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: J13110436

Project Name: WWTS FGD-Routine 2013

Lab Contact: Jason C Perkins

Date: 1/6/2014

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 17
Sample ID's & Descriptions:

Sample ID Plant/Station

Collection 

Date and Time Collected By Sample Description

2013028681 BELEWS 22-Nov-13 9:49 AM MC/TO FGD Purge Eff 

2013028682 BELEWS 22-Nov-13 9:50 AM MC/TO EQ Tank Eff 

2013028683 BELEWS 22-Nov-13 9:55 AM MC/TO BioReactor 1 Inf 

2013028684 BELEWS 22-Nov-13 9:55 AM MC/TO BioReactor 2 Inf 

2013028685 BELEWS 22-Nov-13 10:00 AM MC/TO BioReactor 2 Eff 

2013028686 BELEWS 22-Nov-13 10:00 AM MC/TO Filter Blk 

2013028687 BELEWS 11-Nov-13 1:45 PM DB TRIP BLANK 

7 Total Samples

Page 2 of 17
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: 1/6/2014

Electronic Data Deliverable (EDD) Sent Separatel

Page 3 of 17
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13110436

2013028681

Collection Date: 22-Nov-13 9:49 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) 9.0 mg-N/L 0.25 25 EPA 353.2 12/05/2013 13:55 TLINN

INORGANIC IONS BY IC

Bromide 130 mg/L 5 50 EPA 300.0 12/02/2013 22:19 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 8.10 ug/L 5 100 EPA 245.1 12/06/2013 12:59 DKJOHN2

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 235 mg/L 0.5 10 EPA 200.7 12/02/2013 13:24 MHH7131

DISSOLVED METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 12/09/2013 13:05 DJSULL1

Selenium (Se) 73.9 ug/L 10 10 EPA 200.8 12/09/2013 13:05 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 21.0 ug/L 10 10 EPA 200.8 12/06/2013 13:38 DJSULL1

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:38 DJSULL1

Chromium (Cr) 21.9 ug/L 10 10 EPA 200.8 12/06/2013 13:38 DJSULL1

Copper (Cu) 10.6 ug/L 10 10 EPA 200.8 12/06/2013 13:38 DJSULL1

Nickel (Ni) 157 ug/L 10 10 EPA 200.8 12/06/2013 13:38 DJSULL1

Selenium (Se) 274 ug/L 10 10 EPA 200.8 12/06/2013 13:38 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:38 DJSULL1

Zinc (Zn) 49.9 ug/L 10 10 EPA 200.8 12/06/2013 13:38 DJSULL1

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

Vendor Parameter Complete Vendor Method V_AS&C

2013028682

Collection Date: 22-Nov-13 9:50 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) 7.85 ug/L 2.5 50 EPA 245.1 12/06/2013 12:38 DKJOHN2

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 204 mg/L 0.5 10 EPA 200.7 12/02/2013 13:29 MHH7131

DISSOLVED METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 12/09/2013 13:08 DJSULL1

Selenium (Se) 57.4 ug/L 10 10 EPA 200.8 12/09/2013 13:08 DJSULL1

Page 4 of 17
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13110436

2013028682

Collection Date: 22-Nov-13 9:50 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) 17.6 ug/L 10 10 EPA 200.8 12/06/2013 13:41 DJSULL1

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:41 DJSULL1

Chromium (Cr) 18.8 ug/L 10 10 EPA 200.8 12/06/2013 13:41 DJSULL1

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:41 DJSULL1

Nickel (Ni) 106 ug/L 10 10 EPA 200.8 12/06/2013 13:41 DJSULL1

Selenium (Se) 256 ug/L 10 10 EPA 200.8 12/06/2013 13:41 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:41 DJSULL1

Zinc (Zn) 33.5 ug/L 10 10 EPA 200.8 12/06/2013 13:41 DJSULL1

2013028683

Collection Date: 22-Nov-13 9:55 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) 9.0 mg-N/L 0.25 25 EPA 353.2 12/05/2013 13:56 TLINN

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) 184 mg/L 0.5 10 EPA 200.7 12/02/2013 13:33 MHH7131

DISSOLVED METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 12/09/2013 13:12 DJSULL1

Selenium (Se) 67.1 ug/L 10 10 EPA 200.8 12/09/2013 13:12 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:45 DJSULL1

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:45 DJSULL1

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:45 DJSULL1

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:45 DJSULL1

Nickel (Ni) 18.3 ug/L 10 10 EPA 200.8 12/06/2013 13:45 DJSULL1

Selenium (Se) 82.1 ug/L 10 10 EPA 200.8 12/06/2013 13:45 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:45 DJSULL1

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:45 DJSULL1

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

Vendor Parameter Complete Vendor Method V_AS&C

Page 5 of 17
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13110436

2013028684

Collection Date: 22-Nov-13 9:55 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) 179 mg/L 0.5 10 EPA 200.7 12/02/2013 13:37 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:48 DJSULL1

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:48 DJSULL1

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:48 DJSULL1

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:48 DJSULL1

Nickel (Ni) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:48 DJSULL1

Selenium (Se) 19.4 ug/L 10 10 EPA 200.8 12/06/2013 13:48 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:48 DJSULL1

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 12/06/2013 13:48 DJSULL1

2013028685

Collection Date: 22-Nov-13 10:00 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 12/05/2013 13:57 TLINN

INORGANIC IONS BY IC

Bromide 87 mg/L 5 50 EPA 300.0 12/02/2013 22:38 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) 182 mg/L 0.5 10 EPA 200.7 12/02/2013 13:41 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 5 ug/L 5 5 EPA 200.8 12/06/2013 13:52 DJSULL1

Cadmium (Cd) < 5 ug/L 5 5 EPA 200.8 12/06/2013 13:52 DJSULL1

Chromium (Cr) < 5 ug/L 5 5 EPA 200.8 12/06/2013 13:52 DJSULL1

Copper (Cu) < 5 ug/L 5 5 EPA 200.8 12/06/2013 13:52 DJSULL1

Nickel (Ni) < 5 ug/L 5 5 EPA 200.8 12/06/2013 13:52 DJSULL1

Selenium (Se) 6.63 ug/L 5 5 EPA 200.8 12/06/2013 13:52 DJSULL1

Silver (Ag) < 5 ug/L 5 5 EPA 200.8 12/06/2013 13:52 DJSULL1

Zinc (Zn) < 5 ug/L 5 5 EPA 200.8 12/06/2013 13:52 DJSULL1

Page 6 of 17
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13110436

2013028685

Collection Date: 22-Nov-13 10:00 AM

Site: BioReactor 2 Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

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 12/02/2013 11:45 DSBAKE1

2013028686

Collection Date: 22-Nov-13 10:00 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 12/09/2013 13:20 DJSULL1

2013028687

Collection Date: 11-Nov-13 1:45 PM

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 12/02/2013 13:00 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 1 ug/L 1 1 EPA 200.8 12/06/2013 13:10 DJSULL1

Cadmium (Cd) < 1 ug/L 1 1 EPA 200.8 12/06/2013 13:10 DJSULL1

Chromium (Cr) < 1 ug/L 1 1 EPA 200.8 12/06/2013 13:10 DJSULL1

Copper (Cu) < 1 ug/L 1 1 EPA 200.8 12/06/2013 13:10 DJSULL1

Nickel (Ni) < 1 ug/L 1 1 EPA 200.8 12/06/2013 13:10 DJSULL1

Selenium (Se) < 1 ug/L 1 1 EPA 200.8 12/06/2013 13:10 DJSULL1

Silver (Ag) < 1 ug/L 1 1 EPA 200.8 12/06/2013 13:10 DJSULL1

Zinc (Zn) < 1 ug/L 1 1 EPA 200.8 12/06/2013 13:10 DJSULL1

Page 7 of 17
 

December 11, 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 & DSI) (LIMS# J13110436) 

Mr. Perkins,

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

selenium speciation analysis on November 26, 2013. The samples were received in a sealed 

cooler at -0.1°C on November 27, 2013. Selenium speciation analysis was performed via ion 

chromatography inductively coupled plasma collision reaction cell mass spectrometry (IC-ICPCRC-MS). Mercury quantitation was performed via cold vapor inductively coupled plasma 

mass spectrometry (CV-ICP-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, 

Jeremy Maute 

Project Coordinator 

Applied Speciation and Consulting, LLC 

Page 8 of 17
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 & DSI) (LIMS# J13110436) 

December 11, 2013 

1. Sample Reception 

Three (3) aqueous samples were submitted for selenium speciation analysis on November 26, 

2013. Three (3) additional samples were submitted for total mercury quantitation. All 

samples were received in acceptable condition on November 27, 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 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. 

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). 

Page 9 of 17
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 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 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. 

Page 10 of 17
4. Analytical Issues 

The overall analyses went well and no significant analytical issues were encountered. With 

the exception 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% (61.0% and 62.4%, respectively). The spiking solution 

also contained selenite, and the spike recoveries for selenite were elevated (120.8% and 

121.2%, 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. 

The estimated method detection limits (eMDLs) for selenite, selenate, and selenocyanate are 

generated from replicate analyses of the lowest standard in the calibration curve. Not all 

selenium species are present in preparation blanks; therefore, eMDL calculations based on 

preparation blanks are artificially biased low. 

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

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

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

bias the results for other selenium species. 

The eMDL for mercury has been calculated using the standard deviation of the preparation 

blanks preserved and analyzed concurrently with the submitted samples. 

Upon validating the data, the project manager at Applied Speciation and Consulting observed 

that all selenium speciation results for the client sample identified as FGD Purge Eff (LIMS 

ID: 2013028681) were non-detects. This is atypical for selenium speciation results 

associated with this client sample for this project. The original sample containers were 

examined, and the FGD Purge Eff sample liquid was completely clear, lacking any 

suspended solid material. This too is atypical, as the aqueous FGD samples received 

routinely contain some dark, solid material suspended in solution. The container for the 

BioReactor 1 Inf (LIMS ID: 2013028683) did contain some dark, solid material suspended in 

solution similar to the characteristic appearance observed for FGD Purge Eff samples. 

The samples were logged in by sample reception staff according to the sample IDs provided 

on the sample containers. 

Page 11 of 17
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 17
Sample Results

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

Unknown Se 

Species (n)

FGD Purge Eff NR ND (< 7.2) ND (< 3.5) ND (< 2.9) ND (< 4.5) ND (< 4.5) 0 (0)

BioReactor 1 Inf 0.122 20.5 41.5 ND (< 0.73) ND (< 1.1) ND (< 1.1) 0 (0)

BioReactor 2 Inf 0.0228 NR NR NR NR NR NR

BioReactor 2 Eff 0.0065 29.9 32.6 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 & Selenium Speciation Results for Duke Energy

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

Contact: Jay Perkins

Date: December 11, 2013

LIMS #J13110436

Page 13 of 17
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 -0.0003 -0.0007 -0.0003 -0.0004 0.0002 0.0001 0.0006 - -

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 1655 105.5

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 & Selenium Speciation Results for Duke Energy

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

Contact: Jay Perkins

LIMS #J13110436

Date: December 11, 2013

Report Generated by: Jeremy Maute

Page 14 of 17
Quality Control Summary - Matrix Duplicates

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

Hg BioReactor 2 Eff 0.0065 0.0065 0.0065 0.0

Se(IV) BioReactor 2 Eff 29.9 30.7 30.3 2.6

Se(VI) BioReactor 2 Eff 32.64 32.07 32.36 1.8

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 BioReactor 2 Eff 2.000 2.138 106.6 2.000 2.222 110.8 3.9

Se(IV) BioReactor 2 Eff 1390 1709 120.8 1390 1715 121.2 0.4

Se(VI) BioReactor 2 Eff 1261 1230 95.0 1261 1231 95.0 0.1

SeCN BioReactor 2 Eff 1144 697.1 61.0* 1144 714.2 62.4* 2.4

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

Applied Speciation and Consulting, LLC

Total Mercury & Selenium Speciation Results for Duke Energy

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

Contact: Jay Perkins

LIMS #J13110436

Date: December 11, 2013

Report Generated by: Jeremy Maute

Page 15 of 17
Page 16 of 17
Page 17 of 17