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: J11100235

Lab Contact: Jason C Perkins

Date: 10/28/2011

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 32
Sample ID's & Descriptions:

Sample ID Plant/Station

Collection 

Date and Time Collected By Sample Description

2011022452 BELEWS 12-Oct-11 9:15 AM TO FGD Purge Eff 

2011022453 BELEWS 12-Oct-11 9:15 AM TO BIOREACTOR 1 INF. 

2011022454 BELEWS 12-Oct-11 9:15 AM TO BIOREACTOR 2 EFF. 

2011022455 BELEWS 12-Oct-11 9:15 AM TO BIOREACTOR 1 INF. BLANK 

2011022456 BELEWS 12-Oct-11 9:15 AM TO BIOREACTOR 2 EFF. BLANK 

2011022457 BELEWS 12-Oct-11 9:15 AM TO FILTER BLANK 

2011022458 BELEWS 12-Oct-11 9:15 AM TO Trip Blank 

7 Total Samples

Page 2 of 32
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: 10/28/2011

Yes

Electronic Data Deliverable (EDD) Sent Separately

Page 3 of 32
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11100235

2011022452

Collection Date: 12-Oct-11 9:15 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

Hydroxide (OH) Complete V_PRISM

Carbonate (CO3) Complete V_PRISM

Bicarbonate (HCO3) Complete V_PRISM

NITRITE + NITRATE (COLORIMETRIC)

Nitrite + Nitrate (Colorimetric) 18 mg-N/L 0.25 EPA 353.2 18-Oct-11 13:08 BGN9034

INORGANIC IONS BY IC

Bromide 100 mg/L EPA 300.0 5 20-Oct-11 14:40 JAHERMA

Chloride 7200 mg/L 100 EPA 300.0 20-Oct-11 14:40 JAHERMA

Sulfate 1200 mg/L 100 EPA 300.0 20-Oct-11 14:40 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 365 ug/L EPA 245.1 5 21-Oct-11 10:10 AGIBBS

Mercury Dissolved (cold vapor) in Water (Filtered)

Mercury (Hg) 56.6 ug/L EPA 245.1 2.5 21-Oct-11 10:58 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 184 mg/L EPA 200.7 0.5 24-Oct-11 14:00 DJSULL1

Calcium (Ca) 4200 mg/L 0.1 EPA 200.7 24-Oct-11 14:00 DJSULL1

Lithium (Li) 0.142 mg/L 0.05 EPA 200.7 24-Oct-11 14:00 DJSULL1

Magnesium (Mg) 633 mg/L 0.05 EPA 200.7 24-Oct-11 14:00 DJSULL1

Potassium (K) 52.1 mg/L 1 EPA 200.7 24-Oct-11 14:00 DJSULL1

Sodium (Na) 44.4 mg/L 0.5 EPA 200.7 24-Oct-11 14:00 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 1200 ug/L EPA 200.8 10 19-Oct-11 12:16 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 152 ug/L EPA 200.8 10 19-Oct-11 12:35 KRICHAR

Cadmium (Cd) < 10 ug/L 10 EPA 200.8 19-Oct-11 12:35 KRICHAR

Chromium (Cr) 214 ug/L 10 EPA 200.8 19-Oct-11 12:35 KRICHAR

Copper (Cu) 116 ug/L 10 EPA 200.8 19-Oct-11 12:35 KRICHAR

Nickel (Ni) 180 ug/L 10 EPA 200.8 19-Oct-11 12:35 KRICHAR

Selenium (Se) 5390 ug/L 20 EPA 200.8 19-Oct-11 12:35 KRICHAR

Silver (Ag) < 10 ug/L 10 EPA 200.8 19-Oct-11 12:35 KRICHAR

Zinc (Zn) 215 ug/L 20 EPA 200.8 19-Oct-11 12:35 KRICHAR

Page 4 of 32
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11100235

2011022452

Collection Date: 12-Oct-11 9:15 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 17000 mg/L SM2540C 200 19-Oct-11 13:25 TJA7067

TOTAL SUSPENDED SOLIDS

TSS 2900 mg/L SM2540D 250 14-Oct-11 10:40 TJA7067

2011022453

Collection Date: 12-Oct-11 9:15 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

Hydroxide (OH) Complete V_PRISM

Carbonate (CO3) Complete V_PRISM

Bicarbonate (HCO3) Complete V_PRISM

NITRITE + NITRATE (COLORIMETRIC)

Nitrite + Nitrate (Colorimetric) 15 mg-N/L 0.25 EPA 353.2 18-Oct-11 13:09 BGN9034

INORGANIC IONS BY IC

Bromide 93 mg/L EPA 300.0 5 20-Oct-11 14:56 JAHERMA

Chloride 6700 mg/L 100 EPA 300.0 20-Oct-11 14:56 JAHERMA

Sulfate 1300 mg/L 100 EPA 300.0 20-Oct-11 14:56 JAHERMA

MERCURY 1631

Vendor Parameter Complete V_BRAND

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 40.7 ug/L EPA 245.1 2.5 21-Oct-11 10:13 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 153 mg/L EPA 200.7 0.5 24-Oct-11 14:04 DJSULL1

Calcium (Ca) 3390 mg/L 0.1 EPA 200.7 24-Oct-11 14:04 DJSULL1

Lithium (Li) < 0.05 mg/L 0.05 EPA 200.7 24-Oct-11 14:04 DJSULL1

Magnesium (Mg) 536 mg/L 0.05 EPA 200.7 24-Oct-11 14:04 DJSULL1

Potassium (K) 22.2 mg/L 1 EPA 200.7 24-Oct-11 14:04 DJSULL1

Sodium (Na) 40.1 mg/L 0.5 EPA 200.7 24-Oct-11 14:04 DJSULL1

Page 5 of 32
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11100235

2011022453

Collection Date: 12-Oct-11 9:15 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 19-Oct-11 11:55 KRICHAR

Cadmium (Cd) < 10 ug/L 10 EPA 200.8 19-Oct-11 11:55 KRICHAR

Chromium (Cr) 11.9 ug/L 10 EPA 200.8 19-Oct-11 11:55 KRICHAR

Copper (Cu) < 10 ug/L 10 EPA 200.8 19-Oct-11 11:55 KRICHAR

Nickel (Ni) < 10 ug/L 10 EPA 200.8 19-Oct-11 11:55 KRICHAR

Selenium (Se) 1200 ug/L 10 EPA 200.8 19-Oct-11 11:55 KRICHAR

Silver (Ag) < 10 ug/L 10 EPA 200.8 19-Oct-11 11:55 KRICHAR

Zinc (Zn) < 20 ug/L 20 EPA 200.8 19-Oct-11 11:55 KRICHAR

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2011022454

Collection Date: 12-Oct-11 9:15 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

Hydroxide (OH) Complete V_PRISM

Carbonate (CO3) Complete V_PRISM

Bicarbonate (HCO3) Complete V_PRISM

NITRITE + NITRATE (COLORIMETRIC)

Nitrite + Nitrate (Colorimetric) 0.019 mg-N/L 0.01 EPA 353.2 18-Oct-11 13:10 BGN9034

INORGANIC IONS BY IC

Bromide 91 mg/L EPA 300.0 5 20-Oct-11 15:12 JAHERMA

Chloride 6600 mg/L 100 EPA 300.0 20-Oct-11 15:12 JAHERMA

Sulfate 1500 mg/L 100 EPA 300.0 20-Oct-11 15:12 JAHERMA

MERCURY 1631

Vendor Parameter Complete V_BRAND

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) < 1 ug/L EPA 245.1 1 21-Oct-11 10:15 AGIBBS

Page 6 of 32
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11100235

2011022454

Collection Date: 12-Oct-11 9:15 AM

Site: BIOREACTOR 2 EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 156 mg/L EPA 200.7 0.5 24-Oct-11 14:08 DJSULL1

Calcium (Ca) 3440 mg/L 0.1 EPA 200.7 24-Oct-11 14:08 DJSULL1

Lithium (Li) < 0.05 mg/L 0.05 EPA 200.7 24-Oct-11 14:08 DJSULL1

Magnesium (Mg) 529 mg/L 0.05 EPA 200.7 24-Oct-11 14:08 DJSULL1

Potassium (K) 27.3 mg/L 1 EPA 200.7 24-Oct-11 14:08 DJSULL1

Sodium (Na) 40.4 mg/L 0.5 EPA 200.7 24-Oct-11 14:08 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 5 ug/L EPA 200.8 5 19-Oct-11 11:58 KRICHAR

Cadmium (Cd) < 5 ug/L 5 EPA 200.8 19-Oct-11 11:58 KRICHAR

Chromium (Cr) < 5 ug/L 5 EPA 200.8 19-Oct-11 11:58 KRICHAR

Copper (Cu) < 5 ug/L 5 EPA 200.8 19-Oct-11 11:58 KRICHAR

Nickel (Ni) < 5 ug/L 5 EPA 200.8 19-Oct-11 11:58 KRICHAR

Selenium (Se) 11.9 ug/L 5 EPA 200.8 19-Oct-11 11:58 KRICHAR

Silver (Ag) < 5 ug/L 5 EPA 200.8 19-Oct-11 11:58 KRICHAR

Zinc (Zn) < 10 ug/L 10 EPA 200.8 19-Oct-11 11:58 KRICHAR

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2011022455

Collection Date: 12-Oct-11 9:15 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

2011022456

Collection Date: 12-Oct-11 9:15 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

Page 7 of 32
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11100235

2011022457

Collection Date: 12-Oct-11 9:15 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 19-Oct-11 10:52 KRICHAR

2011022458

Collection Date: 12-Oct-11 9:15 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 24-Oct-11 13:11 DJSULL1

Calcium (Ca) 0.018 mg/L R1 0.01 EPA 200.7 24-Oct-11 13:11 DJSULL1

Lithium (Li) < 0.005 mg/L 0.005 EPA 200.7 24-Oct-11 13:11 DJSULL1

Magnesium (Mg) 0.006 mg/L 0.005 EPA 200.7 24-Oct-11 13:11 DJSULL1

Potassium (K) < 0.1 mg/L 0.1 EPA 200.7 24-Oct-11 13:11 DJSULL1

Sodium (Na) < 0.05 mg/L 0.05 EPA 200.7 24-Oct-11 13:11 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 1 ug/L EPA 200.8 1 19-Oct-11 10:39 KRICHAR

Cadmium (Cd) < 1 ug/L 1 EPA 200.8 19-Oct-11 10:39 KRICHAR

Chromium (Cr) < 1 ug/L 1 EPA 200.8 19-Oct-11 10:39 KRICHAR

Copper (Cu) < 1 ug/L 1 EPA 200.8 19-Oct-11 10:39 KRICHAR

Nickel (Ni) < 1 ug/L 1 EPA 200.8 19-Oct-11 10:39 KRICHAR

Selenium (Se) < 1 ug/L 1 EPA 200.8 19-Oct-11 10:39 KRICHAR

Silver (Ag) < 1 ug/L 1 EPA 200.8 19-Oct-11 10:39 KRICHAR

Zinc (Zn) < 2 ug/L 2 EPA 200.8 19-Oct-11 10:39 KRICHAR

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

Qualifiers:

R1 Relative Percent Difference exceeded method acceptance limits, see additional notes

Page 8 of 32
 

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

October 26, 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: J11100235 

Dear Mr. Perkins, 

On October 14, 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. 

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 32
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 32
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 1142045-01 Influent Sample 10/12/2011 10/14/2011

BioReactor 1 Inf Hg Blk 1142045-02 DIW Field Blank 10/12/2011 10/14/2011

BioReactor 2 Eff 1142045-03 Effluent Sample 10/12/2011 10/14/2011

BioReactor 2 Eff Hg Blk 1142045-04 DIW Field Blank 10/12/2011 10/14/2011

Batch Summary

Analyte Lab Matrix Method Prepared Analyzed Batch Sequence

Hg Water EPA 1631 10/21/2011 10/25/2011 B111723 1100738

Sample Results

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

BioReactor 1 Inf

1142045-01 Hg Influent T 42700 76.5 204 ng/L B111723 1100738

BioReactor 1 Inf Hg Blk

1142045-02 Hg DIW T 0.15 U 0.15 0.40 ng/L B111723 1100738

BioReactor 2 Eff

1142045-03 Hg Effluent T 464 3.03 8.08 ng/L B111723 1100738

BioReactor 2 Eff Hg Blk

1142045-04 Hg DIW T 0.15 U 0.15 0.41 ng/L B111723 1100738

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

Page 11 of 32
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Accuracy & Precision Summary

Batch: B111723

Analyte Native Spike Result Units REC & Limits RPD & Limits

Method: EPA 1631

Lab Matrix: Water

Sample

B111723-SRM1 Certified Reference Material (1140052, THg ICV 1641d)

Hg 15.68 14.44 ng/L 92% 85-115

B111723-MS2 Matrix Spike (1143014-01)

Hg 436.0 2020 2506 ng/L 102% 71-125

B111723-MSD2 Matrix Spike Duplicate (1143014-01)

Hg 436.0 2020 2473 ng/L 101% 71-125 241%

Method Blanks & Reporting Limits

Batch: B111723

Method: EPA 1631

Matrix: Water

Analyte: Hg

Sample Result Units

B111723-BLK1 0.04 ng/L

B111723-BLK2 0.0008 ng/L

B111723-BLK3 0.05 ng/L

B111723-BLK4 0.02 ng/L

Average: 0.03 Standard Deviation: 0.02 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 32
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Instrument Calibration

Sequence: 1100738

Instrument: THG-05 Method: EPA 1631

Date: 10/25/2011

Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg

Lab ID True Value Result Units REC & Limits

1100738-IBL1 8.42 pg of Hg

1100738-IBL2 8.90 pg of Hg

1100738-IBL3 7.23 pg of Hg

1100738-IBL4 8.50 pg of Hg

1100738-CAL1 25.00 24.03 pg of Hg 96%

1100738-CAL2 100.0 99.48 pg of Hg 99%

1100738-CAL3 500.0 511.0 pg of Hg 102%

1100738-CAL4 2500 2549 pg of Hg 102%

1100738-CAL5 10000 10050 pg of Hg 100%

1100738-ICV1 1568 1444 pg of Hg 92% 85-115

1100738-CCB1 12.1 pg of Hg

1100738-CCV1 500.0 514.6 pg of Hg 103% 77-123

1100738-CCB2 8.55 pg of Hg

1100738-CCV2 500.0 497.9 pg of Hg 100% 77-123

1100738-CCB3 37.1 pg of Hg

1100738-CCV3 500.0 512.1 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 13 of 32
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Sample Containers

Lab ID: 1142045-01 Report Matrix: Influent

Sample: BioReactor 1 Inf Sample Type: Sample Received: 10/14/2011

Collected: 10/12/2011

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

A 71443390

30

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

Lab ID: 1142045-02 Report Matrix: DIW

Sample: BioReactor 1 Inf Hg Blk Sample Type: Field Blank Received: 10/14/2011

Collected: 10/12/2011

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

A 71443390

30

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

Lab ID: 1142045-03 Report Matrix: Effluent

Sample: BioReactor 2 Eff Sample Type: Sample Received: 10/14/2011

Collected: 10/12/2011

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

A 71443390

30

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

Lab ID: 1142045-04 Report Matrix: DIW

Sample: BioReactor 2 Eff Hg Blk Sample Type: Field Blank Received: 10/14/2011

Collected: 10/12/2011

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

A 71443390

30

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

Shipping Containers

Cooler

Tracking No: 472679664810 via FedEx

Temperature: 3.6 °C

Coolant Type: Ice

Description: Cooler

Damaged in transit? No

Returned to client? No

Custody seals present? No

Custody seals intact? No

COC present? Yes

Received: October 14, 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 32
Page 15 of 32
This data package contains the analytical results for the project identified above and includes a Case Narrative, Sample 

Results and Chain of Custody. Unless otherwise noted, all samples were received in acceptable condition and processed 

according to the referenced methods. 

Data qualifiers are flagged individually on each sample. A key reference for the data qualifiers appears at the end of this case 

narrative.

NC Certification No. 402

SC Certification No. 99012

NC Drinking Water Cert No. 37735

Case Narrative

10/20/2011

Duke Energy Corporation (04)

Jay Perkins

13339 Hagers Ferry Road

Huntersville, NC 28078

Project: HAPS/MACT Testing Belews Creek

Project No.: J11100235

Lab Submittal Date: 10/13/2011

Prism Work Order: 1100368

Please call if you have any questions relating to this analytical report.

Respectfully,

PRISM LABORATORIES, INC.

VP Laboratory Services Reviewed By

Data Qualifiers Key Reference:

HT Sample received and analyzed outside of the hold time.

MDL Method Detection Limit

BRL Below Reporting Limit

RPD Relative Percent Difference

*

Results reported to the reporting limit. All other results are reported to the MDL with values between MDL and 

reporting limit indicated with a J.

This report should not be reproduced, except in its entirety, without the written consent of Prism Laboratories, Inc.

449 Springbrook Road - P.O. Box 240543 - Charlotte, NC 28224-0543

Phone: 704/529-6364 - Toll Free Number: 1-800/529-6364 - Fax: 704/525-0409 Page 1 of 8

Page 16 of 32
Sample Receipt Summary

10/20/2011

Prism Work Order: 1100368

Client Sample ID Lab Sample ID Matrix Date Sampled Date Received

2011022452/FGD Purge Eff 1100368-01 Water 10/12/11 10/13/11

2011022453/BioReactor 1 Inf 1100368-02 Water 10/12/11 10/13/11

2011022454/BioReactor 2 Eff 1100368-03 Water 10/12/11 10/13/11

Samples received in good condition at 2.1 degrees C unless otherwise noted.

This report should not be reproduced, except in its entirety, without the written consent of Prism Laboratories, Inc.

449 Springbrook Road - P.O. Box 240543 - Charlotte, NC 28224-0543

Phone: 704/529-6364 - Toll Free Number: 1-800/529-6364 - Fax: 704/525-0409 Page 2 of 8

Page 17 of 32
Laboratory Report

10/20/2011

Parameter Result Batch

ID

Report

Limit

Analysis

Date/Time

Dilution Method

Factor

Units MDL Analyst

13339 Hagers Ferry Road Project No.: 

Project: HAPS/MACT Testing Belews 

Creek

Duke Energy Corporation (04)

Huntersville, NC 28078

Attn: Jay Perkins

Sample Matrix: Water

Client Sample ID: 

Prism Sample ID: 1100368-01

Prism Work Order: 1100368

Time Collected: 10/12/11 00:00

Time Submitted: 10/13/11 16:25

2011022452/FGD Purge Eff

J11100235

General Chemistry Parameters

pH 6.8 HT pH Units 1 *SM4500-H B 10/14/11 11:50 JAB P1J0265

Total Alkalinity 54 mg/L 5.0 1.4 1 *SM2320 B 10/19/11 10:50 JAB P1J0357

Carbonate Alkalinity BRL mg/L 5.0 1.4 1 *SM2320 B 10/19/11 10:50 JAB P1J0358

Bicarbonate Alkalinity 54 mg/L 5.0 1.4 1 *SM2320 B 10/19/11 10:50 JAB P1J0359

This report should not be reproduced, except in its entirety, without the written consent of Prism Laboratories, Inc.

449 Springbrook Road - P.O. Box 240543 - Charlotte, NC 28224-0543

Phone: 704/529-6364 - Toll Free Number: 1-800/529-6364 - Fax: 704/525-0409 Page 3 of 8

Page 18 of 32
Laboratory Report

10/20/2011

Parameter Result Batch

ID

Report

Limit

Analysis

Date/Time

Dilution Method

Factor

Units MDL Analyst

13339 Hagers Ferry Road Project No.: 

Project: HAPS/MACT Testing Belews 

Creek

Duke Energy Corporation (04)

Huntersville, NC 28078

Attn: Jay Perkins

Sample Matrix: Water

Client Sample ID: 

Prism Sample ID: 1100368-02

Prism Work Order: 1100368

Time Collected: 10/12/11 09:15

Time Submitted: 10/13/11 16:25

2011022453/BioReactor 1 Inf

J11100235

General Chemistry Parameters

pH 7.1 HT pH Units 1 *SM4500-H B 10/14/11 11:50 JAB P1J0265

Total Alkalinity 39 mg/L 5.0 1.4 1 *SM2320 B 10/19/11 10:50 JAB P1J0357

Carbonate Alkalinity BRL mg/L 5.0 1.4 1 *SM2320 B 10/19/11 10:50 JAB P1J0358

Bicarbonate Alkalinity 39 mg/L 5.0 1.4 1 *SM2320 B 10/19/11 10:50 JAB P1J0359

This report should not be reproduced, except in its entirety, without the written consent of Prism Laboratories, Inc.

449 Springbrook Road - P.O. Box 240543 - Charlotte, NC 28224-0543

Phone: 704/529-6364 - Toll Free Number: 1-800/529-6364 - Fax: 704/525-0409 Page 4 of 8

Page 19 of 32
Laboratory Report

10/20/2011

Parameter Result Batch

ID

Report

Limit

Analysis

Date/Time

Dilution Method

Factor

Units MDL Analyst

13339 Hagers Ferry Road Project No.: 

Project: HAPS/MACT Testing Belews 

Creek

Duke Energy Corporation (04)

Huntersville, NC 28078

Attn: Jay Perkins

Sample Matrix: Water

Client Sample ID: 

Prism Sample ID: 1100368-03

Prism Work Order: 1100368

Time Collected: 10/12/11 09:25

Time Submitted: 10/13/11 16:25

2011022454/BioReactor 2 Eff

J11100235

General Chemistry Parameters

pH 7.0 HT pH Units 1 *SM4500-H B 10/14/11 11:50 JAB P1J0265

Total Alkalinity 130 mg/L 5.0 1.4 1 *SM2320 B 10/19/11 10:50 JAB P1J0357

Carbonate Alkalinity BRL mg/L 5.0 1.4 1 *SM2320 B 10/19/11 10:50 JAB P1J0358

Bicarbonate Alkalinity 130 mg/L 5.0 1.4 1 *SM2320 B 10/19/11 10:50 JAB P1J0359

This report should not be reproduced, except in its entirety, without the written consent of Prism Laboratories, Inc.

449 Springbrook Road - P.O. Box 240543 - Charlotte, NC 28224-0543

Phone: 704/529-6364 - Toll Free Number: 1-800/529-6364 - Fax: 704/525-0409 Page 5 of 8

Page 20 of 32
10/20/11

Level II QC Report

13339 Hagers Ferry Road Project No: J11100235

Project: HAPS/MACT Testing Belews 

Creek

Duke Energy Corporation (04)

Huntersville, NC 28078

Attn: Jay Perkins

Prism Work Order: 1100368

Time Submitted: 10/13/2011 4:25:00PM

Result Limit

Reporting

Units Level

Spike

Result

Source

%REC

%REC

Limits RPD

RPD

 Analyte Limit Notes 

General Chemistry Parameters - Quality Control

Batch P1J0265 - NO PREP

LCS (P1J0265-BS1) Prepared & Analyzed: 10/14/11 

pH 6.83 pH Units 6.860 100 99-101

Duplicate (P1J0265-DUP1) Source: 1100368-03 Prepared & Analyzed: 10/14/11 

pH 6.95 pH Units 6.97 0.3 10

Batch P1J0357 - NO PREP

Blank (P1J0357-BLK1) Prepared & Analyzed: 10/19/11 

Total Alkalinity BRL 5.0 mg/L

LCS (P1J0357-BS1) Prepared & Analyzed: 10/19/11 

Total Alkalinity 255 5.0 mg/L 250.0 102 90-110

LCS Dup (P1J0357-BSD1) Prepared & Analyzed: 10/19/11 

Total Alkalinity 255 5.0 mg/L 250.0 102 90-110 0 200

Duplicate (P1J0357-DUP1) Source: 1100368-03 Prepared & Analyzed: 10/19/11 

Total Alkalinity 135 5.0 mg/L 131 3 20

Batch P1J0358 - NO PREP

Blank (P1J0358-BLK1) Prepared & Analyzed: 10/19/11 

Carbonate Alkalinity BRL 5.0 mg/L

LCS (P1J0358-BS1) Prepared & Analyzed: 10/19/11 

Carbonate Alkalinity 255 5.0 mg/L 90-110

This report should not be reproduced, except in its entirety, without the written consent of Prism Laboratories, Inc.

449 Springbrook Road - P.O. Box 240543 - Charlotte, NC 28224-0543

Phone: 704/529-6364 - Toll Free Number: 1-800/529-6364 - Fax: 704/525-0409 Page 6 of 8

Page 21 of 32
10/20/11

Level II QC Report

13339 Hagers Ferry Road Project No: J11100235

Project: HAPS/MACT Testing Belews 

Creek

Duke Energy Corporation (04)

Huntersville, NC 28078

Attn: Jay Perkins

Prism Work Order: 1100368

Time Submitted: 10/13/2011 4:25:00PM

Result Limit

Reporting

Units Level

Spike

Result

Source

%REC

%REC

Limits RPD

RPD

 Analyte Limit Notes 

General Chemistry Parameters - Quality Control

Batch P1J0358 - NO PREP

LCS Dup (P1J0358-BSD1) Prepared & Analyzed: 10/19/11 

Carbonate Alkalinity 255 5.0 mg/L 90-110 0 200

Duplicate (P1J0358-DUP1) Source: 1100368-03 Prepared & Analyzed: 10/19/11 

Carbonate Alkalinity BRL 5.0 mg/L BRL 20

Batch P1J0359 - NO PREP

Blank (P1J0359-BLK1) Prepared & Analyzed: 10/19/11 

Bicarbonate Alkalinity BRL 5.0 mg/L

LCS (P1J0359-BS1) Prepared & Analyzed: 10/19/11 

Bicarbonate Alkalinity 255 5.0 mg/L 250.0 102 90-110

LCS Dup (P1J0359-BSD1) Prepared & Analyzed: 10/19/11 

Bicarbonate Alkalinity 255 5.0 mg/L 250.0 102 90-110 0 200

Duplicate (P1J0359-DUP1) Source: 1100368-03 Prepared & Analyzed: 10/19/11 

Bicarbonate Alkalinity 135 5.0 mg/L 131 3 20

This report should not be reproduced, except in its entirety, without the written consent of Prism Laboratories, Inc.

449 Springbrook Road - P.O. Box 240543 - Charlotte, NC 28224-0543

Phone: 704/529-6364 - Toll Free Number: 1-800/529-6364 - Fax: 704/525-0409 Page 7 of 8

Page 22 of 32
Page 8 of 8

Page 23 of 32
 

October 21, 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 # J11100235) 

Dear Mr. Perkins, 

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

speciation analysis on October 13, 2011. The samples were received on October 14, 2011 in a 

sealed cooler at 0.7°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 24 of 32
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 # J11100235) 

October 21, 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 13, 2011. The 

samples were received on October 14, 2011 in a sealed container at 0.7°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 

Page 25 of 32
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 17-18, 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 with 

the following exceptions: 

The recoveries associated with the matrix spike (MS) and matrix spike duplicate (MSD) 

performed on the sample identified as FGD Purge Eff were below the established control 

limit of 75% for selenocyanate (54.4% and 51.2%, respectively). The MS and MSD also 

included selenite in the spiking solution which yielded elevated recoveries (139.1% and 

143.3%, respectively). The low recoveries for selenocyanate correlate with the elevated 

recoveries of selenite suggesting that the sample matrix induces species conversion. The fact 

that no species conversion was observed in the ICV or CCVs, which contain both selenite 

and selenocyanate, demonstrates that the applied method stabilizes these selenium species in 

solution. Since the conversion of selenocyanate to selenite in the MS and MSD is a function 

of the sample matrix and the recoveries confirm a mass balance, no corrective action was 

required. The reported results are deemed representative of the supplied samples and suggest 

that selenocyanate is not stable in the spiked sample matrix. 

Page 26 of 32
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. 

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 

Page 27 of 32
Sample Results

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

Unknown Se 

Species (n)

FGD Purge Eff 12.0 973 ND (<1.3) ND (<1.5) ND (<1.5) 0 (0)

BioReactor 1 Inf 13.3 995 ND (<0.34) 1.56 ND (<0.37) 0 (0)

BioReactor 2 Eff 2.19 3.70 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 21, 2011

LIMS #J11100235

Page 28 of 32
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 #J11100235

Date: October 21, 2011

Report Generated by: Ben Wozniak

Page 29 of 32
Quality Control Summary - Matrix Duplicates

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

Se(IV) FGD Purge Eff 12.0 11.9 11.9 0.8

Se(VI) FGD Purge Eff 973.3 1020 996.7 4.7

SeCN FGD Purge Eff ND (<1.3) ND (<1.3) NC NC

MeSe(IV) FGD Purge Eff ND (<1.5) ND (<1.5) NC NC

SeMe FGD Purge Eff ND (<1.5) ND (<1.5) 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) FGD Purge Eff 1112 1559 139.1** 1112 1606 143.3** 3.0

Se(VI) FGD Purge Eff 1009 2025 101.9 1009 2077 107.1 2.6

SeCN FGD Purge Eff 915.0 497.9 54.4** 915.0 468.2 51.2** 6.1

** The recovery is outside the established control limits of 75-125%; please see narrative

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: HAPS/MACT Testing Belews Creek

Contact: Jay Perkins

LIMS #J11100235

Date: October 21, 2011

Report Generated by: Ben Wozniak

Page 30 of 32
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