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: J 13110456 Project Name: W WTS FGD-Routine 2013

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

### Sample ID's & Descriptions:

Sample ID Plant/Station Collection Date and Time Collected By Sample Description 2013028761 BELEWS 26-Nov-13 11:30 AM Tim Owens FGD Purge Eff 2013028762 BELEWS 26-Nov-13 11:35 AM Tim Owens EQ Tank Eff 2013028763 BELEWS 26-Nov-13 11:40 AM Tim Owens BioReactor 1 Inf 2013028764 BELEWS 26-Nov-13 11:45 AM Tim Owens BioReactor 2 Inf 2013028765 BELEWS 26-Nov-13 11:50 AM Tim Owens BioReactor 2 Eff 2013028766 BELEWS 26-Nov-13 12:00 PM Tim Owens Filter Blk 2013028767 BELEWS 22-Nov-13 TRIP BLANK 7 Total SamplesCOC 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

## Certificate of Laboratory Analysis This report shall not be reproduced, except in full.



### Order # J13110456

2013028761 Collection Date: 26-Nov-13 11:30 AM Site: FGD Purge Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sample #:

Analyst DF NITRITE + NITRATE (COLORIMETRIC) Nitrite + Nitrate (Colorimetric) 4.1 mg-N/L EPA 353.2 12/05/2013 13:58 TLINN 0.25 25
INORGANIC IONS BY IC Bromide 110 mg/L EPA 300.0 12/02/2013 22:57 JAHERMA 5 50 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 21.0 ug/L EPA 245.1 12/06/2013 12:22 DKJOHN2 5 100
TOTAL RECOVERABLE METALS BY ICP Boron (B) 198 mg/L EPA 200.7 12/04/2013 10:51 MHH7131 0.5 10
DISSOLVED METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 12/10/2013 13:37 DJSULL1 10 10 Selenium (Se) 143 ug/L EPA 200.8 12/10/2013 13:37 DJSULL1 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 40.0 ug/L EPA 200.8 12/09/2013 11:42 DJSULL1 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 12/09/2013 11:42 DJSULL1 10 10 Chromium (Cr) 46.3 ug/L EPA 200.8 12/09/2013 11:42 DJSULL1 10 10 Copper (Cu) 26.0 ug/L EPA 200.8 12/09/2013 11:42 DJSULL1 10 10 Nickel (Ni) 154 ug/L EPA 200.8 12/09/2013 11:42 DJSULL1 10 10 Selenium (Se) 511 ug/L EPA 200.8 12/09/2013 11:42 DJSULL1 10 10 Silver (Ag) < 10 ug/L EPA 200.8 12/09/2013 11:42 DJSULL1 10 10 Zinc (Zn) 89.2 ug/L EPA 200.8 12/09/2013 11:42 DJSULL1 10 10 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C

2013028762 Collection Date: 26-Nov-13 11:35 AM Site: EQ Tank Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sample #:

Analyst DF MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 22.4 ug/L EPA 245.1 12/06/2013 12:34 DKJOHN2 2.5 50
TOTAL RECOVERABLE METALS BY ICP Boron (B) 198 mg/L EPA 200.7 12/04/2013 10:56 MHH7131 0.5 10
DISSOLVED METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 12/10/2013 13:40 DJSULL1 10 10 Selenium (Se) 88.3 ug/L EPA 200.8 12/10/2013 13:40 DJSULL1 10 10

## Certificate of Laboratory Analysis This report shall not be reproduced, except in full.



### Order # J13110456

2013028762 Collection Date: 26-Nov-13 11:35 AM Site: EQ Tank Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sample #:

Analyst DF
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 46.1 ug/L EPA 200.8 12/09/2013 11:45 DJSULL1 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 12/09/2013 11:45 DJSULL1 10 10 Chromium (Cr) 57.1 ug/L EPA 200.8 12/09/2013 11:45 DJSULL1 10 10 Copper (Cu) 31.8 ug/L EPA 200.8 12/09/2013 11:45 DJSULL1 10 10 Nickel (Ni) 143 ug/L EPA 200.8 12/09/2013 11:45 DJSULL1 10 10 Selenium (Se) 538 ug/L EPA 200.8 12/09/2013 11:45 DJSULL1 10 10 Silver (Ag) < 10 ug/L EPA 200.8 12/09/2013 11:45 DJSULL1 10 10 Zinc (Zn) 83.9 ug/L EPA 200.8 12/09/2013 11:45 DJSULL1 10 10

2013028763 Collection Date: 26-Nov-13 11:40 AM Site: BioReactor 1 Inf Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sample #:

Analyst DF NITRITE + NITRATE (COLORIMETRIC) Nitrite + Nitrate (Colorimetric) 7.9 mg-N/L EPA 353.2 12/05/2013 13:59 TLINN 0.25 25 Mercury by EPA 200.8 - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete ug/l Vendor Method V_AS&C
TOTAL RECOVERABLE METALS BY ICP Boron (B) 194 mg/L EPA 200.7 12/04/2013 11:00 MHH7131 0.5 10
DISSOLVED METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 12/10/2013 13:44 DJSULL1 10 10 Selenium (Se) 68.8 ug/L EPA 200.8 12/10/2013 13:44 DJSULL1 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 12/09/2013 11:48 DJSULL1 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 12/09/2013 11:48 DJSULL1 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 12/09/2013 11:48 DJSULL1 10 10 Copper (Cu) < 10 ug/L EPA 200.8 12/09/2013 11:48 DJSULL1 10 10 Nickel (Ni) 20.9 ug/L EPA 200.8 12/09/2013 11:48 DJSULL1 10 10 Selenium (Se) 70.9 ug/L EPA 200.8 12/09/2013 11:48 DJSULL1 10 10 Silver (Ag) < 10 ug/L EPA 200.8 12/09/2013 11:48 DJSULL1 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 12/09/2013 11:48 DJSULL1 10 10 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C

## Certificate of Laboratory Analysis This report shall not be reproduced, except in full.



### Order # J13110456

2013028764 Collection Date: 26-Nov-13 11:45 AM Site: BioReactor 2 Inf Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sample #:

Analyst DF 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) 202 mg/L EPA 200.7 12/04/2013 11:04 MHH7131 0.5 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 12/09/2013 11:52 DJSULL1 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 12/09/2013 11:52 DJSULL1 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 12/09/2013 11:52 DJSULL1 10 10 Copper (Cu) < 10 ug/L EPA 200.8 12/09/2013 11:52 DJSULL1 10 10 Nickel (Ni) < 10 ug/L EPA 200.8 12/09/2013 11:52 DJSULL1 10 10 Selenium (Se) 15.2 ug/L EPA 200.8 12/09/2013 11:52 DJSULL1 10 10 Silver (Ag) < 10 ug/L EPA 200.8 12/09/2013 11:52 DJSULL1 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 12/09/2013 11:52 DJSULL1 10 10

2013028766 Collection Date: 26-Nov-13 12:00 PM Site: Filter Blk Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sample #:

Analyst DF
DISSOLVED METALS BY ICP-MS Selenium (Se) < 1 ug/L EPA 200.8 12/10/2013 13:23 DJSULL1 1 1

2013028767 Collection Date: 22-Nov-13 Site: TRIP BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sample #:

Analyst DF
TOTAL RECOVERABLE METALS BY ICP Boron (B) < 0.05 mg/L EPA 200.7 12/04/2013 10:43 MHH7131 0.05 1
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 1 ug/L EPA 200.8 12/09/2013 12:33 DJSULL1 1 1 Cadmium (Cd) < 1 ug/L EPA 200.8 12/09/2013 12:33 DJSULL1 1 1 Chromium (Cr) < 1 ug/L EPA 200.8 12/09/2013 12:33 DJSULL1 1 1 Copper (Cu) 5.51 ug/L EPA 200.8 12/09/2013 12:33 DJSULL1 1 1 Nickel (Ni) < 1 ug/L EPA 200.8 12/09/2013 12:33 DJSULL1 1 1 Selenium (Se) < 1 ug/L EPA 200.8 12/09/2013 12:33 DJSULL1 1 1 Silver (Ag) < 1 ug/L EPA 200.8 12/09/2013 12:33 DJSULL1 1 1 Zinc (Zn) < 1 ug/L EPA 200.8 12/09/2013 12:33 DJSULL1 1 1

### December 1 7 , 2013

Jay Perkins Duke Energy Analytical Laboratory Mail Code MGO3A2 (Building 7405) 13339 Hagers Ferry Rd. Huntersville, NC 28078 (704) 875-5 245 Project: Belews - FGD WWTS (Bi-Monthly & Flex Fuel) (LIMS# J13110456)

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

### 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# J13110456)
December 1 7 , 2013

1. Sample Reception Three (3 ) aq ueous 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 co ntainer 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 req uiring selenium speciation evaluation was filtered (0.45μm) and each filtrate w as 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 ≤6 o 

### C) 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.

### 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 wereanalyzed 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 standard s 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 Eachsample for selenium speciation analysis w as 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)

### 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.

### 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, LLCSample Results

Sample ID Total Hg Se(IV) Se(VI) SeCN MeSe(IV) SeMe Unknown Se Species (n) FGD Purge Eff NR 88.4 44.9 ND (< 3.5) 5.2 ND (< 3.0) 0 (0) BioReactor 1 Inf 0.217 22.3 35.5 ND (< 0.86) 1.11 ND (< 0.76) 0 (0) BioReactor 2 Inf 0.0330 NR NR NR NR NR NR BioReactor 2 Eff 0.0047 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 #J13110456Sample Results

Sample ID As(III) As(V) MMAs DMAs Unknown As Species FGD Purge Eff 0.34 1.96 ND (< 0.11) 0.165 0.46 BioReactor 1 Inf ND (< 0.18) 0.68 ND (< 0.11) ND (< 0.033) 0.45 BioReactor 2 Inf NR NR NR NR NR BioReactor 2 Eff ND (< 0.18) 0.53 ND (< 0.11) 0.274 0.24 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 #J13110456
Date: December 17, 2013 Report Generated by: Jeremy MauteQuality 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 0.00 0.00 0.00 0.00 0.00 0.00 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 #J13110456
Date: December 17, 2013 Report Generated by: Jeremy MauteQuality 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 #J13110456
Date: December 17, 2013Quality 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) BioReactor 1 Inf 22.29 20.68 21.49 7.5 Se(VI) BioReactor 1 Inf 35.54 36.30 35.92 2.1 SeCN BioReactor 1 Inf ND (< 0.86) ND (< 0.86) NC NC MeSe(IV) BioReactor 1 Inf 1.11 0.95 1.03 16.3 SeMe BioReactor 1 Inf ND (< 0.76) ND (< 0.76) NC NC As(III) BioReactor 2 Eff ND (< 0.18) ND (< 0.18) NC NC As(V) BioReactor 2 Eff 0.53 0.48 0.50 10.5 MMAs BioReactor 2 Eff ND (< 0.11) ND (< 0.11) NC NC DMAs BioReactor 2 Eff 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 ten times the eMDL. Difference was less than ten times the eMDL. LIMS #J13110456
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 PerkinsQuality 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) BioReactor 1 Inf 1390 2218 158.1* 1390 2205 157.1* 0.6 Se(VI) BioReactor 1 Inf 1261 1363 105.2 1261 1372 106.0 0.7 SeCN BioReactor 1 Inf 1144 513.2 44.9* 1144 525.7 46.0* 2.4 As(III) BioReactor 2 Eff 50.00 48.08 96.2 50.00 47.08 94.2 2.1 As(V) BioReactor 2 Eff 50.00 51.06 101.1 50.00 49.59 98.2 2.9 DMAs BioReactor 2 Eff 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 #J13110456
Date: December 17, 2013 Report Generated by: Jeremy Maute