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: J12100483

Lab Contact: Jason C Perkins

Date: 11/14/2012

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

2012023123 BELEWS 29-Oct-12 7:30 AM W. B. WORKMAN FGD Purge Eff 

2012023124 BELEWS 29-Oct-12 7:35 AM W. B. WORKMAN EQ TANK 

2012023125 BELEWS 29-Oct-12 7:40 AM W. B. WORKMAN BIOREACTOR 1 INF 

2012023126 BELEWS 29-Oct-12 W. B. WORKMAN biOREACTOR 1 INF HG BLK 

2012023127 BELEWS 29-Oct-12 7:45 AM W. B. WORKMAN BIOREACTOR 2 INF. 

2012023128 BELEWS 29-Oct-12 W. B. WORKMAN BIOREACTOR 2 INF. HG BLANK 

2012023129 BELEWS 29-Oct-12 7:50 AM W. B. WORKMAN BIOREACTOR 2 EFF. 

2012023130 BELEWS 29-Oct-12 W. B. WORKMAN BIOREACTOR 2 EFF. HG BLANK 

2012023131 BELEWS 29-Oct-12 8:00 AM W. B. WORKMAN 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: 11/14/2012

Electronic Data Deliverable (EDD) Sent Separately

Page 3 of 28
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12100483

2012023123

Collection Date: 29-Oct-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 85 mg/L 5 50 EPA 300.0 11/12/2012 17:56 JAHERMA

Chloride 5900 mg/L 100 1000 EPA 300.0 11/12/2012 17:56 JAHERMA

Sulfate 1100 mg/L 100 1000 EPA 300.0 11/12/2012 17:56 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 180 ug/L 5 100 EPA 245.1 11/01/2012 14:21 AGIBBS

DISSOLVED METALS BY ICP

Manganese (Mn) 5.71 mg/L 0.05 10 EPA 200.7 11/05/2012 12:15 DJSULL1

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 137 mg/L 0.5 10 EPA 200.7 11/05/2012 14:29 DJSULL1

Calcium (Ca) 3770 mg/L 0.1 10 EPA 200.7 11/05/2012 14:29 DJSULL1

Iron (Fe) 107 mg/L 0.1 10 EPA 200.7 11/05/2012 14:29 DJSULL1

Magnesium (Mg) 585 mg/L 0.05 10 EPA 200.7 11/05/2012 14:29 DJSULL1

Manganese (Mn) 6.17 mg/L 0.05 10 EPA 200.7 11/05/2012 14:29 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 220 ug/L 10 10 EPA 200.8 11/01/2012 13:13 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 240 ug/L 10 10 EPA 200.8 11/01/2012 13:28 KRICHAR

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 11/01/2012 13:28 KRICHAR

Chromium (Cr) 238 ug/L 10 10 EPA 200.8 11/01/2012 13:28 KRICHAR

Copper (Cu) 159 ug/L 10 10 EPA 200.8 11/01/2012 13:28 KRICHAR

Nickel (Ni) 225 ug/L 10 10 EPA 200.8 11/01/2012 13:28 KRICHAR

Selenium (Se) 5720 ug/L 20 20 EPA 200.8 11/01/2012 13:28 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 11/01/2012 13:28 KRICHAR

Zinc (Zn) 313 ug/L 10 10 EPA 200.8 11/01/2012 13:28 KRICHAR

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

Vendor Parameter Complete Vendor Method V_AS&C

TOTAL DISSOLVED SOLIDS

TDS 16000 mg/L 200 1 SM2540C 10/30/2012 15:43 SWILLI3

TOTAL SUSPENDED SOLIDS

TSS 4000 mg/L 250 1 SM2540D 11/05/2012 10:56 SWILLI3

Page 4 of 28
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12100483

2012023124

Collection Date: 29-Oct-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) 136 ug/L 2.5 50 EPA 245.1 11/01/2012 14:24 AGIBBS

DISSOLVED METALS BY ICP

Manganese (Mn) 4.73 mg/L 0.05 10 EPA 200.7 11/05/2012 12:19 DJSULL1

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 128 mg/L 0.5 10 EPA 200.7 11/05/2012 14:33 DJSULL1

Calcium (Ca) 3370 mg/L 0.1 10 EPA 200.7 11/05/2012 14:33 DJSULL1

Iron (Fe) 81.2 mg/L 0.1 10 EPA 200.7 11/05/2012 14:33 DJSULL1

Magnesium (Mg) 525 mg/L 0.05 10 EPA 200.7 11/05/2012 14:33 DJSULL1

Manganese (Mn) 5.14 mg/L 0.05 10 EPA 200.7 11/05/2012 14:33 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 161 ug/L 10 10 EPA 200.8 11/01/2012 13:16 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 195 ug/L 10 10 EPA 200.8 11/01/2012 12:36 KRICHAR

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 11/01/2012 12:36 KRICHAR

Chromium (Cr) 189 ug/L 10 10 EPA 200.8 11/01/2012 12:36 KRICHAR

Copper (Cu) 122 ug/L 10 10 EPA 200.8 11/01/2012 12:36 KRICHAR

Nickel (Ni) 192 ug/L 10 10 EPA 200.8 11/01/2012 12:36 KRICHAR

Selenium (Se) 4130 ug/L 10 10 EPA 200.8 11/01/2012 12:36 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 11/01/2012 12:36 KRICHAR

Zinc (Zn) 234 ug/L 10 10 EPA 200.8 11/01/2012 12:36 KRICHAR

2012023125

Collection Date: 29-Oct-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) 0.833 mg/L 0.05 10 EPA 200.7 11/05/2012 12:23 DJSULL1

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 120 mg/L 0.5 10 EPA 200.7 11/05/2012 14:37 DJSULL1

Calcium (Ca) 2920 mg/L 0.1 10 EPA 200.7 11/05/2012 14:37 DJSULL1

Iron (Fe) < 0.1 mg/L 0.1 10 EPA 200.7 11/05/2012 14:37 DJSULL1

Magnesium (Mg) 486 mg/L 0.05 10 EPA 200.7 11/05/2012 14:37 DJSULL1

Manganese (Mn) 0.821 mg/L 0.05 10 EPA 200.7 11/05/2012 14:37 DJSULL1

Page 5 of 28
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12100483

2012023125

Collection Date: 29-Oct-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) 121 ug/L 10 10 EPA 200.8 11/01/2012 13:19 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 11/01/2012 12:39 KRICHAR

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 11/01/2012 12:39 KRICHAR

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 11/01/2012 12:39 KRICHAR

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 11/01/2012 12:39 KRICHAR

Nickel (Ni) 13.5 ug/L 10 10 EPA 200.8 11/01/2012 12:39 KRICHAR

Selenium (Se) 113 ug/L 10 10 EPA 200.8 11/01/2012 12:39 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 11/01/2012 12:39 KRICHAR

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 11/01/2012 12:39 KRICHAR

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

Vendor Parameter Complete Vendor Method V_AS&C

2012023126

Collection Date: 29-Oct-12

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

2012023127

Collection Date: 29-Oct-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) 1.41 mg/L 0.05 10 EPA 200.7 11/05/2012 12:26 DJSULL1

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 124 mg/L 0.5 10 EPA 200.7 11/05/2012 14:41 DJSULL1

Calcium (Ca) 3100 mg/L 0.1 10 EPA 200.7 11/05/2012 14:41 DJSULL1

Iron (Fe) < 0.1 mg/L 0.1 10 EPA 200.7 11/05/2012 14:41 DJSULL1

Magnesium (Mg) 516 mg/L 0.05 10 EPA 200.7 11/05/2012 14:41 DJSULL1

Manganese (Mn) 1.47 mg/L 0.05 10 EPA 200.7 11/05/2012 14:41 DJSULL1

Page 6 of 28
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12100483

2012023127

Collection Date: 29-Oct-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) 13.8 ug/L 10 10 EPA 200.8 11/01/2012 13:22 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 11/01/2012 12:42 KRICHAR

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 11/01/2012 12:42 KRICHAR

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 11/01/2012 12:42 KRICHAR

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 11/01/2012 12:42 KRICHAR

Nickel (Ni) < 10 ug/L 10 10 EPA 200.8 11/01/2012 12:42 KRICHAR

Selenium (Se) < 10 ug/L 10 10 EPA 200.8 11/01/2012 12:42 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 11/01/2012 12:42 KRICHAR

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 11/01/2012 12:42 KRICHAR

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

Vendor Parameter Complete Vendor Method V_AS&C

2012023128

Collection Date: 29-Oct-12

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

2012023129

Collection Date: 29-Oct-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 81 mg/L 5 50 EPA 300.0 11/12/2012 18:33 JAHERMA

Chloride 6100 mg/L 100 1000 EPA 300.0 11/12/2012 18:33 JAHERMA

Sulfate 1400 mg/L 100 1000 EPA 300.0 11/12/2012 18:33 JAHERMA

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

Vendor Parameter Complete Vendor Method V_BRAND

DISSOLVED METALS BY ICP

Manganese (Mn) 1.27 mg/L 0.05 10 EPA 200.7 11/05/2012 12:30 DJSULL1

Page 7 of 28
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12100483

2012023129

Collection Date: 29-Oct-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) 121 mg/L 0.5 10 EPA 200.7 11/05/2012 14:45 DJSULL1

Calcium (Ca) 2950 mg/L 0.1 10 EPA 200.7 11/05/2012 14:45 DJSULL1

Iron (Fe) < 0.1 mg/L 0.1 10 EPA 200.7 11/05/2012 14:45 DJSULL1

Magnesium (Mg) 492 mg/L 0.05 10 EPA 200.7 11/05/2012 14:45 DJSULL1

Manganese (Mn) 1.27 mg/L 0.05 10 EPA 200.7 11/05/2012 14:45 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 5.31 ug/L 5 5 EPA 200.8 11/01/2012 13:25 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 5 ug/L 5 5 EPA 200.8 11/01/2012 12:45 KRICHAR

Cadmium (Cd) < 5 ug/L 5 5 EPA 200.8 11/01/2012 12:45 KRICHAR

Chromium (Cr) < 5 ug/L 5 5 EPA 200.8 11/01/2012 12:45 KRICHAR

Copper (Cu) < 5 ug/L 5 5 EPA 200.8 11/01/2012 12:45 KRICHAR

Nickel (Ni) < 5 ug/L 5 5 EPA 200.8 11/01/2012 12:45 KRICHAR

Selenium (Se) 5.68 ug/L 5 5 EPA 200.8 11/01/2012 12:45 KRICHAR

Silver (Ag) < 5 ug/L 5 5 EPA 200.8 11/01/2012 12:45 KRICHAR

Zinc (Zn) < 5 ug/L 5 5 EPA 200.8 11/01/2012 12:45 KRICHAR

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

Vendor Parameter Complete Vendor Method V_AS&C

2012023130

Collection Date: 29-Oct-12

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

2012023131

Collection Date: 29-Oct-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) < 0.005 mg/L 0.005 1 EPA 200.7 11/05/2012 12:03 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) < 1 ug/L 1 1 EPA 200.8 11/01/2012 12:21 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 

November 9, 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: J12100483 

Dear Mr. Perkins, 

On October 31, 2012, Brooks Rand Labs (BRL) received three (3) wastewater samples and 

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

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

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

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

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

within holding time and no qualification was necessary. 

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 CCB1 was slightly greater than the low calibration standard. The cause was 

likely due to carryover from the ICV. No client samples were bracketed by the elevated CCB 

and no further action was required. All data was reported without additional qualification, aside 

from concentration qualifiers, and all associated quality control sample results met the 

acceptance criteria. 

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

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

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

report. 

Sincerely, 

 

Lydia Greaves Mi Sun Um 

Project Manager Data Manager 

lydia@brooksrand.com misun@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 1244007-01 Influent Sample 10/29/2012 10/31/2012

Bioreactor 1 Inf 1244007-02 Influent Sample 10/29/2012 10/31/2012

Bioreactor 1 Inf Hg Blk 1244007-03 DIW Field Blank 10/29/2012 10/31/2012

Bioreactor 1 Inf Hg Blk 1244007-04 DIW Field Blank 10/29/2012 10/31/2012

Bioreactor 2 Inf 1244007-05 Influent Sample 10/29/2012 10/31/2012

Bioreactor 2 Inf 1244007-06 Influent Sample 10/29/2012 10/31/2012

Bioreactor 2 Inf Hg Blk 1244007-07 DIW Field Blank 10/29/2012 10/31/2012

Bioreactor 2 Inf Hg Blk 1244007-08 DIW Field Blank 10/29/2012 10/31/2012

Bioreactor 2 Eff 1244007-09 Effluent Sample 10/29/2012 10/31/2012

Bioreactor 2 Eff 1244007-10 Effluent Sample 10/29/2012 10/31/2012

Bioreactor 2 Eff Hg Blk 1244007-11 DIW Field Blank 10/29/2012 10/31/2012

Bioreactor 2 Eff Hg Blk 1244007-12 DIW Field Blank 10/29/2012 10/31/2012

Batch Summary

Analyte Lab Matrix Method Prepared Analyzed Batch Sequence

Hg Water EPA 1631 11/02/2012 11/05/2012 B122059 1200848

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

1244007-01 Hg Influent T 214 3.79 10.1 ng/L B122059 1200848

1244007-02 Hg Influent D 21.0 0.76 2.02 ng/L B122059 1200848

Bioreactor 1 Inf Hg Blk

1244007-03 Hg DIW T 0.15 U 0.15 0.40 ng/L B122059 1200848

1244007-04 Hg DIW D 0.15 U 0.15 0.40 ng/L B122059 1200848

Bioreactor 2 Eff

1244007-09 Hg Effluent T 10.1 0.38 1.01 ng/L B122059 1200848

1244007-10 Hg Effluent D 2.41 0.15 0.41 ng/L B122059 1200848

Bioreactor 2 Eff Hg Blk

1244007-11 Hg DIW T 0.16 U 0.16 0.41 ng/L B122059 1200848

1244007-12 Hg DIW D 0.15 U 0.15 0.41 ng/L B122059 1200848

Bioreactor 2 Inf

1244007-05 Hg Influent T 49.7 0.76 2.02 ng/L B122059 1200848

1244007-06 Hg Influent D 7.97 0.38 1.01 ng/L B122059 1200848

Bioreactor 2 Inf Hg Blk

1244007-07 Hg DIW T 0.15 U 0.15 0.40 ng/L B122059 1200848

1244007-08 Hg DIW D 0.15 U 0.15 0.41 ng/L B122059 1200848

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: B122059

Analyte Native Spike Result Units REC & Limits RPD & Limits

Method: EPA 1631

Lab Matrix: Water

Sample

B122059-SRM1 Certified Reference Material (1241014, THg ICV 1641d)

Hg 15.68 16.13 ng/L 103% 85-115

B122059-MS1 Matrix Spike (1242012-08)

Hg 114.9 122.7 211.9 ng/L 79% 71-125

B122059-MSD1 Matrix Spike Duplicate (1242012-08)

Hg 114.9 126.9 231.4 ng/L 92% 71-125 249%

B122059-MS2 Matrix Spike (1244007-01)

Hg 213.7 1010 1287 ng/L 106% 71-125

B122059-MSD2 Matrix Spike Duplicate (1244007-01)

Hg 213.7 1010 1289 ng/L 106% 71-125 240.1%

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

Method Blanks & Reporting Limits

Batch: B122059

Method: EPA 1631

Matrix: Water

Analyte: Hg

Sample Result Units

B122059-BLK1 0.18 ng/L

B122059-BLK2 0.21 ng/L

B122059-BLK3 0.19 ng/L

B122059-BLK4 0.18 ng/L

Average: 0.19 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 14 of 28
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Instrument Calibration

Sequence: 1200848

Instrument: THG-05 Method: EPA 1631

Date: 11/05/2012

Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg

Lab ID True Value Result Units REC & Limits

1200848-IBL1 1.58 pg of Hg

1200848-IBL2 4.49 pg of Hg

1200848-IBL3 4.31 pg of Hg

1200848-IBL4 4.87 pg of Hg

1200848-CAL1 10.00 10.20 pg of Hg 102%

1200848-CAL2 25.00 25.23 pg of Hg 101%

1200848-CAL3 100.0 99.31 pg of Hg 99%

1200848-CAL4 500.0 489.5 pg of Hg 98%

1200848-CAL5 2500 2511 pg of Hg 100%

1200848-CAL6 10000 9955 pg of Hg 100%

1200848-ICV1 1568 1613 pg of Hg 103% 85-115

1200848-CCB1 10.6 pg of Hg

1200848-CCV1 500.0 506.2 pg of Hg 101% 77-123

1200848-CCB2 6.92 pg of Hg

1200848-CCB3 5.62 pg of Hg

1200848-CCB4 6.39 pg of Hg

1200848-CCV2 500.0 516.9 pg of Hg 103% 77-123

1200848-CCB5 6.76 pg of Hg

1200848-CCV3 500.0 496.5 pg of Hg 99% 77-123

1200848-CCB6 5.69 pg of Hg

1200848-CCV4 500.0 495.8 pg of Hg 99% 77-123

1200848-CCB7 6.05 pg of Hg

1200848-CCV5 500.0 515.0 pg of Hg 103% 77-123

1200848-CCB8 5.42 pg of Hg

1200848-CCV6 500.0 520.7 pg of Hg 104% 77-123

1200848-CCB9 5.64 pg of Hg

1200848-CCV7 500.0 522.9 pg of Hg 105% 77-123

1200848-CCBA 5.50 pg of Hg

1200848-CCV8 500.0 522.3 pg of Hg 104% 77-123

1200848-CCBB 5.39 pg of Hg

1200848-CCV9 500.0 536.4 pg of Hg 107% 77-123

1200848-CCBC 4.95 pg of Hg

1200848-CCVA 500.0 535.5 pg of Hg 107% 77-123

1200848-CCBD 5.36 pg of Hg

1200848-CCVB 500.0 531.1 pg of Hg 106% 77-123

1200848-CCBE 7.28 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: 1244007-01 Report Matrix: Influent

Sample: Bioreactor 1 Inf Sample Type: Sample Received: 10/31/2012

Collected: 10/29/2012

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: 1244007-02 Report Matrix: Influent

Sample: Bioreactor 1 Inf Sample Type: Sample Received: 10/31/2012

Collected: 10/29/2012

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

A 71659890

20

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

Lab ID: 1244007-03 Report Matrix: DIW

Sample: Bioreactor 1 Inf Hg Blk Sample Type: Field Blank Received: 10/31/2012

Collected: 10/29/2012

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: 1244007-04 Report Matrix: DIW

Sample: Bioreactor 1 Inf Hg Blk Sample Type: Field Blank Received: 10/31/2012

Collected: 10/29/2012

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

A 71659890

20

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

Lab ID: 1244007-05 Report Matrix: Influent

Sample: Bioreactor 2 Inf Sample Type: Sample Received: 10/31/2012

Collected: 10/29/2012

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: 1244007-06 Report Matrix: Influent

Sample: Bioreactor 2 Inf Sample Type: Sample Received: 10/31/2012

Collected: 10/29/2012

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

A 71659890

20

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

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: 1244007-07 Report Matrix: DIW

Sample: Bioreactor 2 Inf Hg Blk Sample Type: Field Blank Received: 10/31/2012

Collected: 10/29/2012

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: 1244007-08 Report Matrix: DIW

Sample: Bioreactor 2 Inf Hg Blk Sample Type: Field Blank Received: 10/31/2012

Collected: 10/29/2012

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

A 71659890

20

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

Lab ID: 1244007-09 Report Matrix: Effluent

Sample: Bioreactor 2 Eff Sample Type: Sample Received: 10/31/2012

Collected: 10/29/2012

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: 1244007-10 Report Matrix: Effluent

Sample: Bioreactor 2 Eff Sample Type: Sample Received: 10/31/2012

Collected: 10/29/2012

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

A 71659890

20

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

Lab ID: 1244007-11 Report Matrix: DIW

Sample: Bioreactor 2 Eff Hg Blk Sample Type: Field Blank Received: 10/31/2012

Collected: 10/29/2012

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: 1244007-12 Report Matrix: DIW

Sample: Bioreactor 2 Eff Hg Blk Sample Type: Field Blank Received: 10/31/2012

Collected: 10/29/2012

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

A 71666330

10

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

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

Tracking No: 535305195230 via FedEx

Temperature: 0.3 °C

Coolant Type: Ice

Description: Cooler

Damaged in transit? No

Returned to client? No

Custody seals present? No

Custody seals intact? No

COC present? Yes

Received: October 31, 2012 8:30

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
 

November 9, 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 # J12100483) 

Dear Mr. Perkins, 

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

speciation analysis on October 30, 2012. The samples were received in a sealed cooler at -0.2°C 

on October 31, 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 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 # J12100483) 

November 9, 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 October 30, 2012. The 

samples were received on October 31, 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 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 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-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 November 2, 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 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 98.8 78.2 ND (<3.1) 5.0 ND (<3.0) 0.0 (0)

BioReactor 1 Inf 16.4 63.1 ND (<0.77) 5.23 ND (<0.75) 3.73 (1)

BioReactor 2 Inf 2.23 ND (<0.66) ND (<0.77) ND (<0.75) ND (<0.75) 0.0 (0)

BioReactor 2 Eff ND (<0.81) ND (<0.66) ND (<0.77) ND (<0.75) ND (<0.75) 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: November 9, 2012

LIMS #J12100483

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) 0.00 0.00 0.00 0.00 0.00 0.00 0.016 0.81 3.2

Se(VI) 0.00 0.00 0.00 0.00 0.00 0.00 0.013 0.66 2.7

SeCN 0.00 0.00 0.00 0.00 0.00 0.00 0.015 0.77 3.1

MeSe(IV) 0.00 0.00 0.00 0.00 0.00 0.00 0.015 0.75 3.0

SeMe 0.00 0.00 0.00 0.00 0.00 0.00 0.015 0.75 3.0

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 8.79 92.7

SeCN LCS 8.92 8.61 96.5

MeSe(IV) LCS 6.47 6.37 98.5

SeMe LCS 9.32 8.84 94.9

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Belews Creek (Flex Fuel) - WW

Contact: Jay Perkins

LIMS #J12100483

Date: November 9, 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 ND (<3.2) ND (<3.2) NC NC

Se(VI) Batch QC 65.6 65.7 65.7 0.1

SeCN Batch QC 13.8 16.3 15.0 16.8

MeSe(IV) Batch QC ND (<3.0) ND (<3.0) NC NC

SeMe Batch QC ND (<3.0) ND (<3.0) 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 1112 1122 100.9 1112 1079 97.0 3.9

Se(VI) Batch QC 1009 1063 98.8 1009 1045 97.0 1.7

SeCN Batch QC 915 931 100.2 915 910 97.9 2.3

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Belews Creek (Flex Fuel) - WW

Contact: Jay Perkins

LIMS #J12100483

Date: November 9, 2012

Report Generated by: Russell Gerads

Page 26 of 28
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