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: J11120225

Lab Contact: Jason C Perkins

Date: 12/28/2011

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.

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 26
Sample ID's & Descriptions:

Sample ID Plant/Station

Collection 

Date and Time Collected By Sample Description

2011026739 ALLEN 12-Dec-11 4:47 AM BILL HASKINS FGD Purge Eff 

2011026740 ALLEN 12-Dec-11 8:46 AM Jeremy D. EQ Tank Eff 

2011026741 ALLEN 12-Dec-11 8:38 AM Jeremy D. BioReactor 1 Inf 

2011026742 ALLEN 12-Dec-11 2:43 PM JBW BioReactor 1 Inf BLANK 

2011026743 ALLEN 12-Dec-11 8:22 AM Jeremy D. BioReactor 2 Inf 

2011026744 ALLEN 12-Dec-11 2:49 PM JBW BioReactor 2 Inf BLANK 

2011026745 ALLEN 12-Dec-11 8:29 AM Jeremy D. BioReactor 2 Eff 

2011026746 ALLEN 12-Dec-11 2:45 PM JBW BioReactor 2 Eff BLANK 

2011026747 ALLEN 12-Dec-11 10:20 AM Jeremy D. Filter Blk 

9 Total Samples

Page 2 of 26
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.

The Vendor Laboratories have been qualified by the 

Analytical Laboratory

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: DataBase Administrator Date: 12/28/2011

Yes

Electronic Data Deliverable (EDD) Sent Separately

Page 3 of 26
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11120225

2011026739

Collection Date: 12-Dec-11 4:47 AM

Site: FGD Purge Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

INORGANIC IONS BY IC

Bromide 58 mg/L EPA 300.0 5 14-Dec-11 16:09 JAHERMA

Chloride 2500 mg/L 50 EPA 300.0 14-Dec-11 16:09 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 170 ug/L EPA 245.1 2.5 16-Dec-11 09:49 AGIBBS

Mercury Dissolved (cold vapor) in Water (Filtered)

Mercury (Hg) 89.1 ug/L EPA 245.1 2.5 16-Dec-11 10:46 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 251 mg/L EPA 200.7 0.5 16-Dec-11 10:56 DJSULL1

Manganese (Mn) 5.15 mg/L 0.05 EPA 200.7 16-Dec-11 10:56 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 2450 ug/L EPA 200.8 10 20-Dec-11 10:55 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 189 ug/L EPA 200.8 10 21-Dec-11 09:55 MHH7131

Chromium (Cr) 260 ug/L 10 EPA 200.8 21-Dec-11 09:55 MHH7131

Copper (Cu) 172 ug/L 10 EPA 200.8 21-Dec-11 09:55 MHH7131

Nickel (Ni) 298 ug/L 10 EPA 200.8 21-Dec-11 09:55 MHH7131

Selenium (Se) 2290 ug/L 10 EPA 200.8 21-Dec-11 09:55 MHH7131

Silver (Ag) < 10.0 ug/L 10 EPA 200.8 21-Dec-11 09:55 MHH7131

Zinc (Zn) 261 ug/L 20 EPA 200.8 21-Dec-11 09:55 MHH7131

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

TOTAL DISSOLVED SOLIDS

TDS 11000 mg/L SM2540C 200 13-Dec-11 16:09 TJA7067

2011026740

Collection Date: 12-Dec-11 8:46 AM

Site: EQ Tank Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

INORGANIC IONS BY IC

Bromide 72 mg/L EPA 300.0 5 14-Dec-11 16:25 JAHERMA

Chloride 2200 mg/L 50 EPA 300.0 14-Dec-11 16:25 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 129 ug/L EPA 245.1 2.5 16-Dec-11 10:03 AGIBBS

Page 4 of 26
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11120225

2011026740

Collection Date: 12-Dec-11 8:46 AM

Site: EQ Tank Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 185 mg/L EPA 200.7 0.5 16-Dec-11 11:00 DJSULL1

Manganese (Mn) 4.07 mg/L 0.05 EPA 200.7 16-Dec-11 11:00 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 2240 ug/L EPA 200.8 10 20-Dec-11 10:55 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 173 ug/L EPA 200.8 10 21-Dec-11 09:55 MHH7131

Chromium (Cr) 214 ug/L 10 EPA 200.8 21-Dec-11 09:55 MHH7131

Copper (Cu) 156 ug/L 10 EPA 200.8 21-Dec-11 09:55 MHH7131

Nickel (Ni) 249 ug/L 10 EPA 200.8 21-Dec-11 09:55 MHH7131

Selenium (Se) 1950 ug/L 10 EPA 200.8 21-Dec-11 09:55 MHH7131

Silver (Ag) < 10.0 ug/L 10 EPA 200.8 21-Dec-11 09:55 MHH7131

Zinc (Zn) 245 ug/L 20 EPA 200.8 21-Dec-11 09:55 MHH7131

2011026741

Collection Date: 12-Dec-11 8:38 AM

Site: BioReactor 1 Inf 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

INORGANIC IONS BY IC

Bromide 88 mg/L EPA 300.0 5 14-Dec-11 16:40 JAHERMA

Chloride 2100 mg/L 50 EPA 300.0 14-Dec-11 16:40 JAHERMA

MERCURY 1631

Vendor Parameter Complete V_BRAND

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 134 mg/L EPA 200.7 0.5 16-Dec-11 11:04 DJSULL1

Manganese (Mn) < 0.050 mg/L 0.05 EPA 200.7 16-Dec-11 11:04 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 1700 ug/L EPA 200.8 10 20-Dec-11 10:55 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10.0 ug/L EPA 200.8 10 21-Dec-11 09:55 MHH7131

Chromium (Cr) 48.8 ug/L 10 EPA 200.8 21-Dec-11 09:55 MHH7131

Copper (Cu) < 10.0 ug/L 10 EPA 200.8 21-Dec-11 09:55 MHH7131

Nickel (Ni) < 10.0 ug/L 10 EPA 200.8 21-Dec-11 09:55 MHH7131

Selenium (Se) 1580 ug/L 10 EPA 200.8 21-Dec-11 09:55 MHH7131

Silver (Ag) < 10.0 ug/L 10 EPA 200.8 21-Dec-11 09:55 MHH7131

Zinc (Zn) < 20.0 ug/L 20 EPA 200.8 21-Dec-11 09:55 MHH7131

Page 5 of 26
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11120225

2011026741

Collection Date: 12-Dec-11 8:38 AM

Site: BioReactor 1 Inf 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2011026742

Collection Date: 12-Dec-11 2:43 PM

Site: BioReactor 1 Inf BLANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY 1631

Vendor Parameter Complete V_BRAND

2011026743

Collection Date: 12-Dec-11 8:22 AM

Site: BioReactor 2 Inf 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

INORGANIC IONS BY IC

Bromide 85 mg/L EPA 300.0 5 14-Dec-11 16:56 JAHERMA

Chloride 2000 mg/L 50 EPA 300.0 14-Dec-11 16:56 JAHERMA

MERCURY 1631

Vendor Parameter Complete V_BRAND

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 117 mg/L EPA 200.7 0.5 16-Dec-11 11:08 DJSULL1

Manganese (Mn) 0.158 mg/L 0.05 EPA 200.7 16-Dec-11 11:08 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 11.9 ug/L EPA 200.8 10 21-Dec-11 09:55 MHH7131

Chromium (Cr) < 10.0 ug/L 10 EPA 200.8 21-Dec-11 09:55 MHH7131

Copper (Cu) < 10.0 ug/L 10 EPA 200.8 21-Dec-11 09:55 MHH7131

Nickel (Ni) < 10.0 ug/L 10 EPA 200.8 21-Dec-11 09:55 MHH7131

Selenium (Se) 675 ug/L 10 EPA 200.8 21-Dec-11 09:55 MHH7131

Silver (Ag) < 10.0 ug/L 10 EPA 200.8 21-Dec-11 09:55 MHH7131

Zinc (Zn) < 20.0 ug/L 20 EPA 200.8 21-Dec-11 09:55 MHH7131

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

Page 6 of 26
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11120225

2011026744

Collection Date: 12-Dec-11 2:49 PM

Site: BioReactor 2 Inf BLANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY 1631

Vendor Parameter Complete V_BRAND

2011026745

Collection Date: 12-Dec-11 8:29 AM

Site: BioReactor 2 Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

INORGANIC IONS BY IC

Bromide 120 mg/L EPA 300.0 5 14-Dec-11 17:12 JAHERMA

Chloride 2100 mg/L 50 EPA 300.0 14-Dec-11 17:12 JAHERMA

MERCURY 1631

Vendor Parameter Complete V_BRAND

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 97.8 mg/L EPA 200.7 0.5 16-Dec-11 11:23 DJSULL1

Manganese (Mn) 0.364 mg/L 0.05 EPA 200.7 16-Dec-11 11:23 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 5.00 ug/L EPA 200.8 5 21-Dec-11 09:55 MHH7131

Chromium (Cr) < 5.00 ug/L 5 EPA 200.8 21-Dec-11 09:55 MHH7131

Copper (Cu) < 5.00 ug/L 5 EPA 200.8 21-Dec-11 09:55 MHH7131

Nickel (Ni) < 5.00 ug/L 5 EPA 200.8 21-Dec-11 09:55 MHH7131

Selenium (Se) 9.89 ug/L 5 EPA 200.8 21-Dec-11 09:55 MHH7131

Silver (Ag) < 5.00 ug/L 5 EPA 200.8 21-Dec-11 09:55 MHH7131

Zinc (Zn) < 10.0 ug/L 10 EPA 200.8 21-Dec-11 09:55 MHH7131

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2011026746

Collection Date: 12-Dec-11 2:45 PM

Site: BioReactor 2 Eff BLANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY 1631

Vendor Parameter Complete V_BRAND

Page 7 of 26
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11120225

2011026747

Collection Date: 12-Dec-11 10:20 AM

Site: Filter Blk 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

Mercury Dissolved (cold vapor) in Water (Filtered)

Mercury (Hg) < 2.50 ug/L EPA 245.1 2.5 16-Dec-11 10:48 AGIBBS

DISSOLVED METALS BY ICP-MS

Selenium (Se) < 1.000 ug/L EPA 200.8 1 20-Dec-11 10:39 MHH7131

Page 8 of 26
 

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

December 27, 2011 

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-HV1101 Client Project: J11120225 

Dear Mr. Perkins, 

On December 15, 2011, Brooks Rand Labs (BRL) received three (3) waste water samples and 

three (3) corresponding field blanks. 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 applicable 

SOP(s) and may be evaluated using adjusted reporting limits to account for sample aliquot size. 

Please refer to the Sample Results page for sample-specific detection limits and other details. 

The limits of the calibration were exceeded several times by the analysis of samples from an 

unrelated work order. As part of the corrective action, BRL analyzed multiple continuing 

calibration blanks to ensure carryover contamination did not impact sample analysis. All 

samples reported from this work order (1151018) were analyzed prior to the analysis of high 

level samples. 

The analysis of samples BioReactor 1 Inf Hg Blk produced detectable results at 0.17 ng/L. The 

concentration was less than the method defined control limit of 0.50 ng/L and not a significant 

source of contamination. Aside from concentration qualifiers, all data was reported without 

further qualification and all associated quality control sample results met the acceptance criteria. 

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

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

page of the report. 

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

Sincerely, 

 

Tiffany Stilwater 

Project Manager 

tiffany@brooksrand.com 

Page 9 of 26
Project ID: DUK-HV1101

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, Ltd., those found in the EPA SOW ILM03.0, 

Exhibit B, Section III, pg. B-18, and the USEPA Laboratory Data Validation Functional Guidelines for Evaluating Inorganic 

Analyses; USEPA; July 2002. 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 26
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Sample Information

Sample Lab ID Report Matrix Type Sampled Received

BioReactor 1 Inf 1151018-01 Influent Sample 12/12/2011 12/15/2011

BioReactor 1 Inf Hg Blk 1151018-02 DIW Field Blank 12/12/2011 12/15/2011

BioReactor 2 Inf 1151018-03 Influent Sample 12/12/2011 12/15/2011

BioReactor 2 Inf Hg Blk 1151018-04 DIW Field Blank 12/12/2011 12/15/2011

BioReactor 2 Eff 1151018-05 Effluent Sample 12/12/2011 12/15/2011

BioReactor 2 Eff Hg Blk 1151018-06 DIW Field Blank 12/12/2011 12/15/2011

Batch Summary

Analyte Lab Matrix Method Prepared Analyzed Batch Sequence

Hg Water EPA 1631 12/16/2011 12/19/2011 B112089 1100897

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

Page 11 of 26
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Sample Results

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

BioReactor 1 Inf

1151018-01 Hg Influent T 76500 152 404 ng/L B112089 1100897

BioReactor 1 Inf Hg Blk

1151018-02 Hg DIW T 0.17 B 0.15 0.40 ng/L B112089 1100897

BioReactor 2 Eff

1151018-05 Hg Effluent T 19.5 0.74 1.98 ng/L B112089 1100897

BioReactor 2 Eff Hg Blk

1151018-06 Hg DIW T 0.15 U 0.15 0.41 ng/L B112089 1100897

BioReactor 2 Inf

1151018-03 Hg Influent T 124 1.52 4.04 ng/L B112089 1100897

BioReactor 2 Inf Hg Blk

1151018-04 Hg DIW T 0.15 U 0.15 0.40 ng/L B112089 1100897

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

Page 12 of 26
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Accuracy & Precision Summary

Batch: B112089

Analyte Native Spike Result Units REC & Limits RPD & Limits

Method: EPA 1631

Lab Matrix: Water

Sample

B112089-SRM1 Certified Reference Material (1149037, NIST 1641d 1000x dilution)

Hg 15.68 16.12 ng/L 103% 85-115

B112089-MS1 Matrix Spike (1151018-05)

Hg 19.55 100.3 130.8 ng/L 111% 71-125

B112089-MSD1 Matrix Spike Duplicate (1151018-05)

Hg 19.55 101.5 122.0 ng/L 101% 71-125 247%

Method Blanks & Reporting Limits

Batch: B112089

Method: EPA 1631

Matrix: Water

Analyte: Hg

Sample Result Units

B112089-BLK1 0.05 ng/L

B112089-BLK2 0.07 ng/L

B112089-BLK3 0.03 ng/L

B112089-BLK4 0.06 ng/L

Average: 0.05 Standard Deviation: 0.02 MDL: 0.15

Limit: 0.50 Limit: 0.10 MRL: 0.40

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

Page 13 of 26
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Instrument Calibration

Sequence: 1100897

Instrument: THG-05 Method: EPA 1631

Date: 12/19/2011

Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg

Lab ID True Value Result Units REC & Limits

1100897-IBL1 8.39 pg of Hg

1100897-IBL2 7.28 pg of Hg

1100897-IBL3 6.33 pg of Hg

1100897-IBL4 5.91 pg of Hg

1100897-CAL1 25.00 25.12 pg of Hg 100%

1100897-CAL2 100.0 100.3 pg of Hg 100%

1100897-CAL3 500.0 471.1 pg of Hg 94%

1100897-CAL4 2500 2573 pg of Hg 103%

1100897-CAL5 10000 10260 pg of Hg 103%

1100897-ICV1 1568 1612 pg of Hg 103% 85-115

1100897-CCB1 10.4 pg of Hg

1100897-CCV1 500.0 448.2 pg of Hg 90% 77-123

1100897-CCB2 3.99 pg of Hg

1100897-CCB3 80.9 pg of Hg

1100897-CCB4 165 pg of Hg

1100897-CCB5 16.1 pg of Hg

1100897-CCB6 64.8 pg of Hg

1100897-CCB7 50.9 pg of Hg

1100897-CCB8 26.6 pg of Hg

1100897-CCB9 30.4 pg of Hg

1100897-CCBA 22.2 pg of Hg

1100897-CCV2 500.0 522.8 pg of Hg 105% 77-123

1100897-CCV3 500.0 508.6 pg of Hg 102% 77-123

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

Page 14 of 26
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Sample Containers

Lab ID: 1151018-01 Report Matrix: Influent

Sample: BioReactor 1 Inf Sample Type: Sample Received: 12/15/2011

Collected: 12/12/2011

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

A 71470160

10

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

Lab ID: 1151018-02 Report Matrix: DIW

Sample: BioReactor 1 Inf Hg Blk Sample Type: Field Blank Received: 12/15/2011

Collected: 12/12/2011

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

A 71470160

10

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

Lab ID: 1151018-03 Report Matrix: Influent

Sample: BioReactor 2 Inf Sample Type: Sample Received: 12/15/2011

Collected: 12/12/2011

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

A 71470160

10

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

Lab ID: 1151018-04 Report Matrix: DIW

Sample: BioReactor 2 Inf Hg Blk Sample Type: Field Blank Received: 12/15/2011

Collected: 12/12/2011

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

A 71470160

10

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

Lab ID: 1151018-05 Report Matrix: Effluent

Sample: BioReactor 2 Eff Sample Type: Sample Received: 12/15/2011

Collected: 12/12/2011

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

A 71470160

10

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

Lab ID: 1151018-06 Report Matrix: DIW

Sample: BioReactor 2 Eff Hg Blk Sample Type: Field Blank Received: 12/15/2011

Collected: 12/12/2011

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

A 71470160

10

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 15 of 26
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Shipping Containers

Cooler

Tracking No: 4726 7966 6798 via FedEx

Temperature: ambient

Coolant Type: None

Description: Cooler

Damaged in transit? No

Returned to client? No

Custody seals present? No

Custody seals intact? No

COC present? Yes

Received: December 15, 2011 8:30

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

Page 16 of 26
Page 17 of 26
 

December 22, 2011 

Jay Perkins 

Duke Energy Analytical Laboratory 

Mail Code MGO3A2 (Building 7405) 

13339 Hagers Ferry Rd. 

Huntersville, NC 28078 

(704) 875-5245 

Project: Allen – FGD Alternative Fuels Test Burn #3 - Daily (LIMS # J11120225) 

Dear Mr. Perkins, 

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

speciation analysis on December 14, 2011. The samples were received in a sealed cooler at -

0.3°C on December 15, 2011. Selenium speciation analysis was performed via ion 

chromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICPDRC-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 

 

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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 Alternative Fuels Test Burn #3 - Daily (LIMS # J11120225) 

December 22, 2011 

1. Sample Reception 

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

Consulting) were submitted for selenium speciation analysis on December 14, 2011. The 

samples were received on December 15, 2011 in a sealed container at -0.3°C. 

The samples were received in a laminar flow clean hood, void of trace metals contamination 

and ultra-violet radiation, and was designated a discrete sample identifier. An aliquot of each 

sample was filtered (0.45μm) and each filtrate was stored in a secure, monitored cryofreezer 

(maintained at a temperature of -80oC) until selenium speciation analysis could be performed 

via ion chromatography inductively coupled plasma dynamic reaction cell mass spectrometry 

(IC-ICP-DRC-MS). 

2. Sample Preparation 

All sample preparation is performed in laminar flow clean hoods known to be free from trace 

metals contamination. All applied water for dilutions and sample preservatives are 

monitored for contamination to account for any biases associated with the sample results. 

Selenium Speciation Analysis by IC-ICP-DRC-MS Prior to analysis, an aliquot of each 

sample was filtered with a syringe filter (0.45μm) and injected directly into a sealed 

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 

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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 minimal interval 

of every ten analytical runs. 

Selenium Speciation Analysis by IC-ICP-DRC-MS Each sample for selenium speciation 

analysis was analyzed by ion chromatography inductively coupled plasma dynamic reaction 

cell mass spectrometry (IC-ICP-DRC-MS) on December 19, 2011. An aliquot of each

sample is injected onto an anion exchange column and mobilized by a basic (pH > 7) 

gradient. The eluting selenium species are then introduced into a radio frequency (RF) 

plasma where energy-transfer processes cause desolvation, atomization, and ionization. The 

ions are extracted from the plasma through a differentially-pumped vacuum interface and 

travel through a pressurized chamber (DRC) containing a specific reactive 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 this sample 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. 

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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 

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Sample Results

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

Unknown Se 

Species (n)

FGD Purge Eff ND (<4.6) 2200 ND (<3.8) ND (<4.0) ND (<4.0) 0 (0)

BioReactor 1 Inf 7.1 1500 ND (<0.96) 1.2 2.1 0 (0)

BioReactor 2 Inf 69.6 590 ND (<0.96) 1.7 1.6 0 (0)

BioReactor 2 Eff 5.3 6.51 ND (<0.96) ND (<1.0) ND (<1.0) 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

n = number of unknown Se species observed

Report Generated by: Russell Gerads

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Allen - FGD Alternate Fuels Test Burn #3 - Daily

Contact: Jay Perkins

Date: December 22, 2011

LIMS #J11120225

Page 22 of 26
Quality Control Summary - Preparation Blank Summary

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

Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.023 1.1 4.6

Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.018 0.89 3.6

SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.019 0.96 3.8

MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.020 1.0 4.0

SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.020 1.0 4.0

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 9.08 94.9

Se(VI) LCS 9.48 9.15 96.5

SeCN LCS 8.92 8.65 97.0

MeSe(IV) LCS 6.47 5.76 89.0

SeMe LCS 9.32 8.66 93.0

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Allen - FGD Alternate Fuels Test Burn #3 - Daily

Contact: Jay Perkins

LIMS #J11120225

Date: December 22, 2011

Report Generated by: Russell Gerads

Page 23 of 26
Quality Control Summary - Matrix Duplicates

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

Se(IV) Batch QC ND (<4.6) ND (<4.6) NC NC

Se(VI) Batch QC 699.8 698.6 699.2 0.2

SeCN Batch QC ND (<3.8) ND (<3.8) NC NC

MeSe(IV) Batch QC ND (<4.0) ND (<4.0) NC NC

SeMe Batch QC ND (<4.0) ND (<4.0) 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 1440 129.5* 1112 1517 136.4* 5.2

Se(VI) Batch QC 1009 1838 112.9 1009 1836 112.6 0.1

SeCN Batch QC 915.0 833.6 91.1 915.0 726.1 79.4 13.8

*Elevated recovery is attributed to matrix induced species conversion

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Allen - FGD Alternate Fuels Test Burn #3 - Daily

Contact: Jay Perkins

LIMS #J11120225

Date: December 22, 2011

Report Generated by: Russell Gerads

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