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: J11100180

Lab Contact: Jason C Perkins

Date: 10/27/2011

Customer Address: 3195 Pine Hall Rd

Customer Name(s): Bill Kennedy, Melonie Martin, Wayne Chapman, Tom Johnson

Mailcode: Belews Steam Station

Belews Creek, NC 28012

Phone: 980-875-5348

Report Authorized By:

(Signature)

Program Comments:

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

Data Flags & Calculations:

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

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

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

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 24
Sample ID's & Descriptions:

Sample ID Plant/Station

Collection 

Date and Time Collected By Sample Description

2011022211 BELEWS 09-Oct-11 10:30 AM dean m FGD Purge Eff 

2011022214 BELEWS 09-Oct-11 10:30 AM dean m BIOREACTOR 1 INF. 

2011022215 BELEWS 09-Oct-11 10:30 AM dean m BIOREACTOR 1 INF. BLANK 

2011022216 BELEWS 09-Oct-11 10:30 AM dean m BIOREACTOR 2 EFF. 

2011022217 BELEWS 09-Oct-11 10:30 AM dean m BIOREACTOR 2 EFF. BLANK 

2011022218 BELEWS 09-Oct-11 10:30 AM dean m FILTER BLANK 

2011022219 BELEWS 09-Oct-11 10:30 AM dean m Trip Blank 

7 Total Samples

Page 2 of 24
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: 10/27/2011

Yes

Electronic Data Deliverable (EDD) Sent Separately

Page 3 of 24
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11100180

2011022211

Collection Date: 09-Oct-11 10:30 AM

Site: FGD Purge Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

ALKALINITY (FIXED END POINT 4.5)

Vendor Parameter Complete V_PRISM

Carbonate, Bicarbonate, and Hydroxide Alkalinity

Carbonate (CO3) Complete V_PRISM

Bicarbonate (HCO3) Complete V_PRISM

Hydroxide (OH) Complete V_PRISM

NITRITE + NITRATE (COLORIMETRIC)

Nitrite + Nitrate (Colorimetric) 16 mg-N/L 0.25 EPA 353.2 10-Oct-11 14:38 BGN9034

INORGANIC IONS BY IC

Bromide 110 mg/L EPA 300.0 5 19-Oct-11 23:38 JAHERMA

Chloride 7400 mg/L 100 EPA 300.0 19-Oct-11 23:38 JAHERMA

Sulfate 1100 mg/L 100 EPA 300.0 19-Oct-11 23:38 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 274 ug/L EPA 245.1 5 21-Oct-11 09:35 AGIBBS

Mercury Dissolved (cold vapor) in Water (Filtered)

Mercury (Hg) < 2.5 ug/L EPA 245.1 2.5 21-Oct-11 10:48 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 183 mg/L EPA 200.7 5 26-Oct-11 13:56 DJSULL1

Calcium (Ca) 3960 mg/L 1 EPA 200.7 26-Oct-11 13:56 DJSULL1

Lithium (Li) < 0.5 mg/L 0.5 EPA 200.7 26-Oct-11 13:56 DJSULL1

Magnesium (Mg) 580 mg/L 0.5 EPA 200.7 26-Oct-11 13:56 DJSULL1

Potassium (K) 53.1 mg/L 10 EPA 200.7 26-Oct-11 13:56 DJSULL1

Sodium (Na) 43.7 mg/L 5 EPA 200.7 26-Oct-11 13:56 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 339 ug/L EPA 200.8 10 12-Oct-11 12:05 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 136 ug/L EPA 200.8 10 12-Oct-11 11:34 DJSULL1

Cadmium (Cd) < 10 ug/L 10 EPA 200.8 12-Oct-11 11:34 DJSULL1

Chromium (Cr) 189 ug/L 10 EPA 200.8 12-Oct-11 11:34 DJSULL1

Copper (Cu) 103 ug/L 10 EPA 200.8 12-Oct-11 11:34 DJSULL1

Nickel (Ni) 156 ug/L 10 EPA 200.8 12-Oct-11 11:34 DJSULL1

Selenium (Se) 5490 ug/L 20 EPA 200.8 12-Oct-11 11:34 DJSULL1

Silver (Ag) < 10 ug/L 10 EPA 200.8 12-Oct-11 11:34 DJSULL1

Zinc (Zn) 188 ug/L 20 EPA 200.8 12-Oct-11 11:34 DJSULL1

Page 4 of 24
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11100180

2011022211

Collection Date: 09-Oct-11 10:30 AM

Site: FGD Purge Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

TOTAL DISSOLVED SOLIDS

TDS 19000 mg/L SM2540C 200 14-Oct-11 16:05 TJA7067

TOTAL SUSPENDED SOLIDS

TSS 1800 mg/L SM2540D 250 14-Oct-11 10:40 TJA7067

2011022214

Collection Date: 09-Oct-11 10:30 AM

Site: BIOREACTOR 1 INF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

ALKALINITY (FIXED END POINT 4.5)

Vendor Parameter Complete V_PRISM

Carbonate, Bicarbonate, and Hydroxide Alkalinity

Carbonate (CO3) Complete V_PRISM

Hydroxide (OH) Complete V_PRISM

Bicarbonate (HCO3) Complete V_PRISM

NITRITE + NITRATE (COLORIMETRIC)

Nitrite + Nitrate (Colorimetric) 14 mg-N/L 0.25 EPA 353.2 10-Oct-11 14:39 BGN9034

INORGANIC IONS BY IC

Bromide 85 mg/L EPA 300.0 5 19-Oct-11 23:54 JAHERMA

Chloride 6200 mg/L 100 EPA 300.0 19-Oct-11 23:54 JAHERMA

Sulfate 1200 mg/L 100 EPA 300.0 19-Oct-11 23:54 JAHERMA

MERCURY 1631

Vendor Parameter Complete V_BRAND

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 26.5 ug/L EPA 245.1 2.5 21-Oct-11 09:37 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 147 mg/L EPA 200.7 5 26-Oct-11 13:36 DJSULL1

Calcium (Ca) 3090 mg/L 1 EPA 200.7 26-Oct-11 13:36 DJSULL1

Lithium (Li) < 0.5 mg/L 0.5 EPA 200.7 26-Oct-11 13:36 DJSULL1

Magnesium (Mg) 469 mg/L 0.5 EPA 200.7 26-Oct-11 13:36 DJSULL1

Potassium (K) 21.1 mg/L 10 EPA 200.7 26-Oct-11 13:36 DJSULL1

Sodium (Na) 37.4 mg/L 5 EPA 200.7 26-Oct-11 13:36 DJSULL1

Page 5 of 24
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11100180

2011022214

Collection Date: 09-Oct-11 10:30 AM

Site: BIOREACTOR 1 INF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L EPA 200.8 10 12-Oct-11 11:37 DJSULL1

Cadmium (Cd) < 10 ug/L 10 EPA 200.8 12-Oct-11 11:37 DJSULL1

Chromium (Cr) 10.7 ug/L 10 EPA 200.8 12-Oct-11 11:37 DJSULL1

Copper (Cu) < 10 ug/L 10 EPA 200.8 12-Oct-11 11:37 DJSULL1

Nickel (Ni) < 10 ug/L 10 EPA 200.8 12-Oct-11 11:37 DJSULL1

Selenium (Se) 1160 ug/L 10 EPA 200.8 12-Oct-11 11:37 DJSULL1

Silver (Ag) < 10 ug/L 10 EPA 200.8 12-Oct-11 11:37 DJSULL1

Zinc (Zn) < 20 ug/L 20 EPA 200.8 12-Oct-11 11:37 DJSULL1

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2011022215

Collection Date: 09-Oct-11 10:30 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

2011022216

Collection Date: 09-Oct-11 10:30 AM

Site: BIOREACTOR 2 EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

ALKALINITY (FIXED END POINT 4.5)

Vendor Parameter Complete V_PRISM

Carbonate, Bicarbonate, and Hydroxide Alkalinity

Carbonate (CO3) Complete V_PRISM

Hydroxide (OH) Complete V_PRISM

Bicarbonate (HCO3) Complete V_PRISM

NITRITE + NITRATE (COLORIMETRIC)

Nitrite + Nitrate (Colorimetric) 0.14 mg-N/L 0.01 EPA 353.2 10-Oct-11 14:40 BGN9034

INORGANIC IONS BY IC

Bromide 86 mg/L EPA 300.0 5 20-Oct-11 00:10 JAHERMA

Chloride 6100 mg/L 100 EPA 300.0 20-Oct-11 00:10 JAHERMA

Sulfate 1400 mg/L 100 EPA 300.0 20-Oct-11 00:10 JAHERMA

MERCURY 1631

Vendor Parameter Complete V_BRAND

Page 6 of 24
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11100180

2011022216

Collection Date: 09-Oct-11 10:30 AM

Site: BIOREACTOR 2 EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) < 1 ug/L EPA 245.1 1 21-Oct-11 09:40 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 146 mg/L EPA 200.7 5 26-Oct-11 13:40 DJSULL1

Calcium (Ca) 3040 mg/L 1 EPA 200.7 26-Oct-11 13:40 DJSULL1

Lithium (Li) < 0.5 mg/L 0.5 EPA 200.7 26-Oct-11 13:40 DJSULL1

Magnesium (Mg) 472 mg/L 0.5 EPA 200.7 26-Oct-11 13:40 DJSULL1

Potassium (K) 25.4 mg/L 10 EPA 200.7 26-Oct-11 13:40 DJSULL1

Sodium (Na) 37.9 mg/L 5 EPA 200.7 26-Oct-11 13:40 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L EPA 200.8 10 12-Oct-11 11:40 DJSULL1

Cadmium (Cd) < 10 ug/L 10 EPA 200.8 12-Oct-11 11:40 DJSULL1

Chromium (Cr) < 10 ug/L 10 EPA 200.8 12-Oct-11 11:40 DJSULL1

Copper (Cu) < 10 ug/L 10 EPA 200.8 12-Oct-11 11:40 DJSULL1

Nickel (Ni) < 10 ug/L 10 EPA 200.8 12-Oct-11 11:40 DJSULL1

Selenium (Se) 12.1 ug/L 10 EPA 200.8 12-Oct-11 11:40 DJSULL1

Silver (Ag) < 10 ug/L 10 EPA 200.8 12-Oct-11 11:40 DJSULL1

Zinc (Zn) < 20 ug/L 20 EPA 200.8 12-Oct-11 11:40 DJSULL1

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2011022217

Collection Date: 09-Oct-11 10:30 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

2011022218

Collection Date: 09-Oct-11 10:30 AM

Site: FILTER BLANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

DISSOLVED METALS BY ICP-MS

Selenium (Se) < 1 ug/L EPA 200.8 1 12-Oct-11 11:56 DJSULL1

Page 7 of 24
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11100180

2011022219

Collection Date: 09-Oct-11 10:30 AM

Site: Trip Blank 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

TOTAL RECOVERABLE METALS BY ICP

Boron (B) < 0.05 mg/L EPA 200.7 0.05 26-Oct-11 13:20 DJSULL1

Calcium (Ca) 0.010 mg/L 0.01 EPA 200.7 26-Oct-11 13:20 DJSULL1

Lithium (Li) < 0.005 mg/L 0.005 EPA 200.7 26-Oct-11 13:20 DJSULL1

Magnesium (Mg) < 0.005 mg/L 0.005 EPA 200.7 26-Oct-11 13:20 DJSULL1

Potassium (K) < 0.1 mg/L 0.1 EPA 200.7 26-Oct-11 13:20 DJSULL1

Sodium (Na) < 0.05 mg/L 0.05 EPA 200.7 26-Oct-11 13:20 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 1 ug/L EPA 200.8 1 12-Oct-11 11:19 DJSULL1

Cadmium (Cd) < 1 ug/L 1 EPA 200.8 12-Oct-11 11:19 DJSULL1

Chromium (Cr) < 1 ug/L 1 EPA 200.8 12-Oct-11 11:19 DJSULL1

Copper (Cu) < 1 ug/L 1 EPA 200.8 12-Oct-11 11:19 DJSULL1

Nickel (Ni) < 1 ug/L 1 EPA 200.8 12-Oct-11 11:19 DJSULL1

Selenium (Se) < 1 ug/L 1 EPA 200.8 12-Oct-11 11:19 DJSULL1

Silver (Ag) < 1 ug/L 1 EPA 200.8 12-Oct-11 11:19 DJSULL1

Zinc (Zn) < 2 ug/L 2 EPA 200.8 12-Oct-11 11:19 DJSULL1

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

Page 8 of 24
 

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

October 18, 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: J11100180 

Dear Mr. Perkins, 

On October 11, 2011, Brooks Rand Labs (BRL) received two (2) flue gas desulfurization (FGD) 

wastewater samples and two (2) corresponding blank samples. 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. 

All data was reported without 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@brooksran.com 

Page 9 of 24
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 24
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 1142019-01 Influent Sample 10/09/2011 10/11/2011

BioReactor 1 Inf Hg Blk 1142019-02 DIW Field Blank 10/09/2011 10/11/2011

BioReactor 2 Eff 1142019-03 Effluent Sample 10/09/2011 10/11/2011

BioReactor 2 Eff Hg Blk 1142019-04 DIW Field Blank 10/09/2011 10/11/2011

Batch Summary

Analyte Lab Matrix Method Prepared Analyzed Batch Sequence

Hg Water EPA 1631 10/14/2011 10/17/2011 B111677 1100722

Sample Results

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

BioReactor 1 Inf

1142019-01 Hg Influent T 31800 76.5 204 ng/L B111677 1100722

BioReactor 1 Inf Hg Blk

1142019-02 Hg DIW T 0.15 U 0.15 0.41 ng/L B111677 1100722

BioReactor 2 Eff

1142019-03 Hg Effluent T 403 15.2 40.4 ng/L B111677 1100722

BioReactor 2 Eff Hg Blk

1142019-04 Hg DIW T 0.15 U 0.15 0.40 ng/L B111677 1100722

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

Page 11 of 24
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Accuracy & Precision Summary

Batch: B111677

Analyte Native Spike Result Units REC & Limits RPD & Limits

Method: EPA 1631

Lab Matrix: Water

Sample

B111677-SRM1 Certified Reference Material (1141046, NIST 1641d 1000x dilution)

Hg 15.68 16.21 ng/L 103% 85-115

B111677-MS1 Matrix Spike (1142018-01)

Hg 184.8 909.1 1260 ng/L 118% 71-125

B111677-MSD1 Matrix Spike Duplicate (1142018-01)

Hg 184.8 909.1 1225 ng/L 114% 71-125 243%

Method Blanks & Reporting Limits

Batch: B111677

Method: EPA 1631

Matrix: Water

Analyte: Hg

Sample Result Units

B111677-BLK1 0.07 ng/L

B111677-BLK2 0.06 ng/L

B111677-BLK3 0.11 ng/L

B111677-BLK4 0.05 ng/L

Average: 0.07 Standard Deviation: 0.03 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 12 of 24
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Instrument Calibration

Sequence: 1100722

Instrument: THG-10 Method: EPA 1631

Date: 10/17/2011

Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg

Lab ID True Value Result Units REC & Limits

1100722-IBL1 6.37 pg of Hg

1100722-IBL2 9.62 pg of Hg

1100722-IBL3 8.87 pg of Hg

1100722-IBL4 7.61 pg of Hg

1100722-CAL1 25.00 25.04 pg of Hg 100%

1100722-CAL2 100.0 95.11 pg of Hg 95%

1100722-CAL3 500.0 472.7 pg of Hg 95%

1100722-CAL4 2500 2668 pg of Hg 107%

1100722-CAL5 10000 10470 pg of Hg 105%

1100722-ICV1 1568 1621 pg of Hg 103% 85-115

1100722-CCB1 10.9 pg of Hg

1100722-CCB2 9.83 pg of Hg

1100722-CCB3 31.0 pg of Hg

1100722-CCB4 11.9 pg of Hg

1100722-CCV1 500.0 528.4 pg of Hg 106% 77-123

1100722-CCV2 500.0 535.0 pg of Hg 107% 77-123

1100722-CCV3 500.0 527.0 pg of Hg 105% 77-123

1100722-CCV4 500.0 484.0 pg of Hg 97% 77-123

1100722-CCB5 6.00 pg of Hg

1100722-CCB6 5.04 pg of Hg

1100722-CCV5 500.0 485.7 pg of Hg 97% 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 24
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Sample Containers

Lab ID: 1142019-01 Report Matrix: Influent

Sample: BioReactor 1 Inf Sample Type: Sample Received: 10/11/2011

Collected: 10/09/2011

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

A 71490150

70

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

Lab ID: 1142019-02 Report Matrix: DIW

Sample: BioReactor 1 Inf Hg Blk Sample Type: Field Blank Received: 10/11/2011

Collected: 10/09/2011

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

A 71470101

0

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

Comments: Volume=250mL

Lab ID: 1142019-03 Report Matrix: Effluent

Sample: BioReactor 2 Eff Sample Type: Sample Received: 10/11/2011

Collected: 10/09/2011

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

A 71470101

0

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

Lab ID: 1142019-04 Report Matrix: DIW

Sample: BioReactor 2 Eff Hg Blk Sample Type: Field Blank Received: 10/11/2011

Collected: 10/09/2011

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

A 71470101

0

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

Shipping Containers

Cooler

Tracking No: 472679664730 via FedEx

Temperature: 0.4 °C

Coolant Type: Ice

Description: Cooler

Damaged in transit? No

Returned to client? No

Custody seals present? Yes

Custody seals intact? Yes

COC present? Yes

Received: October 11, 2011 9:00

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

Page 14 of 24
Page 15 of 24
 

October 18, 2011 

Jay Perkins 

Duke Energy Analytical Laboratory 

Mail Code MGO3A2 (Building 7405) 

13339 Hagers Ferry Rd. 

Huntersville, NC 28078 

(704) 875-5245 

Project: HAPS/MACT Testing Belews Creek (LIMS # J11100180) 

Dear Mr. Perkins, 

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

speciation analysis on October 10, 2011. The samples were received on October 11, 2011 in a 

sealed cooler at -0.4°C. Selenium speciation analysis was performed via ion chromatography 

inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICP-DRC-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, 

 

 Ben Wozniak

 Project Manager 

 Applied Speciation and Consulting, LLC 

 

Page 16 of 24
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: HAPS/MACT Testing Belews Creek (LIMS # J11100180) 

October 18, 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 October 10, 2011. The 

samples were received on October 11, 2011 in a sealed container at -0.4°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. 

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 All samples for selenium speciation 

analysis were analyzed by ion chromatography inductively coupled plasma dynamic reaction 

cell mass spectrometry (IC-ICP-DRC-MS) on October 17, 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 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. 

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, 

Ben Wozniak 

Project Manager 

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 57.2 248 ND (<1.3) ND (<1.5) ND (<1.5) 0 (0)

BioReactor 1 Inf 14.8 1170 ND (<0.34) ND (<0.37) ND (<0.37) 0 (0)

BioReactor 2 Eff 2.11 6.72 ND (<0.34) ND (<0.37) ND (<0.37) 0 (0)

Metals Trip Blk ND (<0.097) ND (<0.055) ND (<0.067) ND (<0.073) ND (<0.073) 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: Ben Wozniak

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: HAPS/MACT Testing Belews Creek

Contact: Jay Perkins

Date: October 18, 2011

LIMS #J11100180

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Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 10x eMDL 50x eMDL 200x

Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.097 0.48 1.9

Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.006 0.055 0.28 1.1

SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.007 0.067 0.34 1.3

MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.007 0.073 0.37 1.5

SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.007 0.073 0.37 1.5

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 11.24 117.5

Se(VI) LCS 9.48 10.01 105.6

SeCN LCS 8.92 9.239 103.6

MeSe(IV) LCS 6.47 5.847 90.4

SeMe LCS 9.32 9.200 98.7

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: HAPS/MACT Testing Belews Creek

Contact: Jay Perkins

LIMS #J11100180

Date: October 18, 2011

Report Generated by: Ben Wozniak

Page 21 of 24
Quality Control Summary - Matrix Duplicates

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

Se(IV) Batch QC* ND (<0.48) ND (<0.48) NC NC

Se(VI) Batch QC* ND (<0.28) ND (<0.28) NC NC

SeCN Batch QC* ND (<0.34) ND (<0.34) NC NC

MeSe(IV) Batch QC* ND (<0.37) ND (<0.37) NC NC

SeMe Batch QC* ND (<0.37) ND (<0.37) NC NC

ND = Not detected at the applied dilution

NC = Value was not calculated due to one or more concentrations below the eMDL

* Batch QC performed on sample from LIMS # J11100175

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* 278.0 268.0 96.4 278.0 265.4 95.5 1.0

Se(VI) Batch QC* 252.3 247.5 98.1 252.3 245.9 97.5 0.6

SeCN Batch QC* 228.8 219.4 95.9 228.8 221.4 96.8 0.9

* Batch QC performed on sample from LIMS # J11100175

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: HAPS/MACT Testing Belews Creek

Contact: Jay Perkins

LIMS #J11100180

Date: October 18, 2011

Report Generated by: Ben Wozniak

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