### 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 13110158 Project Name:

L ab Contact: Jason C Perkins


### Date: 12/3/2013 Customer Address: 3195 Pine Hall Rd Customer Name(s): Bill Kennedy, Wayne Chapman

Mailcode: Belews Steam Station Belews Creek, NC 28012

Phone: 980-875-5348 Report Authorized By: (Signature)


### Program Comments: Please contact the Program Manager (Jason C Perkins) with any questions regarding this report. Data Flags & Calculations: Any analytical tests or individual analytes within a test flagged with a Qualifier indicate a deviation from the method quality system or quality control requirement. The qualifier description is found at the end of the Certificate of Analysis (sample results) under the qualifiers heading. All results are reported on a dry weight basis unless otherwise noted. Subcontracted data included on the Duke Certificate of Analysis is to be used as information only. Certified vendor results can be found in the subcontracted lab final report. Duke Energy Analytical Laboratory subcontracts analyses to other vendor laboratories that have been qualified by Duke Energy to perform these analyses except where noted. Data Package: This data package includes analytical results that are applicable only to the samples described in this narrative. An estimation of the uncertainty of measurement for the results in the report is available upon request. This report shall not be reproduced, except in full, without the written consent of the Analytical Laboratory. Please contact the Analytical laboratory with any questions. The order of individual sections within this report is as follows: Job Summary Report, Sample Identification, Technical Validation of Data Package, Analytical Laboratory Certificate of Analysis, Analytical Laboratory QC Reports, Sub-contracted Laboratory Results, Customer Specific Data Sheets, Reports & Documentation, Customer Database Entries, Test Case Narratives, Chain of Custody (COC)
Certification: The Analytical Laboratory holds the following State Certifications : North Carolina (DENR) Certificate #248, South Carolina (DHEC) Laboratory ID # 99005. Contact the Analytical Laboratory for definitive information about the certification status of specific methods. Jason C Perkins

# Sample ID's & Descriptions:

Sample ID Plant/Station Collection Date and Time Collected By Sample Description 2013027419 BELEWS 06-Nov-13 8:05 AM TO FGD Purge Eff 2013027420 BELEWS 06-Nov-13 8:10 AM TO EQ Tank Eff 2013027421 BELEWS 06-Nov-13 8:15 AM TO BIOREACTOR 1 INF 2013027422 BELEWS 06-Nov-13 8:17 AM TO BioReactor 2 Inf 2013027423 BELEWS 06-Nov-13 8:17 AM TO BioReactor 2 Eff 2013027424 BELEWS 06-Nov-13 2:15 PM RG Bio Pilot Eff 2013027425 BELEWS FILTER BLANK 2013027426 BELEWS 28-Oct-13 4:35 PM DB METALS TRIP BLANK 8 Total Samples

### 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: 

### 12/3/2013 Electronic Data Deliverable (EDD) Sent Separatel

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



## Order # J13110158

2013027419 Collection Date: 06-Nov-13 8:05 AM 

### Site: FGD Purge Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF INORGANIC IONS BY IC Bromide 99 mg/L EPA 300.0 11/11/2013 15:23 JAHERMA 5 50 Chloride 7000 mg/L EPA 300.0 11/11/2013 15:23 JAHERMA 100 1000 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 219 ug/L EPA 245.1 11/23/2013 10:13 DKJOHN2 5 100
TOTAL RECOVERABLE METALS BY ICP Boron (B) 210 mg/L EPA 200.7 11/13/2013 12:22 MHH7131 0.5 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 147 ug/L EPA 200.8 11/20/2013 14:02 DJSULL1 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 172 ug/L EPA 200.8 11/18/2013 14:49 DJSULL1 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 11/18/2013 14:49 DJSULL1 10 10 Chromium (Cr) 311 ug/L EPA 200.8 11/18/2013 14:49 DJSULL1 10 10 Copper (Cu) 127 ug/L EPA 200.8 11/18/2013 14:49 DJSULL1 10 10 Nickel (Ni) 243 ug/L EPA 200.8 11/18/2013 14:49 DJSULL1 10 10 Selenium (Se) 4080 ug/L EPA 200.8 11/18/2013 14:49 DJSULL1 10 10 Silver (Ag) < 10 ug/L EPA 200.8 11/18/2013 14:49 DJSULL1 10 10 Thallium (Tl) < 10 ug/L EPA 200.8 11/18/2013 14:49 DJSULL1 10 10 Vanadium (V) 192 ug/L EPA 200.8 11/18/2013 14:49 DJSULL1 10 10 Zinc (Zn) 246 ug/L EPA 200.8 11/18/2013 14:49 DJSULL1 10 10 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C
TOTAL DISSOLVED SOLIDS TDS 19000 mg/L SM2540C 11/19/2013 14:19 DSBAKE1 250 1
TOTAL SUSPENDED SOLIDS TSS 3200 mg/L SM2540D 11/12/2013 12:27 DSBAKE1 250 1



### 2013027420 Collection Date: 06-Nov-13 8:10 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) 152 ug/L EPA 245.1 11/23/2013 10:15 DKJOHN2 2.5 50
TOTAL RECOVERABLE METALS BY ICP Boron (B) 194 mg/L EPA 200.7 11/13/2013 12:26 MHH7131 0.5 10

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



## Order # J13110158

2013027420 Collection Date: 06-Nov-13 8:10 AM 

### Site: EQ Tank Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF DISSOLVED METALS BY ICP-MS Selenium (Se) 122 ug/L EPA 200.8 11/20/2013 14:05 DJSULL1 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 145 ug/L EPA 200.8 11/18/2013 14:53 DJSULL1 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 11/18/2013 14:53 DJSULL1 10 10 Chromium (Cr) 264 ug/L EPA 200.8 11/18/2013 14:53 DJSULL1 10 10 Copper (Cu) 105 ug/L EPA 200.8 11/18/2013 14:53 DJSULL1 10 10 Nickel (Ni) 202 ug/L EPA 200.8 11/18/2013 14:53 DJSULL1 10 10 Selenium (Se) 3300 ug/L EPA 200.8 11/18/2013 14:53 DJSULL1 10 10 Silver (Ag) < 10 ug/L EPA 200.8 11/18/2013 14:53 DJSULL1 10 10 Thallium (Tl) < 10 ug/L EPA 200.8 11/18/2013 14:53 DJSULL1 10 10 Vanadium (V) 177 ug/L EPA 200.8 11/18/2013 14:53 DJSULL1 10 10 Zinc (Zn) 197 ug/L EPA 200.8 11/18/2013 14:53 DJSULL1 10 10



### 2013027421 Collection Date: 06-Nov-13 8:15 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) < 0.01 mg-N/L EPA 353.2 11/15/2013 11:37 BGN9034 0.01 1
INORGANIC IONS BY IC Bromide 86 mg/L EPA 300.0 11/11/2013 15:42 JAHERMA 5 50 Chloride 6400 mg/L EPA 300.0 11/11/2013 15:42 JAHERMA 100 1000 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) 183 mg/L EPA 200.7 11/13/2013 12:30 MHH7131 0.5 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 88.1 ug/L EPA 200.8 11/20/2013 14:09 DJSULL1 10 10

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



## Order # J13110158

2013027421 Collection Date: 06-Nov-13 8:15 AM 

### Site: BIOREACTOR 1 INF Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 11/18/2013 14:56 DJSULL1 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 11/18/2013 14:56 DJSULL1 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 11/18/2013 14:56 DJSULL1 10 10 Copper (Cu) < 10 ug/L EPA 200.8 11/18/2013 14:56 DJSULL1 10 10 Nickel (Ni) 24.6 ug/L EPA 200.8 11/18/2013 14:56 DJSULL1 10 10 Selenium (Se) 76.8 ug/L EPA 200.8 11/18/2013 14:56 DJSULL1 10 10 Silver (Ag) < 10 ug/L EPA 200.8 11/18/2013 14:56 DJSULL1 10 10 Thallium (Tl) < 10 ug/L EPA 200.8 11/18/2013 14:56 DJSULL1 10 10 Vanadium (V) < 10 ug/L EPA 200.8 11/18/2013 14:56 DJSULL1 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 11/18/2013 14:56 DJSULL1 10 10 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 SM2540C 11/19/2013 14:19 DSBAKE1 25 1
TOTAL SUSPENDED SOLIDS TSS < 5 mg/L SM2540D 11/12/2013 12:27 DSBAKE1 5 1



### 2013027422 Collection Date: 06-Nov-13 8:17 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) 187 mg/L EPA 200.7 11/13/2013 12:34 MHH7131 0.5 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 11/18/2013 15:00 DJSULL1 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 11/18/2013 15:00 DJSULL1 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 11/18/2013 15:00 DJSULL1 10 10 Copper (Cu) < 10 ug/L EPA 200.8 11/18/2013 15:00 DJSULL1 10 10 Nickel (Ni) < 10 ug/L EPA 200.8 11/18/2013 15:00 DJSULL1 10 10 Selenium (Se) < 10 ug/L EPA 200.8 11/18/2013 15:00 DJSULL1 10 10 Silver (Ag) < 10 ug/L EPA 200.8 11/18/2013 15:00 DJSULL1 10 10 Thallium (Tl) < 10 ug/L EPA 200.8 11/18/2013 15:00 DJSULL1 10 10 Vanadium (V) < 10 ug/L EPA 200.8 11/18/2013 15:00 DJSULL1 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 11/18/2013 15:00 DJSULL1 10 10

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



## Order # J13110158

2013027422 Collection Date: 06-Nov-13 8:17 AM 

### Site: BioReactor 2 Inf Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF


### 2013027423 Collection Date: 06-Nov-13 8:17 AM 

### Site: BioReactor 2 Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF NITRITE + NITRATE (COLORIMETRIC) Nitrite + Nitrate (Colorimetric) < 0.01 mg-N/L EPA 353.2 11/15/2013 11:34 BGN9034 0.01 1
INORGANIC IONS BY IC Bromide 86 mg/L EPA 300.0 11/11/2013 16:01 JAHERMA 5 50 Chloride 6300 mg/L EPA 300.0 11/11/2013 16:01 JAHERMA 100 1000 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 11/13/2013 12:38 MHH7131 0.5 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 5 ug/L EPA 200.8 11/18/2013 15:13 DJSULL1 5 5 Cadmium (Cd) < 5 ug/L EPA 200.8 11/18/2013 15:13 DJSULL1 5 5 Chromium (Cr) < 5 ug/L EPA 200.8 11/18/2013 15:13 DJSULL1 5 5 Copper (Cu) < 5 ug/L EPA 200.8 11/18/2013 15:13 DJSULL1 5 5 Nickel (Ni) < 5 ug/L EPA 200.8 11/18/2013 15:13 DJSULL1 5 5 Selenium (Se) < 5 ug/L EPA 200.8 11/18/2013 15:13 DJSULL1 5 5 Silver (Ag) < 5 ug/L EPA 200.8 11/18/2013 15:13 DJSULL1 5 5 Thallium (Tl) < 5 ug/L EPA 200.8 11/18/2013 15:13 DJSULL1 5 5 Vanadium (V) < 5 ug/L EPA 200.8 11/18/2013 15:13 DJSULL1 5 5 Zinc (Zn) < 5 ug/L EPA 200.8 11/18/2013 15:13 DJSULL1 5 5 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C



### 2013027424 Collection Date: 06-Nov-13 2:15 PM 

### Site: Bio Pilot Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF NITRITE + NITRATE (COLORIMETRIC) Nitrite + Nitrate (Colorimetric) < 0.01 mg-N/L EPA 353.2 11/15/2013 11:29 BGN9034 0.01 1 Mercury by EPA 200.8 - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete ug/l Vendor Method V_AS&C

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



## Order # J13110158

2013027424 Collection Date: 06-Nov-13 2:15 PM 

### Site: Bio Pilot Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF TOTAL RECOVERABLE METALS BY ICP Boron (B) 186 mg/L EPA 200.7 11/13/2013 12:42 MHH7131 0.5 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 72.7 ug/L EPA 200.8 11/20/2013 14:12 DJSULL1 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 11/18/2013 15:16 DJSULL1 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 11/18/2013 15:16 DJSULL1 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 11/18/2013 15:16 DJSULL1 10 10 Copper (Cu) < 10 ug/L EPA 200.8 11/18/2013 15:16 DJSULL1 10 10 Nickel (Ni) 19.0 ug/L EPA 200.8 11/18/2013 15:16 DJSULL1 10 10 Selenium (Se) 63.5 ug/L EPA 200.8 11/18/2013 15:16 DJSULL1 10 10 Silver (Ag) < 10 ug/L EPA 200.8 11/18/2013 15:16 DJSULL1 10 10 Thallium (Tl) < 10 ug/L EPA 200.8 11/18/2013 15:16 DJSULL1 10 10 Vanadium (V) < 10 ug/L EPA 200.8 11/18/2013 15:16 DJSULL1 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 11/18/2013 15:16 DJSULL1 10 10 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C



### 2013027425 Collection Date: 

### Site: FILTER BLANK 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 11/20/2013 13:26 DJSULL1 1 1



### 2013027426 Collection Date: 28-Oct-13 4:35 PM 

### Site: METALS 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 11/13/2013 11:41 MHH7131 0.05 1

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



## Order # J13110158

2013027426 Collection Date: 28-Oct-13 4:35 PM 

### Site: METALS TRIP BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 1 ug/L EPA 200.8 11/18/2013 14:09 DJSULL1 1 1 Cadmium (Cd) < 1 ug/L EPA 200.8 11/18/2013 14:09 DJSULL1 1 1 Chromium (Cr) < 1 ug/L EPA 200.8 11/18/2013 14:09 DJSULL1 1 1 Copper (Cu) < 1 ug/L EPA 200.8 11/18/2013 14:09 DJSULL1 1 1 Nickel (Ni) < 1 ug/L EPA 200.8 11/18/2013 14:09 DJSULL1 1 1 Selenium (Se) < 1 ug/L EPA 200.8 11/18/2013 14:09 DJSULL1 1 1 Silver (Ag) < 1 ug/L EPA 200.8 11/18/2013 14:09 DJSULL1 1 1 Thallium (Tl) < 1 ug/L EPA 200.8 11/18/2013 14:09 DJSULL1 1 1 Vanadium (V) < 1 ug/L EPA 200.8 11/18/2013 14:09 DJSULL1 1 1 Zinc (Zn) < 1 ug/L EPA 200.8 11/18/2013 14:09 DJSULL1 1 1

# November 2 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: Fontier Pilot (Belews Creek) WWTS (Weekly Sampling) (LIMS#J13110158)

Mr. Perkins, Attached is the report associated with five (5 ) aqueous samples submitted for total mercury , hexavalent chromium, and selenium speciation analyses on November 11 , 2013. The samples were received in a sealed cooler at -0.2° C on November 12 , 2013

. Mercury quantitation was performed via cold vapor inductively coupled plasma mass spectrometry (CV-ICP-MS). Hexavalent chromium analysis was performed via ion chromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICP-D RC -MS). Selenium speciation analysis was performed via ion chromatography inductively coupled plasma collision reaction cell mass spectrometry (IC-ICP- CRC -MS). Any issues associated with the analyses are addressed in the following report. If you have any questions, please feel free to contact me at your convenience.

Sincerely,

Jeremy Maute Project Coordinator Applied Speciation and Consulting, LLC

# 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: Fontier Pilot (Belews Creek) WWTS (Weekly Sampling) (LIMS# J13110158) November 2 7 , 2013

1. Sample Reception Four (4 ) aqueous samples were submitted for hexavalent chromium and selenium speciation analyses on November 11 , 2013. Four (4 ) additional samples were submitted for total mercury quantitation. All samples were received in acceptable condition on November 12 , 2013 in a sealed co ntainer at -0.2° C. All samples were received in a laminar flow clean hood, void of trace metals contamination and ultra-violet radiation, and were designated discrete sample identifiers. The 40mL borosilicate glass vials submitted for total mercury were preserved with bromine monochloride (BrCl) solution. The resulting samples were stored in a secure polyethylene container, known to be free from trace metals contamination, until the analyses could be performed. An aliquot of each sample submitted for hexavalent chromium analysis was filtered (0.45um) and stored in a secure refrigerator maintained at a temperature of 4 o

# C, 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. SamplePreparation 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). Hexavalent Chromium Analysis by IC-ICP-DRC-MS Prior to analysis, all samples were injected directly into autosampler vials. No further sample preparation was performed as any chemical alteration of the samples may shift the equilibrium of the system resulting in changes in speciation ratios. Selenium Speciation Analysis by IC-ICP-CRC-MS Prior to analysis, an aliquot of each sample was filtered with a syringe filter (0.45μm) and injected directly into a sealed autosampler vial. No further sample preparation was performed as any chemical alteration of a sample may shift the equilibrium of the system, resulting in changes in speciation ratios.

3. Sample Analysis All sample analysis is preceded by a minimum of a five-point calibration curve spanning the entire concentration range of interest. Calibration curves are performed at the beginning of each analytical day. All calibration curves, associated with each species of interest, are standardized by linear regression resulting in a response factor. All sample results are instrument blank correctedto 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 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 formed is then swept by a stream of argon gas into a radio frequency (RF) plasma where energy-transfer processes cause desolvation, atomization, and ionization. The ions are extracted from the plasma through a differentially-pumped vacuum interface and separated on the basis of their mass- to -charge ratio (m/z) by a mass spectrometer. A solid-state detector detects ions transmitted through the mass analyzer and the resulting current is processed by a data handling system. Hexavalent Chromium Analysis by IC-ICP-DRC

-MS Each sample for hexavalent chromium analysis was analyzed by ion chromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICP-DRC-MS) on November 26 , 2013. An aliquot of each sample is injected onto an anion exchange column and mobilized by a basic (pH > 7)

# gradient. The eluting chromium species are then introduced into a radio frequency (RF)

plasma where energy-transfer processes cause desolvation, atomization, and ionization. The ions are extracted from the plasma through a differentially-pumped vacuum interface and travel through a pressurized chamber (DRC) containing a reaction gas which preferentially reacts with interfering ions of the same target mass to charge ratios (m/z). A solid-state detector detects ions transmitted through the mass analyzer and the resulting current is processed by a data handling system. Retention times for each eluting species are compared to known standards for species identification. Selenium Speciation Analysis by IC-ICP-CRC-MS Eachsample for selenium speciation analysis w asanalyzed by ion chromatography inductively coupled plasma collision reaction cell mass spectrometry (IC-ICP- CRC -MS) on November 15, 2013. An aliquot of each sample isinjected onto an anion exchange column and mobilized by a basic (pH > 7) gradient. The eluting selenium species are then introduced into a radio frequency (RF) plasma where energy-transfer processes cause desolvation, atomization, and ionization. The ions are extracted from the plasma through a differentially-pumped vacuum interface and travel through a pressurized chamber ( CRC ) containing a reaction gas which preferentially reacts with interfering ions of the same target mass to charge ratios (m/z). A solid-state detector detects ions transmitted through the mass analyzer and the resulting current is processed by a data handling system. Retention times for each eluting species are compared to known standards for species identification.

4. Analytical Issues The overall analyses went well and no significant analytical issues were encountered. All quality control parameters associated with these samples were within acceptance limits. The estimated method detection limits (eMDLs) for selenite, selenate, and selenocyanate are generated from replicate analyses of the lowest standard in the calibration curve. Not all selenium species are present in preparation blanks; therefore, eMDL calculations based on preparation blanks are artificially biased low. The eMDL values for methylseleninic acid and selenomethionine are calculated from the average eMDL of selenite, selenate, and selenocyanate. The calibration does not contain methylseleninic acid or selenomethionine due to impurities in these standards which would bias the results for other selenium species. The eMDL values for hexavalent chromium and mercury are calculated using the standard deviation of the preparation blanks preserved and analyzed concurrently with the submitted samples.

# 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

### Sample Results

Sample ID Total Hg Cr(VI) Se(IV) Se(VI) SeCN MeSe(IV) SeMe Unknown Se Species (n) FGD Purge Eff NR 1.8 74.0 50.5 ND (< 2.1) 3.1 ND (< 1.7) 0 (0) BioReactor 1 Inf 0.232 ND (< 1.0) 18.5 35.9 ND (< 0.53) 0.65 ND (< 0.43) 2.64 (1) BioReactor 2 Inf 0.0345 NR NR NR NR NR NR NR BioReactor 2 Eff 0.0076 1.6 ND (< 0.47) ND (< 0.30) ND (< 0.53) ND (< 0.43) ND (< 0.43) 0 (0) Bio Pilot Eff 0.0725 ND (< 1.0) 17.3 36.3 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, Hexavalent Chromium, and Selenium Speciation Results for Duke Energy

Project Name: Fontier Pilot (Belews Creek) WWTS (Weekly Sampling) Contact: Jay Perkins

Date: November 27, 2013 LIMS #J13110158

### 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

- - Cr(VI) -0.8 -0.4 -0.2 0.0 -0.3 0.3 0.002

- - 1.0 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 Cr(VI) LCS 1.000 1.054 105.4 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, Hexavalent Chromium, and Selenium Speciation Results for Duke Energy

Project Name: Fontier Pilot (Belews Creek) WWTS (Weekly Sampling) Contact: Jay Perkins LIMS #J13110158 Date: November 27, 2013 Report Generated by: Jeremy Maute

### 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 Cr(VI) Bio Pilot Eff ND (< 1.0) ND (< 1.0) NC NC Se(IV) Bio Pilot Eff 17.33 18.07 17.70 4.2 Se(VI) Bio Pilot Eff 36.27 38.29 37.28 5.4 SeCN Bio Pilot Eff ND (< 0.53) ND (< 0.53) NC NC MeSe(IV) Bio Pilot Eff ND (< 0.43) ND (< 0.43) NC NC SeMe Bio Pilot Eff 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 Cr(VI) Bio Pilot Eff 1000 986.4 98.6 1000 986.9 98.7 0.0 Se(IV) Bio Pilot Eff 1390 1312 93.1 1390 1344 95.4 2.4 Se(VI) Bio Pilot Eff 1261 1203 92.4 1261 1224 94.1 1.7 SeCN Bio Pilot Eff 1144 1037 90.6 1144 1056 92.3 1.8 Applied Speciation and Consulting, LLC Total Mercury, Hexavalent Chromium, and Selenium Speciation Results for Duke Energy

Project Name: Fontier Pilot (Belews Creek) WWTS (Weekly Sampling) Contact: Jay Perkins LIMS #J13110158 Date: November 27, 2013 Report Generated by: Jeremy Maute