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: J12120171

Project Name: Flex Fuel WW

Lab Contact: Jason C Perkins

Date: 1/7/2013

Customer Address: 3195 Pine Hall Rd

Customer Name(s): Bill K, Wayne C, Melonie M, and Tom J

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 28
Sample ID's & Descriptions:

Sample ID Plant/Station

Collection 

Date and Time Collected By Sample Description

2012026438 BELEWS 10-Dec-12 7:30 AM P. GASSETT FGD Purge Eff 

2012026439 BELEWS 10-Dec-12 7:35 AM P. GASSETT EQ TANK 

2012026440 BELEWS 10-Dec-12 7:40 AM P. GASSETT BIOREACTOR 1 INF 

2012026441 BELEWS 10-Dec-12 7:40 AM P. GASSETT biOREACTOR 1 INF HG BLK 

2012026442 BELEWS 10-Dec-12 7:45 AM P. GASSETT BIOREACTOR 2 INF. 

2012026443 BELEWS 10-Dec-12 7:45 AM P. GASSETT BIOREACTOR 2 INF. HG BLANK 

2012026444 BELEWS 10-Dec-12 7:50 AM P. GASSETT BIOREACTOR 2 EFF. 

2012026445 BELEWS 10-Dec-12 7:50 AM P. GASSETT BIOREACTOR 2 EFF. HG BLANK 

2012026446 BELEWS 10-Dec-12 7:55 AM P. GASSETT FILTER BLANK 

9 Total Samples

Page 2 of 28
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: 1/7/2013

Electronic Data Deliverable (EDD) Sent Separately

Page 3 of 28
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12120171

2012026438

Collection Date: 10-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 12/21/2012 17:03 JAHERMA

Chloride 7400 mg/L 100 1000 EPA 300.0 12/21/2012 17:03 JAHERMA

Sulfate 1500 mg/L 100 1000 EPA 300.0 12/21/2012 17:03 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 201 ug/L 5 100 EPA 245.1 12/20/2012 13:16 AGIBBS

DISSOLVED METALS BY ICP

Manganese (Mn) 11.3 mg/L 0.05 10 EPA 200.7 01/02/2013 12:41 MHH7131

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 216 mg/L 0.5 10 EPA 200.7 01/02/2013 09:10 MHH7131

Calcium (Ca) 4160 mg/L 0.1 10 EPA 200.7 01/02/2013 09:10 MHH7131

Iron (Fe) 198 mg/L 0.1 10 EPA 200.7 01/02/2013 09:10 MHH7131

Magnesium (Mg) 1090 mg/L 0.05 10 EPA 200.7 01/02/2013 09:10 MHH7131

Manganese (Mn) 12.7 mg/L 0.05 10 EPA 200.7 01/02/2013 09:10 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 209 ug/L 10 10 EPA 200.8 12/19/2012 13:49 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 393 ug/L 10 10 EPA 200.8 12/20/2012 14:08 KRICHAR

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 12/20/2012 14:08 KRICHAR

Chromium (Cr) 416 ug/L 10 10 EPA 200.8 12/20/2012 14:08 KRICHAR

Copper (Cu) 261 ug/L 10 10 EPA 200.8 12/20/2012 14:08 KRICHAR

Nickel (Ni) 330 ug/L 10 10 EPA 200.8 12/20/2012 14:08 KRICHAR

Selenium (Se) 2410 ug/L 10 10 EPA 200.8 12/20/2012 14:08 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 12/20/2012 14:08 KRICHAR

Zinc (Zn) 466 ug/L 10 10 EPA 200.8 12/20/2012 14:08 KRICHAR

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

Vendor Parameter Complete Vendor Method V_AS&C

TOTAL DISSOLVED SOLIDS

TDS 21000 mg/L 200 1 SM2540C 12/12/2012 15:30 SWILLI3

TOTAL SUSPENDED SOLIDS

TSS 5300 mg/L 250 1 SM2540D 12/14/2012 10:10 TJA7067

Page 4 of 28
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12120171

2012026439

Collection Date: 10-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) 80.1 ug/L 2.5 50 EPA 245.1 12/20/2012 13:18 AGIBBS

DISSOLVED METALS BY ICP

Manganese (Mn) 9.80 mg/L 0.05 10 EPA 200.7 01/02/2013 12:45 MHH7131

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 222 mg/L 0.5 10 EPA 200.7 01/02/2013 09:14 MHH7131

Calcium (Ca) 3610 mg/L 0.1 10 EPA 200.7 01/02/2013 09:14 MHH7131

Iron (Fe) 95.9 mg/L 0.1 10 EPA 200.7 01/02/2013 09:14 MHH7131

Magnesium (Mg) 1050 mg/L 0.05 10 EPA 200.7 01/02/2013 09:14 MHH7131

Manganese (Mn) 10.9 mg/L 0.05 10 EPA 200.7 01/02/2013 09:14 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 105 ug/L 10 10 EPA 200.8 12/19/2012 13:52 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 213 ug/L 10 10 EPA 200.8 12/20/2012 14:14 KRICHAR

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 12/20/2012 14:14 KRICHAR

Chromium (Cr) 206 ug/L 10 10 EPA 200.8 12/20/2012 14:14 KRICHAR

Copper (Cu) 121 ug/L 10 10 EPA 200.8 12/20/2012 14:14 KRICHAR

Nickel (Ni) 218 ug/L 10 10 EPA 200.8 12/20/2012 14:14 KRICHAR

Selenium (Se) 1770 ug/L 10 10 EPA 200.8 12/20/2012 14:14 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 12/20/2012 14:14 KRICHAR

Zinc (Zn) 239 ug/L 10 10 EPA 200.8 12/20/2012 14:14 KRICHAR

2012026440

Collection Date: 10-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) 2.29 mg/L 0.05 10 EPA 200.7 01/02/2013 12:49 MHH7131

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 204 mg/L 0.5 10 EPA 200.7 01/02/2013 09:18 MHH7131

Calcium (Ca) 3150 mg/L 0.1 10 EPA 200.7 01/02/2013 09:18 MHH7131

Iron (Fe) < 0.1 mg/L 0.1 10 EPA 200.7 01/02/2013 09:18 MHH7131

Magnesium (Mg) 940 mg/L 0.05 10 EPA 200.7 01/02/2013 09:18 MHH7131

Manganese (Mn) 2.43 mg/L 0.05 10 EPA 200.7 01/02/2013 09:18 MHH7131

Page 5 of 28
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12120171

2012026440

Collection Date: 10-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) 89.8 ug/L 10 10 EPA 200.8 12/19/2012 13:55 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 12/20/2012 14:17 KRICHAR

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 12/20/2012 14:17 KRICHAR

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 12/20/2012 14:17 KRICHAR

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 12/20/2012 14:17 KRICHAR

Nickel (Ni) 19.6 ug/L 10 10 EPA 200.8 12/20/2012 14:17 KRICHAR

Selenium (Se) 95.4 ug/L 10 10 EPA 200.8 12/20/2012 14:17 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 12/20/2012 14:17 KRICHAR

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 12/20/2012 14:17 KRICHAR

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

Vendor Parameter Complete Vendor Method V_AS&C

2012026441

Collection Date: 10-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

2012026442

Collection Date: 10-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) 1.91 mg/L 0.05 10 EPA 200.7 01/02/2013 12:53 MHH7131

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 208 mg/L 0.5 10 EPA 200.7 01/02/2013 09:22 MHH7131

Calcium (Ca) 3280 mg/L 0.1 10 EPA 200.7 01/02/2013 09:22 MHH7131

Iron (Fe) 0.232 mg/L 0.1 10 EPA 200.7 01/02/2013 09:22 MHH7131

Magnesium (Mg) 955 mg/L 0.05 10 EPA 200.7 01/02/2013 09:22 MHH7131

Manganese (Mn) 2.10 mg/L 0.05 10 EPA 200.7 01/02/2013 09:22 MHH7131

Page 6 of 28
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12120171

2012026442

Collection Date: 10-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) 16.7 ug/L 10 10 EPA 200.8 12/19/2012 13:59 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 12/20/2012 14:20 KRICHAR

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 12/20/2012 14:20 KRICHAR

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 12/20/2012 14:20 KRICHAR

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 12/20/2012 14:20 KRICHAR

Nickel (Ni) < 10 ug/L 10 10 EPA 200.8 12/20/2012 14:20 KRICHAR

Selenium (Se) 24.3 ug/L 10 10 EPA 200.8 12/20/2012 14:20 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 12/20/2012 14:20 KRICHAR

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 12/20/2012 14:20 KRICHAR

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

Vendor Parameter Complete Vendor Method V_AS&C

2012026443

Collection Date: 10-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

2012026444

Collection Date: 10-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 94 mg/L 5 50 EPA 300.0 12/21/2012 17:22 JAHERMA

Chloride 7000 mg/L 100 1000 EPA 300.0 12/21/2012 17:22 JAHERMA

Sulfate 1800 mg/L 100 1000 EPA 300.0 12/21/2012 17:22 JAHERMA

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

Vendor Parameter Complete Vendor Method V_BRAND

DISSOLVED METALS BY ICP

Manganese (Mn) 1.62 mg/L 0.05 10 EPA 200.7 01/02/2013 12:56 MHH7131

Page 7 of 28
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12120171

2012026444

Collection Date: 10-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) 189 mg/L 0.5 10 EPA 200.7 01/02/2013 09:26 MHH7131

Calcium (Ca) 3170 mg/L 0.1 10 EPA 200.7 01/02/2013 09:26 MHH7131

Iron (Fe) < 0.1 mg/L 0.1 10 EPA 200.7 01/02/2013 09:26 MHH7131

Magnesium (Mg) 878 mg/L 0.05 10 EPA 200.7 01/02/2013 09:26 MHH7131

Manganese (Mn) 1.72 mg/L 0.05 10 EPA 200.7 01/02/2013 09:26 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 7.67 ug/L 5 5 EPA 200.8 12/19/2012 14:02 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 5 ug/L 5 5 EPA 200.8 12/20/2012 15:16 KRICHAR

Cadmium (Cd) < 5 ug/L 5 5 EPA 200.8 12/20/2012 15:16 KRICHAR

Chromium (Cr) < 5 ug/L 5 5 EPA 200.8 12/20/2012 15:16 KRICHAR

Copper (Cu) < 5 ug/L 5 5 EPA 200.8 12/20/2012 15:16 KRICHAR

Nickel (Ni) < 5 ug/L 5 5 EPA 200.8 12/20/2012 15:16 KRICHAR

Selenium (Se) 7.78 ug/L 5 5 EPA 200.8 12/20/2012 15:16 KRICHAR

Silver (Ag) < 5 ug/L 5 5 EPA 200.8 12/20/2012 15:16 KRICHAR

Zinc (Zn) < 5 ug/L 5 5 EPA 200.8 12/20/2012 15:16 KRICHAR

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

Vendor Parameter Complete Vendor Method V_AS&C

2012026445

Collection Date: 10-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

2012026446

Collection Date: 10-Dec-12 7:55 AM

Site: FILTER BLANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

DISSOLVED METALS BY ICP

Manganese (Mn) 0.014 mg/L 0.005 1 EPA 200.7 01/02/2013 12:29 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) < 1 ug/L 1 1 EPA 200.8 12/19/2012 10:51 KRICHAR

Page 8 of 28
3958 6th Ave NW • Seattle, WA 98107 • T: 206-632-6206 • F: 206-632-6017 • www.brooksrand.com • brl@brooksrand.com

December 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: J12120171

Dear Mr. Perkins,

On December 14, 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. 

The analysis of continuing calibration blanks CCB1, CCB3, and CCB6 were slightly elevated. 

These CCBs did not bracket the analysis of client samples however and no further corrective 

action was necessary. 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 me if you have any questions regarding this report.

Sincerely,

 

 

Tiffany Stilwater 

Project Manager 

tiffany@brooksrand.com 

Page 9 of 28
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 28
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 1250033-01 Influent Sample 12/10/2012 12/14/2012

BioReactor 1 Inf 1250033-02 Influent Sample 12/10/2012 12/14/2012

BioReactor 1 Inf Hg Blk 1250033-03 DIW Field Blank 12/10/2012 12/14/2012

BioReactor 1 Inf Hg Blk 1250033-04 DIW Field Blank 12/10/2012 12/14/2012

BioReactor 2 Inf 1250033-05 Influent Sample 12/10/2012 12/14/2012

BioReactor 2 Inf 1250033-06 Influent Sample 12/10/2012 12/14/2012

BioReactor 2 Inf Hg Blk 1250033-07 DIW Field Blank 12/10/2012 12/14/2012

BioReactor 2 Inf Hg Blk 1250033-08 DIW Field Blank 12/10/2012 12/14/2012

BioReactor 2 Eff 1250033-09 Effluent Sample 12/10/2012 12/14/2012

BioReactor 2 Eff 1250033-10 Effluent Sample 12/10/2012 12/14/2012

BioReactor 2 Eff Hg Blk 1250033-11 DIW Field Blank 12/10/2012 12/14/2012

BioReactor 2 Eff Hg Blk 1250033-12 DIW Field Blank 12/10/2012 12/14/2012

Batch Summary

Analyte Lab Matrix Method Prepared Analyzed Batch Sequence

Hg Water EPA 1631 12/19/2012 12/21/2012 B122396 1200954

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

Page 11 of 28
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

1250033-01 Hg Influent T 91.0 3.79 10.1 ng/L B122396 1200954

1250033-02 Hg Influent D 25.0 H 0.76 2.02 ng/L B122396 1200954

BioReactor 1 Inf Hg Blk

1250033-03 Hg DIW T 0.15 U 0.15 0.41 ng/L B122396 1200954

1250033-04 Hg DIW D 0.15 H, U 0.15 0.40 ng/L B122396 1200954

BioReactor 2 Eff

1250033-09 Hg Effluent T 3.11 0.15 0.39 ng/L B122396 1200954

1250033-10 Hg Effluent D 0.94 H 0.15 0.39 ng/L B122396 1200954

BioReactor 2 Eff Hg Blk

1250033-11 Hg DIW T 0.15 U 0.15 0.40 ng/L B122396 1200954

1250033-12 Hg DIW D 0.16 H, U 0.16 0.42 ng/L B122396 1200954

BioReactor 2 Inf

1250033-05 Hg Influent T 51.3 0.38 1.01 ng/L B122396 1200954

1250033-06 Hg Influent D 3.74 H 0.15 0.41 ng/L B122396 1200954

BioReactor 2 Inf Hg Blk

1250033-07 Hg DIW T 0.16 U 0.16 0.41 ng/L B122396 1200954

1250033-08 Hg DIW D 0.16 H, U 0.16 0.42 ng/L B122396 1200954

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

Page 12 of 28
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Accuracy & Precision Summary

Batch: B122396

Analyte Native Spike Result Units REC & Limits RPD & Limits

Method: EPA 1631

Lab Matrix: Water

Sample

B122396-SRM1 Certified Reference Material (1249026, NIST 1641d 1000x dilution)

Hg 15.68 15.84 ng/L 101% 85-115

B122396-MS3 Matrix Spike (1250030-01)

Hg 72.93 505.1 539.5 ng/L 92% 71-125

B122396-MSD3 Matrix Spike Duplicate (1250030-01)

Hg 72.93 505.1 567.7 ng/L 98% 71-125 245%

Method Blanks & Reporting Limits

Batch: B122396

Method: EPA 1631

Matrix: Water

Analyte: Hg

Sample Result Units

B122396-BLK1 -0.02 ng/L

B122396-BLK2 -0.04 ng/L

B122396-BLK3 -0.03 ng/L

B122396-BLK4 -0.03 ng/L

Average: -0.03 Standard Deviation: 0.01 MDL: 0.15

Limit: 0.50 Limit: 0.10 MRL: 0.41

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

Page 13 of 28
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Instrument Calibration

Sequence: 1200954

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

Date: 12/21/2012

Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg

Lab ID True Value Result Units REC & Limits

1200954-IBL1 8.24 pg of Hg

1200954-IBL2 8.54 pg of Hg

1200954-IBL3 8.31 pg of Hg

1200954-IBL4 8.69 pg of Hg

1200954-CAL1 10.00 10.49 pg of Hg 105%

1200954-CAL2 25.00 25.58 pg of Hg 102%

1200954-CAL3 100.0 101.3 pg of Hg 101%

1200954-CAL4 500.0 490.8 pg of Hg 98%

1200954-CAL5 2500 2476 pg of Hg 99%

1200954-CAL6 10000 9486 pg of Hg 95%

1200954-ICV1 1568 1584 pg of Hg 101% 85-115

1200954-CCB1 10.3 pg of Hg

1200954-CCV1 500.0 492.7 pg of Hg 99% 77-123

1200954-CCB2 9.98 pg of Hg

1200954-CCB3 10.4 pg of Hg

1200954-CCB4 9.18 pg of Hg

1200954-CCV2 500.0 494.2 pg of Hg 99% 77-123

1200954-CCB5 8.97 pg of Hg

1200954-CCV3 500.0 490.6 pg of Hg 98% 77-123

1200954-CCB6 10.8 pg of Hg

1200954-CCV4 500.0 489.0 pg of Hg 98% 77-123

1200954-CCB7 8.34 pg of Hg

1200954-CCV5 500.0 484.3 pg of Hg 97% 77-123

1200954-CCB8 7.82 pg of Hg

1200954-CCV6 500.0 483.7 pg of Hg 97% 77-123

1200954-CCB9 6.67 pg of Hg

1200954-CCV7 500.0 483.3 pg of Hg 97% 77-123

1200954-CCBA 6.93 pg of Hg

1200954-CCV8 500.0 478.7 pg of Hg 96% 77-123

1200954-CCBB 6.60 pg of Hg

1200954-CCV9 500.0 480.3 pg of Hg 96% 77-123

1200954-CCBC 7.40 pg of Hg

1200954-CCVA 500.0 480.0 pg of Hg 96% 77-123

1200954-CCBD 5.20 pg of Hg

1200954-CCVB 500.0 480.7 pg of Hg 96% 77-123

1200954-CCBE 5.37 pg of Hg

1200954-CCVC 500.0 483.4 pg of Hg 97% 77-123

1200954-CCBF 7.00 pg of Hg

1200954-CCVD 500.0 487.7 pg of Hg 98% 77-123

1200954-CCBG 6.56 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 14 of 28
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Instrument Calibration

Sequence: 1200954

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

Date: 12/21/2012

Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg

Lab ID True Value Result Units REC & Limits

1200954-CCVE 500.0 487.5 pg of Hg 97% 77-123

1200954-CCBH 6.30 pg of Hg

1200954-CCVF 500.0 494.4 pg of Hg 99% 77-123

1200954-CCBI 8.34 pg of Hg

1200954-CCVG 500.0 501.2 pg of Hg 100% 77-123

1200954-CCBJ 8.30 pg of Hg

1200954-CCVH 500.0 491.3 pg of Hg 98% 77-123

1200954-CCBK 8.77 pg of Hg

1200954-CCVI 500.0 490.8 pg of Hg 98% 77-123

1200954-CCBL 8.05 pg of Hg

1200954-CCVJ 500.0 480.2 pg of Hg 96% 77-123

1200954-CCBM 6.68 pg of Hg

1200954-CCVK 500.0 476.3 pg of Hg 95% 77-123

1200954-CCBN 6.40 pg of Hg

1200954-CCVL 500.0 479.9 pg of Hg 96% 77-123

1200954-CCBO 8.78 pg of Hg

1200954-CCVM 500.0 443.9 pg of Hg 89% 77-123

1200954-CCBP 8.26 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 15 of 28
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Sample Containers

Lab ID: 1250033-01 Report Matrix: Influent

Sample: BioReactor 1 Inf Sample Type: Sample Received: 12/14/2012

Collected: 12/10/2012

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

A 71666330

10

Bottle FLPE Hg-T 500 mL none n/a Cooler 1

Lab ID: 1250033-02 Report Matrix: Influent

Sample: BioReactor 1 Inf Sample Type: Sample Received: 12/14/2012

Collected: 12/10/2012

Comments: Qualify H

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

A 71691270

10

Bottle FLPE Hg-T 250 mL none n/a Cooler 1

Lab ID: 1250033-03 Report Matrix: DIW

Sample: BioReactor 1 Inf Hg Blk Sample Type: Field Blank Received: 12/14/2012

Collected: 12/10/2012

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

A 71666330

10

Bottle FLPE Hg-T 500 mL none n/a Cooler 1

Lab ID: 1250033-04 Report Matrix: DIW

Sample: BioReactor 1 Inf Hg Blk Sample Type: Field Blank Received: 12/14/2012

Collected: 12/10/2012

Comments: Qualify H

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

A 71691270

10

Bottle FLPE Hg-T 250 mL none n/a Cooler 1

Lab ID: 1250033-05 Report Matrix: Influent

Sample: BioReactor 2 Inf Sample Type: Sample Received: 12/14/2012

Collected: 12/10/2012

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

A 71666330

10

Bottle FLPE Hg-T 500 mL none n/a Cooler 1

Lab ID: 1250033-06 Report Matrix: Influent

Sample: BioReactor 2 Inf Sample Type: Sample Received: 12/14/2012

Collected: 12/10/2012

Comments: Qualify H

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

A 71691270

10

Bottle FLPE Hg-T 250 mL none n/a Cooler 1

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

Page 16 of 28
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Sample Containers

Lab ID: 1250033-07 Report Matrix: DIW

Sample: BioReactor 2 Inf Hg Blk Sample Type: Field Blank Received: 12/14/2012

Collected: 12/10/2012

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

A 71666330

10

Bottle FLPE Hg-T 500 mL none n/a Cooler 1

Lab ID: 1250033-08 Report Matrix: DIW

Sample: BioReactor 2 Inf Hg Blk Sample Type: Field Blank Received: 12/14/2012

Collected: 12/10/2012

Comments: Qualify H

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

A 71691270

10

Bottle FLPE Hg-T 250 mL none n/a Cooler 1

Lab ID: 1250033-09 Report Matrix: Effluent

Sample: BioReactor 2 Eff Sample Type: Sample Received: 12/14/2012

Collected: 12/10/2012

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

A 71666330

10

Bottle FLPE Hg-T 500 mL none n/a Cooler 1

Lab ID: 1250033-10 Report Matrix: Effluent

Sample: BioReactor 2 Eff Sample Type: Sample Received: 12/14/2012

Collected: 12/10/2012

Comments: Qualify H

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

A 71691270

10

Bottle FLPE Hg-T 250 mL none n/a Cooler 1

Lab ID: 1250033-11 Report Matrix: DIW

Sample: BioReactor 2 Eff Hg Blk Sample Type: Field Blank Received: 12/14/2012

Collected: 12/10/2012

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

A 71666330

10

Bottle FLPE Hg-T 500 mL none n/a Cooler 1

Lab ID: 1250033-12 Report Matrix: DIW

Sample: BioReactor 2 Eff Hg Blk Sample Type: Field Blank Received: 12/14/2012

Collected: 12/10/2012

Comments: Qualify H

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

A 71691270

10

Bottle FLPE Hg-T 250 mL none n/a Cooler 1

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

Page 17 of 28
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Shipping Containers

Cooler 1

Tracking No: 535305196800 via FedEx

Temperature: -0.4 °C

Coolant Type: Ice

Description: Cooler 1

Damaged in transit? No

Returned to client? No

Custody seals present? No

Custody seals intact? No

COC present? Yes

Received: December 14, 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 18 of 28
Page 19 of 28
 

December 19, 2012 

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 #J12120171) 

Dear Mr. Perkins, 

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

speciation on December 13, 2012. The samples were received in a sealed cooler at -0.2°C on 

December 14, 2012. Selenium speciation analysis was performed via ion chromatography 

inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICP-DRC-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 20 of 28
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 #J12120171) 

December 19, 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 December 13, 2012. The 

samples were received on December 14, 2012 in a sealed container at -0.2°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 dynamic reaction cell 

mass spectrometry (IC-ICP-DRC-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-DRC-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 21 of 28
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-DRC-MS Each sample for selenium speciation 

analysis was analyzed by ion chromatography inductively coupled plasma dynamic reaction 

cell mass spectrometry (IC-ICP-DRC-MS) on December 14, 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 (DRC) 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 22 of 28
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 23 of 28
Sample Results

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

Unknown Se 

Species (n)

FGD Purge Eff 114 55.8 ND (<0.63) 3.20 ND (<0.83) 6.09 (2)

BioReactor 1 Inf 23.9 53.9 ND (<0.16) 2.22 ND (<0.21) 1.31 (1)

BioReactor 2 Inf 3.39 2.04 ND (<0.16) ND (<0.21) ND (<0.21) 0 (0)

BioReactor 2 Eff ND (<0.17) ND (<0.29) ND (<0.16) ND (<0.21) ND (<0.21) 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: December 19, 2012

LIMS #J12120171

Page 24 of 28
Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 50x eMDL 200x

Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.003 0.17 0.70

Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.006 0.29 1.2

SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.003 0.16 0.63

MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.21 0.83

SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.21 0.83

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 10.09 105.4

Se(VI) LCS 9.48 9.58 101.0

SeCN LCS 8.92 9.00 100.9

MeSe(IV) LCS 6.47 6.58 101.7

SeMe LCS 9.32 9.54 102.4

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Belews Creek (Flex Fuel) - WW

Contact: Jay Perkins

LIMS #J12120171

Date: December 19, 2012

Report Generated by: Russell Gerads

Page 25 of 28
Quality Control Summary - Matrix Duplicates

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

Se(IV) Batch QC 0.26 0.22 0.24 14.8

Se(VI) Batch QC ND (<0.29) ND (<0.29) NC NC

SeCN Batch QC ND (<0.16) ND (<0.16) NC NC

MeSe(IV) Batch QC ND (<0.21) ND (<0.21) NC NC

SeMe Batch QC ND (<0.21) ND (<0.21) 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 278.0 297.2 106.8 278.0 294.9 106.0 0.8

Se(VI) Batch QC 252.3 268.0 106.2 252.3 254.4 100.9 5.2

SeCN Batch QC 228.8 232.5 101.6 228.8 225.3 98.5 3.2

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Belews Creek (Flex Fuel) - WW

Contact: Jay Perkins

LIMS #J12120171

Date: December 19, 2012

Report Generated by: Russell Gerads

Page 26 of 28
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