### 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: J12080079 Project Name: WWTS - Biweekly (1)

L ab Contact: Jason C Perkins 

### Date: 8/30/2012 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 2012016850 BELEWS 08-Aug-12 8:30 AM TRAVIS THORNTON FGD Purge Eff 2012016851 BELEWS 08-Aug-12 8:30 AM TRAVIS THORNTON EQ TANK EFF. 2012016852 BELEWS 08-Aug-12 8:30 AM TRAVIS THORNTON BIOREACTOR 1 INF. 2012016853 BELEWS 08-Aug-12 8:30 AM TRAVIS THORNTON BIOREACTOR 2 INF. 2012016854 BELEWS 08-Aug-12 8:30 AM TRAVIS THORNTON BIOREACTOR 2 EFF. 2012016855 BELEWS 08-Aug-12 8:30 AM TRAVIS THORNTON FILTER BLANK 2012016856 BELEWS 08-Aug-12 8:30 AM TRAVIS THORNTON Trip Blank 2012016857 BELEWS 08-Aug-12 8:00 AM TRAVIS THORNTON BIOREACTOR 1 INF (HG) 2012016858 BELEWS 08-Aug-12 8:00 AM TRAVIS THORNTON HG BLANK BIOREACTOR 1 INF. 2012016859 BELEWS 08-Aug-12 8:00 AM TRAVIS THORNTON BIOREACTOR 2 INF (HG) 2012016860 BELEWS 08-Aug-12 8:00 AM TRAVIS THORNTON Hg Blk BioReactor 2 Inf 2012016861 BELEWS 08-Aug-12 8:00 AM TRAVIS THORNTON BIOREACTOR 2 EFF (HG) 2012016862 BELEWS 08-Aug-12 8:00 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: 

### 8/30/2012 Electronic Data Deliverable (EDD) Sent Separately

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



### Order # J12080079

2012016850 Collection Date: 08-Aug-12 8:30 AM 

### Site: FGD Purge Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF INORGANIC IONS BY IC Bromide 120 mg/L EPA 300.0 8/13/2012 6:37:00 PM JAHERMA 5 50 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 295 ug/L EPA 245.1 8/16/2012 1:22:53 PM AGIBBS 5 100 DISSOLVED METALS BY ICP Manganese (Mn) 9.20 mg/L EPA 200.7 8/14/2012 10:50:00 AM MHH7131 0.05 10 TOTAL RECOVERABLE METALS BY ICP Boron (B) 218 mg/L EPA 200.7 8/22/2012 12:31:00 PM DJSULL1 0.5 10 Manganese (Mn) 9.75 mg/L EPA 200.7 8/22/2012 12:31:00 PM DJSULL1 0.05 10 DISSOLVED METALS BY ICP-MS Selenium (Se) 179 ug/L EPA 200.8 8/14/2012 1:55:00 PM DJSULL1 10 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 230 ug/L EPA 200.8 8/16/2012 11:16:00 AM KRICHAR 10 10 Chromium (Cr) 257 ug/L EPA 200.8 8/16/2012 11:16:00 AM KRICHAR 10 10 Copper (Cu) 145 ug/L EPA 200.8 8/16/2012 11:16:00 AM KRICHAR 10 10 Nickel (Ni) 222 ug/L EPA 200.8 8/16/2012 11:16:00 AM KRICHAR 10 10 Selenium (Se) 5610 ug/L EPA 200.8 8/16/2012 11:16:00 AM KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 8/16/2012 11:16:00 AM KRICHAR 10 10 Zinc (Zn) 273 ug/L EPA 200.8 8/16/2012 11:16:00 AM 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 21000 mg/L SM2540C 8/15/2012 4:29:00 PM TJA7067 200 1


### 2012016851 Collection Date: 08-Aug-12 8:30 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) 206 ug/L EPA 245.1 8/16/2012 1:25:13 PM AGIBBS 2.5 50 DISSOLVED METALS BY ICP Manganese (Mn) 8.89 mg/L EPA 200.7 8/14/2012 10:54:00 AM MHH7131 0.05 10 TOTAL RECOVERABLE METALS BY ICP Boron (B) 220 mg/L EPA 200.7 8/22/2012 12:35:00 PM DJSULL1 0.5 10 Manganese (Mn) 9.71 mg/L EPA 200.7 8/22/2012 12:35:00 PM DJSULL1 0.05 10

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



### Order # J12080079

2012016851 Collection Date: 08-Aug-12 8:30 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) 127 ug/L EPA 200.8 8/14/2012 1:58:00 PM DJSULL1 10 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 204 ug/L EPA 200.8 8/16/2012 11:20:00 AM KRICHAR 10 10 Chromium (Cr) 223 ug/L EPA 200.8 8/16/2012 11:20:00 AM KRICHAR 10 10 Copper (Cu) 129 ug/L EPA 200.8 8/16/2012 11:20:00 AM KRICHAR 10 10 Nickel (Ni) 202 ug/L EPA 200.8 8/16/2012 11:20:00 AM KRICHAR 10 10 Selenium (Se) 5010 ug/L EPA 200.8 8/16/2012 11:20:00 AM KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 8/16/2012 11:20:00 AM KRICHAR 10 10 Zinc (Zn) 235 ug/L EPA 200.8 8/16/2012 11:20:00 AM KRICHAR 10 10


### 2012016852 Collection Date: 08-Aug-12 8:30 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) 8.73 mg/L EPA 200.7 8/14/2012 10:58:00 AM MHH7131 0.05 10 TOTAL RECOVERABLE METALS BY ICP Boron (B) 220 mg/L EPA 200.7 8/22/2012 12:39:00 PM DJSULL1 0.5 10 Manganese (Mn) 8.79 mg/L EPA 200.7 8/22/2012 12:39:00 PM DJSULL1 0.05 10 DISSOLVED METALS BY ICP-MS Selenium (Se) 114 ug/L EPA 200.8 8/14/2012 2:01:00 PM DJSULL1 10 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 8/16/2012 11:23:00 AM KRICHAR 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 8/16/2012 11:23:00 AM KRICHAR 10 10 Copper (Cu) < 10 ug/L EPA 200.8 8/16/2012 11:23:00 AM KRICHAR 10 10 Nickel (Ni) 115 ug/L EPA 200.8 8/16/2012 11:23:00 AM KRICHAR 10 10 Selenium (Se) 104 ug/L EPA 200.8 8/16/2012 11:23:00 AM KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 8/16/2012 11:23:00 AM KRICHAR 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 8/16/2012 11:23:00 AM 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 # J12080079

2012016853 Collection Date: 08-Aug-12 8:30 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) 218 mg/L EPA 200.7 8/22/2012 12:43:00 PM DJSULL1 0.5 10 Manganese (Mn) 7.57 mg/L EPA 200.7 8/22/2012 12:43:00 PM DJSULL1 0.05 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 8/16/2012 11:26:00 AM KRICHAR 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 8/16/2012 11:26:00 AM KRICHAR 10 10 Copper (Cu) < 10 ug/L EPA 200.8 8/16/2012 11:26:00 AM KRICHAR 10 10 Nickel (Ni) 15.0 ug/L EPA 200.8 8/16/2012 11:26:00 AM KRICHAR 10 10 Selenium (Se) 22.4 ug/L EPA 200.8 8/16/2012 11:26:00 AM KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 8/16/2012 11:26:00 AM KRICHAR 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 8/16/2012 11:26:00 AM KRICHAR 10 10


### 2012016854 Collection Date: 08-Aug-12 8:30 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF INORGANIC IONS BY IC Bromide 120 mg/L EPA 300.0 8/13/2012 6:19:00 PM JAHERMA 5 50 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) < 1 ug/L EPA 245.1 8/16/2012 1:27:33 PM AGIBBS 1 20 TOTAL RECOVERABLE METALS BY ICP Boron (B) 213 mg/L EPA 200.7 8/22/2012 12:47:00 PM DJSULL1 0.5 10 Manganese (Mn) 5.56 mg/L EPA 200.7 8/22/2012 12:47:00 PM DJSULL1 0.05 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 5 ug/L EPA 200.8 8/16/2012 11:29:00 AM KRICHAR 5 5 Chromium (Cr) < 5 ug/L EPA 200.8 8/16/2012 11:29:00 AM KRICHAR 5 5 Copper (Cu) < 5 ug/L EPA 200.8 8/16/2012 11:29:00 AM KRICHAR 5 5 Nickel (Ni) < 5 ug/L EPA 200.8 8/16/2012 11:29:00 AM KRICHAR 5 5 Selenium (Se) 8.35 ug/L EPA 200.8 8/16/2012 11:29:00 AM KRICHAR 5 5 Silver (Ag) < 5 ug/L EPA 200.8 8/16/2012 11:29:00 AM KRICHAR 5 5 Zinc (Zn) < 5 ug/L EPA 200.8 8/16/2012 11:29:00 AM 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 # J12080079

2012016855 Collection Date: 08-Aug-12 8:30 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 8/14/2012 11:02:00 AM MHH7131 0.005 1 DISSOLVED METALS BY ICP-MS Selenium (Se) 1.05 ug/L EPA 200.8 8/14/2012 1:27:00 PM B DJSULL1

1 1


### 2012016856 Collection Date: 08-Aug-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 8/22/2012 12:23:00 PM DJSULL1 0.05 1 Manganese (Mn) < 0.005 mg/L EPA 200.7 8/22/2012 12:23:00 PM DJSULL1 0.005 1 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 1 ug/L EPA 200.8 8/16/2012 10:28:00 AM KRICHAR 1 1 Chromium (Cr) < 1 ug/L EPA 200.8 8/16/2012 10:28:00 AM KRICHAR 1 1 Copper (Cu) < 1 ug/L EPA 200.8 8/16/2012 10:28:00 AM KRICHAR 1 1 Nickel (Ni) < 1 ug/L EPA 200.8 8/16/2012 10:28:00 AM KRICHAR 1 1 Selenium (Se) < 1 ug/L EPA 200.8 8/16/2012 10:28:00 AM KRICHAR 1 1 Silver (Ag) < 1 ug/L EPA 200.8 8/16/2012 10:28:00 AM KRICHAR 1 1 Zinc (Zn) < 1 ug/L EPA 200.8 8/16/2012 10:28:00 AM KRICHAR 1 1 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C


### 2012016857 Collection Date: 08-Aug-12 8:00 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


### 2012016858 Collection Date: 08-Aug-12 8:00 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 # J12080079

2012016858 Collection Date: 08-Aug-12 8:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF


### 2012016859 Collection Date: 08-Aug-12 8:00 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


### 2012016860 Collection Date: 08-Aug-12 8:00 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


### 2012016861 Collection Date: 08-Aug-12 8:00 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


### 2012016862 Collection Date: 08-Aug-12 8:00 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



### Qualifiers: B Target analyte detected in method blank at or above the reporting limit. Target analyte concentration in sample is less than 10X the concentration in the method blank. Analyte concentration in sample could be due to contamination.

## August 20 , 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 #J12080079 )

Dear Mr. Perkins, Attached is the report associated with four (4 ) aqueous samples submitted for selenium speciation analysis on August 9 , 2012. The samples were received in a sealed cooler at -0.3 ° C on August 10 , 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 - FGD WWTS Bi-Monthly Sampling) (LIMS #J12080079)
August 20 , 2012

1. Sample Reception Four (4 ) aqueous samples in 125mL HDPE bottles (provided by Applied Speciation and Consulting) were submitted for selenium speciation analysis on August 9 , 2012. The samples were received on August 10 , 201 2 in a sealed container at -0.3 ° 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 Each sample for selenium speciation analysis w as analyzed by ion chromatography inductively coupled plasma collision reaction cell mass spectrometry (IC-ICP- CRC -MS) on August 17, 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 87.7 65.0 ND (<0.40) ND (<1.7) ND (<1.7) 0.0 (0) BioReactor 1 Inf 23.0 69.3 ND (<0.099) 2.31 ND (<0.42) 0.0 (0) BioReactor 2 Eff ND (<0.81) ND (<0.35) ND (<0.099) ND (<0.42) ND (<0.42) 0.0 (0) Metals Trip Blk ND (<0.032) ND (<0.014) ND (<0.0040) ND (<0.017) ND (<0.017) 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: August 20, 2012 LIMS #J12080079

### Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 10x eMDL 250x Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.0032 0.032 0.81 Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.0014 0.014 0.35 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.00040 0.0040 0.099 MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.0017 0.017 0.42 SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.0017 0.017 0.42 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 9.38 98.0 Se(VI) LCS 9.48 8.95 94.4 SeCN LCS 8.92 8.61 96.5 MeSe(IV) LCS 6.47 6.60 102.0 SeMe LCS 9.32 8.40 90.1 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS Bi-Monthly Sampling)

Contact: Jay Perkins LIMS #J12080079 Date: August 20, 2012 Report Generated by: Russell Gerads

### Quality Control Summary - Matrix Duplicates

Analyte (μg/L) Sample ID Rep 1 Rep 2 Mean RPD Se(IV) BioReactor 2 Eff ND (<0.81) ND (<0.81) NC NC Se(VI) BioReactor 2 Eff ND (<0.35) ND (<0.35) NC NC SeCN BioReactor 2 Eff ND (<0.099) ND (<0.099) NC NC MeSe(IV) BioReactor 2 Eff ND (<0.42) ND (<0.42) NC NC SeMe BioReactor 2 Eff ND (<0.42) ND (<0.42) 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 1390 1484 106.8 1390 1493 107.4 0.6 Se(VI) BioReactor 2 Eff 1261 1301 103.1 1261 1318 104.5 1.3 SeCN BioReactor 2 Eff 1144 1124 98.3 1144 1141 99.7 1.5 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS Bi-Monthly Sampling)

Contact: Jay Perkins LIMS #J12080079 Date: August 20, 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 

### August 24, 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 : J12080079 Dear Mr. Perkins, O n August 10 , 2012, Brooks Rand Labs ( BRL ) received three (3 ) wastewater sample s and three (3) corresponding field blank s. The samples were logged

- in for total mercury (Hg) analysis according to the chain

- of

- custody form. 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(s) 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. Several continuing calibration blanks (CCBs) were analyzed on purge vessel (PV4) to remove any possible carryover. Follow ing the CCBs, a non

- reported continuing calibration verification (CCV) was analyzed on this same purge vessel, which resulted in an elevated recovery (157%). Since the result of the CCV was indicative of the carryover contamination, PV4 retired from service and no other client samples were analyzed using that purge vessel. All samples analyzed on PV4 were re

- analyzed. Sample BioReactor 2 Inf (1232034

- 03) yielded a non

- detectable result. The BRL label and Duke Energy label were verified. The sample was re

- analyzed twice and confirmed the original non

detectable result. Also, the result of field blank sample, Hg Blk BioReactor 2 Eff (1232034

- 06 ), was 29.9 ng/L and was significant when compared to the associated total Hg field sample result. It is entirely likely these samples were mislabeled in the field. All data wa s reported without qualification, aside from concentration qualifiers, and all a ssociated q uality control sample results m et 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,

Tiffany Stilwater Project Manager tiffany@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 1232034-01 BioReactor 1 Inf 08/08/2012 08/10/2012 Sample Influent 1232034-02 Hg Blk BioReactor 1 Inf 08/08/2012 08/10/2012 Field Blank DIW 1232034-03 BioReactor 2 Inf 08/08/2012 08/10/2012 QC Sample Influent 1232034-04 Hg Blk BioReactor 2 Inf 08/08/2012 08/10/2012 Field Blank DIW 1232034-05 BioReactor 2 Eff 08/08/2012 08/10/2012 Sample Effluent 1232034-06 Hg Blk BioReactor 2 Eff 08/08/2012 08/10/2012 Field Blank DIW 

# Batch Summary

Analyte Prepared Analyzed Sequence Batch Lab Matrix Method B121451 08/15/2012 08/17/2012 1200642 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 252 T 1200642 B121451 Influent 40.8 15.3 1232034-01 Hg ng/L

BioReactor 2 Eff 106 T 1200642 B121451 Effluent 4.08 1.53 1232034-05 Hg ng/L

BioReactor 2 Inf 0.15 T U 1200642 B121451 Influent 0.41 0.15 1232034-03 Hg ng/L
Hg Blk BioReactor 1 Inf 0.15 T U 1200642 B121451 DIW 0.40 0.15 1232034-02 Hg ng/L
Hg Blk BioReactor 2 Ef f 29.9 T 1200642 B121451 DIW 0.40 0.15 1232034-06 Hg ng/L
Hg Blk BioReactor 2 Inf 0.15 T U 1200642 B121451 DIW 0.40 0.15 1232034-04 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: B121451

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

Sample Certified Reference Material (1232065, NIST 1641d 1000x dilution) B121451-SRM1 15.68 100% ng/L 85-115 Hg 15.73
Matrix Spike (1232034-01) B121451-MS2 1224 113% ng/L 71-125 Hg 1641

260.0
Matrix Spike Duplicate (1232034-01) B121451-MSD2 1224 112% ng/L 71-125 240.2% Hg 1637

260.0
Matrix Spike (1232034-03) B121451-MS3 2.035 108% ng/L 71-125 Hg 2.19 ND



# Method Blanks & Reporting Limits

Batch: B121451
Method: EPA 1631 Matrix: Water Analyte: Hg Result Units Sample B121451-BLK1 ng/L 0.23 B121451-BLK2 ng/L 0.17 B121451-BLK3 ng/L 0.08 B121451-BLK4 ng/L 0.07 MDL: 0.15 Average: 0.14 Standard Deviation: 0.08 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: 1200642 Method: EPA 1631 Instrument: THG-05 Date: 08/17/2012 Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg REC & Limits Result True Value Lab ID Units 1200642-IBL1 5.91 pg of Hg 1200642-IBL2 5.43 pg of Hg 1200642-IBL3 4.83 pg of Hg 1200642-IBL4 6.71 pg of Hg 1200642-CAL1 25.00 25.25 pg of Hg 101% 1200642-CAL2 100.0 93.67 pg of Hg 94% 1200642-CAL3 500.0 477.2 pg of Hg 95% 1200642-CAL4 2500 2661 pg of Hg 106% 1200642-CAL5 10000 10470 pg of Hg 105% 1200642-ICV1 1568 1573 pg of Hg 100% 85-115 1200642-CCV1 500.0 469.5 pg of Hg 94% 77-123 1200642-CCB1 12.0 pg of Hg 1200642-CCB2 3260 pg of Hg 1200642-CCB3 462 pg of Hg 1200642-CCB4 645 pg of Hg 1200642-CCB5 378 pg of Hg 1200642-CCB6 284 pg of Hg 1200642-CCB7 357 pg of Hg 1200642-CCB8 222 pg of Hg 1200642-CCV3 500.0 516.3 pg of Hg 103% 77-123 1200642-CCB9 2.30 pg of Hg 1200642-CCV4 500.0 546.6 pg of Hg 109% 77-123 1200642-CCBA 3.49 pg of Hg 1200642-ICB2 9.07 pg of Hg 1200642-CCV5 500.0 546.0 pg of Hg 109% 77-123

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: 1232034-01 Report Matrix: Influent Sample Type: Sample Received: 08/10/2012 Sample: BioReactor 1 Inf Collected: 08/08/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71392670 10 Cooler

none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 1232034-02 Report Matrix: DIW Sample Type: Field Blank Received: 08/10/2012 Sample: Hg Blk BioReactor 1 Inf Collected: 08/08/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71392670 10 Cooler

none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 1232034-03 Report Matrix: Influent Sample Type: QC Sample Received: 08/10/2012 Sample: BioReactor 2 Inf Collected: 08/08/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71392670 10 Cooler

none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 1232034-04 Report Matrix: DIW Sample Type: Field Blank Received: 08/10/2012 Sample: Hg Blk BioReactor 2 Inf Collected: 08/08/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71392670 10 Cooler

none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 1232034-05 Report Matrix: Effluent Sample Type: Sample Received: 08/10/2012 Sample: BioReactor 2 Eff Collected: 08/08/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71392670 10 Cooler

none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 1232034-06 Report Matrix: DIW Sample Type: Field Blank Received: 08/10/2012 Sample: Hg Blk BioReactor 2 Eff Collected: 08/08/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71392670 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 2892 via FedEx Temperature: -0.8 °C Coolant T

ype: Ice Description: Cooler Damaged in transit? No Returned to client? No Custody seals present? No Custody seals intact? No COC present? Yes Received: August 10, 2012 9:00

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