### 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: J12050473 Project Name: N/A

Lab Contact: Jason C Perkins 

### Date: 6/11/2012 Customer Address: 3195 Pine Hall Rd Customer Name(s): Bill Kennedy, Meloni e Martin, Wayne Chapman, Tom Johnson

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 Cert ificate of Analysis (sample re sults) under the qualifiers heading. All results are repo rted on a dry weight basis unless otherwise noted. Data Package: This data package includes analytical results that are applicable only to the samples described in this narrative. An estimatio n of the uncertainty of measurement for the results in the report is available upon request. This report shall not be reproduced, ex cept in full, without the written consent of t he 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, A nalytical Laboratory Certificate of Analysis, Analytical Laboratory QC Reports, Sub-contracted Laboratory Results, Customer Specific Data Sheets, Reports & Documentation, Customer Database Entries, Te st Case Narratives, Chain of Custody (COC) Certification: The Analytical Laboratory holds the follow ing 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.

## Sample ID's & Descriptions:
Sample ID Plant/Station Collection Date and Time Collected By Sample Description 2012012051 BELEWS 30-May-12 8:00 AM R. HENDRICKS FGD Purge Eff 2012012052 BELEWS 30-May-12 8:00 AM R. HENDRICKS EQ TANK EFF. 2012012053 BELEWS 30-May-12 8:00 AM R. HENDRICKS BIOREACTOR 1 INF 2012012054 BELEWS 30-May-12 8:00 AM R. HENDRICKS HG BLANK BIOREACTOR 1 INF. 2012012055 BELEWS 30-May-12 8:00 AM R. HENDRICKS BIOREACTOR 2 INF. 2012012056 BELEWS 30-May-12 8:00 AM R. HENDRICKS Hg Blk BioReactor 2 Inf 2012012057 BELEWS 30-May-12 8:00 AM R. HENDRICKS BIOREACTOR 2 EFF. 2012012058 BELEWS 30-May-12 8:00 AM R. HENDRICKS Hg Blk BioReactor 2 Eff 2012012059 BELEWS 30-May-12 8:00 AM R. HENDRICKS FILTER BLANK 2012012060 BELEWS 30-May-12 8:00 AM R. HENDRICKS METALS TRIP BLANK 10 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. The Vendor Laboratories have been qualified by the Analytical Laboratory 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: 

### Mary Ann Ogle Date: 

### 6/11/2012 Yes

Electronic Data Deliverable (EDD) Sent Separately

# Certificate of Laboratory Analysis This re p ort shall not be rep roduced, excep t in full. 

## Order # J12050473

2012012051 Collection Date: 30-May-12 8:00 AM 

### Site: FGD Purge Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF INORGANIC IONS BY IC Bromide 110 mg/L EPA 300.0 04-Jun-12 14:32 BGN9034 5 50 Chloride 7300 mg/L EPA 300.0 04-Jun-12 14:32 BGN9034 100 1000 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 277 ug/L EPA 245.1 07-Jun-12 11:05 AGIBBS 5 100 TOTAL RECOVERABLE METALS BY ICP Boron (B) 220 mg/L EPA 200.7 06-Jun-12 15:04 MHH7131 0.5 10 DISSOLVED METALS BY ICP-MS Selenium (Se) 194 ug/L EPA 200.8 31-May-12 14:59 KRICHAR 20 20 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 181 ug/L EPA 200.8 05-Jun-12 12:33 DJSULL1 20 20 Chromium (Cr) 265 ug/L EPA 200.8 05-Jun-12 12:33 DJSULL1 20 20 Copper (Cu) 145 ug/L EPA 200.8 05-Jun-12 12:33 DJSULL1 20 20 Manganese (Mn) 7380 ug/L EPA 200.8 05-Jun-12 12:33 DJSULL1 20 20 Nickel (Ni) 214 ug/L EPA 200.8 05-Jun-12 12:33 DJSULL1 20 20 Selenium (Se) 5690 ug/L EPA 200.8 05-Jun-12 12:33 DJSULL1 20 20 Silver (Ag) < 20 ug/L EPA 200.8 05-Jun-12 12:33 DJSULL1 20 20 Zinc (Zn) 286 ug/L EPA 200.8 05-Jun-12 12:33 DJSULL1 20 20 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 1 TOTAL DISSOLVED SOLIDS Vendor Parameter Complete V_PACE 1


### 2012012052 Collection Date: 30-May-12 8:00 AM 

### Site: EQ TANK EFF. Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 216 ug/L EPA 245.1 07-Jun-12 11:08 AGIBBS 2.5 50 TOTAL RECOVERABLE METALS BY ICP Boron (B) 223 mg/L EPA 200.7 06-Jun-12 15:08 MHH7131 0.5 10 DISSOLVED METALS BY ICP-MS Selenium (Se) 114 ug/L EPA 200.8 31-May-12 15:03 KRICHAR 10 10

# Certificate of Laboratory Analysis This re p ort shall not be rep roduced, excep t in full. 

## Order # J12050473

2012012052 Collection Date: 30-May-12 8:00 AM 

### Site: EQ TANK EFF. Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 171 ug/L EPA 200.8 05-Jun-12 12:36 DJSULL1 20 20 Chromium (Cr) 238 ug/L EPA 200.8 05-Jun-12 12:36 DJSULL1 20 20 Copper (Cu) 124 ug/L EPA 200.8 05-Jun-12 12:36 DJSULL1 20 20 Manganese (Mn) 7050 ug/L EPA 200.8 05-Jun-12 12:36 DJSULL1 20 20 Nickel (Ni) 200 ug/L EPA 200.8 05-Jun-12 12:36 DJSULL1 20 20 Selenium (Se) 5130 ug/L EPA 200.8 05-Jun-12 12:36 DJSULL1 20 20 Silver (Ag) < 20 ug/L EPA 200.8 05-Jun-12 12:36 DJSULL1 20 20 Zinc (Zn) 254 ug/L EPA 200.8 05-Jun-12 12:36 DJSULL1 20 20


### 2012012053 Collection Date: 30-May-12 8:00 AM 

### Site: BIOREACTOR 1 INF Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF MERCURY 1631 Vendor Parameter Complete V_BRAND 1 TOTAL RECOVERABLE METALS BY ICP Boron (B) 211 mg/L EPA 200.7 06-Jun-12 15:12 MHH7131 0.5 10 DISSOLVED METALS BY ICP-MS Selenium (Se) 91.5 ug/L EPA 200.8 31-May-12 15:07 KRICHAR 10 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 05-Jun-12 12:40 DJSULL1 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 05-Jun-12 12:40 DJSULL1 10 10 Copper (Cu) < 10 ug/L EPA 200.8 05-Jun-12 12:40 DJSULL1 10 10 Manganese (Mn) 5030 ug/L EPA 200.8 05-Jun-12 12:40 DJSULL1 10 10 Nickel (Ni) 39.9 ug/L EPA 200.8 05-Jun-12 12:40 DJSULL1 10 10 Selenium (Se) 92.4 ug/L EPA 200.8 05-Jun-12 12:40 DJSULL1 10 10 Silver (Ag) < 10 ug/L EPA 200.8 05-Jun-12 12:40 DJSULL1 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 05-Jun-12 12:40 DJSULL1 10 10 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 1

# Certificate of Laboratory Analysis This re p ort shall not be rep roduced, excep t in full. 

## Order # J12050473

2012012054 Collection Date: 30-May-12 8:00 AM 

### Site: HG BLANK BIOREACTOR 1 INF. Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF MERCURY 1631 Vendor Parameter Complete V_BRAND 1


### 2012012055 Collection Date: 30-May-12 8:00 AM 

### Site: BIOREACTOR 2 INF. Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF MERCURY 1631 Vendor Parameter Complete V_BRAND 1 TOTAL RECOVERABLE METALS BY ICP Boron (B) 207 mg/L EPA 200.7 06-Jun-12 15:16 MHH7131 0.5 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 05-Jun-12 13:57 DJSULL1 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 05-Jun-12 13:57 DJSULL1 10 10 Copper (Cu) < 10 ug/L EPA 200.8 05-Jun-12 13:57 DJSULL1 10 10 Manganese (Mn) 5210 ug/L EPA 200.8 05-Jun-12 13:57 DJSULL1 10 10 Nickel (Ni) 13.7 ug/L EPA 200.8 05-Jun-12 13:57 DJSULL1 10 10 Selenium (Se) 23.8 ug/L EPA 200.8 05-Jun-12 13:57 DJSULL1 10 10 Silver (Ag) < 10 ug/L EPA 200.8 05-Jun-12 13:57 DJSULL1 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 05-Jun-12 13:57 DJSULL1 10 10


### 2012012056 Collection Date: 30-May-12 8:00 AM 

### Site: Hg Blk BioReactor 2 Inf Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF MERCURY 1631 Vendor Parameter Complete V_BRAND 1


### 2012012057 Collection Date: 30-May-12 8:00 AM 

### Site: BIOREACTOR 2 EFF. Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF MERCURY 1631 Vendor Parameter Complete V_BRAND 1 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) < 1 ug/L EPA 245.1 07-Jun-12 11:10 AGIBBS 1 20

# Certificate of Laboratory Analysis This re p ort shall not be rep roduced, excep t in full. 

## Order # J12050473

2012012057 Collection Date: 30-May-12 8:00 AM 

### Site: BIOREACTOR 2 EFF. Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF TOTAL RECOVERABLE METALS BY ICP Boron (B) 203 mg/L EPA 200.7 06-Jun-12 15:20 MHH7131 0.5 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 05-Jun-12 14:00 DJSULL1 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 05-Jun-12 14:00 DJSULL1 10 10 Copper (Cu) < 10 ug/L EPA 200.8 05-Jun-12 14:00 DJSULL1 10 10 Manganese (Mn) 3900 ug/L EPA 200.8 05-Jun-12 14:00 DJSULL1 10 10 Nickel (Ni) < 10 ug/L EPA 200.8 05-Jun-12 14:00 DJSULL1 10 10 Selenium (Se) 15.9 ug/L EPA 200.8 05-Jun-12 14:00 DJSULL1 10 10 Silver (Ag) < 10 ug/L EPA 200.8 05-Jun-12 14:00 DJSULL1 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 05-Jun-12 14:00 DJSULL1 10 10 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 1


### 2012012058 Collection Date: 30-May-12 8:00 AM 

### Site: Hg Blk BioReactor 2 Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF MERCURY 1631 Vendor Parameter Complete V_BRAND 1


### 2012012059 Collection Date: 30-May-12 8:00 AM 

### Site: FILTER BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF DISSOLVED METALS BY ICP-MS Selenium (Se) < 1 ug/L EPA 200.8 31-May-12 14:54 KRICHAR 1 1


### 2012012060 Collection Date: 30-May-12 8:00 AM 

### Site: METALS TRIP BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF TOTAL RECOVERABLE METALS BY ICP Boron (B) < 0.05 mg/L EPA 200.7 06-Jun-12 15:00 MHH7131 0.05 1

# Certificate of Laboratory Analysis This re p ort shall not be rep roduced, excep t in full. 

## Order # J12050473

2012012060 Collection Date: 30-May-12 8:00 AM 

### Site: METALS TRIP BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DF TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 1 ug/L EPA 200.8 05-Jun-12 13:48 DJSULL1 1 1 Chromium (Cr) < 1 ug/L EPA 200.8 05-Jun-12 13:48 DJSULL1 1 1 Copper (Cu) < 1 ug/L EPA 200.8 05-Jun-12 13:48 DJSULL1 1 1 Manganese (Mn) < 1 ug/L EPA 200.8 05-Jun-12 13:48 DJSULL1 1 1 Nickel (Ni) < 1 ug/L EPA 200.8 05-Jun-12 13:48 DJSULL1 1 1 Selenium (Se) 1.08 ug/L EPA 200.8 05-Jun-12 13:48 DJSULL1 1 1 Silver (Ag) < 1 ug/L EPA 200.8 05-Jun-12 13:48 DJSULL1 1 1 Zinc (Zn) < 1 ug/L EPA 200.8 05-Jun-12 13:48 DJSULL1 1 1 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 1

## June 8 , 201 2

Jay Perkins Duke Energy Analytical Laboratory Mail Code MGO3A2 (Building 7405) 13339 Hagers Ferry Rd. Huntersville, NC 28078 (704) 875-5 245 Project: Belews Creek

–

FGD Alternate Fuels Test Burn (LIMS # J1 20 50 4 73 )

Dear Mr. Perkins, Attached is the report associated with four (4 ) aqueous samples submitted for selenium speciation analysis on May 31 , 2012

. The samples were received in a sealed cooler at0.0 ° C on June 1, 2012

. 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 analysis are addressed in the following report. If you have any questions, please feel free to contact me at your convenience.
Sincerely,

Russell Gerads Vice President 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 Creek

–

FGD Alternate Fuels Test Burn (LIMS # J12050473 )

June 7 , 2012

1. Sample Reception Four (4 ) aqueous samples in 125mL HDPE bottles (provided by Applied Speciation and Consulting) were submitted for selenium speciation analysi s on May 31 , 2012. The samples were received on June 1 , 201 2 in a sealed co ntainer at 0. 0 ° C. The samples were received in a laminar flow clean hood, void of trace metals contamination and ultra-violet radiation, and was designated a discrete sample identifier. An aliquot of each sample was filtered (0.45μm) and each filtrate w as stored in a secure, monitored cryofreezer (maintained at a temperature of -80 o 

## 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. 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 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 minimal interval of every ten analytical runs. 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 June 5, 2012. An aliquot of eachsample 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 this sample 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.

## If you have any questions or concerns regarding this report, please feel free to contact me.

Si ncerely,

Russell Gerads Vice President Applied Speciation and Consulting, LLC

### Sample Results

Sample ID Se(IV) Se(VI) SeCN MeSe(IV) SeMe Unknown Se Species (n) FGD Purge Eff 93.1 77.7 ND (<0.45) ND (<0.59) ND (<0.59) 0 (0) BioReactor 1 Inf 18.8 62.5 ND (<0.11) 1.79 ND (<0.15) 0 (0) BioReactor 2 Eff 0.415 ND (<0.25) ND (<0.11) ND (<0.15) ND (<0.15) 0 (0) Metals Trip Blk ND (<0.016) ND (<0.050) ND (<0.023) ND (<0.030) ND (<0.030) 0 (0) All results reflect the applied dilution and are reported in μg/L 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: Russell Gerads Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews Creek - FGD Alternate Fuels Test Burn

Contact: Jay Perkins
Date: June 8, 2012 LIMS #J12050473

### Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 10x eMDL 50x eMDL 200x Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.016 0.082 0.33 Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.050 0.25 1.00 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.023 0.11 0.45 MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.003 0.030 0.15 0.59 SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.003 0.030 0.15 0.59 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 Se(IV) LCS 9.57 9.96 104.0 Se(VI) LCS 9.48 9.37 98.9 SeCN LCS 8.92 8.73 97.9 MeSe(IV) LCS 6.47 5.70 88.1 SeMe LCS 9.32 8.79 94.3 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews Creek - FGD Alternate Fuels Test Burn

Contact: Jay Perkins LIMS #J12050473 Date: June 8, 2012 Report Generated by: Russell Gerads

### Quality Control Summary - Matrix Duplicates

Analyte (μg/L) Sample ID Rep 1 Rep 2 Mean RPD Se(IV) Batch QC 46.21 45.82 46.02 0.9 Se(VI) Batch QC 64.75 63.22 63.99 2.4 SeCN Batch QC ND (<0.45) ND (<0.45) NC NC MeSe(IV) Batch QC ND (<0.15) ND (<0.15) NC NC SeMe Batch QC ND (<0.15) ND (<0.15) 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 Se(IV) Batch QC 1112 1892 166.0 1112 1900 166.7 0.4 Se(VI) Batch QC 1009 1168 109.4 1009 1183 110.9 1.3 SeCN Batch QC 915.0 462.9 50.6* 915.0 470.7 51.4* 1.7 *The low recovery is attributed to matrix induced species conversion Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews Creek - FGD Alternate Fuels Test Burn

Contact: Jay Perkins LIMS #J12050473 Date: June 8, 2012 Report Generated by: Russell Gerads

### 3958 6 th 

### Ave NW • Seattle, WA 98107 • T: 206-632-6206 • F: 206-632-6017 • www.brooksrand.com • brl@brooksrand.com 

## June 8, 2012
Duke Energy ATTN: Jay Perkins Scientific Support-Laboratory 13339 Hagers Ferry Road Huntersville NC 28078 jcperkins@duke-energy.com labcustomer@duke-energy.com
RE: Project DUK-HV1201 Client Project: J12050473 Dear Mr. Perkins, On June 1, 2012, Brooks Rand Labs (BRL) received three (3) wastewater samples and three (3) corresponding field blanks. Samples were logged-in for total mercury (THg) analysis. All samples were received, prepared, analyzed, and stored according to BRL SOPs and EPA methodology. The results were blank-corrected as described in the calculations section of the applicable SOP(s) and may be evaluated using adjusted reporting limits to account for sample aliquot size. Please refer to the Sample Results page for sample-specific detection limits and other details. Aside from concentration qualifiers, all data was reported without qualification and all associated quality control sample results met the acceptance criteria. BRL, an accredited laboratory, certifies the reported results of all analyses for which BRL is NELAP accredited meet all NELAP requirements. For more details, see the Report Information page of the report. Please feel free to contact me if you have any questions regarding this report. Sincerely,

Tiffany Stilwater Project Manager tiffany@brooksrand.comProject ID: 

### DUK-HV1201

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



### Definition of Data Qualifiers

(Effective 9/23/09) 

### Laboratory Accreditation BRL is accredited by the National Environmental Laboratory Accreditation Program (NELAP) through the State of Florida Department of Health, Bureau of Laboratories (E87982) and is certified to perform many environmental analyses. BRL is also certified by many other states to perform environmental analyses. For a current list of our accreditations /certifications, please visit our website at <http://www.brooksrand.com/default.asp?contentID=586>. Results reported relate only to the samples listed in the report. 

# Report Information

BLK BRL BS CAL CCV CRM D DUP ICV MSD ND NR PS REC RPD RSD SCV SOP 

### method blank Brooks Rand Labs laboratory fortified blank calibration standard continuing calibration verification certified reference material dissolved fraction duplicate initial calibration verification matrix spike duplicate non-detect non-reportable post preparation spike percent recovery relative percent difference relative standard deviation secondary calibration verification standard operating procedure MDL MRL MS



### method detection limit method reporting limit matrix spike

SRM T COC



### standard reference material total recoverable fraction chain of custody record 

### Common Abbreviations

These qualifiers are based on those previously utilized by Brooks Rand, Ltd., those found in the EPA SOW ILM03.0, Exhibit B, Section III, pg. B-18, and the USEPA Laboratory Data Validation Functional Guidelines for Evaluating Inorganic Analyses; USEPA; July 2002. These supersede all previous qualifiers ever employed by BRL. Detected by the instrument, the result is > the MDL but ≤ the MRL. Result is reported and considered an estimate. B E 

### An estimated value due to the presence of interferences. A full explanation is presented in the narrative. H 

### Holding time and/or preservation requirements not met. Result is estimated. J 

### Estimated value. A full explanation is presented in the narrative. J-M 

### Duplicate precision (RPD) for associated QC sample was not within acceptance criteria. Result is estimated. J-N 

### Spike recovery for associated QC sample was not within acceptance criteria. Result is estimated. M 

### Duplicate precision (RPD) was not within acceptance criteria. Result is estimated. N 

### Spike recovery was not within acceptance criteria. Result is estimated. R 

### Rejected, unusable value. A full explanation is presented in the narrative. U 

### Result is ≤ the MDL or client requested reporting limit (CRRL). Result reported as the MDL or CRRL. X 

### Result is not BLK-corrected and is within 10x the absolute value of the highest detectable BLK in the batch. Result is estimated. 

### Field Quality Control Samples Please be notified that certain EPA methods require the collection of field quality control samples of an appropriate type and frequency; failure to do so is considered a deviation from some methods and for compliance purposes should only be done with the approval of regulatory authorities. Please see the specific EPA methods for details regarding required field quality control samples.

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: 

### DUK-HV1201

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Sample Information

Report Matrix Type Received Sampled Sample Lab ID 

### 1222026-01 BioReactor 1 Inf 05/30/2012 06/01/2012 Sample Influent 1222026-02 Hg Blk BioReactor 1 Inf 05/30/2012 06/01/2012 Field Blank DIW 1222026-03 BioReactor 2 Inf 05/30/2012 06/01/2012 QC Sample Influent 1222026-04 Hg Blk BioReactor 2 Inf 05/30/2012 06/01/2012 Field Blank DIW 1222026-05 BioReactor 2 Eff 05/30/2012 06/01/2012 Sample Effluent 1222026-06 Hg Blk BioReactor 2 Eff 05/30/2012 06/01/2012 Field Blank DIW 

# Batch Summary

Analyte Prepared Analyzed Sequence Batch Lab Matrix Method 

### B120918 06/04/2012 06/06/2012 1200419 Water EPA 1631 Hg

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: 

### DUK-HV1201

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Sample Results

Sample Sequence Result MDL MRL Unit Batch

Qualifier Analyte Fraction

Report Matrix BioReactor 1 Inf 

### ng/L 91.4 T 1200419 B120918 Influent 8.16 3.06 1222026-01 Hg

BioReactor 2 Eff 

### ng/L 7.55 T 1200419 B120918 Effluent 1.63 0.61 1222026-05 Hg

BioReactor 2 Inf 

### ng/L 20.5 T 1200419 B120918 Influent 8.16 3.06 1222026-03 Hg
Hg Blk BioReactor 1 Inf 

### ng/L 0.15 T U 1200419 B120918 DIW 0.41 0.15 1222026-02 Hg
Hg Blk BioReactor 2 Eff 

### ng/L 0.15 T U 1200419 B120918 DIW 0.40 0.15 1222026-06 Hg
Hg Blk BioReactor 2 Inf 

### ng/L 0.15 T U 1200419 B120918 DIW 0.41 0.15 1222026-04 Hg

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: 

### DUK-HV1201

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Accuracy & Precision Summary

Batch: 

### B120918

Analyte Result Units Native Spike REC & Limits RPD & Limits Method: 

### EPA 1631 Lab Matrix: 

### Water

Sample Certified Reference Material (1221029, NIST 1641d 1000x dilution) B120918-SRM1 

### 15.68 103% ng/L 85-115 Hg 16.09
Matrix Spike (1222026-03) B120918-MS1 

### 102.0 113% ng/L 71-125 Hg 136.2

20.51
Matrix Spike Duplicate (1222026-03) B120918-MSD1 

### 102.0 110% ng/L 71-125 242% Hg 133.0

20.51
Matrix Spike (1222026-05) B120918-MS2 

### 38.39 111% ng/L 71-125 Hg 50.24

7.55
Matrix Spike Duplicate (1222026-05) B120918-MSD2 

### 38.10 110% ng/L 71-125 241% Hg 49.63

7.55

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: 

### DUK-HV1201

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Method Blanks & Reporting Limits

Batch: 

### B120918
Method: 

### EPA 1631 Matrix: 

### Water Analyte: 

### Hg Result Units Sample 

### B120918-BLK1 ng/L 0.27 B120918-BLK2 ng/L 0.30 B120918-BLK3 ng/L 0.29 B120918-BLK4 ng/L 0.18 MDL: 

### 0.15 Average: 

### 0.26 Standard Deviation: 

### 0.05 Limit: 

### 0.10 Limit: 

### 0.50 MRL: 

### 0.40

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: 

### DUK-HV1201

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Instrument Calibration

Sequence: 

### 1200419 Method: 

### EPA 1631 Instrument: 

### THG-05 Date: 

### 06/06/2012 Total Mercury and Mercury Speciation by CVAFS

Analyte: 

### Hg REC & Limits Result True Value Lab ID Units 

### 1200419-IBL1 5.61 pg of Hg 1200419-IBL2 7.11 pg of Hg 1200419-IBL3 5.37 pg of Hg 1200419-IBL4 5.64 pg of Hg 1200419-CAL1 25.00 24.78 pg of Hg 99% 1200419-CAL2 100.0 100.2 pg of Hg 100% 1200419-CAL3 500.0 499.9 pg of Hg 100% 1200419-CAL4 2500 2487 pg of Hg 99% 1200419-CAL5 10000 10120 pg of Hg 101% 1200419-ICV1 1568 1609 pg of Hg 103% 85-115 1200419-CCV1 500.0 509.5 pg of Hg 102% 77-123 1200419-CCB1 11.3 pg of Hg 1200419-CCV2 500.0 515.0 pg of Hg 103% 77-123 1200419-CCV3 500.0 503.7 pg of Hg 101% 77-123 1200419-CCV4 500.0 503.0 pg of Hg 101% 77-123

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: 

### DUK-HV1201

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Sample Containers

Lab ID: 

### 1222026-01 Report Matrix: 

### Influent Sample Type: 

### Sample Received: 

### 06/01/2012 Sample: 

### BioReactor 1 Inf Collected: 

### 05/30/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71628390 10 Cooler

none n/a 500 mL Bottle FLPE Hg-T

Lab ID: 

### 1222026-02 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 06/01/2012 Sample: 

### Hg Blk BioReactor 1 Inf Collected: 

### 05/30/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71628390 10 Cooler

none n/a 500 mL Bottle FLPE Hg-T

Lab ID: 

### 1222026-03 Report Matrix: 

### Influent Sample Type: 

### QC Sample Received: 

### 06/01/2012 Sample: 

### BioReactor 2 Inf Collected: 

### 05/30/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71628390 10 Cooler

none n/a 500 mL Bottle FLPE Hg-T

Lab ID: 

### 1222026-04 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 06/01/2012 Sample: 

### Hg Blk BioReactor 2 Inf Collected: 

### 05/30/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71628390 10 Cooler

none n/a 500 mL Bottle FLPE Hg-T

Lab ID: 

### 1222026-05 Report Matrix: 

### Effluent Sample Type: 

### Sample Received: 

### 06/01/2012 Sample: 

### BioReactor 2 Eff Collected: 

### 05/30/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71628390 10 Cooler

none n/a 500 mL Bottle FLPE Hg-T

Lab ID: 

### 1222026-06 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 06/01/2012 Sample: 

### Hg Blk BioReactor 2 Eff Collected: 

### 05/30/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71628390 10 Cooler

none n/a 500 mL Bottle FLPE Hg-T

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: 

### DUK-HV1201

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Shipping Containers

Cooler Tracking No: 

### 4726 7967 1661 via FedEx Temperature: 

### 0.8 °C Coolant Type: 

### Ice Description: 

### Cooler Damaged in transit? 

### No Returned to client? 

### No Custody seals present? 

### No Custody seals intact? 

### No COC present? 

### Yes Received: 

### June 1, 2012 9:15

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.com

## June 05, 2012

LIMS USE: FR - PROGRAM MANAGER LIMS OBJECT ID: 92119701



## 92119701 Project: Pace Project No.: RE: Program Manager Duke Energy

,

J12050473

Dear Program Manager: Enclosed are the analytical results for sample(s) received by the laboratory on May 31, 2012. The results relate only to the samples included in this report. Results reported herein conform to the most current TNI standards and the laboratory's Quality Assurance Manual, where applicable, unless otherwise noted in the body of the report.
Analyses were performed at the Pace Analytical Services location indicated on the sample analyte page for analysis unless otherwise footnoted. If you have any questions concerning this report, please feel free to contact me.
Sincerely,

Kevin Herring kevin.herring@pacelabs.com Project Manager

Enclosures



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Page 1 of 8 Pace Analytical Services, Inc. 9800 Kincey Ave. Suite 100 Huntersville, NC 28078 (704)875-9092 Pace Analytical Services, Inc.

2225 Riverside Dr. Asheville, NC 28804 (828)254-7176 Pace Analytical Services, Inc. 205 East Meadow Road - Suite A

Eden, NC 27288 (336)623-8921

### CERTIFICATIONS

Pace Project No.: Project: 92119701

J12050473

Asheville Certification IDs 2225 Riverside Dr., Asheville, NC 28804 Florida/NELAP Certification #: E87648 Massachusetts Certification #: M-NC030 North Carolina Drinking Water Certification #: 37712 North Carolina Wastewater Certification #: 40 South Carolina Certification #: 99030001 Virginia Certification #: 00072 West Virginia Certification #: 356 Virgina/VELAP Certification #: 460147



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Page 2 of 8 Pace Analytical Services, Inc. 9800 Kincey Ave. Suite 100 Huntersville, NC 28078 (704)875-9092 Pace Analytical Services, Inc.

2225 Riverside Dr. Asheville, NC 28804 (828)254-7176 Pace Analytical Services, Inc. 205 East Meadow Road - Suite A

Eden, NC 27288 (336)623-8921

### SAMPLE SUMMARY

Pace Project No.: Project: 92119701

J12050473

Lab ID Sample ID Matrix Date Collected Date Received 92119701001 2012012051 Water 05/30/12 08:00 05/31/12 14:50



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Page 3 of 8 Pace Analytical Services, Inc. 9800 Kincey Ave. Suite 100 Huntersville, NC 28078 (704)875-9092 Pace Analytical Services, Inc.

2225 Riverside Dr. Asheville, NC 28804 (828)254-7176 Pace Analytical Services, Inc. 205 East Meadow Road - Suite A

Eden, NC 27288 (336)623-8921

### SAMPLE ANALYTE COUNT

Pace Project No.: Project: 92119701

J12050473

Lab ID Sample ID Method Analytes Reported Laboratory Analysts 92119701001 2012012051 SM 2540C 1 PASI-A LMD



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Page 4 of 8 Pace Analytical Services, Inc. 9800 Kincey Ave. Suite 100 Huntersville, NC 28078 (704)875-9092 Pace Analytical Services, Inc.

2225 Riverside Dr. Asheville, NC 28804 (828)254-7176 Pace Analytical Services, Inc. 205 East Meadow Road - Suite A

Eden, NC 27288 (336)623-8921

### ANALYTICAL RESULTS

Pace Project No.: Project: 92119701

J12050473
Sample: 2012012051 Lab ID: 92119701001 Collected: 05/30/12 08:00 Received: 05/31/12 14:50 Matrix: Water

Parameters Results Units DF Prepared Analyzed CAS No. Qual MDL Limit Report

2540C Total Dissolved Solids Analytical Method: SM 2540C Total Dissolved Solids 16600 mg/L 1 05/31/12 22:53 500 500



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Date: 06/05/2012 05:36 PM Page 5 of 8 Pace Analytical Services, Inc. 9800 Kincey Ave. Suite 100 Huntersville, NC 28078 (704)875-9092 Pace Analytical Services, Inc.

2225 Riverside Dr. Asheville, NC 28804 (828)254-7176 Pace Analytical Services, Inc. 205 East Meadow Road - Suite A

Eden, NC 27288 (336)623-8921

### QUALITY CONTROL DATA

Pace Project No.: Project: 92119701

J12050473

QC Batch: QC Batch Method: Analysis Method: Analysis Description: WET/21050 SM 2540C SM 2540C 2540C Total Dissolved Solids Associated Lab Samples: 92119701001

Parameter Units Blank Result Reporting

Limit Qualifiers METHOD BLANK: 771370 Associated Lab Samples: 92119701001 Matrix: Water

Analyzed Total Dissolved Solids mg/L ND 25.0 05/31/12 22:50

Parameter Units LCS Result % Rec Limits Qualifiers % Rec Conc. 771371 LABORATORY CONTROL SAMPLE: LCS Spike

Total Dissolved Solids mg/L 246 250 98 80-120

Parameter Units Dup Result Max RPD Qualifiers RPD Result 92119558001 771372 SAMPLE DUPLICATE:

Total Dissolved Solids mg/L 8320 5 10 8760

Parameter Units Dup Result Max RPD Qualifiers RPD Result 92119703003 771373 SAMPLE DUPLICATE:

Total Dissolved Solids mg/L 57.0 7 10 61.0



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Date: 06/05/2012 05:36 PM Page 6 of 8 Pace Analytical Services, Inc. 9800 Kincey Ave. Suite 100 Huntersville, NC 28078 (704)875-9092 Pace Analytical Services, Inc.

2225 Riverside Dr. Asheville, NC 28804 (828)254-7176 Pace Analytical Services, Inc. 205 East Meadow Road - Suite A

Eden, NC 27288 (336)623-8921

### QUALIFIERS

Pace Project No.: Project: 92119701

J12050473

DEFINITIONS DF - Dilution Factor, if reported, represents the factor applied to the reported data due to changes in sample preparation, dilution of the sample aliquot, or moisture content. ND - Not Detected at or above adjusted reporting limit. J - Estimated concentration above the adjusted method detection limit and below the adjusted reporting limit. MDL - Adjusted Method Detection Limit. PRL - Pace Reporting Limit. RL - Reporting Limit. S - Surrogate 1,2-Diphenylhydrazine (8270 listed analyte) decomposes to Azobenzene. Consistent with EPA guidelines, unrounded data are displayed and have been used to calculate % recovery and RPD values. LCS(D) - Laboratory Control Sample (Duplicate) MS(D) - Matrix Spike (Duplicate) DUP - Sample Duplicate RPD - Relative Percent Difference NC - Not Calculable. SG - Silica Gel - Clean-Up U - Indicates the compound was analyzed for, but not detected. N-Nitrosodiphenylamine decomposes and cannot be separated from Diphenylamine using Method 8270. The result reported for each analyte is a combined concentration. Acid preservation may not be appropriate for 2-Chloroethylvinyl ether, Styrene, and Vinyl chloride. Pace Analytical is TNI accredited. Contact your Pace PM for the current list of accredited analytes. TNI - The NELAC Institute. LABORATORIES Pace Analytical Services - Asheville PASI-A



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Date: 06/05/2012 05:36 PM Page 7 of 8 Pace Analytical Services, Inc. 9800 Kincey Ave. Suite 100 Huntersville, NC 28078 (704)875-9092 Pace Analytical Services, Inc.

2225 Riverside Dr. Asheville, NC 28804 (828)254-7176 Pace Analytical Services, Inc. 205 East Meadow Road - Suite A

Eden, NC 27288 (336)623-8921

### QUALITY CONTROL DATA CROSS REFERENCE TABLE

Pace Project No.: Project: 92119701

J12050473

Lab ID Sample ID QC Batch Method QC Batch Analytical Method Analytical Batch 92119701001 WET/21050 2012012051 SM 2540C



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Date: 06/05/2012 05:36 PM Page 8 of 8 Pace Analytical Services, Inc. 9800 Kincey Ave. Suite 100 Huntersville, NC 28078 (704)875-9092 Pace Analytical Services, Inc.

2225 Riverside Dr. Asheville, NC 28804 (828)254-7176 Pace Analytical Services, Inc. 205 East Meadow Road - Suite A

Eden, NC 27288 (336)623-8921