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: J12110008

Lab Contact: Jason C Perkins
Date: 11/19/2012 Customer Address: 3195 Pine Hall Rd Customer Name(s): Bill K, Wayne C, Melonie M, and Tom J

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.

### Sample ID's & Descriptions:

Sample ID Plant/Station Collection Date and Time Collected By Sample Description 2012023312 BELEWS 31-Oct-12 1:20 PM TRAVIS THORNTON FGD Purge Eff 2012023313 BELEWS 31-Oct-12 7:30 AM TRAVIS THORNTON EQ TANK 2012023314 BELEWS 31-Oct-12 7:35 AM TRAVIS THORNTON BIOREACTOR 1 INF 2012023315 BELEWS 31-Oct-12 7:40 AM TRAVIS THORNTON biOREACTOR 1 INF HG BLK 2012023316 BELEWS 31-Oct-12 7:45 AM TRAVIS THORNTON BIOREACTOR 2 INF. 2012023317 BELEWS 31-Oct-12 7:50 AM TRAVIS THORNTON BIOREACTOR 2 INF. HG BLANK 2012023318 BELEWS 31-Oct-12 7:55 AM TRAVIS THORNTON BIOREACTOR 2 EFF. 2012023319 BELEWS 31-Oct-12 8:00 AM TRAVIS THORNTON BIOREACTOR 2 EFF. HG BLANK 2012023320 BELEWS 31-Oct-12 8:05 AM TRAVIS THORNTON FILTER BLANK 9 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: 11/19/2012 Electronic Data Deliverable (EDD) Sent Separately

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



### Order # J12110008

2012023312 Collection Date: 31-Oct-12 1:20 PM Site: FGD Purge Eff Matrix: OTHER

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

Analyst DF INORGANIC IONS BY IC Bromide 83 mg/L EPA 300.0 11/12/2012 18:52 JAHERMA 5 50 Chloride 5700 mg/L EPA 300.0 11/12/2012 18:52 JAHERMA 100 1000 Sulfate 1100 mg/L EPA 300.0 11/12/2012 18:52 JAHERMA 100 1000 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 106 ug/L EPA 245.1 11/08/2012 14:05 AGIBBS 5 100
DISSOLVED METALS BY ICP Manganese (Mn) 5.07 mg/L EPA 200.7 11/05/2012 12:54 DJSULL1 0.05 10
TOTAL RECOVERABLE METALS BY ICP Boron (B) 137 mg/L EPA 200.7 11/09/2012 12:43 DJSULL1 0.5 10 Calcium (Ca) 3440 mg/L EPA 200.7 11/09/2012 12:43 DJSULL1 0.1 10 Iron (Fe) 92.5 mg/L EPA 200.7 11/09/2012 12:43 DJSULL1 0.1 10 Magnesium (Mg) 537 mg/L EPA 200.7 11/09/2012 12:43 DJSULL1 0.05 10 Manganese (Mn) 5.68 mg/L EPA 200.7 11/09/2012 12:43 DJSULL1 0.05 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 228 ug/L EPA 200.8 11/09/2012 14:40 KRICHAR 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 201 ug/L EPA 200.8 11/09/2012 13:55 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 11/09/2012 13:55 KRICHAR 10 10 Chromium (Cr) 220 ug/L EPA 200.8 11/09/2012 13:55 KRICHAR 10 10 Copper (Cu) 153 ug/L EPA 200.8 11/09/2012 13:55 KRICHAR 10 10 Nickel (Ni) 193 ug/L EPA 200.8 11/09/2012 13:55 KRICHAR 10 10 Selenium (Se) 4480 ug/L EPA 200.8 11/09/2012 13:55 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 11/09/2012 13:55 KRICHAR 10 10 Zinc (Zn) 308 ug/L EPA 200.8 11/09/2012 13:55 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 11/12/2012 16:32 SWILLI3 200 1
TOTAL SUSPENDED SOLIDS TSS 3500 mg/L SM2540D 11/05/2012 10:56 SWILLI3 250 1

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



### Order # J12110008

2012023313 Collection Date: 31-Oct-12 7:30 AM Site: EQ TANK Matrix: OTHER

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

Analyst DF MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 117 ug/L EPA 245.1 11/08/2012 14:07 AGIBBS 2.5 50
DISSOLVED METALS BY ICP Manganese (Mn) 4.35 mg/L EPA 200.7 11/05/2012 12:58 DJSULL1 0.05 10
TOTAL RECOVERABLE METALS BY ICP Boron (B) 133 mg/L EPA 200.7 11/09/2012 12:47 DJSULL1 0.5 10 Calcium (Ca) 3460 mg/L EPA 200.7 11/09/2012 12:47 DJSULL1 0.1 10 Iron (Fe) 91.4 mg/L EPA 200.7 11/09/2012 12:47 DJSULL1 0.1 10 Magnesium (Mg) 542 mg/L EPA 200.7 11/09/2012 12:47 DJSULL1 0.05 10 Manganese (Mn) 5.48 mg/L EPA 200.7 11/09/2012 12:47 DJSULL1 0.05 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 188 ug/L EPA 200.8 11/09/2012 14:43 KRICHAR 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 201 ug/L EPA 200.8 11/09/2012 13:58 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 11/09/2012 13:58 KRICHAR 10 10 Chromium (Cr) 218 ug/L EPA 200.8 11/09/2012 13:58 KRICHAR 10 10 Copper (Cu) 144 ug/L EPA 200.8 11/09/2012 13:58 KRICHAR 10 10 Nickel (Ni) 192 ug/L EPA 200.8 11/09/2012 13:58 KRICHAR 10 10 Selenium (Se) 4660 ug/L EPA 200.8 11/09/2012 13:58 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 11/09/2012 13:58 KRICHAR 10 10 Zinc (Zn) 284 ug/L EPA 200.8 11/09/2012 13:58 KRICHAR 10 10

2012023314 Collection Date: 31-Oct-12 7:35 AM Site: 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
DISSOLVED METALS BY ICP Manganese (Mn) 0.950 mg/L EPA 200.7 11/05/2012 13:02 DJSULL1 0.05 10
TOTAL RECOVERABLE METALS BY ICP Boron (B) 127 mg/L EPA 200.7 11/09/2012 12:51 DJSULL1 0.5 10 Calcium (Ca) 2940 mg/L EPA 200.7 11/09/2012 12:51 DJSULL1 0.1 10 Iron (Fe) < 0.1 mg/L EPA 200.7 11/09/2012 12:51 DJSULL1 0.1 10 Magnesium (Mg) 514 mg/L EPA 200.7 11/09/2012 12:51 DJSULL1 0.05 10 Manganese (Mn) 1.01 mg/L EPA 200.7 11/09/2012 12:51 DJSULL1 0.05 10

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



### Order # J12110008

2012023314 Collection Date: 31-Oct-12 7:35 AM Site: BIOREACTOR 1 INF Matrix: OTHER

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

Analyst DF DISSOLVED METALS BY ICP-MS Selenium (Se) 110 ug/L EPA 200.8 11/09/2012 14:46 KRICHAR 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 11/09/2012 14:01 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 11/09/2012 14:01 KRICHAR 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 11/09/2012 14:01 KRICHAR 10 10 Copper (Cu) < 10 ug/L EPA 200.8 11/09/2012 14:01 KRICHAR 10 10 Nickel (Ni) 14.7 ug/L EPA 200.8 11/09/2012 14:01 KRICHAR 10 10 Selenium (Se) 102 ug/L EPA 200.8 11/09/2012 14:01 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 11/09/2012 14:01 KRICHAR 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 11/09/2012 14:01 KRICHAR 10 10 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C

2012023315 Collection Date: 31-Oct-12 7:40 AM Site: biOREACTOR 1 INF HG BLK 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

2012023316 Collection Date: 31-Oct-12 7:45 AM Site: 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
DISSOLVED METALS BY ICP Manganese (Mn) 1.11 mg/L EPA 200.7 11/05/2012 13:06 DJSULL1 0.05 10
TOTAL RECOVERABLE METALS BY ICP Boron (B) 123 mg/L EPA 200.7 11/09/2012 12:55 DJSULL1 0.5 10 Calcium (Ca) 2870 mg/L EPA 200.7 11/09/2012 12:55 DJSULL1 0.1 10 Iron (Fe) < 0.1 mg/L EPA 200.7 11/09/2012 12:55 DJSULL1 0.1 10 Magnesium (Mg) 499 mg/L EPA 200.7 11/09/2012 12:55 DJSULL1 0.05 10 Manganese (Mn) 1.13 mg/L EPA 200.7 11/09/2012 12:55 DJSULL1 0.05 10

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



### Order # J12110008

2012023316 Collection Date: 31-Oct-12 7:45 AM Site: BIOREACTOR 2 INF. Matrix: OTHER

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

Analyst DF DISSOLVED METALS BY ICP-MS Selenium (Se) 12.5 ug/L EPA 200.8 11/09/2012 14:49 KRICHAR 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 11/09/2012 14:04 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 11/09/2012 14:04 KRICHAR 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 11/09/2012 14:04 KRICHAR 10 10 Copper (Cu) < 10 ug/L EPA 200.8 11/09/2012 14:04 KRICHAR 10 10 Nickel (Ni) < 10 ug/L EPA 200.8 11/09/2012 14:04 KRICHAR 10 10 Selenium (Se) < 10 ug/L EPA 200.8 11/09/2012 14:04 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 11/09/2012 14:04 KRICHAR 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 11/09/2012 14:04 KRICHAR 10 10 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C

2012023317 Collection Date: 31-Oct-12 7:50 AM Site: BIOREACTOR 2 INF. HG BLANK 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

2012023318 Collection Date: 31-Oct-12 7:55 AM Site: BIOREACTOR 2 EFF. Matrix: OTHER

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

Analyst DF INORGANIC IONS BY IC Bromide 81 mg/L EPA 300.0 11/12/2012 19:11 JAHERMA 5 50 Chloride 6000 mg/L EPA 300.0 11/12/2012 19:11 JAHERMA 100 1000 Sulfate 1200 mg/L EPA 300.0 11/12/2012 19:11 JAHERMA 100 1000 MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND
DISSOLVED METALS BY ICP Manganese (Mn) 1.35 mg/L EPA 200.7 11/05/2012 13:10 DJSULL1 0.05 10

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



### Order # J12110008

2012023318 Collection Date: 31-Oct-12 7:55 AM Site: BIOREACTOR 2 EFF. Matrix: OTHER

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

Analyst DF TOTAL RECOVERABLE METALS BY ICP Boron (B) 121 mg/L EPA 200.7 11/09/2012 12:59 DJSULL1 0.5 10 Calcium (Ca) 3030 mg/L EPA 200.7 11/09/2012 12:59 DJSULL1 0.1 10 Iron (Fe) < 0.1 mg/L EPA 200.7 11/09/2012 12:59 DJSULL1 0.1 10 Magnesium (Mg) 511 mg/L EPA 200.7 11/09/2012 12:59 DJSULL1 0.05 10 Manganese (Mn) 1.41 mg/L EPA 200.7 11/09/2012 12:59 DJSULL1 0.05 10
DISSOLVED METALS BY ICP-MS Selenium (Se) < 5 ug/L EPA 200.8 11/09/2012 14:52 KRICHAR 5 5
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 5 ug/L EPA 200.8 11/09/2012 14:07 KRICHAR 5 5 Cadmium (Cd) < 5 ug/L EPA 200.8 11/09/2012 14:07 KRICHAR 5 5 Chromium (Cr) < 5 ug/L EPA 200.8 11/09/2012 14:07 KRICHAR 5 5 Copper (Cu) < 5 ug/L EPA 200.8 11/09/2012 14:07 KRICHAR 5 5 Nickel (Ni) < 5 ug/L EPA 200.8 11/09/2012 14:07 KRICHAR 5 5 Selenium (Se) 5.48 ug/L EPA 200.8 11/09/2012 14:07 KRICHAR 5 5 Silver (Ag) < 5 ug/L EPA 200.8 11/09/2012 14:07 KRICHAR 5 5 Zinc (Zn) < 5 ug/L EPA 200.8 11/09/2012 14:07 KRICHAR 5 5 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C

2012023319 Collection Date: 31-Oct-12 8:00 AM Site: BIOREACTOR 2 EFF. HG BLANK 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

2012023320 Collection Date: 31-Oct-12 8:05 AM Site: FILTER BLANK Matrix: OTHER

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

Analyst DF DISSOLVED METALS BY ICP Manganese (Mn) < 0.005 mg/L EPA 200.7 11/05/2012 12:11 DJSULL1 0.005 1
DISSOLVED METALS BY ICP-MS Selenium (Se) < 1 ug/L EPA 200.8 11/09/2012 14:56 KRICHAR 1 1

### November 9 , 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 Creek (Flex Fuel) - WW (LIMS # J12110008 )

Dear Mr. Perkins, Attached is the report associated with four (4 ) aqueous samples submitted for selenium speciation analysis on November 1, 2012

. The samples were received in a sealed cooler at -0. 2 ° C on November 2, 2012

. Selenium speciation analysis was performed via ionchromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICPDRC-MS). Any issues associated with the analysis are addressed in the following report. If you have any questions, please feel free to contact me at your convenience.

Sincerely,

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 Creek (Flex Fuel) - WW (LIMS # J12110008)

November 9 , 2012

1. Sample Reception Four (4 ) aqueous samples in125mL HDPE bottles (provided by Applied Speciation and Consulting) were submitted for selenium speciation analysi s on November 1, 2012 . The samples were received on November 2 , 201 2 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 dynamic reaction cell mass spectrometry (IC-ICP-DRC-MS).

2. Sample Preparation All sample preparation is performed in laminar flow clean hoods known to be free from trace metals contamination. All applied water for dilutions and sample preservatives are monitored for contamination to account for any biases associated with the sample results. Selenium Speciation Analysis by IC -ICP-DRC

- MS Prior to analysis, an aliquot of each sample was filtered with a syringe filter (0.45μm) and injected directly into 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-DRC

- MS Eachsample for selenium speciation analysis w as analyzed by ion chromatography inductively coupled plasma dynamic reactio n cell mass spectrometry (IC-ICP-DRC-MS) on November 8 , 2012

. Analiquot of each sample is injected onto an anion exchange column and mobilized by a basic (pH > 7) gradient. The eluting selenium species are then introduced into a radio frequency (RF) plasma where energy-transfer processes cause desolvation, atomization, and ionization. The ions are extracted from the plasma through a differentially-pumped vacuum interface and travel through a pressurized chamber (DRC) containing a reaction gas which pref erentially 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 th e 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 118 78.5 ND (<2.5) 4.0 ND (<3.2) 0.0 (0) BioReactor 1 Inf 18.0 57.7 ND (<0.63) 2.12 ND (<0.81) 2.79 (1) BioReactor 2 Inf 0.92 ND (<0.95) ND (<0.63) ND (<0.81) ND (<0.81) 0.0 (0) BioReactor 2 Eff ND (<0.85) ND (<0.95) ND (<0.63) ND (<0.81) ND (<0.81) 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 Creek (Flex Fuel) - WW

Contact: Jay Perkins

Date: November 9, 2012 LIMS #J12110008Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 50x eMDL 200x Se(IV) 0.00 0.00 0.00 0.00 0.00 0.00 0.017 0.85 3.4 Se(VI) 0.00 0.00 0.00 0.00 0.00 0.00 0.019 0.95 3.8 SeCN 0.00 0.00 0.00 0.00 0.00 0.00 0.013 0.63 2.5 MeSe(IV) 0.00 0.00 0.00 0.00 0.00 0.00 0.016 0.81 3.2 SeMe 0.00 0.00 0.00 0.00 0.00 0.00 0.016 0.81 3.2 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 9.11 95.2 Se(VI) LCS 9.48 8.44 89.0 SeCN LCS 8.92 8.31 93.2 MeSe(IV) LCS 6.47 6.31 97.5 SeMe LCS 9.32 8.29 89.0 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews Creek (Flex Fuel) - WW

Contact: Jay Perkins LIMS #J12110008 Date: November 9, 2012 Report Generated by: Russell GeradsQuality Control Summary - Matrix Duplicates

Analyte (μg/L) Sample ID Rep 1 Rep 2 Mean RPD Se(IV) BioReactor 2 Eff ND (<0.85) ND (<0.85) NC NC Se(VI) BioReactor 2 Eff ND (<0.95) ND (<0.95) NC NC SeCN BioReactor 2 Eff ND (<0.63) ND (<0.63) NC NC MeSe(IV) BioReactor 2 Eff ND (<0.81) ND (<0.81) NC NC SeMe BioReactor 2 Eff ND (<0.81) ND (<0.81) 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) BioReactor 2 Eff 278.0 251.4 90.4 278.0 259.2 93.2 3.1 Se(VI) BioReactor 2 Eff 252.3 243.9 96.7 252.3 241.3 95.6 1.1 SeCN BioReactor 2 Eff 228.8 199.0 87.0 228.8 194.4 85.0 2.4 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews Creek (Flex Fuel) - WW

Contact: Jay Perkins LIMS #J12110008 Date: November 9, 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 

### November 16, 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: J12110008 Dear Mr. Perkins, On November 02, 2012, Brooks Rand Labs (BRL) received three (3) wastewater samples and three (3) corresponding field blanks. An aliquot was removed from each sample bottle and filtered into a separate container designed for dissolved mercury (Hg) analysis. The sample volume from the original container was logged-in for total Hg analysis. All samples were received, prepared, analyzed, and stored acco rding to BRL SOPs and EPA methodology.Data used for regulatory purposes has a 24 hour filtration holding time requirement. Nonregulatory purposed data has a 48 hour filtration holding time. The samples were received within holding time. 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. Aside from concentration qualifiers, all data was reported without further qualification 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 Mi Sun Um Project Manager Data Manager lydia@brooksrand.com misun@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 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 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 1244023-01 BioReactor 1 Inf 10/31/2012 11/02/2012 Sample Influent 1244023-02 BioReactor 1 Inf 10/31/2012 11/02/2012 Sample Influent 1244023-03 BioReactor 1 Inf Hg Blk 10/31/2012 11/02/2012 Field Blank DIW 1244023-04 BioReactor 1 Inf Hg Blk 10/31/2012 11/02/2012 Field Blank DIW 1244023-05 BioReactor 2 Inf 10/31/2012 11/02/2012 Sample Influent 1244023-06 BioReactor 2 Inf 10/31/2012 11/02/2012 Sample Influent 1244023-07 BioReactor 2 Inf Hg Blk 10/31/2012 11/02/2012 Field Blank DIW 1244023-08 BioReactor 2 Inf Hg Blk 10/31/2012 11/02/2012 Field Blank DIW 1244023-09 BioReactor 2 Eff 10/31/2012 11/02/2012 Sample Effluent 1244023-10 BioReactor 2 Eff 10/31/2012 11/02/2012 Sample Effluent 1244023-11 BioReactor 2 Eff Hg Blk 10/31/2012 11/02/2012 Field Blank DIW 1244023-12 BioReactor 2 Eff Hg Blk 10/31/2012 11/02/2012 Field Blank DIW 

# Batch Summary

Analyte Prepared Analyzed Sequence Batch Lab Matrix Method B122072 11/05/2012 11/09/2012 1200858 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 105 T 1200858 B122072 Influent 10.1 3.79 1244023-01 Hg ng/L 54.1 D 1200858 B122072 Influent 2.02 0.76 1244023-02 Hg ng/L

BioReactor 1 Inf H g

Blk 0.15 T U 1200858 B122072 DIW 0.41 0.15 1244023-03 Hg ng/L 0.15 D U 1200858 B122072 DIW 0.40 0.15 1244023-04 Hg ng/L

BioReactor 2 Ef f 2.59 T 1200858 B122072 Effluent 1.01 0.38 1244023-09 Hg ng/L 1.33 D 1200858 B122072 Effluent 0.41 0.16 1244023-10 Hg ng/L

BioReactor 2 Eff H g

Blk 0.16 T U 1200858 B122072 DIW 0.42 0.16 1244023-11 Hg ng/L 0.15 D U 1200858 B122072 DIW 0.41 0.15 1244023-12 Hg ng/L

BioReactor 2 In f 20.4 T 1200858 B122072 Influent 1.01 0.38 1244023-05 Hg ng/L 4.31 D 1200858 B122072 Influent 0.40 0.15 1244023-06 Hg ng/L

BioReactor 2 Inf H g

Blk 0.15 T U 1200858 B122072 DIW 0.39 0.15 1244023-07 Hg ng/L 0.15 D U 1200858 B122072 DIW 0.41 0.15 1244023-08 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: B122072

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

Sample Certified Reference Material ( 1245026, NIST 1641d 1000x dilution ) B122072-SRM1 15.68 98% ng/L 85-115 Hg 15.38
Matrix Spike ( 1244022-01 ) B122072-MS2 1053 97% ng/L 71-125 Hg 1126 101.2
Matrix Spike Duplicate ( 1244022-01 ) B122072-MSD2 1053 92% ng/L 71-125 245% Hg 1073 101.2
Matrix Spike ( 1244023-01 ) B122072-MS3 1162 93% ng/L 71-125 Hg 1181 104.5
Matrix Spike Duplicate ( 1244023-01 ) B122072-MSD3 1162 97% ng/L 71-125 245% Hg 1236 104.5

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



# Method Blanks & Reporting Limits

Batch: B122072
Method: EPA 1631 Matrix: Water
Anal yte: H g Result Units Sample B122072-BLK1 ng/L -0.003 B122072-BLK2 ng/L -0.01 B122072-BLK3 ng/L 0.008 B122072-BLK4 ng/L 0.005 MDL: 0.15 Avera g e: 0.00 Standard Deviation: 0.01 Limit: 0.10 Limit: 0.50 MRL: 0.41

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



# Instrument Calibration

Sequence: 1200858 Method: EPA 1631 Instrument: THG-06 ( MerxT ) Date: 11/09/2012 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 1200858-IBL1 3.90 pg of Hg 1200858-IBL2 4.98 pg of Hg 1200858-IBL3 5.98 pg of Hg 1200858-IBL4 6.46 pg of Hg 1200858-CAL1 10.00 10.63 pg of Hg 1 06% 1200858-CAL2 25.00 25.09 pg of Hg 1 00% 1200858-CAL3 100.0 99.20 pg of Hg 99% 1200858-CAL4 500.0 488.6 pg of Hg 98% 1200858-CAL5 2500 2514 pg of Hg 1 01% 1200858-CAL6 10000 9644 pg of Hg 96% 1200858-ICV1 1568 1538 pg of Hg 98% 85-115 1200858-CCB1 7.41 pg of Hg 1200858-CCV1 500.0 499.7 pg of Hg 1 00% 77-123 1200858-CCB2 5.67 pg of Hg 1200858-CCB3 5.12 pg of Hg 1200858-CCB4 5.18 pg of Hg 1200858-CCV2 500.0 501.4 pg of Hg 1 00% 77-123 1200858-CCB5 5.17 pg of Hg 1200858-CCV3 500.0 497.5 pg of Hg 99% 77-123 1200858-CCB6 5.19 pg of Hg 1200858-CCV4 500.0 492.2 pg of Hg 98% 77-123 1200858-CCB7 6.12 pg of Hg 1200858-CCV5 500.0 485.4 pg of Hg 97% 77-123 1200858-CCB8 4.59 pg of Hg 1200858-CCV6 500.0 484.2 pg of Hg 97% 77-123 1200858-CCB9 5.47 pg of Hg 1200858-CCV7 500.0 485.9 pg of Hg 97% 77-123 1200858-CCB A 4.72 pg of Hg 1200858-CCV8 500.0 486.5 pg of Hg 97% 77-123 1200858-CCBB 5.76 pg of Hg 1200858-CCV9 500.0 482.7 pg of Hg 97% 77-123 1200858-CCBC 4.04 pg of Hg 1200858-CCVA 500.0 489.2 pg of Hg 98% 77-123 1200858-CCBD 4.32 pg of Hg 1200858-CCVB 500.0 479.9 pg of Hg 96% 77-123 1200858-CCBE 3.89 pg of Hg 1200858-CCVC 500.0 482.7 pg of Hg 97% 77-123 1200858-CCBF 4.06 pg of Hg 1200858-CCVD 500.0 487.3 pg of Hg 97% 77-123 1200858-CCBG 4.06 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: 1200858 Method: EPA 1631 Instrument: THG-06 ( MerxT ) Date: 11/09/2012 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 1200858-CCVE 500.0 488.5 pg of Hg 98% 77-123 1200858-CCBH 4.17 pg of Hg 1200858-CCVF 500.0 461.8 pg of Hg 92% 77-123 1200858-CCBI 3.83 pg of Hg 1200858-CCVG 500.0 472.0 pg of Hg 94% 77-123 1200858-CCBJ 5.18 pg of Hg 1200858-CCVH 500.0 480.4 pg of Hg 96% 77-123 1200858-CCBK 3.69 pg of Hg 1200858-ICV2 1568 1475 pg of Hg 94% 85-115 1200858-CCVI 500.0 503.2 pg of Hg 1 01% 77-123 1200858-CCBL 3.92 pg of Hg 1200858-CCVJ 500.0 484.8 pg of Hg 97% 77-123 1200858-CCBM 3.26 pg of Hg 1200858-CCVK 500.0 487.1 pg of Hg 97% 77-123 1200858-CCBN 3.41 pg of Hg 1200858-CCVL 500.0 478.1 pg of Hg 96% 77-123 1200858-CCBO 3.00 pg of Hg 1200858-CCVM 500.0 473.2 pg of Hg 95% 77-123 1200858-CCBP 3.23 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: 1244023-01 Re p ort Matrix: Influent Sam p le Typ e: Sam p le Received: 11 / 02 / 2012 Sample: BioReactor 1 Inf Collected: 10 / 31 /2012
Shi p . Cont. p H P-Lot Preservation Lot Size Containe r Des A 71666330 10 Cooler none n/a 500 mL Bottle FLPE H g -T

Lab ID: 1244023-02 Re p ort Matrix: Influent Sam p le Typ e: Sam p le Received: 11 / 02 / 2012 Sample: BioReactor 1 Inf Collected: 10 / 31 /2012
Shi p . Cont. p H P-Lot Preservation Lot Size Containe r Des A 71659890 20 Cooler none n/a 250 mL Bottle FLPE H g -T

Lab ID: 1244023-03 Re p ort Matrix: DIW Sam p le Typ e: Field Blank Received: 11 / 02 / 2012 Sample: BioReactor 1 Inf Hg Blk Collected: 10 / 31 /2012
Shi p . Cont. p H P-Lot Preservation Lot Size Containe r Des A 71666330 10 Cooler none n/a 500 mL Bottle FLPE H g -T

Lab ID: 1244023-04 Re p ort Matrix: DIW Sam p le Typ e: Field Blank Received: 11 / 02 / 2012 Sample: BioReactor 1 Inf Hg Blk Collected: 10 / 31 /2012
Shi p . Cont. p H P-Lot Preservation Lot Size Containe r Des A 71659890 20 Cooler none n/a 250 mL Bottle FLPE H g -T

Lab ID: 1244023-05 Re p ort Matrix: Influent Sam p le Typ e: Sam p le Received: 11 / 02 / 2012 Sample: BioReactor 2 Inf Collected: 10 / 31 /2012
Shi p . Cont. p H P-Lot Preservation Lot Size Containe r Des A 71666330 10 Cooler none n/a 500 mL Bottle FLPE H g -T

Lab ID: 1244023-06 Re p ort Matrix: Influent Sam p le Typ e: Sam p le Received: 11 / 02 / 2012 Sample: BioReactor 2 Inf Collected: 10 / 31 /2012
Shi p . Cont. p H P-Lot Preservation Lot Size Containe r Des A 71659890 20 Cooler none n/a 250 mL 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



# Sample Containers

Lab ID: 1244023-07 Re p ort Matrix: DIW Sam p le Typ e: Field Blank Received: 11 / 02 / 2012 Sample: BioReactor 2 Inf Hg Blk Collected: 10 / 31 /2012
Shi p . Cont. p H P-Lot Preservation Lot Size Containe r Des A 71666330 10 Cooler none n/a 500 mL Bottle FLPE H g -T

Lab ID: 1244023-08 Re p ort Matrix: DIW Sam p le Typ e: Field Blank Received: 11 / 02 / 2012 Sample: BioReactor 2 Inf Hg Blk Collected: 10 / 31 /2012
Shi p . Cont. p H P-Lot Preservation Lot Size Containe r Des A 71659890 20 Cooler none n/a 250 mL Bottle FLPE H g -T

Lab ID: 1244023-09 Re p ort Matrix: Effluent Sam p le Typ e: Sam p le Received: 11 / 02 / 2012 Sample: BioReactor 2 Eff Collected: 10 / 31 /2012
Shi p . Cont. p H P-Lot Preservation Lot Size Containe r Des A 71666330 10 Cooler none n/a 500 mL Bottle FLPE H g -T

Lab ID: 1244023-10 Re p ort Matrix: Effluent Sam p le Typ e: Sam p le Received: 11 / 02 / 2012 Sample: BioReactor 2 Eff Collected: 10 / 31 /2012
Shi p . Cont. p H P-Lot Preservation Lot Size Containe r Des A 71659890 20 Cooler none n/a 250 mL Bottle FLPE H g -T

Lab ID: 1244023-11 Re p ort Matrix: DIW Sam p le Typ e: Field Blank Received: 11 / 02 / 2012 Sample: BioReactor 2 Eff Hg Blk Collected: 10 / 31 /2012
Shi p . Cont. p H P-Lot Preservation Lot Size Containe r Des A 71666330 10 Cooler none n/a 500 mL Bottle FLPE H g -T

Lab ID: 1244023-12 Re p ort Matrix: DIW Sam p le Typ e: Field Blank Received: 11 / 02 / 2012 Sample: BioReactor 2 Eff Hg Blk Collected: 10 / 31 /2012
Shi p . Cont. p H P-Lot Preservation Lot Size Containe r Des A 71659890 20 Cooler none n/a 250 mL 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: 535305195310 via FedEx
Tem p erature: 0.8 °C Coolant Typ 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: November 2, 2012 9:55

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