### 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: J13010342

Lab Contact: Jason C Perkins 

### Date: 2/11/2013 Customer Address: 253 Plant Allen Road Customer Name(s): Bill K., Ron L., Don S.

Belmont, 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. Subcontracted data included on the Duke Certificate of Analysis is to be used as information only. Certified vendor results can be found in the subcontracted lab final report. Duke Energy Analytical Laboratory subcontracts analyses to other vendor laboratories that have been qualified by Duke Energy to perform these analyses except where 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. Jason C Perkins

## Sample ID's & Descriptions:

Sample ID Plant/Station Collection Date and Time Collected By Sample Description 2013001388 ALLEN 18-Jan-13 10:51 AM JBW FGD Purge Eff 2013001389 ALLEN 18-Jan-13 8:27 AM JBW EQ Tank 2013001390 ALLEN 18-Jan-13 8:30 AM JBW BioReactor 1 Inf 2013001397 ALLEN 18-Jan-13 8:57 AM JBW BioReactor 1 Inf BLANK 2013001400 ALLEN 18-Jan-13 8:40 AM JBW BioReactor 2 Inf 2013001401 ALLEN 18-Jan-13 9:09 AM JBW BioReactor 2 Inf BLANK 2013001402 ALLEN 18-Jan-13 8:34 AM JBW BioReactor 2 Eff 2013001403 ALLEN 18-Jan-13 9:05 AM JBW BioReactor 2 Eff BLANK 2013001404 ALLEN 18-Jan-13 12:10 PM JBW Filter Blk 9 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. 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: 

### DBA Account Date: 

### 2/11/2013 Electronic Data Deliverable (EDD) Sent Separately

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



## Order # J13010342

2013001388 Collection Date: 18-Jan-13 10:51 AM 

### Site: FGD Purge Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF ALKALINITY - (Analysis Performed by Prism Labs) Vendor Parameter Complete Vendor Method V_PRISM INORGANIC IONS BY IC Bromide 760 mg/L EPA 300.0 01/28/2013 14:34 JAHERMA 100 1000 Chloride 2000 mg/L EPA 300.0 01/28/2013 14:34 JAHERMA 100 1000 Sulfate 1300 mg/L EPA 300.0 01/28/2013 14:34 JAHERMA 100 1000 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 26.3 ug/L EPA 245.1 01/24/2013 12:23 AGIBBS 2.5 50 DISSOLVED METALS BY ICP Manganese (Mn) 4.10 mg/L EPA 200.7 01/28/2013 12:03 MHH7131 0.05 10 TOTAL RECOVERABLE METALS BY ICP Boron (B) 46.2 mg/L EPA 200.7 01/29/2013 13:30 MHH7131 0.5 10 Calcium (Ca) 2150 mg/L EPA 200.7 01/29/2013 13:30 MHH7131 0.1 10 Iron (Fe) 84.3 mg/L EPA 200.7 01/29/2013 13:30 MHH7131 0.1 10 Magnesium (Mg) 374 mg/L EPA 200.7 01/29/2013 13:30 MHH7131 0.05 10 Manganese (Mn) 4.63 mg/L EPA 200.7 01/29/2013 13:30 MHH7131 0.05 10 DISSOLVED METALS BY ICP-MS Selenium (Se) 833 ug/L EPA 200.8 01/24/2013 11:27 KRICHAR 10 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 287 ug/L EPA 200.8 01/24/2013 10:07 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 01/24/2013 10:07 KRICHAR 10 10 Chromium (Cr) 176 ug/L EPA 200.8 01/24/2013 10:07 KRICHAR 10 10 Copper (Cu) 260 ug/L EPA 200.8 01/24/2013 10:07 KRICHAR 10 10 Nickel (Ni) 268 ug/L EPA 200.8 01/24/2013 10:07 KRICHAR 10 10 Selenium (Se) 4490 ug/L EPA 200.8 01/24/2013 10:07 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 01/24/2013 10:07 KRICHAR 10 10 Zinc (Zn) 457 ug/L EPA 200.8 01/24/2013 10:07 KRICHAR 10 10 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C
TOTAL DISSOLVED SOLIDS TDS 8300 mg/L SM2540C 01/22/2013 16:15 SWILLI3 200 1 TOTAL SUSPENDED SOLIDS TSS 3300 mg/L SM2540D 01/24/2013 13:25 SWILLI3 250 1

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



## Order # J13010342

2013001389 Collection Date: 18-Jan-13 8:27 AM 

### Site: EQ Tank Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 32.6 ug/L EPA 245.1 01/24/2013 12:26 AGIBBS 2.5 50 DISSOLVED METALS BY ICP Manganese (Mn) 2.20 mg/L EPA 200.7 01/28/2013 12:07 MHH7131 0.05 10 TOTAL RECOVERABLE METALS BY ICP Boron (B) 34.9 mg/L EPA 200.7 01/29/2013 13:34 MHH7131 0.5 10 Calcium (Ca) 1780 mg/L EPA 200.7 01/29/2013 13:34 MHH7131 0.1 10 Iron (Fe) 115 mg/L EPA 200.7 01/29/2013 13:34 MHH7131 0.1 10 Magnesium (Mg) 302 mg/L EPA 200.7 01/29/2013 13:34 MHH7131 0.05 10 Manganese (Mn) 5.98 mg/L EPA 200.7 01/29/2013 13:34 MHH7131 0.05 10 DISSOLVED METALS BY ICP-MS Selenium (Se) 212 ug/L EPA 200.8 01/24/2013 11:30 KRICHAR 10 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 282 ug/L EPA 200.8 01/24/2013 10:10 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 01/24/2013 10:10 KRICHAR 10 10 Chromium (Cr) 208 ug/L EPA 200.8 01/24/2013 10:10 KRICHAR 10 10 Copper (Cu) 284 ug/L EPA 200.8 01/24/2013 10:10 KRICHAR 10 10 Nickel (Ni) 291 ug/L EPA 200.8 01/24/2013 10:10 KRICHAR 10 10 Selenium (Se) 4720 ug/L EPA 200.8 01/24/2013 10:10 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 01/24/2013 10:10 KRICHAR 10 10 Zinc (Zn) 440 ug/L EPA 200.8 01/24/2013 10:10 KRICHAR 10 10


### 2013001390 Collection Date: 18-Jan-13 8:30 AM 

### Site: BioReactor 1 Inf Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF ALKALINITY - (Analysis Performed by Prism Labs) Vendor Parameter Complete Vendor Method V_PRISM MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND MERCURY 1631 - DISSOLVED - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND DISSOLVED METALS BY ICP Manganese (Mn) 0.080 mg/L EPA 200.7 01/28/2013 12:11 MHH7131 0.05 10

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



## Order # J13010342

2013001390 Collection Date: 18-Jan-13 8:30 AM 

### Site: BioReactor 1 Inf Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF TOTAL RECOVERABLE METALS BY ICP Boron (B) 15.4 mg/L EPA 200.7 01/29/2013 13:38 MHH7131 0.5 10 Calcium (Ca) 796 mg/L EPA 200.7 01/29/2013 13:38 MHH7131 0.1 10 Iron (Fe) < 0.1 mg/L EPA 200.7 01/29/2013 13:38 MHH7131 0.1 10 Magnesium (Mg) 113 mg/L EPA 200.7 01/29/2013 13:38 MHH7131 0.05 10 Manganese (Mn) 0.082 mg/L EPA 200.7 01/29/2013 13:38 MHH7131 0.05 10 DISSOLVED METALS BY ICP-MS Selenium (Se) 81.6 ug/L EPA 200.8 01/24/2013 11:34 KRICHAR 10 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 01/24/2013 10:14 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 01/24/2013 10:14 KRICHAR 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 01/24/2013 10:14 KRICHAR 10 10 Copper (Cu) < 10 ug/L EPA 200.8 01/24/2013 10:14 KRICHAR 10 10 Nickel (Ni) < 10 ug/L EPA 200.8 01/24/2013 10:14 KRICHAR 10 10 Selenium (Se) 78.0 ug/L EPA 200.8 01/24/2013 10:14 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 01/24/2013 10:14 KRICHAR 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 01/24/2013 10:14 KRICHAR 10 10 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C


### 2013001397 Collection Date: 18-Jan-13 8:57 AM 

### Site: BioReactor 1 Inf BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND MERCURY 1631 - DISSOLVED - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND


### 2013001400 Collection Date: 18-Jan-13 8:40 AM 

### Site: BioReactor 2 Inf Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF ALKALINITY - (Analysis Performed by Prism Labs) Vendor Parameter Complete Vendor Method V_PRISM

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



## Order # J13010342

2013001400 Collection Date: 18-Jan-13 8:40 AM 

### Site: BioReactor 2 Inf Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND MERCURY 1631 - DISSOLVED - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND DISSOLVED METALS BY ICP Manganese (Mn) 0.091 mg/L EPA 200.7 01/28/2013 12:15 MHH7131 0.05 10 TOTAL RECOVERABLE METALS BY ICP Boron (B) 22.4 mg/L EPA 200.7 01/29/2013 13:42 MHH7131 0.5 10 Calcium (Ca) 802 mg/L EPA 200.7 01/29/2013 13:42 MHH7131 0.1 10 Iron (Fe) 0.140 mg/L EPA 200.7 01/29/2013 13:42 MHH7131 0.1 10 Magnesium (Mg) 127 mg/L EPA 200.7 01/29/2013 13:42 MHH7131 0.05 10 Manganese (Mn) 0.090 mg/L EPA 200.7 01/29/2013 13:42 MHH7131 0.05 10 DISSOLVED METALS BY ICP-MS Selenium (Se) 15.6 ug/L EPA 200.8 01/24/2013 11:37 KRICHAR 10 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 01/24/2013 10:17 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 01/24/2013 10:17 KRICHAR 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 01/24/2013 10:17 KRICHAR 10 10 Copper (Cu) < 10 ug/L EPA 200.8 01/24/2013 10:17 KRICHAR 10 10 Nickel (Ni) < 10 ug/L EPA 200.8 01/24/2013 10:17 KRICHAR 10 10 Selenium (Se) 14.0 ug/L EPA 200.8 01/24/2013 10:17 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 01/24/2013 10:17 KRICHAR 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 01/24/2013 10:17 KRICHAR 10 10 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C



### 2013001401 Collection Date: 18-Jan-13 9:09 AM 

### Site: BioReactor 2 Inf BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND MERCURY 1631 - DISSOLVED - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND

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



## Order # J13010342

2013001402 Collection Date: 18-Jan-13 8:34 AM 

### Site: BioReactor 2 Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF ALKALINITY - (Analysis Performed by Prism Labs) Vendor Parameter Complete Vendor Method V_PRISM INORGANIC IONS BY IC Bromide 310 mg/L EPA 300.0 01/28/2013 17:41 JAHERMA 5 50 Chloride 960 mg/L EPA 300.0 01/28/2013 17:41 JAHERMA 100 1000 Sulfate 1500 mg/L EPA 300.0 01/28/2013 17:41 JAHERMA 100 1000 MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND MERCURY 1631 - DISSOLVED - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND DISSOLVED METALS BY ICP Manganese (Mn) 0.079 mg/L EPA 200.7 01/28/2013 12:19 MHH7131 0.05 10 TOTAL RECOVERABLE METALS BY ICP Boron (B) 35.5 mg/L EPA 200.7 01/29/2013 13:46 MHH7131 0.5 10 Calcium (Ca) 945 mg/L EPA 200.7 01/29/2013 13:46 MHH7131 0.1 10 Iron (Fe) 0.740 mg/L EPA 200.7 01/29/2013 13:46 MHH7131 0.1 10 Magnesium (Mg) 175 mg/L EPA 200.7 01/29/2013 13:46 MHH7131 0.05 10 Manganese (Mn) 0.081 mg/L EPA 200.7 01/29/2013 13:46 MHH7131 0.05 10 DISSOLVED METALS BY ICP-MS Selenium (Se) 15.5 ug/L EPA 200.8 01/24/2013 11:41 KRICHAR 5 5 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 9.90 ug/L EPA 200.8 01/24/2013 10:20 KRICHAR 5 5 Cadmium (Cd) < 5 ug/L EPA 200.8 01/24/2013 10:20 KRICHAR 5 5 Chromium (Cr) < 5 ug/L EPA 200.8 01/24/2013 10:20 KRICHAR 5 5 Copper (Cu) < 5 ug/L EPA 200.8 01/24/2013 10:20 KRICHAR 5 5 Nickel (Ni) < 5 ug/L EPA 200.8 01/24/2013 10:20 KRICHAR 5 5 Selenium (Se) 11.9 ug/L EPA 200.8 01/24/2013 10:20 KRICHAR 5 5 Silver (Ag) < 5 ug/L EPA 200.8 01/24/2013 10:20 KRICHAR 5 5 Zinc (Zn) < 5 ug/L EPA 200.8 01/24/2013 10:20 KRICHAR 5 5 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C

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



## Order # J13010342

2013001403 Collection Date: 18-Jan-13 9:05 AM 

### Site: BioReactor 2 Eff BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND MERCURY 1631 - DISSOLVED - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND


### 2013001404 Collection Date: 18-Jan-13 12:10 PM 

### Site: Filter Blk Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF DISSOLVED METALS BY ICP Manganese (Mn) < 0.005 mg/L EPA 200.7 01/28/2013 11:44 MHH7131 0.005 1 DISSOLVED METALS BY ICP-MS Selenium (Se) 2.01 ug/L EPA 200.8 01/24/2013 11:17 KRICHAR 1 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 01/28/2013

Duke Energy Corporation Jay Perkins 13339 Hagers Ferry Road Huntersville, NC 28078 Project: Allen Wastewater - Nietering Project No.: J13010342 Lab Submittal Date: 01/22/2013 Prism Work Order: 3010460 VA Certification No. 1287 DoD ELAP Certification No. L2307



### 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 9

# Sample Receipt Summary 01/28/2013 

### Prism Work Order: 3010460 Client Sample ID Matrix Lab Sample ID Date Sampled Date Received 

### 3010460-01 01/18/13 2013001388/FGD Purge Eff 01/22/13 Water 3010460-02 01/18/13 2013001390/BioReactor 1 Inf 01/22/13 Water 3010460-03 01/18/13 2013001400/BioReactor 2 Inf 01/22/13 Water 3010460-04 01/18/13 2013001402/BioReactor 2 Eff 01/22/13 Water
Samples received in good condition at 3.0 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 9

# Laboratory Report 01/28/2013

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

### 13339 Hagers Ferry Road Project No.: Project: Allen Wastewater - Nietering Duke Energy Corporation

Huntersville, NC 28078 Attn: Jay Perkins Sample Matrix: Water Client Sample ID: Prism Sample ID: 3010460-01 Prism Work Order: 3010460 Time Collected: 01/18/13 10:51 Time Submitted: 01/22/13 11:00 2013001388/FGD Purge Eff


### J13010342

General Chemistry Parameters 7.3 *SM4500-H B P3A0402 1 1/22/13 14:35 JAB HT pH Units pH 37 *SM2320 B P3A0411 1 5.0 1/23/13 9:30 JAB mg/L 0.59 Total Alkalinity BRL *SM2320 B P3A0412 1 5.0 1/23/13 9:30 JAB mg/L 0.59 Carbonate Alkalinity 37 *SM2320 B P3A0413 1 5.0 1/23/13 9:30 JAB mg/L 0.59 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 9

# Laboratory Report 01/28/2013

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

### 13339 Hagers Ferry Road Project No.: Project: Allen Wastewater - Nietering Duke Energy Corporation

Huntersville, NC 28078 Attn: Jay Perkins Sample Matrix: Water Client Sample ID: Prism Sample ID: 3010460-02 Prism Work Order: 3010460 Time Collected: 01/18/13 08:30 Time Submitted: 01/22/13 11:00 2013001390/BioReactor 1 Inf


### J13010342

General Chemistry Parameters 6.8 *SM4500-H B P3A0402 1 1/22/13 14:35 JAB HT pH Units pH BRL *SM2320 B P3A0411 1 5.0 1/23/13 9:30 JAB mg/L 0.59 Total Alkalinity BRL *SM2320 B P3A0412 1 5.0 1/23/13 9:30 JAB mg/L 0.59 Carbonate Alkalinity BRL *SM2320 B P3A0413 1 5.0 1/23/13 9:30 JAB mg/L 0.59 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 9

# Laboratory Report 01/28/2013

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

### 13339 Hagers Ferry Road Project No.: Project: Allen Wastewater - Nietering Duke Energy Corporation

Huntersville, NC 28078 Attn: Jay Perkins Sample Matrix: Water Client Sample ID: Prism Sample ID: 3010460-03 Prism Work Order: 3010460 Time Collected: 01/18/13 08:40 Time Submitted: 01/22/13 11:00 2013001400/BioReactor 2 Inf


### J13010342

General Chemistry Parameters 7.2 *SM4500-H B P3A0402 1 1/22/13 14:35 JAB HT pH Units pH 70 *SM2320 B P3A0411 1 5.0 1/23/13 9:30 JAB mg/L 0.59 Total Alkalinity BRL *SM2320 B P3A0412 1 5.0 1/23/13 9:30 JAB mg/L 0.59 Carbonate Alkalinity 70 *SM2320 B P3A0413 1 5.0 1/23/13 9:30 JAB mg/L 0.59 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 9

# Laboratory Report 01/28/2013

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

### 13339 Hagers Ferry Road Project No.: Project: Allen Wastewater - Nietering Duke Energy Corporation

Huntersville, NC 28078 Attn: Jay Perkins Sample Matrix: Water Client Sample ID: Prism Sample ID: 3010460-04 Prism Work Order: 3010460 Time Collected: 01/18/13 08:34 Time Submitted: 01/22/13 11:00 2013001402/BioReactor 2 Eff


### J13010342

General Chemistry Parameters 7.3 *SM4500-H B P3A0402 1 1/22/13 14:35 JAB HT pH Units pH 98 *SM2320 B P3A0411 1 5.0 1/23/13 9:30 JAB mg/L 0.59 Total Alkalinity BRL *SM2320 B P3A0412 1 5.0 1/23/13 9:30 JAB mg/L 0.59 Carbonate Alkalinity 98 *SM2320 B P3A0413 1 5.0 1/23/13 9:30 JAB mg/L 0.59 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 6 of 91/28/13 

### Level II QC Report

13339 Hagers Ferry Road Project No: J13010342 Project: Allen Wastewater - Nietering Duke Energy Corporation

Huntersville, NC 28078 Attn: Jay Perkins Prism Work Order: 3010460 Time Submitted: 1/22/2013 11:00:00AM

Result Limit

Reporting Units Level Spike Result

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

Batch P3A0402 - NO PREP LCS (P3A0402-BS1) Prepared & Analyzed: 01/22/13 pH pH Units 6.86 6.860 99-101 100 Duplicate (P3A0402-DUP1) Prepared & Analyzed: 01/22/13 Source: 3010460-04 pH pH Units 7.34 7.34 10 0 Batch P3A0411 - NO PREP Blank (P3A0411-BLK1) Prepared & Analyzed: 01/23/13 Total Alkalinity mg/L BRL 5.0 LCS (P3A0411-BS1) Prepared & Analyzed: 01/23/13 Total Alkalinity mg/L 239 5.0 250.0 90-110 96 LCS Dup (P3A0411-BSD1) Prepared & Analyzed: 01/23/13 Total Alkalinity mg/L 239 5.0 250.0 200 90-110 96 0 Duplicate (P3A0411-DUP1) Prepared & Analyzed: 01/23/13 Source: 3010460-04 Total Alkalinity mg/L 102 5.0 98.0 20 4 Batch P3A0412 - NO PREP Blank (P3A0412-BLK1) Prepared & Analyzed: 01/23/13 Carbonate Alkalinity mg/L BRL 5.0 Duplicate (P3A0412-DUP1) Prepared & Analyzed: 01/23/13 Source: 3010460-04 Carbonate Alkalinity mg/L BRL 5.0 BRL 20

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 91/28/13 

### Level II QC Report

13339 Hagers Ferry Road Project No: J13010342 Project: Allen Wastewater - Nietering Duke Energy Corporation

Huntersville, NC 28078 Attn: Jay Perkins Prism Work Order: 3010460 Time Submitted: 1/22/2013 11:00:00AM

Result Limit

Reporting Units Level Spike Result

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

Batch P3A0413 - NO PREP Blank (P3A0413-BLK1) Prepared & Analyzed: 01/23/13 Bicarbonate Alkalinity mg/L BRL 5.0 LCS (P3A0413-BS1) Prepared & Analyzed: 01/23/13 Bicarbonate Alkalinity mg/L 239 5.0 250.0 90-110 96 LCS Dup (P3A0413-BSD1) Prepared & Analyzed: 01/23/13 Bicarbonate Alkalinity mg/L 239 5.0 250.0 200 90-110 96 0 Duplicate (P3A0413-DUP1) Prepared & Analyzed: 01/23/13 Source: 3010460-04 Bicarbonate Alkalinity mg/L 102 5.0 98.0 20 4

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 8 of 9

### Page 9 of 9

### 3958 6 th 

### Ave NW • Seattle, WA 98107 • T: 206

- 632

- 6206 • F: 206

- 632

- 6017 • www.brooksrand.com • brl@brooksrand.com 

## February 7, 2013 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

- HV1 201 Client P roject : J13010342 Dear Mr. Perkins, O n January 25, 2013 , Brooks Rand Labs ( BRL) received three(3 ) wastewater sample and one (1 ) corresponding field blank

. An aliquot was removed from each sample bottle and filtered into a separate container designed for dissolved mercury (Hg) analysis. The sample volume from the original container was logged

- in for total Hg analysis. A ll samples were received, prepared, analyzed, and stored according to BRL SOPs and EPA methodology. Data used for regulatory purposes has a 24 hour filtration holding time requirement. Non

regulatory purposed data has a 48 hour filtration holding time. The samples were received outside of the non

- regulatory requirement holding time and were qualified H

. The results were blank

- corrected as described in the calculations section of the relevant SOP and may have been evaluated using reporting limits that have been adjusted to account for sample aliquot size. Please refer to the Sample Results page for sample

- specific MDLs, MRLs, and other details. The dissolved Hg result of sample BioReactor 2 Eff H g Blk (1304022

- 12) was detectable at 0.19 ng/L and was qualified B . This concentration was less than the method defined control limit of 0.50 ng/L however; and the associated field sample result was greater than 10x the concentration of the blank. Contamination was considered insignificant. All data was reported without additional qualification, aside from concentration qualifiers, and all associated q uality 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 us if you have any questions regarding this report. Sincerely,

Tiffany Stilwater Mi Sun Um Project Manager Data Manager tiffany@brooksrand.com misun@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 Labs, those found in the EPA SOW ILM03.0, Exhibit B, Section III, pg. B-18, and the USEPA Contract Laboratory Program National Functional Guidelines for Inorganic Superfund Data Review; USEPA; January 2010. 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 

### 1304022-01 BioReactor 1 Inf 01/18/2013 01/25/2013 Sample Influent 1304022-02 BioReactor 1 Inf 01/18/2013 01/25/2013 Sample Influent 1304022-03 BioReactor 1 Inf Hg Blk 01/18/2013 01/25/2013 Field Blank DIW 1304022-04 BioReactor 1 Inf Hg Blk 01/18/2013 01/25/2013 Field Blank DIW 1304022-05 BioReactor 2 Inf 01/18/2013 01/25/2013 Sample Influent 1304022-06 BioReactor 2 Inf 01/18/2013 01/25/2013 Sample Influent 1304022-07 BioReactor 2 Inf Hg Blk 01/18/2013 01/25/2013 Field Blank DIW 1304022-08 BioReactor 2 Inf Hg Blk 01/18/2013 01/25/2013 Field Blank DIW 1304022-09 BioReactor 2 Eff 01/18/2013 01/25/2013 Sample Effluent 1304022-10 BioReactor 2 Eff 01/18/2013 01/25/2013 Sample Effluent 1304022-11 BioReactor 2 Eff Hg Blk 01/18/2013 01/25/2013 Field Blank DIW 1304022-12 BioReactor 2 Eff Hg Blk 01/18/2013 01/25/2013 Field Blank DIW 

# Batch Summary

Analyte Prepared Analyzed Sequence Batch Lab Matrix Method 

### B130128 01/29/2013 01/31/2013 1300071 Water EPA 1631 Hg

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

### DUK-HV1201

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Sample Results

Sample Sequence Result MDL MRL Unit Batch

Qualifier Analyte Basis

Report Matrix BioReactor 1 Inf 

### 152 T 1300071 B130128 Influent 2.02 0.76 1304022-01 Hg ng/L 26.1 D H 1300071 B130128 Influent 2.02 0.76 1304022-02 Hg ng/L
BioReactor 1 Inf Hg Blk 

### 0.15 T U 1300071 B130128 DIW 0.39 0.15 1304022-03 Hg ng/L 0.15 D H, U 1300071 B130128 DIW 0.39 0.15 1304022-04 Hg ng/L

BioReactor 2 Eff 

### 38.6 T 1300071 B130128 Effluent 0.40 0.15 1304022-09 Hg ng/L 4.85 D H 1300071 B130128 Effluent 0.40 0.15 1304022-10 Hg ng/L
BioReactor 2 Eff Hg Blk 

### 0.15 T U 1300071 B130128 DIW 0.41 0.15 1304022-11 Hg ng/L 0.19 D H, B 1300071 B130128 DIW 0.40 0.15 1304022-12 Hg ng/L

BioReactor 2 Inf 

### 105 T 1300071 B130128 Influent 1.02 0.38 1304022-05 Hg ng/L 7.70 D H 1300071 B130128 Influent 0.40 0.15 1304022-06 Hg ng/L
BioReactor 2 Inf Hg Blk 

### 0.15 T U 1300071 B130128 DIW 0.41 0.15 1304022-07 Hg ng/L 0.15 D H, U 1300071 B130128 DIW 0.41 0.15 1304022-08 Hg ng/L

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: 

### B130128

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

### EPA 1631 Lab Matrix: 

### Water

Sample Certified Reference Material (1301006, THg ICV 1641d) B130128-SRM1 

### 15.68 102% ng/L 85-115 Hg 16.07
Matrix Spike (1304021-05) B130128-MS2 

### 255.1 105% ng/L 71-125 Hg 345.3

76.86
Matrix Spike Duplicate (1304021-05) B130128-MSD2 

### 255.1 105% ng/L 71-125 240.1% Hg 345.8

76.86
Matrix Spike (1304022-09) B130128-MS3 

### 53.08 104% ng/L 71-125 Hg 93.59

38.63
Matrix Spike Duplicate (1304022-09) B130128-MSD3 

### 52.67 102% ng/L 71-125 242% Hg 92.14

38.63

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: 

### B130128
Method: 

### EPA 1631 Matrix: 

### Water Analyte: 

### Hg Result Units Sample 

### B130128-BLK1 ng/L 0.35 B130128-BLK2 ng/L 0.43 B130128-BLK3 ng/L 0.24 B130128-BLK4 ng/L 0.25 MDL: 

### 0.15 Average: 

### 0.32 Standard Deviation: 

### 0.09 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: 

### 1300071 Method: 

### EPA 1631 Instrument: 

### THG-05 Date: 

### 01/31/2013 Total Mercury and Mercury Speciation by CVAFS

Analyte: 

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

### 1300071-IBL1 1.14 pg of Hg 1300071-IBL2 2.63 pg of Hg 1300071-IBL3 3.17 pg of Hg 1300071-IBL4 3.35 pg of Hg 1300071-CAL1 10.00 10.27 pg of Hg 103% 1300071-CAL2 25.00 25.06 pg of Hg 100% 1300071-CAL3 100.0 98.35 pg of Hg 98% 1300071-CAL4 500.0 492.3 pg of Hg 98% 1300071-CAL5 2500 2478 pg of Hg 99% 1300071-CAL6 10000 10130 pg of Hg 101% 1300071-ICV1 1568 1607 pg of Hg 102% 85-115 1300071-CCB1 7.92 pg of Hg 1300071-CCV1 500.0 502.1 pg of Hg 100% 77-123 1300071-CCB2 5.03 pg of Hg 1300071-CCB3 5.29 pg of Hg 1300071-CCB4 4.31 pg of Hg 1300071-CCV2 500.0 500.9 pg of Hg 100% 77-123 1300071-CCB5 6.92 pg of Hg 1300071-CCV3 500.0 500.9 pg of Hg 100% 77-123 1300071-CCB6 4.05 pg of Hg 1300071-CCV4 500.0 511.4 pg of Hg 102% 77-123 1300071-CCB7 9.42 pg of Hg 1300071-CCV5 500.0 533.0 pg of Hg 107% 77-123 1300071-CCB8 7.74 pg of Hg 1300071-CCV6 500.0 532.6 pg of Hg 107% 77-123 1300071-CCB9 8.66 pg of Hg 1300071-CCV7 500.0 536.4 pg of Hg 107% 77-123 1300071-CCBA 8.76 pg of Hg 1300071-CCV8 500.0 526.2 pg of Hg 105% 77-123 1300071-CCBB 5.55 pg of Hg 1300071-CCV9 500.0 529.6 pg of Hg 106% 77-123 1300071-CCBC 6.39 pg of Hg 1300071-CCVA 500.0 524.4 pg of Hg 105% 77-123 1300071-CCBD 5.13 pg of Hg 1300071-CCVB 500.0 529.8 pg of Hg 106% 77-123 1300071-CCBE 5.65 pg of Hg 1300071-CCVC 500.0 523.0 pg of Hg 105% 77-123 1300071-CCBF 5.54 pg of Hg 1300071-CCVD 500.0 523.6 pg of Hg 105% 77-123 1300071-CCBG 4.88 pg of 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



# Instrument Calibration

Sequence: 

### 1300071 Method: 

### EPA 1631 Instrument: 

### THG-05 Date: 

### 01/31/2013 Total Mercury and Mercury Speciation by CVAFS

Analyte: 

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

### 1300071-CCVE 500.0 523.6 pg of Hg 105% 77-123 1300071-CCBH 3.67 pg of Hg 1300071-CCVF 500.0 516.9 pg of Hg 103% 77-123 1300071-CCBI 4.48 pg of Hg 1300071-CCVG 500.0 509.2 pg of Hg 102% 77-123 1300071-CCBJ 3.59 pg of Hg 1300071-CCVH 500.0 525.4 pg of Hg 105% 77-123 1300071-CCBK 5.51 pg of Hg 1300071-ICV2 1568 1672 pg of Hg 107% 85-115 1300071-CCVI 500.0 509.8 pg of Hg 102% 77-123 1300071-CCBL 4.04 pg of Hg 1300071-CCVJ 500.0 531.6 pg of Hg 106% 77-123 1300071-CCBM 4.48 pg of Hg 1300071-CCVK 500.0 531.4 pg of Hg 106% 77-123 1300071-CCBN 4.38 pg of 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



# Sample Containers

Lab ID: 

### 1304022-01 Report Matrix: 

### Influent Sample Type: 

### Sample Received: 

### 01/25/2013 Sample: 

### BioReactor 1 Inf Collected: 

### 01/18/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 76663301 0 Cooler

none n/a 500mL Bottle FLPE Hg-T

Lab ID: 

### 1304022-02 Report Matrix: 

### Influent Sample Type: 

### Sample Received: 

### 01/25/2013 Sample: 

### BioReactor 1 Inf Collected: 

### 01/18/2013
Comments: 

### Qualify H Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 13-0001 Cooler none n/a 250mL Bottle FLPE Hg-T

Lab ID: 

### 1304022-03 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 01/25/2013 Sample: 

### BioReactor 1 Inf Hg Blk Collected: 

### 01/18/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 76663301 0 Cooler

none n/a 500mL Bottle FLPE Hg-T

Lab ID: 

### 1304022-04 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 01/25/2013 Sample: 

### BioReactor 1 Inf Hg Blk Collected: 

### 01/18/2013
Comments: 

### Qualify H Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 13-0001 Cooler none n/a 250mL Bottle FLPE Hg-T

Lab ID: 

### 1304022-05 Report Matrix: 

### Influent Sample Type: 

### Sample Received: 

### 01/25/2013 Sample: 

### BioReactor 2 Inf Collected: 

### 01/18/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 76663301 0 Cooler

none n/a 500mL Bottle FLPE Hg-T

Lab ID: 

### 1304022-06 Report Matrix: 

### Influent Sample Type: 

### Sample Received: 

### 01/25/2013 Sample: 

### BioReactor 2 Inf Collected: 

### 01/18/2013
Comments: 

### Qualify H Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 13-0001 Cooler none n/a 250mL Bottle FLPE Hg-T

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

### DUK-HV1201

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Sample Containers

Lab ID: 

### 1304022-07 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 01/25/2013 Sample: 

### BioReactor 2 Inf Hg Blk Collected: 

### 01/18/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 76663301 0 Cooler

none n/a 500mL Bottle FLPE Hg-T

Lab ID: 

### 1304022-08 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 01/25/2013 Sample: 

### BioReactor 2 Inf Hg Blk Collected: 

### 01/18/2013
Comments: 

### Qualify H Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 13-0001 Cooler none n/a 250mL Bottle FLPE Hg-T

Lab ID: 

### 1304022-09 Report Matrix: 

### Effluent Sample Type: 

### Sample Received: 

### 01/25/2013 Sample: 

### BioReactor 2 Eff Collected: 

### 01/18/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 76663301 0 Cooler

none n/a 500mL Bottle FLPE Hg-T

Lab ID: 

### 1304022-10 Report Matrix: 

### Effluent Sample Type: 

### Sample Received: 

### 01/25/2013 Sample: 

### BioReactor 2 Eff Collected: 

### 01/18/2013
Comments: 

### Qualify H Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 13-0001 Cooler none n/a 250mL Bottle FLPE Hg-T

Lab ID: 

### 1304022-11 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 01/25/2013 Sample: 

### BioReactor 2 Eff Hg Blk Collected: 

### 01/18/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 76663301 0 Cooler

none n/a 500mL Bottle FLPE Hg-T

Lab ID: 

### 1304022-12 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 01/25/2013 Sample: 

### BioReactor 2 Eff Hg Blk Collected: 

### 01/18/2013
Comments: 

### Qualify H Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 13-0001 Cooler none n/a 250mL Bottle FLPE Hg-T

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

### DUK-HV1201

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Shipping Containers

Cooler Tracking No: 

### 535305197910 via FedEx Temperature: 

### 0.9 °C Coolant Type: 

### Ice Description: 

### Cooler Damaged in transit? 

### No Returned to client? 

### No Custody seals present? 

### Yes Custody seals intact? 

### Yes COC present? 

### Yes Received: 

### January 25, 2013 8:30

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

## February 7, 201 3

Jay Perkins Duke Energy Analytical Laboratory Mail Code MGO3A2 (Building 7405) 13339 Hagers Ferry Rd. Huntersville, NC 28078 (704) 875-5 245 Project: Allen Wastewater - Nietering (January 2013 - Test Burn) (LIMS #J13010342)

Dear Mr. Perkins, Attached is the report associated with four (4 ) aqueous samples submitted for selenium speciation on January 24 , 2013

. The samples were received in a sealed cooler at-0. 1 ° C on January 25 , 2013

. Selenium speciation analysis was performed via ion chromatography inductively coupled plasma collision reaction cell mass spectrometry (IC-ICP- CRC -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: Allen Wastewater - Nietering (January 2013 - Test Burn) (LIMS #J13010342)
February 7, 2013

1. Sample Reception Four (4 ) aqueous samples in125mL HDPE bottles (provided by Applied Speciation and Consulting) were submitted for selenium speciation analysis on January 24 , 2013 . The samples were received on January 25 , 201 3 in a sealed container at -0. 1 °C. The samples were received in a laminar flow clean hood, void of trace metals contamination and ultra-violet radiation, and were designated discrete sample identifiers. An aliquot of each sample was filtered (0.45μm) and each filtrate w asstored 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 an 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 correctedto 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 minimum interval of every ten analytical runs. Selenium Speciation Analysis by IC-ICP-CRC-MS Eachsample for selenium speciation analysis w asanalyzed by ion chromatography inductively coupled plasma collision reaction cell mass spectrometry (IC-ICP- CRC -MS) on January 30, 2013. Analiquot of each sample isinjected 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 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 the 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,

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 499 86.4 ND (<5.2) ND (<6.3) ND (<6.3) 0.0 (0) BioReactor 1 Inf 27.3 15.1 ND (<1.3) ND (<1.6) ND (<1.6) 0.0 (0) BioReactor 2 Inf 2.5 ND (<0.95) ND (<1.3) ND (<1.6) ND (<1.6) 0.0 (0) BioReactor 2 Eff ND (<2.5) ND (<0.95) ND (<1.3) ND (<1.6) ND (<1.6) 0.0 (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 Report Generated by: Russell Gerads Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Allen Wastewater - Nietering (January 2013 - Test Burn) Contact: Jay Perkins
Date: February 7, 2013 LIMS #J13010342

### Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 250x eMDL 1000x Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.010 2.5 9.8 Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.95 3.8 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.005 1.3 5.2 MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.006 1.6 6.3 SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.006 1.6 6.3 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 9.64 100.8 Se(VI) LCS 9.48 9.01 95.1 SeCN LCS 8.92 8.50 95.2 MeSe(IV) LCS 6.47 6.09 94.2 SeMe LCS 9.32 8.58 92.0 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Allen Wastewater - Nietering (January 2013 - Test Burn) Contact: Jay Perkins LIMS #J13010342 Date: February 7, 2013 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 5.80 5.27 5.5 9.7 Se(VI) Batch QC ND (<0.95) ND (<0.95) NC NC SeCN Batch QC ND (<1.3) ND (<1.3) NC NC MeSe(IV) Batch QC ND (<1.6) ND (<1.6) NC NC SeMe Batch QC ND (<1.6) ND (<1.6) 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 1390 1272 91.1 1390 1256 90.0 1.3 Se(VI) Batch QC 1261 1049 83.2 1261 1031 81.8 1.7 SeCN Batch QC 1144 879.6 76.9 1144 867.2 75.8 1.4 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Allen Wastewater - Nietering (January 2013 - Test Burn) Contact: Jay Perkins LIMS #J13010342 Date: February 7, 2013 Report Generated by: Russell Gerads