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: J11030084

Lab Contact: Jason C Perkins

Date: 3/21/2011

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:

Test Burn - Day 1

Data Flags & Calculations:

Any analytical tests or individual analytes within a test flagged with an "X" or "1" indicate a deviation from the method quality 

system or quality control requirement. 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 25
Sample ID's & Descriptions:

Sample ID Plant/Station

Collection 

Date and Time Collected By Sample Description

2011004957 ALLEN 02-Mar-11 9:12 AM Chris Williams FGD Purge Eff 

2011004958 ALLEN 02-Mar-11 8:33 AM Chris Williams EQ Tank Eff 

2011004959 ALLEN 02-Mar-11 8:38 AM Chris Williams BioReactor 1 Inf 

2011004960 ALLEN 02-Mar-11 8:36 AM Chris Williams BioReactor 2 Inf 

2011004961 ALLEN 02-Mar-11 8:41 AM Chris Williams BioReactor 2 Eff 

2011004962 ALLEN 02-Mar-11 11:25 AM illegible BioReactor 1 Inf BLANK 

2011004963 ALLEN 02-Mar-11 11:40 AM illegible BioReactor 2 Inf BLANK 

2011004964 ALLEN 02-Mar-11 11:30 AM illegible BioReactor 2 Eff BLANK 

2011004965 ALLEN 02-Mar-11 7:59 AM Chris Williams Filter Blk 

9 Total Samples

Page 2 of 25
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 Test Case Narratives

Analytical Laboratory QC Report Chain of Custody

Reviewed By: DataBase Administrator Date: 3/21/2011

Yes

Electronic Data Deliverable (EDD) Sent Separately

Page 3 of 25
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11030084

2011004957

Collection Date: 02-Mar-11 9:12 AM

Site: FGD Purge Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 63.1 ug/L EPA 245.1 2.5 17-Mar-11 10:15 MHH7131

Mercury Dissolved (cold vapor) in Water (Filtered)

Mercury (Hg) 37.6 ug/L EPA 245.1 1 17-Mar-11 10:29 MHH7131

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 62.0 mg/L EPA 200.7 0.5 14-Mar-11 12:55 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 1560 ug/L EPA 200.8 10 11-Mar-11 10:19 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 142 ug/L EPA 200.8 10 14-Mar-11 13:31 KRICHAR

Chromium (Cr) 109 ug/L 10 EPA 200.8 14-Mar-11 13:31 KRICHAR

Copper (Cu) 163 ug/L 10 EPA 200.8 14-Mar-11 13:31 KRICHAR

Nickel (Ni) 223 ug/L 10 EPA 200.8 14-Mar-11 13:31 KRICHAR

Selenium (Se) 1660 ug/L 10 EPA 200.8 14-Mar-11 13:31 KRICHAR

Silver (Ag) < 10 ug/L 10 EPA 200.8 14-Mar-11 13:31 KRICHAR

Zinc (Zn) 267 ug/L 20 EPA 200.8 14-Mar-11 13:31 KRICHAR

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2011004958

Collection Date: 02-Mar-11 8:33 AM

Site: EQ Tank Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 40.4 ug/L EPA 245.1 2.5 17-Mar-11 10:20 MHH7131

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 50.6 mg/L EPA 200.7 0.5 14-Mar-11 12:59 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 1090 ug/L EPA 200.8 10 11-Mar-11 10:23 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 95.9 ug/L EPA 200.8 10 14-Mar-11 13:26 KRICHAR

Chromium (Cr) 78.5 ug/L 10 EPA 200.8 14-Mar-11 13:26 KRICHAR

Copper (Cu) 112 ug/L 10 EPA 200.8 14-Mar-11 13:26 KRICHAR

Nickel (Ni) 150 ug/L 10 EPA 200.8 14-Mar-11 13:26 KRICHAR

Selenium (Se) 1110 ug/L 10 EPA 200.8 14-Mar-11 13:26 KRICHAR

Page 4 of 25
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11030084

2011004958

Collection Date: 02-Mar-11 8:33 AM

Site: EQ Tank Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

TOTAL RECOVERABLE METALS BY ICP-MS

Silver (Ag) 12.2 ug/L EPA 200.8 10 14-Mar-11 13:26 KRICHAR

Zinc (Zn) 174 ug/L 20 EPA 200.8 14-Mar-11 13:26 KRICHAR

2011004959

Collection Date: 02-Mar-11 8:38 AM

Site: BioReactor 1 Inf 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY 1631

Vendor Parameter Complete V_BRAND

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 46.1 mg/L EPA 200.7 0.5 14-Mar-11 13:03 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 726 ug/L EPA 200.8 10 11-Mar-11 10:27 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L EPA 200.8 10 14-Mar-11 13:21 KRICHAR

Chromium (Cr) < 10 ug/L 10 EPA 200.8 14-Mar-11 13:21 KRICHAR

Copper (Cu) < 10 ug/L 10 EPA 200.8 14-Mar-11 13:21 KRICHAR

Nickel (Ni) 17.7 ug/L 10 EPA 200.8 14-Mar-11 13:21 KRICHAR

Selenium (Se) 781 ug/L 10 EPA 200.8 14-Mar-11 13:21 KRICHAR

Silver (Ag) < 10 ug/L 10 EPA 200.8 14-Mar-11 13:21 KRICHAR

Zinc (Zn) < 20 ug/L 20 EPA 200.8 14-Mar-11 13:21 KRICHAR

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2011004960

Collection Date: 02-Mar-11 8:36 AM

Site: BioReactor 2 Inf 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY 1631

Vendor Parameter Complete V_BRAND

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 49.4 mg/L EPA 200.7 0.5 14-Mar-11 13:07 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L EPA 200.8 10 14-Mar-11 13:17 KRICHAR

Chromium (Cr) < 10 ug/L 10 EPA 200.8 14-Mar-11 13:17 KRICHAR

Copper (Cu) < 10 ug/L 10 EPA 200.8 14-Mar-11 13:17 KRICHAR

Nickel (Ni) 11.5 ug/L 10 EPA 200.8 14-Mar-11 13:17 KRICHAR

Page 5 of 25
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11030084

2011004960

Collection Date: 02-Mar-11 8:36 AM

Site: BioReactor 2 Inf 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

TOTAL RECOVERABLE METALS BY ICP-MS

Selenium (Se) < 10 ug/L EPA 200.8 10 14-Mar-11 13:17 KRICHAR

Silver (Ag) 18.1 ug/L 10 EPA 200.8 14-Mar-11 13:17 KRICHAR

Zinc (Zn) < 20 ug/L 20 EPA 200.8 14-Mar-11 13:17 KRICHAR

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2011004961

Collection Date: 02-Mar-11 8:41 AM

Site: BioReactor 2 Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY 1631

Vendor Parameter Complete V_BRAND

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 58.6 mg/L EPA 200.7 0.5 14-Mar-11 13:11 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 5 ug/L EPA 200.8 5 14-Mar-11 13:02 KRICHAR

Chromium (Cr) < 5 ug/L 5 EPA 200.8 14-Mar-11 13:02 KRICHAR

Copper (Cu) < 5 ug/L 5 EPA 200.8 14-Mar-11 13:02 KRICHAR

Nickel (Ni) < 5 ug/L 5 EPA 200.8 14-Mar-11 13:02 KRICHAR

Selenium (Se) < 5 ug/L 5 EPA 200.8 14-Mar-11 13:02 KRICHAR

Silver (Ag) < 5 ug/L 5 EPA 200.8 14-Mar-11 13:02 KRICHAR

Zinc (Zn) < 10 ug/L 10 EPA 200.8 14-Mar-11 13:02 KRICHAR

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2011004962

Collection Date: 02-Mar-11 11:25 AM

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

2011004963

Collection Date: 02-Mar-11 11:40 AM

Site: BioReactor 2 Inf BLANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY 1631

Page 6 of 25
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11030084

2011004963

Collection Date: 02-Mar-11 11:40 AM

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

2011004964

Collection Date: 02-Mar-11 11:30 AM

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

2011004965

Collection Date: 02-Mar-11 7:59 AM

Site: Filter Blk 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

DISSOLVED METALS BY ICP-MS

Selenium (Se) < 2 ug/L EPA 200.8 2 11-Mar-11 10:30 KRICHAR

Page 7 of 25
March 11, 2011

Duke Energy

ATTN: Jay Perkins

13339 Hagers Ferry Road

Huntersville NC 28078

jperkins@duke-energy.com

RE: Project DUK-HV1101

Dear Jay Perkins,

This report contains results for the 6 samples received by Brooks Rand Labs (BRL) on March 

04, 2011. The samples were logged-in for the contracted analyses according to the 

chain-of-custody form(s). The samples were received, prepared, analyzed, and stored 

according to BRL SOPs and EPA methodology.

The results were method blank corrected as described in the calculations section of the relevant 

BRL SOP(s) 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 data is reported without qualification and all associated 

quality control sample results meet the acceptance criteria.

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

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

Information page in your report. Please feel free to contact me if you have any questions 

regarding this report.

Sincerely,

Tiffany Stilwater

Project Manager

tiffany@brooksrand.com

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

Page 8 of 25
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 9 of 25
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 1110038-01 FGD Wastewater Sample 03/02/2011 03/04/2011

BioReactor 1 Inf Hg Blk 1110038-02 DIW Field Blank 03/02/2011 03/04/2011

BioReactor 2 Inf 1110038-03 FGD Wastewater Sample 03/02/2011 03/04/2011

BioReactor 2 Inf Hg Blk 1110038-04 DIW Field Blank 03/02/2011 03/04/2011

BioReactor 2 Eff 1110038-05 FGD Wastewater Sample 03/02/2011 03/04/2011

BioReactor 2 Eff Hg Blk 1110038-06 DIW Field Blank 03/02/2011 03/04/2011

Batch Summary

Analyte Lab Matrix Method Prepared Analyzed Batch Sequence

Hg Water EPA 1631 03/07/2011 03/09/2011 B110275 1100153

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

Page 10 of 25
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

1110038-01 Hg FGD Wastewater T 265 30.3 80.8 ng/L B110275 1100153

BioReactor 1 Inf Hg Blk

1110038-02 Hg DIW T 0.15 U 0.15 0.40 ng/L B110275 1100153

BioReactor 2 Eff

1110038-05 Hg FGD Wastewater T 11.0 0.15 0.41 ng/L B110275 1100153

BioReactor 2 Eff Hg Blk

1110038-06 Hg DIW T 0.15 U 0.15 0.41 ng/L B110275 1100153

BioReactor 2 Inf

1110038-03 Hg FGD Wastewater T 24.7 0.30 0.80 ng/L B110275 1100153

BioReactor 2 Inf Hg Blk

1110038-04 Hg DIW T 0.15 U 0.15 0.40 ng/L B110275 1100153

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

Page 11 of 25
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Accuracy & Precision Summary

Analyte Native Spike Result Units REC & Limits RPD & Limits

Batch: B110275

Method: EPA 1631

Lab Matrix: Water

Sample

B110275-SRM1 Certified Reference Material (1107115, NIST 1641d 1000x dilution)

Hg 15.68 16.83 ng/L 107% 85-115

B110275-MS1 Matrix Spike (1110038-01)

Hg 265.0 1010 1306 ng/L 103% 71-125

B110275-MSD1 Matrix Spike Duplicate (1110038-01)

Hg 265.0 1010 1348 ng/L 107% 71-125 243%

Method Blanks & Reporting Limits

Batch: B110275

Method: EPA 1631

Matrix: Water

Analyte: Hg

Sample Result Units

B110275-BLK1 0.06 ng/L

B110275-BLK2 0.18 ng/L

B110275-BLK3 0.07 ng/L

B110275-BLK4 0.25 ng/L

Average: 0.14 Standard Deviation: 0.09 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 12 of 25
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Instrument Calibration

Method: EPA 1631

Sequence: 1100153

Instrument: THG-05

Date: 03/09/2011

Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg

Lab ID True Value Result Units REC & Limits

1100153-IBL1 9.93 pg of Hg

1100153-IBL2 9.40 pg of Hg

1100153-IBL3 10.13 pg of Hg

1100153-IBL4 7.10 pg of Hg

1100153-CAL1 25.00 24.72 pg of Hg 99%

1100153-CAL2 100.0 96.80 pg of Hg 97%

1100153-CAL3 500.0 509.2 pg of Hg 102%

1100153-CAL4 2500 2497 pg of Hg 100%

1100153-CAL5 10000 10280 pg of Hg 103%

1100153-ICV1 1568 1683 pg of Hg 107% 85-115

1100153-CCB1 11.9 pg of Hg

1100153-CCV1 500.0 521.3 pg of Hg 104% 77-123

1100153-CCV2 500.0 507.5 pg of Hg 102% 77-123

1100153-CCV3 500.0 520.7 pg of Hg 104% 77-123

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

Page 13 of 25
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Sample Containers

Lab ID: 1110038-01 Report Matrix: FGD Wastewater

Sample: BioReactor 1 Inf Sample Type: Sample Received: 03/04/2011

Collected: 03/02/2011

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

A 71284002

0

Cardboard 

Box

Bottle FLPE Hg-T 250-mL None N/A

Lab ID: 1110038-02 Report Matrix: DIW

Sample: BioReactor 1 Inf Hg Blk Sample Type: Field Blank Received: 03/04/2011

Collected: 03/02/2011

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

A 71284002

0

Cardboard 

Box

Bottle FLPE Hg-T 250-mL None N/A

Lab ID: 1110038-03 Report Matrix: FGD Wastewater

Sample: BioReactor 2 Inf Sample Type: Sample Received: 03/04/2011

Collected: 03/02/2011

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

A 71284002

0

Cardboard 

Box

Bottle FLPE Hg-T 250-mL None N/A

Lab ID: 1110038-04 Report Matrix: DIW

Sample: BioReactor 2 Inf Hg Blk Sample Type: Field Blank Received: 03/04/2011

Collected: 03/02/2011

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

A 71284002

0

Cardboard 

Box

Bottle FLPE Hg-T 250-mL None N/A

Lab ID: 1110038-05 Report Matrix: FGD Wastewater

Sample: BioReactor 2 Eff Sample Type: Sample Received: 03/04/2011

Collected: 03/02/2011

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

A 71284002

0

Cardboard 

Box

Bottle FLPE Hg-T 250-mL None N/A

Lab ID: 1110038-06 Report Matrix: DIW

Sample: BioReactor 2 Eff Hg Blk Sample Type: Field Blank Received: 03/04/2011

Collected: 03/02/2011

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

A 71284002

0

Cardboard 

Box

Bottle FLPE Hg-T 250-mL None N/A

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

Page 14 of 25
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Shipping Containers

Cardboard Box

Tracking No: 472679658138 via FedEx

Temperature: ambient

Coolant Type: None

Description: Cardboard Box

Damaged in transit? No

Returned to client? No

Custody seals present? No

Custody seals intact? No

COC present? Yes

Received: March 4, 2011 8:50

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

Page 15 of 25
Page 16 of 25
 

March 14, 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 # J11030084) 

Dear Mr. Perkins, 

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

speciation analysis on March 3, 2011. The samples were received on March 4, 2011 in a 

sealed cooler at 1.0o

C. Selenium speciation analysis was performed via ion 

chromatography inductively coupled plasma dynamic reaction cell mass spectrometry 

(IC-ICP-DRC-MS). Any analytical 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 17 of 25
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 # J11030084) 

March 14, 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 March 3, 2011. 

The samples were received on March 4, 2011 in a sealed container at 1.0o

C. 

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

contamination and ultra-violet radiation. Upon reception, the samples were 

designated discrete sample identifiers. An aliquot of each sample was filtered 

(0.45μm) and these filtrates were 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 the samples may shift the equilibrium of the system resulting in 

changes in speciation ratios. 

Page 18 of 25
3. Sample Analysis 

All sample analysis is precluded 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 

minimal interval of every ten analytical runs. 

Selenium Speciation Analysis by IC-ICP-DRC-MS All samples for selenium 

speciation analysis were analyzed by ion chromatography inductively coupled plasma 

dynamic reaction cell mass spectrometry (IC-ICP-DRC-MS) on March 4, 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 very well and no analytical issues were encountered. All 

quality control parameters associated with these 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. 

Page 19 of 25
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. 

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 20 of 25
Sample Results

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

Unkn

Spec

FGD Purge Eff ND (<3.8) 1570 ND (<1.5) ND (<2.2) ND (<2.2) 0 BioReactor 1 Inf 6.87 670 ND (<0.37) 0.71 ND (<0.55) 0 BioReactor 2 Inf 1.47 ND (<0.34) ND (<0.37) ND (<0.55) ND (<0.55) 0 BioReactor 2 Eff 1.33 ND (<0.34) ND (<0.37) ND (<0.55) ND (<0.55) 0 

All results reflect the applied dilution and are reported in μg/LND = Not detected at the applied dilutionSeCN = SelenocyanateMeSe(IV) = Methylseleninic acidSeMe = SelenomethionineUnknown Se Species = Total concentration of all unknown Se species observed by IC-ICP-MSn = 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 Alternative Fuels Test Burn #3 - Daily

Contact: Jay Perkins

Date: March 14, 2011

LIMS #J11030084
Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 5Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.019 0.95 Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.007 0.34 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.007 0.37 MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.011 0.55 SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.011 0.55 eMDL = Estimated Method Detection Limit*Please see narrative regarding eMDL calculationsQuality Control Summary - Certified Reference MaterialsAnalyte (μg/L) CRM True Value Result RecoverySe(IV) ICV 9.57 9.52 99.5Se(VI) ICV 9.48 9.07 95.6SeCN ICV 8.92 8.95 100.3MeSe(IV) ICV 6.47 5.75 88.9SeMe ICV 9.32 8.65 92.8

LIMS #J11030084

Date: March 14, 2011

Report Generated by: Russell Gerads

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

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

Contact: Jay Perkins
Quality Control Summary - Matrix Duplicates

Analyte (μg/L) Sample ID Rep 1 Rep 2 Mean RPDSe(IV) BioReactor 2 Eff 1.33 1.27 1.30 4.7Se(VI) BioReactor 2 Eff ND (<0.34) ND (<0.34) NC NCSeCN BioReactor 2 Eff ND (<0.37) ND (<0.37) NC NCMeSe(IV) BioReactor 2 Eff ND (<0.55) ND (<0.55) NC NCSeMe BioReactor 2 Eff ND (<0.55) ND (<0.55) NC NCND = Not detected at the applied dilutionNC = Value was not calculated due to one or more concentrations below the eMDL Quality Control Summary - Matrix Spike/ Matrix Spike DuplicateAnalyte (μg/L) Sample ID Spike Conc MS Result Recovery Spike Conc MSD Result Recovery RPDSe(IV) BioReactor 2 Eff 278.0 275.4 98.6 278.0 282.9 101.3 2.7Se(VI) BioReactor 2 Eff 252.3 247.1 97.9 252.3 243.5 96.5 1.5SeCN BioReactor 2 Eff 228.8 219.6 96.0 228.8 215.5 94.2 0.0

LIMS #J11030084

Date: March 14, 2011

Report Generated by: Russell Gerads

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

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

Contact: Jay Perkins
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