### 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: J 13110187 Project Name: W WTS FGD-Routine 2013

Lab Contact: Jason C Perkins


### Date: 12/5/2013 Customer Address: 3195 Pine Hall Rd Customer Name(s): BIll K, Wayne C, and Melonie M

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 2013027575 BELEWS 11-Nov-13 7:30 AM W.WORKMAN FGD Purge Eff 2013027576 BELEWS 11-Nov-13 7:35 AM W.WORKMAN EQ Tank Eff 2013027577 BELEWS 11-Nov-13 7:40 AM W.WORKMAN BioReactor 1 Inf 2013027578 BELEWS 11-Nov-13 7:45 AM W.WORKMAN BioReactor 2 Inf 2013027579 BELEWS 11-Nov-13 7:50 AM W.WORKMAN BioReactor 2 Eff 2013027580 BELEWS 11-Nov-13 8:00 AM W.WORKMAN Filter Blk 2013027581 BELEWS 31-Oct-13 2:10 PM D. Baker 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: 

### 12/5/2013 Electronic Data Deliverable (EDD) Sent Separatel

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



### Order # J13110187

2013027575 Collection Date: 11-Nov-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) 6.0 mg-N/L EPA 353.2 11/15/2013 11:42 BGN9034 0.25 25
INORGANIC IONS BY IC Bromide 200 mg/L EPA 300.0 11/22/2013 17:02 JAHERMA 5 50 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 278 ug/L EPA 245.1 11/23/2013 10:34 DKJOHN2 5 100
TOTAL RECOVERABLE METALS BY ICP Boron (B) 229 mg/L EPA 200.7 11/14/2013 10:01 MHH7131 0.5 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 792 ug/L EPA 200.8 11/26/2013 14:02 DJSULL1 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 372 ug/L EPA 200.8 11/20/2013 12:03 DJSULL1 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 11/20/2013 12:03 DJSULL1 10 10 Chromium (Cr) 615 ug/L EPA 200.8 11/20/2013 12:03 DJSULL1 10 10 Copper (Cu) 259 ug/L EPA 200.8 11/20/2013 12:03 DJSULL1 10 10 Nickel (Ni) 382 ug/L EPA 200.8 11/20/2013 12:03 DJSULL1 10 10 Selenium (Se) 4990 ug/L EPA 200.8 11/20/2013 12:03 DJSULL1 20 20 Silver (Ag) < 10 ug/L EPA 200.8 11/20/2013 12:03 DJSULL1 10 10 Zinc (Zn) 478 ug/L EPA 200.8 11/20/2013 12:03 DJSULL1 10 10 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C



### 2013027576 Collection Date: 11-Nov-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) 134 ug/L EPA 245.1 11/23/2013 10:36 DKJOHN2 2.5 50
TOTAL RECOVERABLE METALS BY ICP Boron (B) 217 mg/L EPA 200.7 11/14/2013 10:05 MHH7131 0.5 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 461 ug/L EPA 200.8 11/26/2013 14:05 DJSULL1 10 10

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



### Order # J13110187

2013027576 Collection Date: 11-Nov-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) 238 ug/L EPA 200.8 11/20/2013 12:06 DJSULL1 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 11/20/2013 12:06 DJSULL1 10 10 Chromium (Cr) 368 ug/L EPA 200.8 11/20/2013 12:06 DJSULL1 10 10 Copper (Cu) 156 ug/L EPA 200.8 11/20/2013 12:06 DJSULL1 10 10 Nickel (Ni) 260 ug/L EPA 200.8 11/20/2013 12:06 DJSULL1 10 10 Selenium (Se) 3390 ug/L EPA 200.8 11/20/2013 12:06 DJSULL1 10 10 Silver (Ag) < 10 ug/L EPA 200.8 11/20/2013 12:06 DJSULL1 10 10 Zinc (Zn) 303 ug/L EPA 200.8 11/20/2013 12:06 DJSULL1 10 10



### 2013027577 Collection Date: 11-Nov-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) 5.4 mg-N/L EPA 353.2 11/15/2013 11:43 BGN9034 0.25 25 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 11/14/2013 10:10 MHH7131 0.5 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 495 ug/L EPA 200.8 11/26/2013 14:08 DJSULL1 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 11/20/2013 12:10 DJSULL1 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 11/20/2013 12:10 DJSULL1 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 11/20/2013 12:10 DJSULL1 10 10 Copper (Cu) < 10 ug/L EPA 200.8 11/20/2013 12:10 DJSULL1 10 10 Nickel (Ni) 13.2 ug/L EPA 200.8 11/20/2013 12:10 DJSULL1 10 10 Selenium (Se) 603 ug/L EPA 200.8 11/20/2013 12:10 DJSULL1 10 10 Silver (Ag) < 10 ug/L EPA 200.8 11/20/2013 12:10 DJSULL1 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 11/20/2013 12:10 DJSULL1 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 # J13110187

2013027578 Collection Date: 11-Nov-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) 191 mg/L EPA 200.7 11/14/2013 10:14 MHH7131 0.5 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 11/20/2013 12:13 DJSULL1 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 11/20/2013 12:13 DJSULL1 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 11/20/2013 12:13 DJSULL1 10 10 Copper (Cu) < 10 ug/L EPA 200.8 11/20/2013 12:13 DJSULL1 10 10 Nickel (Ni) < 10 ug/L EPA 200.8 11/20/2013 12:13 DJSULL1 10 10 Selenium (Se) < 10 ug/L EPA 200.8 11/20/2013 12:13 DJSULL1 10 10 Silver (Ag) < 10 ug/L EPA 200.8 11/20/2013 12:13 DJSULL1 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 11/20/2013 12:13 DJSULL1 10 10



### 2013027579 Collection Date: 11-Nov-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 11/15/2013 11:45 BGN9034 0.01 1
INORGANIC IONS BY IC Bromide 200 mg/L EPA 300.0 11/22/2013 17:21 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) 187 mg/L EPA 200.7 11/14/2013 10:18 MHH7131 0.5 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 5 ug/L EPA 200.8 11/20/2013 12:16 DJSULL1 5 5 Cadmium (Cd) < 5 ug/L EPA 200.8 11/20/2013 12:16 DJSULL1 5 5 Chromium (Cr) < 5 ug/L EPA 200.8 11/20/2013 12:16 DJSULL1 5 5 Copper (Cu) < 5 ug/L EPA 200.8 11/20/2013 12:16 DJSULL1 5 5 Nickel (Ni) < 5 ug/L EPA 200.8 11/20/2013 12:16 DJSULL1 5 5 Selenium (Se) 5.12 ug/L EPA 200.8 11/20/2013 12:16 DJSULL1 5 5 Silver (Ag) < 5 ug/L EPA 200.8 11/20/2013 12:16 DJSULL1 5 5 Zinc (Zn) < 5 ug/L EPA 200.8 11/20/2013 12:16 DJSULL1 5 5

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



### Order # J13110187

2013027579 Collection Date: 11-Nov-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 14000 mg/L SM2540C 11/19/2013 14:19 DSBAKE1 25 1



### 2013027580 Collection Date: 11-Nov-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 11/26/2013 13:52 B2 DJSULL1

1 1



### 2013027581 Collection Date: 31-Oct-13 2:10 PM 

### 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 11/14/2013 09:27 MHH7131 0.05 1
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 1 ug/L EPA 200.8 11/20/2013 11:42 DJSULL1 1 1 Cadmium (Cd) < 1 ug/L EPA 200.8 11/20/2013 11:42 DJSULL1 1 1 Chromium (Cr) < 1 ug/L EPA 200.8 11/20/2013 11:42 DJSULL1 1 1 Copper (Cu) < 1 ug/L EPA 200.8 11/20/2013 11:42 DJSULL1 1 1 Nickel (Ni) < 1 ug/L EPA 200.8 11/20/2013 11:42 DJSULL1 1 1 Selenium (Se) < 1 ug/L EPA 200.8 11/20/2013 11:42 DJSULL1 1 1 Silver (Ag) < 1 ug/L EPA 200.8 11/20/2013 11:42 DJSULL1 1 1 Zinc (Zn) < 1 ug/L EPA 200.8 11/20/2013 11:42 DJSULL1 1 1



### Qualifiers:
B2 Target analyte was detected in blank(s) at a concentration greater than 1⁄2 the reporting limit but less than the reporting limit. Analyte concentration in sample is valid and may be used for compliance purposes.

## December 3 , 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 & Flex Fuel & DSI) (LIMS#J13110187)

Mr. Pe rkins , Attached is the report associated with four (4 ) aqueous samples submitted for total mercury and selenium speciation analysis on November 13 , 2013. The samples were received in a sealed cooler at 0.1 ° C on November 14 , 2013. Selenium speciation analysis was performed via ionchromatography inductively coupled plasma collision reaction cell mass spectrometry (IC-ICPCRC -MS). Mercury quantitation was performed via cold vapor inductively coupled plasma mass spectrometry (CV-ICP-MS). Any issues associ ated with the analysis are addressed in the following report. If you have any questions, please feel free to contact me at your convenience.

Sincerely,

Jeremy Maute Project Coordinator 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 & Flex Fuel & DSI) (LIMS# J13110187)
December 3 , 2013

1. Sample Reception Four (4 ) aqueous samples were submitted for selenium speciation analysis on November 13 , 2013. Three (3 ) additional samples were submitted for total mercury quantitation. All samples were received in acceptable condition on November 14 , 2013 in a sealed container at 0.1 ° 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). Two 40 mL glass vials were received that listed a LIMS ID of 2013027570. Both bottles were labeled with a sample ID of BioReactor 2 Inf and both bottles listed a collection date/time of (11/8/13, 0955). These descriptive parameters match the BioReactor 2 Inf sample entry on the chain-of-custody (COC) form associated with LIMS ID J13110185. There was no way to discern between the two samples visibly. The COC form associated with LIMS ID J13110187 was also present in the cooler and the COC indicated that the client sample (requesting total mercury analysis) identified as (2013027578, BioReactor 2 Inf, 11/11/13, 0745) should be present. A 40 mL glass container with the client sampl e BioReactor 2 Inf (LIMS ID 2013027578) was absent from the cooler. The two identically labeled samples requesting total mercury analysis were labeled internally by the laboratory sample reception staff at Applied Speciation as (2013027570 -BioReactor 2 Inf A) and

## (2013027570 -BioReactor 2 Inf B). The samples were analyzed for total mercury yielding

similar values, 0.0363 μ g/L and 0.0296 μ g/L, respectively. The client was informed of this sample ID issue. Si nce the total mercury results were similar in quantity, Applied Speciation was directed to report the total mercury result for (2013027570-BioReactor 2 Inf A) in the report associated with LIMS ID J13110185. Applied Speciation was instructed to report the total mercury result for (2013027570- BioReactor 2 Inf B) in the report associated with LIMS ID J13110187.

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 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. 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 November 18 , 2013 . Aliquots of each sample are reacted with a reductant in -line and transported to a gas-liquid separator. The volatile elemental mercury that is

## formed is then swept by a stream of argon gas 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 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 November 19, 2013. 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, andionization. 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. 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,

Jeremy Maute Project Coordinator 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 1280 30.5 13.3 4.5 ND (< 1.7) 3.4 (1) BioReactor 1 Inf 0.0765 489 19.6 ND (< 0.53) 6.40 ND (< 0.43) 1.20 (1) BioReactor 2 Inf 0.0296 NR NR NR NR NR NR BioReactor 2 Eff 0.0054 ND (< 0.47) ND (< 0.30) ND (< 0.53) ND (< 0.43) ND (< 0.43) 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: Jeremy Maute Applied Speciation and Consulting, LLC Total Mercury & Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS (Bi-Monthly & Flex Fuel & DSI) Contact: Jay Perkins

Date: December 3, 2013 LIMS #J13110187

### Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 5x eMDL 250x eMDL 1000x Hg -0.0003 -0.0002 -0.0007 -0.0004 -0.0004 0.0002 0.0001 0.0006

- - Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.002

- 0.47 1.9 Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.001

- 0.30 1.2 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.002

- 0.53 2.1 MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.002

- 0.43 1.7 SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.002

- 0.43 1.7 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 1626 103.7 Se(IV) LCS 9.57 9.28 96.9 Se(VI) LCS 9.48 9.22 97.3 SeCN LCS 8.92 8.55 95.9 MeSe(IV) LCS 6.47 6.23 96.3 SeMe LCS 9.32 8.84 94.8 Applied Speciation and Consulting, LLC Total Mercury & Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS (Bi-Monthly & Flex Fuel & DSI) Contact: Jay Perkins LIMS #J13110187 Date: December 3, 2013 Report Generated by: Jeremy Maute

### Quality Control Summary - Matrix Duplicates

Analyte (μg/L) Sample ID Rep 1 Rep 2 Mean RPD Hg Batch QC 0.1934 0.1955 0.1945 1.1 Se(IV) Batch QC ND (< 0.47) ND (< 0.47) NC NC Se(VI) Batch QC ND (< 0.30) ND (< 0.30) NC NC SeCN Batch QC ND (< 0.53) ND (< 0.53) NC NC MeSe(IV) Batch QC ND (< 0.43) ND (< 0.43) NC NC SeMe Batch QC ND (< 0.43) ND (< 0.43) 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 2.347 107.6 2.000 2.320 106.3 1.2 Se(IV) Batch QC 1390 1336 96.1 1390 1344 96.7 0.6 Se(VI) Batch QC 1261 1176 93.3 1261 1190 94.3 1.1 SeCN Batch QC 1144 1026 89.7 1144 1043 91.2 1.7 Applied Speciation and Consulting, LLC Total Mercury & Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS (Bi-Monthly & Flex Fuel & DSI) Contact: Jay Perkins LIMS #J13110187 Date: December 3, 2013 Report Generated by: Jeremy Maute