### 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: J12030359 Project Name: WWTS - Biweekly

L ab Contact: Jason C Perkins 

### Date: 4/12/2012 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. 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 2012006863 BELEWS 28-Mar-12 8:00 AM Tim Owens FGD Purge Eff 2012006864 BELEWS 28-Mar-12 8:00 AM Tim Owens EQ TANK EFF. 2012006865 BELEWS 28-Mar-12 8:00 AM Tim Owens BIOREACTOR 1 INF. 2012006866 BELEWS 28-Mar-12 8:00 AM Tim Owens BIOREACTOR 2 INF. 2012006867 BELEWS 28-Mar-12 8:00 AM Tim Owens BIOREACTOR 2 EFF. 2012006868 BELEWS 22-Mar-12 10:15 AM CPK FILTER BLANK 2012006869 BELEWS 22-Mar-12 10:15 AM CPK Trip Blank 7 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: 

### DataBase Administrator Date: 

### 4/12/2012 Yes

Electronic Data Deliverable (EDD) Sent Separately

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



## Order # J12030359

2012006863 Collection Date: 28-Mar-12 8:00 AM 

### Site: FGD Purge Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF INORGANIC IONS BY IC Bromide 220 mg/L EPA 300.0 02-Apr-12 21:28 JAHERMA 5 50 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 193 ug/L EPA 245.1 05-Apr-12 13:19 AGIBBS 5 100 TOTAL RECOVERABLE METALS BY ICP Boron (B) 202 mg/L EPA 200.7 10-Apr-12 12:42 DJSULL1 0.5 10 Manganese (Mn) 7.43 mg/L EPA 200.7 10-Apr-12 12:42 DJSULL1 0.05 10 DISSOLVED METALS BY ICP-MS Manganese (Mn) 6550 ug/L EPA 200.8 10-Apr-12 02:13 KRICHAR 10 10 Selenium (Se) 315 ug/L EPA 200.8 10-Apr-12 02:13 KRICHAR 10 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 170 ug/L EPA 200.8 05-Apr-12 22:28 KRICHAR 10 10 Chromium (Cr) 312 ug/L EPA 200.8 05-Apr-12 22:28 KRICHAR 10 10 Copper (Cu) 119 ug/L EPA 200.8 05-Apr-12 22:28 KRICHAR 10 10 Nickel (Ni) 549 ug/L EPA 200.8 05-Apr-12 22:28 KRICHAR 10 10 Selenium (Se) 4390 ug/L EPA 200.8 05-Apr-12 22:28 KRICHAR 10 10 Silver (Ag) 17.9 ug/L EPA 200.8 05-Apr-12 22:28 KRICHAR 10 10 Zinc (Zn) 243 ug/L EPA 200.8 05-Apr-12 22:28 KRICHAR 10 10 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 1 TOTAL DISSOLVED SOLIDS Vendor Parameter Complete V_PACE 1


### 2012006864 Collection Date: 28-Mar-12 8:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 122 ug/L EPA 245.1 05-Apr-12 13:21 AGIBBS 2.5 50 TOTAL RECOVERABLE METALS BY ICP Boron (B) 178 mg/L EPA 200.7 10-Apr-12 12:46 DJSULL1 0.5 10 Manganese (Mn) 6.02 mg/L EPA 200.7 10-Apr-12 12:46 DJSULL1 0.05 10

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



## Order # J12030359

2012006864 Collection Date: 28-Mar-12 8:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF DISSOLVED METALS BY ICP-MS Manganese (Mn) 5560 ug/L EPA 200.8 10-Apr-12 02:17 KRICHAR 10 10 Selenium (Se) 211 ug/L EPA 200.8 10-Apr-12 02:17 KRICHAR 10 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 117 ug/L EPA 200.8 05-Apr-12 22:31 KRICHAR 10 10 Chromium (Cr) 231 ug/L EPA 200.8 05-Apr-12 22:31 KRICHAR 10 10 Copper (Cu) 87.8 ug/L EPA 200.8 05-Apr-12 22:31 KRICHAR 10 10 Nickel (Ni) 438 ug/L EPA 200.8 05-Apr-12 22:31 KRICHAR 10 10 Selenium (Se) 3080 ug/L EPA 200.8 05-Apr-12 22:31 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 05-Apr-12 22:31 KRICHAR 10 10 Zinc (Zn) 181 ug/L EPA 200.8 05-Apr-12 22:31 KRICHAR 10 10


### 2012006865 Collection Date: 28-Mar-12 8:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF INORGANIC IONS BY IC Bromide 180 mg/L EPA 300.0 02-Apr-12 21:46 JAHERMA 5 50 TOTAL RECOVERABLE METALS BY ICP Boron (B) 155 mg/L EPA 200.7 10-Apr-12 12:19 DJSULL1 0.5 10 Manganese (Mn) 1.15 mg/L EPA 200.7 10-Apr-12 12:19 DJSULL1 0.05 10 DISSOLVED METALS BY ICP-MS Manganese (Mn) 1050 ug/L EPA 200.8 10-Apr-12 02:21 KRICHAR 10 10 Selenium (Se) 126 ug/L EPA 200.8 10-Apr-12 02:21 KRICHAR 10 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 05-Apr-12 22:34 KRICHAR 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 05-Apr-12 22:34 KRICHAR 10 10 Copper (Cu) < 10 ug/L EPA 200.8 05-Apr-12 22:34 KRICHAR 10 10 Nickel (Ni) 63.6 ug/L EPA 200.8 05-Apr-12 22:34 KRICHAR 10 10 Selenium (Se) 135 ug/L EPA 200.8 05-Apr-12 22:34 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 05-Apr-12 22:34 KRICHAR 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 05-Apr-12 22:34 KRICHAR 10 10 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 1

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



## Order # J12030359

2012006866 Collection Date: 28-Mar-12 8:00 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) 147 mg/L EPA 200.7 10-Apr-12 12:22 DJSULL1 0.5 10 Manganese (Mn) 0.646 mg/L EPA 200.7 10-Apr-12 12:22 DJSULL1 0.05 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 05-Apr-12 22:37 KRICHAR 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 05-Apr-12 22:37 KRICHAR 10 10 Copper (Cu) < 10 ug/L EPA 200.8 05-Apr-12 22:37 KRICHAR 10 10 Nickel (Ni) < 10 ug/L EPA 200.8 05-Apr-12 22:37 KRICHAR 10 10 Selenium (Se) < 10 ug/L EPA 200.8 05-Apr-12 22:37 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 05-Apr-12 22:37 KRICHAR 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 05-Apr-12 22:37 KRICHAR 10 10


### 2012006867 Collection Date: 28-Mar-12 8:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF INORGANIC IONS BY IC Bromide 150 mg/L EPA 300.0 02-Apr-12 22:04 JAHERMA 5 50 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) < 1 ug/L EPA 245.1 05-Apr-12 13:24 AGIBBS 1 20 TOTAL RECOVERABLE METALS BY ICP Boron (B) 152 mg/L EPA 200.7 10-Apr-12 12:26 DJSULL1 0.5 10 Manganese (Mn) 0.530 mg/L EPA 200.7 10-Apr-12 12:26 DJSULL1 0.05 10 DISSOLVED METALS BY ICP-MS Manganese (Mn) 544 ug/L EPA 200.8 10-Apr-12 02:25 KRICHAR 5 5 Selenium (Se) 6.41 ug/L EPA 200.8 10-Apr-12 02:25 KRICHAR 5 5 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 5 ug/L EPA 200.8 05-Apr-12 22:40 KRICHAR 5 5 Chromium (Cr) < 5 ug/L EPA 200.8 05-Apr-12 22:40 KRICHAR 5 5 Copper (Cu) < 5 ug/L EPA 200.8 05-Apr-12 22:40 KRICHAR 5 5 Nickel (Ni) < 5 ug/L EPA 200.8 05-Apr-12 22:40 KRICHAR 5 5 Selenium (Se) < 5 ug/L EPA 200.8 05-Apr-12 22:40 KRICHAR 5 5 Silver (Ag) < 5 ug/L EPA 200.8 05-Apr-12 22:40 KRICHAR 5 5 Zinc (Zn) < 5 ug/L EPA 200.8 05-Apr-12 22:40 KRICHAR 5 5 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 1

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



## Order # J12030359

2012006868 Collection Date: 22-Mar-12 10:15 AM 

### Site: FILTER BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF DISSOLVED METALS BY ICP-MS Manganese (Mn) 3.85 ug/L EPA 200.8 10-Apr-12 01:57 KRICHAR 1 1 Selenium (Se) 1.06 ug/L EPA 200.8 10-Apr-12 01:57 KRICHAR 1 1


### 2012006869 Collection Date: 22-Mar-12 10:15 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 10-Apr-12 12:15 DJSULL1 0.05 1 Manganese (Mn) < 0.005 mg/L EPA 200.7 10-Apr-12 12:15 DJSULL1 0.005 1 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 1 ug/L EPA 200.8 05-Apr-12 22:25 KRICHAR 1 1 Chromium (Cr) < 1 ug/L EPA 200.8 05-Apr-12 22:25 KRICHAR 1 1 Copper (Cu) < 1 ug/L EPA 200.8 05-Apr-12 22:25 KRICHAR 1 1 Nickel (Ni) < 1 ug/L EPA 200.8 05-Apr-12 22:25 KRICHAR 1 1 Selenium (Se) < 1 ug/L EPA 200.8 05-Apr-12 22:25 KRICHAR 1 1 Silver (Ag) 1.43 ug/L EPA 200.8 05-Apr-12 22:25 KRICHAR 1 1 Zinc (Zn) < 1 ug/L EPA 200.8 05-Apr-12 22:25 KRICHAR 1 1 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 1

## April 04, 2012

LIMS USE: FR - TERRY WHITNER LIMS OBJECT ID: 92115350



## 92115350 Project: Pace Project No.: RE: Terry Whitner Duke Energy Carolinas, LLC PO Box 37929 DPEHS Charlotte, NC 28237

J12030359

Dear Terry Whitner: Enclosed are the analytical results for sample(s) received by the laboratory on March 29, 2012. The results relate only to the samples included in this report. Results reported herein conform to the most current TNI standards and the laboratory's Quality Assurance Manual, where applicable, unless otherwise noted in the body of the report.
Analyses were performed at the Pace Analytical Services location indicated on the sample analyte page for analysis unless otherwise footnoted. If you have any questions concerning this report, please feel free to contact me.
Sincerely,

Kevin Herring kevin.herring@pacelabs.com Project Manager

Enclosures



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Page 1 of 7 Pace Analytical Services, Inc. 9800 Kincey Ave. Suite 100 Huntersville, NC 28078 (704)875-9092 Pace Analytical Services, Inc.

2225 Riverside Dr. Asheville, NC 28804 (828)254-7176 Pace Analytical Services, Inc. 205 East Meadow Road - Suite A

Eden, NC 27288 (336)623-8921

### CERTIFICATIONS

Pace Project No.: Project: 92115350

J12030359

Asheville Certification IDs 2225 Riverside Dr., Asheville, NC 28804 Florida/NELAP Certification #: E87648 Massachusetts Certification #: M-NC030 North Carolina Drinking Water Certification #: 37712 North Carolina Wastewater Certification #: 40 South Carolina Certification #: 99030001 Virginia Certification #: 00072 West Virginia Certification #: 356 Virgina/VELAP Certification #: 460147



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Page 2 of 7 Pace Analytical Services, Inc. 9800 Kincey Ave. Suite 100 Huntersville, NC 28078 (704)875-9092 Pace Analytical Services, Inc.

2225 Riverside Dr. Asheville, NC 28804 (828)254-7176 Pace Analytical Services, Inc. 205 East Meadow Road - Suite A

Eden, NC 27288 (336)623-8921

### SAMPLE ANALYTE COUNT

Pace Project No.: Project: 92115350

J12030359

Lab ID Sample ID Method Analytes Reported Laboratory Analysts 92115350001 2012006863 SM 2540C 1 PASI-A LMD



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Page 3 of 7 Pace Analytical Services, Inc. 9800 Kincey Ave. Suite 100 Huntersville, NC 28078 (704)875-9092 Pace Analytical Services, Inc.

2225 Riverside Dr. Asheville, NC 28804 (828)254-7176 Pace Analytical Services, Inc. 205 East Meadow Road - Suite A

Eden, NC 27288 (336)623-8921

### ANALYTICAL RESULTS

Pace Project No.: Project: 92115350

J12030359
Sample: 2012006863 Lab ID: 92115350001 Collected: 03/28/12 08:00 Received: 03/29/12 15:10 Matrix: Water

Parameters Results Units DF Prepared Analyzed CAS No. Qual Report Limit
2540C Total Dissolved Solids Analytical Method: SM 2540C Total Dissolved Solids 20300 mg/L 1 04/02/12 15:11 500



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Date: 04/04/2012 03:59 PM Page 4 of 7 Pace Analytical Services, Inc. 9800 Kincey Ave. Suite 100 Huntersville, NC 28078 (704)875-9092 Pace Analytical Services, Inc.

2225 Riverside Dr. Asheville, NC 28804 (828)254-7176 Pace Analytical Services, Inc. 205 East Meadow Road - Suite A

Eden, NC 27288 (336)623-8921

### QUALITY CONTROL DATA

Pace Project No.: Project: 92115350

J12030359

QC Batch: QC Batch Method: Analysis Method: Analysis Description: WET/20301 SM 2540C SM 2540C 2540C Total Dissolved Solids Associated Lab Samples: 92115350001

Parameter Units Blank Result Reporting

Limit Qualifiers METHOD BLANK: 744524 Associated Lab Samples: 92115350001 Matrix: Water

Analyzed Total Dissolved Solids mg/L ND 25.0 04/02/12 15:01

Parameter Units LCS Result % Rec Limits Qualifiers % Rec Conc. 744525 LABORATORY CONTROL SAMPLE: LCS Spike

Total Dissolved Solids mg/L 226 250 90 80-120

Parameter Units Dup Result Qualifiers

RPD Result 92115151012 744526 SAMPLE DUPLICATE:

Total Dissolved Solids mg/L 49.0 D6 22 61.0

Parameter Units Dup Result Qualifiers

RPD Result 92115267003 744527 SAMPLE DUPLICATE:

Total Dissolved Solids mg/L 6280 D6 31 4600



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Date: 04/04/2012 03:59 PM Page 5 of 7 Pace Analytical Services, Inc. 9800 Kincey Ave. Suite 100 Huntersville, NC 28078 (704)875-9092 Pace Analytical Services, Inc.

2225 Riverside Dr. Asheville, NC 28804 (828)254-7176 Pace Analytical Services, Inc. 205 East Meadow Road - Suite A

Eden, NC 27288 (336)623-8921

### QUALIFIERS

Pace Project No.: Project: 92115350

J12030359

DEFINITIONS DF - Dilution Factor, if reported, represents the factor applied to the reported data due to changes in sample preparation, dilution of the sample aliquot, or moisture content. ND - Not Detected at or above adjusted reporting limit. J - Estimated concentration above the adjusted method detection limit and below the adjusted reporting limit. MDL - Adjusted Method Detection Limit. S - Surrogate 1,2-Diphenylhydrazine (8270 listed analyte) decomposes to Azobenzene. Consistent with EPA guidelines, unrounded data are displayed and have been used to calculate % recovery and RPD values. LCS(D) - Laboratory Control Sample (Duplicate) MS(D) - Matrix Spike (Duplicate) DUP - Sample Duplicate RPD - Relative Percent Difference NC - Not Calculable. SG - Silica Gel - Clean-Up U - Indicates the compound was analyzed for, but not detected. N-Nitrosodiphenylamine decomposes and cannot be separated from Diphenylamine using Method 8270. The result reported for each analyte is a combined concentration. Acid preservation may not be appropriate for 2-Chloroethylvinyl ether, Styrene, and Vinyl chloride. Pace Analytical is TNI accredited. Contact your Pace PM for the current list of accredited analytes. TNI - The NELAC Institute. LABORATORIES Pace Analytical Services - Asheville PASI-A
ANALYTE QUALIFIERS

The relative percent difference (RPD) between the sample and sample duplicate exceeded laboratory control limits. D6



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Date: 04/04/2012 03:59 PM Page 6 of 7 Pace Analytical Services, Inc. 9800 Kincey Ave. Suite 100 Huntersville, NC 28078 (704)875-9092 Pace Analytical Services, Inc.

2225 Riverside Dr. Asheville, NC 28804 (828)254-7176 Pace Analytical Services, Inc. 205 East Meadow Road - Suite A

Eden, NC 27288 (336)623-8921

### QUALITY CONTROL DATA CROSS REFERENCE TABLE

Pace Project No.: Project: 92115350

J12030359

Lab ID Sample ID QC Batch Method QC Batch Analytical Method Analytical Batch 92115350001 WET/20301 2012006863 SM 2540C



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Date: 04/04/2012 03:59 PM Page 7 of 7 Pace Analytical Services, Inc. 9800 Kincey Ave. Suite 100 Huntersville, NC 28078 (704)875-9092 Pace Analytical Services, Inc.

2225 Riverside Dr. Asheville, NC 28804 (828)254-7176 Pace Analytical Services, Inc. 205 East Meadow Road - Suite A

Eden, NC 27288 (336)623-8921

## April 3 , 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- Wed -Sampling) (LIMS # J1 20 30 359)

Dear Mr. Perkins, Attached is the report associated with four (4 ) aqueous samples submitted for selenium speciation analysis on March 29 , 2012

. The samples were received in a sealed cooler at-0. 3 ° C on March 30 , 2012

. Selenium speciation analysis was performed via ion chromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICP-D RC -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- Wed -Sampling) (LIMS # J1 2030 359 )
April 3 , 2012

1. Sample Reception Four (4 ) aqueous samples in125mL HDPE bottles (provided by Applied Speciation and Consulting) were submitted for selenium speciation analysi s on March 29 , 2012 . The samples were received on March 30 , 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 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-D RC -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 Eachsample for selenium speciation analysis w as analyzed by ion chromatography inductively coupled plasm a dynamic reaction cell mass spectrometry (IC-ICP-D RC -MS) on March 30, 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 (D RC ) 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 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 219 98.7 ND (<1.8) 2.6 ND (<1.9) 0 (0) BioReactor 1 Inf 28.8 96.4 ND (<0.45) 2.62 ND (<0.47) 0 (0) BioReactor 2 Eff ND (<0.59) ND (<0.36) ND (<0.45) ND (<0.47) ND (<0.47) 0 (0) Metals Trip Blk ND (<0.12) ND (<0.071) ND (<0.089) ND (<0.093) ND (<0.093) 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-Wed-Sampling)

Contact: Jay Perkins
Date: April 3, 2012 LIMS #J12030359

### 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 0.012 0.12 0.59 2.4 Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.007 0.071 0.36 1.4 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.009 0.089 0.45 1.8 MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.009 0.093 0.47 1.9 SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.009 0.093 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 9.57 9.07 94.8 Se(VI) LCS 9.48 9.03 95.3 SeCN LCS 8.92 8.28 92.8 MeSe(IV) LCS 6.47 5.92 91.5 SeMe LCS 9.32 8.49 91.0 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS (Bi-Monthly-Wed-Sampling)

Contact: Jay Perkins LIMS #J12030359 Date: April 3, 2012 Report Generated by: Russell Gerads

### Quality Control Summary - Matrix Duplicates

Analyte (μg/L) Sample ID Rep 1 Rep 2 Mean RPD Se(IV) Batch QC ND (<2.4) ND (<2.4) NC NC Se(VI) Batch QC ND (<1.4) ND (<1.4) NC NC SeCN Batch QC 4.6 4.1 4.3 11.1 MeSe(IV) Batch QC ND (<1.9) ND (<1.9) NC NC SeMe Batch QC ND (<1.9) ND (<1.9) NC NC ND = Not detected at the applied dilution NC = Value was not calculated due to one or more concentrations below the eMDL

Quality Control Summary - Matrix Spike/ Matrix Spike Duplicate Analyte (μg/L) Sample ID Spike Conc MS Result Recovery Spike Conc MSD Result Recovery RPD Se(IV) Batch QC 1112 1339 120.4 1112 1331 119.7 0.6 Se(VI) Batch QC 1009 1175 116.4 1009 1147 113.7 2.4 SeCN Batch QC 915.0 1000 108.8 915.0 960.7 104.5 4.0 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS (Bi-Monthly-Wed-Sampling)

Contact: Jay Perkins LIMS #J12030359 Date: April 3, 2012 Report Generated by: Russell Gerads