### 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: J11060066 Project Name: WWTS - Biweekly

L ab Contact: Jason C Perkins 

### Date: 6/23/2011 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 Sampling Data Flags & Calculations: Any analytical tests or individual analytes within a test flagged with an "X" or "1" indicate a deviation from the method quality 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 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 2011012191 BELEWS 08-Jun-11 8:00 AM W. B. WORKMAN FGD Purge Eff 2011012192 BELEWS 08-Jun-11 8:05 AM W. B. WORKMAN EQ TANK EFF. 2011012193 BELEWS 08-Jun-11 8:10 AM W. B. WORKMAN BIOREACTOR 1 INF. 2011012194 BELEWS 08-Jun-11 8:15 AM W. B. WORKMAN BIOREACTOR 2 INF. 2011012195 BELEWS 08-Jun-11 8:20 AM W. B. WORKMAN BIOREACTOR 2 EFF. 2011012196 BELEWS 02-Jun-11 10:00 AM S.S. Trip Blank 2011012197 BELEWS 02-Jun-11 10:00 AM S.S. FILTER BLANK 2011012198 BELEWS 08-Jun-11 11:17 AM ILLEGIBLE BIOREACTOR 1 INF. 2011012199 BELEWS 08-Jun-11 11:17 AM ILLEGIBLE HG BLANK BIOREACTOR 1 INF. 2011012200 BELEWS 08-Jun-11 11:34 AM ILLEGIBLE BIOREACTOR 2 INF. 2011012201 BELEWS 08-Jun-11 11:34 AM ILLEGIBLE Hg Blk BioReactor 2 Inf 2011012202 BELEWS 08-Jun-11 11:27 AM ILLEGIBLE BIOREACTOR 2 EFF. 2011012203 BELEWS 08-Jun-11 11:27 AM ILLEGIBLE 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 C hecklist:

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: 

### DataBase Administrator Date: 

### 6/23/2011 Yes

Electronic Data Deliverable (EDD) Sent Separately

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



### Order # J11060066

2011012191 Collection Date: 08-Jun-11 8:00 AM 

### Site: FGD Purge Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 167 ug/L EPA 245.1 10-Jun-11 12:15 TLINN 5
TOTAL RECOVERABLE METALS BY ICP Boron (B) 160 mg/L EPA 200.7 16-Jun-11 12:30 MHH7131 0.5
DISSOLVED METALS BY ICP-MS Selenium (Se) 457 ug/L EPA 200.8 13-Jun-11 13:08 KRICHAR 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 248 ug/L EPA 200.8 20-Jun-11 15:06 KRICHAR 10 Chromium (Cr) 204 ug/L EPA 200.8 20-Jun-11 15:06 KRICHAR 10 Copper (Cu) 194 ug/L EPA 200.8 20-Jun-11 15:06 KRICHAR 10 Nickel (Ni) 213 ug/L EPA 200.8 20-Jun-11 15:06 KRICHAR 10 Selenium (Se) 3680 ug/L EPA 200.8 20-Jun-11 15:06 KRICHAR 10 Silver (Ag) < 10 ug/L EPA 200.8 20-Jun-11 15:06 KRICHAR 10 Zinc (Zn) 321 ug/L EPA 200.8 20-Jun-11 15:06 KRICHAR 20
SELENIUM SPECIATION Vendor Parameter Complete V_AS&C
TOTAL DISSOLVED SOLIDS TDS 21000 mg/L SM2540C 14-Jun-11 17:00 CLEEMAN 10 

### 2011012192 Collection Date: 08-Jun-11 8:05 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 154 ug/L EPA 245.1 10-Jun-11 12:17 TLINN 2.5
TOTAL RECOVERABLE METALS BY ICP Boron (B) 150 mg/L EPA 200.7 16-Jun-11 12:34 MHH7131 0.5
DISSOLVED METALS BY ICP-MS Selenium (Se) 518 ug/L EPA 200.8 13-Jun-11 13:05 KRICHAR 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 191 ug/L EPA 200.8 20-Jun-11 14:56 KRICHAR 10 Chromium (Cr) 187 ug/L EPA 200.8 20-Jun-11 14:56 KRICHAR 10 Copper (Cu) 160 ug/L EPA 200.8 20-Jun-11 14:56 KRICHAR 10 Nickel (Ni) 188 ug/L EPA 200.8 20-Jun-11 14:56 KRICHAR 10

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



### Order # J11060066

2011012192 Collection Date: 08-Jun-11 8:05 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst TOTAL RECOVERABLE METALS BY ICP-MS Selenium (Se) 3740 ug/L EPA 200.8 20-Jun-11 14:56 KRICHAR 10 Silver (Ag) < 10 ug/L EPA 200.8 20-Jun-11 14:56 KRICHAR 10 Zinc (Zn) 267 ug/L EPA 200.8 20-Jun-11 14:56 KRICHAR 20 

### 2011012193 Collection Date: 08-Jun-11 8:10 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst TOTAL RECOVERABLE METALS BY ICP Boron (B) 151 mg/L EPA 200.7 16-Jun-11 12:38 MHH7131 0.5
DISSOLVED METALS BY ICP-MS Selenium (Se) 533 ug/L EPA 200.8 13-Jun-11 13:01 KRICHAR 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 20-Jun-11 14:17 KRICHAR 10 Chromium (Cr) < 10 ug/L EPA 200.8 20-Jun-11 14:17 KRICHAR 10 Copper (Cu) < 10 ug/L EPA 200.8 20-Jun-11 14:17 KRICHAR 10 Nickel (Ni) 21.3 ug/L EPA 200.8 20-Jun-11 14:17 KRICHAR 10 Selenium (Se) 521 ug/L EPA 200.8 20-Jun-11 14:17 KRICHAR 10 Silver (Ag) < 10 ug/L EPA 200.8 20-Jun-11 14:17 KRICHAR 10 Zinc (Zn) < 20 ug/L EPA 200.8 20-Jun-11 14:17 KRICHAR 20
SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011012194 Collection Date: 08-Jun-11 8:15 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst TOTAL RECOVERABLE METALS BY ICP Boron (B) 149 mg/L EPA 200.7 16-Jun-11 12:42 MHH7131 0.5
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 20-Jun-11 14:07 KRICHAR 10 Chromium (Cr) < 10 ug/L EPA 200.8 20-Jun-11 14:07 KRICHAR 10 Copper (Cu) < 10 ug/L EPA 200.8 20-Jun-11 14:07 KRICHAR 10 Nickel (Ni) < 10 ug/L EPA 200.8 20-Jun-11 14:07 KRICHAR 10 Selenium (Se) 30.1 ug/L EPA 200.8 20-Jun-11 14:07 KRICHAR 10 Silver (Ag) < 10 ug/L EPA 200.8 20-Jun-11 14:07 KRICHAR 10 Zinc (Zn) < 20 ug/L EPA 200.8 20-Jun-11 14:07 KRICHAR 20

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



### Order # J11060066

2011012195 Collection Date: 08-Jun-11 8:20 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY (COLD VAPOR) IN WATER Mercury (Hg) < 1 ug/L EPA 245.1 10-Jun-11 12:32 TLINN 1
TOTAL RECOVERABLE METALS BY ICP Boron (B) 146 mg/L EPA 200.7 16-Jun-11 12:46 MHH7131 0.5
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 5 ug/L EPA 200.8 20-Jun-11 13:57 KRICHAR 5 Chromium (Cr) < 5 ug/L EPA 200.8 20-Jun-11 13:57 KRICHAR 5 Copper (Cu) < 5 ug/L EPA 200.8 20-Jun-11 13:57 KRICHAR 5 Nickel (Ni) < 5 ug/L EPA 200.8 20-Jun-11 13:57 KRICHAR 5 Selenium (Se) < 5 ug/L EPA 200.8 20-Jun-11 13:57 KRICHAR 5 Silver (Ag) < 5 ug/L EPA 200.8 20-Jun-11 13:57 KRICHAR 5 Zinc (Zn) < 10 ug/L EPA 200.8 20-Jun-11 13:57 KRICHAR 10
SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011012196 Collection Date: 02-Jun-11 10:00 AM 

### Site: Trip Blank Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst TOTAL RECOVERABLE METALS BY ICP Boron (B) < 0.05 mg/L EPA 200.7 16-Jun-11 12:14 MHH7131 0.05
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 1 ug/L EPA 200.8 20-Jun-11 13:53 KRICHAR 1 Chromium (Cr) < 1 ug/L EPA 200.8 20-Jun-11 13:53 KRICHAR 1 Copper (Cu) 1.78 ug/L EPA 200.8 20-Jun-11 13:53 KRICHAR 1 Nickel (Ni) < 1 ug/L EPA 200.8 20-Jun-11 13:53 KRICHAR 1 Selenium (Se) 1.30 ug/L EPA 200.8 20-Jun-11 13:53 KRICHAR 1 Silver (Ag) < 1 ug/L EPA 200.8 20-Jun-11 13:53 KRICHAR 1 Zinc (Zn) 2.51 ug/L EPA 200.8 20-Jun-11 13:53 KRICHAR 2
SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011012197 Collection Date: 02-Jun-11 10:00 AM 

### Site: FILTER BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DISSOLVED METALS BY ICP-MS

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



### Order # J11060066

2011012197 Collection Date: 02-Jun-11 10:00 AM 

### Site: FILTER BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DISSOLVED METALS BY ICP-MS Selenium (Se) < 2 ug/L EPA 200.8 13-Jun-11 12:48 KRICHAR 2 

### 2011012198 Collection Date: 08-Jun-11 11:17 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND 

### 2011012199 Collection Date: 08-Jun-11 11:17 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND 

### 2011012200 Collection Date: 08-Jun-11 11:34 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND 

### 2011012201 Collection Date: 08-Jun-11 11:34 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND 

### 2011012202 Collection Date: 08-Jun-11 11:27 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND

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



### Order # J11060066

2011012203 Collection Date: 08-Jun-11 11:27 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND3958 6 th Ave NW • Seattle, WA 98107 • T: 206-632-6206 • F: 206-632-6017 • www.brooksrand.com • brl@brooksrand.com 

### June 17, 2011 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-HV1101 Client Project: J11060066 Dear Mr. Perkins, On June 10, 2011, Brooks Rand Labs (BRL) received three (3) flue gas desulfurization (FGD) waste water samples and three (3) corresponding field blanks. During shipping the sample container for BioReactor 2 EFF was broken and unsalvageable. The client was contacted andinformed BRL to proceed with the analysis of the five remaining samples. Samples were loggedin for total mercury (Hg) analysis and 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. All quality assurance criteria were satisfied, and all data was reported without additional qualification, aside from concentration qualifiers. 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-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 1124031-01 BioReactor 1 Inf 06/08/2011 06/10/2011 Sample FGD Wastewater 1124031-02 Hg Blk BioReactor 1 Inf 06/08/2011 06/10/2011 Field Blank DIW 1124031-03 BioReactor 2 Inf 06/08/2011 06/10/2011 QC Sample FGD Wastewater 1124031-04 Hg Blk BioReactor 2 Inf 06/08/2011 06/10/2011 Field Blank DIW 1124031-05 Hg Blk BioReactor 2 Eff 06/08/2011 06/10/2011 Field Blank DIW 

# Batch Summary

Analyte Prepared Analyzed Sequence Batch Lab Matrix Method B110838 06/13/2011 06/14/2011 1100399 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 120 T 1100399 B110838 FGD Wastewater 4.04 1.52 1124031-01 Hg

BioReactor 2 Inf ng/L 197 T 1100399 B110838 FGD Wastewater 8.08 3.03 1124031-03 Hg
Hg Blk BioReactor 1 Inf ng/L 0.15 T U 1100399 B110838 DIW 0.40 0.15 1124031-02 Hg
Hg Blk BioReactor 2 Eff ng/L 0.15 T U 1100399 B110838 DIW 0.40 0.15 1124031-05 Hg
Hg Blk BioReactor 2 Inf ng/L 0.15 T U 1100399 B110838 DIW 0.40 0.15 1124031-04 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: B110838
Method: EPA 1631 Lab Matrix: Water

Sample Certified Reference Material (1125015, NIST 1641d 1000x dilution) B110838-SRM1 15.68 99% ng/L 85-115 Hg 15.55 Matrix Spike (1124031-03) B110838-MS1 1010 100% ng/L 71-125 Hg 1208

197.2 Matrix Spike Duplicate (1124031-03) B110838-MSD1 1010 105% ng/L 71-125 244% Hg 1257

197.2



# Method Blanks & Reporting Limits

Batch: B110838
Method: EPA 1631 Matrix: Water Analyte: Hg Result Units Sample B110838-BLK1 ng/L 0.07 B110838-BLK2 ng/L 0.04 B110838-BLK3 ng/L 0.10 B110838-BLK4 ng/L 0.05 MDL: 0.15 Average: 0.07 Standard Deviation: 0.03 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-HV1101

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



# Instrument Calibration

Method: EPA 1631 Sequence: 1100399 Instrument: THG-10 Date: 06/14/2011 Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg REC & Limits Result True Value Lab ID Units 1100399-IBL1 pg of Hg 10.72 1100399-IBL2 pg of Hg 8.78 1100399-IBL3 pg of Hg 10.52 1100399-IBL4 pg of Hg 10.17 1100399-CAL1 25.00 105% pg of Hg 26.14 1100399-CAL2 100.0 95% pg of Hg 95.39 1100399-CAL3 500.0 100% pg of Hg 501.9 1100399-CAL4 2500 102% pg of Hg 2542 1100399-CAL5 10000 98% pg of Hg 9849 1100399-ICV1 1568 99% pg of Hg 85-115 1555 1100399-CCB1 pg of Hg 14.3 1100399-CCV1 500.0 97% pg of Hg 77-123 486.3 1100399-CCV2 500.0 97% pg of Hg 77-123 487.4

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: 1124031-01 Report Matrix: FGD Wastewater Sample Type: Sample Received: 06/10/2011 Sample: BioReactor 1 Inf Collected: 06/08/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A No Lot # Cardboard Box None N/A 500 mL Bottle Glass

Lab ID: 1124031-02 Report Matrix: DIW Sample Type: Field Blank Received: 06/10/2011 Sample: Hg Blk BioReactor 1 Inf Collected: 06/08/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A No Lot # Cardboard Box None N/A 500 mL Bottle Glass

Lab ID: 1124031-03 Report Matrix: FGD Wastewater Sample Type: QC Sample Received: 06/10/2011 Sample: BioReactor 2 Inf Collected: 06/08/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A No Lot # Cardboard Box None N/A 500 mL Bottle Glass

Lab ID: 1124031-04 Report Matrix: DIW Sample Type: Field Blank Received: 06/10/2011 Sample: Hg Blk BioReactor 2 Inf Collected: 06/08/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A No Lot # Cardboard Box None N/A 500 mL Bottle Glass

Lab ID: 1124031-05 Report Matrix: DIW Sample Type: Field Blank Received: 06/10/2011 Sample: Hg Blk BioReactor 2 Eff Collected: 06/08/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A No Lot # Cardboard Box 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

Cardboard Box Tracking No: 4726 7966 1248 via FedEx Temperature: ambient Coolant Type: None Description: Cardboard Box Damaged in transit? No Returned to client? No Custody seals present? No Custody seals intact? No COC present? Yes Received: June 10, 2011 8:45

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

## June 16 , 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 Bi-Monthly Sampling) (LIMS # J11060066) Dear Mr. Perkins, Attached is the report associated with four (4 ) aqueous samples submitted for selenium speciation analysis on June 9 , 2011. The samples were received in a sealed cooler at9.4 o 

## C on June 10, 2011. 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 Bi-Monthly Sampling) (LIMS # J11060066) June 16, 201 1

1. Sample Reception Four (4 ) aqueous samples in 125mL HDPE bottles (provided by Applied Speciation and Consulting) were su bmitted for selenium speciation analysi s on June 9 , 2011 . The samples were received on June 10, 2011 in a sealed co ntainer at 9.4 o 

## C. Applied Speciation and Consulting strongly recommends that samples submitted for selenium speciation analysis remain at a temperature of ≤6 o 

## C to maintain sample integrity prior to analysis. 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 usin g 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- IC P-DRC-MS) on June 11, 2011 . An aliquot of each sample 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. 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 159 299 6.0 ND (<4.6) ND (<4.6) 0 (0) BioReactor 1 Inf 40.5 476 4.1 1.3 ND (<1.2) 2.6 (1) BioReactor 2 Eff 2.4 ND (<0.74) ND (<1.2) ND (<1.2) ND (<1.2) 0 (0) Metals Trip Blk ND (<0.30) ND (<0.15) ND (<0.24) ND (<0.23) ND (<0.23) 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 Bi-Monthly Sampling)

Contact: Jay Perkins

Date: June 16, 2011 LIMS #J11060066

### 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 0.030 0.30 1.5 6.0 Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.015 0.15 0.74 3.0 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.024 0.24 1.2 4.9 MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.023 0.23 1.2 4.6 SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.023 0.23 1.2 4.6 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 9.43 98.6 Se(VI) LCS 9.48 9.16 96.7 SeCN LCS 8.92 8.77 98.3 MeSe(IV) LCS 6.47 6.36 98.4 SeMe LCS 9.32 9.12 97.9 LIMS #J11060066 Date: June 16, 2011 Report Generated by: Ben Wozniak Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD (WWTS Bi-Monthly 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 2.4 2.5 2.4 3.0 Se(VI) BioReactor 2 Eff ND (<0.74) ND (<0.74) NC NC SeCN BioReactor 2 Eff ND (<1.2) ND (<1.2) NC NC MeSe(IV) BioReactor 2 Eff ND (<1.2) ND (<1.2) NC NC SeMe BioReactor 2 Eff ND (<1.2) ND (<1.2) 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 278.0 261.9 93.3 278.0 268.6 95.8 2.5 Se(VI) BioReactor 2 Eff 252.3 253.8 100.6 252.3 253.7 100.6 0.0 SeCN BioReactor 2 Eff 228.8 224.2 98.0 228.8 224.6 98.2 0.2 Date: June 16, 2011 Report Generated by: Ben Wozniak Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD (WWTS Bi-Monthly Sampling)

Contact: Jay Perkins LIMS #J11060066