### 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: J12090007 Project Name: WWTS - Biweekly (1)

L ab Contact: Jason C Perkins


### Date: 10/2/2012 Customer Address: 3195 Pine Hall Rd Customer Name(s): Bill Kennedy, Melonie Martin, Wayne Chapman, Tom Johnson

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 2012018998 BELEWS 12-Sep-12 8:00 AM TRAVIS THORNTON FGD Purge Eff 2012018999 BELEWS 12-Sep-12 8:05 AM TRAVIS THORNTON EQ TANK EFF. 2012019000 BELEWS 12-Sep-12 8:10 AM TRAVIS THORNTON BIOREACTOR 1 INF. 2012019001 BELEWS 12-Sep-12 8:15 AM TRAVIS THORNTON BIOREACTOR 2 INF. 2012019002 BELEWS 12-Sep-12 8:20 AM TRAVIS THORNTON BIOREACTOR 2 EFF. 2012019003 BELEWS 12-Sep-12 8:25 AM TRAVIS THORNTON FILTER BLANK 2012019004 BELEWS 12-Sep-12 8:30 AM TRAVIS THORNTON Trip Blank 2012019005 BELEWS 12-Sep-12 8:30 AM TRAVIS THORNTON BIOREACTOR 1 INF (HG) 2012019006 BELEWS 12-Sep-12 8:35 AM TRAVIS THORNTON HG BLANK BIOREACTOR 1 INF. 2012019007 BELEWS 12-Sep-12 8:40 AM TRAVIS THORNTON BIOREACTOR 2 INF (HG) 2012019008 BELEWS 12-Sep-12 8:45 AM TRAVIS THORNTON Hg Blk BioReactor 2 Inf 2012019009 BELEWS 12-Sep-12 8:50 AM TRAVIS THORNTON BIOREACTOR 2 EFF (HG) 2012019010 BELEWS 12-Sep-12 8:50 AM TRAVIS THORNTON Hg Blk BioReactor 2 Eff 13 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: 

### DataBase Administrator Date: 

### 10/2/2012 Electronic Data Deliverable (EDD) Sent Separately

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



### Order # J12090007

2012018998 Collection Date: 12-Sep-12 8:00 AM 

### Site: FGD Purge Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF INORGANIC IONS BY IC Bromide 94 mg/L EPA 300.0 9/18/2012 12:18:00 AM JAHERMA 5 50 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 191 ug/L EPA 245.1 9/20/2012 1:51:38 PM AGIBBS 5 100
DISSOLVED METALS BY ICP Manganese (Mn) 6.03 mg/L EPA 200.7 9/21/2012 2:33:00 PM DJSULL1 0.05 10
TOTAL RECOVERABLE METALS BY ICP Boron (B) 187 mg/L EPA 200.7 9/25/2012 12:48:00 PM DJSULL1 0.5 10 Manganese (Mn) 6.03 mg/L EPA 200.7 9/25/2012 12:48:00 PM DJSULL1 0.05 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 391 ug/L EPA 200.8 9/18/2012 2:36:00 PM KRICHAR 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 300 ug/L EPA 200.8 9/18/2012 12:39:00 PM KRICHAR 10 10 Chromium (Cr) 264 ug/L EPA 200.8 9/18/2012 12:39:00 PM KRICHAR 10 10 Copper (Cu) 162 ug/L EPA 200.8 9/18/2012 12:39:00 PM KRICHAR 10 10 Nickel (Ni) 275 ug/L EPA 200.8 9/18/2012 12:39:00 PM KRICHAR 10 10 Selenium (Se) 3790 ug/L EPA 200.8 9/18/2012 12:39:00 PM KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 9/18/2012 12:39:00 PM KRICHAR 10 10 Zinc (Zn) 270 ug/L EPA 200.8 9/18/2012 12:39:00 PM 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 19000 mg/L SM2540C 9/17/2012 3:18:00 PM SWILLI3 200 1



### 2012018999 Collection Date: 12-Sep-12 8:05 AM 

### Site: EQ TANK EFF. Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 122 ug/L EPA 245.1 9/20/2012 1:58:45 PM AGIBBS 2.5 50
DISSOLVED METALS BY ICP Manganese (Mn) 4.49 mg/L EPA 200.7 9/21/2012 2:37:00 PM DJSULL1 0.05 10
TOTAL RECOVERABLE METALS BY ICP Boron (B) 185 mg/L EPA 200.7 9/25/2012 12:52:00 PM DJSULL1 0.5 10 Manganese (Mn) 4.49 mg/L EPA 200.7 9/25/2012 12:52:00 PM DJSULL1 0.05 10

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



### Order # J12090007

2012018999 Collection Date: 12-Sep-12 8:05 AM 

### Site: EQ TANK EFF. Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF DISSOLVED METALS BY ICP-MS Selenium (Se) 277 ug/L EPA 200.8 9/18/2012 2:39:00 PM KRICHAR 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 170 ug/L EPA 200.8 9/18/2012 12:42:00 PM KRICHAR 10 10 Chromium (Cr) 177 ug/L EPA 200.8 9/18/2012 12:42:00 PM KRICHAR 10 10 Copper (Cu) 99.0 ug/L EPA 200.8 9/18/2012 12:42:00 PM KRICHAR 10 10 Nickel (Ni) 193 ug/L EPA 200.8 9/18/2012 12:42:00 PM KRICHAR 10 10 Selenium (Se) 2740 ug/L EPA 200.8 9/18/2012 12:42:00 PM KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 9/18/2012 12:42:00 PM KRICHAR 10 10 Zinc (Zn) 174 ug/L EPA 200.8 9/18/2012 12:42:00 PM KRICHAR 10 10



### 2012019000 Collection Date: 12-Sep-12 8:10 AM 

### Site: BIOREACTOR 1 INF. Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF DISSOLVED METALS BY ICP Manganese (Mn) 0.563 mg/L EPA 200.7 9/21/2012 2:41:00 PM DJSULL1 0.05 10
TOTAL RECOVERABLE METALS BY ICP Boron (B) 174 mg/L EPA 200.7 9/25/2012 12:56:00 PM DJSULL1 0.5 10 Manganese (Mn) 0.563 mg/L EPA 200.7 9/25/2012 12:56:00 PM DJSULL1 0.05 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 328 ug/L EPA 200.8 9/18/2012 2:42:00 PM KRICHAR 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 9/18/2012 12:46:00 PM KRICHAR 10 10 Chromium (Cr) 11.5 ug/L EPA 200.8 9/18/2012 12:46:00 PM KRICHAR 10 10 Copper (Cu) < 10 ug/L EPA 200.8 9/18/2012 12:46:00 PM KRICHAR 10 10 Nickel (Ni) 22.5 ug/L EPA 200.8 9/18/2012 12:46:00 PM KRICHAR 10 10 Selenium (Se) 352 ug/L EPA 200.8 9/18/2012 12:46:00 PM KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 9/18/2012 12:46:00 PM KRICHAR 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 9/18/2012 12:46:00 PM KRICHAR 10 10 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C

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



### Order # J12090007

2012019001 Collection Date: 12-Sep-12 8:15 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF TOTAL RECOVERABLE METALS BY ICP Boron (B) 183 mg/L EPA 200.7 9/25/2012 1:00:00 PM DJSULL1 0.5 10 Manganese (Mn) 0.143 mg/L EPA 200.7 9/25/2012 1:00:00 PM DJSULL1 0.05 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 9/18/2012 12:49:00 PM KRICHAR 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 9/18/2012 12:49:00 PM KRICHAR 10 10 Copper (Cu) < 10 ug/L EPA 200.8 9/18/2012 12:49:00 PM KRICHAR 10 10 Nickel (Ni) < 10 ug/L EPA 200.8 9/18/2012 12:49:00 PM KRICHAR 10 10 Selenium (Se) 20.2 ug/L EPA 200.8 9/18/2012 12:49:00 PM KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 9/18/2012 12:49:00 PM KRICHAR 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 9/18/2012 12:49:00 PM KRICHAR 10 10



### 2012019002 Collection Date: 12-Sep-12 8:20 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF INORGANIC IONS BY IC Bromide 100 mg/L EPA 300.0 9/18/2012 12:36:00 AM JAHERMA 5 50 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) < 1 ug/L EPA 245.1 9/20/2012 2:01:06 PM AGIBBS 1 20
TOTAL RECOVERABLE METALS BY ICP Boron (B) 196 mg/L EPA 200.7 9/25/2012 1:04:00 PM DJSULL1 0.5 10 Manganese (Mn) 0.173 mg/L EPA 200.7 9/25/2012 1:04:00 PM DJSULL1 0.05 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 5 ug/L EPA 200.8 9/18/2012 12:52:00 PM KRICHAR 5 5 Chromium (Cr) < 5 ug/L EPA 200.8 9/18/2012 12:52:00 PM KRICHAR 5 5 Copper (Cu) < 5 ug/L EPA 200.8 9/18/2012 12:52:00 PM KRICHAR 5 5 Nickel (Ni) < 5 ug/L EPA 200.8 9/18/2012 12:52:00 PM KRICHAR 5 5 Selenium (Se) 6.09 ug/L EPA 200.8 9/18/2012 12:52:00 PM KRICHAR 5 5 Silver (Ag) < 5 ug/L EPA 200.8 9/18/2012 12:52:00 PM KRICHAR 5 5 Zinc (Zn) < 5 ug/L EPA 200.8 9/18/2012 12:52:00 PM KRICHAR 5 5 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C

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



### Order # J12090007

2012019003 Collection Date: 12-Sep-12 8:25 AM 

### Site: FILTER BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF DISSOLVED METALS BY ICP Manganese (Mn) 0.016 mg/L EPA 200.7 9/21/2012 2:21:00 PM DJSULL1 0.005 1
DISSOLVED METALS BY ICP-MS Selenium (Se) 3.91 ug/L EPA 200.8 9/18/2012 2:12:00 PM KRICHAR 1 1



### 2012019004 Collection Date: 12-Sep-12 8:30 AM 

### Site: Trip Blank Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF TOTAL RECOVERABLE METALS BY ICP Boron (B) < 0.05 mg/L EPA 200.7 9/25/2012 12:25:00 PM DJSULL1 0.05 1 Manganese (Mn) < 0.005 mg/L EPA 200.7 9/25/2012 12:25:00 PM DJSULL1 0.005 1
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 1 ug/L EPA 200.8 9/18/2012 12:35:00 PM KRICHAR 1 1 Chromium (Cr) < 1 ug/L EPA 200.8 9/18/2012 12:35:00 PM KRICHAR 1 1 Copper (Cu) < 1 ug/L EPA 200.8 9/18/2012 12:35:00 PM KRICHAR 1 1 Nickel (Ni) < 1 ug/L EPA 200.8 9/18/2012 12:35:00 PM KRICHAR 1 1 Selenium (Se) 10.3 ug/L EPA 200.8 9/18/2012 12:35:00 PM KRICHAR 1 1 Silver (Ag) < 1 ug/L EPA 200.8 9/18/2012 12:35:00 PM KRICHAR 1 1 Zinc (Zn) 1.02 ug/L EPA 200.8 9/18/2012 12:35:00 PM KRICHAR 1 1 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C



### 2012019005 Collection Date: 12-Sep-12 8:30 AM 

### Site: BIOREACTOR 1 INF (HG) Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

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



### 2012019006 Collection Date: 12-Sep-12 8:35 AM 

### Site: HG BLANK BIOREACTOR 1 INF. Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

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

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



### Order # J12090007

2012019006 Collection Date: 12-Sep-12 8:35 AM 

### Site: HG BLANK BIOREACTOR 1 INF. Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF



### 2012019007 Collection Date: 12-Sep-12 8:40 AM 

### Site: BIOREACTOR 2 INF (HG) Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

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



### 2012019008 Collection Date: 12-Sep-12 8:45 AM 

### Site: Hg Blk BioReactor 2 Inf Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

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



### 2012019009 Collection Date: 12-Sep-12 8:50 AM 

### Site: BIOREACTOR 2 EFF (HG) Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

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



### 2012019010 Collection Date: 12-Sep-12 8:50 AM 

### Site: Hg Blk BioReactor 2 Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

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

## September 2 5 , 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 - FGD WWTS Bi-Monthly Sampling) (LIMS#J12090007 )

Dear Mr. Perki ns, Attached is the report associated with four (4 ) aqueous samples submitted for selenium speciation analysis on September 13 , 2012

. The samples were received in a sealed cooler at -0. 5 ° C on September 14, 2012

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

Russell Gerads Vice President Applied Speciation and Consulting, LLC

## Applied Speciation and Consulting, LLC Report prepared for: Jay Perkins Duke Energy Analytical Laboratory Mail Code MGO3A2 (Building 7405) 13339 Hagers Ferry Rd. Huntersville, NC 28078 Project: Belews - FGD WWTS Bi-Monthly Sampling) (LIMS#J12090007)
September 2 5 , 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 September 13 , 2012 . The samples were received on September 14 , 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 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 minimal 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 September 21, 2012. 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, 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 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, LLC

### Sample Results

Sample ID Se(IV) Se(VI) SeCN MeSe(IV) SeMe Unknown Se Species (n) FGD Purge Eff 149 264 ND (<1.2) 2.16 ND (<0.92) 0.0 (0) BioReactor 1 Inf 17.3 286 ND (<0.31) 2.83 ND (<0.23) 0.65 (1) BioReactor 2 Eff 0.46 ND (<0.12) ND (<0.31) ND (<0.23) ND (<0.23) 0.0 (0) Metals Trip Blk ND (<0.010) ND (<0.0047) ND (<0.012) ND (<0.0092) ND (<0.0092) 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 n = number of unknown Se species observed Report Generated by: Russell Gerads Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS Bi-Monthly Sampling)

Contact: Jay Perkins

Date: September 25, 2012 LIMS #J12090007

### Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 10x eMDL 250x eMDL 1000x Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.0010 0.010 0.26 1.0 Se(VI) 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0005 0.0047 0.12 0.47 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.0012 0.012 0.31 1.2 MeSe(IV) 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0009 0.0092 0.23 0.92 SeMe 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0009 0.0092 0.23 0.92 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 9.30 97.2 Se(VI) LCS 9.48 8.94 94.3 SeCN LCS 8.92 8.60 96.4 MeSe(IV) LCS 6.47 6.07 93.9 SeMe LCS 9.32 8.67 93.1 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS Bi-Monthly Sampling)

Contact: Jay Perkins LIMS #J12090007 Date: September 25, 2012 Report Generated by: Russell Gerads

### Quality Control Summary - Matrix Duplicates

Analyte (μg/L) Sample ID Rep 1 Rep 2 Mean RPD Se(IV) Batch QC 8.3 7.4 7.8 11.9 Se(VI) Batch QC 3068 3106 3087 1.2 SeCN Batch QC ND (<1.2) ND (<1.2) NC NC MeSe(IV) Batch QC ND (<0.92) ND (<0.92) NC NC SeMe Batch QC ND (<0.92) ND (<0.92) 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 5668 101.8 5560 5668 101.8 0.0 Se(VI) Batch QC 5045 8168 100.7 5045 8145 100.3 0.3 SeCN Batch QC 4575 4437 97.0 4575 4452 97.3 0.4 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS Bi-Monthly Sampling)

Contact: Jay Perkins LIMS #J12090007 Date: September 25, 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 

### October 1, 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: J12090007

Dear Mr. Perkins, On September 14, 2012, Brooks Rand Labs (BRL) received three (3) wastewater samples and three (3) corresponding field blanks. The samples were logged-in for total Hg analysis. All samples were received, prepared, analyzed, and stored according to BRL SOPs and EPA methodology. The results were blank-corrected as described in the calculations section of the relevant SOP and may have been evaluated using reporting limits that have been adjusted to account for sample aliquot size. Please refer to the Sample Results page for sample-specific MDLs, MRLs, and other details. In sequence 1200740, CCBB was greater than the low calibration standard. No samples from this work order were bracketed by the elevated CCB. All samples that were bracketed by this CCB were greater than 10x the concentration and no further action was required. Sample Hg Blk BioReactor 2 Inf (1237041-04) was identified as a field blank and produced a detectable Hg concentration of 0.20 ng/L. The result was less than the method limit of 0.50 ng/L and not considered a significant source of contamination. Aside from concentration qualifiers, all data was reported without 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 Project Manager lydia@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 1237041-01 BioReactor 1 Inf 09/12/2012 09/14/2012 Sample Influent 1237041-02 Hg Blk BioReactor 1 Inf 09/12/2012 09/14/2012 Field Blank DIW 1237041-03 BioReactor 2 Inf 09/12/2012 09/14/2012 QC Sample Influent 1237041-04 Hg Blk BioReactor 2 Inf 09/12/2012 09/14/2012 Field Blank DIW 1237041-05 BioReactor 2 Eff 09/12/2012 09/14/2012 Sample Effluent 1237041-06 Hg Blk BioReactor 2 Eff 09/12/2012 09/14/2012 Field Blank DIW 

# Batch Summary

Analyte Prepared Analyzed Sequence Batch Lab Matrix Method B121743 09/20/2012 09/25/2012 1200740 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 173 T 1200740 B121743 Influent 20.2 7.58 1237041-01 Hg ng/L

BioReactor 2 Eff 36.8 T 1200740 B121743 Effluent 1.01 0.38 1237041-05 Hg ng/L

BioReactor 2 Inf 87.2 T 1200740 B121743 Influent 10.1 3.79 1237041-03 Hg ng/L

Hg Blk BioReactor 1 Inf 0.15 T U 1200740 B121743 DIW 0.41 0.15 1237041-02 Hg ng/L

Hg Blk BioReactor 2 Eff 0.15 T U 1200740 B121743 DIW 0.40 0.15 1237041-06 Hg ng/L

Hg Blk BioReactor 2 Inf 0.20 T B 1200740 B121743 DIW 0.40 0.15 1237041-04 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: B121743

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

Sample Certified Reference Material (1237042, NIST 1641d 1000x dilution) B121743-SRM1 62.72 99% ng/L 85-115 Hg 62.13

Duplicate (1237041-03) B121743-DUP1 ng/L 2411% Hg 96.92

87.20

Matrix Spike (1237041-03) B121743-MS1 1515 95% ng/L 71-125 Hg 1531

87.20

Matrix Spike Duplicate (1237041-03) B121743-MSD1 1515 95% ng/L 71-125 24 0.001% Hg 1531

87.20

Duplicate (1237042-05) B121743-DUP2 ng/L 2416% Hg 8.11

6.94

Matrix Spike (1237042-05) B121743-MS2 63.56 82% ng/L 71-125 Hg 58.89

6.94

Matrix Spike Duplicate (1237042-05) B121743-MSD2 63.14 82% ng/L 71-125 240.2% Hg 59.00

6.94

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: B121743
Method: EPA 1631 Matrix: Water Analyte: Hg Result Units Sample B121743-BLK1 ng/L 0.13 B121743-BLK2 ng/L 0.18 B121743-BLK3 ng/L 0.16 B121743-BLK4 ng/L 0.14 MDL: 0.16 Average: 0.15 Standard Deviation: 0.02 Limit: 0.11 Limit: 0.50 MRL: 0.42

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

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



# Instrument Calibration

Sequence: 1200740 Method: EPA 1631 Instrument: THG-05 Date: 09/25/2012 Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg REC & Limits Result True Value Lab ID Units 1200740-IBL1 1.40 pg of Hg 1200740-IBL2 1.85 pg of Hg 1200740-IBL3 2.50 pg of Hg 1200740-IBL4 4.25 pg of Hg 1200740-CAL1 10.00 10.11 pg of Hg 101% 1200740-CAL2 25.00 23.88 pg of Hg 96% 1200740-CAL3 100.0 99.90 pg of Hg 100% 1200740-CAL4 500.0 501.1 pg of Hg 100% 1200740-CAL5 2500 2574 pg of Hg 103% 1200740-CAL6 10000 10060 pg of Hg 101% 1200740-ICV1 1568 1553 pg of Hg 99% 85-115 1200740-CCB1 8.83 pg of Hg 1200740-CCV1 500.0 508.8 pg of Hg 102% 77-123 1200740-CCB2 7.14 pg of Hg 1200740-CCB3 4.51 pg of Hg 1200740-CCB4 4.97 pg of Hg 1200740-CCV2 500.0 499.8 pg of Hg 100% 77-123 1200740-CCB5 4.84 pg of Hg 1200740-CCV3 500.0 479.7 pg of Hg 96% 77-123 1200740-CCB6 5.48 pg of Hg 1200740-CCV4 500.0 473.9 pg of Hg 95% 77-123 1200740-CCB7 3.66 pg of Hg 1200740-CCV5 500.0 486.7 pg of Hg 97% 77-123 1200740-CCB8 3.81 pg of Hg 1200740-CCV6 500.0 439.8 pg of Hg 88% 77-123 1200740-CCB9 3.87 pg of Hg 1200740-CCV7 500.0 451.7 pg of Hg 90% 77-123 1200740-CCBA 3.43 pg of Hg 1200740-CCV8 500.0 497.9 pg of Hg 100% 77-123 1200740-CCBB 11.2 pg of Hg 1200740-CCV9 500.0 494.2 pg of Hg 99% 77-123 1200740-CCBC 7.75 pg of Hg 1200740-CCVA 500.0 496.0 pg of Hg 99% 77-123 1200740-CCBD 7.09 pg of Hg 1200740-CCVB 500.0 492.0 pg of Hg 98% 77-123 1200740-CCBE 6.35 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: 1237041-01 Report Matrix: Influent Sample Type: Sample Received: 09/14/2012 Sample: BioReactor 1 Inf Collected: 09/12/2012
Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71659890 20 Cooler

none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 1237041-02 Report Matrix: DIW Sample Type: Field Blank Received: 09/14/2012 Sample: Hg Blk BioReactor 1 Inf Collected: 09/12/2012
Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71659890 20 Cooler

none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 1237041-03 Report Matrix: Influent Sample Type: QC Sample Received: 09/14/2012 Sample: BioReactor 2 Inf Collected: 09/12/2012
Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71659890 20 Cooler

none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 1237041-04 Report Matrix: DIW Sample Type: Field Blank Received: 09/14/2012 Sample: Hg Blk BioReactor 2 Inf Collected: 09/12/2012
Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71659890 20 Cooler

none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 1237041-05 Report Matrix: Effluent Sample Type: Sample Received: 09/14/2012 Sample: BioReactor 2 Eff Collected: 09/12/2012
Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71659890 20 Cooler

none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 1237041-06 Report Matrix: DIW Sample Type: Field Blank Received: 09/14/2012 Sample: Hg Blk BioReactor 2 Eff Collected: 09/12/2012
Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71659890 20 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 4130 via FedEx Temperature: -1.1 °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: September 14, 2012 9:00

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