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: J12050473

Project Name: N/A

Lab Contact: Jason C Perkins

Date: 6/11/2012

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. 

Analytical Lab 

Page 1 of 35
Sample ID's & Descriptions:

Sample ID Plant/Station

Collection 

Date and Time Collected By Sample Description

2012012051 BELEWS 30-May-12 8:00 AM R. HENDRICKS FGD Purge Eff 

2012012052 BELEWS 30-May-12 8:00 AM R. HENDRICKS EQ TANK EFF. 

2012012053 BELEWS 30-May-12 8:00 AM R. HENDRICKS BIOREACTOR 1 INF 

2012012054 BELEWS 30-May-12 8:00 AM R. HENDRICKS HG BLANK BIOREACTOR 1 INF. 

2012012055 BELEWS 30-May-12 8:00 AM R. HENDRICKS BIOREACTOR 2 INF. 

2012012056 BELEWS 30-May-12 8:00 AM R. HENDRICKS Hg Blk BioReactor 2 Inf 

2012012057 BELEWS 30-May-12 8:00 AM R. HENDRICKS BIOREACTOR 2 EFF. 

2012012058 BELEWS 30-May-12 8:00 AM R. HENDRICKS Hg Blk BioReactor 2 Eff 

2012012059 BELEWS 30-May-12 8:00 AM R. HENDRICKS FILTER BLANK 

2012012060 BELEWS 30-May-12 8:00 AM R. HENDRICKS METALS TRIP BLANK 

10 Total Samples

Analytical Lab 

Page 2 of 35
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: Mary Ann Ogle Date: 6/11/2012

Yes

Electronic Data Deliverable (EDD) Sent Separately

Analytical Lab 

Page 3 of 35
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12050473

2012012051

Collection Date: 30-May-12 8:00 AM

Site: FGD Purge Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

INORGANIC IONS BY IC

Bromide 110 mg/L EPA 300.0 5 50 04-Jun-12 14:32 BGN9034

Chloride 7300 mg/L EPA 300.0 100 1000 04-Jun-12 14:32 BGN9034

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 277 ug/L EPA 245.1 5 100 07-Jun-12 11:05 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 220 mg/L EPA 200.7 0.5 10 06-Jun-12 15:04 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 194 ug/L EPA 200.8 20 20 31-May-12 14:59 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 181 ug/L EPA 200.8 20 20 05-Jun-12 12:33 DJSULL1

Chromium (Cr) 265 ug/L EPA 200.8 20 20 05-Jun-12 12:33 DJSULL1

Copper (Cu) 145 ug/L EPA 200.8 20 20 05-Jun-12 12:33 DJSULL1

Manganese (Mn) 7380 ug/L EPA 200.8 20 20 05-Jun-12 12:33 DJSULL1

Nickel (Ni) 214 ug/L EPA 200.8 20 20 05-Jun-12 12:33 DJSULL1

Selenium (Se) 5690 ug/L EPA 200.8 20 20 05-Jun-12 12:33 DJSULL1

Silver (Ag) < 20 ug/L EPA 200.8 20 20 05-Jun-12 12:33 DJSULL1

Zinc (Zn) 286 ug/L EPA 200.8 20 20 05-Jun-12 12:33 DJSULL1

SELENIUM SPECIATION

Vendor Parameter Complete 1 V_AS&C

TOTAL DISSOLVED SOLIDS

Vendor Parameter Complete 1 V_PACE

2012012052

Collection Date: 30-May-12 8:00 AM

Site: EQ TANK EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 216 ug/L EPA 245.1 2.5 50 07-Jun-12 11:08 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 223 mg/L EPA 200.7 0.5 10 06-Jun-12 15:08 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 114 ug/L EPA 200.8 10 10 31-May-12 15:03 KRICHAR

Analytical Lab 

Page 4 of 35
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12050473

2012012052

Collection Date: 30-May-12 8:00 AM

Site: EQ TANK EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 171 ug/L EPA 200.8 20 20 05-Jun-12 12:36 DJSULL1

Chromium (Cr) 238 ug/L EPA 200.8 20 20 05-Jun-12 12:36 DJSULL1

Copper (Cu) 124 ug/L EPA 200.8 20 20 05-Jun-12 12:36 DJSULL1

Manganese (Mn) 7050 ug/L EPA 200.8 20 20 05-Jun-12 12:36 DJSULL1

Nickel (Ni) 200 ug/L EPA 200.8 20 20 05-Jun-12 12:36 DJSULL1

Selenium (Se) 5130 ug/L EPA 200.8 20 20 05-Jun-12 12:36 DJSULL1

Silver (Ag) < 20 ug/L EPA 200.8 20 20 05-Jun-12 12:36 DJSULL1

Zinc (Zn) 254 ug/L EPA 200.8 20 20 05-Jun-12 12:36 DJSULL1

2012012053

Collection Date: 30-May-12 8:00 AM

Site: BIOREACTOR 1 INF 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

MERCURY 1631

Vendor Parameter Complete 1 V_BRAND

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 211 mg/L EPA 200.7 0.5 10 06-Jun-12 15:12 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 91.5 ug/L EPA 200.8 10 10 31-May-12 15:07 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L EPA 200.8 10 10 05-Jun-12 12:40 DJSULL1

Chromium (Cr) < 10 ug/L EPA 200.8 10 10 05-Jun-12 12:40 DJSULL1

Copper (Cu) < 10 ug/L EPA 200.8 10 10 05-Jun-12 12:40 DJSULL1

Manganese (Mn) 5030 ug/L EPA 200.8 10 10 05-Jun-12 12:40 DJSULL1

Nickel (Ni) 39.9 ug/L EPA 200.8 10 10 05-Jun-12 12:40 DJSULL1

Selenium (Se) 92.4 ug/L EPA 200.8 10 10 05-Jun-12 12:40 DJSULL1

Silver (Ag) < 10 ug/L EPA 200.8 10 10 05-Jun-12 12:40 DJSULL1

Zinc (Zn) < 10 ug/L EPA 200.8 10 10 05-Jun-12 12:40 DJSULL1

SELENIUM SPECIATION

Vendor Parameter Complete 1 V_AS&C

Analytical Lab 

Page 5 of 35
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12050473

2012012054

Collection Date: 30-May-12 8:00 AM

Site: HG BLANK BIOREACTOR 1 INF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

MERCURY 1631

Vendor Parameter Complete 1 V_BRAND

2012012055

Collection Date: 30-May-12 8:00 AM

Site: BIOREACTOR 2 INF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

MERCURY 1631

Vendor Parameter Complete 1 V_BRAND

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 207 mg/L EPA 200.7 0.5 10 06-Jun-12 15:16 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L EPA 200.8 10 10 05-Jun-12 13:57 DJSULL1

Chromium (Cr) < 10 ug/L EPA 200.8 10 10 05-Jun-12 13:57 DJSULL1

Copper (Cu) < 10 ug/L EPA 200.8 10 10 05-Jun-12 13:57 DJSULL1

Manganese (Mn) 5210 ug/L EPA 200.8 10 10 05-Jun-12 13:57 DJSULL1

Nickel (Ni) 13.7 ug/L EPA 200.8 10 10 05-Jun-12 13:57 DJSULL1

Selenium (Se) 23.8 ug/L EPA 200.8 10 10 05-Jun-12 13:57 DJSULL1

Silver (Ag) < 10 ug/L EPA 200.8 10 10 05-Jun-12 13:57 DJSULL1

Zinc (Zn) < 10 ug/L EPA 200.8 10 10 05-Jun-12 13:57 DJSULL1

2012012056

Collection Date: 30-May-12 8:00 AM

Site: Hg Blk BioReactor 2 Inf 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

MERCURY 1631

Vendor Parameter Complete 1 V_BRAND

2012012057

Collection Date: 30-May-12 8:00 AM

Site: BIOREACTOR 2 EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

MERCURY 1631

Vendor Parameter Complete 1 V_BRAND

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) < 1 ug/L EPA 245.1 1 20 07-Jun-12 11:10 AGIBBS

Analytical Lab 

Page 6 of 35
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12050473

2012012057

Collection Date: 30-May-12 8:00 AM

Site: BIOREACTOR 2 EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 203 mg/L EPA 200.7 0.5 10 06-Jun-12 15:20 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L EPA 200.8 10 10 05-Jun-12 14:00 DJSULL1

Chromium (Cr) < 10 ug/L EPA 200.8 10 10 05-Jun-12 14:00 DJSULL1

Copper (Cu) < 10 ug/L EPA 200.8 10 10 05-Jun-12 14:00 DJSULL1

Manganese (Mn) 3900 ug/L EPA 200.8 10 10 05-Jun-12 14:00 DJSULL1

Nickel (Ni) < 10 ug/L EPA 200.8 10 10 05-Jun-12 14:00 DJSULL1

Selenium (Se) 15.9 ug/L EPA 200.8 10 10 05-Jun-12 14:00 DJSULL1

Silver (Ag) < 10 ug/L EPA 200.8 10 10 05-Jun-12 14:00 DJSULL1

Zinc (Zn) < 10 ug/L EPA 200.8 10 10 05-Jun-12 14:00 DJSULL1

SELENIUM SPECIATION

Vendor Parameter Complete 1 V_AS&C

2012012058

Collection Date: 30-May-12 8:00 AM

Site: Hg Blk BioReactor 2 Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

MERCURY 1631

Vendor Parameter Complete 1 V_BRAND

2012012059

Collection Date: 30-May-12 8:00 AM

Site: FILTER BLANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

DISSOLVED METALS BY ICP-MS

Selenium (Se) < 1 ug/L EPA 200.8 1 1 31-May-12 14:54 KRICHAR

2012012060

Collection Date: 30-May-12 8:00 AM

Site: METALS TRIP BLANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

TOTAL RECOVERABLE METALS BY ICP

Boron (B) < 0.05 mg/L EPA 200.7 0.05 1 06-Jun-12 15:00 MHH7131

Analytical Lab 

Page 7 of 35
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12050473

2012012060

Collection Date: 30-May-12 8:00 AM

Site: METALS TRIP BLANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 1 ug/L EPA 200.8 1 1 05-Jun-12 13:48 DJSULL1

Chromium (Cr) < 1 ug/L EPA 200.8 1 1 05-Jun-12 13:48 DJSULL1

Copper (Cu) < 1 ug/L EPA 200.8 1 1 05-Jun-12 13:48 DJSULL1

Manganese (Mn) < 1 ug/L EPA 200.8 1 1 05-Jun-12 13:48 DJSULL1

Nickel (Ni) < 1 ug/L EPA 200.8 1 1 05-Jun-12 13:48 DJSULL1

Selenium (Se) 1.08 ug/L EPA 200.8 1 1 05-Jun-12 13:48 DJSULL1

Silver (Ag) < 1 ug/L EPA 200.8 1 1 05-Jun-12 13:48 DJSULL1

Zinc (Zn) < 1 ug/L EPA 200.8 1 1 05-Jun-12 13:48 DJSULL1

SELENIUM SPECIATION

Vendor Parameter Complete 1 V_AS&C

Analytical Lab 

Page 8 of 35
 

June 8, 2012 

Jay Perkins 

Duke Energy Analytical Laboratory 

Mail Code MGO3A2 (Building 7405) 

13339 Hagers Ferry Rd. 

Huntersville, NC 28078 

(704) 875-5245 

Project: Belews Creek – FGD Alternate Fuels Test Burn (LIMS # J12050473) 

Dear Mr. Perkins, 

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

speciation analysis on May 31, 2012. The samples were received in a sealed cooler at 0.0°C on 

June 1, 2012. Selenium speciation analysis was performed via ion chromatography inductively 

coupled plasma collision reaction cell mass spectrometry (IC-ICP-CRC-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 

 

Analytical Lab 

Page 9 of 35
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 Creek – FGD Alternate Fuels Test Burn (LIMS # J12050473) 

June 7, 2012 

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 31, 2012. The samples 

were received on June 1, 2012 in a sealed container at 0.0°C.

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

and ultra-violet radiation, and was 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 collision reaction cell mass spectrometry 

(IC-ICP-CRC-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-CRC-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 

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 

Analytical Lab 

Page 10 of 35
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-CRC-MS Each sample for selenium speciation 

analysis was analyzed by ion chromatography inductively coupled plasma collision reaction 

cell mass spectrometry (IC-ICP-CRC-MS) on June 5, 2012. 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 (CRC) containing a reaction 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. 

Analytical Lab 

Page 11 of 35
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 

Analytical Lab 

Page 12 of 35
Sample Results

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

Unknown Se 

Species (n)

FGD Purge Eff 93.1 77.7 ND (<0.45) ND (<0.59) ND (<0.59) 0 (0)

BioReactor 1 Inf 18.8 62.5 ND (<0.11) 1.79 ND (<0.15) 0 (0)

BioReactor 2 Eff 0.415 ND (<0.25) ND (<0.11) ND (<0.15) ND (<0.15) 0 (0)

Metals Trip Blk ND (<0.016) ND (<0.050) ND (<0.023) ND (<0.030) ND (<0.030) 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 Creek - FGD Alternate Fuels Test Burn

Contact: Jay Perkins

Date: June 8, 2012

LIMS #J12050473

Analytical Lab 

Page 13 of 35
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 0.002 0.016 0.082 0.33

Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.050 0.25 1.00

SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.023 0.11 0.45

MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.003 0.030 0.15 0.59

SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.003 0.030 0.15 0.59

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 9.96 104.0

Se(VI) LCS 9.48 9.37 98.9

SeCN LCS 8.92 8.73 97.9

MeSe(IV) LCS 6.47 5.70 88.1

SeMe LCS 9.32 8.79 94.3

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Belews Creek - FGD Alternate Fuels Test Burn

Contact: Jay Perkins

LIMS #J12050473

Date: June 8, 2012

Report Generated by: Russell Gerads

Analytical Lab 

Page 14 of 35
Quality Control Summary - Matrix Duplicates

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

Se(IV) Batch QC 46.21 45.82 46.02 0.9

Se(VI) Batch QC 64.75 63.22 63.99 2.4

SeCN Batch QC ND (<0.45) ND (<0.45) NC NC

MeSe(IV) Batch QC ND (<0.15) ND (<0.15) NC NC

SeMe Batch QC ND (<0.15) ND (<0.15) 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) Batch QC 1112 1892 166.0 1112 1900 166.7 0.4

Se(VI) Batch QC 1009 1168 109.4 1009 1183 110.9 1.3

SeCN Batch QC 915.0 462.9 50.6* 915.0 470.7 51.4* 1.7

*The low recovery is attributed to matrix induced species conversion

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Belews Creek - FGD Alternate Fuels Test Burn

Contact: Jay Perkins

LIMS #J12050473

Date: June 8, 2012

Report Generated by: Russell Gerads

Analytical Lab 

Page 15 of 35
Analytical Lab 

Page 16 of 35
 

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

June 8, 2012 

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-HV1201 Client Project: J12050473 

Dear Mr. Perkins, 

On June 1, 2012, Brooks Rand Labs (BRL) received three (3) wastewater samples and three (3) 

corresponding field blanks. Samples were logged-in for total mercury (THg) 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. 

Aside from concentration qualifiers, all data was reported without qualification and all associated 

quality control sample results met the acceptance criteria. 

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

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

page of the report. 

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

Sincerely, 

 

Tiffany Stilwater 

Project Manager 

tiffany@brooksrand.com 

Analytical Lab 

Page 17 of 35
Project ID: DUK-HV1201

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

Analytical Lab 

Page 18 of 35
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Sample Information

Sample Lab ID Report Matrix Type Sampled Received

BioReactor 1 Inf 1222026-01 Influent Sample 05/30/2012 06/01/2012

Hg Blk BioReactor 1 Inf 1222026-02 DIW Field Blank 05/30/2012 06/01/2012

BioReactor 2 Inf 1222026-03 Influent QC Sample 05/30/2012 06/01/2012

Hg Blk BioReactor 2 Inf 1222026-04 DIW Field Blank 05/30/2012 06/01/2012

BioReactor 2 Eff 1222026-05 Effluent Sample 05/30/2012 06/01/2012

Hg Blk BioReactor 2 Eff 1222026-06 DIW Field Blank 05/30/2012 06/01/2012

Batch Summary

Analyte Lab Matrix Method Prepared Analyzed Batch Sequence

Hg Water EPA 1631 06/04/2012 06/06/2012 B120918 1200419

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

Analytical Lab 

Page 19 of 35
Project ID: DUK-HV1201

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

1222026-01 Hg Influent T 91.4 3.06 8.16 ng/L B120918 1200419

BioReactor 2 Eff

1222026-05 Hg Effluent T 7.55 0.61 1.63 ng/L B120918 1200419

BioReactor 2 Inf

1222026-03 Hg Influent T 20.5 3.06 8.16 ng/L B120918 1200419

Hg Blk BioReactor 1 Inf

1222026-02 Hg DIW T 0.15 U 0.15 0.41 ng/L B120918 1200419

Hg Blk BioReactor 2 Eff

1222026-06 Hg DIW T 0.15 U 0.15 0.40 ng/L B120918 1200419

Hg Blk BioReactor 2 Inf

1222026-04 Hg DIW T 0.15 U 0.15 0.41 ng/L B120918 1200419

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

Analytical Lab 

Page 20 of 35
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Accuracy & Precision Summary

Batch: B120918

Analyte Native Spike Result Units REC & Limits RPD & Limits

Method: EPA 1631

Lab Matrix: Water

Sample

B120918-SRM1 Certified Reference Material (1221029, NIST 1641d 1000x dilution)

Hg 15.68 16.09 ng/L 103% 85-115

B120918-MS1 Matrix Spike (1222026-03)

Hg 20.51 102.0 136.2 ng/L 113% 71-125

B120918-MSD1 Matrix Spike Duplicate (1222026-03)

Hg 20.51 102.0 133.0 ng/L 110% 71-125 242%

B120918-MS2 Matrix Spike (1222026-05)

Hg 7.55 38.39 50.24 ng/L 111% 71-125

B120918-MSD2 Matrix Spike Duplicate (1222026-05)

Hg 7.55 38.10 49.63 ng/L 110% 71-125 241%

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

Analytical Lab 

Page 21 of 35
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Method Blanks & Reporting Limits

Batch: B120918

Method: EPA 1631

Matrix: Water

Analyte: Hg

Sample Result Units

B120918-BLK1 0.27 ng/L

B120918-BLK2 0.30 ng/L

B120918-BLK3 0.29 ng/L

B120918-BLK4 0.18 ng/L

Average: 0.26 Standard Deviation: 0.05 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

Analytical Lab 

Page 22 of 35
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Instrument Calibration

Sequence: 1200419

Instrument: THG-05 Method: EPA 1631

Date: 06/06/2012

Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg

Lab ID True Value Result Units REC & Limits

1200419-IBL1 5.61 pg of Hg

1200419-IBL2 7.11 pg of Hg

1200419-IBL3 5.37 pg of Hg

1200419-IBL4 5.64 pg of Hg

1200419-CAL1 25.00 24.78 pg of Hg 99%

1200419-CAL2 100.0 100.2 pg of Hg 100%

1200419-CAL3 500.0 499.9 pg of Hg 100%

1200419-CAL4 2500 2487 pg of Hg 99%

1200419-CAL5 10000 10120 pg of Hg 101%

1200419-ICV1 1568 1609 pg of Hg 103% 85-115

1200419-CCV1 500.0 509.5 pg of Hg 102% 77-123

1200419-CCB1 11.3 pg of Hg

1200419-CCV2 500.0 515.0 pg of Hg 103% 77-123

1200419-CCV3 500.0 503.7 pg of Hg 101% 77-123

1200419-CCV4 500.0 503.0 pg of Hg 101% 77-123

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

Analytical Lab 

Page 23 of 35
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Sample Containers

Lab ID: 1222026-01 Report Matrix: Influent

Sample: BioReactor 1 Inf Sample Type: Sample Received: 06/01/2012

Collected: 05/30/2012

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

A 71628390

10

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

Lab ID: 1222026-02 Report Matrix: DIW

Sample: Hg Blk BioReactor 1 Inf Sample Type: Field Blank Received: 06/01/2012

Collected: 05/30/2012

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

A 71628390

10

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

Lab ID: 1222026-03 Report Matrix: Influent

Sample: BioReactor 2 Inf Sample Type: QC Sample Received: 06/01/2012

Collected: 05/30/2012

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

A 71628390

10

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

Lab ID: 1222026-04 Report Matrix: DIW

Sample: Hg Blk BioReactor 2 Inf Sample Type: Field Blank Received: 06/01/2012

Collected: 05/30/2012

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

A 71628390

10

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

Lab ID: 1222026-05 Report Matrix: Effluent

Sample: BioReactor 2 Eff Sample Type: Sample Received: 06/01/2012

Collected: 05/30/2012

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

A 71628390

10

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

Lab ID: 1222026-06 Report Matrix: DIW

Sample: Hg Blk BioReactor 2 Eff Sample Type: Field Blank Received: 06/01/2012

Collected: 05/30/2012

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

A 71628390

10

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

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

Analytical Lab 

Page 24 of 35
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Shipping Containers

Cooler

Tracking No: 4726 7967 1661 via FedEx

Temperature: 0.8 °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: June 1, 2012 9:15

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

Analytical Lab 

Page 25 of 35
Analytical Lab 

Page 26 of 35
June 05, 2012

LIMS USE: FR - PROGRAM MANAGER

LIMS OBJECT ID: 92119701

92119701

Project:

Pace Project No.:

RE:

Program Manager

Duke Energy

,

J12050473

Dear Program Manager:

Enclosed are the analytical results for sample(s) received by the laboratory on May 31, 2012. The

results relate only to the samples included in this report. Results reported herein conform to the

most current TNI standards and the laboratory's Quality Assurance Manual, where applicable, unless

otherwise noted in the body of the report.

Analyses were performed at the Pace Analytical Services location indicated on the sample analyte

page for analysis unless otherwise footnoted.

If you have any questions concerning this report, please feel free to contact me.

Sincerely,

Kevin Herring

kevin.herring@pacelabs.com

Project Manager

Enclosures

REPORT OF LABORATORY ANALYSIS

This report shall not be reproduced, except in full,

without the written consent of Pace Analytical Services, Inc..

Page 1 of 8

Pace Analytical Services, Inc.

9800 Kincey Ave. Suite 100

Huntersville, NC 28078

(704)875-9092

Pace Analytical Services, Inc.

2225 Riverside Dr.

Asheville, NC 28804

(828)254-7176

Pace Analytical Services, Inc.

205 East Meadow Road - Suite A

Eden, NC 27288

(336)623-8921

Analytical Lab 

Page 27 of 35
CERTIFICATIONS

Pace Project No.:

Project:

92119701

J12050473

Asheville Certification IDs

2225 Riverside Dr., Asheville, NC 28804

Florida/NELAP Certification #: E87648

Massachusetts Certification #: M-NC030

North Carolina Drinking Water Certification #: 37712

North Carolina Wastewater Certification #: 40

South Carolina Certification #: 99030001

Virginia Certification #: 00072

West Virginia Certification #: 356

Virgina/VELAP Certification #: 460147

REPORT OF LABORATORY ANALYSIS

This report shall not be reproduced, except in full,

without the written consent of Pace Analytical Services, Inc..

Page 2 of 8

Pace Analytical Services, Inc.

9800 Kincey Ave. Suite 100

Huntersville, NC 28078

(704)875-9092

Pace Analytical Services, Inc.

2225 Riverside Dr.

Asheville, NC 28804

(828)254-7176

Pace Analytical Services, Inc.

205 East Meadow Road - Suite A

Eden, NC 27288

(336)623-8921

Analytical Lab 

Page 28 of 35
SAMPLE SUMMARY

Pace Project No.:

Project:

92119701

J12050473

Lab ID Sample ID Matrix Date Collected Date Received

92119701001 2012012051 Water 05/30/12 08:00 05/31/12 14:50

REPORT OF LABORATORY ANALYSIS

This report shall not be reproduced, except in full,

without the written consent of Pace Analytical Services, Inc..

Page 3 of 8

Pace Analytical Services, Inc.

9800 Kincey Ave. Suite 100

Huntersville, NC 28078

(704)875-9092

Pace Analytical Services, Inc.

2225 Riverside Dr.

Asheville, NC 28804

(828)254-7176

Pace Analytical Services, Inc.

205 East Meadow Road - Suite A

Eden, NC 27288

(336)623-8921

Analytical Lab 

Page 29 of 35
SAMPLE ANALYTE COUNT

Pace Project No.:

Project:

92119701

J12050473

Lab ID Sample ID Method

Analytes

Analysts Reported Laboratory

92119701001 2012012051 SM 2540C LMD 1 PASI-A

REPORT OF LABORATORY ANALYSIS

This report shall not be reproduced, except in full,

without the written consent of Pace Analytical Services, Inc..

Page 4 of 8

Pace Analytical Services, Inc.

9800 Kincey Ave. Suite 100

Huntersville, NC 28078

(704)875-9092

Pace Analytical Services, Inc.

2225 Riverside Dr.

Asheville, NC 28804

(828)254-7176

Pace Analytical Services, Inc.

205 East Meadow Road - Suite A

Eden, NC 27288

(336)623-8921

Analytical Lab 

Page 30 of 35
ANALYTICAL RESULTS

Pace Project No.:

Project:

92119701

J12050473

Sample: 2012012051 Lab ID: 92119701001 Collected: 05/30/12 08:00 Received: 05/31/12 14:50 Matrix: Water

Parameters Results Units Limit MDL DF Prepared Analyzed CAS No. Qual

Report

2540C Total Dissolved Solids Analytical Method: SM 2540C

Total Dissolved Solids 16600 mg/L 500 500 1 05/31/12 22:53

REPORT OF LABORATORY ANALYSIS

This report shall not be reproduced, except in full,

without the written consent of Pace Analytical Services, Inc..

Date: 06/05/2012 05:36 PM Page 5 of 8

Pace Analytical Services, Inc.

9800 Kincey Ave. Suite 100

Huntersville, NC 28078

(704)875-9092

Pace Analytical Services, Inc.

2225 Riverside Dr.

Asheville, NC 28804

(828)254-7176

Pace Analytical Services, Inc.

205 East Meadow Road - Suite A

Eden, NC 27288

(336)623-8921

Analytical Lab 

Page 31 of 35
QUALITY CONTROL DATA

Pace Project No.:

Project:

92119701

J12050473

QC Batch:

QC Batch Method:

Analysis Method:

Analysis Description:

WET/21050

SM 2540C

SM 2540C

2540C Total Dissolved Solids

Associated Lab Samples: 92119701001

Parameter Units

Blank

Result

Reporting

Limit Qualifiers

METHOD BLANK: 771370

Associated Lab Samples: 92119701001

Matrix: Water

Analyzed

Total Dissolved Solids mg/L ND 25.0 05/31/12 22:50

Parameter Units

LCS

Result

% Rec

Conc. % Rec Limits Qualifiers

LABORATORY CONTROL SAMPLE: 771371

Spike LCS

Total Dissolved Solids mg/L 250 246 98 80-120

Parameter Units

Dup

Result

Max

Result RPD RPD Qualifiers

92119558001

SAMPLE DUPLICATE: 771372

Total Dissolved Solids mg/L 8760 8320 5 10

Parameter Units

Dup

Result

Max

Result RPD RPD Qualifiers

92119703003

SAMPLE DUPLICATE: 771373

Total Dissolved Solids mg/L 61.0 57.0 7 10

REPORT OF LABORATORY ANALYSIS

This report shall not be reproduced, except in full,

without the written consent of Pace Analytical Services, Inc..

Date: 06/05/2012 05:36 PM Page 6 of 8

Pace Analytical Services, Inc.

9800 Kincey Ave. Suite 100

Huntersville, NC 28078

(704)875-9092

Pace Analytical Services, Inc.

2225 Riverside Dr.

Asheville, NC 28804

(828)254-7176

Pace Analytical Services, Inc.

205 East Meadow Road - Suite A

Eden, NC 27288

(336)623-8921

Analytical Lab 

Page 32 of 35
QUALIFIERS

Pace Project No.:

Project:

92119701

J12050473

DEFINITIONS

DF - Dilution Factor, if reported, represents the factor applied to the reported data due to changes in sample preparation, dilution of

the sample aliquot, or moisture content.

ND - Not Detected at or above adjusted reporting limit.

J - Estimated concentration above the adjusted method detection limit and below the adjusted reporting limit.

MDL - Adjusted Method Detection Limit.

PRL - Pace Reporting Limit.

RL - Reporting Limit.

S - Surrogate

1,2-Diphenylhydrazine (8270 listed analyte) decomposes to Azobenzene.

Consistent with EPA guidelines, unrounded data are displayed and have been used to calculate % recovery and RPD values.

LCS(D) - Laboratory Control Sample (Duplicate)

MS(D) - Matrix Spike (Duplicate)

DUP - Sample Duplicate

RPD - Relative Percent Difference

NC - Not Calculable.

SG - Silica Gel - Clean-Up

U - Indicates the compound was analyzed for, but not detected.

N-Nitrosodiphenylamine decomposes and cannot be separated from Diphenylamine using Method 8270. The result reported for

each analyte is a combined concentration.

Acid preservation may not be appropriate for 2-Chloroethylvinyl ether, Styrene, and Vinyl chloride.

Pace Analytical is TNI accredited. Contact your Pace PM for the current list of accredited analytes.

TNI - The NELAC Institute.

LABORATORIES

PASI-A Pace Analytical Services - Asheville

REPORT OF LABORATORY ANALYSIS

This report shall not be reproduced, except in full,

without the written consent of Pace Analytical Services, Inc..

Date: 06/05/2012 05:36 PM Page 7 of 8

Pace Analytical Services, Inc.

9800 Kincey Ave. Suite 100

Huntersville, NC 28078

(704)875-9092

Pace Analytical Services, Inc.

2225 Riverside Dr.

Asheville, NC 28804

(828)254-7176

Pace Analytical Services, Inc.

205 East Meadow Road - Suite A

Eden, NC 27288

(336)623-8921

Analytical Lab 

Page 33 of 35
QUALITY CONTROL DATA CROSS REFERENCE TABLE

Pace Project No.:

Project:

92119701

J12050473

Lab ID Sample ID QC Batch Method QC Batch Analytical Method

Analytical

Batch

92119701001 2012012051 SM 2540C WET/21050

REPORT OF LABORATORY ANALYSIS

This report shall not be reproduced, except in full,

without the written consent of Pace Analytical Services, Inc..

Date: 06/05/2012 05:36 PM Page 8 of 8

Pace Analytical Services, Inc.

9800 Kincey Ave. Suite 100

Huntersville, NC 28078

(704)875-9092

Pace Analytical Services, Inc.

2225 Riverside Dr.

Asheville, NC 28804

(828)254-7176

Pace Analytical Services, Inc.

205 East Meadow Road - Suite A

Eden, NC 27288

(336)623-8921

Analytical Lab 

Page 34 of 35
Analytical Lab 

Page 35 of 35