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: J12120256

Project Name: Flex Fuel WW

Lab Contact: Jason C Perkins

Date: 1/10/2013

Customer Address: 3195 Pine Hall Rd

Customer Name(s): Bill K, Wayne C, Melonie M, and Tom J

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. Subcontracted data 

included on the Duke Certificate of Analysis is to be used as information only. Certified vendor results can be found in the 

subcontracted lab final report. Duke Energy Analytical Laboratory subcontracts analyses to other vendor laboratories that have 

been qualified by Duke Energy to perform these analyses except where 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 28
Sample ID's & Descriptions:

Sample ID Plant/Station

Collection 

Date and Time Collected By Sample Description

2012026870 BELEWS 17-Dec-12 7:30 AM L. TURNER FGD Purge Eff 

2012026871 BELEWS 17-Dec-12 7:35 AM L. TURNER EQ TANK 

2012026872 BELEWS 17-Dec-12 7:40 AM L. TURNER BIOREACTOR 1 INF 

2012026873 BELEWS 17-Dec-12 7:40 AM L. TURNER biOREACTOR 1 INF HG BLK 

2012026874 BELEWS 17-Dec-12 7:45 AM L. TURNER BIOREACTOR 2 INF. 

2012026875 BELEWS 17-Dec-12 7:45 AM L. TURNER BIOREACTOR 2 INF. HG BLANK 

2012026876 BELEWS 17-Dec-12 7:50 AM L. TURNER BIOREACTOR 2 EFF. 

2012026877 BELEWS 17-Dec-12 7:50 AM L. TURNER BIOREACTOR 2 EFF. HG BLANK 

2012026878 BELEWS 17-Dec-12 8:00 AM L. TURNER FILTER BLANK 

9 Total Samples

Page 2 of 28
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.

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: DBA Account Date: 1/10/2013

Electronic Data Deliverable (EDD) Sent Separately

Page 3 of 28
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12120256

2012026870

Collection Date: 17-Dec-12 7:30 AM

Site: FGD Purge Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

INORGANIC IONS BY IC

Bromide 88 mg/L 5 50 EPA 300.0 12/21/2012 19:34 JAHERMA

Chloride 6100 mg/L 100 1000 EPA 300.0 12/21/2012 19:34 JAHERMA

Sulfate 1200 mg/L 100 1000 EPA 300.0 12/21/2012 19:34 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 110 ug/L 5 100 EPA 245.1 12/20/2012 14:43 AGIBBS

DISSOLVED METALS BY ICP

Manganese (Mn) 10.1 mg/L 0.05 10 EPA 200.7 01/03/2013 13:40 MHH7131

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 189 mg/L 0.5 10 EPA 200.7 01/02/2013 11:34 MHH7131

Calcium (Ca) 3400 mg/L 0.1 10 EPA 200.7 01/02/2013 11:34 MHH7131

Iron (Fe) 101 mg/L 0.1 10 EPA 200.7 01/02/2013 11:34 MHH7131

Magnesium (Mg) 897 mg/L 0.05 10 EPA 200.7 01/02/2013 11:34 MHH7131

Manganese (Mn) 10.4 mg/L 0.05 10 EPA 200.7 01/02/2013 11:34 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 92.1 ug/L 10 10 EPA 200.8 01/08/2013 10:36 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 223 ug/L 10 10 EPA 200.8 12/26/2012 10:59 DJSULL1

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 12/26/2012 10:59 DJSULL1

Chromium (Cr) 214 ug/L 10 10 EPA 200.8 12/26/2012 10:59 DJSULL1

Copper (Cu) 123 ug/L 10 10 EPA 200.8 12/26/2012 10:59 DJSULL1

Nickel (Ni) 285 ug/L 10 10 EPA 200.8 12/26/2012 10:59 DJSULL1

Selenium (Se) 2060 ug/L 10 10 EPA 200.8 12/26/2012 10:59 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 12/26/2012 10:59 DJSULL1

Zinc (Zn) 234 ug/L 10 10 EPA 200.8 12/26/2012 10:59 DJSULL1

SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC)

Vendor Parameter Complete Vendor Method V_AS&C

TOTAL DISSOLVED SOLIDS

TDS 17000 mg/L 200 1 SM2540C 12/26/2012 14:25 SWILLI3

TOTAL SUSPENDED SOLIDS

TSS 2300 mg/L 250 1 SM2540D 12/20/2012 09:05 TJA7067

Page 4 of 28
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12120256

2012026871

Collection Date: 17-Dec-12 7:35 AM

Site: EQ TANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 90.4 ug/L 2.5 50 EPA 245.1 12/20/2012 14:46 AGIBBS

DISSOLVED METALS BY ICP

Manganese (Mn) 11.5 mg/L 0.05 10 EPA 200.7 01/03/2013 13:44 MHH7131

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 236 mg/L 0.5 10 EPA 200.7 01/02/2013 11:38 MHH7131

Calcium (Ca) 3910 mg/L 0.1 10 EPA 200.7 01/02/2013 11:38 MHH7131

Iron (Fe) 91.2 mg/L 0.1 10 EPA 200.7 01/02/2013 11:38 MHH7131

Magnesium (Mg) 1140 mg/L 0.05 10 EPA 200.7 01/02/2013 11:38 MHH7131

Manganese (Mn) 12.0 mg/L 0.05 10 EPA 200.7 01/02/2013 11:38 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 69.5 ug/L 10 10 EPA 200.8 01/08/2013 10:39 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 170 ug/L 10 10 EPA 200.8 12/26/2012 11:03 DJSULL1

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 12/26/2012 11:03 DJSULL1

Chromium (Cr) 185 ug/L 10 10 EPA 200.8 12/26/2012 11:03 DJSULL1

Copper (Cu) 99.3 ug/L 10 10 EPA 200.8 12/26/2012 11:03 DJSULL1

Nickel (Ni) 254 ug/L 10 10 EPA 200.8 12/26/2012 11:03 DJSULL1

Selenium (Se) 1560 ug/L 10 10 EPA 200.8 12/26/2012 11:03 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 12/26/2012 11:03 DJSULL1

Zinc (Zn) 219 ug/L 10 10 EPA 200.8 12/26/2012 11:03 DJSULL1

2012026872

Collection Date: 17-Dec-12 7:40 AM

Site: BIOREACTOR 1 INF 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC)

Vendor Parameter Complete Vendor Method V_BRAND

DISSOLVED METALS BY ICP

Manganese (Mn) 1.94 mg/L 0.05 10 EPA 200.7 01/03/2013 13:48 MHH7131

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 236 mg/L 0.5 10 EPA 200.7 01/02/2013 11:53 MHH7131

Calcium (Ca) 3590 mg/L 0.1 10 EPA 200.7 01/02/2013 11:53 MHH7131

Iron (Fe) < 0.1 mg/L 0.1 10 EPA 200.7 01/02/2013 11:53 MHH7131

Magnesium (Mg) 1120 mg/L 0.05 10 EPA 200.7 01/02/2013 11:53 MHH7131

Manganese (Mn) 1.95 mg/L 0.05 10 EPA 200.7 01/02/2013 11:53 MHH7131

Page 5 of 28
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12120256

2012026872

Collection Date: 17-Dec-12 7:40 AM

Site: BIOREACTOR 1 INF 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

DISSOLVED METALS BY ICP-MS

Selenium (Se) 95.2 ug/L 10 10 EPA 200.8 01/08/2013 10:43 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 12/26/2012 11:11 DJSULL1

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 12/26/2012 11:11 DJSULL1

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 12/26/2012 11:11 DJSULL1

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 12/26/2012 11:11 DJSULL1

Nickel (Ni) 17.6 ug/L 10 10 EPA 200.8 12/26/2012 11:11 DJSULL1

Selenium (Se) 78.3 ug/L 10 10 EPA 200.8 12/26/2012 11:11 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 12/26/2012 11:11 DJSULL1

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 12/26/2012 11:11 DJSULL1

SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC)

Vendor Parameter Complete Vendor Method V_AS&C

2012026873

Collection Date: 17-Dec-12 7:40 AM

Site: biOREACTOR 1 INF HG BLK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC)

Vendor Parameter Complete Vendor Method V_BRAND

2012026874

Collection Date: 17-Dec-12 7:45 AM

Site: BIOREACTOR 2 INF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC)

Vendor Parameter Complete Vendor Method V_BRAND

DISSOLVED METALS BY ICP

Manganese (Mn) 1.50 mg/L 0.05 10 EPA 200.7 01/03/2013 13:52 MHH7131

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 225 mg/L 0.5 10 EPA 200.7 01/02/2013 11:45 MHH7131

Calcium (Ca) 3580 mg/L 0.1 10 EPA 200.7 01/02/2013 11:45 MHH7131

Iron (Fe) 0.309 mg/L 0.1 10 EPA 200.7 01/02/2013 11:45 MHH7131

Magnesium (Mg) 1090 mg/L 0.05 10 EPA 200.7 01/02/2013 11:45 MHH7131

Manganese (Mn) 1.49 mg/L 0.05 10 EPA 200.7 01/02/2013 11:45 MHH7131

Page 6 of 28
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12120256

2012026874

Collection Date: 17-Dec-12 7:45 AM

Site: BIOREACTOR 2 INF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

DISSOLVED METALS BY ICP-MS

Selenium (Se) 15.4 ug/L 10 10 EPA 200.8 01/08/2013 10:46 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 12/26/2012 11:15 DJSULL1

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 12/26/2012 11:15 DJSULL1

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 12/26/2012 11:15 DJSULL1

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 12/26/2012 11:15 DJSULL1

Nickel (Ni) < 10 ug/L 10 10 EPA 200.8 12/26/2012 11:15 DJSULL1

Selenium (Se) 18.2 ug/L 10 10 EPA 200.8 12/26/2012 11:15 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 12/26/2012 11:15 DJSULL1

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 12/26/2012 11:15 DJSULL1

SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC)

Vendor Parameter Complete Vendor Method V_AS&C

2012026875

Collection Date: 17-Dec-12 7:45 AM

Site: BIOREACTOR 2 INF. HG BLANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC)

Vendor Parameter Complete Vendor Method V_BRAND

2012026876

Collection Date: 17-Dec-12 7:50 AM

Site: BIOREACTOR 2 EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

INORGANIC IONS BY IC

Bromide 100 mg/L 5 50 EPA 300.0 12/21/2012 19:53 JAHERMA

Chloride 7700 mg/L 100 1000 EPA 300.0 12/21/2012 19:53 JAHERMA

Sulfate 1600 mg/L 100 1000 EPA 300.0 12/21/2012 19:53 JAHERMA

MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC)

Vendor Parameter Complete Vendor Method V_BRAND

DISSOLVED METALS BY ICP

Manganese (Mn) 1.90 mg/L 0.05 10 EPA 200.7 01/03/2013 13:56 MHH7131

Page 7 of 28
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12120256

2012026876

Collection Date: 17-Dec-12 7:50 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) 211 mg/L 0.5 10 EPA 200.7 01/02/2013 11:49 MHH7131

Calcium (Ca) 3430 mg/L 0.1 10 EPA 200.7 01/02/2013 11:49 MHH7131

Iron (Fe) < 0.1 mg/L 0.1 10 EPA 200.7 01/02/2013 11:49 MHH7131

Magnesium (Mg) 1020 mg/L 0.05 10 EPA 200.7 01/02/2013 11:49 MHH7131

Manganese (Mn) 1.90 mg/L 0.05 10 EPA 200.7 01/02/2013 11:49 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 11.8 ug/L 5 5 EPA 200.8 01/08/2013 10:49 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 5 ug/L 5 5 EPA 200.8 12/26/2012 11:18 DJSULL1

Cadmium (Cd) < 5 ug/L 5 5 EPA 200.8 12/26/2012 11:18 DJSULL1

Chromium (Cr) < 5 ug/L 5 5 EPA 200.8 12/26/2012 11:18 DJSULL1

Copper (Cu) < 5 ug/L 5 5 EPA 200.8 12/26/2012 11:18 DJSULL1

Nickel (Ni) < 5 ug/L 5 5 EPA 200.8 12/26/2012 11:18 DJSULL1

Selenium (Se) < 5 ug/L 5 5 EPA 200.8 12/26/2012 11:18 DJSULL1

Silver (Ag) < 5 ug/L 5 5 EPA 200.8 12/26/2012 11:18 DJSULL1

Zinc (Zn) < 5 ug/L 5 5 EPA 200.8 12/26/2012 11:18 DJSULL1

SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC)

Vendor Parameter Complete Vendor Method V_AS&C

2012026877

Collection Date: 17-Dec-12 7:50 AM

Site: BIOREACTOR 2 EFF. HG BLANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC)

Vendor Parameter Complete Vendor Method V_BRAND

2012026878

Collection Date: 17-Dec-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

Manganese (Mn) 0.045 mg/L 0.005 1 EPA 200.7 01/03/2013 13:11 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 3.18 ug/L 1 1 EPA 200.8 01/08/2013 10:06 DJSULL1

Page 8 of 28
 

January 2, 2013 

Jay Perkins 

Duke Energy Analytical Laboratory 

Mail Code MGO3A2 (Building 7405) 

13339 Hagers Ferry Rd. 

Huntersville, NC 28078 

(704) 875-5245 

Project: Belews Creek (Flex Fuel) - WW (LIMS #J12120256) 

Dear Mr. Perkins, 

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

speciation on December 20, 2012. The samples were received in a sealed cooler at 0.0°C on 

December 22, 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 

 

 

Page 9 of 28
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 (Flex Fuel) - WW (LIMS #J12120256) 

January 2, 2013 

1. Sample Reception 

Four (4) aqueous samples in 125mL HDPE bottles (provided by Applied Speciation and 

Consulting) were submitted for selenium speciation analysis on December 20, 2012. The 

samples were received on December 22, 2012 in a sealed container at 0.0°C.

The chain-of-custody (COC) form received with the samples lists a LIMS number of J20256. 

Applied Speciation and Consulting is aware of the LIMS number format routinely used by 

the client (specifically, eight numerical characters following an alphabetical unit). The LIMS 

number listed on the COC does not conform to this format, and a small gap in the middle of 

the LIMS number listed suggests that there are characters missing. In this report, Applied 

Speciation and Consulting populated the remaining characters in the LIMS number 

identification given on the COC in order to conform to the standard LIMS number format. 

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

and ultra-violet radiation, and were designated discrete sample identifiers. 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 an autosampler 

Page 10 of 28
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 

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 minimum 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 December 28, 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 the 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. 

Page 11 of 28
The eMDL for methylseleninic acid and selenomethionine is calculated from the average 

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

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

bias the results for other selenium species. 

If you have any questions or concerns regarding this report, please feel free to contact me. 

Sincerely, 

Russell Gerads 

Vice President 

Applied Speciation and Consulting, LLC 

Page 12 of 28
Sample Results

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

Unknown Se 

Species (n)

FGD Purge Eff 9.3 29.1 ND (<1.2) ND (<1.8) ND (<1.8) 0.0 (0)

BioReactor 1 Inf 26.1 40.6 ND (<0.31) 1.98 ND (<0.44) 0.51 (1)

BioReactor 2 Inf 2.39 2.10 ND (<0.31) ND (<0.44) ND (<0.44) 0.0 (0)

BioReactor 2 Eff ND (<0.44) ND (<0.56) ND (<0.31) ND (<0.44) ND (<0.44) 0.0 (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

Report Generated by: Russell Gerads

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Belews Creek (Flex Fuel) - WW

Contact: Jay Perkins

Date: January 2, 2013

LIMS #J12120256

Page 13 of 28
Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 250x eMDL 1000x

Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.44 1.8

Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.56 2.3

SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.31 1.2

MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.44 1.8

SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.44 1.8

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) LCS 9.57 9.64 100.7

Se(VI) LCS 9.48 9.15 96.5

SeCN LCS 8.92 8.84 99.1

MeSe(IV) LCS 6.47 6.28 97.1

SeMe LCS 9.32 9.08 97.4

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Belews Creek (Flex Fuel) - WW

Contact: Jay Perkins

LIMS #J12120256

Date: January 2, 2013

Report Generated by: Russell Gerads

Page 14 of 28
Quality Control Summary - Matrix Duplicates

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

Se(IV) Batch QC 70.2 70.9 70.6 0.9

Se(VI) Batch QC 28.6 28.0 28.3 2.3

SeCN Batch QC ND (<1.2) ND (<1.2) NC NC

MeSe(IV) Batch QC 6.8 7.2 7.0 5.2

SeMe Batch QC ND (<1.8) ND (<1.8) 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 5560 5636 100.1 5560 5670 100.7 0.6

Se(VI) Batch QC 5045 4921 97.0 5045 4942 97.4 0.4

SeCN Batch QC 4575 4393 96.0 4575 4392 96.0 0.0

Report Generated by: Russell Gerads

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Belews Creek (Flex Fuel) - WW

Contact: Jay Perkins

LIMS #J12120256

Date: January 2, 2013

Page 15 of 28
Page 16 of 28
3958 6th Ave NW • Seattle, WA 98107 • T: 206-632-6206 • F: 206-632-6017 • www.brooksrand.com • brl@brooksrand.com

January 9, 2013

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: J12120256

Dear Mr. Perkins,

On December 22, 2012, Brooks Rand Labs (BRL) received three (3) wastewater samples and 

three (3) associated field blanks. An aliquot was removed from each sample bottle and filtered 

into a separate container designed for dissolved mercury (Hg) analysis. The sample volume 

from the original container was logged-in for total Hg analysis. All samples were received, 

prepared, analyzed, and stored according to BRL SOPs and EPA methodology.

Data used for regulatory purposes has a 24 hour filtration holding time requirement. Nonregulatory purposed data has a 48 hour filtration holding time. The samples were received

outside of the 48 hour filtration requirement and the results were qualified H. 

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

and may have been evaluated using reporting limits that have been adjusted to account for 

sample aliquot size. Please refer to the Sample Results page for sample-specific MDLs, MRLs, 

and other details. Aside from concentration qualifiers, all data was reported without further 

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 

Page 17 of 28
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 Labs, those found in the EPA SOW ILM03.0, 

Exhibit B, Section III, pg. B-18, and the USEPA Contract Laboratory Program National Functional Guidelines for Inorganic 

Superfund Data Review; USEPA; January 2010. 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 28
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 1251037-01 Influent Sample 12/17/2012 12/22/2012

BioReactor 1 Inf 1251037-02 Influent Sample 12/17/2012 12/22/2012

BioReactor 1 Inf Hg Blk 1251037-03 DIW Field Blank 12/17/2012 12/22/2012

BioReactor 1 Inf Hg Blk 1251037-04 DIW Field Blank 12/17/2012 12/22/2012

BioReactor 2 Inf 1251037-05 Influent Sample 12/17/2012 12/22/2012

BioReactor 2 Inf 1251037-06 Influent Sample 12/17/2012 12/22/2012

BioReactor 2 Inf Hg Blk 1251037-07 DIW Field Blank 12/17/2012 12/22/2012

BioReactor 2 Inf Hg Blk 1251037-08 DIW Field Blank 12/17/2012 12/22/2012

BioReactor 2 Eff 1251037-09 Effluent Sample 12/17/2012 12/22/2012

BioReactor 2 Eff 1251037-10 Effluent Sample 12/17/2012 12/22/2012

BioReactor 2 Eff Hg Blk 1251037-11 DIW Field Blank 12/17/2012 12/22/2012

BioReactor 2 Eff Hg Blk 1251037-12 DIW Field Blank 12/17/2012 12/22/2012

Batch Summary

Analyte Lab Matrix Method Prepared Analyzed Batch Sequence

Hg Water EPA 1631 12/28/2012 01/02/2013 B122438 1300003

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

Page 19 of 28
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Sample Results

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

BioReactor 1 Inf

1251037-01 Hg Influent T 77.3 3.79 10.1 ng/L B122438 1300003

1251037-02 Hg Influent D 42.8 H 0.76 2.02 ng/L B122438 1300003

BioReactor 1 Inf Hg Blk

1251037-03 Hg DIW T 0.15 U 0.15 0.39 ng/L B122438 1300003

1251037-04 Hg DIW D 0.15 H, U 0.15 0.41 ng/L B122438 1300003

BioReactor 2 Eff

1251037-09 Hg Effluent T 4.56 0.15 0.40 ng/L B122438 1300003

1251037-10 Hg Effluent D 0.76 H 0.15 0.39 ng/L B122438 1300003

BioReactor 2 Eff Hg Blk

1251037-11 Hg DIW T 0.15 U 0.15 0.41 ng/L B122438 1300003

1251037-12 Hg DIW D 0.15 H, U 0.15 0.40 ng/L B122438 1300003

BioReactor 2 Inf

1251037-05 Hg Influent T 13.0 0.38 1.01 ng/L B122438 1300003

1251037-06 Hg Influent D 1.10 H 0.15 0.40 ng/L B122438 1300003

BioReactor 2 Inf Hg Blk

1251037-07 Hg DIW T 0.15 U 0.15 0.40 ng/L B122438 1300003

1251037-08 Hg DIW D 0.15 H, U 0.15 0.40 ng/L B122438 1300003

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

Page 20 of 28
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Accuracy & Precision Summary

Batch: B122438

Analyte Native Spike Result Units REC & Limits RPD & Limits

Method: EPA 1631

Lab Matrix: Water

Sample

B122438-SRM1 Certified Reference Material (1249026, NIST 1641d 1000x dilution)

Hg 15.68 15.90 ng/L 101% 85-115

B122438-MS2 Matrix Spike (1251036-01)

Hg 60.93 505.1 539.5 ng/L 95% 71-125

B122438-MSD2 Matrix Spike Duplicate (1251036-01)

Hg 60.93 505.1 554.2 ng/L 98% 71-125 243%

B122438-MS1 Matrix Spike (1252008-01)

Hg 2.17 8.199 10.41 ng/L 101% 71-125

B122438-MSD1 Matrix Spike Duplicate (1252008-01)

Hg 2.17 8.166 10.13 ng/L 98% 71-125 243%

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

Page 21 of 28
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Method Blanks & Reporting Limits

Batch: B122438

Method: EPA 1631

Matrix: Water

Analyte: Hg

Sample Result Units

B122438-BLK1 0.13 ng/L

B122438-BLK2 0.14 ng/L

B122438-BLK3 0.13 ng/L

B122438-BLK4 0.14 ng/L

Average: 0.14 Standard Deviation: 0.01 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 28
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Instrument Calibration

Sequence: 1300003

Instrument: THG-06(MerxT) Method: EPA 1631

Date: 01/02/2013

Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg

Lab ID True Value Result Units REC & Limits

1300003-IBL1 2.77 pg of Hg

1300003-IBL2 4.00 pg of Hg

1300003-IBL3 4.87 pg of Hg

1300003-IBL4 4.70 pg of Hg

1300003-CAL1 10.00 11.14 pg of Hg 111%

1300003-CAL2 25.00 24.59 pg of Hg 98%

1300003-CAL3 100.0 100.6 pg of Hg 101%

1300003-CAL4 500.0 487.0 pg of Hg 97%

1300003-CAL5 2500 2472 pg of Hg 99%

1300003-CAL6 10000 9487 pg of Hg 95%

1300003-ICV1 1568 1590 pg of Hg 101% 85-115

1300003-CCB1 7.16 pg of Hg

1300003-CCV1 500.0 500.5 pg of Hg 100% 77-123

1300003-CCB2 5.73 pg of Hg

1300003-CCB3 5.16 pg of Hg

1300003-CCB4 4.63 pg of Hg

1300003-CCV2 500.0 500.1 pg of Hg 100% 77-123

1300003-CCB5 5.66 pg of Hg

1300003-CCV3 500.0 498.3 pg of Hg 100% 77-123

1300003-CCB6 5.20 pg of Hg

1300003-CCV4 500.0 483.4 pg of Hg 97% 77-123

1300003-CCB7 4.64 pg of Hg

1300003-CCV5 500.0 485.1 pg of Hg 97% 77-123

1300003-CCB8 6.39 pg of Hg

1300003-CCV6 500.0 487.1 pg of Hg 97% 77-123

1300003-CCB9 5.62 pg of Hg

1300003-CCV7 500.0 483.0 pg of Hg 97% 77-123

1300003-CCBA 4.80 pg of Hg

1300003-CCV8 500.0 490.7 pg of Hg 98% 77-123

1300003-CCBB 4.97 pg of Hg

1300003-CCV9 500.0 484.0 pg of Hg 97% 77-123

1300003-CCBC 5.77 pg of Hg

1300003-CCVA 500.0 479.4 pg of Hg 96% 77-123

1300003-CCBD 5.76 pg of Hg

1300003-CCVB 500.0 475.8 pg of Hg 95% 77-123

1300003-CCBE 5.08 pg of Hg

1300003-CCVC 500.0 442.2 pg of Hg 88% 77-123

1300003-CCBF 5.99 pg of Hg

1300003-CCVD 500.0 447.7 pg of Hg 90% 77-123

1300003-CCBG 6.40 pg of Hg

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

Page 23 of 28
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Sample Containers

Lab ID: 1251037-01 Report Matrix: Influent

Sample: BioReactor 1 Inf Sample Type: Sample Received: 12/22/2012

Collected: 12/17/2012

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

A 71666330

10

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

Lab ID: 1251037-02 Report Matrix: Influent

Sample: BioReactor 1 Inf Sample Type: Sample Received: 12/22/2012

Collected: 12/17/2012

Comments: Qualify H

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

A 71691270

10

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

Comments: split from THg container

Lab ID: 1251037-03 Report Matrix: DIW

Sample: BioReactor 1 Inf Hg Blk Sample Type: Field Blank Received: 12/22/2012

Collected: 12/17/2012

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

A 71666330

10

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

Lab ID: 1251037-04 Report Matrix: DIW

Sample: BioReactor 1 Inf Hg Blk Sample Type: Field Blank Received: 12/22/2012

Collected: 12/17/2012

Comments: Qualify H

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

A 71691270

10

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

Comments: split from THg container

Lab ID: 1251037-05 Report Matrix: Influent

Sample: BioReactor 2 Inf Sample Type: Sample Received: 12/22/2012

Collected: 12/17/2012

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

A 71666330

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

Page 24 of 28
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Sample Containers

Lab ID: 1251037-06 Report Matrix: Influent

Sample: BioReactor 2 Inf Sample Type: Sample Received: 12/22/2012

Collected: 12/17/2012

Comments: Qualify H

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

A 71691270

10

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

Comments: split from THg container

Lab ID: 1251037-07 Report Matrix: DIW

Sample: BioReactor 2 Inf Hg Blk Sample Type: Field Blank Received: 12/22/2012

Collected: 12/17/2012

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

A 71666330

10

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

Lab ID: 1251037-08 Report Matrix: DIW

Sample: BioReactor 2 Inf Hg Blk Sample Type: Field Blank Received: 12/22/2012

Collected: 12/17/2012

Comments: Qualify H

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

A 71691270

10

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

Comments: split from THg container

Lab ID: 1251037-09 Report Matrix: Effluent

Sample: BioReactor 2 Eff Sample Type: Sample Received: 12/22/2012

Collected: 12/17/2012

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

A 71666330

10

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

Lab ID: 1251037-10 Report Matrix: Effluent

Sample: BioReactor 2 Eff Sample Type: Sample Received: 12/22/2012

Collected: 12/17/2012

Comments: Qualify H

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

A 71691270

10

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

Comments: split from THg container

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

Page 25 of 28
Project ID: DUK-HV1201

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Sample Containers

Lab ID: 1251037-11 Report Matrix: DIW

Sample: BioReactor 2 Eff Hg Blk Sample Type: Field Blank Received: 12/22/2012

Collected: 12/17/2012

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

A 71666330

10

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

Lab ID: 1251037-12 Report Matrix: DIW

Sample: BioReactor 2 Eff Hg Blk Sample Type: Field Blank Received: 12/22/2012

Collected: 12/17/2012

Comments: Qualify H

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

A 71691270

10

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

Comments: split from THg container

Shipping Containers

Cooler

Tracking No: 535305196946 via FedEx

Temperature: -0.2 °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: December 22, 2012 11:20

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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