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: J13030193

Project Name: WWTS - Biweekly (2)

Lab Contact: Jason C Perkins

Date: 3/28/2013

Customer Address: 253 Plant Allen Road

Customer Name(s): Bill K., Ron L., Don S., Ray L.

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. 

Jason C Perkins

Page 1 of 28
Sample ID's & Descriptions:

Sample ID Plant/Station

Collection 

Date and Time Collected By Sample Description

2013005716 ALLEN 08-Mar-13 6:37 AM C. MCHUGH FGD Purge Eff 

2013005717 ALLEN 08-Mar-13 6:40 AM C. MCHUGH EQ Tank Eff 

2013005718 ALLEN 08-Mar-13 6:44 AM C. MCHUGH BioReactor 1 Inf 

2013005719 ALLEN 08-Mar-13 6:55 AM C. MCHUGH BioReactor 2 Inf 

2013005720 ALLEN 08-Mar-13 6:50 AM C. MCHUGH BioReactor 2 Eff 

2013005721 ALLEN 08-Mar-13 8:20 AM C. MCHUGH Filter Blk 

2013005722 ALLEN 18-Dec-13 9:00 AM C. KNOX TRIP BLANK 

2013005723 ALLEN 08-Mar-13 7:20 AM C. MCHUGH HG BioReactor 1 Inf 

2013005724 ALLEN 08-Mar-13 7:20 AM C. MCHUGH Hg Blk BioReactor 1 Inf 

2013005725 ALLEN 08-Mar-13 7:27 AM C. MCHUGH Hg BioReactor 2 Inf 

2013005726 ALLEN 08-Mar-13 7:27 AM C. MCHUGH Hg Blk BioReactor 2 Inf 

2013005727 ALLEN 08-Mar-13 7:24 AM C. MCHUGH Hg BioReactor 2 Eff 

2013005728 ALLEN 08-Mar-13 7:24 AM C. MCHUGH 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: 3/28/2013

Electronic Data Deliverable (EDD) Sent Separately

Page 3 of 28
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13030193

2013005716

Collection Date: 08-Mar-13 6:37 AM

Site: FGD Purge Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

INORGANIC IONS BY IC

Bromide 720 mg/L 10 100 EPA 300.0 03/25/2013 08:12 BGN9034

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 39.1 ug/L 2.5 50 EPA 245.1 03/21/2013 13:14 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 84.2 mg/L 0.5 10 EPA 200.7 03/19/2013 13:19 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 3760 ug/L 10 10 EPA 200.8 03/22/2013 12:18 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 192 ug/L 10 10 EPA 200.8 03/19/2013 11:31 KRICHAR

Chromium (Cr) 151 ug/L 10 10 EPA 200.8 03/19/2013 11:31 KRICHAR

Copper (Cu) 191 ug/L 10 10 EPA 200.8 03/19/2013 11:31 KRICHAR

Nickel (Ni) 218 ug/L 10 10 EPA 200.8 03/19/2013 11:31 KRICHAR

Selenium (Se) 10600 ug/L 50 50 EPA 200.8 03/19/2013 11:31 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 03/19/2013 11:31 KRICHAR

Zinc (Zn) 262 ug/L 10 10 EPA 200.8 03/19/2013 11:31 KRICHAR

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

Vendor Parameter Complete Vendor Method V_AS&C

TOTAL DISSOLVED SOLIDS

TDS 8200 mg/L 200 1 SM2540C 03/19/2013 15:35 SWILLI3

2013005717

Collection Date: 08-Mar-13 6:40 AM

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) 35.1 ug/L 2.5 50 EPA 245.1 03/21/2013 13:17 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 90.5 mg/L 0.5 10 EPA 200.7 03/19/2013 13:23 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 4300 ug/L 10 10 EPA 200.8 03/22/2013 12:21 KRICHAR

Page 4 of 28
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13030193

2013005717

Collection Date: 08-Mar-13 6:40 AM

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) 166 ug/L 10 10 EPA 200.8 03/19/2013 11:35 KRICHAR

Chromium (Cr) 126 ug/L 10 10 EPA 200.8 03/19/2013 11:35 KRICHAR

Copper (Cu) 161 ug/L 10 10 EPA 200.8 03/19/2013 11:35 KRICHAR

Nickel (Ni) 192 ug/L 10 10 EPA 200.8 03/19/2013 11:35 KRICHAR

Selenium (Se) 9930 ug/L 50 50 EPA 200.8 03/19/2013 11:35 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 03/19/2013 11:35 KRICHAR

Zinc (Zn) 227 ug/L 10 10 EPA 200.8 03/19/2013 11:35 KRICHAR

2013005718

Collection Date: 08-Mar-13 6:44 AM

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) 120 mg/L 0.5 10 EPA 200.7 03/19/2013 13:27 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 3750 ug/L 10 10 EPA 200.8 03/22/2013 12:25 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 03/19/2013 11:38 KRICHAR

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 03/19/2013 11:38 KRICHAR

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 03/19/2013 11:38 KRICHAR

Nickel (Ni) < 10 ug/L 10 10 EPA 200.8 03/19/2013 11:38 KRICHAR

Selenium (Se) 3980 ug/L 10 10 EPA 200.8 03/19/2013 11:38 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 03/19/2013 11:38 KRICHAR

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 03/19/2013 11:38 KRICHAR

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

Vendor Parameter Complete Vendor Method V_AS&C

2013005719

Collection Date: 08-Mar-13 6:55 AM

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) 153 mg/L 0.5 10 EPA 200.7 03/19/2013 13:31 MHH7131

Page 5 of 28
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13030193

2013005719

Collection Date: 08-Mar-13 6:55 AM

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 03/19/2013 11:42 KRICHAR

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 03/19/2013 11:42 KRICHAR

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 03/19/2013 11:42 KRICHAR

Nickel (Ni) < 10 ug/L 10 10 EPA 200.8 03/19/2013 11:42 KRICHAR

Selenium (Se) 120 ug/L 10 10 EPA 200.8 03/19/2013 11:42 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 03/19/2013 11:42 KRICHAR

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 03/19/2013 11:42 KRICHAR

2013005720

Collection Date: 08-Mar-13 6:50 AM

Site: BioReactor 2 Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

INORGANIC IONS BY IC

Bromide 210 mg/L 5 50 EPA 300.0 03/22/2013 15:29 BGN9034

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) < 1 ug/L 1 20 EPA 245.1 03/21/2013 13:19 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 215 mg/L 0.5 10 EPA 200.7 03/19/2013 13:35 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 5 ug/L 5 5 EPA 200.8 03/19/2013 11:45 KRICHAR

Chromium (Cr) < 5 ug/L 5 5 EPA 200.8 03/19/2013 11:45 KRICHAR

Copper (Cu) < 5 ug/L 5 5 EPA 200.8 03/19/2013 11:45 KRICHAR

Nickel (Ni) < 5 ug/L 5 5 EPA 200.8 03/19/2013 11:45 KRICHAR

Selenium (Se) < 5 ug/L 5 5 EPA 200.8 03/19/2013 11:45 KRICHAR

Silver (Ag) < 5 ug/L 5 5 EPA 200.8 03/19/2013 11:45 KRICHAR

Zinc (Zn) < 5 ug/L 5 5 EPA 200.8 03/19/2013 11:45 KRICHAR

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

Vendor Parameter Complete Vendor Method V_AS&C

2013005721

Collection Date: 08-Mar-13 8:20 AM

Site: Filter Blk 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

DISSOLVED METALS BY ICP-MS

Selenium (Se) 1.70 ug/L 1 1 EPA 200.8 03/22/2013 11:59 KRICHAR

Page 6 of 28
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13030193

2013005722

Collection Date: 18-Dec-13 9:00 AM

Site: TRIP BLANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

TOTAL RECOVERABLE METALS BY ICP

Boron (B) < 0.05 mg/L 0.05 1 EPA 200.7 03/19/2013 12:52 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 1 ug/L 1 1 EPA 200.8 03/19/2013 11:07 KRICHAR

Chromium (Cr) < 1 ug/L 1 1 EPA 200.8 03/19/2013 11:07 KRICHAR

Copper (Cu) < 1 ug/L 1 1 EPA 200.8 03/19/2013 11:07 KRICHAR

Nickel (Ni) < 1 ug/L 1 1 EPA 200.8 03/19/2013 11:07 KRICHAR

Selenium (Se) < 1 ug/L 1 1 EPA 200.8 03/19/2013 11:07 KRICHAR

Silver (Ag) < 1 ug/L 1 1 EPA 200.8 03/19/2013 11:07 KRICHAR

Zinc (Zn) < 1 ug/L 1 1 EPA 200.8 03/19/2013 11:07 KRICHAR

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

Vendor Parameter Complete Vendor Method V_AS&C

2013005723

Collection Date: 08-Mar-13 7:20 AM

Site: HG 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

2013005724

Collection Date: 08-Mar-13 7:20 AM

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

2013005725

Collection Date: 08-Mar-13 7:27 AM

Site: Hg 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

Page 7 of 28
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13030193

2013005726

Collection Date: 08-Mar-13 7:27 AM

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

2013005727

Collection Date: 08-Mar-13 7:24 AM

Site: Hg 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

2013005728

Collection Date: 08-Mar-13 7:24 AM

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

March 27, 2013

Duke Energy

ATTN: Jay Perkins

Scientific Support-Laboratory

13339 Hagers Ferry Road

Huntersville NC 28078

jcperkins@duke-energy.com

labcustomer@duke-energy.com

RE: Project DUK-HV1201 Client Project: J13030193

Dear Mr. Perkins,

On March 15, 2013, Brooks Rand Labs (BRL) received three (3) waste water samples and three 

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

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

methodology.

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

All field blanks yielded detectable results; however, all results were less than the method 

defined control limit of 0.5 ng/L and were considered insignificant sources of contamination. All 

data was reported without further 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,

 

 

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 1311019-01 Influent Sample 03/08/2013 03/15/2013

Hg Blk BioReactor 1 Inf 1311019-02 DIW Field Blank 03/08/2013 03/15/2013

BioReactor 2 Inf 1311019-03 Influent Sample 03/08/2013 03/15/2013

Hg Blk BioReactor 2 Inf 1311019-04 DIW Field Blank 03/08/2013 03/15/2013

BioReactor 2 Eff 1311019-05 Effluent Sample 03/08/2013 03/15/2013

Hg Blk BioReactor 2 Eff 1311019-06 DIW Field Blank 03/08/2013 03/15/2013

Batch Summary

Analyte Lab Matrix Method Prepared Analyzed Batch Sequence

Hg Water EPA 1631 03/18/2013 03/20/2013 B130434 1300194

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

1311019-01 Hg Influent T 433 0.77 2.04 ng/L B130434 1300194

BioReactor 2 Eff

1311019-05 Hg Effluent T 20.8 0.15 0.41 ng/L B130434 1300194

BioReactor 2 Inf

1311019-03 Hg Influent T 96.0 0.15 0.41 ng/L B130434 1300194

Hg Blk BioReactor 1 Inf

1311019-02 Hg DIW T 0.42 0.15 0.40 ng/L B130434 1300194

Hg Blk BioReactor 2 Eff

1311019-06 Hg DIW T 0.40 B 0.15 0.41 ng/L B130434 1300194

Hg Blk BioReactor 2 Inf

1311019-04 Hg DIW T 0.37 B 0.15 0.40 ng/L B130434 1300194

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: B130434

Analyte Native Spike Result Units REC & Limits RPD & Limits

Method: EPA 1631

Lab Matrix: Water

Sample

B130434-SRM1 Certified Reference Material (1310011, NIST 1641d 1000x dilution)

Hg 15.68 15.58 ng/L 99% 75-125

B130434-MS2 Matrix Spike (1311004-01)

Hg 221.2 1263 1318 ng/L 87% 71-125

B130434-MSD2 Matrix Spike Duplicate (1311004-01)

Hg 221.2 1263 1415 ng/L 95% 71-125 247%

Method Blanks & Reporting Limits

Batch: B130434

Method: EPA 1631

Matrix: Water

Analyte: Hg

Sample Result Units

B130434-BLK1 0.21 ng/L

B130434-BLK2 0.22 ng/L

B130434-BLK3 0.33 ng/L

B130434-BLK4 0.20 ng/L

Average: 0.24 Standard Deviation: 0.06 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: 1300194

Instrument: THG-06 Method: EPA 1631

Date: 03/20/2013

Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg

Lab ID True Value Result Units REC & Limits

1300194-IBL1 3.23 pg of Hg

1300194-IBL2 3.95 pg of Hg

1300194-IBL3 5.38 pg of Hg

1300194-IBL4 5.99 pg of Hg

1300194-CAL1 10.00 11.55 pg of Hg 115%

1300194-CAL2 25.00 25.16 pg of Hg 101%

1300194-CAL3 100.0 99.72 pg of Hg 100%

1300194-CAL4 500.0 481.8 pg of Hg 96%

1300194-CAL5 2500 2434 pg of Hg 97%

1300194-CAL6 10000 9322 pg of Hg 93%

1300194-ICV1 1568 1558 pg of Hg 99% 85-115

1300194-CCB1 8.06 pg of Hg

1300194-CCV1 500.0 498.4 pg of Hg 100% 77-123

1300194-CCB2 7.41 pg of Hg

1300194-CCB3 7.66 pg of Hg

1300194-CCB4 7.23 pg of Hg

1300194-CCV2 500.0 496.2 pg of Hg 99% 77-123

1300194-CCB5 6.78 pg of Hg

1300194-CCV3 500.0 496.0 pg of Hg 99% 77-123

1300194-CCB6 6.96 pg of Hg

1300194-CCV4 500.0 494.8 pg of Hg 99% 77-123

1300194-CCB7 7.24 pg of Hg

1300194-CCV5 500.0 498.3 pg of Hg 100% 77-123

1300194-CCB8 6.79 pg of Hg

1300194-CCV6 500.0 484.5 pg of Hg 97% 77-123

1300194-CCB9 6.49 pg of Hg

1300194-CCV7 500.0 476.7 pg of Hg 95% 77-123

1300194-CCBA 5.77 pg of Hg

1300194-CCV8 500.0 481.0 pg of Hg 96% 77-123

1300194-CCBB 6.21 pg of Hg

1300194-CCV9 500.0 479.0 pg of Hg 96% 77-123

1300194-CCBC 6.14 pg of Hg

1300194-CCVA 500.0 481.4 pg of Hg 96% 77-123

1300194-CCBD 5.75 pg of Hg

1300194-CCVB 500.0 479.2 pg of Hg 96% 77-123

1300194-CCBE 6.15 pg of Hg

1300194-CCVC 500.0 472.7 pg of Hg 95% 77-123

1300194-CCBF 6.26 pg of Hg

1300194-CCVD 500.0 475.0 pg of Hg 95% 77-123

1300194-CCBG 6.13 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: 1300194

Instrument: THG-06 Method: EPA 1631

Date: 03/20/2013

Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg

Lab ID True Value Result Units REC & Limits

1300194-CCVE 500.0 474.8 pg of Hg 95% 77-123

1300194-CCBH 5.59 pg of Hg

1300194-CCVF 500.0 482.9 pg of Hg 97% 77-123

1300194-CCBI 5.63 pg of Hg

1300194-CCVG 500.0 479.3 pg of Hg 96% 77-123

1300194-CCBJ 5.51 pg of Hg

1300194-CCVH 500.0 494.4 pg of Hg 99% 77-123

1300194-CCBK 6.08 pg of Hg

1300194-CCVI 500.0 498.7 pg of Hg 100% 77-123

1300194-CCBL 7.30 pg of Hg

1300194-CCVJ 500.0 496.1 pg of Hg 99% 77-123

1300194-CCBM 5.76 pg of Hg

1300194-CCVK 500.0 494.3 pg of Hg 99% 77-123

1300194-CCBN 6.17 pg of Hg

1300194-CCVL 500.0 486.1 pg of Hg 97% 77-123

1300194-CCBO 6.11 pg of Hg

1300194-CCVM 500.0 493.1 pg of Hg 99% 77-123

1300194-CCBP 5.92 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: 1311019-01 Report Matrix: Influent

Sample: BioReactor 1 Inf Sample Type: Sample Received: 03/15/2013

Collected: 03/08/2013

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

A 71691270

10

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

Lab ID: 1311019-02 Report Matrix: DIW

Sample: Hg Blk BioReactor 1 Inf Sample Type: Field Blank Received: 03/15/2013

Collected: 03/08/2013

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

A 71691270

10

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

Lab ID: 1311019-03 Report Matrix: Influent

Sample: BioReactor 2 Inf Sample Type: Sample Received: 03/15/2013

Collected: 03/08/2013

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

A 71691270

10

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

Lab ID: 1311019-04 Report Matrix: DIW

Sample: Hg Blk BioReactor 2 Inf Sample Type: Field Blank Received: 03/15/2013

Collected: 03/08/2013

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

A 71691270

10

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

Lab ID: 1311019-05 Report Matrix: Effluent

Sample: BioReactor 2 Eff Sample Type: Sample Received: 03/15/2013

Collected: 03/08/2013

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

A 71691270

10

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

Lab ID: 1311019-06 Report Matrix: DIW

Sample: Hg Blk BioReactor 2 Eff Sample Type: Field Blank Received: 03/15/2013

Collected: 03/08/2013

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

A 71691270

10

Bottle FLPE Hg-T 250mL 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: 557566432441 via FedEx

Temperature: -0.5 °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: March 15, 2013 8:50

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
 

March 21, 2013 

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 #J13030193) 

Dear Mr. Perkins, 

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

speciation on March 14, 2013. The samples were received in a sealed cooler at -0.5°C on March 

15, 2013. 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 #J13030193) 

March 21, 2013 

1. Sample Reception 

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

Consulting) were submitted for selenium speciation analysis on March 14, 2013. The 

samples were received on March 15, 2013 in a sealed container at -0.5°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 20 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 March 16, 2013. 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 4170 1560 217 ND (< 3.0) ND (< 3.0) 117 (3)

BioReactor 1 Inf 1440 1560 120 3.83 ND (< 0.75) 85.6 (3)

BioReactor 2 Eff 1.26 ND (<1.1) ND (< 0.60) ND (< 0.75) ND (< 0.75) 0.0 (0)

Metals Trip Blk ND (< 0.023) ND (< 0.043) ND (< 0.024) ND (< 0.030) ND (< 0.030) 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: Allen - FGD WWTS (2010, Bi-Monthly Sampling)

Contact: Jay Perkins

Date: March 21, 2013

LIMS #J13030193

Page 23 of 28
Quality Control Summary - Preparation Blank Summary

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

Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.023 0.57 2.3

Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.043 1.1 4.3

SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.024 0.60 2.4

MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.003 0.030 0.75 3.0

SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.003 0.030 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 9.123 95.3

Se(VI) LCS 9.48 8.707 91.8

SeCN LCS 8.92 8.484 95.1

MeSe(IV) LCS 6.47 6.152 95.1

SeMe LCS 9.32 8.709 93.4

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

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

Contact: Jay Perkins

LIMS #J13030193

Date: March 21, 2013

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) Batch QC ND (< 2.3) ND (< 2.3) NC NC

Se(VI) Batch QC 458.6 434.9 446.7 5.3

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

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 5560 5287 95.1 5560 5194 93.4 1.8

Se(VI) Batch QC 5045 5127 92.8 5045 5116 92.6 0.2

SeCN Batch QC 4575 4252 92.9 4575 4158 90.9 2.2

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

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

Contact: Jay Perkins

LIMS #J13030193

Date: March 21, 2013

Report Generated by: Russell Gerads

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