### 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: J13050477 Project Name: WWTS FGD-Routine 2013

L ab Contact: Jason C Perkins


## Date: 6/14/2013 Customer Address: 3195 Pine Hall Rd Customer Name(s): Bill Kennedy, Wayne Chapman, Melonie Martin

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 2013012163 BELEWS 24-May-13 7:30 AM TRAVIS THORNTON FGD Purge Eff 2013012164 BELEWS 24-May-13 7:35 AM TRAVIS THORNTON EQ Tank Eff 2013012165 BELEWS 24-May-13 7:40 AM TRAVIS THORNTON BioReactor 1 Inf 2013012166 BELEWS 24-May-13 7:45 AM TRAVIS THORNTON BioReactor 2 Inf 2013012167 BELEWS 24-May-13 7:50 AM TRAVIS THORNTON BioReactor 2 Eff 2013012168 BELEWS 24-May-13 8:00 AM TRAVIS THORNTON Filter Blk 2013012169 BELEWS 21-May-13 10:30 AM CPK TRIP BLANK 7 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. 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: 

### 6/14/2013 Electronic Data Deliverable (EDD) Sent Separately

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



## Order # J13050477

2013012163 Collection Date: 24-May-13 7:30 AM 

## Site: FGD Purge Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

## Sample #:

Analyst DF NITRITE + NITRATE (COLORIMETRIC) Nitrite + Nitrate (Colorimetric) 16 mg-N/L EPA 353.2 06/03/2013 12:06 BGN9034 0.1 10
INORGANIC IONS BY IC Bromide 110 mg/L EPA 300.0 06/03/2013 16:33 JAHERMA 5 50 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 239 ug/L EPA 245.1 05/31/2013 12:59 AGIBBS 5 100
TOTAL RECOVERABLE METALS BY ICP Boron (B) 226 mg/L EPA 200.7 06/07/2013 12:12 DJSULL1 0.5 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 298 ug/L EPA 200.8 06/12/2013 11:33 KRICHAR 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 207 ug/L EPA 200.8 06/12/2013 14:04 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 06/12/2013 14:04 KRICHAR 10 10 Chromium (Cr) 259 ug/L EPA 200.8 06/12/2013 14:04 KRICHAR 10 10 Copper (Cu) 119 ug/L EPA 200.8 06/12/2013 14:04 KRICHAR 10 10 Nickel (Ni) 243 ug/L EPA 200.8 06/12/2013 14:04 KRICHAR 10 10 Selenium (Se) 3180 ug/L EPA 200.8 06/12/2013 14:04 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 06/12/2013 14:04 KRICHAR 10 10 Zinc (Zn) 262 ug/L EPA 200.8 06/12/2013 14:04 KRICHAR 10 10 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C



## 2013012164 Collection Date: 24-May-13 7:35 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) 215 ug/L EPA 245.1 05/31/2013 13:01 AGIBBS 2.5 50
TOTAL RECOVERABLE METALS BY ICP Boron (B) 215 mg/L EPA 200.7 06/07/2013 12:15 DJSULL1 0.5 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 234 ug/L EPA 200.8 06/12/2013 11:37 KRICHAR 10 10

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



## Order # J13050477

2013012164 Collection Date: 24-May-13 7:35 AM 

## Site: EQ Tank Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

## Sample #:

Analyst DF TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 202 ug/L EPA 200.8 06/12/2013 14:08 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 06/12/2013 14:08 KRICHAR 10 10 Chromium (Cr) 248 ug/L EPA 200.8 06/12/2013 14:08 KRICHAR 10 10 Copper (Cu) 114 ug/L EPA 200.8 06/12/2013 14:08 KRICHAR 10 10 Nickel (Ni) 226 ug/L EPA 200.8 06/12/2013 14:08 KRICHAR 10 10 Selenium (Se) 3120 ug/L EPA 200.8 06/12/2013 14:08 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 06/12/2013 14:08 KRICHAR 10 10 Zinc (Zn) 242 ug/L EPA 200.8 06/12/2013 14:08 KRICHAR 10 10



## 2013012165 Collection Date: 24-May-13 7:40 AM 

## Site: BioReactor 1 Inf Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

## Sample #:

Analyst DF NITRITE + NITRATE (COLORIMETRIC) Nitrite + Nitrate (Colorimetric) 16 mg-N/L EPA 353.2 06/03/2013 12:07 BGN9034 0.1 10 Mercury by EPA 200.8 - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete ug/l Vendor Method V_AS&C
TOTAL RECOVERABLE METALS BY ICP Boron (B) 191 mg/L EPA 200.7 06/07/2013 12:19 DJSULL1 0.5 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 177 ug/L EPA 200.8 06/12/2013 11:40 KRICHAR 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 06/12/2013 14:11 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 06/12/2013 14:11 KRICHAR 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 06/12/2013 14:11 KRICHAR 10 10 Copper (Cu) < 10 ug/L EPA 200.8 06/12/2013 14:11 KRICHAR 10 10 Nickel (Ni) < 10 ug/L EPA 200.8 06/12/2013 14:11 KRICHAR 10 10 Selenium (Se) 167 ug/L EPA 200.8 06/12/2013 14:11 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 06/12/2013 14:11 KRICHAR 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 06/12/2013 14:11 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 # J13050477

2013012166 Collection Date: 24-May-13 7:45 AM 

## Site: BioReactor 2 Inf Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

## Sample #:

Analyst DF Mercury by EPA 200.8 - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete ug/l Vendor Method V_AS&C
TOTAL RECOVERABLE METALS BY ICP Boron (B) 192 mg/L EPA 200.7 06/07/2013 12:23 DJSULL1 0.5 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 06/12/2013 14:15 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 06/12/2013 14:15 KRICHAR 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 06/12/2013 14:15 KRICHAR 10 10 Copper (Cu) < 10 ug/L EPA 200.8 06/12/2013 14:15 KRICHAR 10 10 Nickel (Ni) < 10 ug/L EPA 200.8 06/12/2013 14:15 KRICHAR 10 10 Selenium (Se) 13.9 ug/L EPA 200.8 06/12/2013 14:15 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 06/12/2013 14:15 KRICHAR 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 06/12/2013 14:15 KRICHAR 10 10



## 2013012167 Collection Date: 24-May-13 7:50 AM 

## Site: BioReactor 2 Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

## Sample #:

Analyst DF NITRITE + NITRATE (COLORIMETRIC) Nitrite + Nitrate (Colorimetric) < 0.01 mg-N/L EPA 353.2 06/03/2013 12:08 BGN9034 0.01 1
INORGANIC IONS BY IC Bromide 89 mg/L EPA 300.0 06/03/2013 16:52 JAHERMA 5 50 Mercury by EPA 200.8 - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete ug/l Vendor Method V_AS&C
TOTAL RECOVERABLE METALS BY ICP Boron (B) 182 mg/L EPA 200.7 06/07/2013 12:26 DJSULL1 0.5 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 5 ug/L EPA 200.8 06/12/2013 14:18 KRICHAR 5 5 Cadmium (Cd) < 5 ug/L EPA 200.8 06/12/2013 14:18 KRICHAR 5 5 Chromium (Cr) < 5 ug/L EPA 200.8 06/12/2013 14:18 KRICHAR 5 5 Copper (Cu) < 5 ug/L EPA 200.8 06/12/2013 14:18 KRICHAR 5 5 Nickel (Ni) < 5 ug/L EPA 200.8 06/12/2013 14:18 KRICHAR 5 5 Selenium (Se) < 5 ug/L EPA 200.8 06/12/2013 14:18 KRICHAR 5 5 Silver (Ag) < 5 ug/L EPA 200.8 06/12/2013 14:18 KRICHAR 5 5 Zinc (Zn) < 5 ug/L EPA 200.8 06/12/2013 14:18 KRICHAR 5 5

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



## Order # J13050477

2013012167 Collection Date: 24-May-13 7:50 AM 

## Site: BioReactor 2 Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

## Sample #:

Analyst DF SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C
TOTAL DISSOLVED SOLIDS TDS 15000 mg/L SM2540C 06/03/2013 15:03 JDTALLE 25 1



## 2013012168 Collection Date: 24-May-13 8:00 AM 

## Site: Filter Blk Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

## Sample #:

Analyst DF DISSOLVED METALS BY ICP-MS Selenium (Se) < 1 ug/L EPA 200.8 06/12/2013 10:42 KRICHAR 1 1



## 2013012169 Collection Date: 21-May-13 10:30 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 06/07/2013 11:51 DJSULL1 0.05 1
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 1 ug/L EPA 200.8 06/12/2013 13:44 KRICHAR 1 1 Cadmium (Cd) < 1 ug/L EPA 200.8 06/12/2013 13:44 KRICHAR 1 1 Chromium (Cr) < 1 ug/L EPA 200.8 06/12/2013 13:44 KRICHAR 1 1 Copper (Cu) < 1 ug/L EPA 200.8 06/12/2013 13:44 KRICHAR 1 1 Nickel (Ni) < 1 ug/L EPA 200.8 06/12/2013 13:44 KRICHAR 1 1 Selenium (Se) < 1 ug/L EPA 200.8 06/12/2013 13:44 KRICHAR 1 1 Silver (Ag) < 1 ug/L EPA 200.8 06/12/2013 13:44 KRICHAR 1 1 Zinc (Zn) < 1 ug/L EPA 200.8 06/12/2013 13:44 KRICHAR 1 1

# June 1 1 , 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 Routine 2013) (LIMS #J13050477)

Mr. Perkins, Attached is the report associated with four (4 ) aqueous samples submitted for total mercury and selenium speciation analysis on May 29 , 2013. The samples were received in a sealed cooler at -0. 3 ° C on May 31 , 2013. Selenium speciation analysis was performed via ion chromatography inductively coupled plasma collision reaction cell mass spectrometry (IC-ICP- CRC -MS). Mercury quantitation was performed via cold vapor inductively coupled plasma mass spectrometry (CV-ICP-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 Routine 2013) (LIMS #J13050477)
June 1 1 2013

1. Sample Reception Three (3 ) aqueous samples in125mL HDPE bottles (provided by Applied Speciation and Consulting) were submitted for selenium speciation analysis on May 29 , 2013. Three (3 ) additional samples in 40ml borosilicate glass bottles (p rovided by Applied Speciation and Consulting) were submitted for total mercury quantitation. All samples were received in acceptable condition on May 31 , 2013 in a sealed container at -0.3 ° C. All samples were received in a laminar flow clean hood, void of trace metals contamination and ultra-violet radiation, and were designated discrete sample identifiers. The 40mL borosilicate glass vials submitted for total mercury were preserved with bromine monochloride (BrCl) solution. The resulting samples were stored in a secure polyethylene container, known to be free from trace metals contamination, until the analyses could be performed. An aliquot of each sample requiring selenium speciation evaluation was filtered (0.45μm) and each filtrate w as stored in a secure, monitored cryofreezer (maintained at a temperature of -80 ° 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. Total Mercury Quantitation by CV -ICP- MS All samples and preparation blanks for total mercury quantitation were preserved with 2% (v/v) BrCl. The resulting samples were analyzed for mercury via cold vapor inductively coupled plasma mass spectrometry (CV

ICP-MS).

# 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 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 in strument 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. Total Mercury Quantitation by CV -ICP- MS The sample fractions for total mercury quantitation were analyzed by cold vapor inductively coupled plasma mass spectrometry (CV-ICP- MS ) on May 31 , 2013 . Aliquots of each sample are reacted with a reductant in-line and transported to a gas- liq uid separator. The volatile elemental mercury that is formed isthen swept by a stream of argon gas into a radio frequency (RF) plasma where energytransfer processes cause desolvation, atomization, and ionization. The ions are extracted from the plasma through a differentially-pumped vacuum interface and separated on the basis of their mass- to -charge ratio (m/z) by a mass spectrometer. A solid-state detector detects ions transmitted through the mass analyzer and the resulting current is processed by a data handling system. 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 June 6-7, 2013. An aliquot 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 these samples were within acceptance limits. A miscommunication between the ion chromatography unit and the eluent pump caused a delay in the eluent gradient during the analysis of the matrix spike performed on the sample identified as BioReactor 2 Eff. Consequently the retention time for the selenocyanate peak in the matrix spike duplicate sample was shifted to a larger value (from approximately 10.2 minutes to 11.6 minutes). This shift was confirmed by measurement of an internal standard (roxarsone), which typically falls within the same late eluting retention time range. The roxarsone peak experienced a similar retention time shift due to the delay in the eluent gradient. The selenocyanate peak occurring at 11.6 minutes in the matrix spike sample was integrated and the value produced an acceptable selenocyanate recovery. 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. The eMDL for mercury has been calculated using the standard deviation of the preparation blanks preserved and analyzed concurrently with the submitted samples. 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 Total Hg Se(IV) Se(VI) SeCN MeSe(IV) SeMe Unknown Se Species (n) FGD Purge Eff NR 235 68.6 ND (< 5.0) ND (< 5.6) ND (< 5.6) 0 (0) BioReactor 1 Inf 0.0339 71.0 102 ND (< 1.2) 3.6 ND (< 1.4) 0 (0) BioReactor 2 Inf 0.0158 NR NR NR NR NR NR BioReactor 2 Eff 0.0049 ND (< 1.3) ND (< 1.6) ND (< 1.2) ND (< 1.4) ND (< 1.4) 0 (0) All results reflect the applied dilution and are reported in μg/L NR = Analysis not requested 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 Total Mercury & Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS (Bi-Monthly Routine 2013)

Contact: Jay Perkins

Date: June 11, 2013 LIMS #J13050477

### Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 5x eMDL 250x eMDL 1000x Hg 0.0007 0.0016 0.0016 0.0016 0.0014 0.0005 0.0003 0.0014

- - Se(IV) 0.000 0.000 0.144 0.000 0.036 0.072 0.005

- 1.3 5.4 Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.006

- 1.6 6.4 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.005

- 1.2 5.0 MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.006

- 1.4 5.6 SeMe 0.000 0.000 0.049 0.000 0.012 0.024 0.006

- 1.4 5.6 eMDL = Estimated Method Detection Limit *Please see narrative regarding eMDL calculations

Quality Control Summary - Certified Reference Materials Analyte (μg/L) CRM True Value Result Recovery Hg NIST 1641d 1568 1580 100.8 Se(IV) LCS 4.79 5.23 109.2 Se(VI) LCS 4.74 4.87 102.8 SeCN LCS 4.46 4.75 106.6 MeSe(IV) LCS 3.24 3.37 104.1 SeMe LCS 4.66 4.56 97.9 Applied Speciation and Consulting, LLC Total Mercury & Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS (Bi-Monthly Routine 2013)

Contact: Jay Perkins LIMS #J13050477
Date: June 11, 2013 Report Generated by: Russell Gerads

### Quality Control Summary - Matrix Duplicates

Analyte (μg/L) Sample ID Rep 1 Rep 2 Mean RPD Hg Batch QC 0.0682 0.0671 0.0677 1.6 Se(IV) BioReactor 2 Eff ND (< 1.3) ND (< 1.3) NC NC Se(VI) BioReactor 2 Eff ND (< 1.6) ND (< 1.6) NC NC SeCN BioReactor 2 Eff ND (< 1.2) ND (< 1.2) NC NC MeSe(IV) BioReactor 2 Eff ND (< 1.4) ND (< 1.4) NC NC SeMe BioReactor 2 Eff ND (< 1.4) ND (< 1.4) 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 Hg Batch QC 2.000 2.159 104.6 2.000 2.169 105.1 0.4 Se(IV) BioReactor 2 Eff 1390 1535 110.4 1390 1530 110.1 0.3 Se(VI) BioReactor 2 Eff 1261 1377 109.2 1261 1358 107.7 1.4 SeCN * BioReactor 2 Eff 1144 1232 107.7 1144 1222 106.9 0.8 * Please see narrative regarding MSD selenocyanate result. Applied Speciation and Consulting, LLC Total Mercury & Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS (Bi-Monthly Routine 2013)

Contact: Jay Perkins LIMS #J13050477
Date: June 11, 2013 Report Generated by: Russell Gerads