### 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: J11050020

Lab Contact: Jason C Perkins 

### Date: 5/26/2011 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: FGD BiMonthly Data Flags & Calculations: Any analytical tests or individual analytes within a test flagged with an "X" or "1" indicate a deviation from the method quali ty system or quality control requirement. 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 estimatio n of the uncertainty of measurement for the results in the report is available upon request. This report shall not be reproduced, ex cept in full, without the written consent of the Analytical Laborator y. 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 Certificati ons : North Carolina (DENR) Certificate #248, South Carolina (DHEC) Laboratory ID # 99005. Contact t he Analytical Laboratory for definitive inform ation about the certification status of specific methods.

## Sample ID's & Descriptions: Sample ID Plant/Station Collection Date and Time Collected By Sample Description 2011009703 BELEWS 11-May-11 8:00 AM Tim Owens FGD Purge Eff 2011009704 BELEWS 11-May-11 8:00 AM Tim Owens EQ TANK EFF. 2011009705 BELEWS 11-May-11 8:00 AM Tim Owens BIOREACTOR 1 INF. 2011009706 BELEWS 11-May-11 8:00 AM Tim Owens BIOREACTOR 2 INF. 2011009707 BELEWS 11-May-11 8:00 AM Tim Owens BIOREACTOR 2 EFF. 2011009708 BELEWS 03-May-11 8:00 AM L.DAVIS FILTER BLANK 2011009709 BELEWS 03-May-11 8:00 AM L.DAVIS Trip Blank 2011009715 BELEWS 11-May-11 8:00 AM Tim Owens BIOREACTOR 1 INF. 2011009723 BELEWS 11-May-11 8:00 AM Tim Owens HG BLANK BIOREACTOR 1 INF. 2011009724 BELEWS 11-May-11 8:00 AM Tim Owens BIOREACTOR 2 INF. 2011009725 BELEWS 11-May-11 8:00 AM Tim Owens Hg Blk BioReactor 2 Inf 2011009726 BELEWS 11-May-11 8:00 AM Tim Owens BIOREACTOR 2 EFF. 2011009727 BELEWS 11-May-11 8:00 AM Tim Owens 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 Test Case Narratives Analytical Laboratory QC Report Chain of Custody

Reviewed By: 

### Mary Ann Ogle Date: 

### 5/26/2011 Yes

Electronic Data Deliverable (EDD) Sent Separately

# Certificate of Laboratory Analysis This re p ort shall not be re p roduced, exce p t in full. 

### Order # J11050020

2011009703 Collection Date: 11-May-11 8:00 AM 

### Site: FGD Purge Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 183 ug/L EPA 245.1 23-May-11 16:00 TLINN 5 TOTAL RECOVERABLE METALS BY ICP Boron (B) 159 mg/L EPA 200.7 13-May-11 12:26 DJSULL1 0.5 DISSOLVED METALS BY ICP-MS Selenium (Se) 4460 ug/L EPA 200.8 19-May-11 14:38 KRICHAR 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 214 ug/L EPA 200.8 18-May-11 13:57 KRICHAR 10 Chromium (Cr) 293 ug/L EPA 200.8 18-May-11 13:57 KRICHAR 10 Copper (Cu) 256 ug/L EPA 200.8 18-May-11 13:57 KRICHAR 10 Nickel (Ni) 284 ug/L EPA 200.8 18-May-11 13:57 KRICHAR 10 Selenium (Se) 5550 ug/L EPA 200.8 18-May-11 13:57 KRICHAR 20 Silver (Ag) < 10 ug/L EPA 200.8 18-May-11 13:57 KRICHAR 10 Zinc (Zn) 430 ug/L EPA 200.8 18-May-11 13:57 KRICHAR 20 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C TOTAL DISSOLVED SOLIDS TDS 24000 mg/L SM2540C 12-May-11 16:50 TJA7067 200 

### 2011009704 Collection Date: 11-May-11 8:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 151 ug/L EPA 245.1 23-May-11 16:02 TLINN 2.5 TOTAL RECOVERABLE METALS BY ICP Boron (B) 167 mg/L EPA 200.7 13-May-11 12:30 DJSULL1 0.5 DISSOLVED METALS BY ICP-MS Selenium (Se) 3820 ug/L EPA 200.8 19-May-11 14:42 KRICHAR 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 181 ug/L EPA 200.8 18-May-11 13:53 KRICHAR 10 Chromium (Cr) 255 ug/L EPA 200.8 18-May-11 13:53 KRICHAR 10 Copper (Cu) 221 ug/L EPA 200.8 18-May-11 13:53 KRICHAR 10 Nickel (Ni) 271 ug/L EPA 200.8 18-May-11 13:53 KRICHAR 10

# Certificate of Laboratory Analysis This re p ort shall not be re p roduced, exce p t in full. 

### Order # J11050020

2011009704 Collection Date: 11-May-11 8:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst TOTAL RECOVERABLE METALS BY ICP-MS Selenium (Se) 4800 ug/L EPA 200.8 18-May-11 13:53 KRICHAR 10 Silver (Ag) < 10 ug/L EPA 200.8 18-May-11 13:53 KRICHAR 10 Zinc (Zn) 391 ug/L EPA 200.8 18-May-11 13:53 KRICHAR 20 

### 2011009705 Collection Date: 11-May-11 8:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst TOTAL RECOVERABLE METALS BY ICP Boron (B) 164 mg/L EPA 200.7 13-May-11 12:34 DJSULL1 0.5 DISSOLVED METALS BY ICP-MS Selenium (Se) 114 ug/L EPA 200.8 19-May-11 14:45 KRICHAR 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 18-May-11 13:48 KRICHAR 10 Chromium (Cr) < 10 ug/L EPA 200.8 18-May-11 13:48 KRICHAR 10 Copper (Cu) < 10 ug/L EPA 200.8 18-May-11 13:48 KRICHAR 10 Nickel (Ni) 40.7 ug/L EPA 200.8 18-May-11 13:48 KRICHAR 10 Selenium (Se) 111 ug/L EPA 200.8 18-May-11 13:48 KRICHAR 10 Silver (Ag) < 10 ug/L EPA 200.8 18-May-11 13:48 KRICHAR 10 Zinc (Zn) < 20 ug/L EPA 200.8 18-May-11 13:48 KRICHAR 20 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011009706 Collection Date: 11-May-11 8:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst TOTAL RECOVERABLE METALS BY ICP Boron (B) 166 mg/L EPA 200.7 13-May-11 12:38 DJSULL1 0.5 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 18-May-11 13:43 KRICHAR 10 Chromium (Cr) < 10 ug/L EPA 200.8 18-May-11 13:43 KRICHAR 10 Copper (Cu) < 10 ug/L EPA 200.8 18-May-11 13:43 KRICHAR 10 Nickel (Ni) < 10 ug/L EPA 200.8 18-May-11 13:43 KRICHAR 10 Selenium (Se) 40.3 ug/L EPA 200.8 18-May-11 13:43 KRICHAR 10 Silver (Ag) < 10 ug/L EPA 200.8 18-May-11 13:43 KRICHAR 10 Zinc (Zn) < 20 ug/L EPA 200.8 18-May-11 13:43 KRICHAR 20

# Certificate of Laboratory Analysis This re p ort shall not be re p roduced, exce p t in full. 

### Order # J11050020

2011009707 Collection Date: 11-May-11 8:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst MERCURY (COLD VAPOR) IN WATER Mercury (Hg) < 1 ug/L EPA 245.1 23-May-11 16:05 TLINN 1 TOTAL RECOVERABLE METALS BY ICP Boron (B) 185 mg/L EPA 200.7 13-May-11 12:42 DJSULL1 0.5 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 5 ug/L EPA 200.8 18-May-11 13:38 KRICHAR 5 Chromium (Cr) < 5 ug/L EPA 200.8 18-May-11 13:38 KRICHAR 5 Copper (Cu) < 5 ug/L EPA 200.8 18-May-11 13:38 KRICHAR 5 Nickel (Ni) < 5 ug/L EPA 200.8 18-May-11 13:38 KRICHAR 5 Selenium (Se) < 5 ug/L EPA 200.8 18-May-11 13:38 KRICHAR 5 Silver (Ag) < 5 ug/L EPA 200.8 18-May-11 13:38 KRICHAR 5 Zinc (Zn) < 10 ug/L EPA 200.8 18-May-11 13:38 KRICHAR 10 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011009708 Collection Date: 03-May-11 8:00 AM 

### Site: FILTER BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DISSOLVED METALS BY ICP-MS Selenium (Se) < 2 ug/L EPA 200.8 19-May-11 14:49 KRICHAR 2 

### 2011009709 Collection Date: 03-May-11 8:00 AM 

### Site: Trip Blank Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst TOTAL RECOVERABLE METALS BY ICP Boron (B) < 0.05 mg/L EPA 200.7 13-May-11 12:02 DJSULL1 0.05 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 1 ug/L EPA 200.8 18-May-11 13:33 KRICHAR 1 Chromium (Cr) < 1 ug/L EPA 200.8 18-May-11 13:33 KRICHAR 1 Copper (Cu) < 1 ug/L EPA 200.8 18-May-11 13:33 KRICHAR 1 Nickel (Ni) < 1 ug/L EPA 200.8 18-May-11 13:33 KRICHAR 1 Selenium (Se) 1.08 ug/L EPA 200.8 18-May-11 13:33 KRICHAR 1 Silver (Ag) < 1 ug/L EPA 200.8 18-May-11 13:33 KRICHAR 1 Zinc (Zn) < 2 ug/L EPA 200.8 18-May-11 13:33 KRICHAR 2 SELENIUM SPECIATION

# Certificate of Laboratory Analysis This re p ort shall not be re p roduced, exce p t in full. 

### Order # J11050020

2011009709 Collection Date: 03-May-11 8:00 AM 

### Site: Trip Blank Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011009715 Collection Date: 11-May-11 8:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst MERCURY 1631 Mercury (Hg) Complete ng/L V_BRAND 1 

### 2011009723 Collection Date: 11-May-11 8:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst MERCURY 1631 Mercury (Hg) Complete ng/L V_BRAND 1 

### 2011009724 Collection Date: 11-May-11 8:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst MERCURY 1631 Mercury (Hg) Complete ng/L V_BRAND 1 

### 2011009725 Collection Date: 11-May-11 8:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst MERCURY 1631 Mercury (Hg) Complete ng/L V_BRAND 1 

### 2011009726 Collection Date: 11-May-11 8:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst MERCURY 1631 Mercury (Hg) Complete ng/L V_BRAND 1

# Certificate of Laboratory Analysis This re p ort shall not be re p roduced, exce p t in full. 

### Order # J11050020

2011009727 Collection Date: 11-May-11 8:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst MERCURY 1631 Mercury (Hg) Complete ng/L V_BRAND 1

### May 20, 2011

Duke Energy ATTN: Jay Perkins 13339 Hagers Ferry Road Huntersville NC 28078 jperkins@duke-energy.com
RE: Project DUK-HV1101 Dear Jay Perkins, This report contains results for the 6 samples received by Brooks Rand Labs (BRL) on May 13, 2011. The samples were logged-in for the contracted analyses according to the chain-of-custody form(s). The samples were received, prepared, analyzed, and stored according to BRL SOPs and EPA methodology. The results were method blank corrected as described in the calculations section of the relevant BRL SOP(s) and may have been evaluated using reporting limits that have been adjusted to account for sample aliquot size. Please refer to the 

### Sample Results page for sample-specific MDLs, MRLs, and other details. All data is reported without qualification (with the exception of concentration qualifiers), and all associated quality control sample results meet the acceptance criteria. BRL, an accredited laboratory, certifies that the reported results of all analyses for which BRL is NELAP accredited meet all NELAP requirements. For more details, please see the 

### Report Information page in your report. Please feel free to contact me if you have any questions regarding this report. Sincerely,

Tiffany Stilwater Project Manager tiffany@brooksrand.com

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: DUK-HV1101

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-HV1101

PM: Tiffany Stilwater Client PM: Jay Perkins Client PO: 141391



# Sample Information

Report Matrix Type Received Sampled Sample Lab ID 1120032-01 BioReactor 1 Inf 05/11/2011 05/13/2011 Sample FGD Wastewater 1120032-02 Hg Blk BioReactor 1 Inf 05/11/2011 05/13/2011 Field Blank DIW 1120032-03 BioReactor 2 Inf 05/11/2011 05/13/2011 Sample FGD Wastewater 1120032-04 Hg Blk BioReactor 2 Inf 05/11/2011 05/13/2011 Field Blank DIW 1120032-05 BioReactor 2 Eff 05/11/2011 05/13/2011 Sample FGD Wastewater 1120032-06 Hg Blk BioReactor 2 Eff 05/11/2011 05/13/2011 Field Blank DIW 

# Batch Summary

Analyte Prepared Analyzed Sequence Batch Lab Matrix Method B110676 05/16/2011 05/19/2011 1100332 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-HV1101

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 101 T 1100332 B110676 FGD Wastewater 4.04 1.52 1120032-01 Hg

BioReactor 2 Eff ng/L 8.65 T 1100332 B110676 FGD Wastewater 0.80 0.30 1120032-05 Hg

BioReactor 2 Inf ng/L 44.1 T 1100332 B110676 FGD Wastewater 4.04 1.52 1120032-03 Hg
Hg Blk BioReactor 1 Inf ng/L 0.15 T U 1100332 B110676 DIW 0.41 0.15 1120032-02 Hg
Hg Blk BioReactor 2 Eff ng/L 0.15 T U 1100332 B110676 DIW 0.41 0.15 1120032-06 Hg
Hg Blk BioReactor 2 Inf ng/L 0.15 T U 1100332 B110676 DIW 0.40 0.15 1120032-04 Hg

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: DUK-HV1101

PM: Tiffany Stilwater Client PM: Jay Perkins Client PO: 141391



# Accuracy & Precision Summary

Analyte Result Units

Native Spike REC & Limits RPD & Limits Batch: B110676
Method: EPA 1631 Lab Matrix: Water

Sample Certified Reference Material (1120043, NIST 1641d 1000x dilution) B110676-SRM1 15.68 103% ng/L 85-115 Hg 16.09 Matrix Spike (1120032-03) B110676-MS2 212.1 114% ng/L 71-125 Hg 286.0

44.08 Matrix Spike Duplicate (1120032-03) B110676-MSD2 212.1 110% ng/L 71-125 243% Hg 277.3

44.08



# Method Blanks & Reporting Limits

Batch: B110676
Method: EPA 1631 Matrix: Water Analyte: Hg Result Units Sample B110676-BLK1 ng/L 0.13 B110676-BLK2 ng/L 0.11 B110676-BLK3 ng/L 0.08 B110676-BLK4 ng/L 0.04 MDL: 0.15 Average: 0.09 Standard Deviation: 0.04 Limit: 0.10 Limit: 0.50 MRL: 0.41

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: DUK-HV1101

PM: Tiffany Stilwater Client PM: Jay Perkins Client PO: 141391



# Instrument Calibration

Method: EPA 1631 Sequence: 1100332 Instrument: THG-05 Date: 05/19/2011 Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg REC & Limits Result True Value Lab ID Units 1100332-CAL1 25.00 93% pg of Hg 23.18 1100332-CAL2 100.0 97% pg of Hg 97.42 1100332-CAL3 500.0 102% pg of Hg 511.6 1100332-CAL4 2500 103% pg of Hg 2581 1100332-CAL5 10000 105% pg of Hg 10530 1100332-CCB1 pg of Hg 16.0 1100332-CCV1 500.0 106% pg of Hg 77-123 528.3 1100332-CCV2 500.0 103% pg of Hg 77-123 514.8 1100332-CCV3 500.0 108% pg of Hg 77-123 539.8 1100332-IBL1 pg of Hg 10.47 1100332-IBL2 pg of Hg 9.81 1100332-IBL3 pg of Hg 11.16 1100332-IBL4 pg of Hg 10.23 1100332-ICV1 1568 103% pg of Hg 85-115 1609

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: DUK-HV1101

PM: Tiffany Stilwater Client PM: Jay Perkins Client PO: 141391



# Sample Containers

Lab ID: 1120032-01 Report Matrix: FGD Wastewater Sample Type: Sample Received: 05/13/2011 Sample: BioReactor 1 Inf Collected: 05/11/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A No Lot # Cooler None N/A 500 mL Bottle Glass

Lab ID: 1120032-02 Report Matrix: DIW Sample Type: Field Blank Received: 05/13/2011 Sample: Hg Blk BioReactor 1 Inf Collected: 05/11/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A No Lot # Cooler None N/A 500 mL Bottle Glass

Lab ID: 1120032-03 Report Matrix: FGD Wastewater Sample Type: Sample Received: 05/13/2011 Sample: BioReactor 2 Inf Collected: 05/11/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A No Lot # Cooler None N/A 500 mL Bottle Glass

Lab ID: 1120032-04 Report Matrix: DIW Sample Type: Field Blank Received: 05/13/2011 Sample: Hg Blk BioReactor 2 Inf Collected: 05/11/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A No Lot # Cooler None N/A 500 mL Bottle Glass

Lab ID: 1120032-05 Report Matrix: FGD Wastewater Sample Type: Sample Received: 05/13/2011 Sample: BioReactor 2 Eff Collected: 05/11/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A No Lot # Cooler None N/A 500 mL Bottle Glass

Lab ID: 1120032-06 Report Matrix: DIW Sample Type: Field Blank Received: 05/13/2011 Sample: Hg Blk BioReactor 2 Eff Collected: 05/11/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A No Lot # Cooler None N/A 500 mL Bottle Glass

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: DUK-HV1101

PM: Tiffany Stilwater Client PM: Jay Perkins Client PO: 141391



# Shipping Containers

Cooler Tracking No: 4726 7966 0403 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 13, 2011 8:45

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

## May 1 9 , 201 1

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 (2010, Bi -Weekly Sampling ) (LIMS # J11050020)

Dear Mr. Perkins, Attached is the report associated with four (4 ) aqueous samples submitted for selenium speciation analysis on May 1 1 , 2011. The samples were received on May 1 3 , 2011 in a sealed cooler at0. 0 o 

## C. Selenium speciation analysis was performed via ion chromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICP-DRC-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,

Ben Wozniak Project Manager 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 (2010, Bi -Weekly Sampling ) (LIMS # J11050020) May 1 9 , 201 1

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 11 , 2011 . The samples were received on May 1 3, 2011 in a sealed co ntainer at 0. 0 o 

## C. The samples were received in a laminar flow clean hood void of trace metals contamination and ultra-violet radiation. Upon reception, the samples were designated discrete sample identifiers. An aliquot of each sample was filtered (0.45μm) and these filtrates were 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 the samples may shift the equilibrium of the system resulting in changes in speciation ratios.

3. Sample Analysis All sample analysis is precluded 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 All samples for selenium speciation analysis were analyzed by ion chromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICP-DRC-MS) on May 18 , 2011 . 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 specific reactive gas 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 very well and no analytical issues were encountered. All sample results have been corrected in accordance with the continuing calibration verification recoveries to account for perceived instrument drift. All quality control parameters associated with these samples were within acceptance limits, demonstrating the suitability of these corrections. 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.

Sincerely,

Ben Wozniak Project Manager Applied Speciation and Consulting, LLC

### Sample Results
Sample ID Se(IV) Se(VI) SeCN MeSe(IV) SeMe Unknown Se Species (n) FGD Purge Eff 94.2 88.8 ND (<2.0) ND (<1.5) ND (<1.5) 0 (0) Bioreactor 1 Inf 9.41 84.6 ND (<0.50) 1.81 ND (<0.38) 0 (0) Bioreactor 2 Eff ND (<0.27) ND (<0.37) ND (<0.50) ND (<0.38) ND (<0.38) 0 (0) Metals Trip Blk ND (<0.055) ND (<0.073) ND (<0.10) ND (<0.076) ND (<0.076) 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: Ben Wozniak Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS (2010, Bi-Weekly Sampling)

Contact: Jay Perkins
Date: May 19, 2011 LIMS #J11050020

### 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 0.005 0.055 0.27 1.1 Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.007 0.073 0.37 1.5 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.10 0.50 2.0 MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.076 0.38 1.5 SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.076 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) ICV 9.57 9.39 98.1 Se(VI) ICV 9.48 9.04 95.4 SeCN ICV 8.92 8.88 99.6 MeSe(IV) ICV 6.47 5.41 83.6 SeMe ICV 9.32 8.31 89.2 LIMS #J11050020 Date: May 19, 2011 Report Generated by: Ben Wozniak Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS (2010, Bi-Weekly Sampling)

Contact: Jay Perkins

### Quality Control Summary - Matrix Duplicates

Analyte (μg/L) Sample ID Rep 1 Rep 2 Mean RPD Se(IV) Bioreactor 2 Eff ND (<0.27) ND (<0.27) NC NC Se(VI) Bioreactor 2 Eff ND (<0.37) ND (<0.37) NC NC SeCN Bioreactor 2 Eff ND (<0.50) ND (<0.50) NC NC MeSe(IV) Bioreactor 2 Eff ND (<0.38) ND (<0.38) NC NC SeMe Bioreactor 2 Eff ND (<0.38) ND (<0.38) NC NC 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) Bioreactor 2 Eff 278.0 264.1 95.0 278.0 267.4 96.2 1.2 Se(VI) Bioreactor 2 Eff 252.3 246.4 97.7 252.3 246.4 97.7 0.0 SeCN Bioreactor 2 Eff 228.8 214.2 93.6 228.8 215.3 94.1 0.5 Report Generated by: Ben Wozniak Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS (2010, Bi-Weekly Sampling)

Contact: Jay Perkins LIMS #J11050020 Date: May 19, 2011