### 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: J11120115

Lab Contact: Jason C Perkins 

### Date: 1/4/2012 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 Perk ins) 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 re sults) under the qualifiers heading. All results are repor ted on a dry weight basis unless otherwise noted. Data Package: This data package includes analytical results that are applicable only to the samples described in this narrative. An estimatio n of the uncertainty of measurement for the results in the report is available upon request. This report shall not be reproduced, ex cept in full, without the written consent of the Analytical Laborator y. 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 Certificati ons : North Carolina (DENR) Certificate #248, South Carolina (DHEC) Laboratory ID # 99005. Contact t he Analytical Laboratory for definitive inform ation about the certification status of specific methods.

## Sample ID's & Descriptions: Sample ID Plant/Station Collection Date and Time Collected By Sample Description 2011026219 BELEWS 14-Dec-11 11:30 AM DAVID MORRIS FGD Purge Eff 2011026342 BELEWS 14-Dec-11 11:30 AM DAVID MORRIS EQ TANK EFF. 2011026343 BELEWS 14-Dec-11 11:30 AM DAVID MORRIS BIOREACTOR 1 INF. 2011026344 BELEWS 14-Dec-11 11:30 AM DAVID MORRIS BIOREACTOR 2 INF. 2011026345 BELEWS 14-Dec-11 11:30 AM DAVID MORRIS BIOREACTOR 2 EFF. 2011026346 BELEWS 14-Dec-11 11:30 AM DAVID MORRIS FILTER BLANK 2011026347 BELEWS 14-Dec-11 11:30 AM DAVID MORRIS Trip Blank 2011026356 BELEWS 14-Dec-11 11:40 AM DAVID MORRIS BIOREACTOR 1 INF. 2011026357 BELEWS 14-Dec-11 11:40 AM DAVID MORRIS HG BLANK BIOREACTOR 1 INF. 2011026358 BELEWS 14-Dec-11 11:50 AM DAVID MORRIS BIOREACTOR 2 INF. 2011026359 BELEWS 14-Dec-11 11:50 AM DAVID MORRIS Hg Blk BioReactor 2 Inf 2011026360 BELEWS 14-Dec-11 11:45 AM DAVID MORRIS BIOREACTOR 2 EFF. 2011026361 BELEWS 14-Dec-11 11:45 AM DAVID MORRIS 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. The Vendor Laboratories have been qualified by the Analytical Laboratory 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: 

### Mary Ann Ogle Date: 

### 1/4/2012 Yes

Electronic Data Deliverable (EDD) Sent Separately

# Certificate of Laboratory Analysis This rep ort shall not be re p roduced, exce p t in full. 

### Order # J11120115

2011026219 Collection Date: 14-Dec-11 11:30 AM 

### Site: FGD Purge Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst INORGANIC IONS BY IC Bromide 84 mg/L EPA 300.0 19-Dec-11 19:30 JAHERMA 5 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 229 ug/L EPA 245.1 16-Dec-11 09:09 AGIBBS 5 TOTAL RECOVERABLE METALS BY ICP Boron (B) 146 mg/L EPA 200.7 16-Dec-11 10:17 DJSULL1 0.5 DISSOLVED METALS BY ICP-MS Selenium (Se) 419 ug/L EPA 200.8 20-Dec-11 10:55 MHH7131 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 170 ug/L EPA 200.8 21-Dec-11 09:43 MHH7131 10 Chromium (Cr) 172 ug/L EPA 200.8 21-Dec-11 09:43 MHH7131 10 Copper (Cu) 108 ug/L EPA 200.8 21-Dec-11 09:43 MHH7131 10 Nickel (Ni) 166 ug/L EPA 200.8 21-Dec-11 09:43 MHH7131 10 Selenium (Se) 4440 ug/L EPA 200.8 21-Dec-11 09:43 MHH7131 10 Silver (Ag) < 10.0 ug/L EPA 200.8 21-Dec-11 09:43 MHH7131 10 Zinc (Zn) 181 ug/L EPA 200.8 21-Dec-11 09:43 MHH7131 20 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C TOTAL DISSOLVED SOLIDS TDS 15000 mg/L SM2540C 19-Dec-11 14:36 AGIBBS 200 

### 2011026342 Collection Date: 14-Dec-11 11:30 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 208 ug/L EPA 245.1 16-Dec-11 09:12 AGIBBS 2.5 TOTAL RECOVERABLE METALS BY ICP Boron (B) 152 mg/L EPA 200.7 16-Dec-11 10:21 DJSULL1 0.5 DISSOLVED METALS BY ICP-MS Selenium (Se) 180 ug/L EPA 200.8 20-Dec-11 10:55 MHH7131 10

# Certificate of Laboratory Analysis This rep ort shall not be re p roduced, exce p t in full. 

### Order # J11120115

2011026342 Collection Date: 14-Dec-11 11:30 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 164 ug/L EPA 200.8 21-Dec-11 09:46 MHH7131 10 Chromium (Cr) 169 ug/L EPA 200.8 21-Dec-11 09:46 MHH7131 10 Copper (Cu) 106 ug/L EPA 200.8 21-Dec-11 09:46 MHH7131 10 Nickel (Ni) 162 ug/L EPA 200.8 21-Dec-11 09:46 MHH7131 10 Selenium (Se) 4160 ug/L EPA 200.8 21-Dec-11 09:46 MHH7131 10 Silver (Ag) < 10.0 ug/L EPA 200.8 21-Dec-11 09:46 MHH7131 10 Zinc (Zn) 178 ug/L EPA 200.8 21-Dec-11 09:46 MHH7131 20 

### 2011026343 Collection Date: 14-Dec-11 11:30 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst TOTAL RECOVERABLE METALS BY ICP Boron (B) 146 mg/L EPA 200.7 16-Dec-11 10:25 DJSULL1 0.5 DISSOLVED METALS BY ICP-MS Selenium (Se) 141 ug/L EPA 200.8 20-Dec-11 10:55 MHH7131 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10.0 ug/L EPA 200.8 21-Dec-11 09:49 MHH7131 10 Chromium (Cr) < 10.0 ug/L EPA 200.8 21-Dec-11 09:49 MHH7131 10 Copper (Cu) < 10.0 ug/L EPA 200.8 21-Dec-11 09:49 MHH7131 10 Nickel (Ni) 39.7 ug/L EPA 200.8 21-Dec-11 09:49 MHH7131 10 Selenium (Se) 133 ug/L EPA 200.8 21-Dec-11 09:49 MHH7131 10 Silver (Ag) < 10.0 ug/L EPA 200.8 21-Dec-11 09:49 MHH7131 10 Zinc (Zn) < 20.0 ug/L EPA 200.8 21-Dec-11 09:49 MHH7131 20 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011026344 Collection Date: 14-Dec-11 11:30 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst TOTAL RECOVERABLE METALS BY ICP Boron (B) 138 mg/L EPA 200.7 16-Dec-11 10:29 DJSULL1 0.5

# Certificate of Laboratory Analysis This rep ort shall not be re p roduced, exce p t in full. 

### Order # J11120115

2011026344 Collection Date: 14-Dec-11 11:30 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10.0 ug/L EPA 200.8 21-Dec-11 09:52 MHH7131 10 Chromium (Cr) < 10.0 ug/L EPA 200.8 21-Dec-11 09:52 MHH7131 10 Copper (Cu) < 10.0 ug/L EPA 200.8 21-Dec-11 09:52 MHH7131 10 Nickel (Ni) < 10.0 ug/L EPA 200.8 21-Dec-11 09:52 MHH7131 10 Selenium (Se) 14.5 ug/L EPA 200.8 21-Dec-11 09:52 MHH7131 10 Silver (Ag) < 10.0 ug/L EPA 200.8 21-Dec-11 09:52 MHH7131 10 Zinc (Zn) < 20.0 ug/L EPA 200.8 21-Dec-11 09:52 MHH7131 20 

### 2011026345 Collection Date: 14-Dec-11 11:30 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst INORGANIC IONS BY IC Bromide 82 mg/L EPA 300.0 19-Dec-11 19:46 JAHERMA 5 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) < 1.00 ug/L EPA 245.1 16-Dec-11 09:14 AGIBBS 1 TOTAL RECOVERABLE METALS BY ICP Boron (B) 129 mg/L EPA 200.7 16-Dec-11 10:32 DJSULL1 0.5 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 5.00 ug/L EPA 200.8 21-Dec-11 09:55 MHH7131 5 Chromium (Cr) < 5.00 ug/L EPA 200.8 21-Dec-11 09:55 MHH7131 5 Copper (Cu) < 5.00 ug/L EPA 200.8 21-Dec-11 09:55 MHH7131 5 Nickel (Ni) < 5.00 ug/L EPA 200.8 21-Dec-11 09:55 MHH7131 5 Selenium (Se) < 5.00 ug/L EPA 200.8 21-Dec-11 09:55 MHH7131 5 Silver (Ag) < 5.00 ug/L EPA 200.8 21-Dec-11 09:55 MHH7131 5 Zinc (Zn) < 10.0 ug/L EPA 200.8 21-Dec-11 09:55 MHH7131 10 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011026346 Collection Date: 14-Dec-11 11:30 AM 

### Site: FILTER BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DISSOLVED METALS BY ICP-MS Selenium (Se) < 1.000 ug/L EPA 200.8 20-Dec-11 10:55 MHH7131 1

# Certificate of Laboratory Analysis This rep ort shall not be re p roduced, exce p t in full. 

### Order # J11120115

2011026347 Collection Date: 14-Dec-11 11:30 AM 

### Site: Trip Blank Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst TOTAL RECOVERABLE METALS BY ICP Boron (B) < 0.050 mg/L EPA 200.7 16-Dec-11 10:13 DJSULL1 0.05 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 1.000 ug/L EPA 200.8 21-Dec-11 09:40 MHH7131 1 Chromium (Cr) < 1.000 ug/L EPA 200.8 21-Dec-11 09:40 MHH7131 1 Copper (Cu) < 1.000 ug/L EPA 200.8 21-Dec-11 09:40 MHH7131 1 Nickel (Ni) < 1.000 ug/L EPA 200.8 21-Dec-11 09:40 MHH7131 1 Selenium (Se) < 1.000 ug/L EPA 200.8 21-Dec-11 09:40 MHH7131 1 Silver (Ag) < 1.000 ug/L EPA 200.8 21-Dec-11 09:40 MHH7131 1 Zinc (Zn) < 2.00 ug/L EPA 200.8 21-Dec-11 09:40 MHH7131 2 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011026356 Collection Date: 14-Dec-11 11:40 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND 

### 2011026357 Collection Date: 14-Dec-11 11:40 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND 

### 2011026358 Collection Date: 14-Dec-11 11:50 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND

# Certificate of Laboratory Analysis This rep ort shall not be re p roduced, exce p t in full. 

### Order # J11120115

2011026359 Collection Date: 14-Dec-11 11:50 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND 

### 2011026360 Collection Date: 14-Dec-11 11:45 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND 

### 2011026361 Collection Date: 14-Dec-11 11:45 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND

## December 22 , 201 1

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 # J111 20 115 )

Dear Mr. Perkins, Attached is the report associated with four (4 ) aqueous samples submitted for selenium speciation analysis on December 1 5 , 2011. The samples were received in a sealed cooler at- 0. 7 ° C on December 16, 2011. Selenium speciation analysis was performed via ionchromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICPDRC-MS). Any issues associated with the analysis are addressed in the following report. If you have any questions, please feel free to contact me at your convenience.
Sincerely,

Russell Gerads Vice President Applied Speciation and Consulting, LLC

## Applied Speciation and Consulting, LLC Report prepared for: Jay Perkins Duke Energy Analytical Laboratory Mail Code MGO3A2 (Building 7405) 13339 Hagers Ferry Rd. Huntersville, NC 28078 Project: Belews

– FGD WWTS Bi-Monthly Sampling) (LIMS # J111 20115 )

December 22 , 2011

1. Sample Reception Four (4 ) aqueous samples in 125mL HDPE bottles (provided by Applied Speciation and Consulting) were submitted for selenium speciation analysi s on December 15 , 2011 . The samples were received on December 1 6 , 2011 in a sealed container at -0. 7° C. The samples were received in a laminar flow clean hood, void of trace metals contamination and ultra-violet radiation, and was designated a discrete sample identifier. An aliquot of each sample was filtered (0.45μm) and each filtrate w as stored in a secure, monitored cryofreezer (maintained at a temperature of -80 o 

## C) until selenium speciation analysis could be performed via ion chromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICP-DRC-MS).

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

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

- MS Each sample for selenium speciation analysis w as analyzed by ion chromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICP-DRC-MS) on December 1 6 , 2011 . 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 (DRC) containing a specific reactive 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. A ll quality control parameters associated with this sample 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 54.1 85.8 7.6 ND (<1.9) ND (<1.9) 0 (0) BioReactor 1 Inf 19.3 92.0 ND (<0.39) ND (<0.47) ND (<0.47) 2.00 (1) BioReactor 2 Eff ND (<0.56) ND (<0.47) ND (<0.39) ND (<0.47) ND (<0.47) 0 (0) Metals Trip Blk ND (<0.11) ND (<0.093) ND (<0.078) ND (<0.094) ND (<0.094) 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: December 22, 2011 LIMS #J11120115

### Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 10x eMDL 50x eMDL 200x Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.011 0.11 0.56 2.2 Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.009 0.093 0.47 1.9 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.078 0.39 1.6 MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.009 0.094 0.47 1.9 SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.009 0.094 0.47 1.9 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 3.83 4.09 106.8 Se(VI) LCS 3.79 4.18 110.1 SeCN LCS 3.57 3.83 107.3 MeSe(IV) LCS 2.59 2.52 97.4 SeMe LCS 3.73 3.77 101.1 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS Bi-Monthly Sampling)

Contact: Jay Perkins LIMS #J11120115 Date: December 22, 2011 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 (<0.56) ND (<0.56) NC NC Se(VI) BioReactor 2 Eff ND (<0.47) ND (<0.47) NC NC SeCN BioReactor 2 Eff ND (<0.39) ND (<0.39) NC NC MeSe(IV) BioReactor 2 Eff ND (<0.47) ND (<0.47) NC NC SeMe BioReactor 2 Eff ND (<0.47) ND (<0.47) NC NC ND = Not detected at the applied dilution NC = Value was not calculated due to one or more concentrations below the eMDL

Quality Control Summary - Matrix Spike/ Matrix Spike Duplicate Analyte (μg/L) Sample ID Spike Conc MS Result Recovery Spike Conc MSD Result Recovery RPD Se(IV) BioReactor 2 Eff 278.0 266.0 95.7 278.0 261.6 94.1 1.6 Se(VI) BioReactor 2 Eff 252.3 252.5 100.1 252.3 251.7 99.8 0.3 SeCN BioReactor 2 Eff 228.8 211.8 92.6 228.8 213.0 93.1 0.6 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS Bi-Monthly Sampling)

Contact: Jay Perkins LIMS #J11120115 Date: December 22, 2011 Report Generated by: Russell Gerads

### December 28, 2011

Duke Energy ATTN: Jay Perkins 13339 Hagers Ferry Road Huntersville NC 28078 jperkins@duke-energy.com
RE: Project DUK-HV1101 Client Project: J11120115 Dear Jay Perkins, This report contains results for the 6 samples received by Brooks Rand Labs (BRL) on December 16, 2011. The samples were logged-in for the contracted analyses according to the chain-of-custody form(s). The samples were received, prepared, analyzed, and stored according to BRL SOPs and EPA methodology. The results were method blank corrected as described in the calculations section of the relevant BRL 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 sample-specific MDLs, MRLs, and other details. All data is reported without qualification (with the exception of concentration qualifiers), and all associated quality control sample results meet the acceptance criteria. BRL, an accredited laboratory, certifies that the reported results of all analyses for which BRL is NELAP accredited meet all NELAP requirements. For more details, please see the 

### Report Information page in your report. Please feel free to contact me if you have any questions regarding this report. Sincerely,

Tiffany Stilwater Project Manager tiffany@brooksrand.com

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: DUK-HV1101

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, Ltd ., those found in the EPA SOW ILM03.0, Exhibit B, Section III, pg. B-18, and the USEPA Laboratory Data Validation Functional Guidelines for Evaluating Inorganic Analyses; USEPA; July 2002. 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-HV1101

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



# Sample Information

Report Matrix Type Received Sampled Sample Lab ID 1151039-01 BioReactor 1 Inf 12/14/2011 12/16/2011 Sample Influent 1151039-02 Hg Blk BioReactor 1 Inf 12/14/2011 12/16/2011 Field Blank DIW 1151039-03 BioReactor 2 Inf 12/14/2011 12/16/2011 QC Sample Influent 1151039-04 Hg Blk BioReactor 2 Inf 12/14/2011 12/16/2011 Field Blank DIW 1151039-05 BioReactor 2 Eff 12/14/2011 12/16/2011 Sample Effluent 1151039-06 Hg Blk BioReactor 2 Eff 12/14/2011 12/16/2011 Field Blank DIW 

# Batch Summary

Analyte Prepared Analyzed Sequence Batch Lab Matrix Method B112132 12/19/2011 12/20/2011 1100906 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-HV1101

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



# Sample Results

Sample Sequence Result MDL MRL Unit Batch

Qualifier Analyte Fraction

Report Matrix BioReactor 1 Inf ng/L 161 T 1100906 B112132 Influent 4.04 1.52 1151039-01 Hg

BioReactor 2 Eff ng/L 39.4 T 1100906 B112132 Effluent 1.61 0.61 1151039-05 Hg

BioReactor 2 Inf ng/L 102 T 1100906 B112132 Influent 4.04 1.52 1151039-03 Hg
Hg Blk BioReactor 1 Inf ng/L 0.15 T U 1100906 B112132 DIW 0.40 0.15 1151039-02 Hg
Hg Blk BioReactor 2 Eff ng/L 0.15 T U 1100906 B112132 DIW 0.40 0.15 1151039-06 Hg
Hg Blk BioReactor 2 Inf ng/L 0.15 T U 1100906 B112132 DIW 0.40 0.15 1151039-04 Hg

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: DUK-HV1101

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



# Accuracy & Precision Summary

Batch: B112132

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

Sample Certified Reference Material (1149037, NIST 1641d 1000x dilution) B112132-SRM1 15.68 98% ng/L 85-115 Hg 15.29
Matrix Spike (1151039-03) B112132-MS2 505.1 111% ng/L 71-125 Hg 664.3

102.3
Matrix Spike Duplicate (1151039-03) B112132-MSD2 505.1 108% ng/L 71-125 242% Hg 648.2

102.3
Matrix Spike (1151039-05) B112132-MS3 177.4 107% ng/L 71-125 Hg 228.6

39.35
Matrix Spike Duplicate (1151039-05) B112132-MSD3 180.9 103% ng/L 71-125 241% Hg 226.1

39.35

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: DUK-HV1101

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



# Method Blanks & Reporting Limits

Batch: B112132
Method: EPA 1631 Matrix: Water Analyte: Hg Result Units Sample B112132-BLK1 ng/L 0.06 B112132-BLK2 ng/L 0.08 B112132-BLK3 ng/L 0.06 B112132-BLK4 ng/L 0.04 MDL: 0.15 Average: 0.06 Standard Deviation: 0.02 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-HV1101

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



# Instrument Calibration

Sequence: 1100906 Method: EPA 1631 Instrument: THG-10 Date: 12/20/2011 Total Mercury and Mercury Speciation by CVAFS
Analyte: Hg REC & Limits Result True Value Lab ID Units 1100906-IBL1 3.72 pg of Hg 1100906-IBL2 3.49 pg of Hg 1100906-IBL3 3.46 pg of Hg 1100906-IBL4 4.98 pg of Hg 1100906-CAL1 25.00 24.38 pg of Hg 98% 1100906-CAL2 100.0 98.22 pg of Hg 98% 1100906-CAL3 500.0 482.6 pg of Hg 97% 1100906-CAL4 2500 2687 pg of Hg 107% 1100906-CAL5 10000 10100 pg of Hg 101% 1100906-ICV1 1568 1529 pg of Hg 98% 85-115 1100906-CCB1 6.98 pg of Hg 1100906-CCV1 500.0 532.2 pg of Hg 106% 77-123 1100906-CCV2 500.0 515.4 pg of Hg 103% 77-123 1100906-CCV3 500.0 514.5 pg of Hg 103% 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-HV1101

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



# Sample Containers

Lab ID: 1151039-01 Report Matrix: Influent Sample Type: Sample Received: 12/16/2011 Sample: BioReactor 1 Inf Collected: 12/14/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71470160 10 Cooler

none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 1151039-02 Report Matrix: DIW Sample Type: Field Blank Received: 12/16/2011 Sample: Hg Blk BioReactor 1 Inf Collected: 12/14/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71470160 10 Cooler

none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 1151039-03 Report Matrix: Influent Sample Type: QC Sample Received: 12/16/2011 Sample: BioReactor 2 Inf Collected: 12/14/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71470160 10 Cooler

none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 1151039-04 Report Matrix: DIW Sample Type: Field Blank Received: 12/16/2011 Sample: Hg Blk BioReactor 2 Inf Collected: 12/14/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71470160 10 Cooler

none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 1151039-05 Report Matrix: Effluent Sample Type: Sample Received: 12/16/2011 Sample: BioReactor 2 Eff Collected: 12/14/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71470160 10 Cooler

none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 1151039-06 Report Matrix: DIW Sample Type: Field Blank Received: 12/16/2011 Sample: Hg Blk BioReactor 2 Eff Collected: 12/14/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71470160 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-HV1101

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



# Shipping Containers

Cooler Tracking No: 4726 7966 6868 via FedEx Temperature: 1.7 °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: December 16, 2011 9:00

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