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: J13030084 Project Name: WWTS - Biweekly (1)

L ab Contact: Jason C Perkins
Date: 4/4/2013 Customer Address: 3195 Pine Hall Rd Customer Name(s): BIll K, Wayne C, Melonie M, and T. THORNTON

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 Certificate of Analysis (sample results) under the qualifiers heading. All results are reported on a dry weight basis unless otherwise noted. Subcontracted data included on the Duke Certificate of Analysis is to be used as information only. Certified vendor results can be found in the subcontracted lab final report. Duke Energy Analytical Laboratory subcontracts analyses to other vendor laboratories that have been qualified by Duke Energy to perform these analyses except where noted. Data Package: This data package includes analytical results that are applicable only to the samples described in this narrative. An estimation of the uncertainty of measurement for the results in the report is available upon request. This report shall not be reproduced, except in full, without the written consent of the Analytical Laboratory. Please contact the Analytical laboratory with any questions. The order of individual sections within this report is as follows: Job Summary Report, Sample Identification, Technical Validation of Data Package, Analytical Laboratory Certificate of Analysis, Analytical Laboratory QC Reports, Sub-contracted Laboratory Results, Customer Specific Data Sheets, Reports & Documentation, Customer Database Entries, Test Case Narratives, Chain of Custody (COC)
Certification: The Analytical Laboratory holds the following State Certifications : North Carolina (DENR) Certificate #248, South Carolina (DHEC) Laboratory ID # 99005. Contact the Analytical Laboratory for definitive information about the certification status of specific methods. Jason C Perkins

### Sample ID's & Descriptions:

Sample ID Plant/Station Collection Date and Time Collected By Sample Description 2013005228 BELEWS 13-Mar-13 8:00 AM W. B. WORKMAN FGD Purge Eff 2013005229 BELEWS 13-Mar-13 8:05 AM W. B. WORKMAN EQ TANK EFF. 2013005230 BELEWS 13-Mar-13 8:10 AM W. B. WORKMAN BIOREACTOR 1 INF. 2013005231 BELEWS 13-Mar-13 8:15 AM W. B. WORKMAN BIOREACTOR 2 INF. 2013005232 BELEWS 13-Mar-13 8:20 AM W. B. WORKMAN BIOREACTOR 2 EFF. 2013005233 BELEWS 13-Mar-13 8:25 AM W. B. WORKMAN FILTER BLANK 2013005234 BELEWS 05-Mar-13 10:50 AM C.KNOX Trip Blank 2013005235 BELEWS 13-Mar-13 8:10 AM W. B. WORKMAN BIOREACTOR 1 INF (HG) 2013005236 BELEWS 13-Mar-13 8:10 AM W. B. WORKMAN HG BLANK BIOREACTOR 1 INF. 2013005237 BELEWS 13-Mar-13 8:15 AM W. B. WORKMAN BIOREACTOR 2 INF (HG) 2013005238 BELEWS 13-Mar-13 8:15 AM W. B. WORKMAN Hg Blk BioReactor 2 Inf 2013005239 BELEWS 13-Mar-13 8:20 AM W. B. WORKMAN BIOREACTOR 2 EFF (HG) 2013005240 BELEWS 13-Mar-13 8:20 AM W. B. WORKMAN Hg Blk BioReactor 2 Eff 13 Total SamplesCOC 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. 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: DBA Account Date: 4/4/2013 Electronic Data Deliverable (EDD) Sent Separately

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



### Order # J13030084

2013005228 Collection Date: 13-Mar-13 8:00 AM Site: FGD Purge Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sample #:

Analyst DF INORGANIC IONS BY IC Bromide 92 mg/L EPA 300.0 03/22/2013 17:04 BGN9034 5 50 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 217 ug/L EPA 245.1 03/21/2013 12:58 AGIBBS 5 100
DISSOLVED METALS BY ICP Manganese (Mn) 8.56 mg/L EPA 200.7 03/18/2013 15:27 MHH7131 0.05 10
TOTAL RECOVERABLE METALS BY ICP Boron (B) 188 mg/L EPA 200.7 03/20/2013 12:58 MHH7131 0.5 10 Manganese (Mn) 9.86 mg/L EPA 200.7 03/20/2013 12:58 MHH7131 0.05 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 130 ug/L EPA 200.8 03/22/2013 12:47 KRICHAR 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 210 ug/L EPA 200.8 03/19/2013 12:43 KRICHAR 10 10 Chromium (Cr) 281 ug/L EPA 200.8 03/19/2013 12:43 KRICHAR 10 10 Copper (Cu) 127 ug/L EPA 200.8 03/19/2013 12:43 KRICHAR 10 10 Nickel (Ni) 268 ug/L EPA 200.8 03/19/2013 12:43 KRICHAR 10 10 Selenium (Se) 2980 ug/L EPA 200.8 03/19/2013 12:43 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 03/19/2013 12:43 KRICHAR 10 10 Zinc (Zn) 218 ug/L EPA 200.8 03/19/2013 12:43 KRICHAR 10 10 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C
TOTAL DISSOLVED SOLIDS TDS 17000 mg/L SM2540C 03/19/2013 15:35 SWILLI3 200 1

2013005229 Collection Date: 13-Mar-13 8:05 AM Site: EQ TANK EFF. Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sample #:

Analyst DF MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 155 ug/L EPA 245.1 03/21/2013 13:00 AGIBBS 2.5 50
DISSOLVED METALS BY ICP Manganese (Mn) 8.18 mg/L EPA 200.7 03/18/2013 15:30 MHH7131 0.05 10
TOTAL RECOVERABLE METALS BY ICP Boron (B) 207 mg/L EPA 200.7 03/20/2013 13:02 MHH7131 0.5 10 Manganese (Mn) 9.65 mg/L EPA 200.7 03/20/2013 13:02 MHH7131 0.05 10

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



### Order # J13030084

2013005229 Collection Date: 13-Mar-13 8:05 AM Site: EQ TANK EFF. Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sample #:

Analyst DF DISSOLVED METALS BY ICP-MS Selenium (Se) 94.0 ug/L EPA 200.8 03/22/2013 12:50 KRICHAR 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 185 ug/L EPA 200.8 03/19/2013 12:47 KRICHAR 10 10 Chromium (Cr) 246 ug/L EPA 200.8 03/19/2013 12:47 KRICHAR 10 10 Copper (Cu) 114 ug/L EPA 200.8 03/19/2013 12:47 KRICHAR 10 10 Nickel (Ni) 260 ug/L EPA 200.8 03/19/2013 12:47 KRICHAR 10 10 Selenium (Se) 2700 ug/L EPA 200.8 03/19/2013 12:47 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 03/19/2013 12:47 KRICHAR 10 10 Zinc (Zn) 196 ug/L EPA 200.8 03/19/2013 12:47 KRICHAR 10 10

2013005230 Collection Date: 13-Mar-13 8:10 AM Site: BIOREACTOR 1 INF. Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sample #:

Analyst DF DISSOLVED METALS BY ICP Manganese (Mn) 2.37 mg/L EPA 200.7 03/18/2013 15:34 MHH7131 0.05 10
TOTAL RECOVERABLE METALS BY ICP Boron (B) 193 mg/L EPA 200.7 03/20/2013 13:06 MHH7131 0.5 10 Manganese (Mn) 2.51 mg/L EPA 200.7 03/20/2013 13:06 MHH7131 0.05 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 84.8 ug/L EPA 200.8 03/22/2013 12:54 KRICHAR 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 03/19/2013 12:51 KRICHAR 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 03/19/2013 12:51 KRICHAR 10 10 Copper (Cu) < 10 ug/L EPA 200.8 03/19/2013 12:51 KRICHAR 10 10 Nickel (Ni) 34.5 ug/L EPA 200.8 03/19/2013 12:51 KRICHAR 10 10 Selenium (Se) 60.2 ug/L EPA 200.8 03/19/2013 12:51 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 03/19/2013 12:51 KRICHAR 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 03/19/2013 12:51 KRICHAR 10 10 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C

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



### Order # J13030084

2013005231 Collection Date: 13-Mar-13 8:15 AM Site: BIOREACTOR 2 INF. Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sample #:

Analyst DF TOTAL RECOVERABLE METALS BY ICP Boron (B) 198 mg/L EPA 200.7 03/20/2013 13:10 MHH7131 0.5 10 Manganese (Mn) 2.92 mg/L EPA 200.7 03/20/2013 13:10 MHH7131 0.05 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 03/19/2013 12:54 KRICHAR 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 03/19/2013 12:54 KRICHAR 10 10 Copper (Cu) < 10 ug/L EPA 200.8 03/19/2013 12:54 KRICHAR 10 10 Nickel (Ni) < 10 ug/L EPA 200.8 03/19/2013 12:54 KRICHAR 10 10 Selenium (Se) < 10 ug/L EPA 200.8 03/19/2013 12:54 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 03/19/2013 12:54 KRICHAR 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 03/19/2013 12:54 KRICHAR 10 10

2013005232 Collection Date: 13-Mar-13 8:20 AM Site: BIOREACTOR 2 EFF. Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sample #:

Analyst DF INORGANIC IONS BY IC Bromide 110 mg/L EPA 300.0 03/22/2013 17:22 BGN9034 5 50 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) < 1 ug/L EPA 245.1 03/21/2013 13:03 AGIBBS 1 20
TOTAL RECOVERABLE METALS BY ICP Boron (B) 204 mg/L EPA 200.7 03/20/2013 13:14 MHH7131 0.5 10 Manganese (Mn) 4.61 mg/L EPA 200.7 03/20/2013 13:14 MHH7131 0.05 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 5 ug/L EPA 200.8 03/19/2013 12:58 KRICHAR 5 5 Chromium (Cr) < 5 ug/L EPA 200.8 03/19/2013 12:58 KRICHAR 5 5 Copper (Cu) < 5 ug/L EPA 200.8 03/19/2013 12:58 KRICHAR 5 5 Nickel (Ni) < 5 ug/L EPA 200.8 03/19/2013 12:58 KRICHAR 5 5 Selenium (Se) < 5 ug/L EPA 200.8 03/19/2013 12:58 KRICHAR 5 5 Silver (Ag) < 5 ug/L EPA 200.8 03/19/2013 12:58 KRICHAR 5 5 Zinc (Zn) < 5 ug/L EPA 200.8 03/19/2013 12:58 KRICHAR 5 5 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C

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



### Order # J13030084

2013005233 Collection Date: 13-Mar-13 8:25 AM Site: FILTER BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sample #:

Analyst DF DISSOLVED METALS BY ICP Manganese (Mn) 0.033 mg/L EPA 200.7 03/18/2013 15:11 MHH7131 0.005 1
DISSOLVED METALS BY ICP-MS Selenium (Se) < 1 ug/L EPA 200.8 03/22/2013 12:12 KRICHAR 1 1

2013005234 Collection Date: 05-Mar-13 10:50 AM Site: Trip Blank Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sample #:

Analyst DF TOTAL RECOVERABLE METALS BY ICP Boron (B) < 0.05 mg/L EPA 200.7 03/20/2013 12:54 MHH7131 0.05 1 Manganese (Mn) < 0.005 mg/L EPA 200.7 03/20/2013 12:54 MHH7131 0.005 1
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 1 ug/L EPA 200.8 03/19/2013 12:36 KRICHAR 1 1 Chromium (Cr) < 1 ug/L EPA 200.8 03/19/2013 12:36 KRICHAR 1 1 Copper (Cu) < 1 ug/L EPA 200.8 03/19/2013 12:36 KRICHAR 1 1 Nickel (Ni) < 1 ug/L EPA 200.8 03/19/2013 12:36 KRICHAR 1 1 Selenium (Se) < 1 ug/L EPA 200.8 03/19/2013 12:36 KRICHAR 1 1 Silver (Ag) < 1 ug/L EPA 200.8 03/19/2013 12:36 KRICHAR 1 1 Zinc (Zn) < 1 ug/L EPA 200.8 03/19/2013 12:36 KRICHAR 1 1 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C

2013005235 Collection Date: 13-Mar-13 8:10 AM Site: BIOREACTOR 1 INF (HG) Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sample #:

Analyst DF MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND

2013005236 Collection Date: 13-Mar-13 8:10 AM Site: HG BLANK BIOREACTOR 1 INF. Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sample #:

Analyst DF MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND

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



### Order # J13030084

2013005236 Collection Date: 13-Mar-13 8:10 AM Site: HG BLANK BIOREACTOR 1 INF. Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sample #:

Analyst DF
2013005237 Collection Date: 13-Mar-13 8:15 AM Site: BIOREACTOR 2 INF (HG) Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sample #:

Analyst DF MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND

2013005238 Collection Date: 13-Mar-13 8:15 AM Site: Hg Blk BioReactor 2 Inf Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sample #:

Analyst DF MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND

2013005239 Collection Date: 13-Mar-13 8:20 AM Site: BIOREACTOR 2 EFF (HG) Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sample #:

Analyst DF MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND

2013005240 Collection Date: 13-Mar-13 8:20 AM Site: Hg Blk BioReactor 2 Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sample #:

Analyst DF MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND

### March 2 7 , 2013

Jay Perkins Duke Energy Analytical Laboratory Mail Code MGO3A2 (Building 7405) 13339 Hagers Ferry Rd. Huntersville, NC 28078 (704) 875-5 245 Project: Belews - FGD WWTS Bi-Monthly Sampling) (LIMS #J13030084)

Dear Mr. Perkins, Attached is the report associated with four (4 ) aqueous samples submitted for selenium speciation on March 18 , 2013

. The samples were received in a sealed cooler at-0.2 ° C on March 1 9 , 2013

. Selenium speciation analysis was performed via ion chromatography inductively coupled plasma collision reaction cell mass spectrometry (IC-ICP-CRC-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,

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 Sampling) (LIMS #J13030084)

March 2 7 , 2013

1. Sample Reception Four (4 ) aqueous samples in125mL HDPE bottles (provided by Applied Speciation and Consulting) were submitted for selenium speciation analysis on March 18 , 2013 . The samples were received on March 1 9 , 201 3 in a sealed container at -0.2 °C. The samples were received in a laminar flow clean hood, void of trace metals contamination and ultra-violet radiation, and were designated discrete sample identifiers. 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 collision reaction cell mass spectrometry (IC-ICP- CRC -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-CRC- MS Prior to analysis, an aliquot of each sample was filtered with a syringe filter (0.45μm) and injected directly into an 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 minimum interval of every ten analytical runs. Selenium Speciation Analysis by IC -ICP-CRC- MS Eachsample for selenium speciation analysis w as analyzed by ion chromatography inductively coupled plasma collision reaction cell mass spectrometry (IC-ICP- CRC -MS) on March 26, 2013. Analiquot of eachsample is injected onto an anion exchange column and mobilized by a basic (pH > 7) gradient. The eluting selenium species are then introduced into a radio frequency (RF) plasma where energy-transfer processes cause desolvation, atomization, and ionization. The ions are extracted from the plasma through a differentially-pumped vacuum interface and travel through a pressurized chamber ( CRC ) containing a reaction 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 the samples were within acceptance limits. The estimated method detection limits (eMDLs) for selenite, selenate, and selenocyanate are generated from replicate analyses of the lowest standard in the calibration curve. Not all selenium species are present in preparation blanks; therefore, eMDL calculations based on preparation blanks are artificially biased low. The eMDL for methylseleninic acid and selenomethionine is calculated from the average eMDL of selenite, selenate, and selenocyanate. The calibration does not contain methylseleninic acid or selenomethionine due to impurities in these standards which would bias the results for other selenium species.

### If you have any questions or concerns regarding this report, please feel free to contact me.

Sincerely,

Russell Gerads Vice President Applied Speciation and Consulting, LLCSample Results
Sample ID Se(IV) Se(VI) SeCN MeSe(IV) SeMe Unknown Se Species (n) FGD Purge Eff 46.0 29.7 ND (< 1.5) ND (< 2.1) ND (< 2.1) 0.0 (0) BioReactor 1 Inf 15.3 30.4 ND (< 0.30) 1.18 ND (< 0.43) 2.69 (1) BioReactor 2 Eff ND (< 0.49) ND (< 0.49) ND (< 0.30) ND (< 0.43) ND (< 0.43) 0.0 (0) Metals Trip Blk 0.228 0.094 ND (< 0.015) ND (< 0.021) ND (< 0.021) 0.0 (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 Report Generated by: Russell Gerads Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS Bi-Monthly Sampling)

Contact: Jay Perkins

Date: March 27, 2013 LIMS #J13030084Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 10x eMDL 200x eMDL 1000x Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.024 0.49 2.4 Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.024 0.49 2.4 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.015 0.30 1.5 MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.021 0.43 2.1 SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.021 0.43 2.1 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 9.407 98.3 Se(VI) LCS 9.48 9.051 95.5 SeCN LCS 8.92 8.658 97.1 MeSe(IV) LCS 6.47 5.959 92.1 SeMe LCS 9.32 8.532 91.5 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS Bi-Monthly Sampling)

Contact: Jay Perkins LIMS #J13030084 Date: March 27, 2013 Report Generated by: Russell GeradsQuality Control Summary - Matrix Duplicates Analyte (μg/L) Sample ID Rep 1 Rep 2 Mean RPD Se(IV) Batch QC 4.5 4.1 4.3 9.2 Se(VI) Batch QC 351.1 353.3 352.2 0.6 SeCN Batch QC ND (< 1.5) ND (< 1.5) NC NC MeSe(IV) Batch QC ND (< 2.1) ND (< 2.1) NC NC SeMe Batch QC ND (< 2.1) ND (< 2.1) 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 5560 5838 104.9 5560 5869 105.5 0.5 Se(VI) Batch QC 5045 5131 94.7 5045 5135 94.8 0.1 SeCN Batch QC 4575 3657 79.9 4575 3757 82.1 2.7 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS Bi-Monthly Sampling)

Contact: Jay Perkins LIMS #J13030084 Date: March 27, 2013 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 

### April 2, 2013 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: J13030084 Dear Mr. Perkins, On March 19, 2013, Brooks Rand Labs (BRL) received three (3) waste water samples and three (3) field blanks samples. The 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 relevant SOP and may have been evaluated using reporting limits that have been adjusted to account for sample aliquot size. Please refer to the Sample Results page for sample-specific MDLs, MRLs, and other details. All data was reported without further qualification, 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,

Lydia Greaves Project Manager lydia@brooksrand.comPro j ect ID: DUK-HV1201 PM: Tiffan yStilwater Client PM: Ja yPerkins 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 ce rtified to perform many environmental analyses. BRL is also certified by many other states to perform environmental analyses. For a current list of ou r accreditations/certifications, please vi sit 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 CC V CRM D DUP IC V MSD ND NR PS REC RPD RSD SC V SOP method blank Brooks Rand Labs laboratoryfortified blank calibration standard continuin g 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 secondarycalibration verification standard operatin g procedure MDL MRL MS

method detection limit method reportin g limit matrix spike

SRM T COC

standard reference material total recoverable fraction chain of custod yrecord 

### Common Abbreviations

These qualifiers are based on those previously ut ilized by Brooks Rand Labs, those found in the EPA SOW ILM 03.0, Exhibit B, Section III, pg. B-18, and the USEPA Contract Laboratory Program Na tional Functional Guidelines for Inorganic Superfund Data Review ; USEPA ; January 2010. These supersede all previous qualifiers ever employed by BRL. Detected b ythe instrument, the result is > the MDL but ≤ the MRL. Result is reported and considered an estimate. B E A n estimated value due to the presence of interferences. A full explanation is presented in the narrative. H Holdin g time and/or preservation requirem ents 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 recoveryfor 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 recoverywas not within acceptance criteria. Result is estimated. R Re j ected, unusable value. A full explanation is presented in the narrative. U Result is ≤ the MDL or client requested reportin g limit ( CRRL ) . Result reported as the MDL or CRRL. X Result is not BLK-corrected and is within 10x the absol ute 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 qualit y 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 author ities. Please see the specific EPA met hods 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.comPro j ect ID: DUK-HV1201 PM: Tiffan yStilwater Client PM: Ja yPerkins Client PO: 141391



# Sample Information

Report Matrix Type Received Sampled Sample Lab ID 1312005-01 BioReactor 1 Inf 03/13/2013 03/19/2013 Sample Influent 1312005-02 Hg Blk BioReactor 1 Inf 03/13/2013 03/19/2013 Field Blank DIW 1312005-03 BioReactor 2 Inf 03/13/2013 03/19/2013 Sample Influent 1312005-04 Hg Blk BioReactor 2 Inf 03/13/2013 03/19/2013 Field Blank DIW 1312005-05 BioReactor 2 Eff 03/13/2013 03/19/2013 Sample Effluent 1312005-06 Hg Blk BioReactor 2 Eff 03/13/2013 03/19/2013 Field Blank DIW 

# Batch Summary

Analyte Prepared Analyzed Sequence Batch Lab Matrix Method B130466 03/25/2013 03/27/2013 1300205 Water EPA 1631 Hg

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comPro j ect ID: DUK-HV1201 PM: Tiffan yStilwater Client PM: Ja yPerkins Client PO: 141391



# Sample Results

Sample Sequenc e Result MDL MRL Unit Batch Qualifier Analyte Basis Report Matrix BioReactor 1 In f 148 T 1300205 B130466 Influent 10.1 3.79 1312005-01 Hg ng/L

BioReactor 2 Ef f 7.57 T 1300205 B130466 Effluent 0.42 0.16 1312005-05 Hg ng/L

BioReactor 2 In f 15.7 T 1300205 B130466 Influent 0.40 0.15 1312005-03 Hg ng/L

H

g

Blk BioReactor 1 In f 0.15 T U 1300205 B130466 DIW 0.40 0.15 1312005-02 Hg ng/L

H

g

Blk BioReactor 2 Ef f 0.16 T U 1300205 B130466 DIW 0.41 0.16 1312005-06 Hg ng/L

H

g

Blk BioReactor 2 In f 0.15 T U 1300205 B130466 DIW 0.41 0.15 1312005-04 Hg ng/L

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comPro j ect ID: DUK-HV1201 PM: Tiffan yStilwater Client PM: Ja yPerkins Client PO: 141391



# Accuracy & Precision Summary

Batch: B130466

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

Sample Certified Reference Material ( 1313016, NIST 1641d 1000x dilution ) B130466-SRM1 15.68 100% ng/L 85-115 Hg 15.64
Matrix Spike ( 1312004-01 ) B130466-MS2 1010 93% ng/L 71-125 Hg 1032 91.47
Matrix Spike Duplicate ( 1312004-01 ) B130466-MSD2 1010 99% ng/L 71-125 246% Hg 1096 91.47



# Method Blanks & Reporting Limits

Batch: B130466
Method: EPA 1631 Matrix: Water
Anal yte: H g Result Units Sample B130466-BLK1 ng/L 0.12 B130466-BLK2 ng/L 0.11 B130466-BLK3 ng/L 0.09 B130466-BLK4 ng/L 0.12 MDL: 0.16 Avera g e: 0.11 Standard Deviation: 0.01 Limit: 0.10 Limit: 0.50 MRL: 0.42

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comPro j ect ID: DUK-HV1201 PM: Tiffan yStilwater Client PM: Ja yPerkins Client PO: 141391



# Instrument Calibration

Sequence: 1300205 Method: EPA 1631 Instrument: THG-06 Date: 03/27/2013 Total Mercur y and Mercur y S p eciation b y CVAFS
Analyte: Hg RE C & Limi ts R esu l t Tr ue V a l ue L ab ID U ni ts 1300205-IBL1 3.86 pg of Hg 1300205-IBL2 4.24 pg of Hg 1300205-IBL3 4.10 pg of Hg 1300205-IBL4 4.15 pg of Hg 1300205-CAL1 10.00 9.71 pg of Hg 97% 1300205-CAL2 25.00 25.72 pg of Hg 1 03% 1300205-CAL3 100.0 99.09 pg of Hg 99% 1300205-CAL4 500.0 514.5 pg of Hg 1 03% 1300205-CAL5 2500 2434 pg of Hg 97% 1300205-CAL6 10000 10090 pg of Hg 1 01% 1300205-ICV1 1568 1564 pg of Hg 1 00% 85-115 1300205-CCB1 7.16 pg of Hg 1300205-CCV1 500.0 496.3 pg of Hg 99% 77-123 1300205-CCB2 5.67 pg of Hg 1300205-CCB3 5.10 pg of Hg 1300205-CCB4 5.16 pg of Hg 1300205-CCV2 500.0 495.6 pg of Hg 99% 77-123 1300205-CCB5 5.39 pg of Hg 1300205-CCV3 500.0 488.5 pg of Hg 98% 77-123 1300205-CCB6 4.87 pg of Hg 1300205-CCV4 500.0 489.8 pg of Hg 98% 77-123 1300205-CCB7 5.49 pg of Hg 1300205-CCV5 500.0 476.2 pg of Hg 95% 77-123 1300205-CCB8 4.32 pg of Hg 1300205-CCV6 500.0 477.9 pg of Hg 96% 77-123 1300205-CCB9 4.57 pg of Hg 1300205-CCV7 500.0 485.9 pg of Hg 97% 77-123 1300205-CCB A 4.64 pg of Hg 1300205-CCV8 500.0 478.9 pg of Hg 96% 77-123 1300205-CCBB 4.61 pg of Hg 1300205-CCV9 500.0 479.5 pg of Hg 96% 77-123 1300205-CCBC 4.63 pg of Hg 1300205-CCVA 500.0 484.4 pg of Hg 97% 77-123 1300205-CCBD 5.20 pg of Hg 1300205-CCVB 500.0 481.7 pg of Hg 96% 77-123 1300205-CCBE 4.53 pg of Hg 1300205-CCVC 500.0 481.2 pg of Hg 96% 77-123 1300205-CCBF 4.36 pg of Hg 1300205-CCVD 500.0 478.7 pg of Hg 96% 77-123 1300205-CCBG 5.19 pg of Hg

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comPro j ect ID: DUK-HV1201 PM: Tiffan yStilwater Client PM: Ja yPerkins Client PO: 141391



# Instrument Calibration

Sequence: 1300205 Method: EPA 1631 Instrument: THG-06 Date: 03/27/2013 Total Mercur y and Mercur y S p eciation b y CVAFS
Analyte: Hg RE C & Limi ts R esu l t Tr ue V a l ue L ab ID U ni ts 1300205-CCVE 500.0 477.9 pg of Hg 96% 77-123 1300205-CCBH 5.10 pg of Hg 1300205-CCVF 500.0 505.9 pg of Hg 1 01% 77-123 1300205-CCBI 4.60 pg of Hg 1300205-CCVG 500.0 509.4 pg of Hg 1 02% 77-123 1300205-CCBJ 5.14 pg of Hg

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comPro j ect ID: DUK-HV1201 PM: Tiffan yStilwater Client PM: Ja yPerkins Client PO: 141391



# Sample Containers

Lab ID: 1312005-01 Re p ort Matrix: Influent Sam p le T yp e: Sam p le Received: 03 / 19 / 2013 Sample: BioReactor 1 Inf Collected: 03 / 13 / 2013
Shi p . Cont. p H P-Lot Preservation Lot Size Containe r Des A 71666330 10 Cooler none n/a 500mL Bottle FLPE H g -T

Lab ID: 1312005-02 Re p ort Matrix: DIW Sam p le T yp e: Field Blank Received: 03 / 19 / 2013 Sample: Hg Blk BioReactor 1 Inf Collected: 03 / 13 / 2013
Shi p . Cont. p H P-Lot Preservation Lot Size Containe r Des A 71666330 10 Cooler none n/a 500mL Bottle FLPE H g -T

Lab ID: 1312005-03 Re p ort Matrix: Influent Sam p le T yp e: Sam p le Received: 03 / 19 / 2013 Sample: BioReactor 2 Inf Collected: 03 / 13 / 2013
Shi p . Cont. p H P-Lot Preservation Lot Size Containe r Des A 71666330 10 Cooler none n/a 500mL Bottle FLPE H g -T

Lab ID: 1312005-04 Re p ort Matrix: DIW Sam p le T yp e: Field Blank Received: 03 / 19 / 2013 Sample: Hg Blk BioReactor 2 Inf Collected: 03 / 13 / 2013
Shi p . Cont. p H P-Lot Preservation Lot Size Containe r Des A 71666330 10 Cooler none n/a 500mL Bottle FLPE H g -T

Lab ID: 1312005-05 Re p ort Matrix: Effluent Sam p le T yp e: Sam p le Received: 03 / 19 / 2013 Sample: BioReactor 2 Eff Collected: 03 / 13 / 2013
Shi p . Cont. p H P-Lot Preservation Lot Size Containe r Des A 71666330 10 Cooler none n/a 500mL Bottle FLPE H g -T

Lab ID: 1312005-06 Re p ort Matrix: DIW Sam p le T yp e: Field Blank Received: 03 / 19 / 2013 Sample: Hg Blk BioReactor 2 Eff Collected: 03 / 13 / 2013
Shi p . Cont. p H P-Lot Preservation Lot Size Containe r Des A 71666330 10 Cooler none n/a 500mL Bottle FLPE H g -T

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comPro j ect ID: DUK-HV1201 PM: Tiffan yStilwater Client PM: Ja yPerkins Client PO: 141391



# Shipping Containers

Cooler
Trackin g No: 1Z76654X0190322681 via UPS Tem p erature: 0.9 °C Coolant T yp e: Ice Descri p tion: Cooler Dama g ed in transit? No Returned to client? No Custod y seals p resent? N o Custod y seals intact? N o COC p resent? Ye s Received: March 19, 2013 9:20

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