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: J11120353 Project Name: WWTS - Biweekly

Lab Contact: Jason C Perkins
Date: 1/11/2012 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 2011027515 BELEWS 28-Dec-11 8:15 AM TRAVIS THORNTON FGD Purge Eff 2011027516 BELEWS 28-Dec-11 8:15 AM TRAVIS THORNTON EQ TANK EFF. 2011027517 BELEWS 28-Dec-11 8:15 AM TRAVIS THORNTON BIOREACTOR 1 INF. 2011027518 BELEWS 28-Dec-11 8:15 AM TRAVIS THORNTON BIOREACTOR 2 INF. 2011027519 BELEWS 28-Dec-11 8:15 AM TRAVIS THORNTON BIOREACTOR 2 EFF. 2011027520 BELEWS 28-Dec-11 8:15 AM TRAVIS THORNTON FILTER BLANK 2011027521 BELEWS 21-Dec-11 8:20 AM CPK Trip 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: 1/11/2012 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 # J11120353

2011027515 Collection Date: 28-Dec-11 8:15 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 74 mg/L EPA 300.0 09-Jan-12 21:21 JAHERMA 5 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 269 ug/L EPA 245.1 30-Dec-11 11:11 AGIBBS 5
TOTAL RECOVERABLE METALS BY ICP Boron (B) 109 mg/L EPA 200.7 03-Jan-12 13:34 DJSULL1 0.5
DISSOLVED METALS BY ICP-MS Selenium (Se) 193 ug/L EPA 200.8 03-Jan-12 13:49 MHH7131 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 141 ug/L EPA 200.8 04-Jan-12 13:59 KRICHAR 10 Chromium (Cr) 200 ug/L EPA 200.8 04-Jan-12 13:59 KRICHAR 10 Copper (Cu) 96.8 ug/L EPA 200.8 04-Jan-12 13:59 KRICHAR 10 Nickel (Ni) 152 ug/L EPA 200.8 04-Jan-12 13:59 KRICHAR 10 Selenium (Se) 4350 ug/L EPA 200.8 04-Jan-12 13:59 KRICHAR 10 Silver (Ag) < 10 ug/L EPA 200.8 04-Jan-12 13:59 KRICHAR 10 Zinc (Zn) 179 ug/L EPA 200.8 04-Jan-12 13:59 KRICHAR 20
SELENIUM SPECIATION Vendor Parameter COMPLETE V_AS&C
TOTAL DISSOLVED SOLIDS TDS 12000 mg/L SM2540C 03-Jan-12 15:03 AGIBBS 200 2011027516 Collection Date: 28-Dec-11 8:15 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) 205 ug/L EPA 245.1 30-Dec-11 11:14 AGIBBS 2.5
TOTAL RECOVERABLE METALS BY ICP Boron (B) 106 mg/L EPA 200.7 03-Jan-12 13:51 DJSULL1 0.5
DISSOLVED METALS BY ICP-MS Selenium (Se) 123 ug/L EPA 200.8 03-Jan-12 13:49 MHH7131 10

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

### Order # J11120353

2011027516 Collection Date: 28-Dec-11 8:15 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) 132 ug/L EPA 200.8 04-Jan-12 14:03 KRICHAR 10 Chromium (Cr) 174 ug/L EPA 200.8 04-Jan-12 14:03 KRICHAR 10 Copper (Cu) 83.8 ug/L EPA 200.8 04-Jan-12 14:03 KRICHAR 10 Nickel (Ni) 144 ug/L EPA 200.8 04-Jan-12 14:03 KRICHAR 10 Selenium (Se) 3740 ug/L EPA 200.8 04-Jan-12 14:03 KRICHAR 10 Silver (Ag) < 10 ug/L EPA 200.8 04-Jan-12 14:03 KRICHAR 10 Zinc (Zn) 149 ug/L EPA 200.8 04-Jan-12 14:03 KRICHAR 20 2011027517 Collection Date: 28-Dec-11 8:15 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) 96.0 mg/L EPA 200.7 03-Jan-12 13:42 DJSULL1 0.5
DISSOLVED METALS BY ICP-MS Selenium (Se) 111 ug/L EPA 200.8 03-Jan-12 13:49 MHH7131 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 04-Jan-12 14:06 KRICHAR 10 Chromium (Cr) < 10 ug/L EPA 200.8 04-Jan-12 14:06 KRICHAR 10 Copper (Cu) < 10 ug/L EPA 200.8 04-Jan-12 14:06 KRICHAR 10 Nickel (Ni) 19.5 ug/L EPA 200.8 04-Jan-12 14:06 KRICHAR 10 Selenium (Se) 103 ug/L EPA 200.8 04-Jan-12 14:06 KRICHAR 10 Silver (Ag) < 10 ug/L EPA 200.8 04-Jan-12 14:06 KRICHAR 10 Zinc (Zn) < 20 ug/L EPA 200.8 04-Jan-12 14:06 KRICHAR 20
SELENIUM SPECIATION Vendor Parameter COMPLETE V_AS&C 2011027518 Collection Date: 28-Dec-11 8:15 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) 99.7 mg/L EPA 200.7 03-Jan-12 13:46 DJSULL1 0.5

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

### Order # J11120353

2011027518 Collection Date: 28-Dec-11 8:15 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 04-Jan-12 14:09 KRICHAR 10 Chromium (Cr) < 10 ug/L EPA 200.8 04-Jan-12 14:09 KRICHAR 10 Copper (Cu) < 10 ug/L EPA 200.8 04-Jan-12 14:09 KRICHAR 10 Nickel (Ni) < 10 ug/L EPA 200.8 04-Jan-12 14:09 KRICHAR 10 Selenium (Se) 10.9 ug/L EPA 200.8 04-Jan-12 14:09 KRICHAR 10 Silver (Ag) < 10 ug/L EPA 200.8 04-Jan-12 14:09 KRICHAR 10 Zinc (Zn) < 20 ug/L EPA 200.8 04-Jan-12 14:09 KRICHAR 20 2011027519 Collection Date: 28-Dec-11 8:15 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 70 mg/L EPA 300.0 09-Jan-12 21:37 JAHERMA 5 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) < 1 ug/L EPA 245.1 30-Dec-11 11:16 AGIBBS 1
TOTAL RECOVERABLE METALS BY ICP Boron (B) 102 mg/L EPA 200.7 03-Jan-12 13:54 DJSULL1 0.5
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 5 ug/L EPA 200.8 04-Jan-12 14:13 KRICHAR 5 Chromium (Cr) < 5 ug/L EPA 200.8 04-Jan-12 14:13 KRICHAR 5 Copper (Cu) < 5 ug/L EPA 200.8 04-Jan-12 14:13 KRICHAR 5 Nickel (Ni) < 5 ug/L EPA 200.8 04-Jan-12 14:13 KRICHAR 5 Selenium (Se) < 5 ug/L EPA 200.8 04-Jan-12 14:13 KRICHAR 5 Silver (Ag) < 5 ug/L EPA 200.8 04-Jan-12 14:13 KRICHAR 5 Zinc (Zn) < 10 ug/L EPA 200.8 04-Jan-12 14:13 KRICHAR 10
SELENIUM SPECIATION Vendor Parameter COMPLETE V_AS&C 2011027520 Collection Date: 28-Dec-11 8:15 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 03-Jan-12 13:39 MHH7131 1

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

### Order # J11120353

2011027521 Collection Date: 21-Dec-11 8:20 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 03-Jan-12 13:11 DJSULL1 0.05
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 1 ug/L EPA 200.8 04-Jan-12 13:27 KRICHAR 1 Chromium (Cr) < 1 ug/L EPA 200.8 04-Jan-12 13:27 KRICHAR 1 Copper (Cu) < 1 ug/L EPA 200.8 04-Jan-12 13:27 KRICHAR 1 Nickel (Ni) < 1 ug/L EPA 200.8 04-Jan-12 13:27 KRICHAR 1 Selenium (Se) < 1 ug/L EPA 200.8 04-Jan-12 13:27 KRICHAR 1 Silver (Ag) < 1 ug/L EPA 200.8 04-Jan-12 13:27 KRICHAR 1 Zinc (Zn) < 2 ug/L EPA 200.8 04-Jan-12 13:27 KRICHAR 2
SELENIUM SPECIATION Vendor Parameter COMPLETE V_AS&C

### January 9 , 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 # J11120353 )

Dear Mr. Perkins, Attached is the report associated with four (4 ) aqueous samples submitted for selenium speciation analysis on December 2 9 , 2011. The samples were received in a sealed cooler at - 0. 4 ° C on December 30 , 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 # J11120353)
January 9 , 2012

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 2 9 , 2011 . The samples were received on December 30 , 2011 in a sealed container at -0. 4° 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 January 6 , 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 (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. All 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, LLCSample Results

Sample ID Se(IV) Se(VI) SeCN MeSe(IV) SeMe Unknown Se Species (n) FGD Purge Eff 68.4 75.0 ND (<0.74) ND (<1.4) ND (<1.4) 0 (0) BioReactor 2 Inf 21.9 59.8 ND (<0.18) 1.47 ND (<0.36) 0.84 (1) BioReactor 2 Eff ND (<0.49) ND (<0.40) ND (<0.18) ND (<0.36) ND (<0.36) 0 (0) Metals Trip Blk ND (<0.099) ND (<0.079) ND (<0.037) ND (<0.072) ND (<0.072) 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: January 9, 2012 LIMS #J11120353Quality 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 0.010 0.099 0.49 2.0 Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.079 0.40 1.6 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.037 0.18 0.74 MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.007 0.072 0.36 1.4 SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.007 0.072 0.36 1.4 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 9.11 95.1 Se(VI) LCS 9.48 8.99 94.8 SeCN LCS 8.92 8.60 96.4 MeSe(IV) LCS 6.47 6.20 95.8 SeMe LCS 9.32 8.75 93.9 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS Bi-Monthly Sampling)

Contact: Jay Perkins LIMS #J11120353 Date: January 9, 2012 Report Generated by: Russell GeradsQuality Control Summary - Matrix Duplicates

Analyte (μg/L) Sample ID Rep 1 Rep 2 Mean RPD Se(IV) Batch QC ND (<2.0) ND (<2.0) NC NC Se(VI) Batch QC 547.5 518.1 532.8 5.5 SeCN Batch QC ND (<0.74) ND (<0.74) NC NC MeSe(IV) Batch QC ND (<1.4) ND (<1.4) NC NC SeMe Batch QC 1.5 1.4 1.5 3.5 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 1112 1217 109.4 1112 1199 107.8 1.5 Se(VI) Batch QC 1009 1651 110.8 1009 1638 109.5 0.8 SeCN Batch QC 915.0 996.3 108.9 915.0 985.4 107.7 1.1 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS Bi-Monthly Sampling)

Contact: Jay Perkins LIMS #J11120353 Date: January 9, 2012 Report Generated by: Russell Gerads