507 RA87SBd0507 Sample ID : MY3BE2 MY39Z9 MDL CRQL

Collection Date : 5/21/2007 5/21/2007

PARAMETER Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com

ARSENIC 5.9 J B 2.4 J B 0.47 1.0

MERCURY 28.8 J A 3.6 J A 0.040 0.10

Percent Solids 90.7% 94.5% N/A N/A

Val - Validity. Refer to Data Qualifiers in Table 1B. D1, D2, etc. - Field Duplicate Pairs Com - Comments. Refer to the Corresponding Section in the Narrative for each letter. FB - Field Blank, EB - Equipment Blank, MDL - Method Detection Limit TB - Trip Blank, BG - Background Sample N/A - Not Applicable NA - Not Analyzed CRQL - Contract Required Quantitation Limit

00105071-8203/36281/MY39Z9RPT.doc.doc

ICF International / Laboratory Data Consultants Environmental Services Assistance Team, Region 9 1337 South 46th Street, Building 201, Richmond, CA 94804-4698 Phone: (510) 412-2300 Fax: (510) 412-2304

MEMORANDUM

TO: Rick Sugarek, Remedial Project Manager Site Cleanup Section 2, SFD-7-2

THROUGH: Rose Fong, ESAT Task Order Manager (TOM) Quality Assurance (QA) Program, MTS-3

FROM: Doug Lindelof, Data Review Task Manager Region 9 Environmental Services Assistance Team (ESAT)

ESAT Contract No.: EP-W-06-041 Technical Direction Form No.: 00105071

DATE: July 30, 2007

SUBJECT: Review of Analytical Data, Tier 3

Attached are comments resulting from ESAT Region 9 review of the following analytical data:

Site: SBMM Road Sampling Site Account No.: 09 K2 LA01

CERCLIS ID No.: CAD981893275 Case No.: 36281 SDG No.: MY39Z9 Laboratory: Bonner Analytical Testing Co. (BONNER) Analysis: CLP Total Arsenic by ICP-AES and Total Mercury Samples: 20 Soil Samples (see Case Summary) Collection Date: May 21, 2007 Reviewer: Stan Kott, ESAT/Laboratory Data Consultants

This report has been reviewed by the EPA TOM for the ESAT contract, whose signature appears above.

If there are any questions, please contact Rose Fong (QA Program/EPA) at (415) 972-3812.

Attachment cc: Cynthia Gurley, CLP PO USEPA Region 4 Steve Remaley, CLP PO USEPA Region 9

CLP PO: [X] FYI [ ] Action

SAMPLING ISSUES: [X] Yes [ ] No

00105071-8203/36281/MY39Z9RPT.doc.doc Page 1

Data Validation Report

Case No.: 36281 SDG No.: MY39Z9 Site: SBMM Road Sampling Laboratory: Bonner Analytical Testing Co. (BONNER) Reviewer: Stan Kott, ESAT/LDC Date: July 30, 2007

I. CASE SUMMARY

Sample Information Samples: MY39Z9, MY3A00 through MY3A03, MY3BC8, MY3BC9, MY3BD0 through MY3BD9, MY3BE0, MY3BE1, and MY3BE2

Concentration and Matrix: Low Concentration Soil Analysis: CLP Total Arsenic by ICP-AES and Total Mercury

SOW: ILM05.4

Collection Date: May 21, 2007 Sample Receipt Date: May 25, 2007 Preparation Date: May 25 and 28, 2007 Analysis Date: May 25, 26, and 29, 2007

Field QC Field Blanks (FB): Not Provided Equipment Blanks (EB): Not Provided Background Samples (BG): Not Provided Field Duplicates (D1): MY3A01 and MY3A02

Laboratory QC Method Blank & Associated Samples: Preparation Blank-Solid (PBS) and samples listed above Matrix Spike: MY39Z9S Duplicates: MY39Z9D ICP Serial Dilution: MY39Z9L

Analysis: CLP Total Arsenic by ICP-AES and Total Mercury

Sample Preparation Analyte and Digestion Date Analysis Date ICP-AES Arsenic May 25, 2007 May 25 and 29, 2007 Mercury May 28, 2007 May 29, 2007 Percent Solids May 25, 2007 May 26, 2007

CLP PO Action

None.

Sampling Issues

1. The laboratory stated that temperature indicator bottles were not provided in the sample coolers. The laboratory used a thermometer to determine the cooler temperatures to be 3.0ºC. No adverse effect on data quality is expected.

00105071-8203/36281/MY39Z9RPT.doc.doc Page 2

2. The Traffic Report/Chain of Custody (TR/COC) record forms did not specify a sample to be used for laboratory quality control (QC). The laboratory selected sample MY39Z9 for QC analysis and notified the Sample Management Office (SMO). The effect on data quality is not known.

3. Airbill number 618471978894 was not provided on the TR/COC record forms. No adverse effect on data quality is expected.

4. The sampler’s signature was not provided on the TR/COC record forms. No adverse effect on data quality is expected.

Additional Comments

Mercury samples that exceed the analyzer calibration curve were analyzed at the following dilutions:

2-fold for MY39Z9 and MY3BD7;

3-fold for MY3A01, MY3BC8, and MY3BD5;

5-fold for MY3BD3, MY3BD0, and MY3BD9;

10-fold for MY3BD4, MY3BD8, MY3BE0, and MY3BE1;

20-fold for MY3BD2 and MY3BE2;

50-fold for MY3BD6;

100-fold for MY3A00. No adverse effect on data quality is expected.

Samples for this SDG were analyzed for CLP total arsenic by inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and CLP total mercury by cold vapor atomic absorption (CVAA).

All method requirements specified in the EPA Contract Laboratory Program (CLP) Inorganic Statement of Work (SOW), except as noted, have been met.

Analytical results are listed in Table 1A with qualifications. Definitions of data qualifiers used in Table 1A are listed in Table 1B.

This report was prepared in accordance with the following documents:

Χ Region 9 Standard Operating Procedure 906, Guidelines for Data Review of Contract

Laboratory Program Analytical Services (CLPAS) Inorganic Data Packages;

Χ USEPA Contract Laboratory Program Statement of Work For Inorganic Analysis Multi-Media, Multi-Concentration ILM05.3, March 2004;

Χ ILM05.3 to ILM05.4 Summary of Changes, December 1, 2006; and

Χ USEPA Contract Laboratory Program National Functional Guidelines for Inorganic

Data Review, October 2004.

00105071-8203/36281/MY39Z9RPT.doc.doc Page 3

II. VALIDATION SUMMARY

The data were evaluated based on the following parameters:

Parameter Acceptable Comment

1. Data Completeness Yes

2. Sample Preservation and Holding Times Yes

3. Calibration Yes

a. Initial

b. Initial and Continuing Calibration Verification

c. CRQL Check Standard (CRI)

4. Blanks Yes

5. ICP Interference Check Sample (ICS) Yes

6. Laboratory Control Sample (LCS) Yes

7. Duplicate Sample Analysis No A

8. Matrix Spike Sample Analysis No B

9. ICP Serial Dilution Analysis Yes

10. ICP-MS Internal Standards N/A

11. Field Duplicate Sample Analysis No C

12. Sample Quantitation Yes

13. Overall Assessment Yes

N/A = Not Applicable

III. VALIDITY AND COMMENTS

A. The following results are estimated and flagged "J" in Table 1A because a laboratory duplicate result is outside the method QC limits.

Χ Mercury in all samples

Laboratory sample MY39Z9D duplicate results do not meet the ∀35 relative percent difference (RPD) criterion for precision as listed below.

Analyte Laboratory Duplicate, RPD Mercury 67

Results for mercury in all samples are considered quantitatively uncertain.

The analysis of field duplicate samples is a measure of both field and analytical precision. The imprecision in the results of the analysis of the field duplicate pair may be due to the sample matrix, sample non-homogeneity, or poor sampling or laboratory technique.

B. The following results are estimated and flagged "J" or "UJ" in Table 1A because a matrix spike recovery result is outside the method QC limits.

Χ Arsenic in all samples

00105071-8203/36281/MY39Z9RPT.doc.doc Page 4

Matrix spike recovery for arsenic in QC sample MY39Z9S did not meet the 75- 125% criterion for accuracy. The percent recovery and possible percent bias for arsenic are presented below and are based on an ideal recovery of 100%.

Analyte % Recovery % Bias Arsenic 73 -27

Results above the MDL are considered quantitatively uncertain. Results reported for arsenic in all samples may be biased low and, where non-detected, false negatives may exist.

According to the inorganic SOW, when the pre-digestion spike recovery results for ICP analytes (except silver) fall outside the control limits of 75-125%, a post-digestion spike must be performed for those elements that do not meet the specified criteria. The following post-digestion spike recovery results were obtained for sample MY39Z9A.

Analyte Post-Digestion Spike, % Recovery Arsenic 136

Since both the post- and pre-digestion spikes did not meet the QC criteria, matrix effects may be present in the sample digestate which may depress or enhance the analyte signal during analysis.

The matrix spike sample analysis provides information about the effect of the sample matrix on the digestion and measurement methodology.

C. An RPD of 122 was obtained for mercury in the analysis of field duplicate pair samples MY3A01 and MY3A02. Since sampling variability is included in the measurement, field duplicate results are expected to vary more than laboratory duplicates which have a ∀35 RPD criterion for precision. The effect on data quality is not known.

The analysis of field duplicate samples is a measure of both field and analytical precision. The imprecision in the results of the analysis of the field duplicate pair

TABLE 1B

DATA QUALIFIER DEFINITIONS FOR INORGANIC DATA REVIEW

The definitions of the following qualifiers are prepared in accordance with the document USEPA Contract Laboratory Program National Functional Guidelines for Inorganic Data Review, October 2004.

U The analyte was analyzed for, but was not detected above the level of the reported sample quantitation limit.

J The result is an estimated quantity. The associated numerical value is the approximate concentration of the analyte in the sample.

J+ The result is an estimated quantity, but the result may be biased high.

J- The result is an estimated quantity, but the result may be biased low.

R The data are unusable. The sample results are rejected due to serious deficiencies in meeting Quality Control (QC) criteria. The analyte may or may not be present in the sample.

UJ The analyte was analyzed for, but was not detected. The reported quantitation limit is approximate and may be inaccurate or imprecise.

00105071-8202/36281/MY39X9T1A,xls

Case No. : 36281 SDG No. : MY39X9 Table 1A

Site : SULPHUR BANK MERCURY MINE Lab : BONNER ANALYTICAL TESTING CO. (BONNER)

Reviewer : Stan Kott, ESAT/LDC QUALIFIED DATA Analysis Type : Low Concentration Soil Samples Date : July 27, 2007 Concentration in mg/kg (Dry Weight) for Total Arsenic and Total Mercury

Station Location : RASS60 RASS61 RASS62 RASS162 RASS63 RA59-2SBf0507 Sample ID : MY39X9 MY39Y0 MY39Y1 D1 MY39Y2 D1 MY39Y3 MY39Y4

Collection Date : 5/22/2007 5/22/2007 5/22/2007 5/22/2007 5/22/2007 5/16/2007

PARAMETER Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com

ARSENIC 39.0 1.9 2.1 2.4 1.2 1.1U

MERCURY 123 20.7 4.9 3.5 2.3 9.2

Percent Solids 87.3 94.1 95.0 95.0 94.1 89.8

Station Location : RA66SBc0507 RA66SBd0507 RA83SBa0507 RA83SBc0507 RA183SBc0507 RA84SBa0507 Sample ID : MY39Y5 MY39Y6 MY39Y7 MY39Y8 D2 MY39Y9 D2 MY39Z0

Collection Date : 5/21/2007 5/21/2007 5/21/2007 5/21/2007 5/21/2007 5/21/2007

PARAMETER Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com

ARSENIC 2.4 0.59L J A 3.0 1.2 2.4 2.7

MERCURY 18.8 5.0 1.7 0.88 0.85 18.1

Percent Solids 94.5 95.3 95.7 92.9 92.7 96.2

Station Location : RA84SBd0507 RA84SBd0507MS/MSD RA85SBa0507 RA85SBb0507 RA86SBa0507 RA86SBb0507 Sample ID : MY39Z1 D3 MY39Z2 D3 MY39Z3 MY39Z4 MY39Z5 MY39Z6

Collection Date : 5/21/2007 5/21/2007 5/21/2007 5/21/2007 5/21/2007 5/21/2007

PARAMETER Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com

ARSENIC 3.4 2.8 4.4 2.6 3.5 5.6

MERCURY 16.4 12.3 301 2.5 4.5 2.6

Percent Solids 92.6 93.2 87.6 93.3 95.6 95.0

Station Location : RA86SBc0507 RA87SBb0507 Sample ID : MY39Z7 MY39Z8 MDL CRQL

Collection Date : 5/21/2007 5/21/2007

PARAMETER Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com

ARSENIC 1.7 70.7 0.47 1.0

MERCURY 4.2 93.5 0.040 0.10

Percent Solids 91.8 81.3 N/A N/A

Val - Validity. Refer to Data Qualifiers in Table 1B. D1, D2, etc. - Field Duplicate Pairs Com - Comments. Refer to the Corresponding Section in the Narrative for each letter. FB - Field Blank, EB - Equipment Blank, 00105071-8202/36281/MY39X9RPT.doc.doc

Environmental Services Assistance Team, Region 9 1337 South 46th Street, Building 201, Richmond, CA 94804-4698 Phone: (510) 412-2300 Fax: (510) 412-2304

MEMORANDUM

DATE: July 27, 2007

CERCLIS ID No.: CAD981893275 Case No.: 36281 SDG No.: MY39X9 Laboratory: Bonner Analytical Testing Co. (BONNER) Analysis: CLP Total Arsenic by ICP-AES and Total Mercury Samples: 20 Soil Samples (see Case Summary) Collection Date: May 16, 21, and 22, 2007 Reviewer: Stan Kott, ESAT/Laboratory Data Consultants

This report has been reviewed by the EPA TOM for the ESAT contract, whose signature appears above.

If there are any questions, please contact Rose Fong (QA Program/EPA) at (415) 972-3812.

Attachment cc: Cynthia Gurley, CLP PO USEPA Region 4 Steve Remaley, CLP PO USEPA Region 9

00105071-8202/36281/MY39X9RPT.doc.doc Page 1

Case No.: 36281 SDG No.: MY39X9 Site: SBMM Road Sampling Laboratory: Bonner Analytical Testing Co. (BONNER) Reviewer: Stan Kott, ESAT/LDC Date: July 27, 2007

I. CASE SUMMARY

Sample Information Samples: MY39X9, MY39Y0 through MY39Y9, and MY39Z0 through MY39Z8 Concentration and Matrix: Low Concentration Soil Analysis: CLP Total Arsenic by ICP-AES and Total Mercury

SOW: ILM05.4

Collection Date: May 16, 21, and 22, 2007 Sample Receipt Date: May 25, 2007 Preparation Date: May 25 and 28, 2007 Analysis Date: May 25, 26, and 29, 2007

Field QC Field Blanks (FB): Not Provided Equipment Blanks (EB): Not Provided Background Samples (BG): Not Provided Field Duplicates (D1): MY39Y1 and MY39Y2 Field Duplicates (D2): MY39Y8 and MY39Y9 Field Duplicates (D3): MY39Z1 and MY39Z2

Laboratory QC Method Blank & Associated Samples: Preparation Blank-Solid (PBS) and samples listed above Matrix Spike: MY39X9S Duplicates: MY39X9D ICP Serial Dilution: MY39X9L

Analysis: CLP Total Arsenic by ICP-AES and Total Mercury

Sample Preparation Analyte and Digestion Date Analysis Date ICP-AES Arsenic May 25, 2007 May 25, 2007 Mercury May 28, 2007 May 29, 2007 Percent Solids May 25, 2007 May 26, 2007 temperatures to be 3.0ºC. No adverse effect on data quality is expected.

00105071-8202/36281/MY39X9RPT.doc.doc Page 2 sample to be used for laboratory quality control (QC). The laboratory selected sample MY39X9 for QC analysis and notified the Sample Management Office

3. Airbill number 618471978894 was not provided on the TR/COC record forms. No following dilutions:

2-fold for MY39Z5;

3-fold for MY39Y1, MY39Y2, MY39Y6, MY39Z4, andMY39Z7;

10-fold for MY39Y0, MY39Y4, MY39Z0, MY39Z1, and MY39Z2;

20-fold for MY39Y5;

50-fold for MY39Z8;

100-fold for MY39X9;

300-fold for MY39Z3. No adverse effect on data quality is expected.

Samples for this SDG were analyzed for CLP total arsenic by inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and CLP total mercury by cold vapor atomic absorption (CVAA).

All method requirements specified in the EPA Contract Laboratory Program (CLP) Inorganic Statement of Work (SOW), except as noted, have been met.

Analytical results are listed in Table 1A with qualifications. Definitions of data qualifiers used in Table 1A are listed in Table 1B.

This report was prepared in accordance with the following documents:

00105071-8202/36281/MY39X9RPT.doc.doc Page 3

1. Data Completeness Yes

2. Sample Preservation and Holding Times Yes

3. Calibration Yes

a. Initial

b. Initial and Continuing Calibration Verification

c. CRQL Check Standard (CRI)

4. Blanks Yes

5. ICP Interference Check Sample (ICS) Yes

6. Laboratory Control Sample (LCS) Yes

7. Duplicate Sample Analysis Yes

8. Matrix Spike Sample Analysis Yes

9. ICP Serial Dilution Analysis Yes

10. ICP-MS Internal Standards N/A

11. Field Duplicate Sample Analysis Yes

12. Sample Quantitation Yes A

A. Results above the method detection limit (MDL) but below the contract required quantitation limit (CRQL) (denoted with an "L" qualifier) are estimated and flagged "J" in Table 1A.

Results above the MDL but below the CRQL are considered qualitatively acceptable but quantitatively unreliable due to uncertainties in the analytical precision near the limit of quantitation.

00105071-8202/36281/MY39X9RPT.doc.doc Page 4

J The result is an estimated quantity. The associated numerical value is the approximate concentration of the analyte in the sample.

J+ The result is an estimated quantity, but the result may be biased high.

J- The result is an estimated quantity, but the result may be biased low.

R The data are unusable. The sample results are rejected due to serious deficiencies in

00105071-8186/36281/MY39S9T1A.xls

Case No. : 36281 SDG No. : MY39S9 Table 1A

Site : SULPHUR BANK MERCURY MINE Lab : BONNER ANALYTICAL TESTING CO. (BONNER)

Reviewer : Stan Kott, ESAT/LDC QUALIFIED DATA Analysis Type : Low Concentration Soil Samples Date : July 25, 2007 Concentration in mg/kg (Dry Weight) for Total Arsenic and Total Mercury

Station Location : RA76SBa0507 RA76SBc0507 RA76SBd0507 RA77SBa0507 RA77SBc0507 RA77SBd0507 Sample ID : MY39S9 MY39T0 MY39T1 MY39T2 MY39T3 MY39T4

Collection Date : 5/16/2007 5/16/2007 5/16/2007 5/16/2007 5/16/2007 5/16/2007

PARAMETER Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com

ARSENIC 6.4 6.3 7.1 1.7 9.7 2.8

MERCURY 19.5 14.5 22.3 2.8 160 12.8

Percent Solids 89.8% 87.7% 83.7% 97.8% 88.4% 92.6%

Station Location : RA78SBa0507 RA78SBb0507 RA79SBa0507 RA79SBb0507 RA179SBb0507 RA80SBa0507 Sample ID : MY39T5 MY39T6 MY39T7 MY39T8 D1 MY39T9 D1 MY39W0

Collection Date : 5/16/2007 5/16/2007 5/16/2007 5/16/2007 5/16/2007 5/16/2007

PARAMETER Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com

ARSENIC 3.4 3.2 2.2 1.4 1.2 8.0

MERCURY 25.1 5.9 4.8 8.4 8.2 320

Percent Solids 96.9% 93.8% 95.6% 93.7% 93.8% 93.3%

Station Location : RA80SBb0507 RA180SBb0507 RA81SBa0507 RA81SBb0507 RA81SBb0507MS/MSD RA81SBc0507 Sample ID : MY39W1 D2 MY39W2 D2 MY39W3 MY39W4 D3 MY39W5 D3 MY39W6

Collection Date : 5/16/2007 5/16/2007 5/16/2007 5/16/2007 5/16/2007 5/16/2007

PARAMETER Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com

ARSENIC 113 A 17.5 A 3.5 4.8 4.8 3.1

MERCURY 242 A 55.0 A 13.6 25.7 20.8 5.4

Percent Solids 90.3% 90.8% 90.8% 80.3% 77.0% 93.0%

Station Location : RA82SBa0507 RA82SBb0507 Sample ID : MY39W7 MY39W8 MDL CRQL

Collection Date : 5/16/2007 5/16/2007

PARAMETER Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com

ARSENIC 4.0 3.9 0.47 1.0

MERCURY 14.7 2.0 0.020 0.10

Percent Solids 94.5% 90.3% N/A N/A

Val - Validity. Refer to Data Qualifiers in Table 1B. D1, D2, etc. - Field Duplicate Pairs Com - Comments. Refer to the Corresponding Section in the Narrative for each letter. FB - Field Blank, EB - Equipment Blank, 00105071-8186/36281/MY39S9RPT.doc.doc

Environmental Services Assistance Team, Region 9 1337 South 46th Street, Building 201, Richmond, CA 94804-4698 Phone: (510) 412-2300 Fax: (510) 412-2304

MEMORANDUM

DATE: July 26, 2007

CERCLIS ID No.: CAD981893275 Case No.: 36281 SDG No.: MY39S9 Laboratory: Bonner Analytical Testing Co. (BONNER) Analysis: CLP Total Arsenic by ICP-AES and Total Mercury Samples: 20 Soil Samples (see Case Summary) Collection Date: May 14 and 15, 2007 Reviewer: Stan Kott, ESAT/Laboratory Data Consultants

This report has been reviewed by the EPA TOM for the ESAT contract, whose signature appears above.

If there are any questions, please contact Rose Fong (QA Program/EPA) at (415) 972-3812.

Attachment cc: Cynthia Gurley, CLP PO USEPA Region 4 Steve Remaley, CLP PO USEPA Region 9

00105071-8186/36281/MY39S9RPT.doc.doc Page 1

Case No.: 36281 SDG No.: MY39S9 Site: SBMM Road Sampling Laboratory: Bonner Analytical Testing Co. (BONNER) Reviewer: Stan Kott, ESAT/LDC Date: July 26, 2007

I. CASE SUMMARY

Sample Information Samples: MY39S9, MY39T0 through MY39T9 and MY39W0 through MY39W8 Concentration and Matrix: Low Concentration Soil Analysis: CLP Total Arsenic by ICP-AES and Total Mercury

SOW: ILM05.4

Collection Date: May 16, 2007 Sample Receipt Date: May 22, 2007 Preparation Date: May 22 and 23, 2007 Analysis Date: May 23 and 24, 2007

Field QC Field Blanks (FB): Not Provided Equipment Blanks (EB): Not Provided Background Samples (BG): Not Provided Field Duplicates (D1): MY39T8 and MY39T9 Field Duplicates (D2): MY39W1 and MY39W2 Field Duplicates (D3): MY39W4 and MY39W5

Laboratory QC Method Blank & Associated Samples: Preparation Blank-Solid (PBS) and samples listed above Matrix Spike: MY39S9S Duplicates: MY39S9D ICP Serial Dilution: MY39S9L

Analysis: CLP Total Arsenic by ICP-AES and Total Mercury

Sample Preparation Analyte and Digestion Date Analysis Date ICP-AES Arsenic May 23, 2007 May 23, 2007 Mercury May 23, 2007 May 24, 2007 Percent Solids May 22, 2007 May 23, 2007

00105071-8186/36281/MY39S9RPT.doc.doc Page 2

1. The laboratory stated that temperature indicator bottles were not provided in the temperatures to be 4.0ºC. No adverse effect on data quality is expected.

sample to be used for laboratory quality control (QC). The laboratory selected sample MY39S9 for QC analysis and notified the Sample Management Office

3. Airbill numbers 618471978450 and 618471978471 were not provided on the

TR/COC record forms. No adverse effect on data quality is expected.

The “laboratory received” date and time were not provided on the TR/COC record form for samples MY39W3 through MY39W8. No adverse effect on data quality is expected.

Mercury samples that exceed the analyzer calibration curve were analyzed at the following dilutions:

2-fold for MY39W8;

3-fold for MY39T6 and MY39T7;

5-fold for MY39T8, MY39T9, and MY39W6;

10-fold for MY39S9, MY39T0, MY39T1, MY39T4, MY39W3, MY39W5, and MY39W7;

20-fold for MY39T5, MY39W2, and MY39W4;

100-fold for MY39T3 and MY39W1;

300-fold for MY39W0. No adverse effect on data quality is expected.

Samples for this SDG were analyzed for CLP total arsenic by inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and CLP total mercury by cold vapor atomic absorption (CVAA).

All method requirements specified in the EPA Contract Laboratory Program (CLP) Inorganic Statement of Work (SOW), except as noted, have been met.

Analytical results are listed in Table 1A with qualifications. Definitions of data qualifiers used in Table 1A are listed in Table 1B.

This report was prepared in accordance with the following documents:

00105071-8186/36281/MY39S9RPT.doc.doc Page 3

1. Data Completeness Yes

2. Sample Preservation and Holding Times Yes

3. Calibration Yes

a. Initial

b. Initial and Continuing Calibration Verification

c. CRQL Check Standard (CRI)

4. Blanks Yes

5. ICP Interference Check Sample (ICS) Yes

6. Laboratory Control Sample (LCS) Yes

7. Duplicate Sample Analysis Yes

8. Matrix Spike Sample Analysis Yes

9. ICP Serial Dilution Analysis Yes

10. ICP-MS Internal Standards N/A

11. Field Duplicate Sample Analysis No A

12. Sample Quantitation Yes

A. Relative percent differences (RPDs) of 146 and 126 were obtained for arsenic and mercury, respectively, in the analysis of field duplicate pair samples MY39W1 and MY39W2. Since sampling variability is included in the measurement, field duplicate results are expected to vary more than laboratory duplicates which have a ∀35 RPD criterion for precision. The effect on data quality is not known.

The analysis of field duplicate samples is a measure of both field and analytical precision. The imprecision in the results of the analysis of the field duplicate pair

00105071-8186/36281/MY39S9RPT.doc.doc Page 4

J The result is an estimated quantity. The associated numerical value is the approximate concentration of the analyte in the sample.

J+ The result is an estimated quantity, but the result may be biased high.

J- The result is an estimated quantity, but the result may be biased low.

R The data are unusable. The sample results are rejected due to serious deficiencies in

00105071-8185/36281/MY39E0T1A.xls

Case No. : 36281 SDG No. : MY39E0 Table 1A

Site : SULPHUR BANK MERCURY MINE Lab : BONNER ANALYTICAL TESTING CO. (BONNER)

Reviewer : Stan Kott, ESAT/LDC QUALIFIED DATA Analysis Type : Low Concentration Soil Samples Date : July 25, 2007 Concentration in mg/kg (Dry Weight) for Total Arsenic and Total Mercury

Station Location : RA45SBb0507 RA45SBc0507 RA46SBa0507 RA46SBa0507MS/MSD RA46SBb0507 RA46SBc0507 Sample ID : MY39E0 MY39E1 MY39E2 D1 MY39E3 D1 MY39E4 MY39E5

Collection Date : 5/15/2007 5/15/2007 5/15/2007 5/15/2007 5/15/2007 5/15/2007

PARAMETER Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com

ARSENIC 5.2 1.0L J A 7.0 6.4 11.4 0.65L J A

MERCURY 13.8 5.1 28.6 22.6 77.4 2.8

Percent Solids 92.9% 80.4% 94.6% 94.6% 92.6% 75.2%

Station Location : RA47SBa0507 RA47SBb0507 RA47SBc0507 RA147SBc0507 RA48SBa0507 RA48SBb0507 Sample ID : MY39E6 MY39E7 MY39E8 D2 MY39E9 D2 MY39F0 MY39F1

Collection Date : 5/15/2007 5/15/2007 5/15/2007 5/15/2007 5/15/2007 5/15/2007

PARAMETER Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com

ARSENIC 6.7 4.4 3.5 3.2 5.6 3.8

MERCURY 13.8 1.1 2.3 B 1.4 B 61.8 2.7

Percent Solids 93.0% 95.2% 94.2% 94.4% 88.8% 91.5%

Station Location : RA48SBc0507 RA49SBa0507 RA49SBb0507 RA49SBc0507 RA50SBa0507 RA50SBb0507 Sample ID : MY39F2 MY39F3 MY39F4 MY39F5 MY39F6 MY39F7 D3

Collection Date : 5/15/2007 5/15/2007 5/15/2007 5/15/2007 5/14/2007 5/14/2007

PARAMETER Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com

ARSENIC 5.2 26.1 8.0 3.1 14.5 14.6

MERCURY 1.8 99.5 29.3 1.4 26.0 40.4

Percent Solids 91.3% 92.3% 91.1% 91.4% 87.2% 85.0%

Station Location : RA150SBb0507 RA50SBc0507 Sample ID : MY39F8 D3 MY39F9 MDL CRQL

Collection Date : 5/14/2007 5/14/2007

PARAMETER Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com

ARSENIC 10.9 1.1U 0.47 1.0

MERCURY 50.5 2.1 0.020 0.10

Percent Solids 82.3% 92.2% N/A N/A

Val - Validity. Refer to Data Qualifiers in Table 1B. D1, D2, etc. - Field Duplicate Pairs Com - Comments. Refer to the Corresponding Section in the Narrative for each letter. FB - Field Blank, EB - Equipment Blank, 00105071-8185/36281/MY39E0RPT.doc.doc

Environmental Services Assistance Team, Region 9 1337 South 46th Street, Building 201, Richmond, CA 94804-4698 Phone: (510) 412-2300 Fax: (510) 412-2304

MEMORANDUM

DATE: July 25, 2007

CERCLIS ID No.: CAD981893275 Case No.: 36281 SDG No.: MY39E0 Laboratory: Bonner Analytical Testing Co. (BONNER) Analysis: CLP Total Arsenic by ICP-AES and Total Mercury Samples: 20 Soil Samples (see Case Summary) Collection Date: May 14 and 15, 2007 Reviewer: Stan Kott, ESAT/Laboratory Data Consultants

This report has been reviewed by the EPA TOM for the ESAT contract, whose signature appears above.

If there are any questions, please contact Rose Fong (QA Program/EPA) at (415) 972-3812.

Attachment cc: Cynthia Gurley, CLP PO USEPA Region 4 Steve Remaley, CLP PO USEPA Region 9

00105071-8185/36281/MY39E0RPT.doc.doc Page 1

Case No.: 36281 SDG No.: MY39E0 Site: SBMM Road Sampling Laboratory: Bonner Analytical Testing Co. (BONNER) Reviewer: Stan Kott, ESAT/LDC Date: July 25, 2007

I. CASE SUMMARY

Sample Information Samples: MY39E0 through MY39E9 and MY39F0 through

MY39F9

Concentration and Matrix: Low Concentration Soil Analysis: CLP Total Arsenic by ICP-AES and Total Mercury

SOW: ILM05.4

Collection Date: May 14 and 15, 2007 Sample Receipt Date: May 18, 2007 Preparation Date: May 18, 2007 Analysis Date: May 19 and 21, 2007

Field QC Field Blanks (FB): Not Provided Equipment Blanks (EB): Not Provided Background Samples (BG): Not Provided Field Duplicates (D1): MY39E2 and MY39E3 Field Duplicates (D2): MY39E8 and MY39E9 Field Duplicates (D3): MY39F7 and MY39F8

Laboratory QC Method Blank & Associated Samples: Preparation Blank-Solid (PBS) and samples listed above Matrix Spike: MY39E0S Duplicates: MY39E0D ICP Serial Dilution: MY39E0L

Analysis: CLP Total Arsenic by ICP-AES and Total Mercury

Sample Preparation Analyte and Digestion Date Analysis Date ICP-AES Arsenic May 18, 2007 May 21, 2007 Mercury May 18, 2007 May 19, 2007 Percent Solids May 18, 2007 May 19, 2007

00105071-8185/36281/MY39E0RPT.doc.doc Page 2

1. The Traffic Report/Chain of Custody (TR/COC) record forms did not specify a sample to be used for laboratory quality control (QC). The laboratory selected sample MY39E0 for QC analysis and notified the Sample Management Office

2. Airbill number 861249545216 was not provided on the TR/COC record forms. No

3. The TR/COC record forms indicate that two bottles per sample were sent. The laboratory indicates only one bottle per sample was received. No adverse effect on data quality is expected.

following dilutions:

2-fold for MY39E1;

10-fold for MY39E0, MY39E2, MY39E3, MY39E6, and MY39F6;

20-fold for MY39F0, MY39F4, MY39F7, and MY39F8;

25-fold for MY39E4;

75-fold for MY39F3. No adverse effect on data quality is expected.

Samples for this SDG were analyzed for CLP total arsenic by inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and CLP total mercury by cold vapor atomic absorption (CVAA).

All method requirements specified in the EPA Contract Laboratory Program (CLP) Inorganic Statement of Work (SOW), except as noted, have been met.

Analytical results are listed in Table 1A with qualifications. Definitions of data qualifiers used in Table 1A are listed in Table 1B.

This report was prepared in accordance with the following documents:

00105071-8185/36281/MY39E0RPT.doc.doc Page 3

1. Data Completeness Yes

2. Sample Preservation and Holding Times Yes

3. Calibration Yes

a. Initial

b. Initial and Continuing Calibration Verification

c. CRQL Check Standard (CRI)

4. Blanks Yes

5. ICP Interference Check Sample (ICS) Yes

6. Laboratory Control Sample (LCS) Yes

7. Duplicate Sample Analysis Yes

8. Matrix Spike Sample Analysis Yes

9. ICP Serial Dilution Analysis Yes

10. ICP-MS Internal Standards N/A

11. Field Duplicate Sample Analysis No B

12. Sample Quantitation Yes A

"J" in Table 1A.

Results above the MDL but below the CRQL are considered qualitatively

B. A relative percent difference (RPD) of 49 was obtained for mercury in the analysis of field duplicate pair samples MY39E8 and MY39E9. Since sampling variability is included in the measurement, field duplicate results are expected to vary more than laboratory duplicates which have a ∀35 RPD criterion for precision. The effect on data quality is not known.

The analysis of field duplicate samples is a measure of both field and analytical precision. The imprecision in the results of the analysis of the field duplicate pair

00105071-8185/36281/MY39E0RPT.doc.doc Page 4

J The result is an estimated quantity. The associated numerical value is the approximate concentration of the analyte in the sample.

J+ The result is an estimated quantity, but the result may be biased high.

J- The result is an estimated quantity, but the result may be biased low.

R The data are unusable. The sample results are rejected due to serious deficiencies in

00105071-8182/36281/MY3999T1A.xls

Case No. : 36281 SDG No. : MY3999 Table 1A

Site : SULPHUR BANK MERCURY MINE Lab : BONNER ANALYTICAL TESTING CO. (BONNER)

Reviewer : Stan Kott, ESAT/LDC QUALIFIED DATA Analysis Type : Low Concentration Soil Samples Date : July 24, 2007 Concentration in mg/kg (Dry Weight) for Total Arsenic and Total Mercury

Station Location : RA32SBd0507 RA33SBa0507 RA33SBb0507 RA33SBc0507 RA34SBa0507 RA34SBb0507 Sample ID : MY39A0 MY39A1 MY39A2 MY39A3 MY39A4 MY39A5 D1

Collection Date : 5/14/2007 5/14/2007 5/14/2007 5/14/2007 5/14/2007 5/14/2007

PARAMETER Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com

ARSENIC 5.7 7.5 6.2 5.5 19.6 6.3

MERCURY 3.8 19.9 4.2 3.2 120 8.0 A

Percent Solids 86.2% 96.8% 91.9% 91.9% 92.4% 83.2%

Station Location : RA34SBc0507 RA34SBb0507MS/MSD RA35SBa0507 RA35SBb0507 RA13SBb0507 RA35SBc0507 Sample ID : MY39A6 MY39A7 D1 MY39A8 MY39A9 D2 MY39B0 D2 MY39B1

Collection Date : 5/14/2007 5/14/2007 5/14/2007 5/14/2007 5/14/2007 5/14/2007

PARAMETER Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com

ARSENIC 6.6 7.1 7.2 5.0 6.3 6.9

MERCURY 3.2 23.9 A 27.4 4.0 3.8 2.2

Percent Solids 92.4% 91.3% 93.5% 90.0% 90.3% 89.6%

Station Location : RA36SBa0507 RA36SBb0507 RA36SBc0507 RA37SBa0507 RA37SBb0507 RA37SBc0507 Sample ID : MY39B2 MY39B3 MY39B4 MY39B5 MY39B6 MY39B7

Collection Date : 5/14/2007 5/14/2007 5/14/2007 5/14/2007 5/14/2007 5/14/2007

PARAMETER Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com

ARSENIC 16.5 110 6.2 6.8 6.7 6.0

MERCURY 406 183 3.8 20.6 29.6 15.8

Percent Solids 94.6% 92.4% 90.5% 92.5% 91.4% 92.1%

Station Location : RA38SBc0507 RA32SBb0507 Sample ID : MY39B9 MY3999 MDL CRQL

Collection Date : 5/15/2007 5/14/2007

PARAMETER Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com

ARSENIC 71.7 5.9 0.31 1.0

MERCURY 273 4.1 0.040 0.10

Percent Solids 78.0% 92.6% N/A N/A

Val - Validity. Refer to Data Qualifiers in Table 1B. D1, D2, etc. - Field Duplicate Pairs Com - Comments. Refer to the Corresponding Section in the Narrative for each letter. FB - Field Blank, EB - Equipment Blank, 00105071-8182/36281/MY3999RPT.doc.doc

Environmental Services Assistance Team, Region 9 1337 South 46th Street, Building 201, Richmond, CA 94804-4698 Phone: (510) 412-2300 Fax: (510) 412-2304

MEMORANDUM

DATE: July 24, 2007

CERCLIS ID No.: CAD981893275 Case No.: 36281 SDG No.: MY3999 Laboratory: Bonner Analytical Testing Co. (BONNER) Analysis: CLP Total Arsenic by ICP-AES and Total Mercury Samples: 20 Soil Samples (see Case Summary) Collection Date: May 14 and 15, 2007 Reviewer: Stan Kott, ESAT/Laboratory Data Consultants

This report has been reviewed by the EPA TOM for the ESAT contract, whose signature appears above.

If there are any questions, please contact Rose Fong (QA Program/EPA) at (415) 972-3812.

Attachment cc: Cynthia Gurley, CLP PO USEPA Region 4 Steve Remaley, CLP PO USEPA Region 9

00105071-8182/36281/MY3999RPT.doc.doc Page 1

Case No.: 36281 SDG No.: MY3999 Site: SBMM Road Sampling Laboratory: Bonner Analytical Testing Co. (BONNER) Reviewer: Stan Kott, ESAT/LDC Date: July 24, 2007

I. CASE SUMMARY

Sample Information Samples: MY3999, MY39A0 through MY39A9, MY39B0 through MY39B7, and MY39B9 Concentration and Matrix: Low Concentration Soil Analysis: CLP Total Arsenic by ICP-AES and Total Mercury

SOW: ILM05.4

Collection Date: May 14 and 15, 2007 Sample Receipt Date: May 17, 2007 Preparation Date: May 18, 2007 Analysis Date: May 19, 2007

Field QC Field Blanks (FB): Not Provided Equipment Blanks (EB): Not Provided Background Samples (BG): Not Provided Field Duplicates (D1): MY39A5 and MY39A7 Field Duplicates (D2): MY39A9 and MY39B0

Laboratory QC Method Blank & Associated Samples: Preparation Blank-Solid (PBS) and samples listed above Matrix Spike: MY3999S Duplicates: MY3999D ICP Serial Dilution: MY3999L

Analysis: CLP Total Arsenic by ICP-AES and Total Mercury

Sample Preparation Analyte and Digestion Date Analysis Date ICP-AES Arsenic May 18, 2007 May 19, 2007 Mercury May 18, 2007 May 19, 2007 Percent Solids May 18, 2007 May 19, 2007

1. The laboratory stated that a temperature indicator bottle was not provided in the cooler for samples MY3999 and MY39A0 through MY39B3. The laboratory used a thermometer to determine the cooler temperature to be 2.5ºC. No adverse effect on

00105071-8182/36281/MY3999RPT.doc.doc Page 2 sample to be used for laboratory quality control (QC). The laboratory selected sample MY3999 for QC analysis and notified the Sample Management Office

3. Airbill number 861249545227 was not provided on the TR/COC record forms. No

4. The TR/COC record forms indicate that two bottles per sample were sent. The laboratory indicates only one bottle per sample was received. No adverse effect on following dilutions:

2-fold for MY3999, MY39A0, MY39A2, MY39A9, MY39B0, and MY39B4;

10-fold for MY39A1, MY39A7, MY39A8, MY39B5, MY39B6, and MY39B7;

50-fold for MY39A4;

100-fold for MY3A4 and MY39B9;

200-fold for MY39B3;

500-fold for MY39B2. No adverse effect on data quality is expected.

Samples for this SDG were analyzed for CLP total arsenic by inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and CLP total mercury by cold vapor atomic absorption (CVAA).

All method requirements specified in the EPA Contract Laboratory Program (CLP) Inorganic Statement of Work (SOW), except as noted, have been met.

Analytical results are listed in Table 1A with qualifications. Definitions of data qualifiers used in Table 1A are listed in Table 1B.

This report was prepared in accordance with the following documents:

00105071-8182/36281/MY3999RPT.doc.doc Page 3

1. Data Completeness Yes

2. Sample Preservation and Holding Times Yes

3. Calibration Yes

a. Initial

b. Initial and Continuing Calibration Verification

c. CRQL Check Standard (CRI)

4. Blanks Yes

5. ICP Interference Check Sample (ICS) Yes

6. Laboratory Control Sample (LCS) Yes

7. Duplicate Sample Analysis Yes

8. Matrix Spike Sample Analysis Yes

9. ICP Serial Dilution Analysis Yes

10. ICP-MS Internal Standards N/A

11. Field Duplicate Sample Analysis No A

12. Sample Quantitation Yes

A. A relative percent difference (RPD) of 100 was obtained for mercury in the analysis of field duplicate pair samples MY39A5 and MY39A7. Since sampling variability is included in the measurement, field duplicate results are expected to vary more than laboratory duplicates which have a ∀35 RPD criterion for precision. The effect on data quality is not known.

The analysis of field duplicate samples is a measure of both field and analytical precision. The imprecision in the results of the analysis of the field duplicate pair

00105071-8182/36281/MY3999RPT.doc.doc Page 4

J The result is an estimated quantity. The associated numerical value is the approximate concentration of the analyte in the sample.

J+ The result is an estimated quantity, but the result may be biased high.

J- The result is an estimated quantity, but the result may be biased low.

R The data are unusable. The sample results are rejected due to serious deficiencies in

00105071-8183/36281/MY3977T1A.xls

Case No. : 36281 SDG No. : MY3977 Table 1A

Site : SULPHUR BANK MERCURY MINE Lab : BONNER ANALYTICAL TESTING CO. (BONNER)

Reviewer : Stan Kott, ESAT/LDC QUALIFIED DATA Analysis Type : Low Concentration Soil Samples Date : July 24, 2007 Concentration in mg/kg (Dry Weight) for Total Arsenic and Total Mercury

Station Location : RA21SBb0507 RA21SBd0507 RA21SBe0507 RA121SBe0507 RA22SBa0507 RA22SBc0507 Sample ID : MY39K4 MY39K5 MY39K6 D1 MY39K7 D1 MY39K8 MY39K9 D2

Collection Date : 5/15/2007 5/15/2007 5/15/2007 5/15/2007 5/15/2007 5/15/2007

PARAMETER Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com

ARSENIC 105 J AB 21.6 J AB 8.7 J ABC 14.8 J ABC 57.8 J AB 117 J AB

MERCURY 224 186 22.6 C 33.0 C 61.8 147

Percent Solids 74.2% 78.8% 67.7% 67.9% 81.0% 76.2%

Station Location : RA22SBc0507MS/MSD RA22SBd0507 RA23SBa0507 RA23SBb0507 RA23SBc0507 RA24SBa0507 Sample ID : MY39L0 D2 MY39L1 MY39L2 MY39L3 MY39L4 MY39L5

Collection Date : 5/15/2007 5/15/2007 5/15/2007 5/15/2007 5/15/2007 5/15/2007

PARAMETER Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com

ARSENIC 108 J AB 19.5 J AB 30.3 J AB 25.0 J AB 12.6 J AB 20.8 J AB

MERCURY 106 178 60.7 43.1 50.0 46.7

Percent Solids 74.4% 78.1% 87.5% 74.6% 75.4% 94.5%

Station Location : RA24SBb0507 RA24SBd0507 RA25SBa0507 RASS35 RASS36 RASS37 Sample ID : MY39L6 MY39L7 MY39L8 MY3977 MY3978 MY3979

Collection Date : 5/15/2007 5/15/2007 5/15/2007 5/17/2007 5/17/2007 5/17/2007

PARAMETER Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com

ARSENIC 54.3 J AB 19.1 J AB 15.5 J AB 21.5 J AB 7.2 J AB 5.6 J AB

MERCURY 41.6 31.3 93.0 18.1 14.4 21.0

Percent Solids 70.8% 82.3% 92.5% 90.7% 91.0% 84.8%

Station Location : RASS38 RASS50 Sample ID : MY3980 MY3983 MDL CRQL

Collection Date : 5/17/2007 5/17/2007

PARAMETER Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com Result Val Com

ARSENIC 11.4 J AB 7.6 J AB 0.31 1.0

MERCURY 26.0 33.3 0.040 0.10

Percent Solids 90.3% 91.2% N/A N/A

Val - Validity. Refer to Data Qualifiers in Table 1B. D1, D2, etc. - Field Duplicate Pairs Com - Comments. Refer to the Corresponding Section in the Narrative for each letter. FB - Field Blank, EB - Equipment Blank, 00105071-8183/36281/MY3977RPT.doc.doc

Environmental Services Assistance Team, Region 9 1337 South 46th Street, Building 201, Richmond, CA 94804-4698 Phone: (510) 412-2300 Fax: (510) 412-2304

MEMORANDUM

DATE: July 24, 2007

CERCLIS ID No.: CAD981893275 Case No.: 36281 SDG No.: MY3977 Laboratory: Bonner Analytical Testing Co. (BONNER) Analysis: CLP Total Arsenic by ICP-AES and Total Mercury Samples: 20 Soil Samples (see Case Summary) Collection Date: May 15 and 17, 2007 Reviewer: Stan Kott, ESAT/Laboratory Data Consultants

This report has been reviewed by the EPA TOM for the ESAT contract, whose signature appears above.

If there are any questions, please contact Rose Fong (QA Program/EPA) at (415) 972-3812.

Attachment cc: Cynthia Gurley, CLP PO USEPA Region 4 Steve Remaley, CLP PO USEPA Region 9

00105071-8183/36281/MY3977RPT.doc.doc Page 1

Case No.: 36281 SDG No.: MY3977 Site: SBMM Road Sampling Laboratory: Bonner Analytical Testing Co. (BONNER) Reviewer: Stan Kott, ESAT/LDC Date: July 24, 2007

I. CASE SUMMARY

Sample Information Samples: MY3977 through MY3980, MY3983, MY39K4 through MY39K9, and MY39L0 through MY39L8 Concentration and Matrix: Low Concentration Soil Analysis: CLP Total Arsenic by ICP-AES and Total Mercury

SOW: ILM05.4

Collection Date: May 15 and 17, 2007 Sample Receipt Date: May 22, 2007 Preparation Date: May 22, 2007 Analysis Date: May 23, 2007

Field QC Field Blanks (FB): Not Provided Equipment Blanks (EB): Not Provided Background Samples (BG): Not Provided Field Duplicates (D1): MY39K6 and MY39K7 Field Duplicates (D2): MY39K9 and MY39L0

Laboratory QC Method Blank & Associated Samples: Preparation Blank-Solid (PBS) and samples listed above Matrix Spike: MY3977S Duplicates: MY3977D ICP Serial Dilution: MY3977L

Analysis: CLP Total Arsenic by ICP-AES and Total Mercury

Sample Preparation Analyte and Digestion Date Analysis Date ICP-AES Arsenic May 22, 2007 May 23, 2007 Mercury May 22, 2007` May 23, 2007

00105071-8183/36281/MY3977RPT.doc.doc Page 2 sample to be used for laboratory quality control (QC). The laboratory selected sample MY3977 for QC analysis and notified the Sample Management Office

3. Airbill numbers 618471978450 and 618471978460 were not provided on the

TR/COC record forms. No adverse effect on data quality is expected.

following dilutions:

10-fold for MY3977, MY3978, MY39K6, and MY39K7;

20-fold for MY3979, MY3980, MY3983, MY39K8, and MY39L2 through MY39L7;

50-fold for MY39K9 and MY39L8;

100-fold for MY39K4, MY39K5, MY39L0, and MY39L1. No adverse effect on data quality is expected.

Samples for this SDG were analyzed for CLP total arsenic by inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and CLP total mercury by cold vapor atomic absorption (CVAA).

All method requirements specified in the EPA Contract Laboratory Program (CLP) Inorganic Statement of Work (SOW), except as noted, have been met.

Analytical results are listed in Table 1A with qualifications. Definitions of data qualifiers used in Table 1A are listed in Table 1B.

This report was prepared in accordance with the following documents:

00105071-8183/36281/MY3977RPT.doc.doc Page 3

1. Data Completeness Yes

2. Sample Preservation and…