### 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: J11070122 Project Name: WWTS - Biweekly

Lab Contact: Jason C Perkins 

### Date: 7/29/2011 Customer Address: 3195 Pine Hall Rd Customer Name(s): FGD WWTS

Mailcode: Belews Steam Station Belews Creek, NC 28012

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


### Program Comments: FGD Bi Monthly There was detectable Se in the filter blank sample. Sample result s were all greater than 10 times the filter blank value. Dat a OK to report. 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 ar e 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 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 Labora tory Results, Customer Specific Data Sheets, Reports & Documentation, Customer Database Entries, Te st Case Narratives, C hain of Custody (COC)
Certification: The Analytical Laboratory holds the followi ng State Certifications : North Carolina (DENR) Certificate #248, South Carolina (DHEC) Laboratory ID # 99005. Contact the Analytical Laborat ory for definitive information abou t the certification status of specific methods.

## Sample ID's & Descriptions:
Sample ID Plant/Station Collection Date and Time Collected By Sample Description 2011015065 BELEWS 13-Jul-11 8:00 AM T. Johnson FGD Purge Eff 2011015066 BELEWS 13-Jul-11 8:00 AM T. Johnson EQ TANK EFF. 2011015067 BELEWS 13-Jul-11 8:00 AM T. Johnson BIOREACTOR 1 INF. 2011015068 BELEWS 13-Jul-11 8:00 AM T. Johnson BIOREACTOR 2 INF. 2011015069 BELEWS 13-Jul-11 8:00 AM T. Johnson BIOREACTOR 2 EFF. 2011015070 BELEWS 13-Jul-11 8:00 AM T. Johnson Trip Blank 2011015071 BELEWS 13-Jul-11 8:00 AM T. Johnson FILTER BLANK 2011015072 BELEWS 13-Jul-11 1:00 PM DAVID MORRIS BIOREACTOR 1 INF. 2011015073 BELEWS 13-Jul-11 1:00 PM DAVID MORRIS HG BLANK BIOREACTOR 1 INF. 2011015074 BELEWS 13-Jul-11 1:10 PM DAVID MORRIS BIOREACTOR 2 INF. 2011015075 BELEWS 13-Jul-11 1:10 PM DAVID MORRIS Hg Blk BioReactor 2 Inf 2011015076 BELEWS 13-Jul-11 1:05 PM DAVID MORRIS BIOREACTOR 2 EFF. 2011015077 BELEWS 13-Jul-11 1:05 PM DAVID MORRIS 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: 

### 7/29/2011 N/A

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 # J11070122

2011015065 Collection Date: 13-Jul-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) 175 ug/L EPA 245.1 22-Jul-11 11:22 AGIBBS 5 TOTAL RECOVERABLE METALS BY ICP Boron (B) 138 mg/L EPA 200.7 27-Jul-11 12:48 DJSULL1 0.5 DISSOLVED METALS BY ICP-MS Selenium (Se) 3330 ug/L EPA 200.8 26-Jul-11 11:22 KRICHAR 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 236 ug/L EPA 200.8 19-Jul-11 12:32 KRICHAR 10 Chromium (Cr) 287 ug/L EPA 200.8 19-Jul-11 12:32 KRICHAR 10 Copper (Cu) 237 ug/L EPA 200.8 19-Jul-11 12:32 KRICHAR 10 Nickel (Ni) 358 ug/L EPA 200.8 19-Jul-11 12:32 KRICHAR 10 Selenium (Se) 4870 ug/L EPA 200.8 19-Jul-11 12:32 KRICHAR 10 Silver (Ag) < 10 ug/L EPA 200.8 19-Jul-11 12:32 KRICHAR 10 Zinc (Zn) 524 ug/L EPA 200.8 19-Jul-11 12:32 KRICHAR 20 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C TOTAL DISSOLVED SOLIDS TDS 19000 mg/L SM2540C 20-Jul-11 14:45 CLEEMAN 10 

### 2011015066 Collection Date: 13-Jul-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) 166 ug/L EPA 245.1 22-Jul-11 11:24 AGIBBS 2.5 TOTAL RECOVERABLE METALS BY ICP Boron (B) 147 mg/L EPA 200.7 27-Jul-11 12:52 DJSULL1 0.5 DISSOLVED METALS BY ICP-MS Selenium (Se) 2890 ug/L EPA 200.8 26-Jul-11 11:06 KRICHAR 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 223 ug/L EPA 200.8 19-Jul-11 12:27 KRICHAR 10 Chromium (Cr) 277 ug/L EPA 200.8 19-Jul-11 12:27 KRICHAR 10 Copper (Cu) 228 ug/L EPA 200.8 19-Jul-11 12:27 KRICHAR 10 Nickel (Ni) 294 ug/L EPA 200.8 19-Jul-11 12:27 KRICHAR 10

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

### Order # J11070122

2011015066 Collection Date: 13-Jul-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) 4940 ug/L EPA 200.8 19-Jul-11 12:27 KRICHAR 10 Silver (Ag) < 10 ug/L EPA 200.8 19-Jul-11 12:27 KRICHAR 10 Zinc (Zn) 448 ug/L EPA 200.8 19-Jul-11 12:27 KRICHAR 20 

### 2011015067 Collection Date: 13-Jul-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) 147 mg/L EPA 200.7 27-Jul-11 12:26 DJSULL1 0.5 DISSOLVED METALS BY ICP-MS Selenium (Se) 136 ug/L EPA 200.8 26-Jul-11 10:44 KRICHAR 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 19-Jul-11 12:22 KRICHAR 10 Chromium (Cr) < 10 ug/L EPA 200.8 19-Jul-11 12:22 KRICHAR 10 Copper (Cu) < 10 ug/L EPA 200.8 19-Jul-11 12:22 KRICHAR 10 Nickel (Ni) 12.9 ug/L EPA 200.8 19-Jul-11 12:22 KRICHAR 10 Selenium (Se) 152 ug/L EPA 200.8 19-Jul-11 12:22 KRICHAR 10 Silver (Ag) < 10 ug/L EPA 200.8 19-Jul-11 12:22 KRICHAR 10 Zinc (Zn) < 20 ug/L EPA 200.8 19-Jul-11 12:22 KRICHAR 20 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011015068 Collection Date: 13-Jul-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) 147 mg/L EPA 200.7 27-Jul-11 12:31 DJSULL1 0.5 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 19-Jul-11 12:17 KRICHAR 10 Chromium (Cr) < 10 ug/L EPA 200.8 19-Jul-11 12:17 KRICHAR 10 Copper (Cu) < 10 ug/L EPA 200.8 19-Jul-11 12:17 KRICHAR 10 Nickel (Ni) < 10 ug/L EPA 200.8 19-Jul-11 12:17 KRICHAR 10 Selenium (Se) 23.9 ug/L EPA 200.8 19-Jul-11 12:17 KRICHAR 10 Silver (Ag) < 10 ug/L EPA 200.8 19-Jul-11 12:17 KRICHAR 10 Zinc (Zn) < 20 ug/L EPA 200.8 19-Jul-11 12:17 KRICHAR 20

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

### Order # J11070122

2011015069 Collection Date: 13-Jul-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 22-Jul-11 11:27 AGIBBS 1 TOTAL RECOVERABLE METALS BY ICP Boron (B) 156 mg/L EPA 200.7 27-Jul-11 12:35 DJSULL1 0.5 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 5 ug/L EPA 200.8 19-Jul-11 12:12 KRICHAR 5 Chromium (Cr) < 5 ug/L EPA 200.8 19-Jul-11 12:12 KRICHAR 5 Copper (Cu) < 5 ug/L EPA 200.8 19-Jul-11 12:12 KRICHAR 5 Nickel (Ni) < 5 ug/L EPA 200.8 19-Jul-11 12:12 KRICHAR 5 Selenium (Se) 6.15 ug/L EPA 200.8 19-Jul-11 12:12 KRICHAR 5 Silver (Ag) < 5 ug/L EPA 200.8 19-Jul-11 12:12 KRICHAR 5 Zinc (Zn) < 10 ug/L EPA 200.8 19-Jul-11 12:12 KRICHAR 10 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011015070 Collection Date: 13-Jul-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 27-Jul-11 12:22 DJSULL1 0.05 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 1 ug/L EPA 200.8 19-Jul-11 12:08 KRICHAR 1 Chromium (Cr) < 1 ug/L EPA 200.8 19-Jul-11 12:08 KRICHAR 1 Copper (Cu) < 1 ug/L EPA 200.8 19-Jul-11 12:08 KRICHAR 1 Nickel (Ni) < 1 ug/L EPA 200.8 19-Jul-11 12:08 KRICHAR 1 Selenium (Se) < 1 ug/L EPA 200.8 19-Jul-11 12:08 KRICHAR 1 Silver (Ag) < 1 ug/L EPA 200.8 19-Jul-11 12:08 KRICHAR 1 Zinc (Zn) < 2 ug/L EPA 200.8 19-Jul-11 12:08 KRICHAR 2 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011015071 Collection Date: 13-Jul-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

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

### Order # J11070122

2011015071 Collection Date: 13-Jul-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) 2.38 ug/L EPA 200.8 26-Jul-11 10:34 KRICHAR 2 

### 2011015072 Collection Date: 13-Jul-11 1:00 PM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND MERCURY 1631 - DISSOLVED Vendor Parameter Complete V_BRAND 

### 2011015073 Collection Date: 13-Jul-11 1:00 PM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND MERCURY 1631 - DISSOLVED Vendor Parameter Complete V_BRAND 

### 2011015074 Collection Date: 13-Jul-11 1:10 PM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND MERCURY 1631 - DISSOLVED Vendor Parameter Complete V_BRAND 

### 2011015075 Collection Date: 13-Jul-11 1:10 PM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND MERCURY 1631 - DISSOLVED

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

### Order # J11070122

2011015075 Collection Date: 13-Jul-11 1:10 PM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst MERCURY 1631 - DISSOLVED Vendor Parameter Complete V_BRAND 

### 2011015076 Collection Date: 13-Jul-11 1:05 PM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND MERCURY 1631 - DISSOLVED Vendor Parameter Complete V_BRAND 

### 2011015077 Collection Date: 13-Jul-11 1:05 PM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND MERCURY 1631 - DISSOLVED Vendor Parameter Complete V_BRAND

## Ju ly 20 , 201 1

Jay Perkins Duke Energy Analytical Laboratory Mail Code MGO3A2 (Building 7405) 13339 Hagers Ferry Rd. Huntersville, NC 28078 (704) 875-5245 P roject: Belews

– FGD (WWTS Bi -Monthly Sampling) (LIMS # J11070122)

De ar Mr. Perkins, Attac hed is the report associated with four (4 ) a queous samples submitted for selenium speciation analysis on Ju ly14, 2011. The samples were received in a sealed cooler at-0. 4 o 

## C on Ju ly 15, 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 # J11070122)

Ju ly 20 , 201 1

1. Sample Reception Four (4 ) a queous samples in 125mL HDPE bottles (provided by Applied Speciation and Consulting) were su bmitted for selenium speciation analysi s on Ju ly 1 4 , 2011 . The samples were received on Ju ly 1 5, 2011 in a sealed co ntainer at -0.4 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 sa mple 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 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 All samples for selenium speciation analysis were analyzed by ion chromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICP-DRC-MS) on Ju ly15, 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 significant analytical issues were encountered. All quality control parameters associated with these samples were within acceptance limits. T he 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 211 103 ND (<3.4) ND (<2.4) ND (<2.4) 0 (0) BioReactor 1 Inf 25.5 87.8 ND (<0.85) 1.06 ND (<0.59) 0 (0) BioReactor 2 Eff ND (<0.28) ND (<0.64) ND (<0.85) ND (<0.59) ND (<0.59) 0 (0) Metals Trip Blk ND (<0.055) ND (<0.13) ND (<0.17) ND (<0.12) ND (<0.12) 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: July 20, 2011 LIMS #J11070122

### 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 0.006 0.055 0.28 1.1 Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.013 0.13 0.64 2.6 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.017 0.17 0.85 3.4 MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.012 0.12 0.59 2.4 SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.012 0.12 0.59 2.4 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 10.16 106.2 Se(VI) LCS 9.48 9.786 103.2 SeCN LCS 8.92 8.875 99.5 MeSe(IV) LCS 6.47 6.446 99.6 SeMe LCS 9.32 9.379 100.6 LIMS #J11070122 Date: July 20, 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 ND (<0.28) ND (<0.28) NC NC Se(VI) BioReactor 2 Eff ND (<0.64) ND (<0.64) NC NC SeCN BioReactor 2 Eff ND (<0.85) ND (<0.85) NC NC MeSe(IV) BioReactor 2 Eff ND (<0.59) ND (<0.59) NC NC SeMe BioReactor 2 Eff ND (<0.59) ND (<0.59) 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 278.0 270.2 97.2 278.0 268.7 96.7 0.5 Se(VI) BioReactor 2 Eff 252.3 239.7 95.0 252.3 239.3 94.9 0.2 SeCN BioReactor 2 Eff 228.8 205.6 89.9 228.8 205.2 89.7 0.2 Date: July 20, 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 #J110701223958 6 th Ave NW • Seattle, WA 98107 • T: 206-632-6206 • F: 206-632-6017 • www.brooksrand.com • brl@brooksrand.com 

### July 21, 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: J11070122 Dear Mr. Perkins, On July 15, 2011, Brooks Rand Labs (BRL) received three (3) flue gas desulfurization (FGD) waste water samples and three (3) corresponding field blanks. Samples were logged-in 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 Lydia Greaves Project Manager Jr. Project Manager tiffany@brooksrand.com lydia@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 1129042-01 BioReactor 1 Inf 07/13/2011 07/15/2011 Sample FGD Wastewater 1129042-02 Hg Blk BioReactor 1 Inf 07/13/2011 07/15/2011 Field Blank DIW 1129042-03 BioReactor 2 Inf 07/13/2011 07/15/2011 QC Sample FGD Wastewater 1129042-04 Hg Blk BioReactor 2 Inf 07/13/2011 07/15/2011 Field Blank DIW 1129042-05 BioReactor 2 Eff 07/13/2011 07/15/2011 Sample FGD Wastewater 1129042-06 Hg Blk BioReactor 2 Eff 07/13/2011 07/15/2011 Field Blank DIW 

# Batch Summary

Analyte Prepared Analyzed Sequence Batch Lab Matrix Method B111039 07/18/2011 07/20/2011 1100496 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 82.7 T 1100496 B111039 FGD Wastewater 8.08 3.03 1129042-01 Hg

BioReactor 2 Eff ng/L 24.5 T 1100496 B111039 FGD Wastewater 2.05 0.77 1129042-05 Hg

BioReactor 2 Inf ng/L 65.4 T 1100496 B111039 FGD Wastewater 8.08 3.03 1129042-03 Hg
Hg Blk BioReactor 1 Inf ng/L 0.15 T U 1100496 B111039 DIW 0.40 0.15 1129042-02 Hg
Hg Blk BioReactor 2 Eff ng/L 0.15 T U 1100496 B111039 DIW 0.40 0.15 1129042-06 Hg
Hg Blk BioReactor 2 Inf ng/L 0.15 T U 1100496 B111039 DIW 0.40 0.15 1129042-04 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: B111039
Method: EPA 1631 Lab Matrix: Water

Sample Certified Reference Material (1128019, NIST 1641d 1000x dilution) B111039-SRM1 15.68 98% ng/L 85-115 Hg 15.39 Matrix Spike (1129042-03) B111039-MS3 323.2 113% ng/L 71-125 Hg 429.8

65.36 Matrix Spike Duplicate (1129042-03) B111039-MSD3 323.2 107% ng/L 71-125 244% Hg 411.2

65.36



# Method Blanks & Reporting Limits

Batch: B111039
Method: EPA 1631 Matrix: Water Analyte: Hg Result Units Sample B111039-BLK1 ng/L 0.08 B111039-BLK2 ng/L 0.10 B111039-BLK3 ng/L 0.07 B111039-BLK4 ng/L 0.05 MDL: 0.15 Average: 0.08 Standard Deviation: 0.02 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: 1100496 Instrument: THG-05 Date: 07/20/2011 Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg REC & Limits Result True Value Lab ID Units 1100496-IBL1 pg of Hg 9.55 1100496-IBL2 pg of Hg 9.37 1100496-IBL3 pg of Hg 8.12 1100496-IBL4 pg of Hg 9.29 1100496-CAL1 25.00 91% pg of Hg 22.79 1100496-CAL2 100.0 100% pg of Hg 100.3 1100496-CAL3 500.0 102% pg of Hg 511.3 1100496-CAL4 2500 106% pg of Hg 2648 1100496-CAL5 10000 102% pg of Hg 10170 1100496-ICV1 1568 98% pg of Hg 85-115 1539 1100496-CCB1 pg of Hg 14.7 1100496-CCV1 500.0 102% pg of Hg 77-123 509.8 1100496-CCV2 500.0 101% pg of Hg 77-123 507.1

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: 1129042-01 Report Matrix: FGD Wastewater Sample Type: Sample Received: 07/15/2011 Sample: BioReactor 1 Inf Collected: 07/13/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A No Lot # Cooler None N/A 125 mL Bottle FLPE Hg-T

Lab ID: 1129042-02 Report Matrix: DIW Sample Type: Field Blank Received: 07/15/2011 Sample: Hg Blk BioReactor 1 Inf Collected: 07/13/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A No Lot # Cooler None N/A 125 mL Bottle FLPE Hg-T

Lab ID: 1129042-03 Report Matrix: FGD Wastewater Sample Type: QC Sample Received: 07/15/2011 Sample: BioReactor 2 Inf Collected: 07/13/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71313080 60 Cooler

None N/A 250 mL Bottle FLPE Hg-T
Comments: About 100 mL Sample Volume

Lab ID: 1129042-04 Report Matrix: DIW Sample Type: Field Blank Received: 07/15/2011 Sample: Hg Blk BioReactor 2 Inf Collected: 07/13/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A No Lot # Cooler None N/A 125 mL Bottle FLPE Hg-T

Lab ID: 1129042-05 Report Matrix: FGD Wastewater Sample Type: Sample Received: 07/15/2011 Sample: BioReactor 2 Eff Collected: 07/13/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A No Lot # Cooler None N/A 125 mL Bottle FLPE Hg-T

Lab ID: 1129042-06 Report Matrix: DIW Sample Type: Field Blank Received: 07/15/2011 Sample: Hg Blk BioReactor 2 Eff Collected: 07/13/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A No Lot # Cooler None N/A 125 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-HV1101

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



# Shipping Containers

Cooler Tracking No: 4726 7966 2152 via FedEx Temperature: 1.4 °C Coolant Type: Ice Description: Cooler Damaged in transit? No Returned to client? No Custody seals present? No Custody seals intact? No COC present? Yes Received: July 15, 2011 8:45

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