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: J13110386

Project Name: Frontier Sampling - Wed

Lab Contact: Jason C Perkins

Date: 12/13/2013

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 18
Sample ID's & Descriptions:

Sample ID Plant/Station

Collection 

Date and Time Collected By Sample Description

2013028500 BELEWS 20-Nov-13 7:30 AM P. GASSETT FGD Purge Eff 

2013028501 BELEWS 20-Nov-13 7:35 AM P. GASSETT EQ Tank Eff 

2013028502 BELEWS 20-Nov-13 7:40 AM P. GASSETT BIOREACTOR 1 INF 

2013028503 BELEWS 20-Nov-13 7:45 AM P. GASSETT BioReactor 2 Inf 

2013028504 BELEWS 20-Nov-13 7:50 AM P. GASSETT BioReactor 2 Eff 

2013028506 BELEWS 20-Nov-13 P. GASSETT FILTER BLANK 

2013028507 BELEWS 11-Nov-13 1:45 PM D. Baker METALS TRIP BLANK 

7 Total Samples

Page 2 of 18
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: 12/13/2013

Electronic Data Deliverable (EDD) Sent Separatel

Page 3 of 18
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13110386

2013028500

Collection Date: 20-Nov-13 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 71 mg/L 5 50 EPA 300.0 11/22/2013 14:31 JAHERMA

Chloride 6500 mg/L 100 1000 EPA 300.0 11/22/2013 14:31 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 129 ug/L 5 100 EPA 245.1 11/26/2013 13:18 DKJOHN2

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 203 mg/L 0.5 10 EPA 200.7 12/02/2013 13:04 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 347 ug/L 10 10 EPA 200.8 12/09/2013 12:46 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 211 ug/L 10 10 EPA 200.8 12/06/2013 13:13 DJSULL1

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:13 DJSULL1

Chromium (Cr) 273 ug/L 10 10 EPA 200.8 12/06/2013 13:13 DJSULL1

Copper (Cu) 123 ug/L 10 10 EPA 200.8 12/06/2013 13:13 DJSULL1

Nickel (Ni) 230 ug/L 10 10 EPA 200.8 12/06/2013 13:13 DJSULL1

Selenium (Se) 2540 ug/L 10 10 EPA 200.8 12/06/2013 13:13 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:13 DJSULL1

Thallium (Tl) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:13 DJSULL1

Vanadium (V) 212 ug/L 10 10 EPA 200.8 12/06/2013 13:13 DJSULL1

Zinc (Zn) 259 ug/L 10 10 EPA 200.8 12/06/2013 13:13 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 11/25/2013 10:28 DSBAKE1

TOTAL SUSPENDED SOLIDS

TSS 2500 mg/L 250 1 SM2540D TJA7067

2013028501

Collection Date: 20-Nov-13 7:35 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) 91.0 ug/L 2.5 50 EPA 245.1 11/26/2013 13:20 DKJOHN2

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 203 mg/L 0.5 10 EPA 200.7 12/02/2013 13:08 MHH7131

Page 4 of 18
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13110386

2013028501

Collection Date: 20-Nov-13 7:35 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) 159 ug/L 10 10 EPA 200.8 12/09/2013 12:50 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 179 ug/L 10 10 EPA 200.8 12/06/2013 13:17 DJSULL1

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:17 DJSULL1

Chromium (Cr) 230 ug/L 10 10 EPA 200.8 12/06/2013 13:17 DJSULL1

Copper (Cu) 104 ug/L 10 10 EPA 200.8 12/06/2013 13:17 DJSULL1

Nickel (Ni) 196 ug/L 10 10 EPA 200.8 12/06/2013 13:17 DJSULL1

Selenium (Se) 2140 ug/L 10 10 EPA 200.8 12/06/2013 13:17 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:17 DJSULL1

Thallium (Tl) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:17 DJSULL1

Vanadium (V) 178 ug/L 10 10 EPA 200.8 12/06/2013 13:17 DJSULL1

Zinc (Zn) 219 ug/L 10 10 EPA 200.8 12/06/2013 13:17 DJSULL1

2013028502

Collection Date: 20-Nov-13 7:40 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) 9.5 mg-N/L 0.25 25 EPA 353.2 11/22/2013 12:02 BGN9034

INORGANIC IONS BY IC

Bromide 69 mg/L 5 50 EPA 300.0 11/22/2013 14:50 JAHERMA

Chloride 6800 mg/L 100 1000 EPA 300.0 11/22/2013 14:50 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) 185 mg/L 0.5 10 EPA 200.7 12/02/2013 13:12 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 105 ug/L 10 10 EPA 200.8 12/09/2013 13:02 DJSULL1

Page 5 of 18
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13110386

2013028502

Collection Date: 20-Nov-13 7:40 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 12/06/2013 13:20 DJSULL1

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:20 DJSULL1

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:20 DJSULL1

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:20 DJSULL1

Nickel (Ni) 10.0 ug/L 10 10 EPA 200.8 12/06/2013 13:20 DJSULL1

Selenium (Se) 131 ug/L 10 10 EPA 200.8 12/06/2013 13:20 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:20 DJSULL1

Thallium (Tl) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:20 DJSULL1

Vanadium (V) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:20 DJSULL1

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:20 DJSULL1

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

Vendor Parameter Complete Vendor Method V_AS&C

TOTAL DISSOLVED SOLIDS

TDS 15000 mg/L 25 1 SM2540C 11/25/2013 10:28 DSBAKE1

TOTAL SUSPENDED SOLIDS

TSS < 5 mg/L 5 1 SM2540D TJA7067

2013028503

Collection Date: 20-Nov-13 7:45 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 12/02/2013 13:16 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:24 DJSULL1

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:24 DJSULL1

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:24 DJSULL1

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:24 DJSULL1

Nickel (Ni) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:24 DJSULL1

Selenium (Se) 27.2 ug/L 10 10 EPA 200.8 12/06/2013 13:24 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:24 DJSULL1

Thallium (Tl) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:24 DJSULL1

Vanadium (V) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:24 DJSULL1

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:24 DJSULL1

Page 6 of 18
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13110386

2013028503

Collection Date: 20-Nov-13 7:45 AM

Site: BioReactor 2 Inf 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

2013028504

Collection Date: 20-Nov-13 7:50 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 11/22/2013 12:03 BGN9034

INORGANIC IONS BY IC

Bromide 71 mg/L 5 50 EPA 300.0 11/22/2013 15:09 JAHERMA

Chloride 6800 mg/L 100 1000 EPA 300.0 11/22/2013 15:09 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) 197 mg/L 0.5 10 EPA 200.7 12/02/2013 13:20 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 5 ug/L 5 5 EPA 200.8 12/06/2013 13:27 DJSULL1

Cadmium (Cd) < 5 ug/L 5 5 EPA 200.8 12/06/2013 13:27 DJSULL1

Chromium (Cr) < 5 ug/L 5 5 EPA 200.8 12/06/2013 13:27 DJSULL1

Copper (Cu) < 5 ug/L 5 5 EPA 200.8 12/06/2013 13:27 DJSULL1

Nickel (Ni) < 5 ug/L 5 5 EPA 200.8 12/06/2013 13:27 DJSULL1

Selenium (Se) 7.24 ug/L 5 5 EPA 200.8 12/06/2013 13:27 DJSULL1

Silver (Ag) < 5 ug/L 5 5 EPA 200.8 12/06/2013 13:27 DJSULL1

Thallium (Tl) < 5 ug/L 5 5 EPA 200.8 12/06/2013 13:27 DJSULL1

Vanadium (V) < 5 ug/L 5 5 EPA 200.8 12/06/2013 13:27 DJSULL1

Zinc (Zn) < 5 ug/L 5 5 EPA 200.8 12/06/2013 13:27 DJSULL1

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

Vendor Parameter Complete Vendor Method V_AS&C

2013028506

Collection Date: 20-Nov-13

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 12/09/2013 12:55 DJSULL1

Page 7 of 18
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13110386

2013028507

Collection Date: 11-Nov-13 1:45 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 12/02/2013 12:56 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 1 ug/L 1 1 EPA 200.8 12/06/2013 13:06 DJSULL1

Cadmium (Cd) < 1 ug/L 1 1 EPA 200.8 12/06/2013 13:06 DJSULL1

Chromium (Cr) < 1 ug/L 1 1 EPA 200.8 12/06/2013 13:06 DJSULL1

Copper (Cu) < 1 ug/L 1 1 EPA 200.8 12/06/2013 13:06 DJSULL1

Nickel (Ni) < 1 ug/L 1 1 EPA 200.8 12/06/2013 13:06 DJSULL1

Selenium (Se) < 1 ug/L 1 1 EPA 200.8 12/06/2013 13:06 DJSULL1

Silver (Ag) < 1 ug/L 1 1 EPA 200.8 12/06/2013 13:06 DJSULL1

Thallium (Tl) < 1 ug/L 1 1 EPA 200.8 12/06/2013 13:06 DJSULL1

Vanadium (V) < 1 ug/L 1 1 EPA 200.8 12/06/2013 13:06 DJSULL1

Zinc (Zn) < 1 ug/L 1 1 EPA 200.8 12/06/2013 13:06 DJSULL1

Page 8 of 18
 

December 6, 2013 

Jay Perkins 

Duke Energy Analytical Laboratory 

Mail Code MGO3A2 (Building 7405) 

13339 Hagers Ferry Rd. 

Huntersville, NC 28078 

(704) 875-5245 

Project: Frontier Pilot (Belews Creek) WWTS (Wed Sampling) (LIMS# J13110386) 

Mr. Perkins,

Attached is the report associated with four (4) aqueous samples submitted for total mercury, 

hexavalent chromium, and selenium speciation analyses on November 21, 2013. The samples 

were received in a sealed cooler at 0.1°C on November 22, 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 9 of 18
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: Frontier Pilot (Belews Creek) WWTS (Wed Sampling) (LIMS# J13110386) 

December 6, 2013 

1. Sample Reception 

Three (3) aqueous samples were submitted for hexavalent chromium and selenium speciation 

analyses on November 21, 2013. Three (3) additional samples were submitted for total 

mercury quantitation. All samples were received in acceptable condition on November 22, 

2013 in a sealed container at 0.1°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 10 of 18
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 25, 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 December 5, 2013. An aliquot of each sample 

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

Page 11 of 18
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 December 4, 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 12 of 18
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 13 of 18
Sample Results

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

Unknown Se 

Species (n)

FGD Purge Eff NR ND (< 1.1) 327 48.1 12.6 ND (< 4.5) ND (< 4.5) 0 (0)

BioReactor 1 Inf 0.0887 ND (< 1.1) 70.8 30.0 ND (< 0.73) 1.9 ND (< 1.1) 0 (0)

BioReactor 2 Inf 0.0245 NR NR NR NR NR NR NR

BioReactor 2 Eff 0.0060 ND (< 1.1) ND (< 1.8) ND (< 0.86) ND (< 0.73) ND (< 1.1) ND (< 1.1) 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: Frontier Pilot (Belews Creek) WWTS (Wed Sampling)

Contact: Jay Perkins

Date: December 6, 2013

LIMS #J13110386

Page 14 of 18
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 -0.0005 -0.0001 0.0002 -0.0002 0.0003 0.0002 0.0009 - -

Cr(VI) -0.4 -1.0 -0.2 -0.2 -0.5 0.4 0.001 - - 1.1

Se(IV) 0.00 0.00 0.00 0.00 0.00 0.00 0.007 - 1.8 7.2

Se(VI) 0.00 0.00 0.00 0.00 0.00 0.00 0.003 - 0.86 3.5

SeCN 0.00 0.00 0.00 0.00 0.00 0.00 0.003 - 0.73 2.9

MeSe(IV) 0.00 0.00 0.00 0.00 0.00 0.00 0.005 - 1.1 4.5

SeMe 0.00 0.00 0.00 0.00 0.00 0.00 0.005 - 1.1 4.5

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 1635 104.3

Cr(VI) LCS 1.000 1.161 116.1

Se(IV) LCS 4.79 4.71 98.5

Se(VI) LCS 4.74 4.59 96.8

SeCN LCS 4.46 4.35 97.6

MeSe(IV) LCS 3.24 3.05 94.2

SeMe LCS 4.66 4.48 96.1

Applied Speciation and Consulting, LLC

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

Project Name: Frontier Pilot (Belews Creek) WWTS (Wed Sampling)

Contact: Jay Perkins

LIMS #J13110386

Date: December 6, 2013

Report Generated by: Jeremy Maute

Page 15 of 18
Quality Control Summary - Matrix Duplicates

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

Hg Batch QC 0.0151 0.0151 0.0151 0.4

Cr(VI) Batch QC ND (< 1.1) ND (< 1.1) NC NC

Se(IV) BioReactor 2 Eff ND (< 1.8) ND (< 1.8) NC NC

Se(VI) BioReactor 2 Eff ND (< 0.86) ND (< 0.86) NC NC

SeCN BioReactor 2 Eff ND (< 0.73) ND (< 0.73) NC NC

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

SeMe BioReactor 2 Eff ND (< 1.1) ND (< 1.1) NC NC

ND = Not detected at the applied dilution

NC = Value was not calculated due to one or more concentrations below the eMDL

Quality Control Summary - Matrix Spike/ Matrix Spike Duplicate

Analyte (μg/L) Sample ID Spike Conc MS Result Recovery Spike Conc MSD Result Recovery RPD

Hg Batch QC 2.000 2.273 112.9 2.000 2.210 109.8 2.8

Cr(VI) Batch QC 1000 860.1 86.0 1000 845.7 84.6 1.7

Se(IV) BioReactor 2 Eff 1390 1297 93.3 1390 1290 92.8 0.6

Se(VI) BioReactor 2 Eff 1261 1221 96.8 1261 1201 95.3 1.6

SeCN BioReactor 2 Eff 1144 1074 93.9 1144 1054 92.2 1.9

Applied Speciation and Consulting, LLC

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

Project Name: Frontier Pilot (Belews Creek) WWTS (Wed Sampling)

Contact: Jay Perkins

LIMS #J13110386

Date: December 6, 2013

Report Generated by: Jeremy Maute

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