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: J13110158

Project Name:

Lab Contact: Jason C Perkins

Date: 12/3/2013

Customer Address: 3195 Pine Hall Rd

Customer Name(s): Bill Kennedy, Wayne Chapman

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. 

Jason C Perkins

Page 1 of 19
Sample ID's & Descriptions:

Sample ID Plant/Station

Collection 

Date and Time Collected By Sample Description

2013027419 BELEWS 06-Nov-13 8:05 AM TO FGD Purge Eff 

2013027420 BELEWS 06-Nov-13 8:10 AM TO EQ Tank Eff 

2013027421 BELEWS 06-Nov-13 8:15 AM TO BIOREACTOR 1 INF 

2013027422 BELEWS 06-Nov-13 8:17 AM TO BioReactor 2 Inf 

2013027423 BELEWS 06-Nov-13 8:17 AM TO BioReactor 2 Eff 

2013027424 BELEWS 06-Nov-13 2:15 PM RG Bio Pilot Eff 

2013027425 BELEWS FILTER BLANK 

2013027426 BELEWS 28-Oct-13 4:35 PM DB METALS TRIP BLANK 

8 Total Samples

Page 2 of 19
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: 12/3/2013

Electronic Data Deliverable (EDD) Sent Separatel

Page 3 of 19
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13110158

2013027419

Collection Date: 06-Nov-13 8:05 AM

Site: FGD Purge Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

INORGANIC IONS BY IC

Bromide 99 mg/L 5 50 EPA 300.0 11/11/2013 15:23 JAHERMA

Chloride 7000 mg/L 100 1000 EPA 300.0 11/11/2013 15:23 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 219 ug/L 5 100 EPA 245.1 11/23/2013 10:13 DKJOHN2

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 210 mg/L 0.5 10 EPA 200.7 11/13/2013 12:22 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 147 ug/L 10 10 EPA 200.8 11/20/2013 14:02 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 172 ug/L 10 10 EPA 200.8 11/18/2013 14:49 DJSULL1

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 11/18/2013 14:49 DJSULL1

Chromium (Cr) 311 ug/L 10 10 EPA 200.8 11/18/2013 14:49 DJSULL1

Copper (Cu) 127 ug/L 10 10 EPA 200.8 11/18/2013 14:49 DJSULL1

Nickel (Ni) 243 ug/L 10 10 EPA 200.8 11/18/2013 14:49 DJSULL1

Selenium (Se) 4080 ug/L 10 10 EPA 200.8 11/18/2013 14:49 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 11/18/2013 14:49 DJSULL1

Thallium (Tl) < 10 ug/L 10 10 EPA 200.8 11/18/2013 14:49 DJSULL1

Vanadium (V) 192 ug/L 10 10 EPA 200.8 11/18/2013 14:49 DJSULL1

Zinc (Zn) 246 ug/L 10 10 EPA 200.8 11/18/2013 14:49 DJSULL1

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

Vendor Parameter Complete Vendor Method V_AS&C

TOTAL DISSOLVED SOLIDS

TDS 19000 mg/L 250 1 SM2540C 11/19/2013 14:19 DSBAKE1

TOTAL SUSPENDED SOLIDS

TSS 3200 mg/L 250 1 SM2540D 11/12/2013 12:27 DSBAKE1

2013027420

Collection Date: 06-Nov-13 8:10 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) 152 ug/L 2.5 50 EPA 245.1 11/23/2013 10:15 DKJOHN2

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 194 mg/L 0.5 10 EPA 200.7 11/13/2013 12:26 MHH7131

Page 4 of 19
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13110158

2013027420

Collection Date: 06-Nov-13 8:10 AM

Site: EQ Tank Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

DISSOLVED METALS BY ICP-MS

Selenium (Se) 122 ug/L 10 10 EPA 200.8 11/20/2013 14:05 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 145 ug/L 10 10 EPA 200.8 11/18/2013 14:53 DJSULL1

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 11/18/2013 14:53 DJSULL1

Chromium (Cr) 264 ug/L 10 10 EPA 200.8 11/18/2013 14:53 DJSULL1

Copper (Cu) 105 ug/L 10 10 EPA 200.8 11/18/2013 14:53 DJSULL1

Nickel (Ni) 202 ug/L 10 10 EPA 200.8 11/18/2013 14:53 DJSULL1

Selenium (Se) 3300 ug/L 10 10 EPA 200.8 11/18/2013 14:53 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 11/18/2013 14:53 DJSULL1

Thallium (Tl) < 10 ug/L 10 10 EPA 200.8 11/18/2013 14:53 DJSULL1

Vanadium (V) 177 ug/L 10 10 EPA 200.8 11/18/2013 14:53 DJSULL1

Zinc (Zn) 197 ug/L 10 10 EPA 200.8 11/18/2013 14:53 DJSULL1

2013027421

Collection Date: 06-Nov-13 8:15 AM

Site: BIOREACTOR 1 INF 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

NITRITE + NITRATE (COLORIMETRIC)

Nitrite + Nitrate (Colorimetric) < 0.01 mg-N/L 0.01 1 EPA 353.2 11/15/2013 11:37 BGN9034

INORGANIC IONS BY IC

Bromide 86 mg/L 5 50 EPA 300.0 11/11/2013 15:42 JAHERMA

Chloride 6400 mg/L 100 1000 EPA 300.0 11/11/2013 15:42 JAHERMA

Mercury by EPA 200.8 - (Analysis Performed by Applied Speciation and Consulting, LLC)

Vendor Parameter Complete ug/l Vendor Method V_AS&C

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 183 mg/L 0.5 10 EPA 200.7 11/13/2013 12:30 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 88.1 ug/L 10 10 EPA 200.8 11/20/2013 14:09 DJSULL1

Page 5 of 19
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13110158

2013027421

Collection Date: 06-Nov-13 8:15 AM

Site: BIOREACTOR 1 INF 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 11/18/2013 14:56 DJSULL1

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 11/18/2013 14:56 DJSULL1

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 11/18/2013 14:56 DJSULL1

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 11/18/2013 14:56 DJSULL1

Nickel (Ni) 24.6 ug/L 10 10 EPA 200.8 11/18/2013 14:56 DJSULL1

Selenium (Se) 76.8 ug/L 10 10 EPA 200.8 11/18/2013 14:56 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 11/18/2013 14:56 DJSULL1

Thallium (Tl) < 10 ug/L 10 10 EPA 200.8 11/18/2013 14:56 DJSULL1

Vanadium (V) < 10 ug/L 10 10 EPA 200.8 11/18/2013 14:56 DJSULL1

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 11/18/2013 14:56 DJSULL1

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

Vendor Parameter Complete Vendor Method V_AS&C

TOTAL DISSOLVED SOLIDS

TDS 14000 mg/L 25 1 SM2540C 11/19/2013 14:19 DSBAKE1

TOTAL SUSPENDED SOLIDS

TSS < 5 mg/L 5 1 SM2540D 11/12/2013 12:27 DSBAKE1

2013027422

Collection Date: 06-Nov-13 8:17 AM

Site: BioReactor 2 Inf 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

Mercury by EPA 200.8 - (Analysis Performed by Applied Speciation and Consulting, LLC)

Vendor Parameter Complete ug/l Vendor Method V_AS&C

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 187 mg/L 0.5 10 EPA 200.7 11/13/2013 12:34 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 11/18/2013 15:00 DJSULL1

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 11/18/2013 15:00 DJSULL1

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 11/18/2013 15:00 DJSULL1

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 11/18/2013 15:00 DJSULL1

Nickel (Ni) < 10 ug/L 10 10 EPA 200.8 11/18/2013 15:00 DJSULL1

Selenium (Se) < 10 ug/L 10 10 EPA 200.8 11/18/2013 15:00 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 11/18/2013 15:00 DJSULL1

Thallium (Tl) < 10 ug/L 10 10 EPA 200.8 11/18/2013 15:00 DJSULL1

Vanadium (V) < 10 ug/L 10 10 EPA 200.8 11/18/2013 15:00 DJSULL1

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 11/18/2013 15:00 DJSULL1

Page 6 of 19
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13110158

2013027422

Collection Date: 06-Nov-13 8:17 AM

Site: BioReactor 2 Inf 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

2013027423

Collection Date: 06-Nov-13 8:17 AM

Site: BioReactor 2 Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

NITRITE + NITRATE (COLORIMETRIC)

Nitrite + Nitrate (Colorimetric) < 0.01 mg-N/L 0.01 1 EPA 353.2 11/15/2013 11:34 BGN9034

INORGANIC IONS BY IC

Bromide 86 mg/L 5 50 EPA 300.0 11/11/2013 16:01 JAHERMA

Chloride 6300 mg/L 100 1000 EPA 300.0 11/11/2013 16:01 JAHERMA

Mercury by EPA 200.8 - (Analysis Performed by Applied Speciation and Consulting, LLC)

Vendor Parameter Complete ug/l Vendor Method V_AS&C

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 194 mg/L 0.5 10 EPA 200.7 11/13/2013 12:38 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 5 ug/L 5 5 EPA 200.8 11/18/2013 15:13 DJSULL1

Cadmium (Cd) < 5 ug/L 5 5 EPA 200.8 11/18/2013 15:13 DJSULL1

Chromium (Cr) < 5 ug/L 5 5 EPA 200.8 11/18/2013 15:13 DJSULL1

Copper (Cu) < 5 ug/L 5 5 EPA 200.8 11/18/2013 15:13 DJSULL1

Nickel (Ni) < 5 ug/L 5 5 EPA 200.8 11/18/2013 15:13 DJSULL1

Selenium (Se) < 5 ug/L 5 5 EPA 200.8 11/18/2013 15:13 DJSULL1

Silver (Ag) < 5 ug/L 5 5 EPA 200.8 11/18/2013 15:13 DJSULL1

Thallium (Tl) < 5 ug/L 5 5 EPA 200.8 11/18/2013 15:13 DJSULL1

Vanadium (V) < 5 ug/L 5 5 EPA 200.8 11/18/2013 15:13 DJSULL1

Zinc (Zn) < 5 ug/L 5 5 EPA 200.8 11/18/2013 15:13 DJSULL1

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

Vendor Parameter Complete Vendor Method V_AS&C

2013027424

Collection Date: 06-Nov-13 2:15 PM

Site: Bio Pilot Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

NITRITE + NITRATE (COLORIMETRIC)

Nitrite + Nitrate (Colorimetric) < 0.01 mg-N/L 0.01 1 EPA 353.2 11/15/2013 11:29 BGN9034

Mercury by EPA 200.8 - (Analysis Performed by Applied Speciation and Consulting, LLC)

Vendor Parameter Complete ug/l Vendor Method V_AS&C

Page 7 of 19
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13110158

2013027424

Collection Date: 06-Nov-13 2:15 PM

Site: Bio Pilot Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 186 mg/L 0.5 10 EPA 200.7 11/13/2013 12:42 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 72.7 ug/L 10 10 EPA 200.8 11/20/2013 14:12 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 11/18/2013 15:16 DJSULL1

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 11/18/2013 15:16 DJSULL1

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 11/18/2013 15:16 DJSULL1

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 11/18/2013 15:16 DJSULL1

Nickel (Ni) 19.0 ug/L 10 10 EPA 200.8 11/18/2013 15:16 DJSULL1

Selenium (Se) 63.5 ug/L 10 10 EPA 200.8 11/18/2013 15:16 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 11/18/2013 15:16 DJSULL1

Thallium (Tl) < 10 ug/L 10 10 EPA 200.8 11/18/2013 15:16 DJSULL1

Vanadium (V) < 10 ug/L 10 10 EPA 200.8 11/18/2013 15:16 DJSULL1

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 11/18/2013 15:16 DJSULL1

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

Vendor Parameter Complete Vendor Method V_AS&C

2013027425

Collection Date:

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 1 1 EPA 200.8 11/20/2013 13:26 DJSULL1

2013027426

Collection Date: 28-Oct-13 4:35 PM

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 0.05 1 EPA 200.7 11/13/2013 11:41 MHH7131

Page 8 of 19
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13110158

2013027426

Collection Date: 28-Oct-13 4:35 PM

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 1 1 EPA 200.8 11/18/2013 14:09 DJSULL1

Cadmium (Cd) < 1 ug/L 1 1 EPA 200.8 11/18/2013 14:09 DJSULL1

Chromium (Cr) < 1 ug/L 1 1 EPA 200.8 11/18/2013 14:09 DJSULL1

Copper (Cu) < 1 ug/L 1 1 EPA 200.8 11/18/2013 14:09 DJSULL1

Nickel (Ni) < 1 ug/L 1 1 EPA 200.8 11/18/2013 14:09 DJSULL1

Selenium (Se) < 1 ug/L 1 1 EPA 200.8 11/18/2013 14:09 DJSULL1

Silver (Ag) < 1 ug/L 1 1 EPA 200.8 11/18/2013 14:09 DJSULL1

Thallium (Tl) < 1 ug/L 1 1 EPA 200.8 11/18/2013 14:09 DJSULL1

Vanadium (V) < 1 ug/L 1 1 EPA 200.8 11/18/2013 14:09 DJSULL1

Zinc (Zn) < 1 ug/L 1 1 EPA 200.8 11/18/2013 14:09 DJSULL1

Page 9 of 19
 

November 27, 2013 

Jay Perkins 

Duke Energy Analytical Laboratory 

Mail Code MGO3A2 (Building 7405) 

13339 Hagers Ferry Rd. 

Huntersville, NC 28078 

(704) 875-5245 

Project: Fontier Pilot (Belews Creek) WWTS (Weekly Sampling) (LIMS# J13110158) 

Mr. Perkins,

Attached is the report associated with five (5) aqueous samples submitted for total mercury, 

hexavalent chromium, and selenium speciation analyses on November 11, 2013. The samples 

were received in a sealed cooler at -0.2°C on November 12, 2013. Mercury quantitation was 

performed via cold vapor inductively coupled plasma mass spectrometry (CV-ICP-MS). 

Hexavalent chromium analysis was performed via ion chromatography inductively coupled 

plasma dynamic reaction cell mass spectrometry (IC-ICP-DRC-MS). 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 analyses are 

addressed in the following report. 

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

 Sincerely, 

Jeremy Maute 

Project Coordinator 

Applied Speciation and Consulting, LLC 

Page 10 of 19
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: Fontier Pilot (Belews Creek) WWTS (Weekly Sampling) (LIMS# J13110158) 

November 27, 2013 

1. Sample Reception 

Four (4) aqueous samples were submitted for hexavalent chromium and selenium speciation 

analyses on November 11, 2013. Four (4) additional samples were submitted for total 

mercury quantitation. All samples were received in acceptable condition on November 12, 

2013 in a sealed container at -0.2°C.

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

and ultra-violet radiation, and were designated discrete sample identifiers. The 40mL 

borosilicate glass vials submitted for total mercury were preserved with bromine 

monochloride (BrCl) solution. The resulting samples were stored in a secure polyethylene 

container, known to be free from trace metals contamination, until the analyses could be 

performed. 

An aliquot of each sample submitted for hexavalent chromium analysis was filtered (0.45um) 

and stored in a secure refrigerator maintained at a temperature of 4oC, until the analyses 

could be performed. 

An aliquot of each sample requiring selenium speciation evaluation was filtered (0.45μm) 

and each filtrate was stored in a secure, monitored cryofreezer (maintained at a temperature 

of -80°C) 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. 

Page 11 of 19
Total Mercury Quantitation by CV-ICP-MS All samples and preparation blanks for total 

mercury quantitation were preserved with 2% (v/v) BrCl. The resulting samples were 

analyzed for mercury via cold vapor inductively coupled plasma mass spectrometry (CVICP-MS). 

Hexavalent Chromium Analysis by IC-ICP-DRC-MS Prior to analysis, all samples were 

injected directly into autosampler vials. 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. 

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 

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. 

Total Mercury Quantitation by CV-ICP-MS The sample fractions for total mercury 

quantitation were analyzed by cold vapor inductively coupled plasma mass spectrometry 

(CV-ICP-MS) on November 18, 2013. Aliquots of each sample are reacted with a reductant 

in-line and transported to a gas-liquid separator. The volatile elemental mercury that is 

formed is then swept by a stream of argon gas 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 separated 

on the basis of their mass-to-charge ratio (m/z) by a mass spectrometer. A solid-state 

detector detects ions transmitted through the mass analyzer and the resulting current is 

processed by a data handling system. 

Hexavalent Chromium Analysis by IC-ICP-DRC-MS Each sample for hexavalent chromium 

analysis was analyzed by ion chromatography inductively coupled plasma dynamic reaction 

cell mass spectrometry (IC-ICP-DRC-MS) on November 26, 2013. An aliquot of each 

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

Page 12 of 19
gradient. The eluting chromium 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 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. 

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 November 15, 2013. 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 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 values for methylseleninic acid and selenomethionine are 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. 

The eMDL values for hexavalent chromium and mercury are calculated using the standard 

deviation of the preparation blanks preserved and analyzed concurrently with the submitted 

samples. 

Page 13 of 19
If you have any questions or concerns regarding this report, please feel free to contact me. 

Sincerely, 

Jeremy Maute 

Project Coordinator 

Applied Speciation and Consulting, LLC 

Page 14 of 19
Sample Results

Sample ID Total Hg Cr(VI) Se(IV) Se(VI) SeCN MeSe(IV) SeMe

Unknown Se 

Species (n)

FGD Purge Eff NR 1.8 74.0 50.5 ND (< 2.1) 3.1 ND (< 1.7) 0 (0)

BioReactor 1 Inf 0.232 ND (< 1.0) 18.5 35.9 ND (< 0.53) 0.65 ND (< 0.43) 2.64 (1)

BioReactor 2 Inf 0.0345 NR NR NR NR NR NR NR

BioReactor 2 Eff 0.0076 1.6 ND (< 0.47) ND (< 0.30) ND (< 0.53) ND (< 0.43) ND (< 0.43) 0 (0)

Bio Pilot Eff 0.0725 ND (< 1.0) 17.3 36.3 ND (< 0.53) ND (< 0.43) ND (< 0.43) 0 (0)

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

NR = Analysis not requested

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: Jeremy Maute

Applied Speciation and Consulting, LLC

Total Mercury, Hexavalent Chromium, and Selenium Speciation Results for Duke Energy

Project Name: Fontier Pilot (Belews Creek) WWTS (Weekly Sampling)

Contact: Jay Perkins

Date: November 27, 2013

LIMS #J13110158

Page 15 of 19
Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 5x eMDL 250x eMDL 1000x

Hg -0.0003 -0.0002 -0.0007 -0.0004 -0.0004 0.0002 0.0001 0.0006 - -

Cr(VI) -0.8 -0.4 -0.2 0.0 -0.3 0.3 0.002 - - 1.0

Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.002 - 0.47 1.9

Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.001 - 0.30 1.2

SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.002 - 0.53 2.1

MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.002 - 0.43 1.7

SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.002 - 0.43 1.7

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

Hg NIST 1641d 1568 1626 103.7

Cr(VI) LCS 1.000 1.054 105.4

Se(IV) LCS 9.57 9.28 96.9

Se(VI) LCS 9.48 9.22 97.3

SeCN LCS 8.92 8.55 95.9

MeSe(IV) LCS 6.47 6.23 96.3

SeMe LCS 9.32 8.84 94.8

Applied Speciation and Consulting, LLC

Total Mercury, Hexavalent Chromium, and Selenium Speciation Results for Duke Energy

Project Name: Fontier Pilot (Belews Creek) WWTS (Weekly Sampling)

Contact: Jay Perkins

LIMS #J13110158

Date: November 27, 2013

Report Generated by: Jeremy Maute

Page 16 of 19
Quality Control Summary - Matrix Duplicates

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

Hg Batch QC 0.1934 0.1955 0.1945 1.1

Cr(VI) Bio Pilot Eff ND (< 1.0) ND (< 1.0) NC NC

Se(IV) Bio Pilot Eff 17.33 18.07 17.70 4.2

Se(VI) Bio Pilot Eff 36.27 38.29 37.28 5.4

SeCN Bio Pilot Eff ND (< 0.53) ND (< 0.53) NC NC

MeSe(IV) Bio Pilot Eff ND (< 0.43) ND (< 0.43) NC NC

SeMe Bio Pilot Eff ND (< 0.43) ND (< 0.43) 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

Hg Batch QC 2.000 2.347 107.6 2.000 2.320 106.3 1.2

Cr(VI) Bio Pilot Eff 1000 986.4 98.6 1000 986.9 98.7 0.0

Se(IV) Bio Pilot Eff 1390 1312 93.1 1390 1344 95.4 2.4

Se(VI) Bio Pilot Eff 1261 1203 92.4 1261 1224 94.1 1.7

SeCN Bio Pilot Eff 1144 1037 90.6 1144 1056 92.3 1.8

Applied Speciation and Consulting, LLC

Total Mercury, Hexavalent Chromium, and Selenium Speciation Results for Duke Energy

Project Name: Fontier Pilot (Belews Creek) WWTS (Weekly Sampling)

Contact: Jay Perkins

LIMS #J13110158

Date: November 27, 2013

Report Generated by: Jeremy Maute

Page 17 of 19
Page 18 of 19
Page 19 of 19