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: J11110004

Lab Contact: Jason C Perkins

Date: 11/22/2011

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 29
Sample ID's & Descriptions:

Sample ID Plant/Station

Collection 

Date and Time Collected By Sample Description

2011023685 BELEWS 09-Nov-11 7:30 AM W. B. WORKMAN FGD Purge Eff 

2011023686 BELEWS 09-Nov-11 7:35 AM W. B. WORKMAN EQ TANK EFF. 

2011023687 BELEWS 09-Nov-11 7:40 AM W. B. WORKMAN BIOREACTOR 1 INF. 

2011023688 BELEWS 09-Nov-11 7:45 AM W. B. WORKMAN BIOREACTOR 2 INF. 

2011023689 BELEWS 09-Nov-11 7:50 AM W. B. WORKMAN BIOREACTOR 2 EFF. 

2011023692 BELEWS 09-Nov-11 7:55 AM W. B. WORKMAN FILTER BLANK 

2011023693 BELEWS 09-Nov-11 8:00 AM W. B. WORKMAN Trip Blank 

2011023694 BELEWS 09-Nov-11 1:10 PM DAVID MORRIS BIOREACTOR 1 INF. 

2011023695 BELEWS 09-Nov-11 1:10 PM DAVID MORRIS HG BLANK BIOREACTOR 1 INF. 

2011023696 BELEWS 09-Nov-11 1:20 PM DAVID MORRIS BIOREACTOR 2 INF. 

2011023697 BELEWS 09-Nov-11 1:20 PM DAVID MORRIS Hg Blk BioReactor 2 Inf 

2011023698 BELEWS 09-Nov-11 1:15 PM DAVID MORRIS BIOREACTOR 2 EFF. 

2011023699 BELEWS 09-Nov-11 1:15 PM DAVID MORRIS Hg Blk BioReactor 2 Eff 

13 Total Samples

Page 2 of 29
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: 11/22/2011

Yes

Electronic Data Deliverable (EDD) Sent Separately

Page 3 of 29
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11110004

2011023685

Collection Date: 09-Nov-11 7:30 AM

Site: FGD Purge Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

INORGANIC IONS BY IC

Bromide 94 mg/L EPA 300.0 5 15-Nov-11 00:21 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 247 ug/L EPA 245.1 5 18-Nov-11 08:44 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 158 mg/L EPA 200.7 0.5 15-Nov-11 14:39 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 267 ug/L EPA 200.8 10 14-Nov-11 11:47 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 164 ug/L EPA 200.8 10 15-Nov-11 11:55 KRICHAR

Chromium (Cr) 191 ug/L 10 EPA 200.8 15-Nov-11 11:55 KRICHAR

Copper (Cu) 106 ug/L 10 EPA 200.8 15-Nov-11 11:55 KRICHAR

Nickel (Ni) 172 ug/L 10 EPA 200.8 15-Nov-11 11:55 KRICHAR

Selenium (Se) 4220 ug/L 10 EPA 200.8 15-Nov-11 11:55 KRICHAR

Silver (Ag) < 10 ug/L 10 EPA 200.8 15-Nov-11 11:55 KRICHAR

Zinc (Zn) 203 ug/L 20 EPA 200.8 15-Nov-11 11:55 KRICHAR

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

TOTAL DISSOLVED SOLIDS

TDS 17000 mg/L SM2540C 200 15-Nov-11 14:50 TJA7067

2011023686

Collection Date: 09-Nov-11 7:35 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) 173 ug/L EPA 245.1 2.5 18-Nov-11 08:46 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 156 mg/L EPA 200.7 0.5 15-Nov-11 14:43 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 195 ug/L EPA 200.8 10 14-Nov-11 11:51 KRICHAR

Page 4 of 29
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11110004

2011023686

Collection Date: 09-Nov-11 7:35 AM

Site: EQ TANK EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 137 ug/L EPA 200.8 10 15-Nov-11 11:58 KRICHAR

Chromium (Cr) 155 ug/L 10 EPA 200.8 15-Nov-11 11:58 KRICHAR

Copper (Cu) 87.6 ug/L 10 EPA 200.8 15-Nov-11 11:58 KRICHAR

Nickel (Ni) 157 ug/L 10 EPA 200.8 15-Nov-11 11:58 KRICHAR

Selenium (Se) 3690 ug/L 10 EPA 200.8 15-Nov-11 11:58 KRICHAR

Silver (Ag) < 10 ug/L 10 EPA 200.8 15-Nov-11 11:58 KRICHAR

Zinc (Zn) 177 ug/L 20 EPA 200.8 15-Nov-11 11:58 KRICHAR

2011023687

Collection Date: 09-Nov-11 7:40 AM

Site: BIOREACTOR 1 INF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 151 mg/L EPA 200.7 0.5 15-Nov-11 14:47 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 137 ug/L EPA 200.8 10 14-Nov-11 11:54 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L EPA 200.8 10 15-Nov-11 12:01 KRICHAR

Chromium (Cr) < 10 ug/L 10 EPA 200.8 15-Nov-11 12:01 KRICHAR

Copper (Cu) < 10 ug/L 10 EPA 200.8 15-Nov-11 12:01 KRICHAR

Nickel (Ni) 57.9 ug/L 10 EPA 200.8 15-Nov-11 12:01 KRICHAR

Selenium (Se) 130 ug/L 10 EPA 200.8 15-Nov-11 12:01 KRICHAR

Silver (Ag) < 10 ug/L 10 EPA 200.8 15-Nov-11 12:01 KRICHAR

Zinc (Zn) < 20 ug/L 20 EPA 200.8 15-Nov-11 12:01 KRICHAR

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2011023688

Collection Date: 09-Nov-11 7:45 AM

Site: BIOREACTOR 2 INF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 153 mg/L EPA 200.7 0.5 15-Nov-11 14:51 DJSULL1

Page 5 of 29
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11110004

2011023688

Collection Date: 09-Nov-11 7:45 AM

Site: BIOREACTOR 2 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 15-Nov-11 12:05 KRICHAR

Chromium (Cr) < 10 ug/L 10 EPA 200.8 15-Nov-11 12:05 KRICHAR

Copper (Cu) < 10 ug/L 10 EPA 200.8 15-Nov-11 12:05 KRICHAR

Nickel (Ni) < 10 ug/L 10 EPA 200.8 15-Nov-11 12:05 KRICHAR

Selenium (Se) 14.6 ug/L 10 EPA 200.8 15-Nov-11 12:05 KRICHAR

Silver (Ag) < 10 ug/L 10 EPA 200.8 15-Nov-11 12:05 KRICHAR

Zinc (Zn) < 20 ug/L 20 EPA 200.8 15-Nov-11 12:05 KRICHAR

2011023689

Collection Date: 09-Nov-11 7:50 AM

Site: BIOREACTOR 2 EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

INORGANIC IONS BY IC

Bromide 88 mg/L EPA 300.0 5 15-Nov-11 00:37 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) < 1 ug/L EPA 245.1 1 18-Nov-11 09:03 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 166 mg/L EPA 200.7 0.5 15-Nov-11 14:55 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 5 ug/L EPA 200.8 5 15-Nov-11 12:08 KRICHAR

Chromium (Cr) < 5 ug/L 5 EPA 200.8 15-Nov-11 12:08 KRICHAR

Copper (Cu) < 5 ug/L 5 EPA 200.8 15-Nov-11 12:08 KRICHAR

Nickel (Ni) < 5 ug/L 5 EPA 200.8 15-Nov-11 12:08 KRICHAR

Selenium (Se) < 5 ug/L 5 EPA 200.8 15-Nov-11 12:08 KRICHAR

Silver (Ag) < 5 ug/L 5 EPA 200.8 15-Nov-11 12:08 KRICHAR

Zinc (Zn) < 10 ug/L 10 EPA 200.8 15-Nov-11 12:08 KRICHAR

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2011023692

Collection Date: 09-Nov-11 7:55 AM

Site: FILTER BLANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

DISSOLVED METALS BY ICP-MS

Selenium (Se) 1.10 ug/L EPA 200.8 1 14-Nov-11 11:31 KRICHAR

Page 6 of 29
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11110004

2011023693

Collection Date: 09-Nov-11 8:00 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 15-Nov-11 14:23 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 1 ug/L EPA 200.8 1 15-Nov-11 11:43 KRICHAR

Chromium (Cr) < 1 ug/L 1 EPA 200.8 15-Nov-11 11:43 KRICHAR

Copper (Cu) < 1 ug/L 1 EPA 200.8 15-Nov-11 11:43 KRICHAR

Nickel (Ni) < 1 ug/L 1 EPA 200.8 15-Nov-11 11:43 KRICHAR

Selenium (Se) < 1 ug/L 1 EPA 200.8 15-Nov-11 11:43 KRICHAR

Silver (Ag) < 1 ug/L 1 EPA 200.8 15-Nov-11 11:43 KRICHAR

Zinc (Zn) < 2 ug/L 2 EPA 200.8 15-Nov-11 11:43 KRICHAR

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2011023694

Collection Date: 09-Nov-11 1:10 PM

Site: BIOREACTOR 1 INF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY 1631

Vendor Parameter Complete V_BRAND

2011023695

Collection Date: 09-Nov-11 1:10 PM

Site: HG BLANK BIOREACTOR 1 INF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY 1631

Vendor Parameter Complete V_BRAND

2011023696

Collection Date: 09-Nov-11 1:20 PM

Site: BIOREACTOR 2 INF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY 1631

Vendor Parameter Complete V_BRAND

Page 7 of 29
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11110004

2011023697

Collection Date: 09-Nov-11 1:20 PM

Site: Hg Blk BioReactor 2 Inf 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY 1631

Vendor Parameter Complete V_BRAND

2011023698

Collection Date: 09-Nov-11 1:15 PM

Site: BIOREACTOR 2 EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY 1631

Vendor Parameter Complete V_BRAND

2011023699

Collection Date: 09-Nov-11 1:15 PM

Site: Hg Blk BioReactor 2 Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY 1631

Vendor Parameter Complete V_BRAND

Page 8 of 29
 

November 14, 2011 

Jay Perkins 

Duke Energy Analytical Laboratory 

Mail Code MGO3A2 (Building 7405) 

13339 Hagers Ferry Rd. 

Huntersville, NC 28078 

(704) 875-5245 

Project: Belews – FGD WWTS Bi-Monthly Sampling) (LIMS # J11110004) 

Dear Mr. Perkins, 

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

speciation analysis on November 10, 2011. The samples were received in a sealed cooler at -

0.3°C on November 11, 2011. Selenium speciation analysis was performed via ion 

chromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICPDRC-MS). Any issues associated with the analysis are addressed in the following report. 

If you have any questions, please feel free to contact me at your convenience. 

 Sincerely, 

 

 Russell Gerads 

 Vice President 

 Applied Speciation and Consulting, LLC 

 

Page 9 of 29
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: Belews – FGD WWTS Bi-Monthly Sampling) (LIMS # J11110004) 

November 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 November 10, 2011. The 

samples were received on November 11, 2011 in a sealed container at -0.3°C. 

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

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

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

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

via ion chromatography inductively coupled plasma dynamic reaction cell mass spectrometry 

(IC-ICP-DRC-MS). 

2. Sample Preparation 

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

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

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

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

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

autosampler vial. No further sample preparation was performed as any chemical alteration of 

a sample may shift the equilibrium of the system, resulting in changes in speciation ratios. 

3. Sample Analysis 

All sample analysis is preceded by a minimum of a five-point calibration curve spanning the 

entire concentration range of interest. Calibration curves are performed at the beginning of 

Page 10 of 29
each analytical day. All calibration curves, associated with each species of interest, are 

standardized by linear regression resulting in a response factor. All sample results are 

instrument blank corrected to account for any operational biases associated with the 

analytical platform. 

Prior to sample analysis, all calibration curves are verified using second source standards 

which are identified as initial calibration verification standards (ICV). 

Ongoing instrument performance is identified by the analysis of continuing calibration 

verification standards (CCV) and continuing calibration blanks (CCB) at a minimal interval 

of every ten analytical runs. 

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

analysis was analyzed by ion chromatography inductively coupled plasma dynamic reaction 

cell mass spectrometry (IC-ICP-DRC-MS) on November 11, 2011. An aliquot of each

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

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

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

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

travel through a pressurized chamber (DRC) containing a specific reactive gas which 

preferentially reacts with interfering ions of the same target mass to charge ratios (m/z). A 

solid-state detector detects ions transmitted through the mass analyzer and the resulting 

current is processed by a data handling system. 

Retention times for each eluting species are compared to known standards for species 

identification. 

4. Analytical Issues 

The overall analyses went well and no significant analytical issues were encountered. All 

quality control parameters associated with this sample were within acceptance limits.

The estimated method detection limits (eMDLs) for selenite, selenate, and selenocyanate are 

generated from replicate analyses of the lowest standard in the calibration curve. Not all 

selenium species are present in preparation blanks; therefore, eMDL calculations based on 

preparation blanks are artificially biased low. 

The eMDL for methylseleninic acid and selenomethionine is calculated from the average 

eMDL of selenite, selenate, and selenocyanate. The calibration does not contain 

methylseleninic acid or selenomethionine due to impurities in these standards which would 

bias the results for other selenium species. 

All selenium speciation results have been corrected for instrument drift in accordance with 

the continuing calibration verification standards. All quality control parameters were within 

acceptance limits signifying that the applied correction was appropriate. 

Page 11 of 29
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 12 of 29
Sample Results

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

Unknown Se 

Species (n)

FGD Purge Eff 176 68.9 ND (<4.3) ND (<5.1) ND (<5.1) 4.8 (1)

BioReactor 1 Inf 46.5 63.9 ND (<1.1) 4.7 ND (<1.3) 0 (0)

BioRector 2 Eff ND (<1.2) ND (<1.5) ND (<1.1) ND (<1.3) ND (<1.3) 0 (0)

Metals Trip Blk ND (<0.24) ND (<0.30) ND (<0.22) ND (<0.25) ND (<0.25) 0 (0)

All results reflect the applied dilution and are reported in μg/L

ND = Not detected at the applied dilution

SeCN = Selenocyanate

MeSe(IV) = Methylseleninic acid

SeMe = Selenomethionine

Unknown Se Species = Total concentration of all unknown Se species observed by IC-ICP-MS

n = number of unknown Se species observed

Report Generated by: Russell Gerads

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Belews - FGD WWTS Bi-Monthly Sampling

Contact: Jay Perkins

Date: November 14, 2011

LIMS #J11110004

Page 13 of 29
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 0.024 0.24 1.2 4.8

Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.030 0.30 1.5 6.1

SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.022 0.22 1.1 4.3

MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.025 0.25 1.3 5.1

SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.025 0.25 1.3 5.1

eMDL = Estimated Method Detection Limit

*Please see narrative regarding eMDL calculations

Quality Control Summary - Certified Reference Materials

Analyte (μg/L) CRM True Value Result Recovery

Se(IV) LCS 9.57 9.76 102.0

Se(VI) LCS 9.48 9.55 100.8

SeCN LCS 8.92 9.43 105.8

MeSe(IV) LCS 6.47 6.38 98.6

SeMe LCS 9.32 9.64 103.5

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Belews - FGD WWTS Bi-Monthly Sampling

Contact: Jay Perkins

LIMS #J11110004

Date: November 14, 2011

Report Generated by: Russell Gerads

Page 14 of 29
Quality Control Summary - Matrix Duplicates

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

Se(IV) FGD Purge Eff 176.2 166.6 171.4 5.6

Se(VI) FGD Purge Eff 68.9 71.0 70.0 3.1

SeCN FGD Purge Eff ND (<4.3) ND (<4.3) NC NC

MeSe(IV) FGD Purge Eff ND (<5.1) ND (<5.1) NC NC

SeMe FGD Purge Eff ND (<5.1) ND (<5.1) 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 1325 103.7 1112 1358 106.7 2.5

Se(VI) FGD Purge Eff 1009 1093 101.4 1009 1091 101.1 0.2

SeCN FGD Purge Eff 915.0 868.8 95.0 915.0 878.4 96.0 1.1

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Belews - FGD WWTS Bi-Monthly Sampling

Contact: Jay Perkins

LIMS #J11110004

Date: November 14, 2011

Report Generated by: Russell Gerads

Page 15 of 29
Page 16 of 29
 

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

November 21, 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: J11110004 

Dear Mr. Perkins, 

On November 11, 2011, Brooks Rand Labs (BRL) received three (3) wastewater samples and 

three (3) corresponding field blanks. Samples were logged-in for total mercury (Hg) analysis. All 

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

methodology. 

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

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

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

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

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

page of the report. 

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

Sincerely, 

 

Tiffany Stilwater 

Project Manager 

tiffany@brooksrand.com 

Page 17 of 29
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 18 of 29
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 1146034-01 FGD Wastewater Sample 11/09/2011 11/11/2011

Hg Blk BioReactor 1 Inf 1146034-02 DIW Field Blank 11/09/2011 11/11/2011

BioReactor 2 Inf 1146034-03 FGD Wastewater QC Sample 11/09/2011 11/11/2011

Hg Blk BioReactor 2 Inf 1146034-04 DIW Field Blank 11/09/2011 11/11/2011

BioReactor 2 Eff 1146034-05 FGD Wastewater QC Sample 11/09/2011 11/11/2011

Hg Blk BioReactor 2 Eff 1146034-06 DIW Field Blank 11/09/2011 11/11/2011

Batch Summary

Analyte Lab Matrix Method Prepared Analyzed Batch Sequence

Hg Water EPA 1631 11/17/2011 11/18/2011 B111855 1100817

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

Page 19 of 29
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

1146034-01 Hg FGD Wastewater T 158 1.52 4.04 ng/L B111855 1100817

BioReactor 2 Eff

1146034-05 Hg FGD Wastewater T 86.8 1.52 4.04 ng/L B111855 1100817

BioReactor 2 Inf

1146034-03 Hg FGD Wastewater T 152 1.52 4.04 ng/L B111855 1100817

Hg Blk BioReactor 1 Inf

1146034-02 Hg DIW T 0.15 U 0.15 0.40 ng/L B111855 1100817

Hg Blk BioReactor 2 Eff

1146034-06 Hg DIW T 0.15 U 0.15 0.40 ng/L B111855 1100817

Hg Blk BioReactor 2 Inf

1146034-04 Hg DIW T 0.15 U 0.15 0.41 ng/L B111855 1100817

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

Page 20 of 29
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Accuracy & Precision Summary

Batch: B111855

Analyte Native Spike Result Units REC & Limits RPD & Limits

Method: EPA 1631

Lab Matrix: Water

Sample

B111855-SRM1 Certified Reference Material (1145032, NIST 1641d 1000x dilution)

Hg 15.68 15.46 ng/L 99% 85-115

B111855-MS4 Matrix Spike (1146034-03)

Hg 152.2 606.1 879.9 ng/L 120% 71-125

B111855-MSD4 Matrix Spike Duplicate (1146034-03)

Hg 152.2 606.1 846.4 ng/L 115% 71-125 244%

B111855-MS3 Matrix Spike (1146034-05)

Hg 86.76 404.0 518.9 ng/L 107% 71-125

B111855-MSD3 Matrix Spike Duplicate (1146034-05)

Hg 86.76 404.0 525.5 ng/L 109% 71-125 241%

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

Page 21 of 29
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Method Blanks & Reporting Limits

Batch: B111855

Method: EPA 1631

Matrix: Water

Analyte: Hg

Sample Result Units

B111855-BLK1 0.09 ng/L

B111855-BLK2 0.05 ng/L

B111855-BLK3 0.09 ng/L

B111855-BLK4 0.07 ng/L

Average: 0.08 Standard Deviation: 0.02 MDL: 0.15

Limit: 0.50 Limit: 0.10 MRL: 0.40

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

Page 22 of 29
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Instrument Calibration

Sequence: 1100817

Instrument: THG-10 Method: EPA 1631

Date: 11/18/2011

Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg

Lab ID True Value Result Units REC & Limits

1100817-IBL1 4.33 pg of Hg

1100817-IBL2 6.20 pg of Hg

1100817-IBL3 5.46 pg of Hg

1100817-IBL4 5.40 pg of Hg

1100817-CAL1 25.00 25.61 pg of Hg 102%

1100817-CAL2 100.0 103.0 pg of Hg 103%

1100817-CAL3 500.0 477.3 pg of Hg 95%

1100817-CAL4 2500 2539 pg of Hg 102%

1100817-CAL5 10000 9801 pg of Hg 98%

1100817-ICV1 1568 1546 pg of Hg 99% 85-115

1100817-CCB1 8.48 pg of Hg

1100817-CCV1 500.0 493.6 pg of Hg 99% 77-123

1100817-CCV2 500.0 552.6 pg of Hg 111% 77-123

1100817-CCV3 500.0 505.6 pg of Hg 101% 77-123

1100817-CCV4 500.0 445.5 pg of Hg 89% 77-123

1100817-CCV5 500.0 524.3 pg of Hg 105% 77-123

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

Page 23 of 29
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Sample Containers

Lab ID: 1146034-01 Report Matrix: FGD Wastewater

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

Collected: 11/09/2011

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

A 71470160

10

Cardboard 

Box

Bottle FLPE Hg-T 250mL none n/a

Lab ID: 1146034-02 Report Matrix: DIW

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

Collected: 11/09/2011

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

A 71470160

10

Cardboard 

Box

Bottle FLPE Hg-T 250mL none n/a

Lab ID: 1146034-03 Report Matrix: FGD Wastewater

Sample: BioReactor 2 Inf Sample Type: QC Sample Received: 11/11/2011

Collected: 11/09/2011

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

A 71470160

10

Cardboard 

Box

Bottle FLPE Hg-T 250mL none n/a

Lab ID: 1146034-04 Report Matrix: DIW

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

Collected: 11/09/2011

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

A 71470160

10

Cardboard 

Box

Bottle FLPE Hg-T 250mL none n/a

Lab ID: 1146034-05 Report Matrix: FGD Wastewater

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

Collected: 11/09/2011

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

A 71490150

70

Cardboard 

Box

Bottle FLPE Hg-T 500mL none n/a

Lab ID: 1146034-06 Report Matrix: DIW

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

Collected: 11/09/2011

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

A 71470160

10

Cardboard 

Box

Bottle FLPE Hg-T 250mL 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 24 of 29
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Shipping Containers

Cardboard Box

Tracking No: 4726 7966 5796 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: November 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

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