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: J13120030

Project Name: Ash Basin Bi-Monthly

Lab Contact: Jason C Perkins

Date: 12/19/2013

Customer Address: 3195 Pine Hall Rd

Customer Name(s): BIll K, Wayne C, and Melonie M

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 20
Sample ID's & Descriptions:

Sample ID Plant/Station

Collection 

Date and Time Collected By Sample Description

2013028907 BELEWS 28-Nov-13 7:30 AM P. GASSETT FGD Purge Eff 

2013028908 BELEWS 28-Nov-13 7:35 AM P. GASSETT EQ Tank Eff 

2013028909 BELEWS 28-Nov-13 7:40 AM P. GASSETT BioReactor 1 Inf 

2013028910 BELEWS 28-Nov-13 7:45 AM P. GASSETT BioReactor 2 Inf 

2013028911 BELEWS 28-Nov-13 7:50 AM P. GASSETT BioReactor 2 Eff 

2013028912 BELEWS 28-Nov-13 7:55 AM P. GASSETT Filter Blk 

2013028913 BELEWS 22-Nov-13 8:45 AM Dale Mace TRIP BLANK 

7 Total Samples

Page 2 of 20
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: 12/19/2013

Electronic Data Deliverable (EDD) Sent Separatel

Page 3 of 20
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13120030

2013028907

Collection Date: 28-Nov-13 7:30 AM

Site: FGD Purge Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

NITRITE + NITRATE (COLORIMETRIC)

Nitrite + Nitrate (Colorimetric) 0.548 mg-N/L 0.01 1 EPA 353.2 12/12/2013 11:52 BGN9034

INORGANIC IONS BY IC

Bromide 160 mg/L 5 50 EPA 300.0 12/06/2013 16:59 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 328 ug/L 5 100 EPA 245.1 12/06/2013 12:31 DKJOHN2

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 206 mg/L 0.5 10 EPA 200.7 12/11/2013 15:32 MHH7131

DISSOLVED METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 12/10/2013 14:07 DJSULL1

Selenium (Se) 213 ug/L 10 10 EPA 200.8 12/10/2013 14:07 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 458 ug/L 10 10 EPA 200.8 12/10/2013 10:52 DJSULL1

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 12/10/2013 10:52 DJSULL1

Chromium (Cr) 632 ug/L 10 10 EPA 200.8 12/10/2013 10:52 DJSULL1

Copper (Cu) 326 ug/L 10 10 EPA 200.8 12/10/2013 10:52 DJSULL1

Nickel (Ni) 399 ug/L 10 10 EPA 200.8 12/10/2013 10:52 DJSULL1

Selenium (Se) 4760 ug/L 10 10 EPA 200.8 12/10/2013 10:52 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 12/10/2013 10:52 DJSULL1

Zinc (Zn) 662 ug/L 10 10 EPA 200.8 12/10/2013 10:52 DJSULL1

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

Vendor Parameter Complete Vendor Method V_AS&C

2013028908

Collection Date: 28-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) 154 ug/L 2.5 50 EPA 245.1 12/06/2013 12:55 DKJOHN2

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 197 mg/L 0.5 10 EPA 200.7 12/11/2013 15:36 MHH7131

DISSOLVED METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 12/10/2013 14:10 DJSULL1

Selenium (Se) 85.8 ug/L 10 10 EPA 200.8 12/10/2013 14:10 DJSULL1

Page 4 of 20
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13120030

2013028908

Collection Date: 28-Nov-13 7:35 AM

Site: EQ Tank Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 273 ug/L 10 10 EPA 200.8 12/10/2013 10:55 DJSULL1

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 12/10/2013 10:55 DJSULL1

Chromium (Cr) 359 ug/L 10 10 EPA 200.8 12/10/2013 10:55 DJSULL1

Copper (Cu) 188 ug/L 10 10 EPA 200.8 12/10/2013 10:55 DJSULL1

Nickel (Ni) 258 ug/L 10 10 EPA 200.8 12/10/2013 10:55 DJSULL1

Selenium (Se) 2690 ug/L 10 10 EPA 200.8 12/10/2013 10:55 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 12/10/2013 10:55 DJSULL1

Zinc (Zn) 404 ug/L 10 10 EPA 200.8 12/10/2013 10:55 DJSULL1

2013028909

Collection Date: 28-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) 5.4 mg-N/L 0.25 25 EPA 353.2 12/12/2013 11:40 BGN9034

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) 188 mg/L 0.5 10 EPA 200.7 12/11/2013 15:41 MHH7131

DISSOLVED METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 12/10/2013 14:14 DJSULL1

Selenium (Se) 82.9 ug/L 10 10 EPA 200.8 12/10/2013 14:14 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 12/10/2013 10:59 DJSULL1

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 12/10/2013 10:59 DJSULL1

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 12/10/2013 10:59 DJSULL1

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 12/10/2013 10:59 DJSULL1

Nickel (Ni) 17.3 ug/L 10 10 EPA 200.8 12/10/2013 10:59 DJSULL1

Selenium (Se) 81.0 ug/L 10 10 EPA 200.8 12/10/2013 10:59 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 12/10/2013 10:59 DJSULL1

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 12/10/2013 10:59 DJSULL1

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

Vendor Parameter Complete Vendor Method V_AS&C

Page 5 of 20
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13120030

2013028910

Collection Date: 28-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) 203 mg/L 0.5 10 EPA 200.7 12/11/2013 15:45 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 12/10/2013 11:02 DJSULL1

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 12/10/2013 11:02 DJSULL1

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 12/10/2013 11:02 DJSULL1

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 12/10/2013 11:02 DJSULL1

Nickel (Ni) < 10 ug/L 10 10 EPA 200.8 12/10/2013 11:02 DJSULL1

Selenium (Se) 17.7 ug/L 10 10 EPA 200.8 12/10/2013 11:02 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 12/10/2013 11:02 DJSULL1

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 12/10/2013 11:02 DJSULL1

2013028911

Collection Date: 28-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 12/12/2013 11:42 BGN9034

INORGANIC IONS BY IC

Bromide 190 mg/L 5 50 EPA 300.0 12/06/2013 17:18 JAHERMA

Fluoride 17 mg/L 50 EPA 300.0 12/06/2013 17:18 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) 195 mg/L 0.5 10 EPA 200.7 12/11/2013 15:49 MHH7131

Page 6 of 20
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13120030

2013028911

Collection Date: 28-Nov-13 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-MS

Arsenic (As) < 5 ug/L 5 5 EPA 200.8 12/10/2013 11:05 DJSULL1

Cadmium (Cd) < 5 ug/L 5 5 EPA 200.8 12/10/2013 11:05 DJSULL1

Chromium (Cr) < 5 ug/L 5 5 EPA 200.8 12/10/2013 11:05 DJSULL1

Copper (Cu) < 5 ug/L 5 5 EPA 200.8 12/10/2013 11:05 DJSULL1

Nickel (Ni) < 5 ug/L 5 5 EPA 200.8 12/10/2013 11:05 DJSULL1

Selenium (Se) 5.02 ug/L 5 5 EPA 200.8 12/10/2013 11:05 DJSULL1

Silver (Ag) < 5 ug/L 5 5 EPA 200.8 12/10/2013 11:05 DJSULL1

Thallium (Tl) < ug/L 5 EPA 200.8 12/10/2013 11:05 DJSULL1

Vanadium (V) < ug/L 5 EPA 200.8 12/10/2013 11:05 DJSULL1

Zinc (Zn) < 5 ug/L 5 5 EPA 200.8 12/10/2013 11:05 DJSULL1

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

Vendor Parameter Complete Vendor Method V_AS&C

2013028912

Collection Date: 28-Nov-13 7:55 AM

Site: Filter Blk 

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 12/10/2013 13:34 DJSULL1

2013028913

Collection Date: 22-Nov-13 8:45 AM

Site: 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 12/11/2013 14:52 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 1 ug/L 1 1 EPA 200.8 12/10/2013 10:18 DJSULL1

Cadmium (Cd) < 1 ug/L 1 1 EPA 200.8 12/10/2013 10:18 DJSULL1

Chromium (Cr) < 1 ug/L 1 1 EPA 200.8 12/10/2013 10:18 DJSULL1

Copper (Cu) < 1 ug/L 1 1 EPA 200.8 12/10/2013 10:18 DJSULL1

Nickel (Ni) < 1 ug/L 1 1 EPA 200.8 12/10/2013 10:18 DJSULL1

Selenium (Se) < 1 ug/L 1 1 EPA 200.8 12/10/2013 10:18 DJSULL1

Silver (Ag) < 1 ug/L 1 1 EPA 200.8 12/10/2013 10:18 DJSULL1

Zinc (Zn) < 1 ug/L 1 1 EPA 200.8 12/10/2013 10:18 DJSULL1

Page 7 of 20
 

December 17, 2013 

Jay Perkins 

Duke Energy Analytical Laboratory 

Mail Code MGO3A2 (Building 7405) 

13339 Hagers Ferry Rd. 

Huntersville, NC 28078 

(704) 875-5245 

Project: Belews - FGD WWTS (Bi-Monthly & Flex Fuel) (LIMS# J13120030) 

Mr. Perkins,

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

selenium speciation, and arsenic speciation analyses on December 3, 2013. The samples were 

received in a sealed cooler at 2.7°C on December 4, 2013. Selenium speciation and arsenic 

speciation analyses were performed via ion chromatography inductively coupled plasma 

collision reaction cell mass spectrometry (IC-ICP-CRC-MS). Mercury quantitation was 

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

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 8 of 20
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 - FGD WWTS (Bi-Monthly & Flex Fuel) (LIMS# J13120030) 

December 17, 2013 

1. Sample Reception 

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

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

mercury quantitation. All samples were received in acceptable condition on December 4, 

2013 in a sealed container at 2.7°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 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). 

An aliquot of each sample submitted for arsenic speciation analysis was filtered (0.45μm) 

into a polypropylene centrifuge tube; all filtrates and original bottles were then stored in a 

secure, monitored refrigerator (maintained at a temperature of ≤6oC) until the analyses could 

be performed. 

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 9 of 20
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). 

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. 

Arsenic 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 December 5, 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. 

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 12, 2013. An aliquot of each 

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

Page 10 of 20
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. 

Arsenic Speciation Analysis by IC-ICP-CRC-MS Each sample was analyzed for arsenic 

speciation via ion chromatography inductively coupled plasma collision reaction cell mass 

spectrometry (IC-ICP-CRC-MS) on December 9, 2013. Aliquots of each sample are injected 

onto an anion exchange column and eluted isocratically. The eluting arsenic 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 specific collision gas. Polyatomic interferences, due to their inherently larger 

size, collide more frequently with the collision gas and therefore may be separated from the 

analyte of interest via kinetic energy discrimination (KED). A solid-state detector detects 

ions transmitted through the mass analyzer on the basis of their mass-to-charge ratio (m/z), 

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. With 

the exceptions noted below, all quality control parameters associated with these samples 

were within acceptance limits. 

The selenocyanate matrix spike and matrix spike duplicate (MS/MSD) recoveries were 

below the lower control limit of 75% (44.9% and 46.0%, respectively). The spiking solution 

also contained selenite, and the spike recoveries for selenite were above the upper control 

limit of 125% (158.1% and 157.1%, respectively). The low recoveries for selenocyanate 

correlate with the elevated recoveries of selenite, suggesting that the sample matrix induces 

species conversion. No species conversion was observed in the bracketing continuing 

calibration verification standards (CCVs), demonstrating that the applied method stabilizes 

these species in solution. Since the low recoveries observed for selenocyanate in the MS and 

MSD are therefore attributable to the sample matrix, no corrective actions were required. 

The reported results are deemed representative of the supplied samples and indicate that the 

spiked sample matrix is oxidizing in nature. 

Page 11 of 20
All arsenic speciation results were corrected for instrument drift in accordance with the 

continuing calibration verification standards. All associated quality control parameters were 

within acceptance limits signifying that the applied calculations were appropriate. 

The relative percent difference value for the dimethylarsinic acid matrix duplicate pair was 

greater than the control limit of 25%, at 34.8%. All associated dimethylarsinic acid results 

were near ten times the estimated method detection limit (eMDL). Results in this range 

exhibit a greater amount of variability. The calculated difference between the results was 

less than ten times the eMDL. No corrective action was necessary. 

The estimated method detection limit (eMDL) for mercury has been calculated using the 

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

submitted samples. 

The eMDL values for selenite, selenate, and selenocyanate are generated from replicate 

analyses of the lowest standard in the calibration curve. Not all selenium species are present 

in preparation blanks; therefore, eMDL calculations based on preparation blanks are 

artificially biased low. 

The eMDL for methylseleninic acid and selenomethionine is calculated from the average 

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

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

bias the results for other selenium species. 

The eMDL values for arsenite, arsenate, and dimethylarsinic acid are generated using the 

standard deviation of replicate analyses of the lowest standard in the calibration curve. The 

eMDL for monomethylarsonic acid has been calculated using the average eMDL of arsenite, 

arsenate, and dimethylarsinic acid. The calibration does not contain monomethylarsonic acid 

due to impurities in the standard which would bias the results for other arsenic species. 

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 12 of 20
Sample Results

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

Unknown Se 

Species (n)

FGD Purge Eff NR 136 50.2 ND (< 3.5) 13.8 ND (< 3.0) 0 (0)

BioReactor 1 Inf 0.268 27.4 36.1 ND (< 0.86) 1.77 ND (< 0.76) 0 (0)

BioReactor 2 Inf 0.0559 NR NR NR NR NR NR

BioReactor 2 Eff 0.0062 ND (< 0.82) ND (< 0.60) ND (< 0.86) ND (< 0.76) ND (< 0.76) 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, Selenium Speciation, and Arsenic Speciation Results for Duke Energy

Project Name: Belews - FGD WWTS (Bi-Monthly & Flex Fuel)

Contact: Jay Perkins

Date: December 17, 2013

LIMS #J13120030

Page 13 of 20
Sample Results

Sample ID As(III) As(V) MMAs DMAs

Unknown As 

Species

FGD Purge Eff ND (< 0.18) 1.57 ND (< 0.11) ND (< 0.033) 0.57

BioReactor 1 Inf ND (< 0.18) 1.05 ND (< 0.11) ND (< 0.033) 0.58

BioReactor 2 Inf NR NR NR NR NR

BioReactor 2 Eff ND (< 0.18) 0.52 ND (< 0.11) 0.232 0.21

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

NR = Analysis not requested

ND = Not detected at the applied dilution

MMAs = monomethylarsonic acid

DMAs = dimethylarsinic acid 

Unknown As Species = Total concentration of all unknown As species observed by IC-ICP-MS

Applied Speciation and Consulting, LLC

Total Mercury, Selenium Speciation, and Arsenic Speciation Results for Duke Energy

Project Name: Belews - FGD WWTS (Bi-Monthly & Flex Fuel)

Contact: Jay Perkins

LIMS #J13120030

Date: December 17, 2013

Report Generated by: Jeremy Maute

Page 14 of 20
Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 5x eMDL 25x eMDL 250x eMDL 1000x

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

Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.003 - - 0.82 3.3

Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.002 - - 0.60 2.4

SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.003 - - 0.86 3.5

MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.003 - - 0.76 3.0

SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.003 - - 0.76 3.0

As(III) 0.00 0.00 0.00 0.00 0.00 0.00 0.007 - 0.18 - -

As(V) 0.00 0.00 0.00 0.00 0.00 0.00 0.005 - 0.13 - -

MMAs 0.00 0.00 0.00 0.00 0.00 0.00 0.005 - 0.11 - -

DMAs 0.000 0.000 0.000 0.000 0.000 0.000 0.001 - 0.033 - -

eMDL = Estimated Method Detection Limit

*Please see narrative regarding eMDL calculations

Applied Speciation and Consulting, LLC

Total Mercury, Selenium Speciation, and Arsenic Speciation Results for Duke Energy

Project Name: Belews - FGD WWTS (Bi-Monthly & Flex Fuel)

Contact: Jay Perkins

LIMS #J13120030

Date: December 17, 2013

Report Generated by: Jeremy Maute

Page 15 of 20
Quality Control Summary - Certified Reference Materials

Analyte (μg/L) CRM True Value Result Recovery

Hg NIST 1641d 1568 1655 105.5

Se(IV) LCS 4.79 4.77 99.7

Se(VI) LCS 4.74 4.59 96.7

SeCN LCS 4.46 4.53 101.5

MeSe(IV) LCS 3.24 3.02 93.3

SeMe LCS 4.66 4.44 95.2

As(III) LCS 5.000 5.739 114.8

As(V) LCS 5.000 4.983 99.7

MMAs LCS 4.610 4.841 105.0

DMAs LCS 3.625 3.254 89.8

Report Generated by: Jeremy Maute

Applied Speciation and Consulting, LLC

Total Mercury, Selenium Speciation, and Arsenic Speciation Results for Duke Energy

Project Name: Belews - FGD WWTS (Bi-Monthly & Flex Fuel)

Contact: Jay Perkins

LIMS #J13120030

Date: December 17, 2013

Page 16 of 20
Quality Control Summary - Matrix Duplicates

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

Hg Batch QC 0.0065 0.0065 0.0065 0.0

Se(IV) Batch QC 22.29 20.68 21.49 7.5

Se(VI) Batch QC 35.54 36.30 35.92 2.1

SeCN Batch QC ND (< 0.86) ND (< 0.86) NC NC

MeSe(IV) Batch QC 1.11 0.95 1.03 16.3

SeMe Batch QC ND (< 0.76) ND (< 0.76) NC NC

As(III) Batch QC ND (< 0.18) ND (< 0.18) NC NC

As(V) Batch QC 0.53 0.48 0.50 10.5

MMAs Batch QC ND (< 0.11) ND (< 0.11) NC NC

DMAs Batch QC 0.27 0.39 0.33 34.8*

ND = Not detected at the applied dilution

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

*Associated results were near than ten times the eMDL. Difference was less than ten times the eMDL.

LIMS #J13120030

Date: December 17, 2013

Report Generated by: Jeremy Maute

Applied Speciation and Consulting, LLC

Total Mercury, Selenium Speciation, and Arsenic Speciation Results for Duke Energy

Project Name: Belews - FGD WWTS (Bi-Monthly & Flex Fuel)

Contact: Jay Perkins

Page 17 of 20
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 2.138 106.6 2.000 2.222 110.8 3.9

Se(IV) Batch QC 1390 2218 158.1* 1390 2205 157.1* 0.6

Se(VI) Batch QC 1261 1363 105.2 1261 1372 106.0 0.7

SeCN Batch QC 1144 513.2 44.9* 1144 525.7 46.0* 2.4

As(III) Batch QC 50.00 48.08 96.2 50.00 47.08 94.2 2.1

As(V) Batch QC 50.00 51.06 101.1 50.00 49.59 98.2 2.9

DMAs Batch QC 52.45 54.87 104.0 52.45 52.36 99.2 4.7

*Low/high recovery is due to matrix induced species conversion. Please see narrative.

Applied Speciation and Consulting, LLC

Total Mercury, Selenium Speciation, and Arsenic Speciation Results for Duke Energy

Project Name: Belews - FGD WWTS (Bi-Monthly & Flex Fuel)

Contact: Jay Perkins

LIMS #J13120030

Date: December 17, 2013

Report Generated by: Jeremy Maute

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