### 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: J13020088 Project Name: Wastewater Nietering

L ab Contact: Jason C Perkins 

### Date: 2/21/2013 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 2013002904 ALLEN 04-Feb-13 8:00 AM BILL HASKINS FGD Purge Eff 2013002905 ALLEN 04-Feb-13 8:05 AM BILL HASKINS EQ Tank Eff 2013002906 ALLEN 04-Feb-13 8:03 AM BILL HASKINS BioReactor 1 Inf 2013002907 ALLEN 04-Feb-13 7:50 AM BILL HASKINS BioReactor 1 Inf BLANK 2013002908 ALLEN 04-Feb-13 8:11 AM BILL HASKINS BioReactor 2 Inf 2013002909 ALLEN 04-Feb-13 7:50 AM BILL HASKINS BioReactor 2 Inf BLANK 2013002910 ALLEN 04-Feb-13 8:08 AM BILL HASKINS BioReactor 2 Eff 2013002911 ALLEN 04-Feb-13 7:50 AM BILL HASKINS BioReactor 2 Eff BLANK 2013002912 ALLEN 04-Feb-13 8:55 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: 

### 2/21/2013 Electronic Data Deliverable (EDD) Sent Separately

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



## Order # J13020088

2013002904 Collection Date: 04-Feb-13 8:00 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 46 mg/L EPA 300.0 02/15/2013 15:56 JAHERMA 10 100 Chloride 1800 mg/L EPA 300.0 02/15/2013 15:56 JAHERMA 100 1000 Sulfate 1900 mg/L EPA 300.0 02/15/2013 15:56 JAHERMA 100 1000 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 34.4 ug/L EPA 245.1 02/07/2013 14:29 AGIBBS 2.5 50 DISSOLVED METALS BY ICP Manganese (Mn) 0.700 mg/L EPA 200.7 02/05/2013 16:07 MHH7131 0.05 10 TOTAL RECOVERABLE METALS BY ICP Boron (B) 206 mg/L EPA 200.7 02/07/2013 11:00 DJSULL1 0.5 10 Calcium (Ca) 1790 mg/L EPA 200.7 02/07/2013 11:00 DJSULL1 0.1 10 Iron (Fe) 90.5 mg/L EPA 200.7 02/07/2013 11:00 DJSULL1 0.1 10 Magnesium (Mg) 709 mg/L EPA 200.7 02/07/2013 11:00 DJSULL1 0.05 10 Manganese (Mn) 4.00 mg/L EPA 200.7 02/07/2013 11:00 DJSULL1 0.05 10 DISSOLVED METALS BY ICP-MS Selenium (Se) 291 ug/L EPA 200.8 02/07/2013 13:18 KRICHAR 10 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 157 ug/L EPA 200.8 02/07/2013 11:36 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 02/07/2013 11:36 KRICHAR 10 10 Chromium (Cr) 165 ug/L EPA 200.8 02/07/2013 11:36 KRICHAR 10 10 Copper (Cu) 130 ug/L EPA 200.8 02/07/2013 11:36 KRICHAR 10 10 Nickel (Ni) 219 ug/L EPA 200.8 02/07/2013 11:36 KRICHAR 10 10 Selenium (Se) 652 ug/L EPA 200.8 02/07/2013 11:36 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 02/07/2013 11:36 KRICHAR 10 10 Zinc (Zn) 308 ug/L EPA 200.8 02/07/2013 11:36 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 9600 mg/L SM2540C 02/12/2013 16:17 SWILLI3 200 1 TOTAL SUSPENDED SOLIDS TSS 2200 mg/L SM2540D 02/07/2013 12:30 TJA7067 250 1

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



## Order # J13020088

2013002905 Collection Date: 04-Feb-13 8:05 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) 43.7 ug/L EPA 245.1 02/07/2013 14:31 AGIBBS 2.5 50 DISSOLVED METALS BY ICP Manganese (Mn) < 0.05 mg/L EPA 200.7 02/05/2013 16:11 MHH7131 0.05 10 TOTAL RECOVERABLE METALS BY ICP Boron (B) 242 mg/L EPA 200.7 02/07/2013 11:04 DJSULL1 0.5 10 Calcium (Ca) 1790 mg/L EPA 200.7 02/07/2013 11:04 DJSULL1 0.1 10 Iron (Fe) 90.9 mg/L EPA 200.7 02/07/2013 11:04 DJSULL1 0.1 10 Magnesium (Mg) 831 mg/L EPA 200.7 02/07/2013 11:04 DJSULL1 0.05 10 Manganese (Mn) 4.80 mg/L EPA 200.7 02/07/2013 11:04 DJSULL1 0.05 10 DISSOLVED METALS BY ICP-MS Selenium (Se) 250 ug/L EPA 200.8 02/07/2013 13:22 KRICHAR 10 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 165 ug/L EPA 200.8 02/07/2013 11:43 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 02/07/2013 11:43 KRICHAR 10 10 Chromium (Cr) 167 ug/L EPA 200.8 02/07/2013 11:43 KRICHAR 10 10 Copper (Cu) 139 ug/L EPA 200.8 02/07/2013 11:43 KRICHAR 10 10 Nickel (Ni) 206 ug/L EPA 200.8 02/07/2013 11:43 KRICHAR 10 10 Selenium (Se) 1180 ug/L EPA 200.8 02/07/2013 11:43 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 02/07/2013 11:43 KRICHAR 10 10 Zinc (Zn) 289 ug/L EPA 200.8 02/07/2013 11:43 KRICHAR 10 10


### 2013002906 Collection Date: 04-Feb-13 8:03 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 02/05/2013 16:15 MHH7131 0.05 10

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



## Order # J13020088

2013002906 Collection Date: 04-Feb-13 8:03 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) 263 mg/L EPA 200.7 02/07/2013 11:08 DJSULL1 0.5 10 Calcium (Ca) 1610 mg/L EPA 200.7 02/07/2013 11:08 DJSULL1 0.1 10 Iron (Fe) < 0.1 mg/L EPA 200.7 02/07/2013 11:08 DJSULL1 0.1 10 Magnesium (Mg) 816 mg/L EPA 200.7 02/07/2013 11:08 DJSULL1 0.05 10 Manganese (Mn) < 0.05 mg/L EPA 200.7 02/07/2013 11:08 DJSULL1 0.05 10 DISSOLVED METALS BY ICP-MS Selenium (Se) 283 ug/L EPA 200.8 02/07/2013 13:25 KRICHAR 10 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 02/07/2013 11:46 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 02/07/2013 11:46 KRICHAR 10 10 Chromium (Cr) 11.3 ug/L EPA 200.8 02/07/2013 11:46 KRICHAR 10 10 Copper (Cu) < 10 ug/L EPA 200.8 02/07/2013 11:46 KRICHAR 10 10 Nickel (Ni) < 10 ug/L EPA 200.8 02/07/2013 11:46 KRICHAR 10 10 Selenium (Se) 312 ug/L EPA 200.8 02/07/2013 11:46 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 02/07/2013 11:46 KRICHAR 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 02/07/2013 11:46 KRICHAR 10 10 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C


### 2013002907 Collection Date: 04-Feb-13 7:50 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


### 2013002908 Collection Date: 04-Feb-13 8:11 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 # J13020088

2013002908 Collection Date: 04-Feb-13 8:11 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 02/05/2013 16:19 MHH7131 0.05 10 TOTAL RECOVERABLE METALS BY ICP Boron (B) 245 mg/L EPA 200.7 02/07/2013 11:12 DJSULL1 0.5 10 Calcium (Ca) 1670 mg/L EPA 200.7 02/07/2013 11:12 DJSULL1 0.1 10 Iron (Fe) < 0.1 mg/L EPA 200.7 02/07/2013 11:12 DJSULL1 0.1 10 Magnesium (Mg) 798 mg/L EPA 200.7 02/07/2013 11:12 DJSULL1 0.05 10 Manganese (Mn) < 0.05 mg/L EPA 200.7 02/07/2013 11:12 DJSULL1 0.05 10 DISSOLVED METALS BY ICP-MS Selenium (Se) 290 ug/L EPA 200.8 02/07/2013 13:29 KRICHAR 10 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 02/07/2013 11:50 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 02/07/2013 11:50 KRICHAR 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 02/07/2013 11:50 KRICHAR 10 10 Copper (Cu) < 10 ug/L EPA 200.8 02/07/2013 11:50 KRICHAR 10 10 Nickel (Ni) < 10 ug/L EPA 200.8 02/07/2013 11:50 KRICHAR 10 10 Selenium (Se) 351 ug/L EPA 200.8 02/07/2013 11:50 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 02/07/2013 11:50 KRICHAR 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 02/07/2013 11:50 KRICHAR 10 10 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C


### 2013002909 Collection Date: 04-Feb-13 7:50 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 # J13020088

2013002910 Collection Date: 04-Feb-13 8:08 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 130 mg/L EPA 300.0 02/15/2013 16:15 JAHERMA 10 100 Chloride 3400 mg/L EPA 300.0 02/15/2013 16:15 JAHERMA 100 1000 Sulfate 2000 mg/L EPA 300.0 02/15/2013 16:15 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) < 0.05 mg/L EPA 200.7 02/05/2013 16:23 MHH7131 0.05 10 TOTAL RECOVERABLE METALS BY ICP Boron (B) 225 mg/L EPA 200.7 02/07/2013 11:16 DJSULL1 0.5 10 Calcium (Ca) 1680 mg/L EPA 200.7 02/07/2013 11:16 DJSULL1 0.1 10 Iron (Fe) 0.218 mg/L EPA 200.7 02/07/2013 11:16 DJSULL1 0.1 10 Magnesium (Mg) 721 mg/L EPA 200.7 02/07/2013 11:16 DJSULL1 0.05 10 Manganese (Mn) < 0.05 mg/L EPA 200.7 02/07/2013 11:16 DJSULL1 0.05 10 DISSOLVED METALS BY ICP-MS Selenium (Se) 11.3 ug/L EPA 200.8 02/07/2013 13:32 KRICHAR 5 5 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 5 ug/L EPA 200.8 02/07/2013 11:53 KRICHAR 5 5 Cadmium (Cd) < 5 ug/L EPA 200.8 02/07/2013 11:53 KRICHAR 5 5 Chromium (Cr) < 5 ug/L EPA 200.8 02/07/2013 11:53 KRICHAR 5 5 Copper (Cu) < 5 ug/L EPA 200.8 02/07/2013 11:53 KRICHAR 5 5 Nickel (Ni) < 5 ug/L EPA 200.8 02/07/2013 11:53 KRICHAR 5 5 Selenium (Se) 11.1 ug/L EPA 200.8 02/07/2013 11:53 KRICHAR 5 5 Silver (Ag) < 5 ug/L EPA 200.8 02/07/2013 11:53 KRICHAR 5 5 Zinc (Zn) < 5 ug/L EPA 200.8 02/07/2013 11:53 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 # J13020088

2013002911 Collection Date: 04-Feb-13 7:50 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


### 2013002912 Collection Date: 04-Feb-13 8:55 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 02/05/2013 15:24 MHH7131 0.005 1 DISSOLVED METALS BY ICP-MS Selenium (Se) 1.22 ug/L EPA 200.8 02/07/2013 12:58 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 02/13/2013

Duke Energy Corporation Jay Perkins 13339 Hagers Ferry Road Huntersville, NC 28078 Project: Allen WW - Nietering (January 2013-Test Burn) Project No.: J13020088 Lab Submittal Date: 02/05/2013 Prism Work Order: 3020072 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 02/13/2013 

### Prism Work Order: 3020072 Client Sample ID Matrix Lab Sample ID Date Sampled Date Received 

### 3020072-01 02/04/13 2013002904/FGD Purge Eff 02/05/13 Water 3020072-02 02/04/13 2013002906/BioReactor 1 Inf 02/05/13 Water 3020072-03 02/04/13 2013002908/BioReactor 2 Inf 02/05/13 Water 3020072-04 02/04/13 2013002910/BioReactor 2 Eff 02/05/13 Water Samples received in good condition at 1.4 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 02/13/2013

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: 3020072-01 Prism Work Order: 3020072 Time Collected: 02/04/13 08:00 Time Submitted: 02/05/13 16:45 2013002904/FGD Purge Eff


### J13020088

General Chemistry Parameters 6.9 *SM4500-H B P3B0117 1 2/6/13 14:40 JAB HT pH Units pH 140 *SM2320 B P3B0114 1 5.0 2/6/13 11:00 JAB mg/L 0.59 Total Alkalinity BRL *SM2320 B P3B0115 1 5.0 2/6/13 11:00 JAB mg/L 0.59 Carbonate Alkalinity 140 *SM2320 B P3B0116 1 5.0 2/6/13 11:00 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 02/13/2013

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: 3020072-02 Prism Work Order: 3020072 Time Collected: 02/04/13 08:03 Time Submitted: 02/05/13 16:45 2013002906/BioReactor 1 Inf


### J13020088

General Chemistry Parameters 7.1 *SM4500-H B P3B0117 1 2/6/13 14:40 JAB HT pH Units pH 58 *SM2320 B P3B0114 1 5.0 2/6/13 11:00 JAB mg/L 0.59 Total Alkalinity BRL *SM2320 B P3B0115 1 5.0 2/6/13 11:00 JAB mg/L 0.59 Carbonate Alkalinity 58 *SM2320 B P3B0116 1 5.0 2/6/13 11:00 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 02/13/2013

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: 3020072-03 Prism Work Order: 3020072 Time Collected: 02/04/13 08:11 Time Submitted: 02/05/13 16:45 2013002908/BioReactor 2 Inf


### J13020088

General Chemistry Parameters 7.5 *SM4500-H B P3B0117 1 2/6/13 14:40 JAB HT pH Units pH 300 *SM2320 B P3B0114 1 5.0 2/6/13 11:00 JAB mg/L 0.59 Total Alkalinity BRL *SM2320 B P3B0115 1 5.0 2/6/13 11:00 JAB mg/L 0.59 Carbonate Alkalinity 300 *SM2320 B P3B0116 1 5.0 2/6/13 11:00 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 02/13/2013

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: 3020072-04 Prism Work Order: 3020072 Time Collected: 02/04/13 08:08 Time Submitted: 02/05/13 16:45 2013002910/BioReactor 2 Eff


### J13020088

General Chemistry Parameters 7.0 *SM4500-H B P3B0117 1 2/6/13 14:40 JAB HT pH Units pH 150 *SM2320 B P3B0114 1 5.0 2/6/13 11:00 JAB mg/L 0.59 Total Alkalinity BRL *SM2320 B P3B0115 1 5.0 2/6/13 11:00 JAB mg/L 0.59 Carbonate Alkalinity 150 *SM2320 B P3B0116 1 5.0 2/6/13 11:00 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 92/13/13 

### Level II QC Report

13339 Hagers Ferry Road Project No: J13020088 Project: Allen WW - Nietering (January 2013-Test Burn) Duke Energy Corporation

Huntersville, NC 28078 Attn: Jay Perkins Prism Work Order: 3020072 Time Submitted: 2/5/2013 4:45:00PM

Result Limit

Reporting Units Level Spike Result

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

Batch P3B0114 - NO PREP Blank (P3B0114-BLK1) Prepared & Analyzed: 02/06/13 Total Alkalinity mg/L BRL 5.0 LCS (P3B0114-BS1) Prepared & Analyzed: 02/06/13 Total Alkalinity mg/L 251 5.0 250.0 90-110 100 LCS Dup (P3B0114-BSD1) Prepared & Analyzed: 02/06/13 Total Alkalinity mg/L 256 5.0 250.0 200 90-110 102 2 Batch P3B0115 - NO PREP Blank (P3B0115-BLK1) Prepared & Analyzed: 02/06/13 Carbonate Alkalinity mg/L BRL 5.0 Batch P3B0116 - NO PREP Blank (P3B0116-BLK1) Prepared & Analyzed: 02/06/13 Bicarbonate Alkalinity mg/L BRL 5.0 LCS (P3B0116-BS1) Prepared & Analyzed: 02/06/13 Bicarbonate Alkalinity mg/L 251 5.0 250.0 90-110 100 LCS Dup (P3B0116-BSD1) Prepared & Analyzed: 02/06/13 Bicarbonate Alkalinity mg/L 256 5.0 250.0 200 90-110 102 2 Batch P3B0117 - NO PREP LCS (P3B0117-BS1) Prepared & Analyzed: 02/06/13 pH pH Units 6.86 6.860 99-101 100

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 92/13/13 

### Level II QC Report

13339 Hagers Ferry Road Project No: J13020088 Project: Allen WW - Nietering (January 2013-Test Burn) Duke Energy Corporation

Huntersville, NC 28078 Attn: Jay Perkins Prism Work Order: 3020072 Time Submitted: 2/5/2013 4:45:00PM

Result Limit

Reporting Units Level Spike Result

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

Batch P3B0117 - NO PREP LCS (P3B0117-BS2) Prepared & Analyzed: 02/06/13 pH pH Units 6.88 6.860 99-101 100 Duplicate (P3B0117-DUP1) Prepared & Analyzed: 02/06/13 Source: 3020072-03 pH pH Units 7.45 7.46 10 0.1

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

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

### Page 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 20, 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 : J13020088 Dear Mr. Perkins, O n February 6, 2013 , Brooks Rand Labs ( BRL ) received three (3 ) wastewater sample and three (3 ) corresponding field blank s. 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 within the non

- regulatory holding time limit and results were not qualified. 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 results of continuing calibration blanks CCB7, CCB8, CCBC, and CCBD were greater than 10 pg of Hg. All bracketed samples were re

- analyzed for confirmation. The total Hg result for field blank samples BioReactor 1 Inf Hg Blk (1306015

- 03) and the dissolved Hg result for sample BioReactor 2 Inf Hg Blk ( 1306015
- 08 ) were slightly greater than the MDL; however, the concentrations were less than the method defined control limit of 0.5 ng/L and contamination was considered insignificant. Additionally, the total Hg result for sample BioReactor 2 Inf Hg Blk (13 06015
- 07) was a positive detect. The sample was re

- analyzed twice more and the results confirmed one another. The associated field sample result was 411 ng/L and the field blank concentration not significant comparatively. All data was reported without add itional qualification, aside from concentration qualifiers, and all associated quality control sample results met the acceptance criteria.

## BRL, an accredited laboratory, certifies the reported results of all analyses for which BRL is NELAP accredited meet all NELAP requirements. For more details , see the Report Information page of the report. Please feel free to contact me if you have any questions. 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: 

### DUK-HV1201

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Sample Information

Report Matrix Type Received Sampled Sample Lab ID 

### 1306015-01 BioReactor 1 Inf 02/04/2013 02/06/2013 Sample Influent 1306015-02 BioReactor 1 Inf 02/04/2013 02/06/2013 Sample Influent 1306015-03 BioReactor 1 Inf Hg Blk 02/04/2013 02/06/2013 Field Blank DIW 1306015-04 BioReactor 1 Inf Hg Blk 02/04/2013 02/06/2013 Field Blank DIW 1306015-05 BioReactor 2 Inf 02/04/2013 02/06/2013 Sample Influent 1306015-06 BioReactor 2 Inf 02/04/2013 02/06/2013 Sample Influent 1306015-07 BioReactor 2 Inf Hg Blk 02/04/2013 02/06/2013 Field Blank DIW 1306015-08 BioReactor 2 Inf Hg Blk 02/04/2013 02/06/2013 Field Blank DIW 1306015-09 BioReactor 2 Eff 02/04/2013 02/06/2013 Sample Effluent 1306015-10 BioReactor 2 Eff 02/04/2013 02/06/2013 Sample Effluent 1306015-11 BioReactor 2 Eff Hg Blk 02/04/2013 02/06/2013 Field Blank DIW 1306015-12 BioReactor 2 Eff Hg Blk 02/04/2013 02/06/2013 Field Blank DIW 

# Batch Summary

Analyte Prepared Analyzed Sequence Batch Lab Matrix Method 

### B130201 02/08/2013 02/11/2013 1300095 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 

### 10700 T 1300095 B130201 Influent 204 76.5 1306015-01 Hg ng/L 103 D 1300095 B130201 Influent 1.02 0.38 1306015-02 Hg ng/L
BioReactor 1 Inf Hg Blk 

### 0.22 T B 1300095 B130201 DIW 0.41 0.15 1306015-03 Hg ng/L 0.15 D U 1300095 B130201 DIW 0.40 0.15 1306015-04 Hg ng/L

BioReactor 2 Eff 

### 149 T 1300095 B130201 Ef fluent 0.40 0.15 1306015-09 Hg ng/L 19.3 D 1300095 B130201 Effluent 0.41 0.15 1306015-10 Hg ng/L
BioReactor 2 Eff Hg Blk 

### 0.16 T U 1300095 B130201 DIW 0.42 0.16 1306015-11 Hg ng/L 0.15 D U 1300095 B130201 DIW 0.39 0.15 1306015-12 Hg ng/L

BioReactor 2 Inf 

### 411 T 1300095 B130201 Influent 1.02 0.38 1306015-05 Hg ng/L 22.7 D 1300095 B130201 Influent 0.41 0.15 1306015-06 Hg ng/L
BioReactor 2 Inf Hg Blk 

### 4.55 T 1300095 B130201 DIW 0.42 0.16 1306015-07 Hg ng/L 0.22 D B 1300095 B130201 DIW 0.41 0.16 1306015-08 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: 

### B130201

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

### EPA

1631 Lab Matrix: 

### Water

Sample Certified Reference Material (1307035, NIST 1641d 1000x dilution) B130201-SRM1 

### 15.68 103% ng/L 85-115 Hg 16.08
Matrix Spike (1306007-01) B130201-MS4 

### 8.123 103% ng/L 71-125 Hg 8.99

0.65
Matrix Spike Duplicate (1306007-01) B130201-MSD4 

### 8.061 121% ng/L 71-125 2414% Hg 10.37

0.65
Matrix Spike (1306009-01) B130201-MS5 

### 8.324 113% ng/L 71-125 Hg 10.22

0.79
Matrix Spike Duplicate (1306009-01) B130201-MSD5 

### 8.212 114% ng/L 71-125 240.3% Hg 10.19

0.79
Matrix Spike (1306013-01) B130201-MS3 

### 30300 116% ng/L 71-125 Hg 41940

6788
Matrix Spike Duplicate (1306013-01) B130201-MSD3 

### 30300 117% ng/L 71-125 241% Hg 42360

6788

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: 

### B130201
Method: 

### EPA

1631 Matrix: 

### Water Analyte: 

### Hg Result Units Sample 

### B130201-BLK1 ng/L 0.31 B130201-BLK2 ng/L 0.32 B130201-BLK3 ng/L 0.27 B130201-BLK4 ng/L 0.31 MDL: 

### 0.16 Average: 

### 0.30 Standard Deviation: 

### 0.02 Limit: 

### 0.10 Limit: 

### 0.50 MRL: 

### 0.42

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: 

### 1300095 Method: 

### EPA 1631 Instrument: 

### THG-05 Date: 

### 02/11/2013 Total Mercury and Mercury Speciation by CVAFS

Analyte: 

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

### 1300095-IBL1 0.78 pg of Hg 1300095-IBL2 2.35 pg of Hg 1300095-IBL3 2.61 pg of Hg 1300095-IBL4 2.86 pg of Hg 1300095-CAL1 10.00 10.06 pg of Hg 101% 1300095-CAL2 25.00 24.27 pg of Hg 97% 1300095-CAL3 100.0 98.89 pg of Hg 99% 1300095-CAL4 500.0 499.0 pg of Hg 100% 1300095-CAL5 2500 2521 pg of Hg 101% 1300095-CAL6 10000 10300 pg of Hg 103% 1300095-ICV1 1568 1608 pg of Hg 103% 85-115 1300095-CCB1 7.23 pg of Hg 1300095-CCV1 500.0 515.4 pg of Hg 103% 77-123 1300095-CCB2 4.67 pg of Hg 1300095-CCB3 4.47 pg of Hg 1300095-CCB4 4.28 pg of Hg 1300095-CCV2 500.0 529.5 pg of Hg 106% 77-123 1300095-CCB5 4.02 pg of Hg 1300095-CCV3 500.0 532.5 pg of Hg 107% 77-123 1300095-CCB6 3.81 pg of Hg 1300095-CCV4 500.0 592.1 pg of Hg 118% 77-123 1300095-CCB7 38.4 pg of Hg 1300095-CCV5 500.0 562.1 pg of Hg 112% 77-123 1300095-CCB8 21.0 pg of Hg 1300095-CCV6 500.0 544.2 pg of Hg 109% 77-123 1300095-CCB9 9.78 pg of Hg 1300095-CCV7 500.0 525.3 pg of Hg 105% 77-123 1300095-CCBA 6.09 pg of Hg 1300095-CCV8 500.0 526.2 pg of Hg 105% 77-123 1300095-CCBB 5.08 pg of Hg 1300095-CCV9 500.0 530.5 pg of Hg 106% 77-123 1300095-CCBC 13.1 pg of Hg 1300095-CCVA 500.0 526.5 pg of Hg 105% 77-123 1300095-CCBD 15.9 pg of Hg 1300095-CCVB 500.0 523.1 pg of Hg 105% 77-123 1300095-CCBE 6.43 pg of Hg 1300095-CCVC 500.0 529.5 pg of Hg 106% 77-123 1300095-CCBF 6.87 pg of Hg 1300095-ICV2 1568 1662 pg of Hg 106% 85-115 1300095-CCVD 500.0 544.6 pg of Hg 109% 77-123

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

### DUK-HV1201

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Instrument Calibration

Sequence: 

### 1300095 Method: 

### EPA 1631 Instrument: 

### THG-05 Date: 

### 02/11/2013 Total Mercury and Mercury Speciation by CVAFS

Analyte: 

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

### 1300095-CCBG 5.21 pg of Hg 1300095-CCVE 500.0 569.9 pg of Hg 114% 77-123 1300095-CCBH 5.66 pg of Hg 1300095-CCVF 500.0 578.9 pg of Hg 116% 77-123 1300095-CCBI 5.45 pg of Hg 1300095-CCVG 500.0 590.1 pg of Hg 118% 77-123 1300095-CCBJ 7.04 pg of Hg 1300095-CCVH 500.0 574.2 pg of Hg 115% 77-123 1300095-CCBK 5.11 pg of Hg 1300095-CCVI 500.0 568.7 pg of Hg 114% 77-123 1300095-CCBL 3.90 pg of Hg 1300095-CCVJ 500.0 571.9 pg of Hg 114% 77-123 1300095-CCBM 4.30 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: 

### 1306015-01 Report Matrix: 

### Influent Sample Type : 

### Sample Received: 

### 02/06/2013 Sample: 

### BioReactor 1 Inf Collected: 

### 02/04/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71666330 10 Cooler

none n/a 500mL Bottle FLPE Hg-T

Lab ID: 

### 1306015-02 Report Matrix: 

### Influent Sample Type: 

### Sample Received: 

### 02/06/2013 Sample: 

### BioReactor 1 Inf Collected: 

### 02/04/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

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

Lab ID: 

### 1306015-03 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 02/06/2013 Sample: 

### BioReactor 1 Inf Hg Blk Collected: 

### 02/04/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71666330 10 Cooler

none n/a 500mL Bottle FLPE Hg-T

Lab ID: 

### 1306015-04 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 02/06/2013 Sample: 

### BioReactor 1 Inf Hg Blk Collected: 

### 02/04/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

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

Lab ID: 

### 1306015-05 Report Matrix: 

### Influent Sample Type: 

### Sample Received: 

### 02/06/2013 Sample: 

### BioReactor 2 Inf Collected: 

### 02/04/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71666330 10 Cooler

none n/a 500mL Bottle FLPE Hg-T

Lab ID: 

### 1306015-06 Report Matrix: 

### Influent Sample Type: 

### Sample Received: 

### 02/06/2013 Sample: 

### BioReactor 2 Inf Collected: 

### 02/04/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

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

Lab ID: 

### 1306015-07 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 02/06/2013 Sample: 

### BioReactor 2 Inf Hg Blk Collected: 

### 02/04/2013 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: 

### 1306015-08 Report Matrix: 

### DIW Sample Type : 

### Field Blank Received: 

### 02/06/2013 Sample: 

### BioReactor 2 Inf Hg Blk Collected: 

### 02/04/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

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

Lab ID: 

### 1306015-09 Report Matrix: 

### Effluent Sample Type: 

### Sample Received: 

### 02/06/2013 Sample: 

### BioReactor 2 Eff Collected: 

### 02/04/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71666330 10 Cooler

none n/a 500mL Bottle FLPE Hg-T

Lab ID: 

### 1306015-10 Report Matrix: 

### Effluent Sample Type: 

### Sample Received: 

### 02/06/2013 Sample: 

### BioReactor 2 Eff Collected: 

### 02/04/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

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

Lab ID: 

### 1306015-11 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 02/06/2013 Sample: 

### BioReactor 2 Eff Hg Blk Collected: 

### 02/04/2013 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71666330 10 Cooler

none n/a 500mL Bottle FLPE Hg-T

Lab ID: 

### 1306015-12 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 02/06/2013 Sample: 

### BioReactor 2 Eff Hg Blk Collected: 

### 02/04/2013 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: 

### 535305198239 via FedEx Temperature: 

### 1.2 °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 6, 2013 9:00

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

## February 12, 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 #J130208 8 )

Dear Mr. Perkins, Attached is the report associated with four (4 ) aqueous samples submitted for selenium speciation on February 5, 2013

. The samples were received in a sealed cooler at-0. 1 ° C on February 6 , 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 #J13020088 )
February 12, 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 5 , 2013 . The samples were received on February 6 , 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 corrected to account for any operational biases associated with the analytical platform. Prior to sample analysis, all calibration curves are verified using second source standard s which are identified as initial calibration verification standards (ICV). Ongoing instrument performance is identified by the analysis of continuing calibration verification standards (CCV) and continuing calibration blanks (CCB) at a minimum interval of every ten analytical runs. Selenium Speciation Analysis by IC-ICP-CRC-MS Eachsample for selenium speciation analysis w as analyzed by ion chromatography inductively coupled plasma collision reaction cell mass spectrometry (IC-ICP- CRC -MS) on February 11, 2013. Analiquot of each sample is injected onto an anion exchange column and mobilized by a basic (pH > 7) gradient. The eluting selenium species are then introduced into a radio frequency (RF) plasma where energy-transfer processes cause desolvation, atomization, and ionization. The ions are extracted from the plasma through a differentially-pumped vacuum interface and travel through a pressurized chamber ( CRC ) containing 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 24.3 270 ND (<1.8) ND (<1.5) ND (<1.5) 0 (0) BioReactor 1 Inf 30.7 315 ND (<0.45) 2.94 ND (<0.39) 0 (0) BioReactor 2 Inf 293 66.5 0.83 4.17 ND (<0.39) 1.91 (2) BioReactor 2 Eff 4.26 ND (<0.46) ND (<0.45) 0.72 ND (<0.39) 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 12, 2013 LIMS #J13020088

### 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 0.001 0.25 0.98 Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.46 1.9 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.45 1.8 MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.39 1.5 SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.39 1.5 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 9.87 103.1 Se(VI) LCS 9.48 9.57 100.9 SeCN LCS 8.92 9.13 102.4 MeSe(IV) LCS 6.47 6.49 100.3 SeMe LCS 9.32 9.12 97.8 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Allen Wastewater - Nietering (January 2013 - Test Burn) Contact: Jay Perkins LIMS #J13020088 Date: February 12, 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 20.36 21.41 20.89 5.0 Se(VI) Batch QC 344.5 322.9 333.7 6.5 SeCN Batch QC ND (<1.9) ND (<1.9) NC NC MeSe(IV) Batch QC ND (<1.5) ND (<1.5) NC NC SeMe Batch QC ND (<1.5) ND (<1.5) 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 5560 5770 103.4 5560 5724 102.6 0.8 Se(VI) Batch QC 5045 5447 101.4 5045 5462 101.6 0.3 SeCN Batch QC 4575 4605 100.7 4575 4592 100.4 0.3 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Allen Wastewater - Nietering (January 2013 - Test Burn) Contact: Jay Perkins LIMS #J13020088 Date: February 12, 2013 Report Generated by: Russell Gerads