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: J12020342

Lab Contact: Jason C Perkins

Date: 3/7/2012

Customer Address: 3195 Pine Hall Rd

Customer Name(s): Bill Kennedy, Melonie Martin, Wayne Chapman, Tom Johnson

Mailcode: Belews Steam Station

Belews Creek, NC 28012

Phone: 980-875-5348

Report Authorized By:

(Signature)

Program Comments:

Please contact the Program Manager (Jason C Perkins) with any questions regarding this report.

Data Flags & Calculations:

Any analytical tests or individual analytes within a test flagged with a Qualifier indicate a deviation from the method quality 

system or quality control requirement. The qualifier description is found at the end of the Certificate of Analysis (sample results) 

under the qualifiers heading. All results are reported on a dry weight basis unless otherwise noted.

Data Package:

This data package includes analytical results that are applicable only to the samples described in this narrative. An estimation of 

the uncertainty of measurement for the results in the report is available upon request. This report shall not be reproduced, except 

in full, without the written consent of the Analytical Laboratory. Please contact the Analytical laboratory with any questions. The 

order of individual sections within this report is as follows:

Job Summary Report, Sample Identification, Technical Validation of Data Package, Analytical Laboratory Certificate of Analysis, 

Analytical Laboratory QC Reports, Sub-contracted Laboratory Results, Customer Specific Data Sheets, Reports & 

Documentation, Customer Database Entries, Test Case Narratives, Chain of Custody (COC)

Certification:

The Analytical Laboratory holds the following State Certifications : North Carolina (DENR) Certificate #248, South Carolina 

(DHEC) Laboratory ID # 99005. Contact the Analytical Laboratory for definitive information about the certification status of 

specific methods. 

Page 1 of 41
Sample ID's & Descriptions:

Sample ID Plant/Station

Collection 

Date and Time Collected By Sample Description

2012004150 BELEWS 19-Feb-12 11:00 AM P. GASSETT FGD Purge Eff 

2012004151 BELEWS 19-Feb-12 11:00 AM P. GASSETT BIOREACTOR 1 INF. 

2012004152 BELEWS 19-Feb-12 11:00 AM P. GASSETT BIOREACTOR 1 INF. BLANK 

2012004153 BELEWS 19-Feb-12 11:00 AM P. GASSETT BIOREACTOR 2 EFF. 

2012004154 BELEWS 19-Feb-12 11:00 AM P. GASSETT BIOREACTOR 2 EFF. BLANK 

2012004155 BELEWS 19-Feb-12 11:00 AM P. GASSETT FILTER BLANK 

2012004156 BELEWS 19-Feb-12 11:00 AM P. GASSETT Trip Blank 

7 Total Samples

Page 2 of 41
COC and .pdf report are in agreement with sample totals 

and analyses (compliance programs and procedures).

All Results are less than the laboratory reporting limits.

All laboratory QA/QC requirements are acceptable.

The Vendor Laboratories have been qualified by the 

Analytical Laboratory

Yes No

Technical Validation Review

Checklist:

Yes No

Yes No

Report Sections Included:

Job Summary Report Sub-contracted Laboratory Results

Sample Identification Customer Specific Data Sheets, Reports, & Documentation

Technical Validation of Data Package Customer Database Entries

Analytical Laboratory Certificate of Analysis

Analytical Laboratory QC Report

Chain of Custody

Reviewed By: DataBase Administrator Date: 3/7/2012

Yes

Electronic Data Deliverable (EDD) Sent Separately

Page 3 of 41
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12020342

2012004150

Collection Date: 19-Feb-12 11:00 AM

Site: FGD Purge Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

Carbonate, Bicarbonate, and Hydroxide Alkalinity

Bicarbonate (HCO3) Complete 1 V_PRISM

Hydroxide (OH) Complete 1 V_PRISM

Carbonate (CO3) Complete 1 V_PRISM

NITRITE + NITRATE (COLORIMETRIC)

Nitrite + Nitrate (Colorimetric) 15 mg-N/L 0.25 25 EPA 353.2 21-Feb-12 14:15 BGN9034

INORGANIC IONS BY IC

Bromide 130 mg/L 5 50 EPA 300.0 24-Feb-12 15:46 JAHERMA

Chloride 8300 mg/L 100 1000 EPA 300.0 24-Feb-12 15:46 JAHERMA

Sulfate 1300 mg/L 100 1000 EPA 300.0 24-Feb-12 15:46 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 212 ug/L 5 100 EPA 245.1 24-Feb-12 09:38 AGIBBS

Mercury Dissolved (cold vapor) in Water (Filtered)

Mercury (Hg) < 2.5 ug/L 2.5 50 EPA 245.1 02-Mar-12 10:00 AGIBBS

DISSOLVED METALS BY ICP

Manganese (Mn) 7.74 mg/L 0.05 10 EPA 200.7 29-Feb-12 09:48 MHH7131

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 265 mg/L 0.5 10 EPA 200.7 22-Feb-12 12:34 DJSULL1

Calcium (Ca) 4590 mg/L 0.1 10 EPA 200.7 22-Feb-12 12:34 DJSULL1

Iron (Fe) 88.5 mg/L 0.1 10 EPA 200.7 22-Feb-12 12:34 DJSULL1

Lithium (Li) 0.112 mg/L 0.05 10 EPA 200.7 22-Feb-12 12:34 DJSULL1

Magnesium (Mg) 891 mg/L 0.05 10 EPA 200.7 22-Feb-12 12:34 DJSULL1

Manganese (Mn) 8.57 mg/L 0.05 10 EPA 200.7 22-Feb-12 12:34 DJSULL1

Potassium (K) 53.0 mg/L 1 10 EPA 200.7 22-Feb-12 12:34 DJSULL1

Sodium (Na) 50.4 mg/L 0.5 10 EPA 200.7 22-Feb-12 12:34 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 251 ug/L 10 10 EPA 200.8 22-Feb-12 14:45 MHH7131

Page 4 of 41
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12020342

2012004150

Collection Date: 19-Feb-12 11:00 AM

Site: FGD Purge Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 130 ug/L 10 10 EPA 200.8 23-Feb-12 12:18 KRICHAR

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 23-Feb-12 12:18 KRICHAR

Chromium (Cr) 168 ug/L 10 10 EPA 200.8 23-Feb-12 12:18 KRICHAR

Copper (Cu) 71.9 ug/L 10 10 EPA 200.8 23-Feb-12 12:18 KRICHAR

Nickel (Ni) 152 ug/L 10 10 EPA 200.8 23-Feb-12 12:18 KRICHAR

Selenium (Se) 3950 ug/L 10 10 EPA 200.8 23-Feb-12 12:18 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 23-Feb-12 12:18 KRICHAR

Zinc (Zn) 124 ug/L 10 10 EPA 200.8 23-Feb-12 12:18 KRICHAR

Speciation of an Element

Vendor Parameter Complete 1 V_AS&C

TOTAL DISSOLVED SOLIDS

TDS 22000 mg/L 200 1 SM2540C 21-Feb-12 15:13 TJA7067

TOTAL SUSPENDED SOLIDS

TSS 3800 mg/L 250 1 SM2540D

2012004151

Collection Date: 19-Feb-12 11:00 AM

Site: BIOREACTOR 1 INF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

Carbonate, Bicarbonate, and Hydroxide Alkalinity

Hydroxide (OH) Complete 1 V_PRISM

Carbonate (CO3) Complete 1 V_PRISM

Bicarbonate (HCO3) Complete 1 V_PRISM

NITRITE + NITRATE (COLORIMETRIC)

Nitrite + Nitrate (Colorimetric) 14 mg-N/L 0.25 25 EPA 353.2 21-Feb-12 14:18 BGN9034

INORGANIC IONS BY IC

Bromide 110 mg/L 5 50 EPA 300.0 24-Feb-12 20:15 JAHERMA

Chloride 7400 mg/L 100 1000 EPA 300.0 24-Feb-12 20:15 JAHERMA

Sulfate 1500 mg/L 100 1000 EPA 300.0 24-Feb-12 20:15 JAHERMA

MERCURY 1631

Vendor Parameter Complete 1 V_BRAND

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) < 2.5 ug/L 2.5 50 EPA 245.1 24-Feb-12 09:41 AGIBBS

Page 5 of 41
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12020342

2012004151

Collection Date: 19-Feb-12 11:00 AM

Site: BIOREACTOR 1 INF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

Mercury Dissolved (cold vapor) in Water (Filtered)

Mercury (Hg) < 2.5 ug/L 2.5 50 EPA 245.1 02-Mar-12 10:02 AGIBBS

DISSOLVED METALS BY ICP

Manganese (Mn) 5.60 mg/L 0.05 10 EPA 200.7 29-Feb-12 09:52 MHH7131

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 229 mg/L 0.5 10 EPA 200.7 22-Feb-12 13:15 DJSULL1

Calcium (Ca) 3400 mg/L 0.1 10 EPA 200.7 22-Feb-12 13:15 DJSULL1

Iron (Fe) < 0.1 mg/L 0.1 10 EPA 200.7 22-Feb-12 13:15 DJSULL1

Lithium (Li) < 0.05 mg/L 0.05 10 EPA 200.7 22-Feb-12 13:15 DJSULL1

Magnesium (Mg) 737 mg/L 0.05 10 EPA 200.7 22-Feb-12 13:15 DJSULL1

Manganese (Mn) 5.93 mg/L 0.05 10 EPA 200.7 22-Feb-12 13:15 DJSULL1

Potassium (K) 22.1 mg/L 1 10 EPA 200.7 22-Feb-12 13:15 DJSULL1

Sodium (Na) 42.3 mg/L 0.5 10 EPA 200.7 22-Feb-12 13:15 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 109 ug/L 10 10 EPA 200.8 22-Feb-12 14:49 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 16.5 ug/L 10 10 EPA 200.8 23-Feb-12 12:21 KRICHAR

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 23-Feb-12 12:21 KRICHAR

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 23-Feb-12 12:21 KRICHAR

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 23-Feb-12 12:21 KRICHAR

Nickel (Ni) 56.1 ug/L 10 10 EPA 200.8 23-Feb-12 12:21 KRICHAR

Selenium (Se) 106 ug/L 10 10 EPA 200.8 23-Feb-12 12:21 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 23-Feb-12 12:21 KRICHAR

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 23-Feb-12 12:21 KRICHAR

Speciation of an Element

Vendor Parameter Complete 1 V_AS&C

2012004152

Collection Date: 19-Feb-12 11:00 AM

Site: BIOREACTOR 1 INF. BLANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

MERCURY 1631

Vendor Parameter Complete 1 V_BRAND

Page 6 of 41
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12020342

2012004153

Collection Date: 19-Feb-12 11:00 AM

Site: BIOREACTOR 2 EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

Carbonate, Bicarbonate, and Hydroxide Alkalinity

Hydroxide (OH) Complete 1 V_PRISM

Carbonate (CO3) Complete 1 V_PRISM

Bicarbonate (HCO3) Complete 1 V_PRISM

NITRITE + NITRATE (COLORIMETRIC)

Nitrite + Nitrate (Colorimetric) 0.013 mg-N/L 0.01 1 EPA 353.2 21-Feb-12 14:19 BGN9034

INORGANIC IONS BY IC

Bromide 120 mg/L 5 50 EPA 300.0 24-Feb-12 20:31 JAHERMA

Chloride 7600 mg/L 100 1000 EPA 300.0 24-Feb-12 20:31 JAHERMA

Sulfate 1600 mg/L 100 1000 EPA 300.0 24-Feb-12 20:31 JAHERMA

MERCURY 1631

Vendor Parameter Complete 1 V_BRAND

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) < 1 ug/L 1 20 EPA 245.1 24-Feb-12 09:43 AGIBBS

DISSOLVED METALS BY ICP

Manganese (Mn) 5.37 mg/L 0.05 10 EPA 200.7 29-Feb-12 09:56 MHH7131

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 232 mg/L 0.5 10 EPA 200.7 22-Feb-12 12:42 DJSULL1

Calcium (Ca) 3470 mg/L 0.1 10 EPA 200.7 22-Feb-12 12:42 DJSULL1

Iron (Fe) < 0.1 mg/L 0.1 10 EPA 200.7 22-Feb-12 12:42 DJSULL1

Lithium (Li) < 0.05 mg/L 0.05 10 EPA 200.7 22-Feb-12 12:42 DJSULL1

Magnesium (Mg) 769 mg/L 0.05 10 EPA 200.7 22-Feb-12 12:42 DJSULL1

Manganese (Mn) 5.80 mg/L 0.05 10 EPA 200.7 22-Feb-12 12:42 DJSULL1

Potassium (K) 26.9 mg/L 1 10 EPA 200.7 22-Feb-12 12:42 DJSULL1

Sodium (Na) 42.9 mg/L 0.5 10 EPA 200.7 22-Feb-12 12:42 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 19.3 ug/L 5 5 EPA 200.8 23-Feb-12 12:24 KRICHAR

Cadmium (Cd) < 5 ug/L 5 5 EPA 200.8 23-Feb-12 12:24 KRICHAR

Chromium (Cr) < 5 ug/L 5 5 EPA 200.8 23-Feb-12 12:24 KRICHAR

Copper (Cu) < 5 ug/L 5 5 EPA 200.8 23-Feb-12 12:24 KRICHAR

Nickel (Ni) 7.38 ug/L 5 5 EPA 200.8 23-Feb-12 12:24 KRICHAR

Selenium (Se) < 5 ug/L 5 5 EPA 200.8 23-Feb-12 12:24 KRICHAR

Silver (Ag) < 5 ug/L 5 5 EPA 200.8 23-Feb-12 12:24 KRICHAR

Zinc (Zn) < 5 ug/L 5 5 EPA 200.8 23-Feb-12 12:24 KRICHAR

Speciation of an Element

Vendor Parameter Complete 1 V_AS&C

Page 7 of 41
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12020342

2012004154

Collection Date: 19-Feb-12 11:00 AM

Site: BIOREACTOR 2 EFF. BLANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

MERCURY 1631

Vendor Parameter Complete 1 V_BRAND

2012004155

Collection Date: 19-Feb-12 11:00 AM

Site: FILTER BLANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

Mercury Dissolved (cold vapor) in Water (Filtered)

Mercury (Hg) < 0.05 ug/L 0.05 1 EPA 245.1 02-Mar-12 10:04 AGIBBS

DISSOLVED METALS BY ICP

Manganese (Mn) < 0.005 mg/L 0.005 1 EPA 200.7 29-Feb-12 09:23 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) < 1 ug/L 1 1 EPA 200.8 22-Feb-12 13:05 MHH7131

2012004156

Collection Date: 19-Feb-12 11:00 AM

Site: Trip Blank 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

TOTAL RECOVERABLE METALS BY ICP

Boron (B) < 0.05 mg/L 0.05 1 EPA 200.7 22-Feb-12 11:55 DJSULL1

Calcium (Ca) 0.012 mg/L 0.01 1 EPA 200.7 22-Feb-12 11:55 DJSULL1

Iron (Fe) < 0.01 mg/L 0.01 1 EPA 200.7 22-Feb-12 11:55 DJSULL1

Lithium (Li) < 0.005 mg/L 0.005 1 EPA 200.7 22-Feb-12 11:55 DJSULL1

Magnesium (Mg) < 0.005 mg/L 0.005 1 EPA 200.7 22-Feb-12 11:55 DJSULL1

Manganese (Mn) < 0.005 mg/L 0.005 1 EPA 200.7 22-Feb-12 11:55 DJSULL1

Potassium (K) < 0.1 mg/L 0.1 1 EPA 200.7 22-Feb-12 11:55 DJSULL1

Sodium (Na) < 0.05 mg/L 0.05 1 EPA 200.7 22-Feb-12 11:55 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 1 ug/L 1 1 EPA 200.8 23-Feb-12 11:38 KRICHAR

Cadmium (Cd) < 1 ug/L 1 1 EPA 200.8 23-Feb-12 11:38 KRICHAR

Chromium (Cr) < 1 ug/L 1 1 EPA 200.8 23-Feb-12 11:38 KRICHAR

Copper (Cu) < 1 ug/L 1 1 EPA 200.8 23-Feb-12 11:38 KRICHAR

Nickel (Ni) < 1 ug/L 1 1 EPA 200.8 23-Feb-12 11:38 KRICHAR

Selenium (Se) < 1 ug/L 1 1 EPA 200.8 23-Feb-12 11:38 KRICHAR

Silver (Ag) < 1 ug/L 1 1 EPA 200.8 23-Feb-12 11:38 KRICHAR

Zinc (Zn) < 1 ug/L 1 1 EPA 200.8 23-Feb-12 11:38 KRICHAR

Page 8 of 41
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12020342

2012004156

Collection Date: 19-Feb-12 11:00 AM

Site: Trip Blank 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

Speciation of an Element

Vendor Parameter Complete 1 V_AS&C

Page 9 of 41
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

02/27/2012

Duke Energy Corporation (04)

Jay Perkins

13339 Hagers Ferry Road

Huntersville, NC 28078

Project: HAPS/MACT Testing Belews Creek

Project No.: J12020342

Lab Submittal Date: 02/21/2012

Prism Work Order: 2020469

VA Certification No. 1287

Please call if you have any questions relating to this analytical report.

Respectfully,

PRISM LABORATORIES, INC.

VP Laboratory Services Reviewed By

Data Qualifiers Key Reference:

HT Sample received and analyzed outside of the hold time.

MDL Method Detection Limit

BRL Below Reporting Limit

RPD Relative Percent Difference

*

Results reported to the reporting limit. All other results are reported to the MDL with values between MDL and 

reporting limit indicated with a J.

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

449 Springbrook Road - P.O. Box 240543 - Charlotte, NC 28224-0543

Phone: 704/529-6364 - Toll Free Number: 1-800/529-6364 - Fax: 704/525-0409 Page 1 of 8

Page 10 of 41
Sample Receipt Summary

02/27/2012

Prism Work Order: 2020469

Client Sample ID Lab Sample ID Matrix Date Sampled Date Received

2012004150/FGD Purge Eff 2020469-01 Water 02/19/12 02/21/12

2012004151/BioReactor 1 Inf 2020469-02 Water 02/19/12 02/21/12

2012004153/BioReactor 2 Eff 2020469-03 Water 02/19/12 02/21/12

Samples received in good condition at 2.5 degrees C unless otherwise noted.

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

449 Springbrook Road - P.O. Box 240543 - Charlotte, NC 28224-0543

Phone: 704/529-6364 - Toll Free Number: 1-800/529-6364 - Fax: 704/525-0409 Page 2 of 8

Page 11 of 41
Laboratory Report

02/27/2012

Parameter Result Batch

ID

Report

Limit

Analysis

Date/Time

Dilution Method

Factor

Units MDL Analyst

13339 Hagers Ferry Road Project No.: 

Project: HAPS/MACT Testing Belews 

Creek

Duke Energy Corporation (04)

Huntersville, NC 28078

Attn: Jay Perkins

Sample Matrix: Water

Client Sample ID: 

Prism Sample ID: 2020469-01

Prism Work Order: 2020469

Time Collected: 02/19/12 11:00

Time Submitted: 02/21/12 15:05

2012004150/FGD Purge Eff

J12020342

General Chemistry Parameters

pH 6.9 HT pH Units 1 *SM4500-H B 2/22/12 14:00 JAB P2B0426

Total Alkalinity 60 mg/L 5.0 0.66 1 *SM2320 B 2/24/12 11:00 JAB P2B0484

Carbonate Alkalinity BRL mg/L 5.0 0.66 1 *SM2320 B 2/24/12 11:00 JAB P2B0485

Bicarbonate Alkalinity 60 mg/L 5.0 0.66 1 *SM2320 B 2/24/12 11:00 JAB P2B0487

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

449 Springbrook Road - P.O. Box 240543 - Charlotte, NC 28224-0543

Phone: 704/529-6364 - Toll Free Number: 1-800/529-6364 - Fax: 704/525-0409 Page 3 of 8

Page 12 of 41
Laboratory Report

02/27/2012

Parameter Result Batch

ID

Report

Limit

Analysis

Date/Time

Dilution Method

Factor

Units MDL Analyst

13339 Hagers Ferry Road Project No.: 

Project: HAPS/MACT Testing Belews 

Creek

Duke Energy Corporation (04)

Huntersville, NC 28078

Attn: Jay Perkins

Sample Matrix: Water

Client Sample ID: 

Prism Sample ID: 2020469-02

Prism Work Order: 2020469

Time Collected: 02/19/12 11:00

Time Submitted: 02/21/12 15:05

2012004151/BioReactor 1 Inf

J12020342

General Chemistry Parameters

pH 7.0 HT pH Units 1 *SM4500-H B 2/22/12 14:00 JAB P2B0426

Total Alkalinity 47 mg/L 5.0 0.66 1 *SM2320 B 2/24/12 11:00 JAB P2B0484

Carbonate Alkalinity BRL mg/L 5.0 0.66 1 *SM2320 B 2/24/12 11:00 JAB P2B0485

Bicarbonate Alkalinity 47 mg/L 5.0 0.66 1 *SM2320 B 2/24/12 11:00 JAB P2B0487

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

449 Springbrook Road - P.O. Box 240543 - Charlotte, NC 28224-0543

Phone: 704/529-6364 - Toll Free Number: 1-800/529-6364 - Fax: 704/525-0409 Page 4 of 8

Page 13 of 41
Laboratory Report

02/27/2012

Parameter Result Batch

ID

Report

Limit

Analysis

Date/Time

Dilution Method

Factor

Units MDL Analyst

13339 Hagers Ferry Road Project No.: 

Project: HAPS/MACT Testing Belews 

Creek

Duke Energy Corporation (04)

Huntersville, NC 28078

Attn: Jay Perkins

Sample Matrix: Water

Client Sample ID: 

Prism Sample ID: 2020469-03

Prism Work Order: 2020469

Time Collected: 02/19/12 11:00

Time Submitted: 02/21/12 15:05

2012004153/BioReactor 2 Eff

J12020342

General Chemistry Parameters

pH 6.9 HT pH Units 1 *SM4500-H B 2/22/12 14:00 JAB P2B0426

Total Alkalinity 130 mg/L 5.0 0.66 1 *SM2320 B 2/24/12 11:00 JAB P2B0484

Carbonate Alkalinity BRL mg/L 5.0 0.66 1 *SM2320 B 2/24/12 11:00 JAB P2B0485

Bicarbonate Alkalinity 130 mg/L 5.0 0.66 1 *SM2320 B 2/24/12 11:00 JAB P2B0487

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 8

Page 14 of 41
2/27/12

Level II QC Report

13339 Hagers Ferry Road Project No: J12020342

Project: HAPS/MACT Testing Belews 

Creek

Duke Energy Corporation (04)

Huntersville, NC 28078

Attn: Jay Perkins

Prism Work Order: 2020469

Time Submitted: 2/21/2012 3:05:00PM

Result Limit

Reporting

Units Level

Spike

Result

Source

%REC

%REC

Limits RPD

RPD

 Analyte Limit Notes 

General Chemistry Parameters - Quality Control

Batch P2B0426 - NO PREP

LCS (P2B0426-BS1) Prepared & Analyzed: 02/22/12 

pH 6.85 pH Units 6.860 100 99-101

Batch P2B0484 - NO PREP

Blank (P2B0484-BLK1) Prepared & Analyzed: 02/24/12 

Total Alkalinity BRL 5.0 mg/L

LCS (P2B0484-BS1) Prepared & Analyzed: 02/24/12 

Total Alkalinity 260 5.0 mg/L 250.0 104 90-110

LCS Dup (P2B0484-BSD1) Prepared & Analyzed: 02/24/12 

Total Alkalinity 259 5.0 mg/L 250.0 103 90-110 0.4 200

Batch P2B0485 - NO PREP

Blank (P2B0485-BLK1) Prepared & Analyzed: 02/24/12 

Carbonate Alkalinity BRL 5.0 mg/L

LCS (P2B0485-BS1) Prepared & Analyzed: 02/24/12 

Carbonate Alkalinity 260 5.0 mg/L 90-110

LCS Dup (P2B0485-BSD1) Prepared & Analyzed: 02/24/12 

Carbonate Alkalinity 259 5.0 mg/L 90-110 0.4 200

Batch P2B0487 - NO PREP

Blank (P2B0487-BLK1) Prepared & Analyzed: 02/24/12 

Bicarbonate Alkalinity BRL 5.0 mg/L

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 8

Page 15 of 41
2/27/12

Level II QC Report

13339 Hagers Ferry Road Project No: J12020342

Project: HAPS/MACT Testing Belews 

Creek

Duke Energy Corporation (04)

Huntersville, NC 28078

Attn: Jay Perkins

Prism Work Order: 2020469

Time Submitted: 2/21/2012 3:05:00PM

Result Limit

Reporting

Units Level

Spike

Result

Source

%REC

%REC

Limits RPD

RPD

 Analyte Limit Notes 

General Chemistry Parameters - Quality Control

Batch P2B0487 - NO PREP

LCS (P2B0487-BS1) Prepared & Analyzed: 02/24/12 

Bicarbonate Alkalinity 260 5.0 mg/L 250.0 104 90-110

LCS Dup (P2B0487-BSD1) Prepared & Analyzed: 02/24/12 

Bicarbonate Alkalinity 259 5.0 mg/L 250.0 103 90-110 0.4 200

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 8

Page 16 of 41

 

3958 6th Ave NW • Seattle, WA 98107 • T: 206-632-6206 • F: 206-632-6017 • www.brooksrand.com • brl@brooksrand.com 

February 29, 2012 

Duke Energy 

ATTN: Jay Perkins 

Scientific Support-Laboratory

13339 Hagers Ferry Road 

Huntersville NC 28078 

jcperkins@duke-energy.com 

labcustomer@duke-energy.com 

RE: Project DUK-HV1201 Client Project: J12020342 

Dear Mr. Perkins, 

On February 22, 2012, Brooks Rand Labs (BRL) received two (2) wastewater samples and two 

(2) corresponding field blanks. Samples were logged-in for total mercury (Hg) analysis. All 

samples were received, prepared, analyzed, and stored according to BRL SOPs and EPA 

methodology. 

The results were blank-corrected as described in the calculations section of the applicable 

SOP(s) and may be evaluated using adjusted reporting limits to account for sample aliquot size. 

Please refer to the Sample Results page for sample-specific detection limits and other details. 

No qualification of the data was warranted, aside from concentration qualifiers, and all 

associated quality control sample results met the acceptance criteria. 

BRL, an accredited laboratory, certifies the reported results of all analyses for which BRL is 

NELAP accredited meet all NELAP requirements. For more details, see the Report Information

page of the report. Please feel free to contact me if you have any questions regarding this 

report. 

Sincerely, 

 

Tiffany Stilwater 

Project Manager 

tiffany@brooksrand.com 

Page 18 of 41
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Definition of Data Qualifiers

(Effective 9/23/09)

Laboratory Accreditation

BRL is accredited by the National Environmental Laboratory Accreditation Program (NELAP) through the State of Florida 

Department of Health, Bureau of Laboratories (E87982) and is certified to perform many environmental analyses. BRL is 

also certified by many other states to perform environmental analyses. For a current list of our accreditations /certifications, 

please visit our website at <http://www.brooksrand.com/default.asp?contentID=586>. Results reported relate only to the 

samples listed in the report.

Report Information

BLK

BRL

BS

CAL

CCV

CRM

D

DUP

ICV

MSD

ND

NR

PS

REC

RPD

RSD

SCV

SOP

method blank 

Brooks Rand Labs

laboratory fortified blank

calibration standard

continuing calibration verification

certified reference material

dissolved fraction

duplicate

initial calibration verification

matrix spike duplicate

non-detect

non-reportable

post preparation spike

percent recovery

relative percent difference

relative standard deviation

secondary calibration verification

standard operating procedure

MDL

MRL

MS

method detection limit

method reporting limit

matrix spike

SRM

T

COC

standard reference material

total recoverable fraction

chain of custody record 

Common Abbreviations

These qualifiers are based on those previously utilized by Brooks Rand, Ltd., those found in the EPA SOW ILM03.0, 

Exhibit B, Section III, pg. B-18, and the USEPA Laboratory Data Validation Functional Guidelines for Evaluating Inorganic 

Analyses; USEPA; July 2002. These supersede all previous qualifiers ever employed by BRL.

B Detected by the instrument, the result is > the MDL but ≤ the MRL. Result is reported and considered an estimate.

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.com

Page 19 of 41
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Sample Information

Sample Lab ID Report Matrix Type Sampled Received

BioReactor 1 Inf 1208014-01 Influent Sample 02/19/2012 02/22/2012

BioReactor 1 Inf Hg Blk 1208014-02 DIW Field Blank 02/19/2012 02/22/2012

BioReactor 2 Eff 1208014-03 Effluent Sample 02/19/2012 02/22/2012

BioReactor 2 Eff Hg Blk 1208014-04 DIW Field Blank 02/19/2012 02/22/2012

Batch Summary

Analyte Lab Matrix Method Prepared Analyzed Batch Sequence

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

Sample Results

Sample Analyte Report Matrix Fraction Result Qualifier MDL MRL Unit Batch Sequence

BioReactor 1 Inf

1208014-01 Hg Influent T 421 15.2 40.4 ng/L B120297 1200129

BioReactor 1 Inf Hg Blk

1208014-02 Hg DIW T 0.15 U 0.15 0.40 ng/L B120297 1200129

BioReactor 2 Eff

1208014-03 Hg Effluent T 12.6 0.57 1.53 ng/L B120297 1200129

BioReactor 2 Eff Hg Blk

1208014-04 Hg DIW T 0.15 U 0.15 0.40 ng/L B120297 1200129

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

Page 20 of 41
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Accuracy & Precision Summary

Batch: B120297

Analyte Native Spike Result Units REC & Limits RPD & Limits

Method: EPA 1631

Lab Matrix: Water

Sample

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

Hg 15.68 14.73 ng/L 94% 85-115

B120297-MS1 Matrix Spike (1208004-01)

Hg 758.5 3535 4800 ng/L 114% 71-125

B120297-MSD1 Matrix Spike Duplicate (1208004-01)

Hg 758.5 3535 4565 ng/L 108% 71-125 245%

B120297-MS2 Matrix Spike (1208004-03)

Hg 29.10 139.0 168.1 ng/L 100% 71-125

B120297-MSD2 Matrix Spike Duplicate (1208004-03)

Hg 29.10 140.2 177.0 ng/L 105% 71-125 245%

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

Page 21 of 41
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Method Blanks & Reporting Limits

Batch: B120297

Method: EPA 1631

Matrix: Water

Analyte: Hg

Sample Result Units

B120297-BLK1 0.11 ng/L

B120297-BLK2 0.04 ng/L

B120297-BLK3 0.04 ng/L

B120297-BLK4 0.04 ng/L

Average: 0.06 Standard Deviation: 0.04 MDL: 0.15

Limit: 0.50 Limit: 0.10 MRL: 0.40

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

Page 22 of 41
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Instrument Calibration

Sequence: 1200129

Instrument: THG-10 Method: EPA 1631

Date: 02/27/2012

Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg

Lab ID True Value Result Units REC & Limits

1200129-IBL1 4.20 pg of Hg

1200129-IBL2 6.75 pg of Hg

1200129-IBL3 4.72 pg of Hg

1200129-IBL4 5.95 pg of Hg

1200129-CAL1 25.00 24.83 pg of Hg 99%

1200129-CAL2 100.0 90.79 pg of Hg 91%

1200129-CAL3 500.0 481.7 pg of Hg 96%

1200129-CAL4 2500 2727 pg of Hg 109%

1200129-CAL5 10000 10670 pg of Hg 107%

1200129-ICV1 1568 1473 pg of Hg 94% 85-115

1200129-CCB1 4.56 pg of Hg

1200129-CCV1 500.0 512.9 pg of Hg 103% 77-123

1200129-CCV2 500.0 512.7 pg of Hg 103% 77-123

1200129-CCV3 500.0 444.8 pg of Hg 89% 77-123

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

Page 23 of 41
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Sample Containers

Lab ID: 1208014-01 Report Matrix: Influent

Sample: BioReactor 1 Inf Sample Type: Sample Received: 02/22/2012

Collected: 02/19/2012

Des Container Size Lot Preservation P-Lot pH Ship. Cont.

A 71470160

10

Bottle FLPE Hg-T 250mL none n/a Cooler

Lab ID: 1208014-02 Report Matrix: DIW

Sample: BioReactor 1 Inf Hg Blk Sample Type: Field Blank Received: 02/22/2012

Collected: 02/19/2012

Des Container Size Lot Preservation P-Lot pH Ship. Cont.

A 71470160

10

Bottle FLPE Hg-T 250mL none n/a Cooler

Lab ID: 1208014-03 Report Matrix: Effluent

Sample: BioReactor 2 Eff Sample Type: Sample Received: 02/22/2012

Collected: 02/19/2012

Des Container Size Lot Preservation P-Lot pH Ship. Cont.

A 71470160

10

Bottle FLPE Hg-T 250mL none n/a Cooler

Lab ID: 1208014-04 Report Matrix: DIW

Sample: BioReactor 2 Eff Hg Blk Sample Type: Field Blank Received: 02/22/2012

Collected: 02/19/2012

Des Container Size Lot Preservation P-Lot pH Ship. Cont.

A 71470160

10

Bottle FLPE Hg-T 250mL none n/a Cooler

Shipping Containers

Cooler

Tracking No: 4726 7966 8573 via FedEx

Temperature: 0.4 °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 22, 2012 9:00

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

Page 24 of 41
Page 25 of 41
 

March 6, 2012 

Jay Perkins 

Duke Energy Analytical Laboratory 

Mail Code MGO3A2 (Building 7405) 

13339 Hagers Ferry Rd. 

Huntersville, NC 28078 

(704) 875-5245 

Project: HAPS/MACT Testing Belews Creek (LIMS # J12020342) 

Dear Mr. Perkins, 

Attached is the report associated with one (1) aqueous sample submitted for permanganate and 

persulfate analyses on February 21, 2012. The samples were received in a sealed cooler at -

0.3°C on February 22, 2012. Permanganate and persulfate analyses were performed via 

spectrophotometry. Any issues associated with the analysis are addressed in the following 

report. 

If you have any questions, please feel free to contact me at your convenience. 

 Sincerely, 

 

 Russell Gerads 

 Vice President 

 Applied Speciation and Consulting, LLC 

 

Page 26 of 41
Applied Speciation and Consulting, LLC 

Report prepared for: 

Jay Perkins 

Duke Energy Analytical Laboratory 

Mail Code MGO3A2 (Building 7405) 

13339 Hagers Ferry Rd. 

Huntersville, NC 28078 

Project: HAPS/MACT Testing Belews Creek (LIMS # J12020342) 

March 6, 2012 

1. Sample Reception 

One (1) aqueous sample in two 125mL HDPE bottles and two 125mL borosilicate glass 

bottles (provided by Applied Speciation and Consulting) was submitted for permanganate 

and persulfate analyses on February 21, 2012. The sample was received on February 22, 

2012 in a sealed container at -0.3°C.

The sample was received in a laminar flow clean hood, void of trace metals contamination 

and ultra-violet radiation, and was designated a discrete sample identifier. All sample 

containers were placed in a secure refrigerator maintained at a temperature of 4oC until 

analysis could be performed. 

2. Sample Preparation 

All sample preparation is performed in laminar flow clean hoods known to be free from trace 

metals contamination. All applied water for dilutions and sample preservatives are 

monitored for contamination to account for any biases associated with the sample results. 

S2O8

-2 and MnO4-

 Analysis by Spectrophotometry Prior to analysis, an aliquot of each sample 

was filtered with a syringe filter (0.45μm). Permanganate standards of known concentrations 

were filtered using the identical filtration apparatus to confirm that filtration does not induce 

loss of the target analyte. 

Filtration is a requirement for samples containing suspended solids due to the light scattering 

properties of particulates. 

Page 27 of 41
3. Sample Analysis 

All sample analysis is preceded by a minimum of a four-point calibration curve spanning the 

entire concentration range of interest. Calibration curves are performed at the beginning of 

each analytical day. All calibration curves, associated with each species of interest, are 

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

instrument blank corrected to account for any operational biases associated with the 

analytical platform. 

Prior to sample analysis, all calibration curves are verified using second source standards 

which are identified as initial calibration verification standards (ICV). 

Ongoing instrument performance is identified by the analysis of continuing calibration 

verification standards (CCV) and continuing calibration blanks (CCB) at a minimal interval 

of every ten analytical runs. 

MnO4

-

 Analysis by Spectrophotometry Each sample for permanganate analysis was analyzed 

by spectrophotometry on February 29, 2012. An aliquot of each sample was transferred to a 

cuvette with a 1cm light path. The permanganate complex was quantified by measuring the 

light absorbance at a wavelength of 545nm. 

S2O8

-2

 Analysis by Spectrophotometry Each sample for persulfate analysis was analyzed by 

spectrophotometry on March 1, 2012. An aliquot of each sample was transferred to a 15mL 

polyethylene centrifuge tube. A starch iodide solution was added to each sample which 

induces conversion of iodide to I2(aq). The I2 complex then reacts with starch to form a blue 

complex which is measured at a wavelength of 525nm. 

4. Analytical Issues 

The permanganate and persulfate recoveries for the matrix spike and matrix spike duplicate 

were below the control limit of 75%. The target analytes are efficient oxidizing agents which 

are amenable to reaction with most compounds. The low recoveries confirm that the sample 

matrix does not support the existence of strong oxidizing agents such as permanganate or 

persulfate. Approximately 2 minutes passed between the time of amending the sample matrix 

with the spikes and measurements which suggests that the low sample concentrations are not 

attributed to the variable of sample holding times. 

If you have any questions or concerns regarding this report, please feel free to contact me. 

Sincerely, 

Russell Gerads 

Vice President 

Applied Speciation and Consulting, LLC 

Page 28 of 41
Sample Results

Sample ID MnO4

- S2O8

-2

FGD Purge Eff ND (<0.50) ND (<100)

All results reflect the applied dilution and are reported in mg/L

ND = Not detected at the applied dilution

Report Generated by: Russell Gerads

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: HAPS/MACT Testing Belews Creek

Contact: Jay Perkins

Date: March 6, 2012

LIMS #J12020342

Page 29 of 41
Quality Control Summary - Preparation Blank Summary

Analyte (mg/L) PBW1 eMDL

MnO4

-

0.00 0.50

S2O8

-2 12 100

eMDL = Estimated Method Detection Limit

Quality Control Summary - Certified Reference Materials

Analyte (mg/L) CRM True Value Result Recovery

MnO4

-

LCS 0.500 0.581 116.3

S2O8

-2 LCS 100 123 123.4

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: HAPS/MACT Testing Belews Creek

Contact: Jay Perkins

LIMS #J12020342

Date: March 6, 2012

Report Generated by: Russell Gerads

Page 30 of 41
Quality Control Summary - Matrix Duplicates

Analyte (mg/L) Sample ID Rep 1 Rep 2 Mean RPD

MnO4

-

Batch QC ND (<0.50) ND (<0.50) NC NC

S2O8

-2

Batch QC 129 116 122.2 10.5

ND = Not detected at the applied dilution

NC = Value was not calculated due to one or more concentrations below the eMDL

Quality Control Summary - Matrix Spike/ Matrix Spike Duplicate

Analyte (mg/L) Sample ID Spike Conc MS Result Recovery Spike Conc MSD Result Recovery RPD

MnO4

-

Batch QC 0.500 0.052 10.5* 0.500 0.052 10.5* 0.0

S2O8

-2

Batch QC 500 167 9.0* 500 137 3.0* 19.7

*Low recovery is attributed to matrix induced species conversion

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: HAPS/MACT Testing Belews Creek

Contact: Jay Perkins

LIMS #J12020342

Date: March 6, 2012

Report Generated by: Russell Gerads

Page 31 of 41
Page 32 of 41
 

February 28, 2012 

Jay Perkins 

Duke Energy Analytical Laboratory 

Mail Code MGO3A2 (Building 7405) 

13339 Hagers Ferry Rd. 

Huntersville, NC 28078 

(704) 875-5245 

Project: HAPS/MACT Testing Belews Creek (LIMS # J12020342) 

Dear Mr. Perkins, 

Attached is the report associated with four (4) aqueous samples submitted for selenium 

speciation analysis on February 21, 2012. The samples were received in a sealed cooler at -

0.3°C on February 22, 2012. Selenium speciation analysis was performed via ion 

chromatography inductively coupled plasma collision reaction cell mass spectrometry (IC-ICPCRC-MS). Any issues associated with the analysis are addressed in the following report. 

If you have any questions, please feel free to contact me at your convenience. 

 Sincerely, 

 

 Russell Gerads 

 Vice President 

 Applied Speciation and Consulting, LLC 

 

Page 33 of 41
Applied Speciation and Consulting, LLC 

Report prepared for: 

Jay Perkins 

Duke Energy Analytical Laboratory 

Mail Code MGO3A2 (Building 7405) 

13339 Hagers Ferry Rd. 

Huntersville, NC 28078 

Project: HAPS/MACT Testing Belews Creek (LIMS # J12020342) 

February 28, 2012 

1. Sample Reception 

Four (4) aqueous samples in 125mL HDPE bottles (provided by Applied Speciation and 

Consulting) were submitted for selenium speciation analysis on February 21, 2012. The 

samples were received on February 22, 2012 in a sealed container at -0.3°C.

The samples were received in a laminar flow clean hood, void of trace metals contamination 

and ultra-violet radiation, and was designated a discrete sample identifier. An aliquot of each 

sample was filtered (0.45μm) and each filtrate was stored in a secure, monitored cryofreezer 

(maintained at a temperature of -80oC) until selenium speciation analysis could be performed 

via ion chromatography inductively coupled plasma collision reaction cell mass spectrometry 

(IC-ICP-CRC-MS). 

2. Sample Preparation 

All sample preparation is performed in laminar flow clean hoods known to be free from trace 

metals contamination. All applied water for dilutions and sample preservatives are 

monitored for contamination to account for any biases associated with the sample results. 

Selenium Speciation Analysis by IC-ICP-CRC-MS Prior to analysis, an aliquot of each 

sample was filtered with a syringe filter (0.45μm) and injected directly into a sealed 

autosampler vial. No further sample preparation was performed as any chemical alteration of 

a sample may shift the equilibrium of the system, resulting in changes in speciation ratios. 

3. Sample Analysis 

All sample analysis is preceded by a minimum of a five-point calibration curve spanning the 

entire concentration range of interest. Calibration curves are performed at the beginning of 

each analytical day. All calibration curves, associated with each species of interest, are 

Page 34 of 41
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 standards 

which are identified as initial calibration verification standards (ICV). 

Ongoing instrument performance is identified by the analysis of continuing calibration 

verification standards (CCV) and continuing calibration blanks (CCB) at a minimal interval 

of every ten analytical runs. 

Selenium Speciation Analysis by IC-ICP-CRC-MS Each sample for selenium speciation 

analysis was analyzed by ion chromatography inductively coupled plasma collision reaction 

cell mass spectrometry (IC-ICP-CRC-MS) on February 23, 2012. An aliquot of each sample 

is injected onto an anion exchange column and mobilized by a basic (pH > 7) gradient. The 

eluting selenium species are then introduced into a radio frequency (RF) plasma where 

energy-transfer processes cause desolvation, atomization, and ionization. The ions are 

extracted from the plasma through a differentially-pumped vacuum interface and travel 

through a pressurized chamber (CRC) containing hydrogen gas which preferentially reacts 

with interfering ions of the same target mass to charge ratios (m/z). A solid-state detector 

detects ions transmitted through the mass analyzer and the resulting current is processed by a 

data handling system. 

Retention times for each eluting species are compared to known standards for species 

identification. 

4. Analytical Issues 

The overall analyses went well and no significant analytical issues were encountered. All 

quality control parameters associated with this sample were within acceptance limits.

The estimated method detection limits (eMDLs) for selenite, selenate, and selenocyanate are 

generated from replicate analyses of the lowest standard in the calibration curve. Not all 

selenium species are present in preparation blanks; therefore, eMDL calculations based on 

preparation blanks are artificially biased low. 

The eMDL for methylseleninic acid and selenomethionine is calculated from the average 

eMDL of selenite, selenate, and selenocyanate. The calibration does not contain 

methylseleninic acid or selenomethionine due to impurities in these standards which would 

bias the results for other selenium species. 

Page 35 of 41
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 

Page 36 of 41
Sample Results

Sample ID Se(IV) Se(VI) SeCN MeSe(IV) SeMe

Unknown Se 

Species (n)

FGd Purge Eff 187 74.3 ND (<1.6) ND (<9.4) ND (<9.4) 0 (0)

BioReactor 1 Inf 25.6 65.5 ND (<0.39) 5.2 ND (<2.4) 0 (0)

BioReactor 2 Eff ND (<2.0) ND (<4.7) ND (<0.39) ND (<2.4) ND (<2.4) 0 (0)

Metals Trip Blk ND (<0.079) ND (<0.19) ND (<0.016) ND (<0.094) ND (<0.094) 0 (0)

All results reflect the applied dilution and are reported in μg/L

ND = Not detected at the applied dilution

SeCN = Selenocyanate

MeSe(IV) = Methylseleninic acid

SeMe = Selenomethionine

Unknown Se Species = Total concentration of all unknown Se species observed by IC-ICP-MS

n = number of unknown Se species observed

Report Generated by: Russell Gerads

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: HAPS/MACT Testing Belews Creek

Contact: Jay Perkins

Date: February 28, 2012

LIMS #J12020342

Page 37 of 41
Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 10x eMDL 250x eMDL 1000x

Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.079 2.0 7.9

Se(VI) 0.019 0.000 0.000 0.000 0.005 0.009 0.019 0.19 4.7 19

SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.016 0.39 1.6

MeSe(IV) 0.000 0.000 0.095 0.000 0.024 0.048 0.009 0.094 2.4 9.4

SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.009 0.094 2.4 9.4

eMDL = Estimated Method Detection Limit

*Please see narrative regarding eMDL calculations

Quality Control Summary - Certified Reference Materials

Analyte (μg/L) CRM True Value Result Recovery

Se(IV) LCS 9.57 9.38 98.0

Se(VI) LCS 9.48 9.09 95.9

SeCN LCS 8.92 8.54 95.7

MeSe(IV) LCS 6.47 5.79 89.4

SeMe LCS 9.32 8.48 91.0

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: HAPS/MACT Testing Belews Creek

Contact: Jay Perkins

LIMS #J12020342

Date: February 28, 2012

Report Generated by: Russell Gerads

Page 38 of 41
Quality Control Summary - Matrix Duplicates

Analyte (μg/L) Sample ID Rep 1 Rep 2 Mean RPD

Se(IV) Batch QC ND (<2.0) ND (<2.0) NC NC

Se(VI) Batch QC ND (<4.7) ND (<4.7) NC NC

SeCN Batch QC ND (<0.39) ND (<0.39) NC NC

MeSe(IV) Batch QC ND (<2.4) ND (<2.4) NC NC

SeMe Batch QC ND (<2.4) ND (<2.4) NC NC

ND = Not detected at the applied dilution

NC = Value was not calculated due to one or more concentrations below the eMDL

Quality Control Summary - Matrix Spike/ Matrix Spike Duplicate

Analyte (μg/L) Sample ID Spike Conc MS Result Recovery Spike Conc MSD Result Recovery RPD

Se(IV) Batch QC 1390 1592 114.6 1390 1594 114.7 0.1

Se(VI) Batch QC 1261 1279 101.4 1261 1284 101.8 0.4

SeCN Batch QC 1144 812.1 71.0* 1144 821.9 71.9* 1.2

*Low recovery is attributed to matrix induced species conversion

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: HAPS/MACT Testing Belews Creek

Contact: Jay Perkins

LIMS #J12020342

Date: February 28, 2012

Report Generated by: Russell Gerads

Page 39 of 41
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