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: J11050005

Lab Contact: Jason C Perkins

Date: 5/20/2011

Customer Address: 253 Plant Allen Road

Customer Name(s): Don Scruggs, Robbin Jolly, Ray Lidke, Bill Kennedy

Belmont, NC 28012

Phone: 980-875-5348

Report Authorized By:

(Signature)

Program Comments:

FGD BiMonthly

Data Flags & Calculations:

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

system or quality control requirement. All results are reported on a dry weight basis unless otherwise noted.

Data Package:

This data package includes analytical results that are applicable only to the samples described in this narrative. An estimation of 

the uncertainty of measurement for the results in the report is available upon request. This report shall not be reproduced, except 

in full, without the written consent of the Analytical Laboratory. Please contact the Analytical laboratory with any questions. The 

order of individual sections within this report is as follows:

Job Summary Report, Sample Identification, Technical Validation of Data Package, Analytical Laboratory Certificate of Analysis, 

Analytical Laboratory QC Reports, Sub-contracted Laboratory Results, Customer Specific Data Sheets, Reports & 

Documentation, Customer Database Entries, Test Case Narratives, Chain of Custody (COC)

Certification:

The Analytical Laboratory holds the following State Certifications : North Carolina (DENR) Certificate #248, South Carolina 

(DHEC) Laboratory ID # 99005. Contact the Analytical Laboratory for definitive information about the certification status of 

specific methods. 

Page 1 of 27
Sample ID's & Descriptions:

Sample ID Plant/Station

Collection 

Date and Time Collected By Sample Description

2011009629 ALLEN 09-May-11 9:18 AM Jeff Womack FGD Purge Eff 

2011009650 ALLEN 09-May-11 9:31 AM Jeff Womack EQ Tank Eff 

2011009651 ALLEN 09-May-11 9:27 AM Jeff Womack BioReactor 1 Inf 

2011009652 ALLEN 09-May-11 9:12 AM Jeff Womack BioReactor 2 Inf 

2011009653 ALLEN 09-May-11 9:34 AM Jeff Womack BioReactor 2 Eff 

2011009654 ALLEN 09-May-11 10:10 AM Jeff Womack Filter Blk 

2011009655 ALLEN 03-May-11 8:00 AM L. Davis Metals Trip Blank 

2011009656 ALLEN 09-May-11 10:20 AM David Morris (Prism) BioReactor 1 Inf 

2011009658 ALLEN 09-May-11 10:20 AM David Morris (Prism) Hg Blk BioReactor 1 Inf 

2011009659 ALLEN 09-May-11 10:30 AM David Morris (Prism) BioReactor 2 Inf 

2011009660 ALLEN 09-May-11 10:30 AM David Morris (Prism) Hg Blk BioReactor 2 Inf 

2011009661 ALLEN 09-May-11 10:25 AM David Morris (Prism) BioReactor 2 Eff 

2011009662 ALLEN 09-May-11 10:25 AM David Morris (Prism) Hg Blk BioReactor 2 Eff 

13 Total Samples

Page 2 of 27
COC and .pdf report are in agreement with sample totals 

and analyses (compliance programs and procedures).

All Results are less than the laboratory reporting limits.

All laboratory QA/QC requirements are acceptable.

The Vendor Laboratories have been qualified by the 

Analytical Laboratory

Yes No

Technical Validation Review

Checklist:

Yes No

Yes No

Report Sections Included:

Job Summary Report Sub-contracted Laboratory Results

Sample Identification Customer Specific Data Sheets, Reports, & Documentation

Technical Validation of Data Package Customer Database Entries

Analytical Laboratory Certificate of Analysis Test Case Narratives

Analytical Laboratory QC Report Chain of Custody

Reviewed By: DataBase Administrator Date: 5/20/2011

Yes

Electronic Data Deliverable (EDD) Sent Separately

Page 3 of 27
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11050005

2011009629

Collection Date: 09-May-11 9:18 AM

Site: FGD Purge Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 67.7 ug/L EPA 245.1 2.5 12-May-11 10:27 MHH7131

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 80.9 mg/L EPA 200.7 0.5 13-May-11 12:06 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 793 ug/L EPA 200.8 10 10-May-11 15:07 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 213 ug/L EPA 200.8 10 17-May-11 14:07 KRICHAR

Chromium (Cr) 139 ug/L 10 EPA 200.8 17-May-11 14:07 KRICHAR

Copper (Cu) 123 ug/L 10 EPA 200.8 17-May-11 14:07 KRICHAR

Nickel (Ni) 190 ug/L 10 EPA 200.8 17-May-11 14:07 KRICHAR

Selenium (Se) 1120 ug/L 10 EPA 200.8 17-May-11 14:07 KRICHAR

Silver (Ag) < 10 ug/L 10 EPA 200.8 17-May-11 14:07 KRICHAR

Zinc (Zn) 175 ug/L 20 EPA 200.8 17-May-11 14:07 KRICHAR

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

TOTAL DISSOLVED SOLIDS

TDS 19000 mg/L SM2540C 200 12-May-11 16:50 TJA7067

2011009650

Collection Date: 09-May-11 9:31 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) 46.6 ug/L EPA 245.1 2.5 12-May-11 10:29 MHH7131

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 68.4 mg/L EPA 200.7 0.5 13-May-11 12:10 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 452 ug/L EPA 200.8 10 10-May-11 15:11 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 146 ug/L EPA 200.8 10 17-May-11 13:50 KRICHAR

Chromium (Cr) 104 ug/L 10 EPA 200.8 17-May-11 13:50 KRICHAR

Copper (Cu) 100 ug/L 10 EPA 200.8 17-May-11 13:50 KRICHAR

Nickel (Ni) 144 ug/L 10 EPA 200.8 17-May-11 13:50 KRICHAR

Page 4 of 27
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11050005

2011009650

Collection Date: 09-May-11 9:31 AM

Site: EQ Tank Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

TOTAL RECOVERABLE METALS BY ICP-MS

Selenium (Se) 826 ug/L EPA 200.8 10 17-May-11 13:50 KRICHAR

Silver (Ag) < 10 ug/L 10 EPA 200.8 17-May-11 13:50 KRICHAR

Zinc (Zn) 146 ug/L 20 EPA 200.8 17-May-11 13:50 KRICHAR

2011009651

Collection Date: 09-May-11 9:27 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) 57.6 mg/L EPA 200.7 0.5 13-May-11 12:14 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 446 ug/L EPA 200.8 10 10-May-11 15:15 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L EPA 200.8 10 17-May-11 13:36 KRICHAR

Chromium (Cr) < 10 ug/L 10 EPA 200.8 17-May-11 13:36 KRICHAR

Copper (Cu) < 10 ug/L 10 EPA 200.8 17-May-11 13:36 KRICHAR

Nickel (Ni) < 10 ug/L 10 EPA 200.8 17-May-11 13:36 KRICHAR

Selenium (Se) 441 ug/L 10 EPA 200.8 17-May-11 13:36 KRICHAR

Silver (Ag) < 10 ug/L 10 EPA 200.8 17-May-11 13:36 KRICHAR

Zinc (Zn) < 20 ug/L 20 EPA 200.8 17-May-11 13:36 KRICHAR

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2011009652

Collection Date: 09-May-11 9:12 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) 58.8 mg/L EPA 200.7 0.5 13-May-11 12:18 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L EPA 200.8 10 17-May-11 13:22 KRICHAR

Chromium (Cr) < 10 ug/L 10 EPA 200.8 17-May-11 13:22 KRICHAR

Copper (Cu) < 10 ug/L 10 EPA 200.8 17-May-11 13:22 KRICHAR

Nickel (Ni) < 10 ug/L 10 EPA 200.8 17-May-11 13:22 KRICHAR

Selenium (Se) 147 ug/L 10 EPA 200.8 17-May-11 13:22 KRICHAR

Silver (Ag) < 10 ug/L 10 EPA 200.8 17-May-11 13:22 KRICHAR

Zinc (Zn) < 20 ug/L 20 EPA 200.8 17-May-11 13:22 KRICHAR

Page 5 of 27
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11050005

2011009653

Collection Date: 09-May-11 9:34 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 12-May-11 10:31 MHH7131

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 53.6 mg/L EPA 200.7 0.5 13-May-11 12:22 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 5 ug/L EPA 200.8 5 17-May-11 13:01 KRICHAR

Chromium (Cr) < 5 ug/L 5 EPA 200.8 17-May-11 13:01 KRICHAR

Copper (Cu) < 5 ug/L 5 EPA 200.8 17-May-11 13:01 KRICHAR

Nickel (Ni) < 5 ug/L 5 EPA 200.8 17-May-11 13:01 KRICHAR

Selenium (Se) < 5 ug/L 5 EPA 200.8 17-May-11 13:01 KRICHAR

Silver (Ag) < 5 ug/L 5 EPA 200.8 17-May-11 13:01 KRICHAR

Zinc (Zn) < 10 ug/L 10 EPA 200.8 17-May-11 13:01 KRICHAR

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2011009654

Collection Date: 09-May-11 10:10 AM

Site: Filter Blk 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

DISSOLVED METALS BY ICP-MS

Selenium (Se) < 2 ug/L EPA 200.8 2 10-May-11 15:19 KRICHAR

2011009655

Collection Date: 03-May-11 8:00 AM

Site: Metals 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 13-May-11 11:58 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 1 ug/L EPA 200.8 1 17-May-11 12:56 KRICHAR

Chromium (Cr) < 1 ug/L 1 EPA 200.8 17-May-11 12:56 KRICHAR

Copper (Cu) < 1 ug/L 1 EPA 200.8 17-May-11 12:56 KRICHAR

Nickel (Ni) < 1 ug/L 1 EPA 200.8 17-May-11 12:56 KRICHAR

Selenium (Se) < 1 ug/L 1 EPA 200.8 17-May-11 12:56 KRICHAR

Silver (Ag) < 1 ug/L 1 EPA 200.8 17-May-11 12:56 KRICHAR

Zinc (Zn) < 2 ug/L 2 EPA 200.8 17-May-11 12:56 KRICHAR

SELENIUM SPECIATION

Page 6 of 27
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11050005

2011009655

Collection Date: 03-May-11 8:00 AM

Site: Metals Trip Blank 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2011009656

Collection Date: 09-May-11 10:20 AM

Site: BioReactor 1 Inf 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY 1631

Vendor Parameter Complete V_BRAND

2011009658

Collection Date: 09-May-11 10:20 AM

Site: Hg Blk BioReactor 1 Inf 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY 1631

Vendor Parameter Complete V_BRAND

2011009659

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

Site: BioReactor 2 Inf 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY 1631

Vendor Parameter Complete V_BRAND

2011009660

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

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

2011009661

Collection Date: 09-May-11 10:25 AM

Site: BioReactor 2 Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY 1631

Vendor Parameter Complete V_BRAND

Page 7 of 27
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11050005

2011009662

Collection Date: 09-May-11 10:25 AM

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 27
 

May 16, 2011 

Jay Perkins 

Duke Energy Analytical Laboratory 

Mail Code MGO3A2 (Building 7405) 

13339 Hagers Ferry Rd. 

Huntersville, NC 28078 

(704) 875-5245 

Project: Allen - FGD WWTS (2010, Bi-Weekly Sampling) (LIMS # J11050005) 

Dear Mr. Perkins, 

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

speciation analysis on May 9, 2011. The samples were received on May 10, 2011 in a sealed 

cooler at -0.5

oC. 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 9 of 27
Applied Speciation and Consulting, LLC 

Report prepared for: 

Jay Perkins 

Duke Energy Analytical Laboratory 

Mail Code MGO3A2 (Building 7405) 

13339 Hagers Ferry Rd. 

Huntersville, NC 28078 

Project: Allen - FGD WWTS (2010, Bi-Weekly Sampling) (LIMS # J11050005) 

May 16, 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 May 9, 2011. The samples 

were received on May 10, 2011 in a sealed container at -0.5oC.

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 precluded by a minimum of a five-point calibration curve spanning the 

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

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

Page 10 of 27
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 May 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 very well and no analytical issues were encountered. All quality 

control parameters associated with these samples were within acceptance limits. 

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

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

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

preparation blanks are artificially biased low. 

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. 

Page 11 of 27
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 12 of 27
Sample Results

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

Unknown Se 

Species (n)

FGD Purge Eff 10.3 711 ND (<5.5) ND (<3.8) ND (<3.8) 0 (0)

BioReactor 1 Inf 8.1 431 ND (<1.4) ND (<0.96) ND (<0.96) 0 (0)

BioReactor 2 Eff ND (<1.1) ND (<0.42) ND (<1.4) ND (<0.96) ND (<0.96) 0 (0)

Metals Trip Blk ND (<0.22) ND (<0.084) ND (<0.27) ND (<0.19) ND (<0.19) 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: Allen - FGD WWTS (2010, Bi-Weekly Sampling)

Contact: Jay Perkins

Date: May 16, 2011

LIMS #J11050005

Page 13 of 27
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 0.022 0.22 1.1 4.3

Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.084 0.42 1.7

SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.027 0.27 1.4 5.5

MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.019 0.19 0.96 3.8

SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.019 0.19 0.96 3.8

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) ICV 9.57 9.55 99.8

Se(VI) ICV 9.48 9.12 96.2

SeCN ICV 8.92 8.87 99.5

MeSe(IV) ICV 6.47 5.63 87.0

SeMe ICV 9.32 9.79 105.0

LIMS #J11050005

Date: May 16, 2011

Report Generated by: Ben Wozniak

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Allen - FGD WWTS (2010, Bi-Weekly Sampling)

Contact: Jay Perkins

Page 14 of 27
Quality Control Summary - Matrix Duplicates

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

Se(IV) BioReactor 2 Eff ND (<1.1) ND (<1.1) NC NC

Se(VI) BioReactor 2 Eff ND (<0.42) ND (<0.42) NC NC

SeCN BioReactor 2 Eff ND (<1.4) ND (<1.4) NC NC

MeSe(IV) BioReactor 2 Eff ND (<0.96) ND (<0.96) NC NC

SeMe BioReactor 2 Eff ND (<0.96) ND (<0.96) 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) BioReactor 2 Eff 278.0 258.6 93.0 278.0 262.9 94.6 1.7

Se(VI) BioReactor 2 Eff 252.3 240.7 95.4 252.3 239.7 95.0 0.4

SeCN BioReactor 2 Eff 228.8 200.9 87.8 228.8 199.9 87.4 0.5

LIMS #J11050005

Date: May 16, 2011

Report Generated by: Ben Wozniak

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Allen - FGD WWTS (2010, Bi-Weekly Sampling)

Contact: Jay Perkins

Page 15 of 27
Page 16 of 27
 

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

May 19, 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: J11050005 

Dear Mr. Perkins, 

On May 10, 2011, Brooks Rand Labs (BRL) received three (3) flue gas desulfurization (FGD) 

waste water samples and three (3) field blanks. Samples were logged-in for total mercury (Hg) 

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

methodology. 

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

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

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

The results for the field blank samples, identified as Hg Blk BioReactor 1 Inf (1120006-02), and 

Hg Blk BioReactor 2 Inf (1120006-04), were less than or equal to the MDL, and as such was 

reported at the MDL and qualified U. Sample Hg Blk BioReactor 2 Eff (1120006-06) was 

identified as a field blanks and produced a detectable Hg concentration of 0.16 ng/L. The result 

was less than the method reporting limit of 0.50 ng/L and considered an insignificant source of 

contamination. This sample was qualified B and should be considered an estimate. All other 

sample results were reported unqualified. 

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 us if you have any questions regarding this report. 

Sincerely, 

 Tiffany Stilwater Michela Powell-Hernandez 

Project Manager Project Coordinator 

tiffany@brooksrand.com michela@brooksrand.com 

Page 17 of 27
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 27
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 1120006-01 FGD Wastewater Sample 05/09/2011 05/10/2011

Hg Blk BioReactor 1 Inf 1120006-02 DIW Field Blank 05/09/2011 05/10/2011

BioReactor 2 Inf 1120006-03 FGD Wastewater QC Sample 05/09/2011 05/10/2011

Hg Blk BioReactor 2 Inf 1120006-04 DIW Field Blank 05/09/2011 05/10/2011

BioReactor 2 Eff 1120006-05 FGD Wastewater Sample 05/09/2011 05/10/2011

Hg Blk BioReactor 2 Eff 1120006-06 DIW Field Blank 05/09/2011 05/10/2011

Batch Summary

Analyte Lab Matrix Method Prepared Analyzed Batch Sequence

Hg Water EPA 1631 05/11/2011 05/13/2011 B110683 1100317

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

Page 19 of 27
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

1120006-01 Hg FGD Wastewater T 80.9 1.52 4.04 ng/L B110683 1100317

BioReactor 2 Eff

1120006-05 Hg FGD Wastewater T 4.38 0.30 0.81 ng/L B110683 1100317

BioReactor 2 Inf

1120006-03 Hg FGD Wastewater T 16.1 1.53 4.08 ng/L B110683 1100317

Hg Blk BioReactor 1 Inf

1120006-02 Hg DIW T 0.15 U 0.15 0.40 ng/L B110683 1100317

Hg Blk BioReactor 2 Eff

1120006-06 Hg DIW T 0.16 B 0.15 0.40 ng/L B110683 1100317

Hg Blk BioReactor 2 Inf

1120006-04 Hg DIW T 0.15 U 0.15 0.40 ng/L B110683 1100317

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

Page 20 of 27
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Accuracy & Precision Summary

Analyte Native Spike Result Units REC & Limits RPD & Limits

Batch: B110683

Method: EPA 1631

Lab Matrix: Water

Sample

B110683-SRM1 Certified Reference Material (1120043, NIST 1641d 1000x dilution)

Hg 15.68 15.98 ng/L 102% 85-115

B110683-MS1 Matrix Spike (1120006-03)

Hg 16.14 76.53 102.1 ng/L 112% 71-125

B110683-MSD1 Matrix Spike Duplicate (1120006-03)

Hg 16.14 76.53 96.62 ng/L 105% 71-125 245%

Method Blanks & Reporting Limits

Batch: B110683

Method: EPA 1631

Matrix: Water

Analyte: Hg

Sample Result Units

B110683-BLK1 0.05 ng/L

B110683-BLK2 0.07 ng/L

B110683-BLK3 0.07 ng/L

B110683-BLK4 0.04 ng/L

Average: 0.06 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 21 of 27
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Instrument Calibration

Method: EPA 1631

Sequence: 1100317

Instrument: THG-10

Date: 05/13/2011

Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg

Lab ID True Value Result Units REC & Limits

1100317-CAL1 25.00 25.39 pg of Hg 102%

1100317-CAL2 100.0 95.00 pg of Hg 95%

1100317-CAL3 500.0 511.1 pg of Hg 102%

1100317-CAL4 2500 2517 pg of Hg 101%

1100317-CAL5 10000 10090 pg of Hg 101%

1100317-CCB1 12.4 pg of Hg

1100317-CCV1 500.0 545.6 pg of Hg 109% 77-123

1100317-CCV2 500.0 532.3 pg of Hg 106% 77-123

1100317-IBL1 7.93 pg of Hg

1100317-IBL2 7.10 pg of Hg

1100317-IBL3 6.72 pg of Hg

1100317-IBL4 8.26 pg of Hg

1100317-ICV1 1568 1598 pg of Hg 102% 85-115

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

Page 22 of 27
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Sample Containers

Lab ID: 1120006-01 Report Matrix: FGD Wastewater

Sample: BioReactor 1 Inf Sample Type: Sample Received: 05/10/2011

Collected: 05/09/2011

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

A 71062020

60

Cardboard 

Box

Bottle FLPE Hg-T 250 mL None N/A

Lab ID: 1120006-02 Report Matrix: DIW

Sample: Hg Blk BioReactor 1 Inf Sample Type: Field Blank Received: 05/10/2011

Collected: 05/09/2011

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

A 71062020

60

Cardboard 

Box

Bottle FLPE Hg-T 250 mL None N/A

Lab ID: 1120006-03 Report Matrix: FGD Wastewater

Sample: BioReactor 2 Inf Sample Type: QC Sample Received: 05/10/2011

Collected: 05/09/2011

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

A 71062020

60

Cardboard 

Box

Bottle FLPE Hg-T 250 mL None N/A

Lab ID: 1120006-04 Report Matrix: DIW

Sample: Hg Blk BioReactor 2 Inf Sample Type: Field Blank Received: 05/10/2011

Collected: 05/09/2011

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

A 71062020

60

Cardboard 

Box

Bottle FLPE Hg-T 250 mL None N/A

Lab ID: 1120006-05 Report Matrix: FGD Wastewater

Sample: BioReactor 2 Eff Sample Type: Sample Received: 05/10/2011

Collected: 05/09/2011

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

A 71062020

60

Cardboard 

Box

Bottle FLPE Hg-T 250 mL None N/A

Lab ID: 1120006-06 Report Matrix: DIW

Sample: Hg Blk BioReactor 2 Eff Sample Type: Field Blank Received: 05/10/2011

Collected: 05/09/2011

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

A 71062020

60

Cardboard 

Box

Bottle FLPE Hg-T 250 mL None N/A

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

Page 23 of 27
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Shipping Containers

Cardboard Box

Tracking No: 4726 7966 0311 via FedEx

Temperature: ambient

Coolant Type: None

Description: Cardboard Box

Damaged in transit? No

Returned to client? No

Custody seals present? Yes

Custody seals intact? Yes

COC present? Yes

Received: May 10, 2011 8:40

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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