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: J13110187

Project Name: WWTS FGD-Routine 2013

Lab Contact: Jason C Perkins

Date: 12/5/2013

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 17
Sample ID's & Descriptions:

Sample ID Plant/Station

Collection 

Date and Time Collected By Sample Description

2013027575 BELEWS 11-Nov-13 7:30 AM W.WORKMAN FGD Purge Eff 

2013027576 BELEWS 11-Nov-13 7:35 AM W.WORKMAN EQ Tank Eff 

2013027577 BELEWS 11-Nov-13 7:40 AM W.WORKMAN BioReactor 1 Inf 

2013027578 BELEWS 11-Nov-13 7:45 AM W.WORKMAN BioReactor 2 Inf 

2013027579 BELEWS 11-Nov-13 7:50 AM W.WORKMAN BioReactor 2 Eff 

2013027580 BELEWS 11-Nov-13 8:00 AM W.WORKMAN Filter Blk 

2013027581 BELEWS 31-Oct-13 2:10 PM D. Baker 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: 12/5/2013

Electronic Data Deliverable (EDD) Sent Separatel

Page 3 of 17
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13110187

2013027575

Collection Date: 11-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) 6.0 mg-N/L 0.25 25 EPA 353.2 11/15/2013 11:42 BGN9034

INORGANIC IONS BY IC

Bromide 200 mg/L 5 50 EPA 300.0 11/22/2013 17:02 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 278 ug/L 5 100 EPA 245.1 11/23/2013 10:34 DKJOHN2

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 229 mg/L 0.5 10 EPA 200.7 11/14/2013 10:01 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 792 ug/L 10 10 EPA 200.8 11/26/2013 14:02 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 372 ug/L 10 10 EPA 200.8 11/20/2013 12:03 DJSULL1

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 11/20/2013 12:03 DJSULL1

Chromium (Cr) 615 ug/L 10 10 EPA 200.8 11/20/2013 12:03 DJSULL1

Copper (Cu) 259 ug/L 10 10 EPA 200.8 11/20/2013 12:03 DJSULL1

Nickel (Ni) 382 ug/L 10 10 EPA 200.8 11/20/2013 12:03 DJSULL1

Selenium (Se) 4990 ug/L 20 20 EPA 200.8 11/20/2013 12:03 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 11/20/2013 12:03 DJSULL1

Zinc (Zn) 478 ug/L 10 10 EPA 200.8 11/20/2013 12:03 DJSULL1

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

Vendor Parameter Complete Vendor Method V_AS&C

2013027576

Collection Date: 11-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) 134 ug/L 2.5 50 EPA 245.1 11/23/2013 10:36 DKJOHN2

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 217 mg/L 0.5 10 EPA 200.7 11/14/2013 10:05 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 461 ug/L 10 10 EPA 200.8 11/26/2013 14:05 DJSULL1

Page 4 of 17
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13110187

2013027576

Collection Date: 11-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) 238 ug/L 10 10 EPA 200.8 11/20/2013 12:06 DJSULL1

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 11/20/2013 12:06 DJSULL1

Chromium (Cr) 368 ug/L 10 10 EPA 200.8 11/20/2013 12:06 DJSULL1

Copper (Cu) 156 ug/L 10 10 EPA 200.8 11/20/2013 12:06 DJSULL1

Nickel (Ni) 260 ug/L 10 10 EPA 200.8 11/20/2013 12:06 DJSULL1

Selenium (Se) 3390 ug/L 10 10 EPA 200.8 11/20/2013 12:06 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 11/20/2013 12:06 DJSULL1

Zinc (Zn) 303 ug/L 10 10 EPA 200.8 11/20/2013 12:06 DJSULL1

2013027577

Collection Date: 11-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 11/15/2013 11:43 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) 191 mg/L 0.5 10 EPA 200.7 11/14/2013 10:10 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 495 ug/L 10 10 EPA 200.8 11/26/2013 14:08 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 11/20/2013 12:10 DJSULL1

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 11/20/2013 12:10 DJSULL1

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 11/20/2013 12:10 DJSULL1

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 11/20/2013 12:10 DJSULL1

Nickel (Ni) 13.2 ug/L 10 10 EPA 200.8 11/20/2013 12:10 DJSULL1

Selenium (Se) 603 ug/L 10 10 EPA 200.8 11/20/2013 12:10 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 11/20/2013 12:10 DJSULL1

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 11/20/2013 12:10 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 # J13110187

2013027578

Collection Date: 11-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) 191 mg/L 0.5 10 EPA 200.7 11/14/2013 10:14 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 11/20/2013 12:13 DJSULL1

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 11/20/2013 12:13 DJSULL1

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 11/20/2013 12:13 DJSULL1

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 11/20/2013 12:13 DJSULL1

Nickel (Ni) < 10 ug/L 10 10 EPA 200.8 11/20/2013 12:13 DJSULL1

Selenium (Se) < 10 ug/L 10 10 EPA 200.8 11/20/2013 12:13 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 11/20/2013 12:13 DJSULL1

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 11/20/2013 12:13 DJSULL1

2013027579

Collection Date: 11-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 11/15/2013 11:45 BGN9034

INORGANIC IONS BY IC

Bromide 200 mg/L 5 50 EPA 300.0 11/22/2013 17:21 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) 187 mg/L 0.5 10 EPA 200.7 11/14/2013 10:18 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 5 ug/L 5 5 EPA 200.8 11/20/2013 12:16 DJSULL1

Cadmium (Cd) < 5 ug/L 5 5 EPA 200.8 11/20/2013 12:16 DJSULL1

Chromium (Cr) < 5 ug/L 5 5 EPA 200.8 11/20/2013 12:16 DJSULL1

Copper (Cu) < 5 ug/L 5 5 EPA 200.8 11/20/2013 12:16 DJSULL1

Nickel (Ni) < 5 ug/L 5 5 EPA 200.8 11/20/2013 12:16 DJSULL1

Selenium (Se) 5.12 ug/L 5 5 EPA 200.8 11/20/2013 12:16 DJSULL1

Silver (Ag) < 5 ug/L 5 5 EPA 200.8 11/20/2013 12:16 DJSULL1

Zinc (Zn) < 5 ug/L 5 5 EPA 200.8 11/20/2013 12:16 DJSULL1

Page 6 of 17
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13110187

2013027579

Collection Date: 11-Nov-13 7:50 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 14000 mg/L 25 1 SM2540C 11/19/2013 14:19 DSBAKE1

2013027580

Collection Date: 11-Nov-13 8:00 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 B2 1 1 EPA 200.8 11/26/2013 13:52 DJSULL1

2013027581

Collection Date: 31-Oct-13 2:10 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 11/14/2013 09:27 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 1 ug/L 1 1 EPA 200.8 11/20/2013 11:42 DJSULL1

Cadmium (Cd) < 1 ug/L 1 1 EPA 200.8 11/20/2013 11:42 DJSULL1

Chromium (Cr) < 1 ug/L 1 1 EPA 200.8 11/20/2013 11:42 DJSULL1

Copper (Cu) < 1 ug/L 1 1 EPA 200.8 11/20/2013 11:42 DJSULL1

Nickel (Ni) < 1 ug/L 1 1 EPA 200.8 11/20/2013 11:42 DJSULL1

Selenium (Se) < 1 ug/L 1 1 EPA 200.8 11/20/2013 11:42 DJSULL1

Silver (Ag) < 1 ug/L 1 1 EPA 200.8 11/20/2013 11:42 DJSULL1

Zinc (Zn) < 1 ug/L 1 1 EPA 200.8 11/20/2013 11:42 DJSULL1

Qualifiers:

B2 Target analyte was detected in blank(s) at a concentration greater than 1⁄2 the reporting limit but less than the 

reporting limit. Analyte concentration in sample is valid and may be used for compliance purposes.

Page 7 of 17
 

December 3, 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#J13110187) 

Mr. Perkins,

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

selenium speciation analysis on November 13, 2013. The samples were received in a sealed 

cooler at 0.1°C on November 14, 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# J13110187) 

December 3, 2013 

1. Sample Reception 

Four (4) aqueous samples were submitted for selenium speciation analysis on November 13, 

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

samples were received in acceptable condition on November 14, 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). 

Two 40 mL glass vials were received that listed a LIMS ID of 2013027570. Both bottles 

were labeled with a sample ID of BioReactor 2 Inf and both bottles listed a collection 

date/time of (11/8/13, 0955). These descriptive parameters match the BioReactor 2 Inf 

sample entry on the chain-of-custody (COC) form associated with LIMS ID J13110185. 

There was no way to discern between the two samples visibly. The COC form associated 

with LIMS ID J13110187 was also present in the cooler and the COC indicated that the client 

sample (requesting total mercury analysis) identified as (2013027578, BioReactor 2 Inf, 

11/11/13, 0745) should be present. A 40 mL glass container with the client sample 

BioReactor 2 Inf (LIMS ID 2013027578) was absent from the cooler. The two identically 

labeled samples requesting total mercury analysis were labeled internally by the laboratory 

sample reception staff at Applied Speciation as (2013027570-BioReactor 2 Inf A) and 

Page 9 of 17
(2013027570-BioReactor 2 Inf B). The samples were analyzed for total mercury yielding 

similar values, 0.0363 μg/L and 0.0296 μg/L, respectively. 

The client was informed of this sample ID issue. Since the total mercury results were similar 

in quantity, Applied Speciation was directed to report the total mercury result for 

(2013027570-BioReactor 2 Inf A) in the report associated with LIMS ID J13110185. 

Applied Speciation was instructed to report the total mercury result for (2013027570-

BioReactor 2 Inf B) in the report associated with LIMS ID J13110187.

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). 

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 

Page 10 of 17
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 November 19, 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 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. 

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 1280 30.5 13.3 4.5 ND (< 1.7) 3.4 (1)

BioReactor 1 Inf 0.0765 489 19.6 ND (< 0.53) 6.40 ND (< 0.43) 1.20 (1)

BioReactor 2 Inf 0.0296 NR NR NR NR NR NR

BioReactor 2 Eff 0.0054 ND (< 0.47) ND (< 0.30) 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 & Selenium Speciation Results for Duke Energy

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

Contact: Jay Perkins

Date: December 3, 2013

LIMS #J13110187

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 -0.0002 -0.0007 -0.0004 -0.0004 0.0002 0.0001 0.0006 - -

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

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 & Selenium Speciation Results for Duke Energy

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

Contact: Jay Perkins

LIMS #J13110187

Date: December 3, 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 Batch QC 0.1934 0.1955 0.1945 1.1

Se(IV) Batch QC ND (< 0.47) ND (< 0.47) NC NC

Se(VI) Batch QC ND (< 0.30) ND (< 0.30) NC NC

SeCN Batch QC ND (< 0.53) ND (< 0.53) NC NC

MeSe(IV) Batch QC ND (< 0.43) ND (< 0.43) NC NC

SeMe Batch QC 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

Se(IV) Batch QC 1390 1336 96.1 1390 1344 96.7 0.6

Se(VI) Batch QC 1261 1176 93.3 1261 1190 94.3 1.1

SeCN Batch QC 1144 1026 89.7 1144 1043 91.2 1.7

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 #J13110187

Date: December 3, 2013

Report Generated by: Jeremy Maute

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