### 13339 Hagers Ferry Road Huntersville, NC 28078-7929 McGuire Nuclear Complex - MG03A2 Phone: 980-875-5245 Fax: 980-875-4349 

# Order Summary Report 

# Analytical Laboratory

Order Number: J12050061 Project Name: WWTS - Biweekly (1)

L ab Contact: Jason C Perkins 

### Date: 5/25/2012 Customer Address: 3195 Pine Hall Rd Customer Name(s): Bill Kennedy, Melonie Martin, Wayne Chapman, Tom Johnson

Mailcode: Belews Steam Station Belews Creek, NC 28012

Phone: 980-875-5348 Report Authorized By: (Signature)


### Program Comments: Please contact the Program Manager (Jason C Perkins) with any questions regarding this report. Data Flags & Calculations: Any analytical tests or individual analytes within a test flagged with a Qualifier indicate a deviation from the method quality system or quality control requirement. The qualifier description is found at the end of the Certificate of Analysis (sample results) under the qualifiers heading. All results are reported on a dry weight basis unless otherwise noted. Data Package: This data package includes analytical results that are applicable only to the samples described in this narrative. An estimation of the uncertainty of measurement for the results in the report is available upon request. This report shall not be reproduced, except in full, without the written consent of the Analytical Laboratory. Please contact the Analytical laboratory with any questions. The order of individual sections within this report is as follows: Job Summary Report, Sample Identification, Technical Validation of Data Package, Analytical Laboratory Certificate of Analysis, Analytical Laboratory QC Reports, Sub-contracted Laboratory Results, Customer Specific Data Sheets, Reports & Documentation, Customer Database Entries, Test Case Narratives, Chain of Custody (COC) Certification: The Analytical Laboratory holds the following State Certifications : North Carolina (DENR) Certificate #248, South Carolina (DHEC) Laboratory ID # 99005. Contact the Analytical Laboratory for definitive information about the certification status of specific methods.

## Sample ID's & Descriptions:

Sample ID Plant/Station Collection Date and Time Collected By Sample Description 2012009938 BELEWS 09-May-12 7:20 AM W. B. WORKMAN FGD Purge Eff 2012009939 BELEWS 09-May-12 7:25 AM W. B. WORKMAN EQ TANK EFF. 2012009940 BELEWS 09-May-12 7:30 AM W. B. WORKMAN BIOREACTOR 1 INF. 2012009941 BELEWS 09-May-12 7:35 AM W. B. WORKMAN BIOREACTOR 2 INF. 2012009942 BELEWS 09-May-12 7:40 AM W. B. WORKMAN BIOREACTOR 2 EFF. 2012009943 BELEWS 09-May-12 8:00 AM W. B. WORKMAN FILTER BLANK 2012009944 BELEWS 09-May-12 8:10 AM W. B. WORKMAN Trip Blank 2012009945 BELEWS 09-May-12 1:00 PM David Morris (Prism) BIOREACTOR 1 INF (HG) 2012009946 BELEWS 09-May-12 1:00 PM David Morris (Prism) HG BLANK BIOREACTOR 1 INF. 2012009947 BELEWS 09-May-12 1:10 PM David Morris (Prism) BIOREACTOR 2 INF (HG) 2012009948 BELEWS 09-May-12 1:10 PM David Morris (Prism) Hg Blk BioReactor 2 Inf 2012009949 BELEWS 09-May-12 1:05 PM David Morris (Prism) BIOREACTOR 2 EFF (HG) 2012009950 BELEWS 09-May-12 1:05 PM David Morris (Prism) Hg Blk BioReactor 2 Eff 13 Total Samples

### COC and .pdf report are in agreement with sample totals

and analyses (compliance programs and procedures). All Results are less than the laboratory reporting limits. All laboratory QA/QC requirements are acceptable. The Vendor Laboratories have been qualified by the Analytical Laboratory Yes No



# Technical Validation Review Checklist:

Yes No

Yes No



## Report Sections Included:

Job Summary Report Sub-contracted Laboratory Results Sample Identification Customer Specific Data Sheets, Reports, & Documentation Technical Validation of Data Package Customer Database Entries Analytical Laboratory Certificate of Analysis Analytical Laboratory QC Report Chain of Custody

Reviewed By: 

### DataBase Administrator Date: 

### 5/25/2012 N/A

Electronic Data Deliverable (EDD) Sent Separately

# Certificate of Laboratory Analysis This report shall not be reproduced, except in full.



## Order # J12050061

2012009938 Collection Date: 09-May-12 7:20 AM 

### Site: FGD Purge Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF INORGANIC IONS BY IC Bromide 210 mg/L EPA 300.0 17-May-12 16:08 JAHERMA 5 50 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 232 ug/L EPA 245.1 10-May-12 14:56 AGIBBS 5 100 TOTAL RECOVERABLE METALS BY ICP Boron (B) 208 mg/L EPA 200.7 22-May-12 13:44 MHH7131 0.5 10 Manganese (Mn) 7.55 mg/L EPA 200.7 22-May-12 13:44 MHH7131 0.05 10 DISSOLVED METALS BY ICP-MS Manganese (Mn) 7020 ug/L EPA 200.8 23-May-12 11:57 DJSULL1 20 20 Selenium (Se) 126 ug/L EPA 200.8 23-May-12 11:57 DJSULL1 20 20 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 207 ug/L EPA 200.8 15-May-12 15:48 MHH7131 10 10 Chromium (Cr) 227 ug/L EPA 200.8 15-May-12 15:48 MHH7131 10 10 Copper (Cu) 113 ug/L EPA 200.8 15-May-12 15:48 MHH7131 10 10 Nickel (Ni) 191 ug/L EPA 200.8 15-May-12 15:48 MHH7131 10 10 Selenium (Se) 4470 ug/L EPA 200.8 15-May-12 15:48 MHH7131 10 10 Silver (Ag) < 10 ug/L EPA 200.8 15-May-12 15:48 MHH7131 10 10 Zinc (Zn) 216 ug/L EPA 200.8 15-May-12 15:48 MHH7131 10 10 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 1 TOTAL DISSOLVED SOLIDS Vendor Parameter Complete V_PACE 1


### 2012009939 Collection Date: 09-May-12 7:25 AM 

### Site: EQ TANK EFF. Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 210 ug/L EPA 245.1 10-May-12 14:58 AGIBBS 2.5 50 TOTAL RECOVERABLE METALS BY ICP Boron (B) 206 mg/L EPA 200.7 22-May-12 13:48 MHH7131 0.5 10 Manganese (Mn) 7.77 mg/L EPA 200.7 22-May-12 13:48 MHH7131 0.05 10

# Certificate of Laboratory Analysis This report shall not be reproduced, except in full.



## Order # J12050061

2012009939 Collection Date: 09-May-12 7:25 AM 

### Site: EQ TANK EFF. Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF DISSOLVED METALS BY ICP-MS Manganese (Mn) 6960 ug/L EPA 200.8 23-May-12 12:00 DJSULL1 20 20 Selenium (Se) 99.2 ug/L EPA 200.8 23-May-12 12:00 DJSULL1 5 5 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 222 ug/L EPA 200.8 15-May-12 15:51 MHH7131 10 10 Chromium (Cr) 235 ug/L EPA 200.8 15-May-12 15:51 MHH7131 10 10 Copper (Cu) 122 ug/L EPA 200.8 15-May-12 15:51 MHH7131 10 10 Nickel (Ni) 199 ug/L EPA 200.8 15-May-12 15:51 MHH7131 10 10 Selenium (Se) 4980 ug/L EPA 200.8 15-May-12 15:51 MHH7131 10 10 Silver (Ag) < 10 ug/L EPA 200.8 15-May-12 15:51 MHH7131 10 10 Zinc (Zn) 211 ug/L EPA 200.8 15-May-12 15:51 MHH7131 10 10


### 2012009940 Collection Date: 09-May-12 7:30 AM 

### Site: BIOREACTOR 1 INF. Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF INORGANIC IONS BY IC Bromide 220 mg/L EPA 300.0 17-May-12 16:26 JAHERMA 5 50 TOTAL RECOVERABLE METALS BY ICP Boron (B) 187 mg/L EPA 200.7 22-May-12 13:52 MHH7131 0.5 10 Manganese (Mn) 1.32 mg/L EPA 200.7 22-May-12 13:52 MHH7131 0.05 10 DISSOLVED METALS BY ICP-MS Manganese (Mn) 1410 ug/L EPA 200.8 23-May-12 12:03 DJSULL1 5 5 Selenium (Se) 90.3 ug/L EPA 200.8 23-May-12 12:03 DJSULL1 5 5 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 15-May-12 15:54 MHH7131 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 15-May-12 15:54 MHH7131 10 10 Copper (Cu) < 10 ug/L EPA 200.8 15-May-12 15:54 MHH7131 10 10 Nickel (Ni) 13.0 ug/L EPA 200.8 15-May-12 15:54 MHH7131 10 10 Selenium (Se) 84.3 ug/L EPA 200.8 15-May-12 15:54 MHH7131 10 10 Silver (Ag) < 10 ug/L EPA 200.8 15-May-12 15:54 MHH7131 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 15-May-12 15:54 MHH7131 10 10 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 1

# Certificate of Laboratory Analysis This report shall not be reproduced, except in full.



## Order # J12050061

2012009941 Collection Date: 09-May-12 7:35 AM 

### Site: BIOREACTOR 2 INF. Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF TOTAL RECOVERABLE METALS BY ICP Boron (B) 192 mg/L EPA 200.7 22-May-12 13:56 MHH7131 0.5 10 Manganese (Mn) 2.20 mg/L EPA 200.7 22-May-12 13:56 MHH7131 0.05 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 15-May-12 15:57 MHH7131 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 15-May-12 15:57 MHH7131 10 10 Copper (Cu) < 10 ug/L EPA 200.8 15-May-12 15:57 MHH7131 10 10 Nickel (Ni) < 10 ug/L EPA 200.8 15-May-12 15:57 MHH7131 10 10 Selenium (Se) 22.8 ug/L EPA 200.8 15-May-12 15:57 MHH7131 10 10 Silver (Ag) < 10 ug/L EPA 200.8 15-May-12 15:57 MHH7131 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 15-May-12 15:57 MHH7131 10 10


### 2012009942 Collection Date: 09-May-12 7:40 AM 

### Site: BIOREACTOR 2 EFF. Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF INORGANIC IONS BY IC Bromide 190 mg/L EPA 300.0 17-May-12 16:44 JAHERMA 5 50 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) < 2.5 ug/L EPA 245.1 10-May-12 15:00 AGIBBS 2.5 50 TOTAL RECOVERABLE METALS BY ICP Boron (B) 196 mg/L EPA 200.7 22-May-12 13:59 MHH7131 0.5 10 Manganese (Mn) 2.46 mg/L EPA 200.7 22-May-12 13:59 MHH7131 0.05 10 DISSOLVED METALS BY ICP-MS Manganese (Mn) 2400 ug/L EPA 200.8 23-May-12 12:06 DJSULL1 10 10 Selenium (Se) 12.6 ug/L EPA 200.8 23-May-12 12:06 DJSULL1 5 5 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 15-May-12 16:00 MHH7131 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 15-May-12 16:00 MHH7131 10 10 Copper (Cu) < 10 ug/L EPA 200.8 15-May-12 16:00 MHH7131 10 10 Nickel (Ni) < 10 ug/L EPA 200.8 15-May-12 16:00 MHH7131 10 10 Selenium (Se) < 10 ug/L EPA 200.8 15-May-12 16:00 MHH7131 10 10 Silver (Ag) < 10 ug/L EPA 200.8 15-May-12 16:00 MHH7131 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 15-May-12 16:00 MHH7131 10 10 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 1

# Certificate of Laboratory Analysis This report shall not be reproduced, except in full.



## Order # J12050061

2012009943 Collection Date: 09-May-12 8:00 AM 

### Site: FILTER BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF DISSOLVED METALS BY ICP-MS Manganese (Mn) 20.2 ug/L EPA 200.8 23-May-12 11:39 DJSULL1 1 1 Selenium (Se) 1.32 ug/L EPA 200.8 23-May-12 11:39 DJSULL1 1 1


### 2012009944 Collection Date: 09-May-12 8:10 AM 

### Site: Trip Blank Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF TOTAL RECOVERABLE METALS BY ICP Boron (B) < 0.05 mg/L EPA 200.7 22-May-12 13:40 MHH7131 0.05 1 Manganese (Mn) < 0.005 mg/L EPA 200.7 22-May-12 13:40 MHH7131 0.005 1 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 1 ug/L EPA 200.8 15-May-12 15:45 MHH7131 1 1 Chromium (Cr) < 1 ug/L EPA 200.8 15-May-12 15:45 MHH7131 1 1 Copper (Cu) < 1 ug/L EPA 200.8 15-May-12 15:45 MHH7131 1 1 Nickel (Ni) < 1 ug/L EPA 200.8 15-May-12 15:45 MHH7131 1 1 Selenium (Se) < 1 ug/L EPA 200.8 15-May-12 15:45 MHH7131 1 1 Silver (Ag) < 1 ug/L EPA 200.8 15-May-12 15:45 MHH7131 1 1 Zinc (Zn) < 1 ug/L EPA 200.8 15-May-12 15:45 MHH7131 1 1 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 1


### 2012009945 Collection Date: 09-May-12 1:00 PM 

### Site: BIOREACTOR 1 INF (HG) Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF MERCURY 1631 Vendor Parameter Complete V_BRAND 1


### 2012009946 Collection Date: 09-May-12 1:00 PM 

### Site: HG BLANK BIOREACTOR 1 INF. Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF MERCURY 1631 Vendor Parameter Complete V_BRAND 1

# Certificate of Laboratory Analysis This report shall not be reproduced, except in full.



## Order # J12050061

2012009947 Collection Date: 09-May-12 1:10 PM 

### Site: BIOREACTOR 2 INF (HG) Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF MERCURY 1631 Vendor Parameter Complete V_BRAND 1


### 2012009948 Collection Date: 09-May-12 1:10 PM 

### Site: Hg Blk BioReactor 2 Inf Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF MERCURY 1631 Vendor Parameter Complete V_BRAND 1


### 2012009949 Collection Date: 09-May-12 1:05 PM 

### Site: BIOREACTOR 2 EFF (HG) Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF MERCURY 1631 Vendor Parameter Complete V_BRAND 1


### 2012009950 Collection Date: 09-May-12 1:05 PM 

### Site: Hg Blk BioReactor 2 Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF MERCURY 1631 Vendor Parameter Complete V_BRAND 1

### 3958 6 th 

### Ave NW • Seattle, WA 98107 • T: 206-632-6206 • F: 206-632-6017 • www.brooksrand.com • brl@brooksrand.com 

## May 21, 2012
Duke Energy ATTN: Jay Perkins Scientific Support-Laboratory 13339 Hagers Ferry Road Huntersville NC 28078 jcperkins@duke-energy.com labcustomer@duke-energy.com
RE: Project DUK-HV1201 Client Project: J12050061 Dear Mr. Perkins, On May 11, 2012, Brooks Rand Labs (BRL) received three (3) wastewater samples and three (3) corresponding field blanks. Samples were logged-in for total mercury (THg) analysis. All samples were received, prepared, analyzed, and stored according to BRL SOPs and EPA methodology. The results were blank-corrected as described in the calculations section of the applicable SOP(s) and may be evaluated using adjusted reporting limits to account for sample aliquot size. Please refer to the Sample Results page for sample-specific detection limits and other details. The analysis of the instrument blank 1200363-IBL2 produced an abnormal peak shape and was re-analyzed as 1200363-IBL5. A typical peak shape was yielded and the re-analysis was reported. The analysis of fourth method blank was a Grubb’s outlier; however, all method blank criteria were met and the method blank was not omitted from the batch. Aside from concentration qualifiers, all data was reported without qualification and all associated quality control sample results met the acceptance criteria. BRL, an accredited laboratory, certifies the reported results of all analyses for which BRL is NELAP accredited meet all NELAP requirements. For more details, see the Report Information page of the report. Please feel free to contact me if you have any questions regarding this report. Sincerely,

Tiffany Stilwater Project Manager tiffany@brooksrand.comProject ID: 

### DUK-HV1201

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



### Definition of Data Qualifiers

(Effective 9/23/09) 

### Laboratory Accreditation BRL is accredited by the National Environmental Laboratory Accreditation Program (NELAP) through the State of Florida Department of Health, Bureau of Laboratories (E87982) and is certified to perform many environmental analyses. BRL is also certified by many other states to perform environmental analyses. For a current list of our accreditations /certifications, please visit our website at <http://www.brooksrand.com/default.asp?contentID=586>. Results reported relate only to the samples listed in the report. 

# Report Information

BLK BRL BS CAL CCV CRM D DUP ICV MSD ND NR PS REC RPD RSD SCV SOP 

### method blank Brooks Rand Labs laboratory fortified blank calibration standard continuing calibration verification certified reference material dissolved fraction duplicate initial calibration verification matrix spike duplicate non-detect non-reportable post preparation spike percent recovery relative percent difference relative standard deviation secondary calibration verification standard operating procedure MDL MRL MS



### method detection limit method reporting limit matrix spike

SRM T COC



### standard reference material total recoverable fraction chain of custody record 

### Common Abbreviations

These qualifiers are based on those previously utilized by Brooks Rand, Ltd., those found in the EPA SOW ILM03.0, Exhibit B, Section III, pg. B-18, and the USEPA Laboratory Data Validation Functional Guidelines for Evaluating Inorganic Analyses; USEPA; July 2002. These supersede all previous qualifiers ever employed by BRL. Detected by the instrument, the result is > the MDL but ≤ the MRL. Result is reported and considered an estimate. B E 

### An estimated value due to the presence of interferences. A full explanation is presented in the narrative. H 

### Holding time and/or preservation requirements not met. Result is estimated. J 

### Estimated value. A full explanation is presented in the narrative. J-M 

### Duplicate precision (RPD) for associated QC sample was not within acceptance criteria. Result is estimated. J-N 

### Spike recovery for associated QC sample was not within acceptance criteria. Result is estimated. M 

### Duplicate precision (RPD) was not within acceptance criteria. Result is estimated. N 

### Spike recovery was not within acceptance criteria. Result is estimated. R 

### Rejected, unusable value. A full explanation is presented in the narrative. U 

### Result is ≤ the MDL or client requested reporting limit (CRRL). Result reported as the MDL or CRRL. X 

### Result is not BLK-corrected and is within 10x the absolute value of the highest detectable BLK in the batch. Result is estimated. 

### Field Quality Control Samples Please be notified that certain EPA methods require the collection of field quality control samples of an appropriate type and frequency; failure to do so is considered a deviation from some methods and for compliance purposes should only be done with the approval of regulatory authorities. Please see the specific EPA methods for details regarding required field quality control samples.

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: 

### DUK-HV1201

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Sample Information

Report Matrix Type Received Sampled Sample Lab ID 

### 1219046-01 BioReactor 1 Inf 05/09/2012 05/11/2012 Sample Influent 1219046-02 Hg Blk BioReactor 1 Inf 05/09/2012 05/11/2012 Field Blank DIW 1219046-03 BioReactor 2 Inf 05/09/2012 05/11/2012 QC Sample Influent 1219046-04 Hg Blk BioReactor 2 Inf 05/09/2012 05/11/2012 Field Blank DIW 1219046-05 BioReactor 2 Eff 05/09/2012 05/11/2012 Sample Effluent 1219046-06 Hg Blk BioReactor 2 Eff 05/09/2012 05/11/2012 Field Blank DIW 

# Batch Summary

Analyte Prepared Analyzed Sequence Batch Lab Matrix Method 

### B120855 05/15/2012 05/17/2012 1200363 Water EPA 1631 Hg

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: 

### DUK-HV1201

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Sample Results

Sample Sequence Result MDL MRL Unit Batch

Qualifier Analyte Fraction

Report Matrix BioReactor 1 Inf 

### ng/L 166 T 1200363 B120855 Influent 8.16 3.06 1219046-01 Hg

BioReactor 2 Eff 

### ng/L 22.1 T 1200363 B120855 Effluent 4.08 1.53 1219046-05 Hg

BioReactor 2 Inf 

### ng/L 42.4 T 1200363 B120855 Influent 8.16 3.06 1219046-03 Hg
Hg Blk BioReactor 1 Inf 

### ng/L 0.15 T U 1200363 B120855 DIW 0.40 0.15 1219046-02 Hg
Hg Blk BioReactor 2 Eff 

### ng/L 0.15 T U 1200363 B120855 DIW 0.41 0.15 1219046-06 Hg
Hg Blk BioReactor 2 Inf 

### ng/L 0.15 T U 1200363 B120855 DIW 0.41 0.15 1219046-04 Hg

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: 

### DUK-HV1201

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Accuracy & Precision Summary

Batch: 

### B120855

Analyte Result Units Native Spike REC & Limits RPD & Limits Method: 

### EPA 1631 Lab Matrix: 

### Water

Sample Certified Reference Material (1217007, NIST 1641d 1000x dilution) B120855-SRM1 

### 15.68 107% ng/L 85-115 Hg 16.75
Matrix Spike (1219046-03) B120855-MS1 

### 204.1 110% ng/L 71-125 Hg 267.1

42.36
Matrix Spike Duplicate (1219046-03) B120855-MSD1 

### 204.1 115% ng/L 71-125 244% Hg 277.7

42.36



# Method Blanks & Reporting Limits

Batch: 

### B120855
Method: 

### EPA 1631 Matrix: 

### Water Analyte: 

### Hg Result Units Sample 

### B120855-BLK1 ng/L 0.06 B120855-BLK2 ng/L 0.05 B120855-BLK3 ng/L 0.03 B120855-BLK4 ng/L 0.24 MDL: 

### 0.15 Average: 

### 0.10 Standard Deviation: 

### 0.10 Limit: 

### 0.10 Limit: 

### 0.50 MRL: 

### 0.40

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: 

### DUK-HV1201

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Instrument Calibration

Sequence: 

### 1200363 Method: 

### EPA 1631 Instrument: 

### THG-05 Date: 

### 05/17/2012 Total Mercury and Mercury Speciation by CVAFS

Analyte: 

### Hg REC & Limits Result True Value Lab ID Units 

### 1200363-IBL1 7.83 pg of Hg 1200363-IBL3 6.63 pg of Hg 1200363-IBL4 8.07 pg of Hg 1200363-CAL1 25.00 23.96 pg of Hg 96% 1200363-CAL2 100.0 100.0 pg of Hg 100% 1200363-CAL3 500.0 484.2 pg of Hg 97% 1200363-CAL4 2500 2638 pg of Hg 106% 1200363-CAL5 10000 10240 pg of Hg 102% 1200363-ICV1 1568 1675 pg of Hg 107% 85-115 1200363-CCV1 500.0 506.7 pg of Hg 101% 77-123 1200363-IBL5 7.14 pg of Hg 1200363-CCB1 17.0 pg of Hg 1200363-CCV2 500.0 492.8 pg of Hg 99% 77-123 1200363-CCV3 500.0 538.0 pg of Hg 108% 77-123

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: 

### DUK-HV1201

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Sample Containers

Lab ID: 

### 1219046-01 Report Matrix: 

### Influent Sample Type: 

### Sample Received: 

### 05/11/2012 Sample: 

### BioReactor 1 Inf Collected: 

### 05/09/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71588260 10 Cooler

None N/A 250 mL Bottle FLPE Hg-T

Lab ID: 

### 1219046-02 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 05/11/2012 Sample: 

### Hg Blk BioReactor 1 Inf Collected: 

### 05/09/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71588260 10 Cooler

None N/A 250 mL Bottle FLPE Hg-T

Lab ID: 

### 1219046-03 Report Matrix: 

### Influent Sample Type: 

### QC Sample Received: 

### 05/11/2012 Sample: 

### BioReactor 2 Inf Collected: 

### 05/09/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71588260 10 Cooler

None N/A 250 mL Bottle FLPE Hg-T

Lab ID: 

### 1219046-04 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 05/11/2012 Sample: 

### Hg Blk BioReactor 2 Inf Collected: 

### 05/09/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71588260 10 Cooler

None N/A 250 mL Bottle FLPE Hg-T

Lab ID: 

### 1219046-05 Report Matrix: 

### Effluent Sample Type: 

### Sample Received: 

### 05/11/2012 Sample: 

### BioReactor 2 Eff Collected: 

### 05/09/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71588260 10 Cooler

None N/A 250 mL Bottle FLPE Hg-T

Lab ID: 

### 1219046-06 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 05/11/2012 Sample: 

### Hg Blk BioReactor 2 Eff Collected: 

### 05/09/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71588260 10 Cooler

None N/A 250 mL Bottle FLPE Hg-T

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: 

### DUK-HV1201

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Shipping Containers

Cooler Tracking No: 

### 4726 7967 0985 via FedEx Temperature: 

### ambient Coolant Type: 

### None Description: 

### Cooler Damaged in transit? 

### No Returned to client? 

### No Custody seals present? 

### No Custody seals intact? 

### No COC present? 

### Yes Received: 

### May 11, 2012 9:00

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.com

## May 1 8 , 201 2

Jay Perkins Duke Energy Analytical Laboratory Mail Code MGO3A2 (Building 7405) 13339 Hagers Ferry Rd. Huntersville, NC 28078 (704) 875-5 245 Project: Belews

– FGD WWTS (Bi-Monthly Wed Sampling) (LIMS # J1 20 500 61)

Dear Mr. Perkins , Attached is the report associated with four (4 ) aqueous samples submitted for selenium speciation analysis on May 10 , 2012

. The samples were received in a sealed cooler at3.7 ° C on May 11, 2012

. Selenium speciation analysis was performed via ion chromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICP-D RC -MS). Any issues associated with the analysis are addressed in the following report. If you have any questions, please feel free to contact me at your convenience.
Sincerely,

Russell Gerads Vice President Applied Speciation and Consulting, LLC

## Applied Speciation and Consulting, LLC Report prepared for: Jay Perkins Duke Energy Analytical Laboratory Mail Code MGO3A2 (Building 7405) 13339 Hagers Ferry Rd. Huntersville, NC 28078 Project: Belews

– FGD WWTS (Bi-Monthly Wed Sampling) (LIMS # J1 20500 61 )
May 1 8 , 2012

1. Sample Reception Four (4 ) aqueous samples in125mL HDPE bottles (provided by Applied Speciation and Consulting) were submitted for selenium speciation analysi s on May 10 , 2012. The samples were received on May 11, 201 2 in a sealed co ntainer at 3.7 ° C. The samples were received in a laminar flow clean hood, void of trace metals contamination and ultra-violet radiation, and was designated a discrete sample identifier. An aliquot of each sample was filtered (0.45μm) and each filtrate w as stored in a secure, monitored cryofreezer (maintained at a temperature of -80 o 

## C) until selenium speciation analysis could be performed via ion chromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICP-DRC-MS).

2. Sample Preparation All sample preparation is performed in laminar flow clean hoods known to be free from trace metals contamination. All applied water for dilutions and sample preservatives are monitored for contamination to account for any biases associated with the sample results. Selenium Speciation Analysis by IC -ICP-DRC

- MS Prior to analysis, an aliquot of each sample was filtered with a syringe filter (0.45μm) and injected directly into a sealed autosampler vial. No further sample preparation was performed as any chemical alteration of a sample may shift the equilibrium of the system, resulting in changes in speciation ratios. 3. Sample Analysis All sample analysis is preceded by a minimum of a five-point calibration curve spanning the entire concentration range of interest. Calibration curves are performed at the beginning of each analytical day. All calibration curves, associated with each species of interest, are

## standardized by linear regression resulting in a response factor. All sample results are

instrument blank corrected to account for any operational biases associated with the analytical platform. Prior to sample analysis, all calibration curves are verified using second source standard s which are identified as initial calibration verification standards (ICV). Ongoing instrument performance is identified by the analysis of continuing calibration verification standards (CCV) and continuing calibration blanks (CCB) at a minimal interval of every ten analytical runs. Selenium Speciation Analysis by IC -ICP-DRC

- MS Eachsample for selenium speciation analysis w as analyzed by ion chromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICP-DRC-MS) on May 11 , 2012 . An aliquot of eachsample is injected onto an anion exchange column and mobilized by a basic (pH > 7) gradient. The eluting selenium species are then introduced into a radio frequency (RF) plasma where energy-transfer processes cause desolvation, atomization, and ionization. The ions are extracted from the plasma through a differentially-pumped vacuum interface and travel through a pressurized chamber (DRC) containing a reactiongas which preferentially reacts with interfering ions of the same target mass to charge ratios (m/z). A solid-state detector detects ions transmitted through the mass analyzer and the resulting current is processed by a data handling system. Retention times for each eluting species are compared to known standards for species identification.

4. Analytical Issues The overall analyses went well and no significant analytical issues were encountered. All quality control parameters associated with this sample were within acceptance limits. The estimated method detection limits (eMDLs) for selenite, selenate, and selenocyanate are generated from replicate analyses of the lowest standard in the calibration curve. Not all selenium species are present in preparation blanks; therefore, eMDL calculations based on preparation blanks are artificially biased low. The eMDL for methylseleninic acid and selenomethionine is calculated from the average eMDL of selenite, selenate, and selenocyanate. The calibration does not contain methylseleninic acid or selenomethionine due to impurities in these standards which would bias the results for other selenium species.

## If you have any questions or concerns regarding this report, please feel free to contact me.

Si ncerely,

Russell Gerads Vice President Applied Speciation and Consulting, LLC

### Sample Results

Sample ID Se(IV) Se(VI) SeCN MeSe(IV) SeMe Unknown Se Species (n) FGD Purge Eff 31.9 61.0 ND (<1.6) 4.1 ND (<1.5) 0 (0) BioReactor 1 Inf 12.3 51.6 ND (<0.41) 1.92 ND (<0.38) 1.06 (1) BioReactor 2 Eff ND (<0.40) ND (<0.34) ND (<0.41) ND (<0.38) ND (<0.38) 0 (0) Metals Trip Blk ND (<0.079) ND (<0.069) ND (<0.082) ND (<0.077) ND (<0.077) 0 (0) All results reflect the applied dilution and are reported in μg/L ND = Not detected at the applied dilution SeCN = Selenocyanate MeSe(IV) = Methylseleninic acid SeMe = Selenomethionine Unknown Se Species = Total concentration of all unknown Se species observed by IC-ICP-MS n = number of unknown Se species observed Report Generated by: Russell Gerads Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS (Bi-Monthly Wed Sampling)

Contact: Jay Perkins
Date: May 18, 2012 LIMS #J12050061

### Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 10x eMDL 50x eMDL 200x Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.079 0.40 1.6 Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.007 0.069 0.34 1.4 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.082 0.41 1.6 MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.077 0.38 1.5 SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.077 0.38 1.5 eMDL = Estimated Method Detection Limit *Please see narrative regarding eMDL calculations
Quality Control Summary - Certified Reference Materials Analyte (μg/L) CRM True Value Result Recovery Se(IV) LCS 9.57 9.59 100.3 Se(VI) LCS 9.48 9.22 97.2 SeCN LCS 8.92 8.92 100.0 MeSe(IV) LCS 6.47 5.77 89.2 SeMe LCS 9.32 8.69 93.2 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS (Bi-Monthly Wed Sampling)

Contact: Jay Perkins LIMS #J12050061 Date: May 18, 2012 Report Generated by: Russell Gerads

### Quality Control Summary - Matrix Duplicates

Analyte (μg/L) Sample ID Rep 1 Rep 2 Mean RPD Se(IV) Batch QC 1.21 1.19 1.20 2.0 Se(VI) Batch QC 1106 1115 1111 0.8 SeCN Batch QC ND (<0.41) ND (<0.41) NC NC MeSe(IV) Batch QC 0.48 ND (<0.38) NC NC SeMe Batch QC 3.16 3.45 3.30 8.7 ND = Not detected at the applied dilution NC = Value was not calculated due to one or more concentrations below the eMDL

Quality Control Summary - Matrix Spike/ Matrix Spike Duplicate Analyte (μg/L) Sample ID Spike Conc MS Result Recovery Spike Conc MSD Result Recovery RPD Se(IV) Batch QC 278.0 290.8 104.2 278.0 296.4 106.2 1.9 Se(VI) Batch QC 252.3 1369 102.5 252.3 1357 97.7 0.9 SeCN Batch QC 228.8 177.2 77.5 228.8 164.3 71.8 7.6 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS (Bi-Monthly Wed Sampling)

Contact: Jay Perkins LIMS #J12050061 Date: May 18, 2012 Report Generated by: Russell Gerads

## May 17, 2012

LIMS USE: FR - PROGRAM MANAGER LIMS OBJECT ID: 92118330



## 92118330 Project: Pace Project No.: RE: Program Manager Duke Energy

,

J12050061

Dear Program Manager: Enclosed are the analytical results for sample(s) received by the laboratory on May 10, 2012. The results relate only to the samples included in this report. Results reported herein conform to the most current TNI standards and the laboratory's Quality Assurance Manual, where applicable, unless otherwise noted in the body of the report.
Analyses were performed at the Pace Analytical Services location indicated on the sample analyte page for analysis unless otherwise footnoted. If you have any questions concerning this report, please feel free to contact me.
Sincerely,

Kevin Herring kevin.herring@pacelabs.com Project Manager

Enclosures



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Page 1 of 7 Pace Analytical Services, Inc. 9800 Kincey Ave. Suite 100 Huntersville, NC 28078 (704)875-9092 Pace Analytical Services, Inc.

2225 Riverside Dr. Asheville, NC 28804 (828)254-7176 Pace Analytical Services, Inc. 205 East Meadow Road - Suite A

Eden, NC 27288 (336)623-8921

### CERTIFICATIONS

Pace Project No.: Project: 92118330

J12050061

Asheville Certification IDs 2225 Riverside Dr., Asheville, NC 28804 Florida/NELAP Certification #: E87648 Massachusetts Certification #: M-NC030 North Carolina Drinking Water Certification #: 37712 North Carolina Wastewater Certification #: 40 South Carolina Certification #: 99030001 Virginia Certification #: 00072 West Virginia Certification #: 356 Virgina/VELAP Certification #: 460147



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Page 2 of 7 Pace Analytical Services, Inc. 9800 Kincey Ave. Suite 100 Huntersville, NC 28078 (704)875-9092 Pace Analytical Services, Inc.

2225 Riverside Dr. Asheville, NC 28804 (828)254-7176 Pace Analytical Services, Inc. 205 East Meadow Road - Suite A

Eden, NC 27288 (336)623-8921

### SAMPLE ANALYTE COUNT

Pace Project No.: Project: 92118330

J12050061

Lab ID Sample ID Method Analytes Reported Laboratory Analysts 92118330001 2012009938 SM 2540C 1 PASI-A LMD



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Page 3 of 7 Pace Analytical Services, Inc. 9800 Kincey Ave. Suite 100 Huntersville, NC 28078 (704)875-9092 Pace Analytical Services, Inc.

2225 Riverside Dr. Asheville, NC 28804 (828)254-7176 Pace Analytical Services, Inc. 205 East Meadow Road - Suite A

Eden, NC 27288 (336)623-8921

### ANALYTICAL RESULTS

Pace Project No.: Project: 92118330

J12050061
Sample: 2012009938 Lab ID: 92118330001 Collected: 05/09/12 07:20 Received: 05/10/12 16:15 Matrix: Water

Parameters Results Units DF Prepared Analyzed CAS No. Qual Report Limit
2540C Total Dissolved Solids Analytical Method: SM 2540C Total Dissolved Solids 11900 mg/L 1 05/15/12 17:59 500



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Date: 05/17/2012 02:59 PM Page 4 of 7 Pace Analytical Services, Inc. 9800 Kincey Ave. Suite 100 Huntersville, NC 28078 (704)875-9092 Pace Analytical Services, Inc.

2225 Riverside Dr. Asheville, NC 28804 (828)254-7176 Pace Analytical Services, Inc. 205 East Meadow Road - Suite A

Eden, NC 27288 (336)623-8921

### QUALITY CONTROL DATA

Pace Project No.: Project: 92118330

J12050061

QC Batch: QC Batch Method: Analysis Method: Analysis Description: WET/20870 SM 2540C SM 2540C 2540C Total Dissolved Solids Associated Lab Samples: 92118330001

Parameter Units Blank Result Reporting

Limit Qualifiers METHOD BLANK: 764179 Associated Lab Samples: 92118330001 Matrix: Water

Analyzed Total Dissolved Solids mg/L ND 25.0 05/15/12 17:53

Parameter Units LCS Result % Rec Limits Qualifiers % Rec Conc. 764180 LABORATORY CONTROL SAMPLE: LCS Spike

Total Dissolved Solids mg/L 258 250 103 80-120

Parameter Units Dup Result Qualifiers

RPD Result 92118279001 764181 SAMPLE DUPLICATE:

Total Dissolved Solids mg/L 3720 6 3520

Parameter Units Dup Result Qualifiers

RPD Result 92118319008 764182 SAMPLE DUPLICATE:

Total Dissolved Solids mg/L 72.0 1 71.0



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Date: 05/17/2012 02:59 PM Page 5 of 7 Pace Analytical Services, Inc. 9800 Kincey Ave. Suite 100 Huntersville, NC 28078 (704)875-9092 Pace Analytical Services, Inc.

2225 Riverside Dr. Asheville, NC 28804 (828)254-7176 Pace Analytical Services, Inc. 205 East Meadow Road - Suite A

Eden, NC 27288 (336)623-8921

### QUALIFIERS

Pace Project No.: Project: 92118330

J12050061

DEFINITIONS DF - Dilution Factor, if reported, represents the factor applied to the reported data due to changes in sample preparation, dilution of the sample aliquot, or moisture content. ND - Not Detected at or above adjusted reporting limit. J - Estimated concentration above the adjusted method detection limit and below the adjusted reporting limit. MDL - Adjusted Method Detection Limit. S - Surrogate 1,2-Diphenylhydrazine (8270 listed analyte) decomposes to Azobenzene. Consistent with EPA guidelines, unrounded data are displayed and have been used to calculate % recovery and RPD values. LCS(D) - Laboratory Control Sample (Duplicate) MS(D) - Matrix Spike (Duplicate) DUP - Sample Duplicate RPD - Relative Percent Difference NC - Not Calculable. SG - Silica Gel - Clean-Up U - Indicates the compound was analyzed for, but not detected. N-Nitrosodiphenylamine decomposes and cannot be separated from Diphenylamine using Method 8270. The result reported for each analyte is a combined concentration. Acid preservation may not be appropriate for 2-Chloroethylvinyl ether, Styrene, and Vinyl chloride. Pace Analytical is TNI accredited. Contact your Pace PM for the current list of accredited analytes. TNI - The NELAC Institute. LABORATORIES Pace Analytical Services - Asheville PASI-A



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Date: 05/17/2012 02:59 PM Page 6 of 7 Pace Analytical Services, Inc. 9800 Kincey Ave. Suite 100 Huntersville, NC 28078 (704)875-9092 Pace Analytical Services, Inc.

2225 Riverside Dr. Asheville, NC 28804 (828)254-7176 Pace Analytical Services, Inc. 205 East Meadow Road - Suite A

Eden, NC 27288 (336)623-8921

### QUALITY CONTROL DATA CROSS REFERENCE TABLE

Pace Project No.: Project: 92118330

J12050061

Lab ID Sample ID QC Batch Method QC Batch Analytical Method Analytical Batch 92118330001 WET/20870 2012009938 SM 2540C



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Date: 05/17/2012 02:59 PM Page 7 of 7 Pace Analytical Services, Inc. 9800 Kincey Ave. Suite 100 Huntersville, NC 28078 (704)875-9092 Pace Analytical Services, Inc.

2225 Riverside Dr. Asheville, NC 28804 (828)254-7176 Pace Analytical Services, Inc. 205 East Meadow Road - Suite A

Eden, NC 27288 (336)623-8921