### 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: J12020079

Lab Contact: Jason C Perkins 

### Date: 2/22/2012 Customer Address: 3195 Pine Hall Rd Customer Name(s): Bill Kennedy, Meloni e Martin, Wayne Chapman, Tom Johnson

Mailcode: Belews Steam Station Belews Creek, NC 28012

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


### Program Comments: Please contact the Program Manager (Jason C Perkins) with any questions regarding this report. Data Flags & Calculations: Any analytical tests or individual analytes within a test flagged with a Qualifier indicate a deviation from the method quality system or quality control requirement. The qualifier description is found at the end of the 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 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 2012002683 BELEWS 08-Feb-12 8:10 AM R. HENDRICKS FGD Purge Eff 2012002684 BELEWS 08-Feb-12 8:10 AM R. HENDRICKS EQ TANK EFF. 2012002685 BELEWS 08-Feb-12 8:15 AM R. HENDRICKS BIOREACTOR 1 INF. 2012002686 BELEWS 08-Feb-12 8:20 AM R. HENDRICKS BIOREACTOR 2 INF. 2012002687 BELEWS 08-Feb-12 8:25 AM R. HENDRICKS BIOREACTOR 2 EFF. 2012002688 BELEWS 08-Feb-12 8:00 AM R. HENDRICKS FILTER BLANK 2012002689 BELEWS 08-Feb-12 8:00 AM R. HENDRICKS Trip Blank 2012002690 BELEWS 08-Feb-12 1:15 PM David Morris (Prism) BIOREACTOR 1 INF. 2012002699 BELEWS 08-Feb-12 1:15 PM David Morris (Prism) HG BLANK BIOREACTOR 1 INF. 2012002700 BELEWS 08-Feb-12 1:25 PM David Morris (Prism) BIOREACTOR 2 INF. 2012002701 BELEWS 08-Feb-12 1:25 PM David Morris (Prism) Hg Blk BioReactor 2 Inf 2012002702 BELEWS 08-Feb-12 1:20 PM David Morris (Prism) BIOREACTOR 2 EFF. 2012002703 BELEWS 08-Feb-12 1:20 PM David Morris (Prism) Hg Blk BioReactor 2 Eff 13 Total Samples

### COC and .pdf report are in agreement with sample totals and analyses (compliance programs and procedures). All Results are less than the laboratory reporting limits. All laboratory QA/QC requirements are acceptable. The Vendor Laboratories have been qualified by the Analytical Laboratory Yes No 

# Technical Validation Review Checklist:

Yes No

Yes No



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

Reviewed By: 

### Mary Ann Ogle Date: 

### 2/22/2012 Yes

Electronic Data Deliverable (EDD) Sent Separately

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

### Order # J12020079

2012002683 Collection Date: 08-Feb-12 8:10 AM 

### Site: FGD Purge Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF INORGANIC IONS BY IC Bromide 100 mg/L EPA 300.0 5 50 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 307 ug/L EPA 245.1 10-Feb-12 10:21 AGIBBS 5 100
TOTAL RECOVERABLE METALS BY ICP Boron (B) 194 mg/L EPA 200.7 21-Feb-12 13:25 DJSULL1 0.5 10 Manganese (Mn) 7.08 mg/L EPA 200.7 21-Feb-12 13:25 DJSULL1 0.05 10
DISSOLVED METALS BY ICP-MS Manganese (Mn) 5660 ug/L EPA 200.8 15-Feb-12 11:24 MHH7131 50 50 Selenium (Se) 275 ug/L EPA 200.8 15-Feb-12 11:24 MHH7131 50 50
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 273 ug/L EPA 200.8 15-Feb-12 10:51 MHH7131 10 10 Chromium (Cr) 299 ug/L EPA 200.8 15-Feb-12 10:51 MHH7131 10 10 Copper (Cu) 160 ug/L EPA 200.8 15-Feb-12 10:51 MHH7131 10 10 Nickel (Ni) 213 ug/L EPA 200.8 15-Feb-12 10:51 MHH7131 10 10 Selenium (Se) 6280 ug/L EPA 200.8 15-Feb-12 10:51 MHH7131 50 50 Silver (Ag) < 10.0 ug/L EPA 200.8 15-Feb-12 10:51 MHH7131 10 10 Zinc (Zn) 300 ug/L EPA 200.8 15-Feb-12 10:51 MHH7131 10 10
SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 1
TOTAL DISSOLVED SOLIDS TDS 16000 mg/L SM2540C 09-Feb-12 15:30 TJA7067 200 1



### 2012002684 Collection Date: 08-Feb-12 8:10 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 173 ug/L EPA 245.1 10-Feb-12 10:42 AGIBBS 2.5 50
TOTAL RECOVERABLE METALS BY ICP Boron (B) 182 mg/L EPA 200.7 21-Feb-12 13:29 DJSULL1 0.5 10 Manganese (Mn) 6.87 mg/L EPA 200.7 21-Feb-12 13:29 DJSULL1 0.05 10

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

### Order # J12020079

2012002684 Collection Date: 08-Feb-12 8:10 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF DISSOLVED METALS BY ICP-MS Manganese (Mn) 5200 ug/L EPA 200.8 15-Feb-12 11:27 MHH7131 50 50 Selenium (Se) 173 ug/L EPA 200.8 15-Feb-12 11:27 MHH7131 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 157 ug/L EPA 200.8 15-Feb-12 10:54 MHH7131 10 10 Chromium (Cr) 180 ug/L EPA 200.8 15-Feb-12 10:54 MHH7131 10 10 Copper (Cu) 96.9 ug/L EPA 200.8 15-Feb-12 10:54 MHH7131 10 10 Nickel (Ni) 156 ug/L EPA 200.8 15-Feb-12 10:54 MHH7131 10 10 Selenium (Se) 3810 ug/L EPA 200.8 15-Feb-12 10:54 MHH7131 10 10 Silver (Ag) < 10.0 ug/L EPA 200.8 15-Feb-12 10:54 MHH7131 10 10 Zinc (Zn) 188 ug/L EPA 200.8 15-Feb-12 10:54 MHH7131 10 10



### 2012002685 Collection Date: 08-Feb-12 8:15 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF INORGANIC IONS BY IC Bromide 93 mg/L EPA 300.0 16-Feb-12 06:53 JAHERMA 5 50
TOTAL RECOVERABLE METALS BY ICP Boron (B) 162 mg/L EPA 200.7 21-Feb-12 13:33 DJSULL1 0.5 10 Manganese (Mn) 3.43 mg/L EPA 200.7 21-Feb-12 13:33 DJSULL1 0.05 10
DISSOLVED METALS BY ICP-MS Manganese (Mn) 3410 ug/L EPA 200.8 15-Feb-12 11:30 MHH7131 10 10 Selenium (Se) 118 ug/L EPA 200.8 15-Feb-12 11:30 MHH7131 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10.0 ug/L EPA 200.8 15-Feb-12 10:57 MHH7131 10 10 Chromium (Cr) < 10.0 ug/L EPA 200.8 15-Feb-12 10:57 MHH7131 10 10 Copper (Cu) < 10.0 ug/L EPA 200.8 15-Feb-12 10:57 MHH7131 10 10 Nickel (Ni) 33.1 ug/L EPA 200.8 15-Feb-12 10:57 MHH7131 10 10 Selenium (Se) 119 ug/L EPA 200.8 15-Feb-12 10:57 MHH7131 10 10 Silver (Ag) < 10.0 ug/L EPA 200.8 15-Feb-12 10:57 MHH7131 10 10 Zinc (Zn) < 10.0 ug/L EPA 200.8 15-Feb-12 10:57 MHH7131 10 10
SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 1

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

### Order # J12020079

2012002686 Collection Date: 08-Feb-12 8:20 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF TOTAL RECOVERABLE METALS BY ICP Boron (B) 162 mg/L EPA 200.7 21-Feb-12 13:37 DJSULL1 0.5 10 Manganese (Mn) 3.61 mg/L EPA 200.7 21-Feb-12 13:37 DJSULL1 0.05 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10.0 ug/L EPA 200.8 15-Feb-12 11:00 MHH7131 10 10 Chromium (Cr) < 10.0 ug/L EPA 200.8 15-Feb-12 11:00 MHH7131 10 10 Copper (Cu) < 10.0 ug/L EPA 200.8 15-Feb-12 11:00 MHH7131 10 10 Nickel (Ni) < 10.0 ug/L EPA 200.8 15-Feb-12 11:00 MHH7131 10 10 Selenium (Se) 24.5 ug/L EPA 200.8 15-Feb-12 11:00 MHH7131 10 10 Silver (Ag) < 10.0 ug/L EPA 200.8 15-Feb-12 11:00 MHH7131 10 10 Zinc (Zn) < 10.0 ug/L EPA 200.8 15-Feb-12 11:00 MHH7131 10 10



### 2012002687 Collection Date: 08-Feb-12 8:25 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF INORGANIC IONS BY IC Bromide 89 mg/L EPA 300.0 16-Feb-12 07:09 JAHERMA 5 50 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) < 1.00 ug/L EPA 245.1 10-Feb-12 10:45 AGIBBS 1 20
TOTAL RECOVERABLE METALS BY ICP Boron (B) 150 mg/L EPA 200.7 21-Feb-12 13:41 DJSULL1 0.5 10 Manganese (Mn) 3.56 mg/L EPA 200.7 21-Feb-12 13:41 DJSULL1 0.05 10
DISSOLVED METALS BY ICP-MS Manganese (Mn) 3270 ug/L EPA 200.8 15-Feb-12 11:33 MHH7131 10 10 Selenium (Se) < 5.00 ug/L EPA 200.8 15-Feb-12 11:33 MHH7131 5 5
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10.0 ug/L EPA 200.8 15-Feb-12 11:03 MHH7131 10 10 Chromium (Cr) < 10.0 ug/L EPA 200.8 15-Feb-12 11:03 MHH7131 10 10 Copper (Cu) < 10.0 ug/L EPA 200.8 15-Feb-12 11:03 MHH7131 10 10 Nickel (Ni) < 10.0 ug/L EPA 200.8 15-Feb-12 11:03 MHH7131 10 10 Selenium (Se) < 10.0 ug/L EPA 200.8 15-Feb-12 11:03 MHH7131 10 10 Silver (Ag) < 10.0 ug/L EPA 200.8 15-Feb-12 11:03 MHH7131 10 10 Zinc (Zn) < 10.0 ug/L EPA 200.8 15-Feb-12 11:03 MHH7131 10 10
SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 1

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

### Order # J12020079

2012002688 Collection Date: 08-Feb-12 8:00 AM 

### Site: FILTER BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF DISSOLVED METALS BY ICP-MS Manganese (Mn) 1.36 ug/L EPA 200.8 15-Feb-12 11:21 MHH7131 1 1 Selenium (Se) 1.41 ug/L EPA 200.8 15-Feb-12 11:21 MHH7131 1 1



### 2012002689 Collection Date: 08-Feb-12 8:00 AM 

### Site: Trip Blank Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF TOTAL RECOVERABLE METALS BY ICP Boron (B) < 0.050 mg/L EPA 200.7 21-Feb-12 13:21 DJSULL1 0.05 1 Manganese (Mn) < 0.005 mg/L EPA 200.7 21-Feb-12 13:21 DJSULL1 0.005 1
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 1.00 ug/L EPA 200.8 15-Feb-12 10:48 MHH7131 1 1 Chromium (Cr) < 1.00 ug/L EPA 200.8 15-Feb-12 10:48 MHH7131 1 1 Copper (Cu) 2.29 ug/L EPA 200.8 15-Feb-12 10:48 MHH7131 1 1 Nickel (Ni) < 1.00 ug/L EPA 200.8 15-Feb-12 10:48 MHH7131 1 1 Selenium (Se) < 1.00 ug/L EPA 200.8 15-Feb-12 10:48 MHH7131 1 1 Silver (Ag) 1.37 ug/L EPA 200.8 15-Feb-12 10:48 MHH7131 1 1 Zinc (Zn) 1.76 ug/L EPA 200.8 15-Feb-12 10:48 MHH7131 1 1
SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 1



### 2012002690 Collection Date: 08-Feb-12 1:15 PM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF MERCURY 1631 Vendor Parameter Complete V_BRAND 1



### 2012002699 Collection Date: 08-Feb-12 1:15 PM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF MERCURY 1631 Vendor Parameter Complete V_BRAND 1

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

### Order # J12020079

2012002700 Collection Date: 08-Feb-12 1:25 PM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF MERCURY 1631 Vendor Parameter Complete V_BRAND 1



### 2012002701 Collection Date: 08-Feb-12 1:25 PM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF MERCURY 1631 Vendor Parameter Complete V_BRAND 1



### 2012002702 Collection Date: 08-Feb-12 1:20 PM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF MERCURY 1631 Vendor Parameter Complete V_BRAND 1



### 2012002703 Collection Date: 08-Feb-12 1:20 PM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF MERCURY 1631 Vendor Parameter Complete V_BRAND 1

## February 21 , 201 2

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

– FGD WWTS (Bi-Monthly Wed-Sampling) (LIMS # J1 20200 79)

Dear Mr. Perkins, Attached is the report associated with four (4 ) aqueous samples submitted for selenium speciation analysis on February 9 , 2012

. The samples were received in a sealed cooler at-0. 5 ° C on February 10 , 2012

. Selenium speciation analysis was performed via ion chromatographyinductively coupled plasma kinetic energy discrimination cell mass spectrometry (IC-ICP-KEDMS). Any issues associated with the analysis are addressed in the following report. If you have any questions, please feel free to contact me at your convenience.
Sincerely,

Russell Gerads Vice President Applied Speciation and Consulting, LLC

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

– FGD WWTS (Bi-Monthly Wed-Sampling) (LIMS # J1 2020079 )
February 21 , 2012

1. Sample Reception Four (4 ) aqueous samples in 125mL HDPE bottles (provided by Applied Speciation and Consulting) were submitted for selenium speciation analysi s on February 9 , 2012 . The samples were received on February 10 , 201 2 in a sealed container at -0. 5 °C. The samples were received in a laminar flow clean hood, void of trace metals contamination and ultra-violet radiation, and was designated a discrete sample identifier. An aliquot of each sample was filtered (0.45μm) and each filtrate w as stored in a secure, monitored cryofreezer (maintained at a temperature of -80 o 

## C) until selenium speciation analysis could be performed via ion chromatography inductively coupled plasma kinetic energy discrimination mass spectrometry (IC-ICP-KED-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-K ED

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

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

instrument blank corrected to account for any operational biases associated with the analytical platform. Prior to sample analysis, all calibration curves are verified using second source standard s which are identified as initial calibration verification standards (ICV). Ongoing instrument performance is identified by the analysis of continuing calibration verification standards (CCV) and continuing calibration blanks (CCB) at a minimal interval of every ten analytical runs. Selenium Speciation Analysis by IC -ICP-KED- MS Each sample for selenium speciation analysis w as analyzed by ion chromatography inductively coupled plasma kinetic energy discrimination mass spectrometry (IC-ICP-KED-MS) on February 16 , 2012 . 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 (KED) containing hydrogen 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. 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,

Russell Gerads Vice President Applied Speciation and Consulting, LLC

### Sample Results
Sample ID Se(IV) Se(VI) SeCN MeSe(IV) SeMe Unknown Se Species (n) FGD Purge Eff 124 64.0 ND (<0.86) 1.96 ND (<0.59) 0 (0) BioReactor 1 Inf 26.0 60.6 ND (<0.21) 3.50 ND (<0.15) 0 (0) BioReactor 2 Eff 0.42 ND (<0.12) ND (<0.21) ND (<0.15) ND (<0.15) 0 (0) Metals Trip Blk ND (<0.022) ND (<0.024) ND (<0.043) ND (<0.030) ND (<0.030) 0 (0) All results reflect the applied dilution and are reported in μg/L ND = Not detected at the applied dilution SeCN = Selenocyanate MeSe(IV) = Methylseleninic acid SeMe = Selenomethionine Unknown Se Species = Total concentration of all unknown Se species observed by IC-ICP-MS n = number of unknown Se species observed Report Generated by: Russell Gerads Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS (Bi-Monthly-Wed-Sampling)

Contact: Jay Perkins
Date: February 21, 2012 LIMS #J12020079

### Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 10x eMDL 50x eMDL 200x Se(IV) 0.010 0.017 0.010 0.011 0.012 0.003 0.002 0.022 0.11 0.43 Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.024 0.12 0.48 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.043 0.21 0.86 MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.003 0.030 0.15 0.59 SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.003 0.030 0.15 0.59 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 9.48 99.1 Se(VI) LCS 9.48 9.04 95.4 SeCN LCS 8.92 8.44 94.6 MeSe(IV) LCS 6.47 6.07 93.8 SeMe LCS 9.32 8.70 93.3 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS (Bi-Monthly-Wed-Sampling)

Contact: Jay Perkins LIMS #J12020079 Date: February 21, 2012 Report Generated by: Russell Gerads

### Quality Control Summary - Matrix Duplicates

Analyte (μg/L) Sample ID Rep 1 Rep 2 Mean RPD Se(IV) Batch QC 0.69 0.62 0.7 10.3 Se(VI) Batch QC ND (<0.48) ND (<0.48) NC NC SeCN Batch QC 4.61 4.36 4.5 5.4 MeSe(IV) Batch QC ND (<0.59) ND (<0.59) NC NC SeMe Batch QC 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) Batch QC 1112 1186 106.7 1112 1185 106.6 0.1 Se(VI) Batch QC 1009 1063 105.4 1009 1056 104.7 0.6 SeCN Batch QC 915.0 955.7 104.0 915.0 946.6 103.0 1.0 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS (Bi-Monthly-Wed-Sampling)

Contact: Jay Perkins LIMS #J12020079 Date: February 21, 2012 Report Generated by: Russell Gerads3958 6 th Ave NW • Seattle, WA 98107 • T: 206-632-6206 • F: 206-632-6017 • www.brooksrand.com • brl@brooksrand.com 

### February 15, 2012
Duke Energy ATTN: Jay Perkins Scientific Support-Laboratory 13339 Hagers Ferry Road Huntersville NC 28078 jcperkins@duke-energy.com labcustomer@duke-energy.com
RE: Project DUK-HV1201 Client Project: J12020079 Dear Mr. Perkins, On February 10, 2012, Brooks Rand Labs (BRL) received three (3) wastewater 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. No qualification of the data was warranted, aside from concentration qualifiers, and all associated quality control sample results met the acceptance criteria. BRL, an accredited laboratory, certifies the reported results of all analyses for which BRL is NELAP accredited meet all NELAP requirements. For more details, see the Report Information page of the report. Please feel free to contact me if you have any questions regarding this report. Sincerely,

Tiffany Stilwater Project Manager tiffany@brooksrand.comProject ID: DUK-HV1201

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



### Definition of Data Qualifiers

(Effective 9/23/09) 

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

# Report Information

BLK BRL BS CAL CCV
CRM D DUP ICV MSD ND NR PS REC RPD RSD SCV SOP method blank Brooks Rand Labs laboratory fortified blank calibration standard continuing calibration verification certified reference material dissolved fraction duplicate initial calibration verification matrix spike duplicate non-detect non-reportable post preparation spike percent recovery relative percent difference relative standard deviation secondary calibration verification standard operating procedure MDL MRL MS

method detection limit method reporting limit matrix spike

SRM T COC

standard reference material total recoverable fraction chain of custody record 

### Common Abbreviations

These qualifiers are based on those previously utilized by Brooks Rand, Ltd., those found in the EPA SOW ILM03.0, Exhibit B, Section III, pg. B-18, and the USEPA Laboratory Data Validation Functional Guidelines for Evaluating Inorganic Analyses; USEPA; July 2002. These supersede all previous qualifiers ever employed by BRL. Detected by the instrument, the result is > the MDL but ≤ the MRL. Result is reported and considered an estimate. B E An estimated value due to the presence of interferences. A full explanation is presented in the narrative. H Holding time and/or preservation requirements not met. Result is estimated. J Estimated value. A full explanation is presented in the narrative. J-M Duplicate precision (RPD) for associated QC sample was not within acceptance criteria. Result is estimated. J-N Spike recovery for associated QC sample was not within acceptance criteria. Result is estimated. M Duplicate precision (RPD) was not within acceptance criteria. Result is estimated. N Spike recovery was not within acceptance criteria. Result is estimated. R Rejected, unusable value. A full explanation is presented in the narrative. U Result is ≤ the MDL or client requested reporting limit (CRRL). Result reported as the MDL or CRRL. X Result is not BLK-corrected and is within 10x the absolute value of the highest detectable BLK in the batch. Result is estimated. 

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

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: DUK-HV1201

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



# Sample Information

Report Matrix Type Received Sampled Sample Lab ID 1206023-01 BioReactor 1 Inf 02/08/2012 02/10/2012 Sample Influent 1206023-02 Hg Blk BioReactor 1 Inf 02/08/2012 02/10/2012 Field Blank DIW 1206023-03 BioReactor 2 Inf 02/08/2012 02/10/2012 QC Sample Influent 1206023-04 Hg Blk BioReactor 2 Inf 02/08/2012 02/10/2012 Field Blank DIW 1206023-05 BioReactor 2 Eff 02/08/2012 02/10/2012 Sample Effluent 1206023-06 Hg Blk BioReactor 2 Eff 02/08/2012 02/10/2012 Field Blank DIW 

# Batch Summary

Analyte Prepared Analyzed Sequence Batch Lab Matrix Method B120211 02/10/2012 02/13/2012 1200098 Water EPA 1631 Hg

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: DUK-HV1201

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



# Sample Results

Sample Sequence Result MDL MRL Unit Batch

Qualifier Analyte Fraction

Report Matrix BioReactor 1 Inf ng/L 229 T 1200098 B120211 Influent 40.8 15.3 1206023-01 Hg

BioReactor 2 Eff ng/L 12.5 T 1200098 B120211 Effluent 4.04 1.52 1206023-05 Hg

BioReactor 2 Inf ng/L 67.6 T 1200098 B120211 Influent 8.08 3.03 1206023-03 Hg
Hg Blk BioReactor 1 Inf ng/L 0.15 T U 1200098 B120211 DIW 0.40 0.15 1206023-02 Hg
Hg Blk BioReactor 2 Eff ng/L 0.15 T U 1200098 B120211 DIW 0.41 0.15 1206023-06 Hg
Hg Blk BioReactor 2 Inf ng/L 0.15 T U 1200098 B120211 DIW 0.40 0.15 1206023-04 Hg

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: DUK-HV1201

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



# Accuracy & Precision Summary

Batch: B120211

Analyte Result Units Native Spike REC & Limits RPD & Limits Method: EPA 1631 Lab Matrix: Water

Sample Certified Reference Material (1205004, NIST 1641d 1000x dilution) B120211-SRM1 15.68 85% ng/L 85-115 Hg 13.35
Matrix Spike (1206023-03) B120211-MS1 303.0 99% ng/L 71-125 Hg 366.7

67.57
Matrix Spike Duplicate (1206023-03) B120211-MSD1 303.0 100% ng/L 71-125 241% Hg 370.4

67.57



# Method Blanks & Reporting Limits

Batch: B120211
Method: EPA 1631 Matrix: Water Analyte: Hg Result Units Sample B120211-BLK1 ng/L 0.03 B120211-BLK2 ng/L 0.07 B120211-BLK3 ng/L 0.05 B120211-BLK4 ng/L 0.05 MDL: 0.15 Average: 0.05 Standard Deviation: 0.02 Limit: 0.10 Limit: 0.50 MRL: 0.40

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: DUK-HV1201

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



# Instrument Calibration

Sequence: 1200098 Method: EPA 1631 Instrument: THG-05 Date: 02/13/2012 Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg REC & Limits Result True Value Lab ID Units 1200098-IBL1 7.33 pg of Hg 1200098-IBL2 6.20 pg of Hg 1200098-IBL3 7.11 pg of Hg 1200098-IBL4 6.03 pg of Hg 1200098-CAL1 25.00 26.31 pg of Hg 105% 1200098-CAL2 100.0 98.31 pg of Hg 98% 1200098-CAL3 500.0 495.9 pg of Hg 99% 1200098-CAL4 2500 2485 pg of Hg 99% 1200098-CAL5 10000 9819 pg of Hg 98% 1200098-ICV1 1568 1335 pg of Hg 85% 85-115 1200098-CCB1 8.51 pg of Hg 1200098-CCV1 500.0 465.7 pg of Hg 93% 77-123 1200098-CCV2 500.0 459.3 pg of Hg 92% 77-123

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: DUK-HV1201

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



# Sample Containers

Lab ID: 1206023-01 Report Matrix: Influent Sample Type: Sample Received: 02/10/2012 Sample: BioReactor 1 Inf Collected: 02/08/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71511970 10 Cardboard Box none n/a 500 mL Bottle FLPE Hg-T

Lab ID: 1206023-02 Report Matrix: DIW Sample Type: Field Blank Received: 02/10/2012 Sample: Hg Blk BioReactor 1 Inf Collected: 02/08/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71470160 10 Cardboard Box none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 1206023-03 Report Matrix: Influent Sample Type: QC Sample Received: 02/10/2012 Sample: BioReactor 2 Inf Collected: 02/08/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71470160 10 Cardboard Box none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 1206023-04 Report Matrix: DIW Sample Type: Field Blank Received: 02/10/2012 Sample: Hg Blk BioReactor 2 Inf Collected: 02/08/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71470160 10 Cardboard Box none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 1206023-05 Report Matrix: Effluent Sample Type: Sample Received: 02/10/2012 Sample: BioReactor 2 Eff Collected: 02/08/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71470160 10 Cardboard Box none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 1206023-06 Report Matrix: DIW Sample Type: Field Blank Received: 02/10/2012 Sample: Hg Blk BioReactor 2 Eff Collected: 02/08/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71470160 10 Cardboard Box none n/a 250 mL Bottle FLPE Hg-T

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: DUK-HV1201

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



# Shipping Containers

Cardboard Box Tracking No: 4726 7966 8183 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: February 10, 2012 8:45

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