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: J12120342

Project Name: Flex Fuel WW

Lab Contact: Jason C Perkins

Date: 1/17/2013

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. 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. 

Page 1 of 29
Sample ID's & Descriptions:

Sample ID Plant/Station

Collection 

Date and Time Collected By Sample Description

2012027306 BELEWS 21-Dec-12 7:30 AM L. TURNER FGD Purge Eff 

2012027307 BELEWS 21-Dec-12 7:35 AM L. TURNER EQ TANK 

2012027308 BELEWS 21-Dec-12 7:40 AM L. TURNER BIOREACTOR 1 INF 

2012027309 BELEWS 21-Dec-12 7:40 AM L. TURNER biOREACTOR 1 INF HG BLK 

2012027310 BELEWS 21-Dec-12 7:45 AM L. TURNER BIOREACTOR 2 INF. 

2012027311 BELEWS 21-Dec-12 7:45 AM L. TURNER BIOREACTOR 2 INF. HG BLANK 

2012027312 BELEWS 21-Dec-12 7:50 AM L. TURNER BIOREACTOR 2 EFF. 

2012027313 BELEWS 21-Dec-12 7:50 AM L. TURNER BIOREACTOR 2 EFF. HG BLANK 

2012027314 BELEWS 21-Dec-12 8:00 AM L. TURNER FILTER BLANK 

9 Total Samples

Page 2 of 29
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: 1/17/2013

Electronic Data Deliverable (EDD) Sent Separately

The following vendor labs are pending 2013 qualification: Applied Speciation

Brooks Rand Lab

Page 3 of 29
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12120342

2012027306

Collection Date: 21-Dec-12 7:30 AM

Site: FGD Purge Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

INORGANIC IONS BY IC

Bromide 100 mg/L 5 50 EPA 300.0 01/02/2013 17:46 BGN9034

Chloride 7300 mg/L 100 1000 EPA 300.0 01/02/2013 17:46 BGN9034

Sulfate 1200 mg/L 100 1000 EPA 300.0 01/02/2013 17:46 BGN9034

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 182 ug/L 5 100 EPA 245.1 12/27/2012 08:41 AGIBBS

DISSOLVED METALS BY ICP

Manganese (Mn) 11.2 mg/L 0.05 10 EPA 200.7 01/08/2013 14:11 MHH7131

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 233 mg/L 0.5 10 EPA 200.7 01/10/2013 12:03 MHH7131

Calcium (Ca) 4930 mg/L 0.1 10 EPA 200.7 01/10/2013 12:03 MHH7131

Iron (Fe) 191 mg/L 0.1 10 EPA 200.7 01/10/2013 12:03 MHH7131

Magnesium (Mg) 1080 mg/L 0.05 10 EPA 200.7 01/10/2013 12:03 MHH7131

Manganese (Mn) 12.7 mg/L 0.05 10 EPA 200.7 01/10/2013 12:03 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 173 ug/L 10 10 EPA 200.8 01/10/2013 14:22 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 429 ug/L 10 10 EPA 200.8 01/10/2013 12:32 KRICHAR

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 01/10/2013 12:32 KRICHAR

Chromium (Cr) 372 ug/L 10 10 EPA 200.8 01/10/2013 12:32 KRICHAR

Copper (Cu) 217 ug/L 10 10 EPA 200.8 01/10/2013 12:32 KRICHAR

Nickel (Ni) 359 ug/L 10 10 EPA 200.8 01/10/2013 12:32 KRICHAR

Selenium (Se) 3890 ug/L 10 10 EPA 200.8 01/10/2013 12:32 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 01/10/2013 12:32 KRICHAR

Zinc (Zn) 496 ug/L 10 10 EPA 200.8 01/10/2013 12:32 KRICHAR

SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC)

Vendor Parameter Complete Vendor Method V_AS&C

TOTAL DISSOLVED SOLIDS

TDS 20000 mg/L 200 1 SM2540C 01/02/2013 11:45 SWILLI3

TOTAL SUSPENDED SOLIDS

TSS 1400 mg/L 250 1 SM2540D 12/31/2012 09:41 SWILLI3

Page 4 of 29
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12120342

2012027307

Collection Date: 21-Dec-12 7:35 AM

Site: EQ TANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 27.4 ug/L 2.5 50 EPA 245.1 12/27/2012 08:44 AGIBBS

DISSOLVED METALS BY ICP

Manganese (Mn) 9.68 mg/L 0.05 10 EPA 200.7 01/08/2013 14:15 MHH7131

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 227 mg/L 0.5 10 EPA 200.7 01/10/2013 12:07 MHH7131

Calcium (Ca) 3400 mg/L 0.1 10 EPA 200.7 01/10/2013 12:07 MHH7131

Iron (Fe) 35.1 mg/L 0.1 10 EPA 200.7 01/10/2013 12:07 MHH7131

Magnesium (Mg) 995 mg/L 0.05 10 EPA 200.7 01/10/2013 12:07 MHH7131

Manganese (Mn) 10.4 mg/L 0.05 10 EPA 200.7 01/10/2013 12:07 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 107 ug/L 10 10 EPA 200.8 01/10/2013 14:26 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 82.5 ug/L 10 10 EPA 200.8 01/10/2013 12:35 KRICHAR

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 01/10/2013 12:35 KRICHAR

Chromium (Cr) 61.5 ug/L 10 10 EPA 200.8 01/10/2013 12:35 KRICHAR

Copper (Cu) 37.7 ug/L 10 10 EPA 200.8 01/10/2013 12:35 KRICHAR

Nickel (Ni) 175 ug/L 10 10 EPA 200.8 01/10/2013 12:35 KRICHAR

Selenium (Se) 821 ug/L 10 10 EPA 200.8 01/10/2013 12:35 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 01/10/2013 12:35 KRICHAR

Zinc (Zn) 110 ug/L 10 10 EPA 200.8 01/10/2013 12:35 KRICHAR

2012027308

Collection Date: 21-Dec-12 7:40 AM

Site: BIOREACTOR 1 INF 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC)

Vendor Parameter Complete Vendor Method V_BRAND

DISSOLVED METALS BY ICP

Manganese (Mn) 2.19 mg/L 0.05 10 EPA 200.7 01/08/2013 14:19 MHH7131

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 209 mg/L 0.5 10 EPA 200.7 01/10/2013 12:11 MHH7131

Calcium (Ca) 3270 mg/L 0.1 10 EPA 200.7 01/10/2013 12:11 MHH7131

Iron (Fe) < 0.1 mg/L 0.1 10 EPA 200.7 01/10/2013 12:11 MHH7131

Magnesium (Mg) 929 mg/L 0.05 10 EPA 200.7 01/10/2013 12:11 MHH7131

Manganese (Mn) 2.35 mg/L 0.05 10 EPA 200.7 01/10/2013 12:11 MHH7131

Page 5 of 29
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12120342

2012027308

Collection Date: 21-Dec-12 7:40 AM

Site: BIOREACTOR 1 INF 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

DISSOLVED METALS BY ICP-MS

Selenium (Se) 120 ug/L 10 10 EPA 200.8 01/10/2013 14:29 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 01/10/2013 12:38 KRICHAR

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 01/10/2013 12:38 KRICHAR

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 01/10/2013 12:38 KRICHAR

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 01/10/2013 12:38 KRICHAR

Nickel (Ni) 23.0 ug/L 10 10 EPA 200.8 01/10/2013 12:38 KRICHAR

Selenium (Se) 97.8 ug/L 10 10 EPA 200.8 01/10/2013 12:38 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 01/10/2013 12:38 KRICHAR

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 01/10/2013 12:38 KRICHAR

SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC)

Vendor Parameter Complete Vendor Method V_AS&C

2012027309

Collection Date: 21-Dec-12 7:40 AM

Site: biOREACTOR 1 INF HG BLK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC)

Vendor Parameter Complete Vendor Method V_BRAND

2012027310

Collection Date: 21-Dec-12 7:45 AM

Site: BIOREACTOR 2 INF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC)

Vendor Parameter Complete Vendor Method V_BRAND

DISSOLVED METALS BY ICP

Manganese (Mn) 1.61 mg/L 0.05 10 EPA 200.7 01/08/2013 14:23 MHH7131

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 203 mg/L 0.5 10 EPA 200.7 01/10/2013 12:15 MHH7131

Calcium (Ca) 3250 mg/L 0.1 10 EPA 200.7 01/10/2013 12:15 MHH7131

Iron (Fe) 0.223 mg/L 0.1 10 EPA 200.7 01/10/2013 12:15 MHH7131

Magnesium (Mg) 926 mg/L 0.05 10 EPA 200.7 01/10/2013 12:15 MHH7131

Manganese (Mn) 1.68 mg/L 0.05 10 EPA 200.7 01/10/2013 12:15 MHH7131

Page 6 of 29
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12120342

2012027310

Collection Date: 21-Dec-12 7:45 AM

Site: BIOREACTOR 2 INF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

DISSOLVED METALS BY ICP-MS

Selenium (Se) 20.0 ug/L 10 10 EPA 200.8 01/10/2013 14:33 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 01/10/2013 12:42 KRICHAR

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 01/10/2013 12:42 KRICHAR

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 01/10/2013 12:42 KRICHAR

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 01/10/2013 12:42 KRICHAR

Nickel (Ni) < 10 ug/L 10 10 EPA 200.8 01/10/2013 12:42 KRICHAR

Selenium (Se) 20.1 ug/L 10 10 EPA 200.8 01/10/2013 12:42 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 01/10/2013 12:42 KRICHAR

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 01/10/2013 12:42 KRICHAR

SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC)

Vendor Parameter Complete Vendor Method V_AS&C

2012027311

Collection Date: 21-Dec-12 7:45 AM

Site: BIOREACTOR 2 INF. HG BLANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC)

Vendor Parameter Complete Vendor Method V_BRAND

2012027312

Collection Date: 21-Dec-12 7:50 AM

Site: BIOREACTOR 2 EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

INORGANIC IONS BY IC

Bromide 90 mg/L 5 50 EPA 300.0 01/02/2013 18:05 BGN9034

Chloride 6600 mg/L 100 1000 EPA 300.0 01/02/2013 18:05 BGN9034

Sulfate 1400 mg/L 100 1000 EPA 300.0 01/02/2013 18:05 BGN9034

MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC)

Vendor Parameter Complete Vendor Method V_BRAND

DISSOLVED METALS BY ICP

Manganese (Mn) 1.39 mg/L 0.05 10 EPA 200.7 01/08/2013 14:27 MHH7131

Page 7 of 29
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12120342

2012027312

Collection Date: 21-Dec-12 7:50 AM

Site: BIOREACTOR 2 EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 205 mg/L 0.5 10 EPA 200.7 01/10/2013 12:19 MHH7131

Calcium (Ca) 3040 mg/L 0.1 10 EPA 200.7 01/10/2013 12:19 MHH7131

Iron (Fe) < 0.1 mg/L 0.1 10 EPA 200.7 01/10/2013 12:19 MHH7131

Magnesium (Mg) 889 mg/L 0.05 10 EPA 200.7 01/10/2013 12:19 MHH7131

Manganese (Mn) 1.43 mg/L 0.05 10 EPA 200.7 01/10/2013 12:19 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 9.24 ug/L 5 5 EPA 200.8 01/10/2013 14:36 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 5 ug/L 5 5 EPA 200.8 01/10/2013 12:45 KRICHAR

Cadmium (Cd) < 5 ug/L 5 5 EPA 200.8 01/10/2013 12:45 KRICHAR

Chromium (Cr) < 5 ug/L 5 5 EPA 200.8 01/10/2013 12:45 KRICHAR

Copper (Cu) < 5 ug/L 5 5 EPA 200.8 01/10/2013 12:45 KRICHAR

Nickel (Ni) < 5 ug/L 5 5 EPA 200.8 01/10/2013 12:45 KRICHAR

Selenium (Se) 10.3 ug/L 5 5 EPA 200.8 01/10/2013 12:45 KRICHAR

Silver (Ag) < 5 ug/L 5 5 EPA 200.8 01/10/2013 12:45 KRICHAR

Zinc (Zn) < 5 ug/L 5 5 EPA 200.8 01/10/2013 12:45 KRICHAR

SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC)

Vendor Parameter Complete Vendor Method V_AS&C

2012027313

Collection Date: 21-Dec-12 7:50 AM

Site: BIOREACTOR 2 EFF. HG BLANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC)

Vendor Parameter Complete Vendor Method V_BRAND

2012027314

Collection Date: 21-Dec-12 8:00 AM

Site: FILTER BLANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

DISSOLVED METALS BY ICP

Manganese (Mn) 0.034 mg/L 0.005 1 EPA 200.7 01/08/2013 14:03 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) < 1 ug/L 1 1 EPA 200.8 01/10/2013 13:52 KRICHAR

Page 8 of 29
 

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

January 14, 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-HV1201 Client Project: J12120342 

Dear Mr. Perkins, 

On December 28, 2012, Brooks Rand Labs (BRL) received three (3) wastewater samples and 

three (3) associated field blanks. An aliquot was removed from each sample bottle and filtered 

into a separate container designed for dissolved mercury (Hg) analysis. The sample volume 

from the original container was logged-in for total Hg analysis. All samples were received, 

prepared, analyzed, and stored according to BRL SOPs and EPA methodology. 

Data used for regulatory purposes has a 24 hour filtration holding time requirement. Nonregulatory purposed data has a 48 hour filtration holding time. The samples were received 

outside of the 48 hour filtration requirement and the results were qualified H. 

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

and may have been evaluated using reporting limits that have been adjusted to account for 

sample aliquot size. Please refer to the Sample Results page for sample-specific MDLs, MRLs, 

and other details. Aside from concentration qualifiers, all data was reported without further 

qualification 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 us if you have any questions regarding this report. 

Sincerely, 

 

 

Lydia Greaves Mi Sun Um 

Project Manager Data Manager 

lydia@brooksrand.com misun@brooksrand.com

Page 9 of 29
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 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.

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 10 of 29
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 1252012-01 Influent Sample 12/21/2012 12/28/2012

BioReactor 1 Inf 1252012-02 Influent Sample 12/21/2012 12/28/2012

BioReactor 1 Inf Hg Blk 1252012-03 DIW Field Blank 12/21/2012 12/28/2012

BioReactor 1 Inf Hg Blk 1252012-04 DIW Field Blank 12/21/2012 12/28/2012

BioReactor 2 Inf 1252012-05 Influent Sample 12/21/2012 12/28/2012

BioReactor 2 Inf 1252012-06 Influent Sample 12/21/2012 12/28/2012

BioReactor 2 Inf Hg Blk 1252012-07 DIW Field Blank 12/21/2012 12/28/2012

BioReactor 2 Inf Hg Blk 1252012-08 DIW Field Blank 12/21/2012 12/28/2012

BioReactor 2 Eff 1252012-09 Effluent Sample 12/21/2012 12/28/2012

BioReactor 2 Eff 1252012-10 Effluent Sample 12/21/2012 12/28/2012

BioReactor 2 Eff Hg Blk 1252012-11 DIW Field Blank 12/21/2012 12/28/2012

BioReactor 2 Eff Hg Blk 1252012-12 DIW Field Blank 12/21/2012 12/28/2012

Batch Summary

Analyte Lab Matrix Method Prepared Analyzed Batch Sequence

Hg Water EPA 1631 01/02/2013 01/03/2013 B122445 1300013

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

Page 11 of 29
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Sample Results

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

BioReactor 1 Inf

1252012-01 Hg Influent T 50.2 0.76 2.02 ng/L B122445 1300013

1252012-02 Hg Influent D 44.2 H 0.76 2.02 ng/L B122445 1300013

BioReactor 1 Inf Hg Blk

1252012-03 Hg DIW T 0.15 U 0.15 0.39 ng/L B122445 1300013

1252012-04 Hg DIW D 0.15 H, U 0.15 0.41 ng/L B122445 1300013

BioReactor 2 Eff

1252012-09 Hg Effluent T 3.71 0.15 0.39 ng/L B122445 1300013

1252012-10 Hg Effluent D 0.55 H 0.15 0.39 ng/L B122445 1300013

BioReactor 2 Eff Hg Blk

1252012-11 Hg DIW T 0.15 U 0.15 0.41 ng/L B122445 1300013

1252012-12 Hg DIW D 0.15 H, U 0.15 0.41 ng/L B122445 1300013

BioReactor 2 Inf

1252012-05 Hg Influent T 11.9 0.38 1.01 ng/L B122445 1300013

1252012-06 Hg Influent D 1.08 H 0.15 0.39 ng/L B122445 1300013

BioReactor 2 Inf Hg Blk

1252012-07 Hg DIW T 0.15 U 0.15 0.39 ng/L B122445 1300013

1252012-08 Hg DIW D 0.15 H, U 0.15 0.41 ng/L B122445 1300013

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

Page 12 of 29
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Accuracy & Precision Summary

Batch: B122445

Analyte Native Spike Result Units REC & Limits RPD & Limits

Method: EPA 1631

Lab Matrix: Water

Sample

B122445-SRM1 Certified Reference Material (1249026, NIST 1641d 1000x dilution)

Hg 15.68 15.97 ng/L 102% 85-115

B122445-MS1 Matrix Spike (1251009-01)

Hg ND 20.24 17.62 ng/L 86% 71-125

B122445-MSD1 Matrix Spike Duplicate (1251009-01)

Hg ND 20.45 15.53 ng/L 75% 71-125 2413%

B122445-MS2 Matrix Spike (1252010-01)

Hg 79.93 505.1 554.7 ng/L 94% 71-125

B122445-MSD2 Matrix Spike Duplicate (1252010-01)

Hg 79.93 505.1 574.7 ng/L 98% 71-125 244%

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

Page 13 of 29
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Method Blanks & Reporting Limits

Batch: B122445

Method: EPA 1631

Matrix: Water

Analyte: Hg

Sample Result Units

B122445-BLK1 0.21 ng/L

B122445-BLK2 0.16 ng/L

B122445-BLK3 0.12 ng/L

B122445-BLK4 0.23 ng/L

Average: 0.18 Standard Deviation: 0.05 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 14 of 29
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Instrument Calibration

Sequence: 1300013

Instrument: THG-06(MerxT) Method: EPA 1631

Date: 01/03/2013

Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg

Lab ID True Value Result Units REC & Limits

1300013-IBL1 2.86 pg of Hg

1300013-IBL2 3.47 pg of Hg

1300013-IBL3 4.89 pg of Hg

1300013-IBL4 4.38 pg of Hg

1300013-CAL1 10.00 10.72 pg of Hg 107%

1300013-CAL2 25.00 25.50 pg of Hg 102%

1300013-CAL3 100.0 100.7 pg of Hg 101%

1300013-CAL4 500.0 470.1 pg of Hg 94%

1300013-CAL5 2500 2569 pg of Hg 103%

1300013-CAL6 10000 9465 pg of Hg 95%

1300013-ICV1 1568 1597 pg of Hg 102% 85-115

1300013-CCB1 7.64 pg of Hg

1300013-CCV1 500.0 490.7 pg of Hg 98% 77-123

1300013-CCB2 5.90 pg of Hg

1300013-CCB3 5.14 pg of Hg

1300013-CCB4 5.31 pg of Hg

1300013-CCV2 500.0 495.5 pg of Hg 99% 77-123

1300013-CCB5 6.03 pg of Hg

1300013-CCV3 500.0 491.4 pg of Hg 98% 77-123

1300013-CCB6 5.29 pg of Hg

1300013-CCV4 500.0 481.9 pg of Hg 96% 77-123

1300013-CCB7 5.09 pg of Hg

1300013-CCV5 500.0 478.2 pg of Hg 96% 77-123

1300013-CCB8 4.69 pg of Hg

1300013-CCV6 500.0 474.5 pg of Hg 95% 77-123

1300013-CCB9 4.76 pg of Hg

1300013-CCV7 500.0 469.6 pg of Hg 94% 77-123

1300013-CCBA 4.83 pg of Hg

1300013-CCV8 500.0 467.6 pg of Hg 94% 77-123

1300013-CCBB 9.57 pg of Hg

1300013-CCV9 500.0 469.9 pg of Hg 94% 77-123

1300013-CCBC 7.19 pg of Hg

1300013-CCVA 500.0 467.9 pg of Hg 94% 77-123

1300013-CCBD 5.26 pg of Hg

1300013-CCVB 500.0 466.9 pg of Hg 93% 77-123

1300013-CCBE 4.71 pg of Hg

1300013-CCVC 500.0 481.6 pg of Hg 96% 77-123

1300013-CCBF 4.20 pg of Hg

1300013-ICV2 1568 1515 pg of Hg 97% 85-115

1300013-CCVD 500.0 488.4 pg of Hg 98% 77-123

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

Page 15 of 29
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Instrument Calibration

Sequence: 1300013

Instrument: THG-06(MerxT) Method: EPA 1631

Date: 01/03/2013

Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg

Lab ID True Value Result Units REC & Limits

1300013-CCBG 4.25 pg of Hg

1300013-CCVE 500.0 491.1 pg of Hg 98% 77-123

1300013-CCBH 4.31 pg of Hg

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

Page 16 of 29
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Sample Containers

Lab ID: 1252012-01 Report Matrix: Influent

Sample: BioReactor 1 Inf Sample Type: Sample Received: 12/28/2012

Collected: 12/21/2012

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

A 71666330

10

Bottle FLPE Hg-T 500 mL none n/a Cooler

Lab ID: 1252012-02 Report Matrix: Influent

Sample: BioReactor 1 Inf Sample Type: Sample Received: 12/28/2012

Collected: 12/21/2012

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

A 71691270

10

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

Comments: Split from THg container

Lab ID: 1252012-03 Report Matrix: DIW

Sample: BioReactor 1 Inf Hg Blk Sample Type: Field Blank Received: 12/28/2012

Collected: 12/21/2012

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

A 71666330

10

Bottle FLPE Hg-T 500 mL none n/a Cooler

Lab ID: 1252012-04 Report Matrix: DIW

Sample: BioReactor 1 Inf Hg Blk Sample Type: Field Blank Received: 12/28/2012

Collected: 12/21/2012

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

A 71691270

10

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

Comments: Split from THg container

Lab ID: 1252012-05 Report Matrix: Influent

Sample: BioReactor 2 Inf Sample Type: Sample Received: 12/28/2012

Collected: 12/21/2012

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

A 71666330

10

Bottle FLPE Hg-T 500 mL none n/a Cooler

Lab ID: 1252012-06 Report Matrix: Influent

Sample: BioReactor 2 Inf Sample Type: Sample Received: 12/28/2012

Collected: 12/21/2012

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

A 71691270

10

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

Comments: Split from THg container

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

Page 17 of 29
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Sample Containers

Lab ID: 1252012-07 Report Matrix: DIW

Sample: BioReactor 2 Inf Hg Blk Sample Type: Field Blank Received: 12/28/2012

Collected: 12/21/2012

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

A 71666330

10

Bottle FLPE Hg-T 500 mL none n/a Cooler

Lab ID: 1252012-08 Report Matrix: DIW

Sample: BioReactor 2 Inf Hg Blk Sample Type: Field Blank Received: 12/28/2012

Collected: 12/21/2012

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

A 71691270

10

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

Comments: Split from THg container

Lab ID: 1252012-09 Report Matrix: Effluent

Sample: BioReactor 2 Eff Sample Type: Sample Received: 12/28/2012

Collected: 12/21/2012

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

A 71666330

10

Bottle FLPE Hg-T 500 mL none n/a Cooler

Lab ID: 1252012-10 Report Matrix: Effluent

Sample: BioReactor 2 Eff Sample Type: Sample Received: 12/28/2012

Collected: 12/21/2012

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

A 71691270

10

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

Comments: Split from THg container

Lab ID: 1252012-11 Report Matrix: DIW

Sample: BioReactor 2 Eff Hg Blk Sample Type: Field Blank Received: 12/28/2012

Collected: 12/21/2012

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

A 71666330

10

Bottle FLPE Hg-T 500 mL none n/a Cooler

Lab ID: 1252012-12 Report Matrix: DIW

Sample: BioReactor 2 Eff Hg Blk Sample Type: Field Blank Received: 12/28/2012

Collected: 12/21/2012

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

A 71691270

10

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

Comments: Split from THg container

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

Page 18 of 29
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Shipping Containers

Cooler

Tracking No: 535305197092 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: December 28, 2012 9:05

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

Page 19 of 29
Page 20 of 29
 

January 8, 2013 

Jay Perkins 

Duke Energy Analytical Laboratory 

Mail Code MGO3A2 (Building 7405) 

13339 Hagers Ferry Rd. 

Huntersville, NC 28078 

(704) 875-5245 

Project: Belews Creek (Flex Fuel) - WW (LIMS #J12120342) 

Dear Mr. Perkins, 

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

speciation on December 27, 2012. The samples were received in a sealed cooler at 0.0°C on 

December 28, 2012. 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 

 

 

Page 21 of 29
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: Belews Creek (Flex Fuel) - WW (LIMS #J12120342) 

January 8, 2013 

1. Sample Reception 

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

Consulting) were submitted for selenium speciation analysis on December 27, 2012. The 

samples were received on December 28, 2012 in a sealed container at 0.0°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 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 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 

Page 22 of 29
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 minimum 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 December 29, 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 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. 

Page 23 of 29
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 24 of 29
Sample Results

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

Unknown Se 

Species (n)

FGD Purge Eff 10.2 54.7 ND (<1.2) 2.0 ND (<1.8) 0.0 (0)

BioReactor 1 Inf 19.0 47.8 ND (<0.31) 1.50 ND (<0.44) 0.0 (0)

BioReactor 2 Inf 4.94 3.07 ND (<0.31) ND (<0.44) ND (<0.44) 0.0 (0)

BioReactor 2 Eff ND (<0.44) ND (<0.56) ND (<0.31) ND (<0.44) ND (<0.44) 0.0 (0)

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

ND = Not detected at the applied dilution

SeCN = Selenocyanate

MeSe(IV) = Methylseleninic acid

SeMe = Selenomethionine

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

Report Generated by: Russell Gerads

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Belews Creek (Flex Fuel) - WW

Contact: Jay Perkins

Date: January 8, 2013

LIMS #J12120342

Page 25 of 29
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 0.002 0.44 1.8

Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.56 2.3

SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.31 1.2

MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.44 1.8

SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.44 1.8

eMDL = Estimated Method Detection Limit

*Please see narrative regarding eMDL calculations

Quality Control Summary - Certified Reference Materials

Analyte (μg/L) CRM True Value Result Recovery

Se(IV) LCS 9.57 9.64 100.7

Se(VI) LCS 9.48 9.15 96.5

SeCN LCS 8.92 8.84 99.1

MeSe(IV) LCS 6.47 6.28 97.1

SeMe LCS 9.32 9.08 97.4

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Belews Creek (Flex Fuel) - WW

Contact: Jay Perkins

LIMS #J12120342

Date: January 8, 2013

Report Generated by: Russell Gerads

Page 26 of 29
Quality Control Summary - Matrix Duplicates

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

Se(IV) Batch QC 5.80 5.87 5.84 1.1

Se(VI) Batch QC 12.77 12.70 12.74 0.5

SeCN Batch QC ND (<0.31) ND (<0.31) NC NC

MeSe(IV) Batch QC ND (<0.44) ND (<0.44) NC NC

SeMe Batch QC ND (<0.44) ND (<0.44) 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 1311 93.9 1390 1304 93.4 0.5

Se(VI) Batch QC 1261 1180 92.5 1261 1171 91.9 0.7

SeCN Batch QC 1144 1057 92.4 1144 1050 91.8 0.7

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Belews Creek (Flex Fuel) - WW

Contact: Jay Perkins

LIMS #J12120342

Date: January 8, 2013

Report Generated by: Russell Gerads

Page 27 of 29
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