### 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: J11090009

Lab Contact: Jason C Perkins 

### Date: 9/28/2011 Customer Address: 253 Plant Allen Road Customer Name(s): Don Scruggs, Ro bbin Jolly, Ray Lidke, Bill Kennedy

Belmont, 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 Cert ificate of Analysis (sample re sults) under the qualifiers heading. All results are repo rted 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 t he 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, A nalytical Laboratory Certificate of Analysis, Analytical Laboratory QC Reports, Sub-contracted Laboratory Results, Customer Specific Data Sheets, Reports & Documentation, Customer Database Entries, Te st Case Narratives, Chain of Custody (COC) Certification: The Analytical Laboratory holds the follow ing State Certifications : North Carolina (DENR) Certificate #248, South Carolina (DHEC) Laboratory ID # 99005. Contact the Analytical Laborator y 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 2011019079 ALLEN 12-Sep-11 10:0 7 AM Chris Williams FGD Purge Eff 2011019081 ALLEN 12-Sep-11 10:2 1 AM Chris Williams EQ Tank Eff 2011019082 ALLEN 12-Sep-11 10:28 AM Chris Williams BioReactor 1 Inf 2011019083 ALLEN 12-Sep-11 10:31 AM Chris Williams BioReactor 2 Inf 2011019084 ALLEN 12-Sep-11 10:25 AM Chris Williams BioReactor 2 Eff 2011019085 ALLEN 12-Sep-11 10:4 1 AM Chris Williams Filter Blk 2011019086 ALLEN 12-Sep-11 10:30 AM Chris Williams Metals Trip Blank 2011019087 ALLEN 12-Sep-11 10:45 AM David Morris (Prism) BioReactor 1 Inf 2011019088 ALLEN 12-Sep-11 10:45 AM David Morris (Prism) Hg Blk BioReactor 1 Inf 2011019089 ALLEN 12-Sep-11 10:55 AM David Morris (Prism) BioReactor 2 Inf 2011019090 ALLEN 12-Sep-11 10:55 AM David Morris (Prism) Hg Blk BioReactor 2 Inf 2011019091 ALLEN 12-Sep-11 10:50 AM David Morris (Prism) BioReactor 2 Eff 2011019092 ALLEN 12-Sep-11 10:50 AM 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: 

### Mary Ann Ogle Date: 

### 9/28/2011 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 # J11090009

2011019079 Collection Date: 12-Sep-11 10:07 AM 

### Site: FGD Purge Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst INORGANIC IONS BY IC Bromide 27 mg/L EPA 300.0 22-Sep-11 19:39 CLEEMAN 5 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 29.2 ug/L EPA 245.1 16-Sep-11 08:58 AGIBBS 2.5 TOTAL RECOVERABLE METALS BY ICP Boron (B) 24.0 mg/L EPA 200.7 16-Sep-11 10:04 DJSULL1 0.5 DISSOLVED METALS BY ICP-MS Selenium (Se) 69.9 ug/L EPA 200.8 15-Sep-11 13:29 KRICHAR 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 215 ug/L EPA 200.8 19-Sep-11 10:00 DJSULL1 10 Chromium (Cr) 134 ug/L EPA 200.8 19-Sep-11 10:00 DJSULL1 10 Copper (Cu) 162 ug/L EPA 200.8 19-Sep-11 10:00 DJSULL1 10 Nickel (Ni) 235 ug/L EPA 200.8 19-Sep-11 10:00 DJSULL1 10 Selenium (Se) 909 ug/L EPA 200.8 19-Sep-11 10:00 DJSULL1 10 Silver (Ag) < 10 ug/L EPA 200.8 19-Sep-11 10:00 DJSULL1 10 Zinc (Zn) 192 ug/L EPA 200.8 19-Sep-11 10:00 DJSULL1 20 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C
TOTAL DISSOLVED SOLIDS TDS 8300 mg/L SM2540C 13-Sep-11 15:00 TJA7067 200 

### 2011019081 Collection Date: 12-Sep-11 10:21 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) 41.8 ug/L EPA 245.1 16-Sep-11 09:00 AGIBBS 2.5 TOTAL RECOVERABLE METALS BY ICP Boron (B) 25.6 mg/L EPA 200.7 16-Sep-11 10:08 DJSULL1 0.5 DISSOLVED METALS BY ICP-MS Selenium (Se) 40.2 ug/L EPA 200.8 15-Sep-11 13:32 KRICHAR 10

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

### Order # J11090009

2011019081 Collection Date: 12-Sep-11 10:21 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 Arsenic (As) 140 ug/L EPA 200.8 19-Sep-11 10:03 DJSULL1 10 Chromium (Cr) 96.5 ug/L EPA 200.8 19-Sep-11 10:03 DJSULL1 10 Copper (Cu) 126 ug/L EPA 200.8 19-Sep-11 10:03 DJSULL1 10 Nickel (Ni) 158 ug/L EPA 200.8 19-Sep-11 10:03 DJSULL1 10 Selenium (Se) 583 ug/L EPA 200.8 19-Sep-11 10:03 DJSULL1 10 Silver (Ag) < 10 ug/L EPA 200.8 19-Sep-11 10:03 DJSULL1 10 Zinc (Zn) 152 ug/L EPA 200.8 19-Sep-11 10:03 DJSULL1 20 

### 2011019082 Collection Date: 12-Sep-11 10:28 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) 31.1 mg/L EPA 200.7 16-Sep-11 10:12 DJSULL1 0.5 DISSOLVED METALS BY ICP-MS Selenium (Se) 53.9 ug/L EPA 200.8 15-Sep-11 13:35 KRICHAR 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 19-Sep-11 10:06 DJSULL1 10 Chromium (Cr) < 10 ug/L EPA 200.8 19-Sep-11 10:06 DJSULL1 10 Copper (Cu) 17.2 ug/L EPA 200.8 19-Sep-11 10:06 DJSULL1 10 Nickel (Ni) 10.3 ug/L EPA 200.8 19-Sep-11 10:06 DJSULL1 10 Selenium (Se) 55.1 ug/L EPA 200.8 19-Sep-11 10:06 DJSULL1 10 Silver (Ag) < 10 ug/L EPA 200.8 19-Sep-11 10:06 DJSULL1 10 Zinc (Zn) < 20 ug/L EPA 200.8 19-Sep-11 10:06 DJSULL1 20 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011019083 Collection Date: 12-Sep-11 10:31 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) 34.5 mg/L EPA 200.7 16-Sep-11 10:16 DJSULL1 0.5

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

### Order # J11090009

2011019083 Collection Date: 12-Sep-11 10:31 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-MS Arsenic (As) < 10 ug/L EPA 200.8 19-Sep-11 10:09 DJSULL1 10 Chromium (Cr) < 10 ug/L EPA 200.8 19-Sep-11 10:09 DJSULL1 10 Copper (Cu) < 10 ug/L EPA 200.8 19-Sep-11 10:09 DJSULL1 10 Nickel (Ni) < 10 ug/L EPA 200.8 19-Sep-11 10:09 DJSULL1 10 Selenium (Se) < 10 ug/L EPA 200.8 19-Sep-11 10:09 DJSULL1 10 Silver (Ag) < 10 ug/L EPA 200.8 19-Sep-11 10:09 DJSULL1 10 Zinc (Zn) < 20 ug/L EPA 200.8 19-Sep-11 10:09 DJSULL1 20 

### 2011019084 Collection Date: 12-Sep-11 10:25 AM 

### Site: BioReactor 2 Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst INORGANIC IONS BY IC Bromide 41 mg/L EPA 300.0 22-Sep-11 19:55 CLEEMAN 5 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) < 1 ug/L EPA 245.1 16-Sep-11 09:03 AGIBBS 1 TOTAL RECOVERABLE METALS BY ICP Boron (B) 35.8 mg/L EPA 200.7 16-Sep-11 10:20 DJSULL1 0.5 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 19-Sep-11 10:12 DJSULL1 10 Chromium (Cr) < 10 ug/L EPA 200.8 19-Sep-11 10:12 DJSULL1 10 Copper (Cu) < 10 ug/L EPA 200.8 19-Sep-11 10:12 DJSULL1 10 Nickel (Ni) < 10 ug/L EPA 200.8 19-Sep-11 10:12 DJSULL1 10 Selenium (Se) < 10 ug/L EPA 200.8 19-Sep-11 10:12 DJSULL1 10 Silver (Ag) < 10 ug/L EPA 200.8 19-Sep-11 10:12 DJSULL1 10 Zinc (Zn) < 20 ug/L EPA 200.8 19-Sep-11 10:12 DJSULL1 20 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011019085 Collection Date: 12-Sep-11 10:41 AM 

### Site: Filter Blk Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DISSOLVED METALS BY ICP-MS Selenium (Se) < 1 ug/L EPA 200.8 15-Sep-11 13:16 KRICHAR 1

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

### Order # J11090009

2011019086 Collection Date: 12-Sep-11 10:30 AM 

### Site: Metals 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 16-Sep-11 10:53 DJSULL1 0.05 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 1 ug/L EPA 200.8 19-Sep-11 09:51 DJSULL1 1 Chromium (Cr) < 1 ug/L EPA 200.8 19-Sep-11 09:51 DJSULL1 1 Copper (Cu) < 1 ug/L EPA 200.8 19-Sep-11 09:51 DJSULL1 1 Nickel (Ni) < 1 ug/L EPA 200.8 19-Sep-11 09:51 DJSULL1 1 Selenium (Se) < 1 ug/L EPA 200.8 19-Sep-11 09:51 DJSULL1 1 Silver (Ag) < 1 ug/L EPA 200.8 19-Sep-11 09:51 DJSULL1 1 Zinc (Zn) < 2 ug/L EPA 200.8 19-Sep-11 09:51 DJSULL1 2 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011019087 Collection Date: 12-Sep-11 10:45 AM 

### 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 

### 2011019088 Collection Date: 12-Sep-11 10:45 AM 

### Site: Hg Blk 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 

### 2011019089 Collection Date: 12-Sep-11 10:55 AM 

### 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

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

### Order # J11090009

2011019090 Collection Date: 12-Sep-11 10:55 AM 

### 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 

### 2011019091 Collection Date: 12-Sep-11 10:50 AM 

### 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 

### 2011019092 Collection Date: 12-Sep-11 10:50 AM 

### 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

## September 2 1 , 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: Allen

– FGD WWTS (2010, Bi-Monthly Sampling) (LIMS # J11090 009 )

Dear Mr. Perkins, Attached is the report associated with four (4 ) aqueous samples submitted for selenium speciation analysis on September 1 3 , 2011. The samples were received in a sealed cooler at - 0.3 o 

## C on September 14 , 2011. Selenium speciation analysis was performed via ionchromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICPDRC-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: Allen

– FGD WWTS (2010, Bi-Monthly Sampling) (LIMS # J11090 009)
September 2 1 , 2011

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 September 1 3 , 2011 . The samples were received on September 1 4 , 2011 in a sealed container at -0.3 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 sp eciation 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 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. Al l 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 September 1 6 , 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 well and no significant analytical issues were encountered. All quality control parameters associated with this sample were within acceptance limits with the following exception: The recoveries associated with the matrix spike (MS) and matrix spike duplicate (MSD) performed on the sample identified as Batch QC were below the established control limit of 75% for selenocyanate (57.1% and 55.5%, respectively). The MS and MSD also included selenite in the spiking solution which yielded elevated recoveries (122.5% and 123.8%, respectively)

. The low recoveries for selenocyanate correlate with the elevated recoveries of selenite suggesting that the sample matrix induces species conversion. The fact that no species conversion was observed in the ICV or CCVs, which contain both selenite and selenocyanate, demonstrates that the applied method stabilizes these selenium species in solution. Since the conversion of selenocyanate to selenite in the MS and MSD is a function of the sample matrix and the recoveries confirm a mass balance, no corrective action was required. The reported results are deemed representative of the supplied samples and suggest that selenocyanate is not stable in the spiked sample matrix.

## 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 29.0 24.2 ND (<1.4) ND (<4.4) ND (<4.4) 0 (0) BioReactor 1 Inf 7.8 35.6 ND (<0.34) 2.1 ND (<1.1) 0 (0) BioReactor 2 Eff 2.5 ND (<1.7) ND (<0.34) ND (<1.1) ND (<1.1) 0 (0) Metals Trip Blk ND (<0.25) ND (<0.34) ND (<0.068) ND (<0.22) ND (<0.22) 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: Allen – FGD WWTS (2010, Bi-Monthly Sampling)

Contact: Jay Perkins
Date: September 21, 2011 LIMS #J11090009

### 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 0.025 0.25 1.2 4.9 Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.034 0.34 1.7 6.8 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.007 0.068 0.34 1.4 MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.022 0.22 1.1 4.4 SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.022 0.22 1.1 4.4 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 9.635 100.7 Se(VI) LCS 9.48 9.371 98.9 SeCN LCS 8.92 8.723 97.8 MeSe(IV) LCS 6.47 6.037 93.3 SeMe LCS 9.32 9.138 98.0 LIMS #J11090009 Date: September 21, 2011 Report Generated by: Ben Wozniak Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Allen – FGD WWTS (2010, Bi-Monthly Sampling)

Contact: Jay Perkins

### Quality Control Summary - Matrix Duplicates Analyte (μg/L) Sample ID Rep 1 Rep 2 Mean RPD Se(IV) Batch QC** 11.5 13.4 12.5 15.0 Se(VI) Batch QC** 103.2 105.0 104.1 1.7 SeCN Batch QC** ND (<1.4) ND (<1.4) NC NC MeSe(IV) Batch QC** ND (<4.4) ND (<4.4) NC NC SeMe Batch QC** ND (<4.4) ND (<4.4) NC NC ND = Not detected at the applied dilution NC = Value was not calculated due to one or more concentrations below the eMDL ** Batch QC performed on sample from LIMS #J11090139
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** 1112 1375 122.5 1112 1389 123.8 1.0 Se(VI) Batch QC** 1009 1124 101.1 1009 1124 101.0 0.0 SeCN Batch QC** 915.0 522.4 57.1* 915.0 508.2 55.5* 2.8 * The recovery is below the established control limit of 75%; please see narrative Contact: Jay Perkins LIMS #J11090009 Date: September 21, 2011 Report Generated by: Ben Wozniak Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Allen – FGD WWTS (2010, Bi-Monthly Sampling)3958 6 th Ave NW • Seattle, WA 98107 • T: 206-632-6206 • F: 206-632-6017 • www.brooksrand.com • brl@brooksrand.com 

### September 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: J11090009 Dear Mr. Perkins, On September 14, 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. 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. All other quality assurance criteria were satisfied and, aside from concentration qualifiers, all data was reported without additional qualification. Sample Hg Blk BioReactor 2 Inf (1138020-04) was identified as a field blank that had a Hg concentration of 1.53 ng/L. This was confirmed by reanalysis (1.50 ng/L). The sample associated with the blank recovered at greater than 40x the high blank and no further action was required. 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,

Lydia Greaves Project Manager lydia@brooksran.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 1138020-01 BioReactor 1 Inf 09/12/2011 09/14/2011 Sample FGD Wastewater 1138020-02 Hg Blk BioReactor 1 Inf 09/12/2011 09/14/2011 Field Blank DIW 1138020-03 BioReactor 2 Inf 09/12/2011 09/14/2011 QC Sample FGD Wastewater 1138020-04 Hg Blk BioReactor 2 Inf 09/12/2011 09/14/2011 Field Blank DIW 1138020-05 BioReactor 2 Eff 09/12/2011 09/14/2011 Sample FGD Wastewater 1138020-06 Hg Blk BioReactor 2 Eff 09/12/2011 09/14/2011 Field Blank DIW 

# Batch Summary

Analyte Prepared Analyzed Sequence Batch Lab Matrix Method B111446 09/16/2011 09/19/2011 1100641 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 321 T 1100641 B111446 FGD Wastewater 4.04 1.52 1138020-01 Hg

BioReactor 2 Eff ng/L 18.8 T 1100641 B111446 FGD Wastewater 1.59 0.59 1138020-05 Hg

BioReactor 2 Inf ng/L 64.2 T 1100641 B111446 FGD Wastewater 4.04 1.52 1138020-03 Hg
Hg Blk BioReactor 1 Inf ng/L 0.15 T U 1100641 B111446 DIW 0.41 0.15 1138020-02 Hg
Hg Blk BioReactor 2 Eff ng/L 0.15 T U 1100641 B111446 DIW 0.41 0.15 1138020-06 Hg
Hg Blk BioReactor 2 Inf ng/L 1.53 T 1100641 B111446 DIW 0.40 0.15 1138020-04 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: B111446
Method: EPA 1631 Lab Matrix: Water

Sample Certified Reference Material (1137004, NIST 1641d 1000x dilution) B111446-SRM1 15.68 96% ng/L 85-115 Hg 15.09 Matrix Spike (1138020-03) B111446-MS1 303.0 111% ng/L 71-125 Hg 399.7

64.17 Matrix Spike Duplicate (1138020-03) B111446-MSD1 303.0 99% ng/L 71-125 2410% Hg 363.2

64.17



# Method Blanks & Reporting Limits

Batch: B111446
Method: EPA 1631 Matrix: Water Analyte: Hg Result Units Sample B111446-BLK1 ng/L 0.05 B111446-BLK2 ng/L 0.06 B111446-BLK3 ng/L 0.08 B111446-BLK4 ng/L 0.05 MDL: 0.15 Average: 0.06 Standard Deviation: 0.01 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

Sequence: 1100641 Method: EPA 1631 Instrument: THG-05 Date: 09/19/2011 Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg REC & Limits Result True Value Lab ID Units 1100641-IBL1 pg of Hg 3.38 1100641-IBL2 pg of Hg 8.55 1100641-IBL3 pg of Hg 11.71 1100641-IBL4 pg of Hg 8.40 1100641-CAL1 25.00 103% pg of Hg 25.78 1100641-CAL2 100.0 102% pg of Hg 102.1 1100641-CAL3 500.0 99% pg of Hg 495.2 1100641-CAL4 2500 102% pg of Hg 2560 1100641-CAL5 10000 94% pg of Hg 9390 1100641-ICV1 1568 96% pg of Hg 85-115 1509 1100641-CCB1 pg of Hg 8.05 1100641-CCV1 500.0 85% pg of Hg 77-123 422.8 1100641-CCV2 500.0 92% pg of Hg 77-123 457.9 1100641-CCV3 500.0 97% pg of Hg 77-123 485.3

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: 1138020-01 Report Matrix: FGD Wastewater Sample Type: Sample Received: 09/14/2011 Sample: BioReactor 1 Inf Collected: 09/12/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71313080 60 Cooler

None N/A 250 mL Bottle FLPE Hg-T

Lab ID: 1138020-02 Report Matrix: DIW Sample Type: Field Blank Received: 09/14/2011 Sample: Hg Blk BioReactor 1 Inf Collected: 09/12/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71313080 60 Cooler

None N/A 250 mL Bottle FLPE Hg-T

Lab ID: 1138020-03 Report Matrix: FGD Wastewater Sample Type: QC Sample Received: 09/14/2011 Sample: BioReactor 2 Inf Collected: 09/12/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71313080 60 Cooler

None N/A 250 mL Bottle FLPE Hg-T

Lab ID: 1138020-04 Report Matrix: DIW Sample Type: Field Blank Received: 09/14/2011 Sample: Hg Blk BioReactor 2 Inf Collected: 09/12/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71313080 60 Cooler

None N/A 250 mL Bottle FLPE Hg-T

Lab ID: 1138020-05 Report Matrix: FGD Wastewater Sample Type: Sample Received: 09/14/2011 Sample: BioReactor 2 Eff Collected: 09/12/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71313080 60 Cooler

None N/A 250 mL Bottle FLPE Hg-T

Lab ID: 1138020-06 Report Matrix: DIW Sample Type: Field Blank Received: 09/14/2011 Sample: Hg Blk BioReactor 2 Eff Collected: 09/12/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71313080 60 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-HV1101

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



# Shipping Containers

Cooler Tracking No: 4726 7966 3870 via FedEx Temperature: 3.5 °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: September 14, 2011 8:30

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