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: J12100090

Lab Contact: Jason C Perkins

Date: 11/5/2012

Customer Address: 253 Plant Allen Road

Customer Name(s): Don Scruggs, Robbin Jolly, Ray Lidke, Bill Kennedy

Belmont, NC 28012

Phone: 980-875-5348

Report Authorized By:

(Signature)

Program Comments:

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

Data Flags & Calculations:

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

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

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

included on the Duke Certificate of Analysis is to be used as information only. Certified vendor results can be found in the 

subcontracted lab final report. Duke Energy Analytical Laboratory subcontracts analyses to other vendor laboratories that have 

been qualified by Duke Energy to perform these analyses except where noted.

Data Package:

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

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

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

order of individual sections within this report is as follows:

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

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

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

Certification:

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

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

specific methods. 

Page 1 of 28
Sample ID's & Descriptions:

Sample ID Plant/Station

Collection 

Date and Time Collected By Sample Description

2012021129 ALLEN 17-Oct-12 12:40 PM Chris Williams FGD Purge Eff 

2012021130 ALLEN 17-Oct-12 12:23 PM Chris Williams EQ Tank Eff 

2012021131 ALLEN 17-Oct-12 12:05 PM Chris Williams BioReactor 1 Inf 

2012021132 ALLEN 17-Oct-12 12:11 PM Chris Williams BioReactor 2 Inf 

2012021133 ALLEN 17-Oct-12 12:18 PM Chris Williams BioReactor 2 Eff 

2012021134 ALLEN 17-Oct-12 12:50 PM Chris Williams Filter Blk 

2012021135 ALLEN 03-Oct-12 11:15 AM J. TALLENT TRIP BLANK 

2012021137 ALLEN 17-Oct-12 12:05 PM Chris Williams BioReactor 1 Inf 

2012021138 ALLEN 17-Oct-12 12:05 PM Chris Williams Hg Blk BioReactor 1 Inf 

2012021139 ALLEN 17-Oct-12 12:11 PM Chris Williams BioReactor 2 Inf 

2012021140 ALLEN 17-Oct-12 12:11 PM Chris Williams Hg Blk BioReactor 2 Inf 

2012021141 ALLEN 17-Oct-12 12:18 PM Chris Williams BioReactor 2 Eff 

2012021142 ALLEN 17-Oct-12 12:18 PM Chris Williams Hg Blk BioReactor 2 Eff 

13 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: 11/5/2012

Electronic Data Deliverable (EDD) Sent Separately

Page 3 of 28
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12100090

2012021129

Collection Date: 17-Oct-12 12:40 PM

Site: FGD Purge Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

INORGANIC IONS BY IC

Bromide 520 mg/L 50 500 EPA 300.0 10/25/2012 11:13 BGN9034

Chloride 1300 mg/L 50 500 EPA 300.0 10/25/2012 11:13 BGN9034

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 9.05 ug/L 2.5 50 EPA 245.1 10/25/2012 13:36 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 22.6 mg/L 0.5 10 EPA 200.7 10/24/2012 11:40 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 999 ug/L 10 10 EPA 200.8 10/23/2012 11:40 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 174 ug/L 10 10 EPA 200.8 10/25/2012 11:46 KRICHAR

Chromium (Cr) 167 ug/L 10 10 EPA 200.8 10/25/2012 11:46 KRICHAR

Copper (Cu) 166 ug/L 10 10 EPA 200.8 10/25/2012 11:46 KRICHAR

Nickel (Ni) 232 ug/L 10 10 EPA 200.8 10/25/2012 11:46 KRICHAR

Selenium (Se) 3290 ug/L 10 10 EPA 200.8 10/25/2012 11:46 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 10/25/2012 11:46 KRICHAR

Zinc (Zn) 209 ug/L 10 10 EPA 200.8 10/25/2012 11:46 KRICHAR

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

Vendor Parameter Complete Vendor Method V_AS&C

TOTAL DISSOLVED SOLIDS

TDS 7500 mg/L 200 1 SM2540C 10/22/2012 16:50 SWILLI3

2012021130

Collection Date: 17-Oct-12 12:23 PM

Site: EQ Tank Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 7.45 ug/L 2.5 50 EPA 245.1 10/25/2012 13:39 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 23.7 mg/L 0.5 10 EPA 200.7 10/24/2012 11:44 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 618 ug/L 10 10 EPA 200.8 10/23/2012 11:44 DJSULL1

Page 4 of 28
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12100090

2012021130

Collection Date: 17-Oct-12 12:23 PM

Site: EQ Tank Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 58.8 ug/L 10 10 EPA 200.8 10/25/2012 11:49 KRICHAR

Chromium (Cr) 69.9 ug/L 10 10 EPA 200.8 10/25/2012 11:49 KRICHAR

Copper (Cu) 74.2 ug/L 10 10 EPA 200.8 10/25/2012 11:49 KRICHAR

Nickel (Ni) 104 ug/L 10 10 EPA 200.8 10/25/2012 11:49 KRICHAR

Selenium (Se) 1030 ug/L 10 10 EPA 200.8 10/25/2012 11:49 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 10/25/2012 11:49 KRICHAR

Zinc (Zn) 102 ug/L 10 10 EPA 200.8 10/25/2012 11:49 KRICHAR

2012021131

Collection Date: 17-Oct-12 12:05 PM

Site: BioReactor 1 Inf 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 23.7 mg/L 0.5 10 EPA 200.7 10/24/2012 11:48 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 673 ug/L 10 10 EPA 200.8 10/23/2012 11:48 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 10/25/2012 11:52 KRICHAR

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 10/25/2012 11:52 KRICHAR

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 10/25/2012 11:52 KRICHAR

Nickel (Ni) < 10 ug/L 10 10 EPA 200.8 10/25/2012 11:52 KRICHAR

Selenium (Se) 714 ug/L 10 10 EPA 200.8 10/25/2012 11:52 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 10/25/2012 11:52 KRICHAR

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 10/25/2012 11:52 KRICHAR

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

Vendor Parameter Complete Vendor Method V_AS&C

2012021132

Collection Date: 17-Oct-12 12:11 PM

Site: BioReactor 2 Inf 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 28.8 mg/L 0.5 10 EPA 200.7 10/24/2012 11:52 DJSULL1

Page 5 of 28
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12100090

2012021132

Collection Date: 17-Oct-12 12:11 PM

Site: BioReactor 2 Inf 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 10/25/2012 11:56 KRICHAR

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 10/25/2012 11:56 KRICHAR

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 10/25/2012 11:56 KRICHAR

Nickel (Ni) < 10 ug/L 10 10 EPA 200.8 10/25/2012 11:56 KRICHAR

Selenium (Se) 20.3 ug/L 10 10 EPA 200.8 10/25/2012 11:56 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 10/25/2012 11:56 KRICHAR

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 10/25/2012 11:56 KRICHAR

2012021133

Collection Date: 17-Oct-12 12:18 PM

Site: BioReactor 2 Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

INORGANIC IONS BY IC

Bromide 360 mg/L 50 500 EPA 300.0 10/25/2012 11:32 BGN9034

Chloride 1100 mg/L 50 500 EPA 300.0 10/25/2012 11:32 BGN9034

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) < 1 ug/L 1 20 EPA 245.1 10/25/2012 13:41 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 32.4 mg/L 0.5 10 EPA 200.7 10/24/2012 11:56 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 5 ug/L 5 5 EPA 200.8 10/25/2012 11:59 KRICHAR

Chromium (Cr) < 5 ug/L 5 5 EPA 200.8 10/25/2012 11:59 KRICHAR

Copper (Cu) < 5 ug/L 5 5 EPA 200.8 10/25/2012 11:59 KRICHAR

Nickel (Ni) < 5 ug/L 5 5 EPA 200.8 10/25/2012 11:59 KRICHAR

Selenium (Se) 7.30 ug/L 5 5 EPA 200.8 10/25/2012 11:59 KRICHAR

Silver (Ag) < 5 ug/L 5 5 EPA 200.8 10/25/2012 11:59 KRICHAR

Zinc (Zn) < 5 ug/L 5 5 EPA 200.8 10/25/2012 11:59 KRICHAR

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

Vendor Parameter Complete Vendor Method V_AS&C

Page 6 of 28
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12100090

2012021134

Collection Date: 17-Oct-12 12:50 PM

Site: Filter Blk 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

DISSOLVED METALS BY ICP-MS

Selenium (Se) < 1 ug/L 1 1 EPA 200.8 10/23/2012 11:14 DJSULL1

2012021135

Collection Date: 03-Oct-12 11:15 AM

Site: TRIP BLANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

TOTAL RECOVERABLE METALS BY ICP

Boron (B) < 0.05 mg/L 0.05 1 EPA 200.7 10/24/2012 11:36 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 1 ug/L 1 1 EPA 200.8 10/25/2012 11:43 KRICHAR

Chromium (Cr) < 1 ug/L 1 1 EPA 200.8 10/25/2012 11:43 KRICHAR

Copper (Cu) < 1 ug/L 1 1 EPA 200.8 10/25/2012 11:43 KRICHAR

Nickel (Ni) < 1 ug/L 1 1 EPA 200.8 10/25/2012 11:43 KRICHAR

Selenium (Se) < 1 ug/L 1 1 EPA 200.8 10/25/2012 11:43 KRICHAR

Silver (Ag) < 1 ug/L 1 1 EPA 200.8 10/25/2012 11:43 KRICHAR

Zinc (Zn) < 1 ug/L 1 1 EPA 200.8 10/25/2012 11:43 KRICHAR

2012021137

Collection Date: 17-Oct-12 12:05 PM

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

2012021138

Collection Date: 17-Oct-12 12:05 PM

Site: Hg Blk 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

Page 7 of 28
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12100090

2012021139

Collection Date: 17-Oct-12 12:11 PM

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

2012021140

Collection Date: 17-Oct-12 12:11 PM

Site: Hg Blk 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

2012021141

Collection Date: 17-Oct-12 12:18 PM

Site: BioReactor 2 Eff 

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

2012021142

Collection Date: 17-Oct-12 12:18 PM

Site: Hg Blk BioReactor 2 Eff 

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

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 2, 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: J12100090 

Dear Mr. Perkins, 

On October 19, 2012, Brooks Rand Labs (BRL) received three (3) wastewater samples and 

three (3) corresponding field blanks. The samples were logged-in for total mercury (Hg) analysis 

according to the chain-of-custody form. All samples were received, prepared, analyzed, and 

stored according to BRL SOPs and EPA methodology. 

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

Two of the field blank samples yielded detectable results. However, the concentrations were 

less than the method defined control limit of 0.5 ng/L and the associated field sample results 

were more than 10x the level of the blank result. Contamination was considered insignificant. 

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 

Project Manager 

lydia@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 1242035-01 Influent Sample 10/17/2012 10/19/2012

Hg Blk BioReactor 1 Inf 1242035-02 DIW Field Blank 10/17/2012 10/19/2012

BioReactor 2 Inf 1242035-03 Influent QC Sample 10/17/2012 10/19/2012

Hg Blk BioReactor 2 Inf 1242035-04 DIW Field Blank 10/17/2012 10/19/2012

BioReactor 2 Eff 1242035-05 Effluent Sample 10/17/2012 10/19/2012

Hg Blk BioReactor 2 Eff 1242035-06 DIW Field Blank 10/17/2012 10/19/2012

Batch Summary

Analyte Lab Matrix Method Prepared Analyzed Batch Sequence

Hg Water EPA 1631 10/25/2012 10/26/2012 B121977 1200826

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

1242035-01 Hg Influent T 167 3.79 10.1 ng/L B121977 1200826

BioReactor 2 Eff

1242035-05 Hg Effluent T 61.9 0.38 1.01 ng/L B121977 1200826

BioReactor 2 Inf

1242035-03 Hg Influent T 98.3 0.79 2.11 ng/L B121977 1200826

Hg Blk BioReactor 1 Inf

1242035-02 Hg DIW T 0.17 B 0.15 0.41 ng/L B121977 1200826

Hg Blk BioReactor 2 Eff

1242035-06 Hg DIW T 0.18 B 0.15 0.40 ng/L B121977 1200826

Hg Blk BioReactor 2 Inf

1242035-04 Hg DIW T 0.16 U 0.16 0.41 ng/L B121977 1200826

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: B121977

Analyte Native Spike Result Units REC & Limits RPD & Limits

Method: EPA 1631

Lab Matrix: Water

Sample

B121977-SRM1 Certified Reference Material (1241042, NIST 1641d 1000x dilution)

Hg 15.68 15.98 ng/L 102% 85-115

B121977-MS1 Matrix Spike (1242035-03)

Hg 98.32 473.7 568.6 ng/L 99% 71-125

B121977-MSD1 Matrix Spike Duplicate (1242035-03)

Hg 98.32 473.7 572.4 ng/L 100% 71-125 240.7%

Method Blanks & Reporting Limits

Batch: B121977

Method: EPA 1631

Matrix: Water

Analyte: Hg

Sample Result Units

B121977-BLK1 0.24 ng/L

B121977-BLK2 0.23 ng/L

B121977-BLK3 0.20 ng/L

B121977-BLK4 0.18 ng/L

Average: 0.21 Standard Deviation: 0.03 MDL: 0.15

Limit: 0.50 Limit: 0.10 MRL: 0.39

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: 1200826

Instrument: THG-05 Method: EPA 1631

Date: 10/26/2012

Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg

Lab ID True Value Result Units REC & Limits

1200826-IBL1 0.72 pg of Hg

1200826-IBL2 2.01 pg of Hg

1200826-IBL3 2.09 pg of Hg

1200826-IBL4 2.05 pg of Hg

1200826-CAL1 10.00 10.10 pg of Hg 101%

1200826-CAL2 25.00 25.08 pg of Hg 100%

1200826-CAL3 100.0 100.7 pg of Hg 101%

1200826-CAL4 500.0 496.8 pg of Hg 99%

1200826-CAL5 2500 2501 pg of Hg 100%

1200826-CAL6 10000 9865 pg of Hg 99%

1200826-ICV1 1568 1598 pg of Hg 102% 85-115

1200826-CCB1 6.94 pg of Hg

1200826-CCV1 500.0 506.2 pg of Hg 101% 77-123

1200826-CCB2 3.77 pg of Hg

1200826-CCB3 2.87 pg of Hg

1200826-CCB4 2.99 pg of Hg

1200826-CCV2 500.0 517.5 pg of Hg 103% 77-123

1200826-CCB5 4.58 pg of Hg

1200826-CCV3 500.0 516.9 pg of Hg 103% 77-123

1200826-CCB6 2.92 pg of Hg

1200826-CCV4 500.0 512.9 pg of Hg 103% 77-123

1200826-CCB7 4.33 pg of Hg

1200826-CCV5 500.0 510.3 pg of Hg 102% 77-123

1200826-CCB8 5.33 pg of Hg

1200826-CCV6 500.0 488.1 pg of Hg 98% 77-123

1200826-CCB9 3.61 pg of Hg

1200826-CCV7 500.0 494.4 pg of Hg 99% 77-123

1200826-CCBA 2.95 pg of Hg

1200826-CCV8 500.0 494.7 pg of Hg 99% 77-123

1200826-CCBB 3.13 pg of Hg

1200826-CCV9 500.0 507.3 pg of Hg 101% 77-123

1200826-CCBC 6.01 pg of Hg

1200826-CCVA 500.0 515.0 pg of Hg 103% 77-123

1200826-CCBD 5.58 pg of Hg

1200826-CCVB 500.0 508.6 pg of Hg 102% 77-123

1200826-CCBE 4.18 pg of Hg

1200826-CCVC 500.0 511.3 pg of Hg 102% 77-123

1200826-CCBF 3.60 pg of Hg

1200826-CCVD 500.0 493.5 pg of Hg 99% 77-123

1200826-CCBG 3.20 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: 1200826

Instrument: THG-05 Method: EPA 1631

Date: 10/26/2012

Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg

Lab ID True Value Result Units REC & Limits

1200826-CCVE 500.0 510.7 pg of Hg 102% 77-123

1200826-CCBH 3.59 pg of Hg

1200826-CCVF 500.0 510.6 pg of Hg 102% 77-123

1200826-CCBI 2.91 pg of Hg

1200826-CCVG 500.0 509.2 pg of Hg 102% 77-123

1200826-CCBJ 4.65 pg of Hg

1200826-CCVH 500.0 511.4 pg of Hg 102% 77-123

1200826-CCBK 5.07 pg of Hg

1200826-CCVI 500.0 510.9 pg of Hg 102% 77-123

1200826-CCBL 3.02 pg of Hg

1200826-CCVJ 500.0 502.5 pg of Hg 100% 77-123

1200826-CCBM 3.43 pg of Hg

1200826-ICV2 1568 1624 pg of Hg 104% 85-115

1200826-CCVK 500.0 514.6 pg of Hg 103% 77-123

1200826-CCBN 3.78 pg of Hg

1200826-CCVL 500.0 513.1 pg of Hg 103% 77-123

1200826-CCBO 2.55 pg of Hg

1200826-CCVM 500.0 516.1 pg of Hg 103% 77-123

1200826-CCBP 2.78 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: 1242035-01 Report Matrix: Influent

Sample: BioReactor 1 Inf Sample Type: Sample Received: 10/19/2012

Collected: 10/17/2012

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: 1242035-02 Report Matrix: DIW

Sample: Hg Blk BioReactor 1 Inf Sample Type: Field Blank Received: 10/19/2012

Collected: 10/17/2012

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: 1242035-03 Report Matrix: Influent

Sample: BioReactor 2 Inf Sample Type: QC Sample Received: 10/19/2012

Collected: 10/17/2012

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: 1242035-04 Report Matrix: DIW

Sample: Hg Blk BioReactor 2 Inf Sample Type: Field Blank Received: 10/19/2012

Collected: 10/17/2012

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: 1242035-05 Report Matrix: Effluent

Sample: BioReactor 2 Eff Sample Type: Sample Received: 10/19/2012

Collected: 10/17/2012

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: 1242035-06 Report Matrix: DIW

Sample: Hg Blk BioReactor 2 Eff Sample Type: Field Blank Received: 10/19/2012

Collected: 10/17/2012

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 16 of 28
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Shipping Containers

Cooler

Tracking No: 7992 2521 0993 via FedEx

Temperature: 1.8 °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 19, 2012 9:45

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
Page 18 of 28
 

October 26, 2012 

Jay Perkins 

Duke Energy Analytical Laboratory 

Mail Code MGO3A2 (Building 7405) 

13339 Hagers Ferry Rd. 

Huntersville, NC 28078 

(704) 875-5245 

Project: Allen - FGD WWTS (2010, Bi-Monthly Sampling) (LIMS #J12100090)

Dear Mr. Perkins, 

Attached is the report associated with three (3) aqueous samples submitted for selenium 

speciation analysis on October 18, 2012. The samples were received in a sealed cooler at 9.4°C 

on October 19, 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 19 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: Allen - FGD WWTS (2010, Bi-Monthly Sampling) (LIMS #J12100090) 

October 26, 2012 

1. Sample Reception 

Three (3) aqueous samples in 125mL HDPE bottles (provided by Applied Speciation and 

Consulting) were submitted for selenium speciation analysis on October 18, 2012. The 

samples were received on October 19, 2012 in a sealed container at 9.4°C. 

Applied Speciation and Consulting strongly recommends that all samples submitted for 

selenium speciation remain at a temperature of ≤6°C to maintain sample integrity prior to 

analysis. 

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. 

Page 20 of 28
3. Sample Analysis 

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

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

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

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

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

analytical platform. 

Prior to sample analysis, all calibration curves are verified using second source 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 October 25, 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 21 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 22 of 28
Sample Results

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

Unknown Se 

Species (n)

FGD Purge Eff 547 324 26.2 ND (<1.4) ND (<1.4) 17.8 (2)

BioReactor 1 Inf ND (<0.34) ND (<0.51) ND (<0.23) ND (<0.36) ND (<0.36) 0.0 (0)

BioReactor 2 Eff 19.2 531 ND (<0.23) 0.80 ND (<0.36) 0.62 (1)

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

ND = Not detected at the applied dilution

SeCN = Selenocyanate

MeSe(IV) = Methylseleninic acid

SeMe = Selenomethionine

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

Report Generated by: Russell Gerads

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Allen - FGD WWTS (2010, Bi-Monthly Sampling)

Contact: Jay Perkins

Date: October 26, 2012

LIMS #J12100090

Page 23 of 28
Quality Control Summary - Preparation Blank Summary

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

Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.34 1.4

Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.51 2.0

SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.23 0.93

MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.36 1.4

SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.36 1.4

eMDL = Estimated Method Detection Limit

*Please see narrative regarding eMDL calculations

Quality Control Summary - Certified Reference Materials

Analyte (μg/L) CRM True Value Result Recovery

Se(IV) LCS 9.57 9.62 100.5

Se(VI) LCS 9.48 9.18 96.8

SeCN LCS 8.92 8.95 100.3

MeSe(IV) LCS 6.47 6.75 104.3

SeMe LCS 9.32 8.32 89.3

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Allen - FGD WWTS (2010, Bi-Monthly Sampling)

Contact: Jay Perkins

LIMS #J12100090

Date: October 26, 2012

Report Generated by: Russell Gerads

Page 24 of 28
Quality Control Summary - Matrix Duplicates

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

Se(IV) BioReactor 2 Eff 19.24 18.58 18.91 3.5

Se(VI) BioReactor 2 Eff 530.9 527.7 529.3 0.6

SeCN BioReactor 2 Eff ND (<0.23) ND (<0.23) NC NC

MeSe(IV) BioReactor 2 Eff 0.80 0.79 0.79 1.7

SeMe BioReactor 2 Eff ND (<0.36) ND (<0.36) 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) BioReactor 2 Eff 1390 1522 108.1 1390 1527 108.5 0.4

Se(VI) BioReactor 2 Eff 1261 1720 94.4 1261 1719 94.3 0.0

SeCN BioReactor 2 Eff 1144 1011 88.4 1144 1003 87.7 0.8

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Allen - FGD WWTS (2010, Bi-Monthly Sampling)

Contact: Jay Perkins

LIMS #J12100090

Date: October 26, 2012

Report Generated by: Russell Gerads

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