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: J11080323 Project Name: WWTS - Biweekly

Lab Contact: Jason C Perkins
Date: 9/7/2011 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 2011017841 BELEWS 24-Aug-11 8:05 AM TO FGD Purge Eff 2011017842 BELEWS 24-Aug-11 8:10 AM TO EQ TANK EFF. 2011017843 BELEWS 24-Aug-11 8:24 AM TO BIOREACTOR 1 INF. 2011017844 BELEWS 24-Aug-11 8:24 AM TO BIOREACTOR 2 INF. 2011017845 BELEWS 24-Aug-11 8:24 AM TO BIOREACTOR 2 EFF. 2011017846 BELEWS 16-Aug-11 11:40 AM L.DAVIS Trip Blank 2011017847 BELEWS 16-Aug-11 11:40 AM L.DAVIS FILTER BLANK 7 Total SamplesCOC and .pdf report are in agreement with sample totals and analyses (compliance programs and procedures). All Results are less than the laboratory reporting limits. All laboratory QA/QC requirements are acceptable. 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: 9/7/2011 Yes

Electronic Data Deliverable (EDD) Sent Separately

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

### Order # J11080323

2011017841 Collection Date: 24-Aug-11 8:05 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 96 mg/L EPA 300.0 31-Aug-11 02:12 JAHERMA 10 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 36.2 ug/L EPA 245.1 26-Aug-11 09:25 AGIBBS 5
TOTAL RECOVERABLE METALS BY ICP Boron (B) 166 mg/L EPA 200.7 31-Aug-11 14:06 DJSULL1 0.5
DISSOLVED METALS BY ICP-MS Selenium (Se) 169 ug/L EPA 200.8 31-Aug-11 12:18 MHH7131 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 24.5 ug/L EPA 200.8 31-Aug-11 12:01 MHH7131 10 Chromium (Cr) 26.4 ug/L EPA 200.8 31-Aug-11 12:01 MHH7131 10 Copper (Cu) 19.2 ug/L EPA 200.8 31-Aug-11 12:01 MHH7131 10 Nickel (Ni) 104 ug/L EPA 200.8 31-Aug-11 12:01 MHH7131 10 Selenium (Se) 745 ug/L EPA 200.8 31-Aug-11 12:01 MHH7131 10 Silver (Ag) < 10 ug/L EPA 200.8 31-Aug-11 12:01 MHH7131 10 Zinc (Zn) 61.9 ug/L EPA 200.8 31-Aug-11 12:01 MHH7131 20
SELENIUM SPECIATION Vendor Parameter Complete V_AS&C
TOTAL DISSOLVED SOLIDS TDS 18000 mg/L SM2540C 31-Aug-11 11:50 TJA7067 200 2011017842 Collection Date: 24-Aug-11 8:10 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) 204 ug/L EPA 245.1 26-Aug-11 09:27 AGIBBS 2.5
TOTAL RECOVERABLE METALS BY ICP Boron (B) 161 mg/L EPA 200.7 31-Aug-11 14:10 DJSULL1 0.5
DISSOLVED METALS BY ICP-MS Selenium (Se) 123 ug/L EPA 200.8 31-Aug-11 12:21 MHH7131 10

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

### Order # J11080323

2011017842 Collection Date: 24-Aug-11 8:10 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) 194 ug/L EPA 200.8 31-Aug-11 12:04 MHH7131 10 Chromium (Cr) 239 ug/L EPA 200.8 31-Aug-11 12:04 MHH7131 10 Copper (Cu) 161 ug/L EPA 200.8 31-Aug-11 12:04 MHH7131 10 Nickel (Ni) 201 ug/L EPA 200.8 31-Aug-11 12:04 MHH7131 10 Selenium (Se) 4650 ug/L EPA 200.8 31-Aug-11 12:04 MHH7131 10 Silver (Ag) < 10 ug/L EPA 200.8 31-Aug-11 12:04 MHH7131 10 Zinc (Zn) 275 ug/L EPA 200.8 31-Aug-11 12:04 MHH7131 20 2011017843 Collection Date: 24-Aug-11 8:24 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) 141 mg/L EPA 200.7 31-Aug-11 14:14 DJSULL1 0.5
DISSOLVED METALS BY ICP-MS Selenium (Se) 102 ug/L EPA 200.8 31-Aug-11 12:24 MHH7131 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 31-Aug-11 12:08 MHH7131 10 Chromium (Cr) < 10 ug/L EPA 200.8 31-Aug-11 12:08 MHH7131 10 Copper (Cu) 17.5 ug/L EPA 200.8 31-Aug-11 12:08 MHH7131 10 Nickel (Ni) 16.1 ug/L EPA 200.8 31-Aug-11 12:08 MHH7131 10 Selenium (Se) 330 ug/L EPA 200.8 31-Aug-11 12:08 MHH7131 10 Silver (Ag) < 10 ug/L EPA 200.8 31-Aug-11 12:08 MHH7131 10 Zinc (Zn) < 20 ug/L EPA 200.8 31-Aug-11 12:08 MHH7131 20
SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 2011017844 Collection Date: 24-Aug-11 8:24 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) 144 mg/L EPA 200.7 31-Aug-11 14:18 DJSULL1 0.5

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

### Order # J11080323

2011017844 Collection Date: 24-Aug-11 8:24 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 ug/L EPA 200.8 31-Aug-11 12:11 MHH7131 10 Chromium (Cr) < 10 ug/L EPA 200.8 31-Aug-11 12:11 MHH7131 10 Copper (Cu) < 10 ug/L EPA 200.8 31-Aug-11 12:11 MHH7131 10 Nickel (Ni) < 10 ug/L EPA 200.8 31-Aug-11 12:11 MHH7131 10 Selenium (Se) 22.0 ug/L EPA 200.8 31-Aug-11 12:11 MHH7131 10 Silver (Ag) < 10 ug/L EPA 200.8 31-Aug-11 12:11 MHH7131 10 Zinc (Zn) < 20 ug/L EPA 200.8 31-Aug-11 12:11 MHH7131 20 2011017845 Collection Date: 24-Aug-11 8:24 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 91 mg/L EPA 300.0 31-Aug-11 03:15 JAHERMA 10 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) < 1 ug/L EPA 245.1 26-Aug-11 09:34 AGIBBS 1
TOTAL RECOVERABLE METALS BY ICP Boron (B) 145 mg/L EPA 200.7 31-Aug-11 14:22 DJSULL1 0.5
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 31-Aug-11 12:14 MHH7131 10 Chromium (Cr) < 10 ug/L EPA 200.8 31-Aug-11 12:14 MHH7131 10 Copper (Cu) < 10 ug/L EPA 200.8 31-Aug-11 12:14 MHH7131 10 Nickel (Ni) < 10 ug/L EPA 200.8 31-Aug-11 12:14 MHH7131 10 Selenium (Se) < 10 ug/L EPA 200.8 31-Aug-11 12:14 MHH7131 10 Silver (Ag) < 10 ug/L EPA 200.8 31-Aug-11 12:14 MHH7131 10 Zinc (Zn) < 20 ug/L EPA 200.8 31-Aug-11 12:14 MHH7131 20
SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 2011017846 Collection Date: 16-Aug-11 11:40 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) < 0.05 mg/L EPA 200.7 31-Aug-11 14:02 DJSULL1 0.05

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

### Order # J11080323

2011017846 Collection Date: 16-Aug-11 11:40 AM Site: Trip Blank Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sam p le #:

Analyst TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 1 ug/L EPA 200.8 31-Aug-11 11:55 MHH7131 1 Chromium (Cr) < 1 ug/L EPA 200.8 31-Aug-11 11:55 MHH7131 1 Copper (Cu) < 1 ug/L EPA 200.8 31-Aug-11 11:55 MHH7131 1 Nickel (Ni) < 1 ug/L EPA 200.8 31-Aug-11 11:55 MHH7131 1 Selenium (Se) < 1 ug/L EPA 200.8 31-Aug-11 11:55 MHH7131 1 Silver (Ag) < 1 ug/L EPA 200.8 31-Aug-11 11:55 MHH7131 1 Zinc (Zn) < 2 ug/L EPA 200.8 31-Aug-11 11:55 MHH7131 2
SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 2011017847 Collection Date: 16-Aug-11 11:40 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 ug/L EPA 200.8 31-Aug-11 11:58 MHH7131 1

### August 30 , 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 #J11080323 )

Dear Mr. Perkins , Attached is the report associated with four (4 ) aqueous samples submitted for selenium speciation analysis on August 25 , 2011. The samples were received in a sealed cooler at -0. 3 o 

### C on August 2 6 , 2011. Selenium speciation analysis was performed via ion chromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICP-DRC-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,

Ben Wozniak Project Manager 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 #J11080323)

August 30 , 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 August 2 5 , 2011 . The samples were received on August 2 6 , 2011 in a sealed container at -0. 3 o 

### C. The samples were received in a laminar flow clean hood void of trace metals contamination and ultra-violet radiation. Upon reception, the samples were designated discrete sample identifiers. An aliquot of each sample was filtered (0.45μm) and these filtrates were 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 the samples 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 All samples for selenium speciation analysis were analyzed by ion chromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICP-DRC-MS) on August 2 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 i s 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 q uality control parameters associated with these 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,

Ben Wozniak Project Manager Applied Speciation and Consulting, LLCSample Results
Sample ID Se(IV) Se(VI) SeCN MeSe(IV) SeMe Unknown Se Species (n) FGD Purge Eff 25.9 90.5 ND (<3.4) ND (<3.4) ND (<3.4) 0 (0) BioReactor 1 Inf 10.8 40.1 ND (<0.86) 0.88 ND (<0.85) 0 (0) BioReactor 2 Eff ND (<0.82) ND (<0.87) ND (<0.86) ND (<0.85) ND (<0.85) 0 (0) Metals Trip Blk ND (<0.16) ND (<0.17) ND (<0.17) ND (<0.17) ND (<0.17) 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: Ben Wozniak Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews – FGD WWTS (Bi-Monthly Sampling)

Contact: Jay Perkins

Date: August 30, 2011 LIMS #J11080323Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 10x eMDL 50x eMDL 200x Se(IV) -0.07 -0.07 -0.07 -0.07 -0.07 0.00 0.016 0.16 0.82 3.3 Se(VI) 0.00 0.00 0.00 0.00 0.00 0.00 0.017 0.17 0.87 3.5 SeCN 0.00 0.00 0.00 0.00 0.00 0.00 0.017 0.17 0.86 3.4 MeSe(IV) 0.00 0.00 0.00 0.00 0.00 0.00 0.017 0.17 0.85 3.4 SeMe 0.00 0.00 0.00 0.00 0.00 0.00 0.017 0.17 0.85 3.4 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 10.15 106.0 Se(VI) LCS 9.48 9.779 103.2 SeCN LCS 8.92 9.296 104.2 MeSe(IV) LCS 6.47 7.082 109.5 SeMe LCS 9.32 9.635 103.4 Report Generated by: Ben Wozniak Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews – FGD WWTS (Bi-Monthly Sampling)

Contact: Jay Perkins LIMS #J11080323 Date: August 30, 2011Quality Control Summary - Matrix Duplicates Analyte (μg/L) Sample ID Rep 1 Rep 2 Mean RPD Se(IV) BioReactor 2 Eff ND (<0.82) ND (<0.82) NC NC Se(VI) BioReactor 2 Eff ND (<0.87) ND (<0.87) NC NC SeCN BioReactor 2 Eff ND (<0.86) ND (<0.86) NC NC MeSe(IV) BioReactor 2 Eff ND (<0.85) ND (<0.85) NC NC SeMe BioReactor 2 Eff ND (<0.85) ND (<0.85) 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 278.0 282.3 101.5 278.0 284.2 102.2 0.7 Se(VI) BioReactor 2 Eff 252.3 255.6 101.3 252.3 259.6 102.9 1.6 SeCN BioReactor 2 Eff 228.8 220.0 96.2 228.8 220.4 96.4 0.2 Date: August 30, 2011 Report Generated by: Ben Wozniak Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews – FGD WWTS (Bi-Monthly Sampling)

Contact: Jay Perkins LIMS #J11080323