### 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: J12020319

Lab Contact: Jason C Perkins


### Date: 3/7/2012 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 2012003972 BELEWS 16-Feb-12 9:00 AM TRAVIS THORNTON FGD Purge Eff 2012003973 BELEWS 16-Feb-12 9:00 AM TRAVIS THORNTON BIOREACTOR 1 INF. 2012003974 BELEWS 16-Feb-12 9:00 AM TRAVIS THORNTON BIOREACTOR 1 INF. BLANK 2012003975 BELEWS 16-Feb-12 9:00 AM TRAVIS THORNTON BIOREACTOR 2 EFF. 2012003976 BELEWS 16-Feb-12 9:00 AM TRAVIS THORNTON BIOREACTOR 2 EFF. BLANK 2012003977 BELEWS 16-Feb-12 9:00 AM TRAVIS THORNTON FILTER BLANK 2012003978 BELEWS 16-Feb-12 9:00 AM TRAVIS THORNTON 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: 

### 3/7/2012 Yes

Electronic Data Deliverable (EDD) Sent Separately

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



## Order # J12020319

2012003972 Collection Date: 16-Feb-12 9:00 AM 

### Site: FGD Purge Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF ALKALINITY (FIXED END POINT 4.5) Vendor Parameter Complete V_PRISM 1 Carbonate, Bicarbonate, and Hydroxide Alkalinity Bicarbonate (HCO3) Complete V_PRISM 1 Carbonate (CO3) Complete V_PRISM 1 Hydroxide (OH) Complete V_PRISM 1 NITRITE + NITRATE (COLORIMETRIC) Nitrite + Nitrate (Colorimetric) 12 mg-N/L EPA 353.2 21-Feb-12 13:54 BGN9034 0.25 25
INORGANIC IONS BY IC Bromide 120 mg/L EPA 300.0 24-Feb-12 13:21 JAHERMA 5 50 Chloride 7600 mg/L EPA 300.0 24-Feb-12 13:21 JAHERMA 100 1000 Sulfate 1200 mg/L EPA 300.0 24-Feb-12 13:21 JAHERMA 100 1000
DIONEX ANIONS BY VENDOR Vendor Parameter Complete V_AS&C 1 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 251 ug/L EPA 245.1 24-Feb-12 08:56 AGIBBS 5 100 Mercury Dissolved (cold vapor) in Water (Filtered) Mercury (Hg) < 2.5 ug/L EPA 245.1 24-Feb-12 10:16 AGIBBS 2.5 50
DISSOLVED METALS BY ICP Manganese (Mn) 6.99 mg/L EPA 200.7 22-Feb-12 14:09 DJSULL1 0.005 1
TOTAL RECOVERABLE METALS BY ICP Boron (B) 244 mg/L EPA 200.7 22-Feb-12 11:59 DJSULL1 0.5 10 Calcium (Ca) 4810 mg/L EPA 200.7 22-Feb-12 11:59 DJSULL1 0.1 10 Iron (Fe) 123 mg/L EPA 200.7 22-Feb-12 11:59 DJSULL1 0.1 10 Lithium (Li) 0.151 mg/L EPA 200.7 22-Feb-12 11:59 DJSULL1 0.05 10 Magnesium (Mg) 838 mg/L EPA 200.7 22-Feb-12 11:59 DJSULL1 0.05 10 Manganese (Mn) 8.05 mg/L EPA 200.7 22-Feb-12 11:59 DJSULL1 0.05 10 Potassium (K) 58.9 mg/L EPA 200.7 22-Feb-12 11:59 DJSULL1 1 10 Sodium (Na) 44.7 mg/L EPA 200.7 22-Feb-12 11:59 DJSULL1 0.5 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 302 ug/L EPA 200.8 22-Feb-12 13:12 MHH7131 10 10

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



## Order # J12020319

2012003972 Collection Date: 16-Feb-12 9:00 AM 

### Site: FGD Purge Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 175 ug/L EPA 200.8 23-Feb-12 11:44 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 23-Feb-12 11:44 KRICHAR 10 10 Chromium (Cr) 237 ug/L EPA 200.8 23-Feb-12 11:44 KRICHAR 10 10 Copper (Cu) 114 ug/L EPA 200.8 23-Feb-12 11:44 KRICHAR 10 10 Nickel (Ni) 181 ug/L EPA 200.8 23-Feb-12 11:44 KRICHAR 10 10 Selenium (Se) 4780 ug/L EPA 200.8 23-Feb-12 11:44 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 23-Feb-12 11:44 KRICHAR 10 10 Zinc (Zn) 182 ug/L EPA 200.8 23-Feb-12 11:44 KRICHAR 10 10
SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 1
TOTAL DISSOLVED SOLIDS TDS 18000 mg/L SM2540C 21-Feb-12 15:13 TJA7067 200 1
TOTAL SUSPENDED SOLIDS TSS 6200 mg/L SM2540D 250 1



### 2012003973 Collection Date: 16-Feb-12 9:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF ALKALINITY (FIXED END POINT 4.5) Vendor Parameter Complete V_PRISM 1 Carbonate, Bicarbonate, and Hydroxide Alkalinity Hydroxide (OH) Complete V_PRISM 1 Carbonate (CO3) Complete V_PRISM 1 Bicarbonate (HCO3) Complete V_PRISM 1 NITRITE + NITRATE (COLORIMETRIC) Nitrite + Nitrate (Colorimetric) 12 mg-N/L EPA 353.2 21-Feb-12 13:56 BGN9034 0.25 25
INORGANIC IONS BY IC Bromide 110 mg/L EPA 300.0 24-Feb-12 13:37 JAHERMA 5 50 Chloride 7300 mg/L EPA 300.0 24-Feb-12 13:37 JAHERMA 100 1000 Sulfate 1400 mg/L EPA 300.0 24-Feb-12 13:37 JAHERMA 100 1000
MERCURY 1631 Vendor Parameter Complete V_BRAND 1

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



## Order # J12020319

2012003973 Collection Date: 16-Feb-12 9:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF MERCURY (COLD VAPOR) IN WATER Mercury (Hg) < 2.5 ug/L EPA 245.1 24-Feb-12 08:58 AGIBBS 2.5 50 Mercury Dissolved (cold vapor) in Water (Filtered) Mercury (Hg) < 2.5 ug/L EPA 245.1 24-Feb-12 10:40 AGIBBS 2.5 50
DISSOLVED METALS BY ICP Manganese (Mn) 6.08 mg/L EPA 200.7 22-Feb-12 14:13 DJSULL1 0.005 1
TOTAL RECOVERABLE METALS BY ICP Boron (B) 223 mg/L EPA 200.7 22-Feb-12 12:03 DJSULL1 0.5 10 Calcium (Ca) 3450 mg/L EPA 200.7 22-Feb-12 12:03 DJSULL1 0.1 10 Iron (Fe) 0.162 mg/L EPA 200.7 22-Feb-12 12:03 DJSULL1 0.1 10 Lithium (Li) < 0.05 mg/L EPA 200.7 22-Feb-12 12:03 DJSULL1 0.05 10 Magnesium (Mg) 792 mg/L EPA 200.7 22-Feb-12 12:03 DJSULL1 0.05 10 Manganese (Mn) 6.38 mg/L EPA 200.7 22-Feb-12 12:03 DJSULL1 0.05 10 Potassium (K) 22.7 mg/L EPA 200.7 22-Feb-12 12:03 DJSULL1 1 10 Sodium (Na) 43.5 mg/L EPA 200.7 22-Feb-12 12:03 DJSULL1 0.5 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 106 ug/L EPA 200.8 22-Feb-12 13:16 MHH7131 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 16.6 ug/L EPA 200.8 23-Feb-12 11:47 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 23-Feb-12 11:47 KRICHAR 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 23-Feb-12 11:47 KRICHAR 10 10 Copper (Cu) < 10 ug/L EPA 200.8 23-Feb-12 11:47 KRICHAR 10 10 Nickel (Ni) 74.0 ug/L EPA 200.8 23-Feb-12 11:47 KRICHAR 10 10 Selenium (Se) 122 ug/L EPA 200.8 23-Feb-12 11:47 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 23-Feb-12 11:47 KRICHAR 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 23-Feb-12 11:47 KRICHAR 10 10
SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 1



### 2012003974 Collection Date: 16-Feb-12 9:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF MERCURY 1631 Vendor Parameter Complete V_BRAND 1

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



## Order # J12020319

2012003975 Collection Date: 16-Feb-12 9:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF ALKALINITY (FIXED END POINT 4.5) Vendor Parameter Complete V_PRISM 1 Carbonate, Bicarbonate, and Hydroxide Alkalinity Hydroxide (OH) Complete V_PRISM 1 Carbonate (CO3) Complete V_PRISM 1 Bicarbonate (HCO3) Complete V_PRISM 1 NITRITE + NITRATE (COLORIMETRIC) Nitrite + Nitrate (Colorimetric) < 0.01 mg-N/L EPA 353.2 21-Feb-12 13:59 BGN9034 0.01 1
INORGANIC IONS BY IC Bromide 110 mg/L EPA 300.0 24-Feb-12 13:53 JAHERMA 5 50 Chloride 7200 mg/L EPA 300.0 24-Feb-12 13:53 JAHERMA 100 1000 Sulfate 1400 mg/L EPA 300.0 24-Feb-12 13:53 JAHERMA 100 1000
MERCURY 1631 Vendor Parameter Complete V_BRAND 1 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) < 1 ug/L EPA 245.1 24-Feb-12 09:01 AGIBBS 1 20
DISSOLVED METALS BY ICP Manganese (Mn) 4.90 mg/L EPA 200.7 22-Feb-12 14:17 DJSULL1 0.005 1
TOTAL RECOVERABLE METALS BY ICP Boron (B) 225 mg/L EPA 200.7 22-Feb-12 12:06 DJSULL1 0.5 10 Calcium (Ca) 3400 mg/L EPA 200.7 22-Feb-12 12:06 DJSULL1 0.1 10 Iron (Fe) < 0.1 mg/L EPA 200.7 22-Feb-12 12:06 DJSULL1 0.1 10 Lithium (Li) < 0.05 mg/L EPA 200.7 22-Feb-12 12:06 DJSULL1 0.05 10 Magnesium (Mg) 777 mg/L EPA 200.7 22-Feb-12 12:06 DJSULL1 0.05 10 Manganese (Mn) 5.03 mg/L EPA 200.7 22-Feb-12 12:06 DJSULL1 0.05 10 Potassium (K) 26.9 mg/L EPA 200.7 22-Feb-12 12:06 DJSULL1 1 10 Sodium (Na) 42.2 mg/L EPA 200.7 22-Feb-12 12:06 DJSULL1 0.5 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 18.2 ug/L EPA 200.8 23-Feb-12 11:51 KRICHAR 5 5 Cadmium (Cd) < 5 ug/L EPA 200.8 23-Feb-12 11:51 KRICHAR 5 5 Chromium (Cr) < 5 ug/L EPA 200.8 23-Feb-12 11:51 KRICHAR 5 5 Copper (Cu) < 5 ug/L EPA 200.8 23-Feb-12 11:51 KRICHAR 5 5 Nickel (Ni) 6.84 ug/L EPA 200.8 23-Feb-12 11:51 KRICHAR 5 5 Selenium (Se) < 5 ug/L EPA 200.8 23-Feb-12 11:51 KRICHAR 5 5 Silver (Ag) < 5 ug/L EPA 200.8 23-Feb-12 11:51 KRICHAR 5 5 Zinc (Zn) < 5 ug/L EPA 200.8 23-Feb-12 11:51 KRICHAR 5 5

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



## Order # J12020319

2012003975 Collection Date: 16-Feb-12 9:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 1



### 2012003976 Collection Date: 16-Feb-12 9:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF MERCURY 1631 Vendor Parameter Complete V_BRAND 1



### 2012003977 Collection Date: 16-Feb-12 9:00 AM 

### Site: FILTER BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF Mercury Dissolved (cold vapor) in Water (Filtered) Mercury (Hg) < 0.05 ug/L EPA 245.1 24-Feb-12 10:42 AGIBBS 0.05 1
DISSOLVED METALS BY ICP Manganese (Mn) < 0.005 mg/L EPA 200.7 22-Feb-12 13:30 DJSULL1 0.005 1
DISSOLVED METALS BY ICP-MS Selenium (Se) < 1 ug/L EPA 200.8 22-Feb-12 12:49 MHH7131 1 1



### 2012003978 Collection Date: 16-Feb-12 9:00 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 22-Feb-12 11:43 DJSULL1 0.05 1 Calcium (Ca) < 0.01 mg/L EPA 200.7 22-Feb-12 11:43 DJSULL1 0.01 1 Iron (Fe) < 0.01 mg/L EPA 200.7 22-Feb-12 11:43 DJSULL1 0.01 1 Lithium (Li) < 0.005 mg/L EPA 200.7 22-Feb-12 11:43 DJSULL1 0.005 1 Magnesium (Mg) < 0.005 mg/L EPA 200.7 22-Feb-12 11:43 DJSULL1 0.005 1 Manganese (Mn) < 0.005 mg/L EPA 200.7 22-Feb-12 11:43 DJSULL1 0.005 1 Potassium (K) < 0.1 mg/L EPA 200.7 22-Feb-12 11:43 DJSULL1 0.1 1 Sodium (Na) < 0.05 mg/L EPA 200.7 22-Feb-12 11:43 DJSULL1 0.05 1

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



## Order # J12020319

2012003978 Collection Date: 16-Feb-12 9:00 AM 

### Site: Trip Blank Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 1 ug/L EPA 200.8 23-Feb-12 11:29 KRICHAR 1 1 Cadmium (Cd) < 1 ug/L EPA 200.8 23-Feb-12 11:29 KRICHAR 1 1 Chromium (Cr) < 1 ug/L EPA 200.8 23-Feb-12 11:29 KRICHAR 1 1 Copper (Cu) < 1 ug/L EPA 200.8 23-Feb-12 11:29 KRICHAR 1 1 Nickel (Ni) < 1 ug/L EPA 200.8 23-Feb-12 11:29 KRICHAR 1 1 Selenium (Se) < 1 ug/L EPA 200.8 23-Feb-12 11:29 KRICHAR 1 1 Silver (Ag) < 1 ug/L EPA 200.8 23-Feb-12 11:29 KRICHAR 1 1 Zinc (Zn) < 1 ug/L EPA 200.8 23-Feb-12 11:29 KRICHAR 1 1
SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 1

### This data package contains the analytical results for the project identified above and includes a Case Narrative, Sample Results and Chain of Custody. Unless otherwise noted, all samples were received in acceptable condition and processed according to the referenced methods. Data qualifiers are flagged individually on each sample. A key reference for the data qualifiers appears at the end of this case narrative. NC Certification No. 402 SC Certification No. 99012 NC Drinking Water Cert No. 37735 

# Case Narrative
02/24/2012

Duke Energy Corporation (04) Jay Perkins 13339 Hagers Ferry Road Huntersville, NC 28078 Project: HAPS/MACT Testing Belews Creek Project No.: J12020319 Lab Submittal Date: 02/17/2012 Prism Work Order: 2020411 VA Certification No. 1287



### Please call if you have any questions relating to this analytical report. Respectfully, PRISM LABORATORIES, INC.



### VP Laboratory Services Reviewed By

Data Qualifiers Key Reference: 

### HT Sample received and analyzed outside of the hold time.

Method Detection Limit MDL Below Reporting Limit BRL
Relative Percent Difference RPD



## * Results reported to the reporting limit. All other results are reported to the MDL with values between MDL and reporting limit indicated with a J.

This report should not be reproduced, except in its entirety, without the written consent of Prism Laboratories, Inc.

449 Springbrook Road - P.O. Box 240543 - Charlotte, NC 28224-0543 Phone: 704/529-6364 - Toll Free Number: 1-800/529-6364 - Fax: 704/525-0409 

### Page 1 of 8

# Sample Receipt Summary 02/24/2012 

### Prism Work Order: 2020411 Client Sample ID Matrix Lab Sample ID Date Sampled Date Received 

### 2020411-01 02/16/12 2012003972/FGD Purge Eff 02/17/12 Water 2020411-02 02/16/12 2012003973/BioReactor 1 Inf 02/17/12 Water 2020411-03 02/16/12 2012003975/BioReactor 2 Eff 02/17/12 Water
Samples received in good condition at 3.8 degrees C unless otherwise noted.

This report should not be reproduced, except in its entirety, without the written consent of Prism Laboratories, Inc.

449 Springbrook Road - P.O. Box 240543 - Charlotte, NC 28224-0543 Phone: 704/529-6364 - Toll Free Number: 1-800/529-6364 - Fax: 704/525-0409 

### Page 2 of 8

# Laboratory Report 02/24/2012

Result Parameter Batch ID Report Limit Analysis Date/Time Method Dilution Factor Units MDL Analyst 

### 13339 Hagers Ferry Road Project No.: Project: HAPS/MACT Testing Belews Creek Duke Energy Corporation (04)

Huntersville, NC 28078 Attn: Jay Perkins Sample Matrix: Water Client Sample ID: Prism Sample ID: 2020411-01 Prism Work Order: 2020411 Time Collected: 02/16/12 09:00 Time Submitted: 02/17/12 13:10 2012003972/FGD Purge Eff



### J12020319

General Chemistry Parameters 6.9 *SM4500-H B P2B0397 1 2/21/12 10:30 JAB HT pH Units pH 68 *SM2320 B P2B0422 1 5.0 2/22/12 11:15 JAB mg/L 0.66 Total Alkalinity BRL *SM2320 B P2B0424 1 5.0 2/22/12 11:15 JAB mg/L 0.66 Carbonate Alkalinity 68 *SM2320 B P2B0425 1 5.0 2/22/12 11:15 JAB mg/L 0.66 Bicarbonate Alkalinity

This report should not be reproduced, except in its entirety, without the written consent of Prism Laboratories, Inc. 449 Springbrook Road - P.O. Box 240543 - Charlotte, NC 28224-0543 Phone: 704/529-6364 - Toll Free Number: 1-800/529-6364 - Fax: 704/525-0409 

### Page 3 of 8

# Laboratory Report 02/24/2012

Result Parameter Batch ID Report Limit Analysis Date/Time Method Dilution Factor Units MDL Analyst 

### 13339 Hagers Ferry Road Project No.: Project: HAPS/MACT Testing Belews Creek Duke Energy Corporation (04)

Huntersville, NC 28078 Attn: Jay Perkins Sample Matrix: Water Client Sample ID: Prism Sample ID: 2020411-02 Prism Work Order: 2020411 Time Collected: 02/16/12 09:00 Time Submitted: 02/17/12 13:10 2012003973/BioReactor 1 Inf



### J12020319

General Chemistry Parameters 7.0 *SM4500-H B P2B0397 1 2/21/12 10:30 JAB HT pH Units pH 59 *SM2320 B P2B0422 1 5.0 2/22/12 11:15 JAB mg/L 0.66 Total Alkalinity BRL *SM2320 B P2B0424 1 5.0 2/22/12 11:15 JAB mg/L 0.66 Carbonate Alkalinity 59 *SM2320 B P2B0425 1 5.0 2/22/12 11:15 JAB mg/L 0.66 Bicarbonate Alkalinity

This report should not be reproduced, except in its entirety, without the written consent of Prism Laboratories, Inc. 449 Springbrook Road - P.O. Box 240543 - Charlotte, NC 28224-0543 Phone: 704/529-6364 - Toll Free Number: 1-800/529-6364 - Fax: 704/525-0409 

### Page 4 of 8

# Laboratory Report 02/24/2012

Result Parameter Batch ID Report Limit Analysis Date/Time Method Dilution Factor Units MDL Analyst 

### 13339 Hagers Ferry Road Project No.: Project: HAPS/MACT Testing Belews Creek Duke Energy Corporation (04)

Huntersville, NC 28078 Attn: Jay Perkins Sample Matrix: Water Client Sample ID: Prism Sample ID: 2020411-03 Prism Work Order: 2020411 Time Collected: 02/16/12 09:00 Time Submitted: 02/17/12 13:10 2012003975/BioReactor 2 Eff



### J12020319

General Chemistry Parameters 7.0 *SM4500-H B P2B0397 1 2/21/12 10:30 JAB HT pH Units pH 140 *SM2320 B P2B0422 1 5.0 2/22/12 11:15 JAB mg/L 0.66 Total Alkalinity BRL *SM2320 B P2B0424 1 5.0 2/22/12 11:15 JAB mg/L 0.66 Carbonate Alkalinity 140 *SM2320 B P2B0425 1 5.0 2/22/12 11:15 JAB mg/L 0.66 Bicarbonate Alkalinity

This report should not be reproduced, except in its entirety, without the written consent of Prism Laboratories, Inc. 449 Springbrook Road - P.O. Box 240543 - Charlotte, NC 28224-0543 Phone: 704/529-6364 - Toll Free Number: 1-800/529-6364 - Fax: 704/525-0409 

### Page 5 of 82/24/12 

### Level II QC Report

13339 Hagers Ferry Road Project No: J12020319 Project: HAPS/MACT Testing Belews Creek Duke Energy Corporation (04)

Huntersville, NC 28078 Attn: Jay Perkins Prism Work Order: 2020411 Time Submitted: 2/17/2012 1:10:00PM

Result Limit

Reporting Units Level Spike Result

Source %REC %REC Limits RPD RPD Limit Notes Analyte General Chemistry Parameters - Quality Control

Batch P2B0397 - NO PREP LCS (P2B0397-BS1) Prepared & Analyzed: 02/21/12 pH pH Units 6.82 6.860 99-101 99 Batch P2B0422 - NO PREP Blank (P2B0422-BLK1) Prepared & Analyzed: 02/22/12 Total Alkalinity mg/L BRL 5.0 LCS (P2B0422-BS1) Prepared & Analyzed: 02/22/12 Total Alkalinity mg/L 256 5.0 250.0 90-110 102 LCS Dup (P2B0422-BSD1) Prepared & Analyzed: 02/22/12 Total Alkalinity mg/L 253 5.0 250.0 200 90-110 101 1 Duplicate (P2B0422-DUP1) Prepared & Analyzed: 02/22/12 Source: 2020411-03 Total Alkalinity mg/L 137 5.0 138 20 0.7 Batch P2B0424 - NO PREP Blank (P2B0424-BLK1) Prepared & Analyzed: 02/22/12 Carbonate Alkalinity mg/L BRL 5.0 LCS (P2B0424-BS1) Prepared & Analyzed: 02/22/12 Carbonate Alkalinity mg/L 256 5.0 90-110 LCS Dup (P2B0424-BSD1) Prepared & Analyzed: 02/22/12 Carbonate Alkalinity mg/L 253 5.0 200 90-110 1

This report should not be reproduced, except in its entirety, without the written consent of Prism Laboratories, Inc.

449 Springbrook Road - P.O. Box 240543 - Charlotte, NC 28224-0543 Phone: 704/529-6364 - Toll Free Number: 1-800/529-6364 - Fax: 704/525-0409 

### Page 6 of 82/24/12 

### Level II QC Report

13339 Hagers Ferry Road Project No: J12020319 Project: HAPS/MACT Testing Belews Creek Duke Energy Corporation (04)

Huntersville, NC 28078 Attn: Jay Perkins Prism Work Order: 2020411 Time Submitted: 2/17/2012 1:10:00PM

Result Limit

Reporting Units Level Spike Result

Source %REC %REC Limits RPD RPD Limit Notes Analyte General Chemistry Parameters - Quality Control

Batch P2B0424 - NO PREP Duplicate (P2B0424-DUP1) Prepared & Analyzed: 02/22/12 Source: 2020411-03 Carbonate Alkalinity mg/L BRL 5.0 BRL 20 Batch P2B0425 - NO PREP Blank (P2B0425-BLK1) Prepared & Analyzed: 02/22/12 Bicarbonate Alkalinity mg/L BRL 5.0 LCS (P2B0425-BS1) Prepared & Analyzed: 02/22/12 Bicarbonate Alkalinity mg/L 256 5.0 250.0 90-110 102 LCS Dup (P2B0425-BSD1) Prepared & Analyzed: 02/22/12 Bicarbonate Alkalinity mg/L 253 5.0 250.0 200 90-110 101 1 Duplicate (P2B0425-DUP1) Prepared & Analyzed: 02/22/12 Source: 2020411-03 Bicarbonate Alkalinity mg/L 137 5.0 138 20 0.7

This report should not be reproduced, except in its entirety, without the written consent of Prism Laboratories, Inc.

449 Springbrook Road - P.O. Box 240543 - Charlotte, NC 28224-0543 Phone: 704/529-6364 - Toll Free Number: 1-800/529-6364 - Fax: 704/525-0409 

### Page 7 of 8Page 8 of 8

### 3958 6 th 

### Ave NW • Seattle, WA 98107 • T: 206-632-6206 • F: 206-632-6017 • www.brooksrand.com • brl@brooksrand.com 

## February 29, 2012
Duke Energy ATTN: Jay Perkins Scientific Support-Laboratory 13339 Hagers Ferry Road Huntersville NC 28078 jcperkins@duke-energy.com labcustomer@duke-energy.com
RE: Project DUK-HV1201 Client Project: J12020319 Dear Mr. Perkins, On February 21, 2012, Brooks Rand Labs (BRL) received two (2) wastewater samples and two (2) corresponding field blanks. Samples were logged-in for total mercury (Hg) analysis. All samples were received, prepared, analyzed, and stored according to BRL SOPs and EPA methodology. The results were blank-corrected as described in the calculations section of the applicable SOP(s) and may be evaluated using adjusted reporting limits to account for sample aliquot size. Please refer to the Sample Results page for sample-specific detection limits and other details. No qualification of the data was warranted, aside from concentration qualifiers, and all associated quality control sample results met the acceptance criteria. BRL, an accredited laboratory, certifies the reported results of all analyses for which BRL is NELAP accredited meet all NELAP requirements. For more details, see the Report Information page of the report. Please feel free to contact me if you have any questions regarding this report. Sincerely,

Tiffany Stilwater Project Manager tiffany@brooksrand.comProject ID: 

### DUK-HV1201

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



### Definition of Data Qualifiers

(Effective 9/23/09) 

### Laboratory Accreditation BRL is accredited by the National Environmental Laboratory Accreditation Program (NELAP) through the State of Florida Department of Health, Bureau of Laboratories (E87982) and is certified to perform many environmental analyses. BRL is also certified by many other states to perform environmental analyses. For a current list of our accreditations /certifications, please visit our website at <http://www.brooksrand.com/default.asp?contentID=586>. Results reported relate only to the samples listed in the report. 

# Report Information

BLK BRL BS CAL CCV
CRM D DUP ICV MSD ND NR PS REC RPD RSD SCV SOP 

### method blank Brooks Rand Labs laboratory fortified blank calibration standard continuing calibration verification
certified reference material dissolved fraction duplicate initial calibration verification matrix spike duplicate non-detect non-reportable post preparation spike percent recovery relative percent difference relative standard deviation secondary calibration verification standard operating procedure MDL MRL MS



### method detection limit method reporting limit matrix spike

SRM T COC



### standard reference material total recoverable fraction chain of custody record 

### Common Abbreviations

These qualifiers are based on those previously utilized by Brooks Rand, 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-HV1201

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Sample Information

Report Matrix Type Received Sampled Sample Lab ID 

### 1208004-01 BioReactor 1 Inf 02/16/2012 02/21/2012 Sample Influent 1208004-02 BioReactor 1 Inf Hg Blk 02/16/2012 02/21/2012 Field Blank DIW 1208004-03 BioReactor 2 Eff 02/16/2012 02/21/2012 Sample Effluent 1208004-04 BioReactor 2 Eff Hg Blk 02/16/2012 02/21/2012 Field Blank DIW 

# Batch Summary

Analyte Prepared Analyzed Sequence Batch Lab Matrix Method 

### B120297 02/25/2012 02/27/2012 1200129 Water EPA 1631 Hg



# Sample Results

Sample Sequence Result MDL MRL Unit Batch

Qualifier Analyte Fraction

Report Matrix BioReactor 1 Inf 

### ng/L 758 T 1200129 B120297 Influent 40.4 15.2 1208004-01 Hg
BioReactor 1 Inf Hg Blk 

### ng/L 0.15 T U 1200129 B120297 DIW 0.40 0.15 1208004-02 Hg

BioReactor 2 Eff 

### ng/L 29.1 T 1200129 B120297 Effluent 1.61 0.61 1208004-03 Hg
BioReactor 2 Eff Hg Blk 

### ng/L 0.15 T U 1200129 B120297 DIW 0.40 0.15 1208004-04 Hg

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

### DUK-HV1201

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Accuracy & Precision Summary

Batch: 

### B120297

Analyte Result Units Native Spike REC & Limits RPD & Limits Method: 

### EPA 1631 Lab Matrix: 

### Water

Sample Certified Reference Material (1209009, NIST 1641d 1000x dilution) B120297-SRM1 

### 15.68 94% ng/L 85-115 Hg 14.73

Matrix Spike (1208004-01) B120297-MS1 

### 3535 114% ng/L 71-125 Hg 4800

758.5

Matrix Spike Duplicate (1208004-01) B120297-MSD1 

### 3535 108% ng/L 71-125 245% Hg 4565

758.5

Matrix Spike (1208004-03) B120297-MS2 

### 139.0 100% ng/L 71-125 Hg 168.1

29.10

Matrix Spike Duplicate (1208004-03) B120297-MSD2 

### 140.2 105% ng/L 71-125 245% Hg 177.0

29.10

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

### DUK-HV1201

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Method Blanks & Reporting Limits

Batch: 

### B120297
Method: 

### EPA 1631 Matrix: 

### Water Analyte: 

### Hg Result Units Sample 

### B120297-BLK1 ng/L 0.11 B120297-BLK2 ng/L 0.04 B120297-BLK3 ng/L 0.04 B120297-BLK4 ng/L 0.04 MDL: 

### 0.15 Average: 

### 0.06 Standard Deviation: 

### 0.04 Limit: 

### 0.10 Limit: 

### 0.50 MRL: 

### 0.40

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

### DUK-HV1201

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Instrument Calibration

Sequence: 

### 1200129 Method: 

### EPA 1631 Instrument: 

### THG-10 Date: 

### 02/27/2012 Total Mercury and Mercury Speciation by CVAFS

Analyte: 

### Hg REC & Limits Result True Value Lab ID Units 

### 1200129-IBL1 4.20 pg of Hg 1200129-IBL2 6.75 pg of Hg 1200129-IBL3 4.72 pg of Hg 1200129-IBL4 5.95 pg of Hg 1200129-CAL1 25.00 24.83 pg of Hg 99% 1200129-CAL2 100.0 90.79 pg of Hg 91% 1200129-CAL3 500.0 481.7 pg of Hg 96% 1200129-CAL4 2500 2727 pg of Hg 109% 1200129-CAL5 10000 10670 pg of Hg 107% 1200129-ICV1 1568 1473 pg of Hg 94% 85-115 1200129-CCB1 4.56 pg of Hg 1200129-CCV1 500.0 512.9 pg of Hg 103% 77-123 1200129-CCV2 500.0 512.7 pg of Hg 103% 77-123 1200129-CCV3 500.0 444.8 pg of Hg 89% 77-123

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

### DUK-HV1201

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Sample Containers

Lab ID: 

### 1208004-01 Report Matrix: 

### Influent Sample Type: 

### Sample Received: 

### 02/21/2012 Sample: 

### BioReactor 1 Inf Collected: 

### 02/16/2012
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: 

### 1208004-02 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 02/21/2012 Sample: 

### BioReactor 1 Inf Hg Blk Collected: 

### 02/16/2012
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: 

### 1208004-03 Report Matrix: 

### Effluent Sample Type: 

### Sample Received: 

### 02/21/2012 Sample: 

### BioReactor 2 Eff Collected: 

### 02/16/2012
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: 

### 1208004-04 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 02/21/2012 Sample: 

### BioReactor 2 Eff Hg Blk Collected: 

### 02/16/2012
Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71511970 10 Cooler

none n/a 500 mL Bottle FLPE Hg-T



# Shipping Containers

Cooler
Tracking No: 

### 4726 7966 8530 via FedEx Temperature: 

### 2.8 °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: 

### February 21, 2012 9:00

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

## February 2 8 , 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: HAPS/MACT Testing Belews Creek (LIMS # J1 2020 319 )

Dear Mr. Perkins, Attached is the report associated with four (4 ) aqueous samples submitted for selenium speciation analysis on February 20 , 2012

. The samples were received in a sealed cooler at - 0.3 ° C on February 21 , 2012

. Selenium speciation analysis was performed via ionchromatography inductively coupled plasma collision reaction cell mass spectrometry (IC-ICPCRC -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: HAPS/MACT Testing Belews Creek (LIMS # J1 2020 319 )

February 2 8 , 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 February 20, 2012 . The samples were received on February 21 , 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 collision reaction cell mass spectrometry (IC-ICP- CRC -MS).

2. Sample Preparation All sample preparation is performed in laminar flow clean hoods known to be free from trace metals contamination. All applied water for dilutions and sample preservatives are monitored for contamination to account for any biases associated with the sample results. Selenium Speciation Analysis by IC -ICP-CRC- MS Prior to analysis, an aliquot of each sample was filtered with a syringe filter (0.45μm) and injected directly into a sealed autosampler vial. No further sample preparation was performed as any chemical alteration of a sample may shift the equilibrium of the system, resulting in changes in speciation ratios.
3. Sample Analysis All sample analysis is preceded by a minimum of a five-point calibration curve spanning the entire concentration range of interest. Calibration curves are performed at the beginning of each analytical day. All calibration c urves, associated with each species of interest, are

## standardized by linear regression resulting in a response factor. All sample results are

instrument blank corrected to account for any operational biases associated with the analytical platform. Prior to sample analysis, all calibration curves are verified using second source standard s which are identified as initial calibration verification standards (ICV). Ongoing instrument performance is identified by the analysis of continuing calibration verification standards (CCV) and continuing calibration blanks (CCB) at a minimal interval of every ten analytical runs. Selenium Speciation Analysis by IC -ICP-CRC- MS Each sample for selenium speciation analysis w as analyzed by ion chromatography inductively coupled plasma collision reaction cell mass spectrometry (IC-ICP- CRC -MS) on February 23, 2012. An aliquot of each sample is injected onto an anion exchange column and mobilized by a basic (pH > 7) gradient. The eluting selenium species are then introduced into a radio frequency (RF) plasma where energy-transfer processes cause desolvation, atomization, and ionization. The ions are extracted from the plasma through a differentially-pumped vacuum interface and travel through a pressurized chamber ( CRC ) containing hydrogen 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 233 70.3 ND (<1.6) ND (<9.4) ND (<9.4) 0 (0) BioReactor 1 Inf 33.2 53.5 ND (<0.39) 4.9 ND (<2.4) 0 (0) BioReactor 2 Eff ND (<2.0) ND (<4.7) ND (<0.39) ND (<2.4) ND (<2.4) 0 (0) Metals Trip Blk ND (<0.079) ND (<0.19) ND (<0.016) 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: HAPS/MACT Testing Belews Creek

Contact: Jay Perkins

Date: February 28, 2012 LIMS #J12020319

### Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 10x eMDL 250x eMDL 1000x Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.079 2.0 7.9 Se(VI) 0.019 0.000 0.000 0.000 0.005 0.009 0.019 0.188 4.7 19 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.016 0.39 1.6 MeSe(IV) 0.000 0.000 0.095 0.000 0.024 0.048 0.009 0.094 2.4 9.4 SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.009 0.094 2.4 9.4 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 9.38 98.0 Se(VI) LCS 9.48 9.09 95.9 SeCN LCS 8.92 8.54 95.7 MeSe(IV) LCS 6.47 5.79 89.4 SeMe LCS 9.32 8.48 91.0 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: HAPS/MACT Testing Belews Creek

Contact: Jay Perkins LIMS #J12020319 Date: February 28, 2012 Report Generated by: Russell Gerads

### Quality Control Summary - Matrix Duplicates

Analyte (μg/L) Sample ID Rep 1 Rep 2 Mean RPD Se(IV) BioReactor 2 Eff ND (<2.0) ND (<2.0) NC NC Se(VI) BioReactor 2 Eff ND (<4.7) ND (<4.7) NC NC SeCN BioReactor 2 Eff ND (<0.39) ND (<0.39) NC NC MeSe(IV) BioReactor 2 Eff ND (<2.4) ND (<2.4) NC NC SeMe BioReactor 2 Eff ND (<2.4) ND (<2.4) NC NC ND = Not detected at the applied dilution NC = Value was not calculated due to one or more concentrations below the eMDL

Quality Control Summary - Matrix Spike/ Matrix Spike Duplicate Analyte (μg/L) Sample ID Spike Conc MS Result Recovery Spike Conc MSD Result Recovery RPD Se(IV) BioReactor 2 Eff 1390 1587 114.2 1390 1585 114.0 0.2 Se(VI) BioReactor 2 Eff 1261 1297 102.8 1261 1304 103.4 0.5 SeCN BioReactor 2 Eff 1144 829.5 72.5* 1144 853.7 74.6* 2.9 *Low recovery is attributed to matrix induced species conversion Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: HAPS/MACT Testing Belews Creek

Contact: Jay Perkins LIMS #J12020319 Date: February 28, 2012 Report Generated by: Russell Gerads

## March 6 , 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: HAPS/MACT Testing Belews Creek (LIMS # J1 2020 319 )

Dear Mr. Perkins, Attached is the report associated with one (1 ) aqueous sample submitted for permanganate and persulfate analyses on February 20 , 2012

. The samples were received in a sealed cooler at - 0.3 ° C on February 21 , 2012

. Permanganate and persulfate analyses w ere performed via spectrophotometry. 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: HA PS/MACT Testing Belews Creek (LIMS # J12020319 )

March 6 , 2012

1. Sample Reception One (1 ) aqueous sample in two 125mL HDPE bottles and two 125mL borosilicate glass bottles (provided by Applied Speciation and Consulting) was submitted for permanganate and persulfate analyses on February 20 , 2012 . The sample w as received on February 21 , 2012 in a sealed co ntainer at -0.3 ° C. The sample was received in a laminar flow clean hood, void of trace metals contamination and ultra-violet radiation, and was designated a discrete sample identifier. All sample containers were placed in a secure refrigerator maintained at a temperature of 4 o 

## C until analysis could be performed.

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.
S 2 

## O 8 -2 

## and MnO 4 - 

## Analysis by Spectrophotometry Prior to analysis, an aliquot of each sample was filtered with a syringe filter (0.45μm). Permanganate standards of known concentrations were filtered using the identical filtration apparatus to confirm that filtration does not induce loss of the target analyte. Filtration is a requirement for samples containing suspended solids due to the light scattering properties of particulates.

## 3. Sample Analysis

All sample analysis is preceded by a minimum of a four-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.
MnO 4 - 

## Analysis by Spectrophotometry Each sample for permanganate analysis w as analyzed by spectrophotometry on February 29, 2012 . An aliquot of each sample was transferred to a cuvette with a 1cm light path. The permanganate complex was quantified by measuring the light absorbance at a wavelength of 545nm.
S 2 

## O 8 -2 

## Analysis by Spectrophotometry Each sample for persulfate analysis was analyzed by spectrophotometry on March 1, 2012. An aliquot of each sample was transferred to a 15mL polyethylene centrifuge tube. A starch iodide solution was added to each sample which induces conversion of iodide to I 2(aq) 

## . The I 2 

## complex then reacts with starch to form a blue complex which is measured at a wavelength of 525nm.
4. Analytical Issues The permanganate and persulfate recoveries for the matrix spike and matrix spike duplicate were below the control limit of 75%. The target analytes are efficient oxidizing agents which are amenable to reaction with most compounds. The low recoveries confirm that the sample matrix does not support the existence of strong oxidizing agents such as permanganate or persulfate. Approximately 2 minutes passed between the time of amending the sample matrix with the spikes and measurements which suggests that the low sample concentrations are not attributed to the variable of sample holding times. 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 MnO 4 - 

### S 2 

### O 8 -2 

### FGD Purge Eff ND (<0.50) ND (<100) All results reflect the applied dilution and are reported in mg/L ND = Not detected at the applied dilution

Report Generated by: Russell Gerads Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: HAPS/MACT Testing Belews Creek

Contact: Jay Perkins

Date: March 6, 2012 LIMS #J12020319

### Quality Control Summary - Preparation Blank Summary Analyte (mg/L) PBW1 eMDL MnO 4 - 

### 0.00 0.50 S 2 

### O 8 -2 

### 12 100 eMDL = Estimated Method Detection Limit

Quality Control Summary - Certified Reference Materials Analyte (mg/L) CRM True Value Result Recovery MnO 4 - 

### LCS 0.500 0.581 116.3 S 2 

### O 8 -2 

### LCS 100 123 123.4 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: HAPS/MACT Testing Belews Creek

Contact: Jay Perkins LIMS #J12020319 Date: March 6, 2012 Report Generated by: Russell Gerads

### Quality Control Summary - Matrix Duplicates Analyte (mg/L) Sample ID Rep 1 Rep 2 Mean RPD MnO 4 - 

### Batch QC ND (<0.50) ND (<0.50) NC NC S 2 

### O 8 -2 

### Batch QC 129 116 122.2 10.5 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 (mg/L) Sample ID Spike Conc MS Result Recovery Spike Conc MSD Result Recovery RPD MnO 4 - 

### Batch QC 0.500 0.052 10.5* 0.500 0.052 10.5* 0.0 S 2 

### O 8 -2 

### Batch QC 500 167 9.0* 500 137 3.0* 19.7 *Low recovery is attributed to matrix induced species conversion Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: HAPS/MACT Testing Belews Creek

Contact: Jay Perkins LIMS #J12020319 Date: March 6, 2012 Report Generated by: Russell Gerads