### 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: J13020306 Project Name: Wastewater Nietering

L ab Contact: Jason C Perkins 

### Date: 3/7/2013 Customer Address: 253 Plant Allen Road Customer Name(s): Robbin Jolly, Bill Kennedy, Ron Laws

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 2013004043 ALLEN 13-Feb-13 7:45 AM BILL HASKINS FGD Purge Eff 2013004044 ALLEN 13-Feb-13 7:50 AM BILL HASKINS EQ Tank Eff 2013004045 ALLEN 13-Feb-13 7:48 AM BILL HASKINS BioReactor 1 Inf 2013004046 ALLEN 13-Feb-13 8:10 AM BILL HASKINS BioReactor 1 Inf BLANK 2013004047 ALLEN 13-Feb-13 7:55 AM BILL HASKINS BioReactor 2 Inf 2013004048 ALLEN 13-Feb-13 8:15 AM BILL HASKINS BioReactor 2 Inf BLANK 2013004049 ALLEN 13-Feb-13 7:52 AM BILL HASKINS BioReactor 2 Eff 2013004050 ALLEN 13-Feb-13 8:12 AM BILL HASKINS BioReactor 2 Eff BLANK 2013004051 ALLEN 13-Feb-13 9:20 AM BILL HASKINS 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: 

### 3/7/2013 Electronic Data Deliverable (EDD) Sent Separately

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



## Order # J13020306

2013004043 Collection Date: 13-Feb-13 7:45 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 22 mg/L EPA 300.0 02/25/2013 18:23 JAHERMA 5 50 Chloride 2400 mg/L EPA 300.0 02/25/2013 18:23 JAHERMA 50 500 Sulfate 2200 mg/L EPA 300.0 02/25/2013 18:23 JAHERMA 50 500 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 37.6 ug/L EPA 245.1 02/21/2013 13:29 AGIBBS 2.5 50 DISSOLVED METALS BY ICP Manganese (Mn) 1.20 mg/L EPA 200.7 02/18/2013 12:38 MHH7131 0.05 10 TOTAL RECOVERABLE METALS BY ICP Boron (B) 330 mg/L EPA 200.7 02/19/2013 12:29 MHH7131 0.5 10 Calcium (Ca) 1710 mg/L EPA 200.7 02/19/2013 12:29 MHH7131 0.1 10 Iron (Fe) 127 mg/L EPA 200.7 02/19/2013 12:29 MHH7131 0.1 10 Magnesium (Mg) 1060 mg/L EPA 200.7 02/19/2013 12:29 MHH7131 0.05 10 Manganese (Mn) 6.63 mg/L EPA 200.7 02/19/2013 12:29 MHH7131 0.05 10 DISSOLVED METALS BY ICP-MS Selenium (Se) 316 ug/L EPA 200.8 03/04/2013 14:33 KRICHAR 10 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 221 ug/L EPA 200.8 03/05/2013 12:54 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 03/05/2013 12:54 KRICHAR 10 10 Chromium (Cr) 207 ug/L EPA 200.8 03/05/2013 12:54 KRICHAR 10 10 Copper (Cu) 137 ug/L EPA 200.8 03/05/2013 12:54 KRICHAR 10 10 Nickel (Ni) 238 ug/L EPA 200.8 03/05/2013 12:54 KRICHAR 10 10 Selenium (Se) 695 ug/L EPA 200.8 03/05/2013 12:54 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 03/05/2013 12:54 KRICHAR 10 10 Zinc (Zn) 322 ug/L EPA 200.8 03/05/2013 12:54 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 9800 mg/L SM2540C 02/21/2013 15:43 SWILLI3 200 1 TOTAL SUSPENDED SOLIDS TSS 2600 mg/L SM2540D 02/21/2013 11:18 SWILLI3 250 1

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



## Order # J13020306

2013004044 Collection Date: 13-Feb-13 7:50 AM 

### Site: EQ Tank Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 24.6 ug/L EPA 245.1 02/21/2013 13:32 AGIBBS 2.5 50 DISSOLVED METALS BY ICP Manganese (Mn) < 0.05 mg/L EPA 200.7 02/18/2013 12:41 MHH7131 0.05 10 TOTAL RECOVERABLE METALS BY ICP Boron (B) 296 mg/L EPA 200.7 02/19/2013 12:33 MHH7131 0.5 10 Calcium (Ca) 1550 mg/L EPA 200.7 02/19/2013 12:33 MHH7131 0.1 10 Iron (Fe) 81.3 mg/L EPA 200.7 02/19/2013 12:33 MHH7131 0.1 10 Magnesium (Mg) 930 mg/L EPA 200.7 02/19/2013 12:33 MHH7131 0.05 10 Manganese (Mn) 4.09 mg/L EPA 200.7 02/19/2013 12:33 MHH7131 0.05 10 DISSOLVED METALS BY ICP-MS Selenium (Se) 234 ug/L EPA 200.8 03/04/2013 14:36 KRICHAR 10 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 142 ug/L EPA 200.8 03/05/2013 12:32 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 03/05/2013 12:32 KRICHAR 10 10 Chromium (Cr) 134 ug/L EPA 200.8 03/05/2013 12:32 KRICHAR 10 10 Copper (Cu) 89.1 ug/L EPA 200.8 03/05/2013 12:32 KRICHAR 10 10 Nickel (Ni) 153 ug/L EPA 200.8 03/05/2013 12:32 KRICHAR 10 10 Selenium (Se) 498 ug/L EPA 200.8 03/05/2013 12:32 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 03/05/2013 12:32 KRICHAR 10 10 Zinc (Zn) 214 ug/L EPA 200.8 03/05/2013 12:32 KRICHAR 10 10


### 2013004045 Collection Date: 13-Feb-13 7:48 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) < 0.05 mg/L EPA 200.7 02/18/2013 12:45 MHH7131 0.05 10

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



## Order # J13020306

2013004045 Collection Date: 13-Feb-13 7:48 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) 280 mg/L EPA 200.7 02/19/2013 12:37 MHH7131 0.5 10 Calcium (Ca) 1460 mg/L EPA 200.7 02/19/2013 12:37 MHH7131 0.1 10 Iron (Fe) < 0.1 mg/L EPA 200.7 02/19/2013 12:37 MHH7131 0.1 10 Magnesium (Mg) 827 mg/L EPA 200.7 02/19/2013 12:37 MHH7131 0.05 10 Manganese (Mn) < 0.05 mg/L EPA 200.7 02/19/2013 12:37 MHH7131 0.05 10 DISSOLVED METALS BY ICP-MS Selenium (Se) 255 ug/L EPA 200.8 03/04/2013 15:10 KRICHAR 10 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 03/05/2013 12:35 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 03/05/2013 12:35 KRICHAR 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 03/05/2013 12:35 KRICHAR 10 10 Copper (Cu) < 10 ug/L EPA 200.8 03/05/2013 12:35 KRICHAR 10 10 Nickel (Ni) < 10 ug/L EPA 200.8 03/05/2013 12:35 KRICHAR 10 10 Selenium (Se) 231 ug/L EPA 200.8 03/05/2013 12:35 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 03/05/2013 12:35 KRICHAR 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 03/05/2013 12:35 KRICHAR 10 10 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C


### 2013004046 Collection Date: 13-Feb-13 8:10 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


### 2013004047 Collection Date: 13-Feb-13 7:55 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 # J13020306

2013004047 Collection Date: 13-Feb-13 7:55 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) < 0.05 mg/L EPA 200.7 02/18/2013 12:49 MHH7131 0.05 10 TOTAL RECOVERABLE METALS BY ICP Boron (B) 292 mg/L EPA 200.7 02/19/2013 12:41 MHH7131 0.5 10 Calcium (Ca) 1510 mg/L EPA 200.7 02/19/2013 12:41 MHH7131 0.1 10 Iron (Fe) < 0.1 mg/L EPA 200.7 02/19/2013 12:41 MHH7131 0.1 10 Magnesium (Mg) 847 mg/L EPA 200.7 02/19/2013 12:41 MHH7131 0.05 10 Manganese (Mn) < 0.05 mg/L EPA 200.7 02/19/2013 12:41 MHH7131 0.05 10 DISSOLVED METALS BY ICP-MS Selenium (Se) 144 ug/L EPA 200.8 03/04/2013 15:13 KRICHAR 10 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 03/05/2013 12:39 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 03/05/2013 12:39 KRICHAR 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 03/05/2013 12:39 KRICHAR 10 10 Copper (Cu) < 10 ug/L EPA 200.8 03/05/2013 12:39 KRICHAR 10 10 Nickel (Ni) < 10 ug/L EPA 200.8 03/05/2013 12:39 KRICHAR 10 10 Selenium (Se) 157 ug/L EPA 200.8 03/05/2013 12:39 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 03/05/2013 12:39 KRICHAR 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 03/05/2013 12:39 KRICHAR 10 10 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C


### 2013004048 Collection Date: 13-Feb-13 8:15 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 # J13020306

2013004049 Collection Date: 13-Feb-13 7:52 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 39 mg/L EPA 300.0 02/25/2013 18:42 JAHERMA 5 50 Chloride 3100 mg/L EPA 300.0 02/25/2013 18:42 JAHERMA 50 500 Sulfate 2300 mg/L EPA 300.0 02/25/2013 18:42 JAHERMA 50 500 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) 0.053 mg/L EPA 200.7 02/18/2013 12:53 MHH7131 0.05 10 TOTAL RECOVERABLE METALS BY ICP Boron (B) 274 mg/L EPA 200.7 02/19/2013 12:45 MHH7131 0.5 10 Calcium (Ca) 1480 mg/L EPA 200.7 02/19/2013 12:45 MHH7131 0.1 10 Iron (Fe) < 0.1 mg/L EPA 200.7 02/19/2013 12:45 MHH7131 0.1 10 Magnesium (Mg) 878 mg/L EPA 200.7 02/19/2013 12:45 MHH7131 0.05 10 Manganese (Mn) 0.053 mg/L EPA 200.7 02/19/2013 12:45 MHH7131 0.05 10 DISSOLVED METALS BY ICP-MS Selenium (Se) 7.02 ug/L EPA 200.8 03/04/2013 15:16 KRICHAR 5 5 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 5 ug/L EPA 200.8 03/05/2013 12:47 KRICHAR 5 5 Cadmium (Cd) < 5 ug/L EPA 200.8 03/05/2013 12:47 KRICHAR 5 5 Chromium (Cr) < 5 ug/L EPA 200.8 03/05/2013 12:47 KRICHAR 5 5 Copper (Cu) < 5 ug/L EPA 200.8 03/05/2013 12:47 KRICHAR 5 5 Nickel (Ni) < 5 ug/L EPA 200.8 03/05/2013 12:47 KRICHAR 5 5 Selenium (Se) 5.31 ug/L EPA 200.8 03/05/2013 12:47 KRICHAR 5 5 Silver (Ag) < 5 ug/L EPA 200.8 03/05/2013 12:47 KRICHAR 5 5 Zinc (Zn) < 5 ug/L EPA 200.8 03/05/2013 12:47 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 # J13020306

2013004050 Collection Date: 13-Feb-13 8:12 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


### 2013004051 Collection Date: 13-Feb-13 9:20 AM 

### 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 02/18/2013 12:30 MHH7131 0.005 1 DISSOLVED METALS BY ICP-MS Selenium (Se) < 1 ug/L EPA 200.8 03/04/2013 13:52 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 02/22/2013

Duke Energy Corporation Jay Perkins 13339 Hagers Ferry Road Huntersville, NC 28078 Project: Allen WW - Nietering (January 2013-Test Burn) Project No.: J13020306 Lab Submittal Date: 02/15/2013 Prism Work Order: 3020381 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 02/22/2013 

### Prism Work Order: 3020381 Client Sample ID Matrix Lab Sample ID Date Sampled Date Received 

### 3020381-01 02/13/13 2013004043/FGD Purge Eff 02/15/13 Water 3020381-02 02/13/13 2013004045/BioReactor 1 Inf 02/15/13 Water 3020381-03 02/13/13 2013004047/BioReactor 2 Inf 02/15/13 Water 3020381-04 02/13/13 2013004049/BioReactor 2 Eff 02/15/13 Water Samples received in good condition at 2.3 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 02/22/2013

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

### 13339 Hagers Ferry Road Project No.: Project: Allen WW - Nietering (January 2013-Test Burn) Duke Energy Corporation

Huntersville, NC 28078 Attn: Jay Perkins Sample Matrix: Water Client Sample ID: Prism Sample ID: 3020381-01 Prism Work Order: 3020381 Time Collected: 02/13/13 07:45 Time Submitted: 02/15/13 15:00 2013004043/FGD Purge Eff


### J13020306

General Chemistry Parameters 6.6 *SM4500-H B P3B0328 1 2/15/13 15:20 JAB HT pH Units pH 47 *SM2320 B P3B0451 1 5.0 2/21/13 13:20 JAB mg/L 0.59 Total Alkalinity BRL *SM2320 B P3B0452 1 5.0 2/21/13 13:20 JAB mg/L 0.59 Carbonate Alkalinity 47 *SM2320 B P3B0453 1 5.0 2/21/13 13:20 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 02/22/2013

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

### 13339 Hagers Ferry Road Project No.: Project: Allen WW - Nietering (January 2013-Test Burn) Duke Energy Corporation

Huntersville, NC 28078 Attn: Jay Perkins Sample Matrix: Water Client Sample ID: Prism Sample ID: 3020381-02 Prism Work Order: 3020381 Time Collected: 02/13/13 07:48 Time Submitted: 02/15/13 15:00 2013004045/BioReactor 1 Inf


### J13020306

General Chemistry Parameters 7.2 *SM4500-H B P3B0328 1 2/15/13 15:20 JAB HT pH Units pH 91 *SM2320 B P3B0451 1 5.0 2/21/13 13:20 JAB mg/L 0.59 Total Alkalinity BRL *SM2320 B P3B0452 1 5.0 2/21/13 13:20 JAB mg/L 0.59 Carbonate Alkalinity 91 *SM2320 B P3B0453 1 5.0 2/21/13 13:20 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 02/22/2013

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

### 13339 Hagers Ferry Road Project No.: Project: Allen WW - Nietering (January 2013-Test Burn) Duke Energy Corporation

Huntersville, NC 28078 Attn: Jay Perkins Sample Matrix: Water Client Sample ID: Prism Sample ID: 3020381-03 Prism Work Order: 3020381 Time Collected: 02/13/13 07:55 Time Submitted: 02/15/13 15:00 2013004047/BioReactor 2 Inf


### J13020306

General Chemistry Parameters 6.9 *SM4500-H B P3B0328 1 2/15/13 15:20 JAB HT pH Units pH 280 *SM2320 B P3B0451 1 5.0 2/21/13 13:20 JAB mg/L 0.59 Total Alkalinity BRL *SM2320 B P3B0452 1 5.0 2/21/13 13:20 JAB mg/L 0.59 Carbonate Alkalinity 280 *SM2320 B P3B0453 1 5.0 2/21/13 13:20 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 02/22/2013

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

### 13339 Hagers Ferry Road Project No.: Project: Allen WW - Nietering (January 2013-Test Burn) Duke Energy Corporation

Huntersville, NC 28078 Attn: Jay Perkins Sample Matrix: Water Client Sample ID: Prism Sample ID: 3020381-04 Prism Work Order: 3020381 Time Collected: 02/13/13 07:52 Time Submitted: 02/15/13 15:00 2013004049/BioReactor 2 Eff


### J13020306

General Chemistry Parameters 7.2 *SM4500-H B P3B0328 1 2/15/13 15:20 JAB HT pH Units pH 290 *SM2320 B P3B0451 1 5.0 2/21/13 13:20 JAB mg/L 0.59 Total Alkalinity BRL *SM2320 B P3B0452 1 5.0 2/21/13 13:20 JAB mg/L 0.59 Carbonate Alkalinity 290 *SM2320 B P3B0453 1 5.0 2/21/13 13:20 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 92/22/13 

### Level II QC Report

13339 Hagers Ferry Road Project No: J13020306 Project: Allen WW - Nietering (January 2013-Test Burn) Duke Energy Corporation

Huntersville, NC 28078 Attn: Jay Perkins Prism Work Order: 3020381 Time Submitted: 2/15/2013 3:00:00PM

Result Limit

Reporting Units Level Spike Result

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

Batch P3B0328 - NO PREP LCS (P3B0328-BS1) Prepared & Analyzed: 02/15/13 pH pH Units 6.90 6.880 99-101 100 Batch P3B0451 - NO PREP Blank (P3B0451-BLK1) Prepared & Analyzed: 02/21/13 Total Alkalinity mg/L BRL 5.0 LCS (P3B0451-BS1) Prepared & Analyzed: 02/21/13 Total Alkalinity mg/L 250 5.0 250.0 90-110 100 LCS Dup (P3B0451-BSD1) Prepared & Analyzed: 02/21/13 Total Alkalinity mg/L 256 5.0 250.0 200 90-110 102 2 Batch P3B0452 - NO PREP Blank (P3B0452-BLK1) Prepared & Analyzed: 02/21/13 Carbonate Alkalinity mg/L BRL 5.0 Batch P3B0453 - NO PREP Blank (P3B0453-BLK1) Prepared & Analyzed: 02/21/13 Bicarbonate Alkalinity mg/L BRL 5.0 LCS (P3B0453-BS1) Prepared & Analyzed: 02/21/13 Bicarbonate Alkalinity mg/L 250 5.0 250.0 90-110 100

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 92/22/13 

### Level II QC Report

13339 Hagers Ferry Road Project No: J13020306 Project: Allen WW - Nietering (January 2013-Test Burn) Duke Energy Corporation

Huntersville, NC 28078 Attn: Jay Perkins Prism Work Order: 3020381 Time Submitted: 2/15/2013 3:00:00PM

Result Limit

Reporting Units Level Spike Result

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

Batch P3B0453 - NO PREP LCS Dup (P3B0453-BSD1) Prepared & Analyzed: 02/21/13 Bicarbonate Alkalinity mg/L 256 5.0 250.0 200 90-110 102 2

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 

## March 4, 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 : J13020306 Dear Mr. Perkins, O n February 20, 2013 , Brooks Rand Labs ( BRL) received three(3 ) wastewater sample and three(3 ) corresponding field blanks. 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 . All 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 time limit and the results 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. Sample BioReactor 2 Eff Hg Blk was identified as a field blank even though the results clearly indicated otherwise. The associated field sample results were non

- detectable and BRL suspects as the cause was mislabeling in the field. 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 me if you have any questions. 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 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: 

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### Tiffany Stilwater Client PM: 

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# Sample Information

Report Matrix Type Received Sampled Sample Lab ID 

### 1308006-01 BioReactor 1 Inf 02/13/2013 02/20/2013 Sample Influent 1308006-02 BioReactor 1 Inf 02/13/2013 02/20/2013 Sample Influent 1308006-03 BioReactor 1 Inf Hg Blk 02/13/2013 02/20/2013 Field Blank DIW 1308006-04 BioReactor 1 Inf Hg Blk 02/13/2013 02/20/2013 Field Blank DIW 1308006-05 BioReactor 2 Inf 02/13/2013 02/20/2013 Sample Influent 1308006-06 BioReactor 2 Inf 02/13/2013 02/20/2013 Sample Influent 1308006-07 BioReactor 2 Inf Hg Blk 02/13/2013 02/20/2013 Field Blank DIW 1308006-08 BioReactor 2 Inf Hg Blk 02/13/2013 02/20/2013 Field Blank DIW 1308006-09 BioReactor 2 Eff 02/13/2013 02/20/2013 Sample Effluent 1308006-10 BioReactor 2 Eff 02/13/2013 02/20/2013 Sample Effluent 1308006-11 BioReactor 2 Eff Hg Blk 02/13/2013 02/20/2013 Field Blank DIW 1308006-12 BioReactor 2 Eff Hg Blk 02/13/2013 02/20/2013 Field Blank DIW 

# Batch Summary

Analyte Prepared Analyzed Sequence Batch Lab Matrix Method 

### B130316 02/22/2013 02/26/2013 1300129 Water EPA 1631 Hg

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# Sample Results

Sample Sequence Result MDL MRL Unit Batch

Qualifier Analyte Basis

Report Matrix BioReactor 1 Inf 

### 450 T 1300129 B130316 Influent 10.1 3.79 1308006-01 Hg ng/L 34.1 D H 1300129 B130316 Influent 2.02 0.76 1308006-02 Hg ng/L
BioReactor 1 Inf Hg Blk 

### 0.15 T U 1300129 B130316 DIW 0.40 0.15 1308006-03 Hg ng/L 0.15 D H, U 1300129 B130316 DIW 0.41 0.15 1308006-04 Hg ng/L

BioReactor 2 Eff 

### 0.31 T B 1300129 B130316 Ef fluent 0.41 0.15 1308006-09 Hg ng/L 0.15 D H, U 1300129 B130316 Effluent 0.40 0.15 1308006-10 Hg ng/L
BioReactor 2 Eff Hg Blk 

### 99.7 T 1300129 B130316 DIW 0.41 0.15 1308006-11 Hg ng/L 22.8 D H 1300129 B130316 DIW 0.39 0.15 1308006-12 Hg ng/L

BioReactor 2 Inf 

### 379 T 1300129 B130316 Influent 2.04 0.77 1308006-05 Hg ng/L 17.0 D H 1300129 B130316 Influent 0.40 0.15 1308006-06 Hg ng/L
BioReactor 2 Inf Hg Blk 

### 0.15 T U 1300129 B130316 DIW 0.41 0.15 1308006-07 Hg ng/L 0.15 D H, U 1300129 B130316 DIW 0.39 0.15 1308006-08 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: 

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# Accuracy & Precision Summary

Batch: 

### B130316

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

### EPA

1631 Lab Matrix: 

### Water

Sample Certified Reference Material (1307035, NIST 1641d 1000x dilution) B130316-SRM1 

### 15.68 100% ng/L 0-200 Hg 15.74
Matrix Spike (1308006-01) B130316-MS2 

### 2525 89% ng/L 71-125 Hg 2695

450.4
Matrix Spike Duplicate (1308006-01) B130316-MSD2 

### 2525 97% ng/L 71-125 248% Hg 2908

450.4
Matrix Spike (1308007-05) B130316-MS3 

### 1786 90% ng/L 71-125 Hg 1761

158.6
Matrix Spike Duplicate (1308007-05) B130316-MSD3 

### 1786 100% ng/L 71-125 2410% Hg 1940

158.6

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

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# Method Blanks & Reporting Limits

Batch: 

### B130316
Method: 

### EPA

1631 Matrix: 

### Water Analyte: 

### Hg Result Units Sample 

### B130316-BLK1 ng/L 0.18 B130316-BLK2 ng/L 0.26 B130316-BLK3 ng/L 0.22 B130316-BLK4 ng/L 0.17 MDL: 

### 0.15 Average: 

### 0.21 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: 

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# Instrument Calibration

Sequence: 

### 1300129 Method: 

### EPA 1631 Instrument: 

### THG-06 Date: 

### 02/26/2013 Total Mercury and Mercury Speciation by CVAFS

Analyte: 

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

### 1300129-IBL1 2.41 pg of Hg 1300129-IBL2 2.83 pg of Hg 1300129-IBL3 4.00 pg of Hg 1300129-IBL4 4.24 pg of Hg 1300129-CAL1 10.00 10.38 pg of Hg 104% 1300129-CAL2 25.00 25.12 pg of Hg 100% 1300129-CAL3 100.0 101.0 pg of Hg 101% 1300129-CAL4 500.0 489.4 pg of Hg 98% 1300129-CAL5 2500 2502 pg of Hg 100% 1300129-CAL6 10000 9706 pg of Hg 97% 1300129-ICV1 1568 1574 pg of Hg 100% 85-115 1300129-CCB1 6.86 pg of Hg 1300129-CCV1 500.0 499.3 pg of Hg 100% 77-123 1300129-CCB2 4.75 pg of Hg 1300129-CCB3 4.72 pg of Hg 1300129-CCB4 5.34 pg of Hg 1300129-CCV2 500.0 500.7 pg of Hg 100% 77-123 1300129-CCB5 5.63 pg of Hg 1300129-CCV3 500.0 492.7 pg of Hg 99% 77-123 1300129-CCB6 7.52 pg of Hg 1300129-CCV4 500.0 488.5 pg of Hg 98% 77-123 1300129-CCB7 5.88 pg of Hg 1300129-CCV5 500.0 470.9 pg of Hg 94% 77-123 1300129-CCB8 5.49 pg of Hg 1300129-CCV6 500.0 452.8 pg of Hg 91% 77-123 1300129-CCB9 4.99 pg of Hg 1300129-CCV7 500.0 458.0 pg of Hg 92% 77-123 1300129-CCBA 5.30 pg of Hg 1300129-CCV8 500.0 469.2 pg of Hg 94% 77-123 1300129-CCBB 5.41 pg of Hg 1300129-CCV9 500.0 452.7 pg of Hg 91% 77-123 1300129-CCBC 6.44 pg of Hg 1300129-CCVA 500.0 461.7 pg of Hg 92% 77-123 1300129-CCBD 6.88 pg of Hg 1300129-CCVB 500.0 456.0 pg of Hg 91% 77-123 1300129-CCBE 5.17 pg of Hg 1300129-CCVC 500.0 458.9 pg of Hg 92% 77-123 1300129-CCBF 4.42 pg of Hg 1300129-CCVD 500.0 462.8 pg of Hg 93% 77-123 1300129-CCBG 5.15 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: 

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# Instrument Calibration

Sequence: 

### 1300129 Method: 

### EPA 1631 Instrument: 

### THG-06 Date: 

### 02/26/2013 Total Mercury and Mercury Speciation by CVAFS

Analyte: 

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

### 1300129-CCVE 500.0 465.0 pg of Hg 93% 77-123 1300129-CCBH 6.13 pg of Hg 1300129-CCVF 500.0 464.5 pg of Hg 93% 77-123 1300129-CCBI 5.88 pg of Hg 1300129-CCVG 500.0 470.0 pg of Hg 94% 77-123 1300129-CCBJ 5.70 pg of Hg 1300129-CCVH 500.0 494.6 pg of Hg 99% 77-123 1300129-CCBK 5.05 pg of Hg 1300129-ICV2 1568 1557 pg of Hg 99% 85-115 1300129-CCVI 500.0 475.0 pg of Hg 95% 77-123 1300129-CCBL 4.94 pg of Hg 1300129-CCVJ 500.0 450.4 pg of Hg 90% 77-123 1300129-CCBM 4.40 pg of Hg 1300129-CCVK 500.0 449.4 pg of Hg 90% 77-123 1300129-CCBN 4.27 pg of Hg 1300129-CCVL 500.0 455.3 pg of Hg 91% 77-123 1300129-CCBO 3.88 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: 

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# Sample Containers

Lab ID: 

### 1308006-01 Report Matrix: 

### Influent Sample Type : 

### Sample Received: 

### 02/20/2013 Sample: 

### BioReactor 1 Inf Collected: 

### 02/13/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71666330 10 Cooler

none n/a 500mL Bottle FLPE Hg-T

Lab ID: 

### 1308006-02 Report Matrix: 

### Influent Sample Type: 

### Sample Received: 

### 02/20/2013 Sample: 

### BioReactor 1 Inf Collected: 

### 02/13/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

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

Lab ID: 

### 1308006-03 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 02/20/2013 Sample: 

### BioReactor 1 Inf Hg Blk Collected: 

### 02/13/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71666330 10 Cooler

none n/a 500mL Bottle FLPE Hg-T

Lab ID: 

### 1308006-04 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 02/20/2013 Sample: 

### BioReactor 1 Inf Hg Blk Collected: 

### 02/13/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

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

Lab ID: 

### 1308006-05 Report Matrix: 

### Influent Sample Type: 

### Sample Received: 

### 02/20/2013 Sample: 

### BioReactor 2 Inf Collected: 

### 02/13/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71666330 10 Cooler

none n/a 500mL Bottle FLPE Hg-T

Lab ID: 

### 1308006-06 Report Matrix: 

### Influent Sample Type: 

### Sample Received: 

### 02/20/2013 Sample: 

### BioReactor 2 Inf Collected: 

### 02/13/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

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

Lab ID: 

### 1308006-07 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 02/20/2013 Sample: 

### BioReactor 2 Inf Hg Blk Collected: 

### 02/13/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71666330 10 Cooler

none n/a 500mL 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: 

### 1308006-08 Report Matrix: 

### DIW Sample Type : 

### Field Blank Received: 

### 02/20/2013 Sample: 

### BioReactor 2 Inf Hg Blk Collected: 

### 02/13/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

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

Lab ID: 

### 1308006-09 Report Matrix: 

### Effluent Sample Type: 

### Sample Received: 

### 02/20/2013 Sample: 

### BioReactor 2 Eff Collected: 

### 02/13/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71666330 10 Cooler

none n/a 500mL Bottle FLPE Hg-T

Lab ID: 

### 1308006-10 Report Matrix: 

### Effluent Sample Type: 

### Sample Received: 

### 02/20/2013 Sample: 

### BioReactor 2 Eff Collected: 

### 02/13/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

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

Lab ID: 

### 1308006-11 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 02/20/2013 Sample: 

### BioReactor 2 Eff Hg Blk Collected: 

### 02/13/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71666330 10 Cooler

none n/a 500mL Bottle FLPE Hg-T

Lab ID: 

### 1308006-12 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 02/20/2013 Sample: 

### BioReactor 2 Eff Hg Blk Collected: 

### 02/13/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

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



# Shipping Containers

Cooler Tracking No: 

### 535305198868 via FedEx Temperature: 

### -0.3 °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 20, 2013 8:35

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

## February 27 , 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 #J13020306)

Dear Mr. Perkins, Attached is the report associated with four (4 ) aqueous samples submitted for selenium speciation on February 19, 2013

. The samples were received in a sealed cooler at-0. 1 ° C on February 20 , 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 # J13020306)
February 27 , 2013

1. Sample Reception Four (4 ) aqueous samples in125mL HDPE bottles (provided by Applied Speciation and Consulting) were submitted for selenium speciation analysis on February 19 , 2013 . The samples were received on February 20 , 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 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 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 February 22, 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 49.6 219 ND (<2.5) ND (<2.6) ND (<2.6) 0.0 (0) BioReactor 1 Inf 1.57 ND (<0.59) ND (<0.63) ND (<0.65) ND (<0.65) 0.0 (0) BioReactor 2 Inf 108 13.4 ND (<0.63) 3.39 ND (<0.65) 1.20 (1) BioReactor 2 Eff 9.30 216 ND (<0.63) 2.50 ND (<0.65) 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 27, 2013 LIMS #J13020306

### 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 0.003 0.73 2.9 Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.59 2.4 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.003 0.63 2.5 MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.003 0.65 2.6 SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.003 0.65 2.6 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 9.57 100.0 Se(VI) LCS 9.48 9.20 97.0 SeCN LCS 8.92 8.90 99.8 MeSe(IV) LCS 6.47 6.05 93.5 SeMe LCS 9.32 8.78 94.2 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Allen Wastewater - Nietering (January 2013 - Test Burn) Contact: Jay Perkins LIMS #J13020306 Date: February 27, 2013 Report Generated by: Russell Gerads

### Quality Control Summary - Matrix Duplicates Analyte (μg/L) Sample ID Rep 1 Rep 2 Mean RPD Se(IV) FGD Purge Eff 49.6 53.5 51.5 7.5 Se(VI) FGD Purge Eff 218.5 217.4 218.0 0.5 SeCN FGD Purge Eff ND (<2.5) ND (<2.5) NC NC MeSe(IV) FGD Purge Eff ND (<2.6) ND (<2.6) NC NC SeMe FGD Purge Eff ND (<2.6) ND (<2.6) 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) FGD Purge Eff 5560 5847 104.2 5560 5803 103.4 0.8 Se(VI) FGD Purge Eff 5045 5384 102.4 5045 5366 102.0 0.3 SeCN FGD Purge Eff 4575 4627 101.1 4575 4596 100.5 0.7 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Allen Wastewater - Nietering (January 2013 - Test Burn) Contact: Jay Perkins LIMS #J13020306 Date: February 27, 2013 Report Generated by: Russell Gerads