### 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: J12110363 Project Name: Flex Fuel WW

L ab Contact: Jason C Perkins


### Date: 12/14/2012 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 2012025125 BELEWS 21-Nov-12 7:30 AM P. GASSETT FGD Purge Eff 2012025126 BELEWS 21-Nov-12 7:30 AM P. GASSETT EQ TANK 2012025127 BELEWS 21-Nov-12 7:40 AM P. GASSETT BIOREACTOR 1 INF 2012025128 BELEWS 21-Nov-12 7:40 AM P. GASSETT biOREACTOR 1 INF HG BLK 2012025129 BELEWS 21-Nov-12 7:45 AM P. GASSETT BIOREACTOR 2 INF. 2012025130 BELEWS 21-Nov-12 7:45 AM P. GASSETT BIOREACTOR 2 INF. HG BLANK 2012025131 BELEWS 21-Nov-12 7:50 AM P. GASSETT BIOREACTOR 2 EFF. 2012025132 BELEWS 21-Nov-12 7:50 AM P. GASSETT BIOREACTOR 2 EFF. HG BLANK 2012025133 BELEWS 21-Nov-12 8:00 AM P. GASSETT FILTER BLANK 9 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: 

### 12/14/2012 Electronic Data Deliverable (EDD) Sent Separately

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



### Order # J12110363

2012025125 Collection Date: 21-Nov-12 7:30 AM 

### Site: FGD Purge Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF INORGANIC IONS BY IC Bromide 100 mg/L EPA 300.0 12/04/2012 14:14 JAHERMA 5 50 Chloride 6800 mg/L EPA 300.0 12/04/2012 14:14 JAHERMA 100 1000 Sulfate 1300 mg/L EPA 300.0 12/04/2012 14:14 JAHERMA 100 1000 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 270 ug/L EPA 245.1 11/29/2012 15:18 AGIBBS 5 100
DISSOLVED METALS BY ICP Manganese (Mn) 8.63 mg/L EPA 200.7 11/29/2012 10:32 MHH7131 0.05 10
TOTAL RECOVERABLE METALS BY ICP Boron (B) 189 mg/L EPA 200.7 11/28/2012 14:02 MHH7131 0.5 10 Calcium (Ca) 4580 mg/L EPA 200.7 11/28/2012 14:02 MHH7131 0.1 10 Iron (Fe) 202 mg/L EPA 200.7 11/28/2012 14:02 MHH7131 0.1 10 Magnesium (Mg) 876 mg/L EPA 200.7 11/28/2012 14:02 MHH7131 0.05 10 Manganese (Mn) 10.5 mg/L EPA 200.7 11/28/2012 14:02 MHH7131 0.05 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 292 ug/L EPA 200.8 11/29/2012 13:28 DJSULL1 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 395 ug/L EPA 200.8 11/30/2012 15:07 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 11/30/2012 15:07 KRICHAR 10 10 Chromium (Cr) 355 ug/L EPA 200.8 11/30/2012 15:07 KRICHAR 10 10 Copper (Cu) 212 ug/L EPA 200.8 11/30/2012 15:07 KRICHAR 10 10 Nickel (Ni) 272 ug/L EPA 200.8 11/30/2012 15:07 KRICHAR 10 10 Selenium (Se) 7130 ug/L EPA 200.8 11/30/2012 15:07 KRICHAR 20 20 Silver (Ag) < 10 ug/L EPA 200.8 11/30/2012 15:07 KRICHAR 10 10 Zinc (Zn) 375 ug/L EPA 200.8 11/30/2012 15:07 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 11/28/2012 15:53 SWILLI3 200 1
TOTAL SUSPENDED SOLIDS TSS 4500 mg/L SM2540D 11/30/2012 13:05 TJA7067 250 1

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



### Order # J12110363

2012025126 Collection Date: 21-Nov-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) 137 ug/L EPA 245.1 11/29/2012 15:20 AGIBBS 2.5 50
DISSOLVED METALS BY ICP Manganese (Mn) 7.46 mg/L EPA 200.7 11/29/2012 10:36 MHH7131 0.05 10
TOTAL RECOVERABLE METALS BY ICP Boron (B) 187 mg/L EPA 200.7 11/28/2012 14:06 MHH7131 0.5 10 Calcium (Ca) 3920 mg/L EPA 200.7 11/28/2012 14:06 MHH7131 0.1 10 Iron (Fe) 116 mg/L EPA 200.7 11/28/2012 14:06 MHH7131 0.1 10 Magnesium (Mg) 820 mg/L EPA 200.7 11/28/2012 14:06 MHH7131 0.05 10 Manganese (Mn) 8.60 mg/L EPA 200.7 11/28/2012 14:06 MHH7131 0.05 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 130 ug/L EPA 200.8 11/29/2012 13:32 DJSULL1 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 251 ug/L EPA 200.8 11/30/2012 14:41 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 11/30/2012 14:41 KRICHAR 10 10 Chromium (Cr) 221 ug/L EPA 200.8 11/30/2012 14:41 KRICHAR 10 10 Copper (Cu) 135 ug/L EPA 200.8 11/30/2012 14:41 KRICHAR 10 10 Nickel (Ni) 211 ug/L EPA 200.8 11/30/2012 14:41 KRICHAR 10 10 Selenium (Se) 3590 ug/L EPA 200.8 11/30/2012 14:41 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 11/30/2012 14:41 KRICHAR 10 10 Zinc (Zn) 242 ug/L EPA 200.8 11/30/2012 14:41 KRICHAR 10 10



### 2012025127 Collection Date: 21-Nov-12 7:40 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) 1.42 mg/L EPA 200.7 11/29/2012 10:40 MHH7131 0.05 10
TOTAL RECOVERABLE METALS BY ICP Boron (B) 178 mg/L EPA 200.7 11/28/2012 14:10 MHH7131 0.5 10 Calcium (Ca) 3320 mg/L EPA 200.7 11/28/2012 14:10 MHH7131 0.1 10 Iron (Fe) < 0.1 mg/L EPA 200.7 11/28/2012 14:10 MHH7131 0.1 10 Magnesium (Mg) 729 mg/L EPA 200.7 11/28/2012 14:10 MHH7131 0.05 10 Manganese (Mn) 1.50 mg/L EPA 200.7 11/28/2012 14:10 MHH7131 0.05 10

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



### Order # J12110363

2012025127 Collection Date: 21-Nov-12 7:40 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) 108 ug/L EPA 200.8 11/29/2012 13:35 DJSULL1 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 11/30/2012 14:44 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 11/30/2012 14:44 KRICHAR 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 11/30/2012 14:44 KRICHAR 10 10 Copper (Cu) < 10 ug/L EPA 200.8 11/30/2012 14:44 KRICHAR 10 10 Nickel (Ni) 23.9 ug/L EPA 200.8 11/30/2012 14:44 KRICHAR 10 10 Selenium (Se) 92.2 ug/L EPA 200.8 11/30/2012 14:44 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 11/30/2012 14:44 KRICHAR 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 11/30/2012 14:44 KRICHAR 10 10 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C



### 2012025128 Collection Date: 21-Nov-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



### 2012025129 Collection Date: 21-Nov-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) 1.62 mg/L EPA 200.7 11/29/2012 10:44 MHH7131 0.05 10
TOTAL RECOVERABLE METALS BY ICP Boron (B) 188 mg/L EPA 200.7 11/28/2012 14:14 MHH7131 0.5 10 Calcium (Ca) 3340 mg/L EPA 200.7 11/28/2012 14:14 MHH7131 0.1 10 Iron (Fe) 0.181 mg/L EPA 200.7 11/28/2012 14:14 MHH7131 0.1 10 Magnesium (Mg) 728 mg/L EPA 200.7 11/28/2012 14:14 MHH7131 0.05 10 Manganese (Mn) 1.77 mg/L EPA 200.7 11/28/2012 14:14 MHH7131 0.05 10

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



### Order # J12110363

2012025129 Collection Date: 21-Nov-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) 17.4 ug/L EPA 200.8 11/29/2012 13:38 DJSULL1 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 11/30/2012 14:47 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 11/30/2012 14:47 KRICHAR 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 11/30/2012 14:47 KRICHAR 10 10 Copper (Cu) < 10 ug/L EPA 200.8 11/30/2012 14:47 KRICHAR 10 10 Nickel (Ni) < 10 ug/L EPA 200.8 11/30/2012 14:47 KRICHAR 10 10 Selenium (Se) 21.4 ug/L EPA 200.8 11/30/2012 14:47 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 11/30/2012 14:47 KRICHAR 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 11/30/2012 14:47 KRICHAR 10 10 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C



### 2012025130 Collection Date: 21-Nov-12 7:45 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



### 2012025131 Collection Date: 21-Nov-12 7:50 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF INORGANIC IONS BY IC Bromide 100 mg/L EPA 300.0 12/04/2012 14:33 JAHERMA 5 50 Chloride 7300 mg/L EPA 300.0 12/04/2012 14:33 JAHERMA 100 1000 Sulfate 1600 mg/L EPA 300.0 12/04/2012 14:33 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) 1.81 mg/L EPA 200.7 11/29/2012 10:48 MHH7131 0.05 10

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



### Order # J12110363

2012025131 Collection Date: 21-Nov-12 7:50 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) 195 mg/L EPA 200.7 11/28/2012 14:18 MHH7131 0.5 10 Calcium (Ca) 3470 mg/L EPA 200.7 11/28/2012 14:18 MHH7131 0.1 10 Iron (Fe) 0.251 mg/L EPA 200.7 11/28/2012 14:18 MHH7131 0.1 10 Magnesium (Mg) 752 mg/L EPA 200.7 11/28/2012 14:18 MHH7131 0.05 10 Manganese (Mn) 1.94 mg/L EPA 200.7 11/28/2012 14:18 MHH7131 0.05 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 6.86 ug/L EPA 200.8 11/29/2012 13:41 DJSULL1 5 5
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 5 ug/L EPA 200.8 11/30/2012 14:51 KRICHAR 5 5 Cadmium (Cd) < 5 ug/L EPA 200.8 11/30/2012 14:51 KRICHAR 5 5 Chromium (Cr) < 5 ug/L EPA 200.8 11/30/2012 14:51 KRICHAR 5 5 Copper (Cu) < 5 ug/L EPA 200.8 11/30/2012 14:51 KRICHAR 5 5 Nickel (Ni) < 5 ug/L EPA 200.8 11/30/2012 14:51 KRICHAR 5 5 Selenium (Se) 5.32 ug/L EPA 200.8 11/30/2012 14:51 KRICHAR 5 5 Silver (Ag) < 5 ug/L EPA 200.8 11/30/2012 14:51 KRICHAR 5 5 Zinc (Zn) < 5 ug/L EPA 200.8 11/30/2012 14:51 KRICHAR 5 5 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C



### 2012025132 Collection Date: 21-Nov-12 7:50 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



### 2012025133 Collection Date: 21-Nov-12 8:00 AM 

### Site: FILTER BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF DISSOLVED METALS BY ICP Manganese (Mn) 0.032 mg/L EPA 200.7 11/29/2012 10:05 MHH7131 0.005 1
DISSOLVED METALS BY ICP-MS Selenium (Se) 1.59 ug/L EPA 200.8 11/29/2012 13:06 DJSULL1 1 1

## December 12 , 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 #J12110363)

Dear Mr. Perkins, Attached is the report associated with four (4 ) aqueous samples submitted for selenium speciation on November 26 , 2012. The samples were received in a sealed cooler at-0. 5 ° C on November 27 , 2012

. 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 Creek (Flex Fuel) - WW (LIMS #J12110363)

December 12 , 2012

1. Sample Reception Four (4 ) aqueous samples in125mL HDPE bottles (provided by Applied Speciation and Consulting) were submitted fo r selenium speciation analysis on November 2 6 , 2012. The samples were received on November 2 7 , 201 2 in a sealed container at -0. 5°C. The samples were received in a laminar flow clean hood, void of trace metals contamination and ultra-violet radiation, and 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 December 1, 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 ( 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, LLC

### Sample Results
Sample ID Se(IV) Se(VI) SeCN MeSe(IV) SeMe Unknown Se Species (n) FGD Purge Eff 220 59.4 ND (<2.0) 4.9 ND (<1.8) 0.0 (0) BioReactor 1 Inf 24.6 44.6 ND (<0.51) 3.19 ND (<0.45) 5.02 (1) BioReactor 2 Inf 2.10 2.05 ND (<0.51) ND (<0.45) ND (<0.45) 0.0 (0) BioReactor 2 Eff 0.47 ND (<0.63) ND (<0.51) ND (<0.45) ND (<0.45) 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: December 12, 2012 LIMS #J12110363

### Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 250x eMDL 1000x Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.22 0.86 Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.003 0.63 2.5 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.51 2.0 MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.45 1.8 SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.45 1.8 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 9.57 100.0 Se(VI) LCS 9.48 9.23 97.3 SeCN LCS 8.92 8.78 98.4 MeSe(IV) LCS 6.47 6.15 95.1 SeMe LCS 9.32 8.78 94.2 Selenium Speciation Results for Duke Energy Project Name: Belews Creek (Flex Fuel) - WW

Contact: Jay Perkins LIMS #J12110363 Date: December 12, 2012 Report Generated by: Russell Gerads Applied Speciation and Consulting, LLC

### Quality Control Summary - Matrix Duplicates Analyte (μg/L) Sample ID Rep 1 Rep 2 Mean RPD Se(IV) Batch QC 505.5 477.2 491.4 5.7 Se(VI) Batch QC 62.7 60.3 61.5 3.9 SeCN Batch QC ND (<2.0) ND (<2.0) NC NC MeSe(IV) Batch QC 6.8 5.8 6.3 16.2 SeMe Batch QC ND (<1.8) ND (<1.8) 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 6395 106.2 5560 6337 105.1 0.9 Se(VI) Batch QC 5045 5285 103.5 5045 5259 103.0 0.5 SeCN Batch QC 4575 4665 102.0 4575 4643 101.5 0.5 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 LIMS #J12110363 Date: December 12, 20123958 6 th Ave NW • Seattle, WA 98107 • T: 206

- 632

- 6206 • F: 206

- 632

- 6017 • www.brooksrand.com • brl@brooksrand.com 

### December 10, 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

- HV1 201 Client P roject : J12110363 Dear Mr. Perkins, O n November27 , 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 according to BRL SOPs and EPA methodology. Data used for regulatory purposes has a 24 hour filtration holding time requirement. Non

regulatory purposed data has a 48 hour filtration holding time. The samples were received outside of the 48 hour filtration requirement and the results were qualified H

. 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 samp le

- 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 us if you have any questions regarding this report. Sincerely,

Tiffany Stilwater Mi Sun Um Project Manager Data Manager tiffany@brooksrand.com misun@brooksrand.comProject ID: DUK-HV1201

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



### Definition of Data Qualifiers

(Effective 9/23/09) 

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

# Report Information

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

method detection limit method reporting limit matrix spike

SRM T COC

standard reference material total recoverable fraction chain of custody record 

### Common Abbreviations

These qualifiers are based on those previously utilized by Brooks Rand Labs, those found in the EPA SOW ILM03.0, Exhibit B, Section III, pg. B-18, and the USEPA Contract Laboratory Program National Functional Guidelines for Inorganic Superfund Data Review; USEPA; January 2010. These supersede all previous qualifiers ever employed by BRL. Detected by the instrument, the result is > the MDL but ≤ the MRL. Result is reported and considered an estimate. B E An estimated value due to the presence of interferences. A full explanation is presented in the narrative. H Holding time and/or preservation requirements not met. Result is estimated. J Estimated value. A full explanation is presented in the narrative. J-M Duplicate precision (RPD) for associated QC sample was not within acceptance criteria. Result is estimated. J-N Spike recovery for associated QC sample was not within acceptance criteria. Result is estimated. M Duplicate precision (RPD) was not within acceptance criteria. Result is estimated. N Spike recovery was not within acceptance criteria. Result is estimated. R Rejected, unusable value. A full explanation is presented in the narrative. U Result is ≤ the MDL or client requested reporting limit (CRRL). Result reported as the MDL or CRRL. X Result is not BLK-corrected and is within 10x the absolute value of the highest detectable BLK in the batch. Result is estimated. 

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

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

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



# Sample Information

Report Matrix Type Received Sampled Sample Lab ID 1248002-01 BioReactor 1 Inf 11/21/2012 11/27/2012 Sample Influent 1248002-02 BioReactor 1 Inf 11/21/2012 11/27/2012 Sample Influent 1248002-03 BioReactor 1 Inf Hg Blk 11/21/2012 11/27/2012 Field Blank DIW 1248002-04 BioReactor 1 Inf Hg Blk 11/21/2012 11/27/2012 Field Blank DIW 1248002-05 BioReactor 2 Inf 11/21/2012 11/27/2012 Sample Influent 1248002-06 BioReactor 2 Inf 11/21/2012 11/27/2012 Sample Influent 1248002-07 BioReactor 2 Inf Hg Blk 11/21/2012 11/27/2012 Field Blank DIW 1248002-08 BioReactor 2 Inf Hg Blk 11/21/2012 11/27/2012 Field Blank DIW 1248002-09 BioReactor 2 Eff 11/21/2012 11/27/2012 Sample Effluent 1248002-10 BioReactor 2 Eff 11/21/2012 11/27/2012 Sample Effluent 1248002-11 BioReactor 2 Eff Hg Blk 11/21/2012 11/27/2012 Field Blank DIW 1248002-12 BioReactor 2 Eff Hg Blk 11/21/2012 11/27/2012 Field Blank DIW 

# Batch Summary

Analyte Prepared Analyzed Sequence Batch Lab Matrix Method B122215 11/30/2012 12/03/2012 1200896 Water EPA 1631 Hg

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

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



# Sample Results

Sample Sequence Result MDL MRL Unit Batch

Qualifier Analyte Basis

Report Matrix BioReactor 1 Inf 81.5 T 1200896 B122215 Influent 10.1 3.79 1248002-01 Hg ng/L 66.5 D H 1200896 B122215 Influent 2.02 0.76 1248002-02 Hg ng/L

BioReactor 1 Inf Hg Blk 0.15 T U 1200896 B122215 DIW 0.41 0.15 1248002-03 Hg ng/L 0.15 D H, U 1200896 B122215 DIW 0.41 0.15 1248002-04 Hg ng/L

BioReactor 2 Eff 17.4 T 1200896 B122215 Effluent 0.40 0.15 1248002-09 Hg ng/L 7.91 D H 1200896 B122215 Effluent 0.42 0.16 1248002-10 Hg ng/L

BioReactor 2 Eff Hg Blk 0.15 T U 1200896 B122215 DIW 0.41 0.15 1248002-11 Hg ng/L 0.15 D H, U 1200896 B122215 DIW 0.40 0.15 1248002-12 Hg ng/L

BioReactor 2 Inf 56.2 T 1200896 B122215 Influent 1.02 0.38 1248002-05 Hg ng/L 0.99 D H 1200896 B122215 Influent 0.42 0.16 1248002-06 Hg ng/L

BioReactor 2 Inf Hg Blk 0.15 T U 1200896 B122215 DIW 0.41 0.15 1248002-07 Hg ng/L 0.15 D H, U 1200896 B122215 DIW 0.40 0.15 1248002-08 Hg ng/L

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

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



# Accuracy & Precision Summary

Batch: B122215

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

Sample Certified Reference Material (1245026, NIST 1641d 1000x dilution) B122215-SRM1 15.68 99% ng/L 85-115 Hg 15.45

Matrix Spike (1248002-01) B122215-MS3 505.1 101% ng/L 71-125 Hg 589.4

81.50

Matrix Spike Duplicate (1248002-01) B122215-MSD3 505.1 103% ng/L 71-125 242% Hg 603.8

81.50

Matrix Spike (1248009-01) B122215-MS2 9.969 72% ng/L 71-125 Hg 7.97

0.76

Matrix Spike Duplicate (1248009-01) B122215-MSD2 10.37 80% ng/L 71-125 2413% Hg 9.04

0.76

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

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



# Method Blanks & Reporting Limits

Batch: B122215
Method: EPA 1631 Matrix: Water Analyte: Hg Result Units Sample B122215-BLK1 ng/L 0.10 B122215-BLK2 ng/L 0.16 B122215-BLK3 ng/L 0.15 B122215-BLK4 ng/L 0.11 MDL: 0.15 Average: 0.13 Standard Deviation: 0.03 Limit: 0.10 Limit: 0.50 MRL: 0.40

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

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



# Instrument Calibration

Sequence: 1200896 Method: EPA 1631 Instrument: THG-06(MerxT) Date: 12/03/2012 Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg REC & Limits Result True Value Lab ID Units 1200896-IBL1 3.09 pg of Hg 1200896-IBL2 3.57 pg of Hg 1200896-IBL3 3.27 pg of Hg 1200896-IBL4 3.35 pg of Hg 1200896-CAL1 10.00 9.94 pg of Hg 99% 1200896-CAL2 25.00 25.16 pg of Hg 101% 1200896-CAL3 100.0 101.6 pg of Hg 102% 1200896-CAL4 500.0 501.7 pg of Hg 100% 1200896-CAL5 2500 2525 pg of Hg 101% 1200896-CAL6 10000 9713 pg of Hg 97% 1200896-ICV1 1568 1545 pg of Hg 99% 85-115 1200896-CCB1 5.95 pg of Hg 1200896-CCV1 500.0 504.0 pg of Hg 101% 77-123 1200896-CCB2 4.12 pg of Hg 1200896-CCB3 3.41 pg of Hg 1200896-CCB4 3.82 pg of Hg 1200896-CCV2 500.0 557.8 pg of Hg 112% 77-123 1200896-CCB5 3.92 pg of Hg 1200896-CCV3 500.0 507.7 pg of Hg 102% 77-123 1200896-CCB6 4.17 pg of Hg 1200896-CCV4 500.0 509.9 pg of Hg 102% 77-123 1200896-CCB7 3.46 pg of Hg 1200896-CCV5 500.0 510.8 pg of Hg 102% 77-123 1200896-CCB8 3.85 pg of Hg 1200896-CCV6 500.0 507.3 pg of Hg 101% 77-123 1200896-CCB9 3.38 pg of Hg 1200896-CCV7 500.0 517.0 pg of Hg 103% 77-123 1200896-CCBA 4.87 pg of Hg 1200896-CCV8 500.0 510.6 pg of Hg 102% 77-123 1200896-CCBB 4.69 pg of Hg 1200896-CCV9 500.0 511.8 pg of Hg 102% 77-123 1200896-CCBC 7.57 pg of Hg 1200896-CCVA 500.0 506.7 pg of Hg 101% 77-123 1200896-CCBD 6.28 pg of Hg 1200896-CCVB 500.0 503.6 pg of Hg 101% 77-123 1200896-CCBE 5.66 pg of Hg 1200896-CCVC 500.0 508.0 pg of Hg 102% 77-123 1200896-CCBF 5.26 pg of Hg 1200896-CCVD 500.0 511.9 pg of Hg 102% 77-123 1200896-CCBG 4.40 pg of Hg

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

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



# Instrument Calibration

Sequence: 1200896 Method: EPA 1631 Instrument: THG-06(MerxT) Date: 12/03/2012 Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg REC & Limits Result True Value Lab ID Units 1200896-CCVE 500.0 520.6 pg of Hg 104% 77-123 1200896-CCBH 4.44 pg of Hg

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

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



# Sample Containers

Lab ID: 1248002-01 Report Matrix: Influent Sample Type: Sample Received: 11/27/2012 Sample: BioReactor 1 Inf Collected: 11/21/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71666330 10 Cooler

none n/a 500 mL Bottle FLPE Hg-T

Lab ID: 1248002-02 Report Matrix: Influent Sample Type: Sample Received: 11/27/2012 Sample: BioReactor 1 Inf Collected: 11/21/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71691270 10 Cooler

none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 1248002-03 Report Matrix: DIW Sample Type: Field Blank Received: 11/27/2012 Sample: BioReactor 1 Inf Hg Blk Collected: 11/21/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71666330 10 Cooler

none n/a 500 mL Bottle FLPE Hg-T

Lab ID: 1248002-04 Report Matrix: DIW Sample Type: Field Blank Received: 11/27/2012 Sample: BioReactor 1 Inf Hg Blk Collected: 11/21/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71691270 10 Cooler

none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 1248002-05 Report Matrix: Influent Sample Type: Sample Received: 11/27/2012 Sample: BioReactor 2 Inf Collected: 11/21/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71666330 10 Cooler

none n/a 500 mL Bottle FLPE Hg-T

Lab ID: 1248002-06 Report Matrix: Influent Sample Type: Sample Received: 11/27/2012 Sample: BioReactor 2 Inf Collected: 11/21/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71691270 10 Cooler

none n/a 250 mL Bottle FLPE Hg-T

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

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



# Sample Containers

Lab ID: 1248002-07 Report Matrix: DIW Sample Type: Field Blank Received: 11/27/2012 Sample: BioReactor 2 Inf Hg Blk Collected: 11/21/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71666330 10 Cooler

none n/a 500 mL Bottle FLPE Hg-T

Lab ID: 1248002-08 Report Matrix: DIW Sample Type: Field Blank Received: 11/27/2012 Sample: BioReactor 2 Inf Hg Blk Collected: 11/21/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71691270 10 Cooler

none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 1248002-09 Report Matrix: Effluent Sample Type: Sample Received: 11/27/2012 Sample: BioReactor 2 Eff Collected: 11/21/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71666330 10 Cooler

none n/a 500 mL Bottle FLPE Hg-T

Lab ID: 1248002-10 Report Matrix: Effluent Sample Type: Sample Received: 11/27/2012 Sample: BioReactor 2 Eff Collected: 11/21/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71691270 10 Cooler

none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 1248002-11 Report Matrix: DIW Sample Type: Field Blank Received: 11/27/2012 Sample: BioReactor 2 Eff Hg Blk Collected: 11/21/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71666330 10 Cooler

none n/a 500 mL Bottle FLPE Hg-T

Lab ID: 1248002-12 Report Matrix: DIW Sample Type: Field Blank Received: 11/27/2012 Sample: BioReactor 2 Eff Hg Blk Collected: 11/21/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71691270 10 Cooler

none n/a 250 mL Bottle FLPE Hg-T

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

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



# Shipping Containers

Cooler
Tracking No: 5353 0519 6155 via FedEx Temperature: -0.6 °C Coolant Type: Ice Description: Cooler Damaged in transit? No Returned to client? No Custody seals present? No Custody seals intact? No COC present? Yes Received: November 27, 2012 9:00

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