### 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: J12100061 Project Name: WWTS - Biweekly (1)

L ab Contact: Jason C Perkins


### Date: 10/31/2012 Customer Address: 3195 Pine Hall Rd Customer Name(s): Bill Kennedy, Melonie 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 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.

## Sample ID's & Descriptions:

Sample ID Plant/Station Collection Date and Time Collected By Sample Description 2012020935 BELEWS 10-Oct-12 7:30 AM W.WORKMAN FGD Purge Eff 2012020936 BELEWS 10-Oct-12 7:35 AM W.WORKMAN EQ TANK EFF. 2012020937 BELEWS 10-Oct-12 7:40 AM W.WORKMAN BIOREACTOR 1 INF. 2012020938 BELEWS 10-Oct-12 7:45 AM W.WORKMAN BIOREACTOR 2 INF. 2012020939 BELEWS 10-Oct-12 7:50 AM W.WORKMAN BIOREACTOR 2 EFF. 2012020940 BELEWS 10-Oct-12 8:00 AM W.WORKMAN FILTER BLANK 2012020941 BELEWS 10-Oct-12 8:10 AM W.WORKMAN Trip Blank 2012020942 BELEWS 10-Oct-12 7:40 AM W.WORKMAN BIOREACTOR 1 INF (HG) 2012020943 BELEWS 10-Oct-12 7:40 AM W.WORKMAN HG BLANK BIOREACTOR 1 INF. 2012020944 BELEWS 10-Oct-12 7:45 AM W.WORKMAN BIOREACTOR 2 INF (HG) 2012020945 BELEWS 10-Oct-12 7:45 AM W.WORKMAN Hg Blk BioReactor 2 Inf 2012020946 BELEWS 10-Oct-12 7:50 AM W.WORKMAN BIOREACTOR 2 EFF (HG) 2012020947 BELEWS 10-Oct-12 7:50 AM W.WORKMAN Hg Blk BioReactor 2 Eff 13 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: 

### 10/31/2012 Electronic Data Deliverable (EDD) Sent Separately

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



### Order # J12100061

2012020935 Collection Date: 10-Oct-12 7:30 AM 

### Site: FGD Purge Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF INORGANIC IONS BY IC Bromide 72 mg/L EPA 300.0 10/16/2012 22:58 JAHERMA 5 50 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 212 ug/L EPA 245.1 10/18/2012 14:01 AGIBBS 5 100
DISSOLVED METALS BY ICP Manganese (Mn) 5.55 mg/L EPA 200.7 10/11/2012 14:08 DJSULL1 0.05 10
TOTAL RECOVERABLE METALS BY ICP Boron (B) 141 mg/L EPA 200.7 10/19/2012 11:19 DJSULL1 5 10 Manganese (Mn) 6.21 mg/L EPA 200.7 10/19/2012 11:19 DJSULL1 0.5 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 294 ug/L EPA 200.8 10/17/2012 13:16 KRICHAR 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 254 ug/L EPA 200.8 10/17/2012 13:07 KRICHAR 10 10 Chromium (Cr) 217 ug/L EPA 200.8 10/17/2012 13:07 KRICHAR 10 10 Copper (Cu) 118 ug/L EPA 200.8 10/17/2012 13:07 KRICHAR 10 10 Nickel (Ni) 161 ug/L EPA 200.8 10/17/2012 13:07 KRICHAR 10 10 Selenium (Se) 5530 ug/L EPA 200.8 10/17/2012 13:07 KRICHAR 20 20 Silver (Ag) < 10 ug/L EPA 200.8 10/17/2012 13:07 KRICHAR 10 10 Zinc (Zn) 193 ug/L EPA 200.8 10/17/2012 13:07 KRICHAR 10 10 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C
TOTAL DISSOLVED SOLIDS TDS 15000 mg/L SM2540C 10/16/2012 14:35 SWILLI3 200 1



### 2012020936 Collection Date: 10-Oct-12 7:35 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) 138 ug/L EPA 245.1 10/18/2012 14:04 AGIBBS 2.5 50
DISSOLVED METALS BY ICP Manganese (Mn) 5.03 mg/L EPA 200.7 10/11/2012 14:12 DJSULL1 0.05 10
TOTAL RECOVERABLE METALS BY ICP Boron (B) 139 mg/L EPA 200.7 10/19/2012 11:23 DJSULL1 5 10 Manganese (Mn) 5.38 mg/L EPA 200.7 10/19/2012 11:23 DJSULL1 0.5 10

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



### Order # J12100061

2012020936 Collection Date: 10-Oct-12 7:35 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) 198 ug/L EPA 200.8 10/17/2012 13:19 KRICHAR 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 204 ug/L EPA 200.8 10/17/2012 12:09 KRICHAR 10 10 Chromium (Cr) 168 ug/L EPA 200.8 10/17/2012 12:09 KRICHAR 10 10 Copper (Cu) 83.7 ug/L EPA 200.8 10/17/2012 12:09 KRICHAR 10 10 Nickel (Ni) 136 ug/L EPA 200.8 10/17/2012 12:09 KRICHAR 10 10 Selenium (Se) 3800 ug/L EPA 200.8 10/17/2012 12:09 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 10/17/2012 12:09 KRICHAR 10 10 Zinc (Zn) 143 ug/L EPA 200.8 10/17/2012 12:09 KRICHAR 10 10



### 2012020937 Collection Date: 10-Oct-12 7:40 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF DISSOLVED METALS BY ICP Manganese (Mn) 0.648 mg/L EPA 200.7 10/11/2012 14:23 DJSULL1 0.05 10
TOTAL RECOVERABLE METALS BY ICP Boron (B) 124 mg/L EPA 200.7 10/19/2012 11:27 DJSULL1 5 10 Manganese (Mn) 0.663 mg/L EPA 200.7 10/19/2012 11:27 DJSULL1 0.5 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 94.4 ug/L EPA 200.8 10/17/2012 13:23 KRICHAR 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 10/17/2012 12:12 KRICHAR 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 10/17/2012 12:12 KRICHAR 10 10 Copper (Cu) < 10 ug/L EPA 200.8 10/17/2012 12:12 KRICHAR 10 10 Nickel (Ni) < 10 ug/L EPA 200.8 10/17/2012 12:12 KRICHAR 10 10 Selenium (Se) 107 ug/L EPA 200.8 10/17/2012 12:12 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 10/17/2012 12:12 KRICHAR 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 10/17/2012 12:12 KRICHAR 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 # J12100061

2012020938 Collection Date: 10-Oct-12 7:45 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF TOTAL RECOVERABLE METALS BY ICP Boron (B) 122 mg/L EPA 200.7 10/19/2012 10:41 DJSULL1 0.5 10 Manganese (Mn) 2.66 mg/L EPA 200.7 10/19/2012 10:41 DJSULL1 0.05 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 10/17/2012 12:15 KRICHAR 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 10/17/2012 12:15 KRICHAR 10 10 Copper (Cu) < 10 ug/L EPA 200.8 10/17/2012 12:15 KRICHAR 10 10 Nickel (Ni) < 10 ug/L EPA 200.8 10/17/2012 12:15 KRICHAR 10 10 Selenium (Se) 10.6 ug/L EPA 200.8 10/17/2012 12:15 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 10/17/2012 12:15 KRICHAR 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 10/17/2012 12:15 KRICHAR 10 10



### 2012020939 Collection Date: 10-Oct-12 7:50 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF INORGANIC IONS BY IC Bromide 71 mg/L EPA 300.0 10/16/2012 23:17 JAHERMA 5 50 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) < 1 ug/L EPA 245.1 10/18/2012 14:11 AGIBBS 1 20
TOTAL RECOVERABLE METALS BY ICP Boron (B) 127 mg/L EPA 200.7 10/19/2012 10:45 DJSULL1 0.5 10 Manganese (Mn) 1.37 mg/L EPA 200.7 10/19/2012 10:45 DJSULL1 0.05 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 5 ug/L EPA 200.8 10/17/2012 12:19 KRICHAR 5 5 Chromium (Cr) < 5 ug/L EPA 200.8 10/17/2012 12:19 KRICHAR 5 5 Copper (Cu) < 5 ug/L EPA 200.8 10/17/2012 12:19 KRICHAR 5 5 Nickel (Ni) < 5 ug/L EPA 200.8 10/17/2012 12:19 KRICHAR 5 5 Selenium (Se) < 5 ug/L EPA 200.8 10/17/2012 12:19 KRICHAR 5 5 Silver (Ag) < 5 ug/L EPA 200.8 10/17/2012 12:19 KRICHAR 5 5 Zinc (Zn) < 5 ug/L EPA 200.8 10/17/2012 12:19 KRICHAR 5 5 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 # J12100061

2012020940 Collection Date: 10-Oct-12 8:00 AM 

### Site: FILTER BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF DISSOLVED METALS BY ICP Manganese (Mn) 0.007 mg/L EPA 200.7 10/11/2012 13:43 DJSULL1 0.005 1
DISSOLVED METALS BY ICP-MS Selenium (Se) < 1 ug/L EPA 200.8 10/17/2012 13:10 KRICHAR 1 1



### 2012020941 Collection Date: 10-Oct-12 8:10 AM 

### 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 10/19/2012 10:37 DJSULL1 0.05 1 Manganese (Mn) < 0.005 mg/L EPA 200.7 10/19/2012 10:37 DJSULL1 0.005 1
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 1 ug/L EPA 200.8 10/17/2012 12:03 KRICHAR 1 1 Chromium (Cr) < 1 ug/L EPA 200.8 10/17/2012 12:03 KRICHAR 1 1 Copper (Cu) 1.60 ug/L EPA 200.8 10/17/2012 12:03 KRICHAR 1 1 Nickel (Ni) < 1 ug/L EPA 200.8 10/17/2012 12:03 KRICHAR 1 1 Selenium (Se) < 1 ug/L EPA 200.8 10/17/2012 12:03 KRICHAR 1 1 Silver (Ag) < 1 ug/L EPA 200.8 10/17/2012 12:03 KRICHAR 1 1 Zinc (Zn) 1.32 ug/L EPA 200.8 10/17/2012 12:03 KRICHAR 1 1 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C



### 2012020942 Collection Date: 10-Oct-12 7:40 AM 

### Site: BIOREACTOR 1 INF (HG) Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND



### 2012020943 Collection Date: 10-Oct-12 7:40 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND

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



### Order # J12100061

2012020943 Collection Date: 10-Oct-12 7:40 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF


### 2012020944 Collection Date: 10-Oct-12 7:45 AM 

### Site: BIOREACTOR 2 INF (HG) Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND



### 2012020945 Collection Date: 10-Oct-12 7:45 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND



### 2012020946 Collection Date: 10-Oct-12 7:50 AM 

### Site: BIOREACTOR 2 EFF (HG) Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND



### 2012020947 Collection Date: 10-Oct-12 7:50 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND

## October 22 , 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 - FGD WWTS Bi-Monthly Sampling) (LIMS #J1200061)

Dear Mr. Perkins, Attached is the report associated with four (4 ) aqueous samples submitted for selenium speciation analysis on October 11 , 2012

. The samples were received in a sealed cooler at 0. 7 ° C on October 12 , 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 - FGD WWTS Bi-Monthly Sampling) (LIMS #J1200061)

October 22 , 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 October 11, 2012 . The samples were received on October 12 , 201 2 in a sealed container at 0.7 °C. The samples were received in a laminar flow clean hood, void of trace metals contamination and ultra-v iolet radiation, and were designated discrete sample identifiers. 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 Each sample for selenium speciation analysis w as analyzed by ion chromatography inductively coupled plasma collision reaction cell mass spectrometry (IC-ICP- CRC -MS) on October 17, 2012. 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.
Re tention 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 th e samples were within acceptance limits. The estimated method detection limits (eMDLs) for selenite, selenate, and selenocyanate are generated from replicate analyses of the lowest standard in the calibration curve. Not all selenium species are present in preparation blanks; therefore, eMDL calculations based on preparation blanks are artificially biased low. The eMDL for methylseleninic acid and selenomethionine is calculated from the average eMDL of selenite, selenate, and selenocyanate. The calibration does not contain methylseleninic acid or selenomethionine due to impurities in these standards which would bias the results for other selenium species.

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

Sincerely,

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 158 67.7 ND (<0.93) 1.8 ND (<1.4) 0.0 (0) BioReactor 1 Inf 32.6 59.8 ND (<0.23) 2.53 ND (<0.36) 0.97 (1) BioReactor 2 Eff ND (<0.34) ND (<0.51) ND (<0.23) ND (<0.36) ND (<0.36) 0.0 (0) Metals Trip Blk 0.182 0.035 ND (<0.009) ND (<0.014) ND (<0.014) 0.0 (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 Report Generated by: Russell Gerads Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS Bi-Monthly Sampling)

Contact: Jay Perkins

Date: October 22, 2012 LIMS #J12100061

### Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 10x eMDL 250x eMDL 1000x Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.014 0.34 1.4 Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.020 0.51 2.0 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.009 0.23 0.93 MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.014 0.36 1.4 SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.014 0.36 1.4 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 9.62 100.5 Se(VI) LCS 9.48 9.18 96.8 SeCN LCS 8.92 8.95 100.3 MeSe(IV) LCS 6.47 6.75 104.3 SeMe LCS 9.32 8.32 89.3 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS Bi-Monthly Sampling)

Contact: Jay Perkins LIMS #J12100061 Date: October 22, 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 ND (<0.34) ND (<0.34) NC NC Se(VI) Batch QC 316.7 318.0 317.3 0.4 SeCN Batch QC ND (<0.23) ND (<0.23) NC NC MeSe(IV) Batch QC 0.48 ND (<0.36) NC NC SeMe Batch QC ND (<0.36) ND (<0.36) 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 1390 1515 109.0 1390 1539 110.7 1.6 Se(VI) Batch QC 1261 1627 103.9 1261 1667 107.0 2.4 SeCN Batch QC 1144 1158 101.2 1144 1168 102.2 0.9 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS Bi-Monthly Sampling)

Contact: Jay Perkins LIMS #J12100061 Date: October 22, 2012 Report Generated by: Russell Gerads3958 6 th Ave NW • Seattle, WA 98107 • T: 206

- 632

- 6206 • F: 206

- 632

- 6017 • www.brooksrand.com • brl@brooksrand.com 

### October 30, 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

- HV1 201 Client P roject : J121 00 061 Dear Mr. Perkins, O n October 12 , 2012 , Brooks Rand Labs ( BRL ) received three (3 ) wastewater samples and three (3) corresponding field blanks. The samples were logged

- in for total mercury (Hg) analysis according to the chain

- of

- custody form. All samples were received, prepared, analyzed, and stored according to BRL SOPs and EPA methodol ogy. The results were blank

- corrected as described in the calculations section of the relevant SOP and may have been evaluated using reporting limits that have been adjusted to account for sample aliquot size. Please refer to the Sample Results page for sample

- specific MDLs, MRLs, and other details. All field blank samples yielded detectable results

. However, all concentration s w ere less than the method defined control limit of 0.5 ng/L and the associated field sample result s w ere more than 10x the level of the blank result s . Contamination was considered insignificant. The analysis of CCB 1 was slightly greater than the low calibration standard. The cause was likely due to carryover from the ICV. No client samples were bracketed by the elevated C CB and no further action was required. 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 Labs, those found in the EPA SOW ILM03.0, Exhibit B, Section III, pg. B-18, and the USEPA Contract Laboratory Program National Functional Guidelines for Inorganic Superfund Data Review; USEPA; January 2010. 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 1241020-01 BioReactor 1 Inf 10/10/2012 10/12/2012 Sample Influent 1241020-02 Hg Blk BioReactor 1 Inf 10/10/2012 10/12/2012 Field Blank DIW 1241020-03 BioReactor 2 Inf 10/10/2012 10/12/2012 QC Sample Influent 1241020-04 Hg Blk BioReactor 2 Inf 10/10/2012 10/12/2012 Field Blank DIW 1241020-05 BioReactor 2 Eff 10/10/2012 10/12/2012 Sample Effluent 1241020-06 Hg Blk BioReactor 2 Eff 10/10/2012 10/12/2012 Field Blank DIW 

# Batch Summary

Analyte Prepared Analyzed Sequence Batch Lab Matrix Method B121932 10/18/2012 10/24/2012 1200820 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 Basis

Report Matrix BioReactor 1 Inf 120 T 1200820 B121932 Influent 2.04 0.77 1241020-01 Hg ng/L

BioReactor 2 Eff 9.04 T 1200820 B121932 Ef fluent 0.41 0.15 1241020-05 Hg ng/L

BioReactor 2 Inf 21.1 T 1200820 B121932 Influent 2.04 0.77 1241020-03 Hg ng/L
Hg Blk BioReactor 1 Inf 0.32 T B 1200820 B121932 DIW 0.39 0.15 1241020-02 Hg ng/L
Hg Blk BioReactor 2 Eff 0.19 T B 1200820 B121932 DIW 0.41 0.15 1241020-06 Hg ng/L
Hg Blk BioReactor 2 Inf 0.30 T B 1200820 B121932 DIW 0.40 0.15 1241020-04 Hg ng/L

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: B121932

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

1631 Lab Matrix: Water

Sample Certified Reference Material (1241042, NIST 1641d 1000x dilution) B121932-SRM1 15.68 106% ng/L 0-200 Hg 16.68
Matrix Spike (1241009-02) B121932-MS2 42.00 95% ng/L 71-125 Hg 44.97

5.10
Matrix Spike Duplicate (1241009-02) B121932-MSD2 42.33 91% ng/L 71-125 243% Hg 43.72

5.10
Matrix Spike (1241020-03) B121932-MS1 408.2 107% ng/L 71-125 Hg 456.5

21.10
Matrix Spike Duplicate (1241020-03) B121932-MSD1 408.2 105% ng/L 71-125 241% Hg 450.1

21.10

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: B121932
Method: EPA

1631 Matrix: Water Analyte: Hg Result Units Sample B121932-BLK1 ng/L 0.10 B121932-BLK2 ng/L 0.09 B121932-BLK3 ng/L 0.05 B121932-BLK4 ng/L 0.07 MDL: 0.15 Average: 0.08 Standard Deviation: 0.02 Limit: 0.10 Limit: 0.50 MRL: 0.39

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: 1200820 Method: EPA 1631 Instrument: THG-05 Date: 10/24/2012 Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg REC & Limits Result True Value Lab ID Units 1200820-IBL1 2.23 pg of Hg 1200820-IBL2 9.44 pg of Hg 1200820-IBL3 4.36 pg of Hg 1200820-IBL4 5.18 pg of Hg 1200820-CAL1 10.00 9.04 pg of Hg 90% 1200820-CAL2 25.00 25.20 pg of Hg 101% 1200820-CAL3 100.0 102.1 pg of Hg 102% 1200820-CAL4 500.0 508.0 pg of Hg 102% 1200820-CAL5 2500 2590 pg of Hg 104% 1200820-CAL6 10000 10280 pg of Hg 103% 1200820-ICV1 1568 1668 pg of Hg 106% 85-115 1200820-CCB1 1 1.1 pg of Hg 1200820-CCV1 500.0 518.0 pg of Hg 104% 77-123 1200820-CCB2 6.66 pg of Hg 1200820-CCB3 4.59 pg of Hg 1200820-CCB4 5.64 pg of Hg 1200820-CCV2 500.0 534.9 pg of Hg 107% 77-123 1200820-CCB5 8.92 pg of Hg 1200820-CCV3 500.0 533.5 pg of Hg 107% 77-123 1200820-CCB6 7.86 pg of Hg 1200820-CCV4 500.0 533.8 pg of Hg 107% 77-123 1200820-CCB7 8.27 pg of Hg 1200820-CCV5 500.0 513.9 pg of Hg 103% 77-123 1200820-CCB8 5.16 pg of Hg 1200820-CCV6 500.0 502.9 pg of Hg 101% 77-123 1200820-CCB9 4.37 pg of Hg 1200820-CCV7 500.0 493.1 pg of Hg 99% 77-123 1200820-CCBA 6.14 pg of Hg 1200820-CCV8 500.0 502.6 pg of Hg 101% 77-123 1200820-CCBB 4.20 pg of Hg 1200820-CCV9 500.0 515.6 pg of Hg 103% 77-123 1200820-CCBC 4.32 pg of Hg 1200820-CCVA 500.0 497.8 pg of Hg 100% 77-123 1200820-CCBD 5.84 pg of Hg 1200820-CCVB 500.0 500.7 pg of Hg 100% 77-123 1200820-CCBE 4.62 pg of Hg 1200820-ICV2 1568 1592 pg of Hg 102% 85-115 1200820-CCVC 500.0 505.8 pg of Hg 101% 77-123 1200820-CCBF 3.85 pg of Hg 1200820-CCVD 500.0 514.6 pg of Hg 103% 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



# Instrument Calibration

Sequence: 1200820 Method: EPA 1631 Instrument: THG-05 Date: 10/24/2012 Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg REC & Limits Result True Value Lab ID Units 1200820-CCBG 3.91 pg of Hg 1200820-CCVE 500.0 524.0 pg of Hg 105% 77-123 1200820-CCBH 4.35 pg of Hg 1200820-CCVF 500.0 521.1 pg of Hg 104% 77-123 1200820-CCBI 3.74 pg of Hg 1200820-CCVG 500.0 513.9 pg of Hg 103% 77-123 1200820-CCBJ 3.71 pg of Hg 1200820-CCVH 500.0 511.0 pg of Hg 102% 77-123 1200820-CCBK 3.03 pg of 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 Containers

Lab ID: 1241020-01 Report Matrix: Influent Sample Type : Sample Received: 10/12/2012 Sample: BioReactor 1 Inf Collected: 10/10/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71666330 10 Cooler

none n/a 500 mL Bottle FLPE Hg-T

Lab ID: 1241020-02 Report Matrix: DIW Sample Type: Field Blank Received: 10/12/2012 Sample: Hg Blk BioReactor 1 Inf Collected: 10/10/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71666330 10 Cooler

none n/a 500 mL Bottle FLPE Hg-T

Lab ID: 1241020-03 Report Matrix: Influent Sample Type: QC Sample Received: 10/12/2012 Sample: BioReactor 2 Inf Collected: 10/10/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71666330 10 Cooler

none n/a 500 mL Bottle FLPE Hg-T

Lab ID: 1241020-04 Report Matrix: DIW Sample Type: Field Blank Received: 10/12/2012 Sample: Hg Blk BioReactor 2 Inf Collected: 10/10/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71666330 10 Cooler

none n/a 500 mL Bottle FLPE Hg-T

Lab ID: 1241020-05 Report Matrix: Effluent Sample Type: Sample Received: 10/12/2012 Sample: BioReactor 2 Eff Collected: 10/10/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71666330 10 Cooler

none n/a 500 mL Bottle FLPE Hg-T

Lab ID: 1241020-06 Report Matrix: DIW Sample Type: Field Blank Received: 10/12/2012 Sample: Hg Blk BioReactor 2 Eff Collected: 10/10/2012 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71666330 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: 535305194840 via FedEx Temperature: 1.0 °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: October 12, 2012 8:45

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