### 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: J11100039

**Lab Contact: Jason C Perkins**  

### Date: **10/27/2011 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.** 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 **2011021606 BELEWS 12-Oct-11 11:08 AM TO**  **FGD Purge Eff 2011021607 BELEWS 12-Oct-11 10:56 AM**  **TO EQ TANK EFF.**  **2011021608 BELEWS 12-Oct-11 10:29 AM TO**  **BIOREACTOR 1 INF. 2011021609 BELEWS 12-Oct-11 10:35 AM**  **TO BIOREACTOR 2 INF.**  **2011021610 BELEWS 12-Oct-11 10:41 AM TO**  **BIOREACTOR 2 EFF. 2011021611 BELEWS 12-Oct-11 10:22 AM**  **TO FILTER BLANK**  **2011021612 BELEWS 12-Oct-11 10:22 AM TO**  **Trip Blank 2011021613 BELEWS 12-Oct-11 10:29 AM**  **TO BIOREACTOR 1 INF.**  **2011021614 BELEWS 12-Oct-11 10:29 AM TO**  **HG BLANK BIOREACTOR 1 INF. 2011021615 BELEWS 12-Oct-11 10:35 AM**  **TO BIOREACTOR 2 INF.**  **2011021616 BELEWS 12-Oct-11 10:35 AM TO**  **Hg Blk BioReactor 2 Inf 2011021617 BELEWS 12-Oct-11 10:41 AM**  **TO BIOREACTOR 2 EFF.**  **2011021618 BELEWS 12-Oct-11 10:41 AM TO**  **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. The Vendor Laboratories have been qualified by the**  **Analytical Laboratory Yes**  **No**



# Technical Validation Review C hecklist:

**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:** 

### DataBase Administrator **Date:** 

### 10/27/2011 **Yes**

**Electronic Data Deliverable (EDD) Sent Separately**

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



### Order # J11100039

2011021606 **Collection Date: 12-Oct-11 11:08 AM** 

### Site: **FGD Purge Eff Matrix: OTHER** 

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst INORGANIC IONS BY IC **Bromide** 88 **mg/L EPA 300.0 25-Oct-11 07:45 JAHERMA**  **10** MERCURY (COLD VAPOR) IN WATER **Mercury (Hg)** 317 **ug/L EPA 245.1 21-Oct-11 09:04 AGIBBS**  **5**
TOTAL RECOVERABLE METALS BY ICP **Boron (B)** 182 **mg/L EPA 200.7 24-Oct-11 13:15 DJSULL1**  **0.5**
DISSOLVED METALS BY ICP-MS **Selenium (Se)** 1130 **ug/L EPA 200.8 19-Oct-11 12:01 KRICHAR**  **10**
TOTAL RECOVERABLE METALS BY ICP-MS **Arsenic (As)** 159 **ug/L EPA 200.8 19-Oct-11 12:25 KRICHAR**  **10 Chromium (Cr)**  228 **ug/L EPA 200.8**  **19-Oct-11 12:25 KRICHAR 10**  **Copper (Cu)** 126 **ug/L EPA 200.8**  **19-Oct-11 12:25 KRICHAR 10**  **Nickel (Ni)** 188 **ug/L EPA 200.8**  **19-Oct-11 12:25 KRICHAR 10**  **Selenium (Se)** 6080 **ug/L EPA 200.8**  **19-Oct-11 12:25 KRICHAR 20**  **Silver (Ag)** < 10 **ug/L EPA 200.8**  **19-Oct-11 12:25 KRICHAR 10**  **Zinc (Zn)** 228 **ug/L EPA 200.8**  **19-Oct-11 12:25 KRICHAR 20** 
SELENIUM SPECIATION **Vendor Parameter** Complete **V_AS&C**
TOTAL DISSOLVED SOLIDS **TDS** 18000 **mg/L SM2540C 19-Oct-11 13:25 TJA7067**  **200** 

### 2011021607 **Collection Date: 12-Oct-11 10:56 AM** 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY (COLD VAPOR) IN WATER **Mercury (Hg)** 199 **ug/L EPA 245.1 21-Oct-11 09:07 AGIBBS**  **2.5**
TOTAL RECOVERABLE METALS BY ICP **Boron (B)** 163 **mg/L EPA 200.7 24-Oct-11 13:19 DJSULL1**  **0.5**
DISSOLVED METALS BY ICP-MS **Selenium (Se)** 1150 **ug/L EPA 200.8 19-Oct-11 12:04 KRICHAR**  **10**

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



### Order # J11100039

2011021607 **Collection Date: 12-Oct-11 10:56 AM** 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst TOTAL RECOVERABLE METALS BY ICP-MS **Arsenic (As)** 113 **ug/L EPA 200.8 19-Oct-11 11:19 KRICHAR**  **10 Chromium (Cr)**  168 **ug/L EPA 200.8**  **19-Oct-11 11:19 KRICHAR 10**  **Copper (Cu)** 90.2 **ug/L EPA 200.8**  **19-Oct-11 11:19 KRICHAR 10**  **Nickel (Ni)** 142 **ug/L EPA 200.8**  **19-Oct-11 11:19 KRICHAR 10**  **Selenium (Se)** 4110 **ug/L EPA 200.8**  **19-Oct-11 11:19 KRICHAR 10**  **Silver (Ag)** < 10 **ug/L EPA 200.8**  **19-Oct-11 11:19 KRICHAR 10**  **Zinc (Zn)** 160 **ug/L EPA 200.8**  **19-Oct-11 11:19 KRICHAR 20**  

### 2011021608 **Collection Date: 12-Oct-11 10:29 AM** 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst TOTAL RECOVERABLE METALS BY ICP **Boron (B)** 152 **mg/L EPA 200.7 24-Oct-11 13:22 DJSULL1**  **0.5**
DISSOLVED METALS BY ICP-MS **Selenium (Se)** 1200 **ug/L EPA 200.8 19-Oct-11 12:07 KRICHAR**  **10**
TOTAL RECOVERABLE METALS BY ICP-MS **Arsenic (As)** < 10 **ug/L EPA 200.8 19-Oct-11 11:22 KRICHAR**  **10 Chromium (Cr)**  11.9 **ug/L EPA 200.8**  **19-Oct-11 11:22 KRICHAR 10**  **Copper (Cu)** < 10 **ug/L EPA 200.8**  **19-Oct-11 11:22 KRICHAR 10**  **Nickel (Ni)** 10.8 **ug/L EPA 200.8**  **19-Oct-11 11:22 KRICHAR 10**  **Selenium (Se)** 1240 **ug/L EPA 200.8**  **19-Oct-11 11:22 KRICHAR 10**  **Silver (Ag)** < 10 **ug/L EPA 200.8**  **19-Oct-11 11:22 KRICHAR 10**  **Zinc (Zn)** < 20 **ug/L EPA 200.8**  **19-Oct-11 11:22 KRICHAR 20** 
SELENIUM SPECIATION **Vendor Parameter** Complete **V_AS&C** 

### 2011021609 **Collection Date: 12-Oct-11 10:35 AM** 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst TOTAL RECOVERABLE METALS BY ICP **Boron (B)** 154 **mg/L EPA 200.7 24-Oct-11 13:26 DJSULL1**  **0.5**

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



### Order # J11100039

2011021609 **Collection Date: 12-Oct-11 10:35 AM** 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst TOTAL RECOVERABLE METALS BY ICP-MS **Arsenic (As)** < 10 **ug/L EPA 200.8 19-Oct-11 11:25 KRICHAR**  **10 Chromium (Cr)**  < 10 **ug/L EPA 200.8**  **19-Oct-11 11:25 KRICHAR 10**  **Copper (Cu)** < 10 **ug/L EPA 200.8**  **19-Oct-11 11:25 KRICHAR 10**  **Nickel (Ni)** 15.9 **ug/L EPA 200.8**  **19-Oct-11 11:25 KRICHAR 10**  **Selenium (Se)** 191 **ug/L EPA 200.8**  **19-Oct-11 11:25 KRICHAR 10**  **Silver (Ag)** < 10 **ug/L EPA 200.8**  **19-Oct-11 11:25 KRICHAR 10**  **Zinc (Zn)** < 20 **ug/L EPA 200.8**  **19-Oct-11 11:25 KRICHAR 20**  

### 2011021610 **Collection Date: 12-Oct-11 10:41 AM** 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst INORGANIC IONS BY IC **Bromide** 78 **mg/L EPA 300.0 25-Oct-11 08:00 JAHERMA**  **10** MERCURY (COLD VAPOR) IN WATER **Mercury (Hg)** < 1 **ug/L EPA 245.1 21-Oct-11 09:09 AGIBBS**  **1**
TOTAL RECOVERABLE METALS BY ICP **Boron (B)** 153 **mg/L EPA 200.7 24-Oct-11 13:30 DJSULL1**  **0.5**
TOTAL RECOVERABLE METALS BY ICP-MS **Arsenic (As)** < 5 **ug/L EPA 200.8 19-Oct-11 11:28 KRICHAR**  **5 Chromium (Cr)**  < 5 **ug/L EPA 200.8**  **19-Oct-11 11:28 KRICHAR 5**  **Copper (Cu)** < 5 **ug/L EPA 200.8**  **19-Oct-11 11:28 KRICHAR 5**  **Nickel (Ni)** < 5 **ug/L EPA 200.8**  **19-Oct-11 11:28 KRICHAR 5**  **Selenium (Se)** 14.2 **ug/L EPA 200.8**  **19-Oct-11 11:28 KRICHAR 5**  **Silver (Ag)** < 5 **ug/L EPA 200.8**  **19-Oct-11 11:28 KRICHAR 5**  **Zinc (Zn)** < 10 **ug/L EPA 200.8**  **19-Oct-11 11:28 KRICHAR 10** 
SELENIUM SPECIATION **Vendor Parameter** Complete **V_AS&C** 

### 2011021611 **Collection Date: 12-Oct-11 10:22 AM** 

### Site: **FILTER BLANK Matrix: OTHER** 

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DISSOLVED METALS BY ICP-MS **Selenium (Se)** 1.17 **ug/L EPA 200.8 19-Oct-11 10:42 KRICHAR**  **1**

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



### Order # J11100039

2011021612 **Collection Date: 12-Oct-11 10:22 AM** 

### Site: **Trip Blank Matrix: OTHER** 

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst TOTAL RECOVERABLE METALS BY ICP **Boron (B)** < 0.05 **mg/L EPA 200.7 24-Oct-11 12:59 DJSULL1**  **0.05**
TOTAL RECOVERABLE METALS BY ICP-MS **Arsenic (As)** < 1 **ug/L EPA 200.8 19-Oct-11 10:30 KRICHAR**  **1 Chromium (Cr)**  < 1 **ug/L EPA 200.8**  **19-Oct-11 10:30 KRICHAR 1**  **Copper (Cu)** < 1 **ug/L EPA 200.8**  **19-Oct-11 10:30 KRICHAR 1**  **Nickel (Ni)** < 1 **ug/L EPA 200.8**  **19-Oct-11 10:30 KRICHAR 1**  **Selenium (Se)** < 1 **ug/L EPA 200.8**  **19-Oct-11 10:30 KRICHAR 1**  **Silver (Ag)** < 1 **ug/L EPA 200.8**  **19-Oct-11 10:30 KRICHAR 1**  **Zinc (Zn)** < 2 **ug/L EPA 200.8**  **19-Oct-11 10:30 KRICHAR 2** 
SELENIUM SPECIATION **Vendor Parameter** Complete **V_AS&C** 

### 2011021613 **Collection Date: 12-Oct-11 10:29 AM** 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 **Vendor Parameter** Complete **V_BRAND** 

### 2011021614 **Collection Date: 12-Oct-11 10:29 AM** 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 **Vendor Parameter** Complete **V_BRAND** 

### 2011021615 **Collection Date: 12-Oct-11 10:35 AM** 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 **Vendor Parameter** Complete **V_BRAND**

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



### Order # J11100039

2011021616 **Collection Date: 12-Oct-11 10:35 AM** 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 **Vendor Parameter** Complete **V_BRAND** 

### 2011021617 **Collection Date: 12-Oct-11 10:41 AM** 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 **Vendor Parameter** Complete **V_BRAND** 

### 2011021618 **Collection Date: 12-Oct-11 10:41 AM** 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 **Vendor Parameter** Complete **V_BRAND**

## October 21 , 201 1

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 # J11100 039 )

Dear Mr. Perkins, Attached is the report associated with four (4 ) aqueous samples submitted for selenium speciation analysis on October 1 3 , 2011. The samples were received on October 1 4, 2011 in a sealed cooler at0. 7 ° C. Selenium speciation analysis was performed via ion chromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICP-DRC-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,

Ben Wozniak Project Manager 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 # J11100 039)

October 21 , 2011

1. Sample Reception Four (4 ) aqueous samples in125mL HDPE bottles (provided by Applied Speciation and Consulting) were submitted for selenium speciation analysi s on October 1 3 , 2011 . The samples were received on October 1 4 , 2011 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-violet radiation. Upon reception, the samples were designated discrete sample identifiers. An aliquot of each sample was filtered (0.45μm) and these filtrates were 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 dynamic reaction cell mass spectrometry (IC-ICP-DRC-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-DRC

- 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 the samples 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-DRC

- MS All samples for selenium speciation analysis were analyzed by ion chromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICP-DRC-MS) on October 1 7 -18 , 2011 . 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 (DRC) containing a specific reactive 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 with the following exceptions: The recoveries associated with the matrix spike (MS) and matrix spike duplicate (MSD) performed on the sample identified as Batch QC were below the established control limit of 75% for selenocyanate (54.4 % and 51.2 %, respectively). The MS and MSD also included selenite in the spiking solution which yielded elevated recoveries (1 39.1% and 143.3 %, respectively)

. The low recoveries for selenocyanate correlate with the elevated recoveries of selenite suggesting that the sample matrix induces species conversion. The fact that no species conversion was observed in the ICV or CCVs, which contain both selenite and selenocyanate, demonstrates that the applied method stabilizes these selenium species in solution. Since the conversion of selenocyanate to selenite in the MS and MSD is a function of the sample matrix and the recoveries confirm a mass balance, no corrective action was required. The reported results are deemed represe ntative of the supplied samples and suggest that selenocyanate is not stable in the spiked sample matrix.

## 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,

Ben Wozniak Project Manager Applied Speciation and Consulting, LLC

### Sample Results
Sample ID Se(IV) Se(VI) SeCN MeSe(IV) SeMe Unknown Se Species (n) FGD Purge Eff 14.9 1030 ND (<1.3) ND (<1.5) ND (<1.5) 0 (0) BioReactor 1 Inf 16.0 1070 ND (<0.34) 1.00 ND (<0.37) 0 (0) BioReactor 2 Eff 1.61 6.40 ND (<0.34) ND (<0.37) ND (<0.37) 0 (0) Metals Trip Blk ND (<0.097) ND (<0.055) ND (<0.067) ND (<0.073) ND (<0.073) 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: Ben Wozniak Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS (Bi-Monthly Sampling)

Contact: Jay Perkins
Date: October 21, 2011 LIMS #J11100039

### 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 0.010 0.097 0.48 1.9 Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.006 0.055 0.28 1.1 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.007 0.067 0.34 1.3 MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.007 0.073 0.37 1.5 SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.007 0.073 0.37 1.5 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 11.24 117.5 Se(VI) LCS 9.48 10.01 105.6 SeCN LCS 8.92 9.239 103.6 MeSe(IV) LCS 6.47 5.847 90.4 SeMe LCS 9.32 9.200 98.7 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS (Bi-Monthly Sampling)

Contact: Jay Perkins LIMS #J11100039 Date: October 21, 2011 Report Generated by: Ben Wozniak

### Quality Control Summary - Matrix Duplicates Analyte (μg/L) Sample ID Rep 1 Rep 2 Mean RPD Se(IV) Batch QC* 12.0 11.9 11.9 0.8 Se(VI) Batch QC* 973.3 1020 996.7 4.7 SeCN Batch QC* ND (<1.3) ND (<1.3) NC NC MeSe(IV) Batch QC* ND (<1.5) ND (<1.5) NC NC SeMe Batch QC* ND (<1.5) ND (<1.5) NC NC ND = Not detected at the applied dilution NC = Value was not calculated due to one or more concentrations below the eMDL * Batch QC performed on sample from LIMS # J11100235
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 1559 139.1** 1112 1606 143.3** 3.0 Se(VI) Batch QC* 1009 2025 101.9 1009 2077 107.1 2.6 SeCN Batch QC* 915.0 497.9 54.4** 915.0 468.2 51.2** 6.1 * Batch QC performed on sample from LIMS # J11100235 ** The recovery is outside the established control limits of 75-125%; please see narrative Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews - FGD WWTS (Bi-Monthly Sampling)

Contact: Jay Perkins LIMS #J11100039 Date: October 21, 2011 Report Generated by: Ben Wozniak3958 6 th Ave NW • Seattle, WA 98107 • T: 206-632-6206 • F: 206-632-6017 • www.brooksrand.com • brl@brooksrand.com 

### October 26, 2011
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-HV1101 Client Project: J11100039 Dear Mr. Perkins, On October 14, 2011, Brooks Rand Labs (BRL) received three (3) flue gas desulfurization(FGD) wastewater samples and three (3) corresponding blank samples. Samples were loggedin for total mercury (Hg) 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. It should be noted that a matrix spike/matrix spike duplicate (MS/MSD) set was not analyzed on one of the samples from this work order. A similar sample from a different work order had a MS/MSD set analyzed and that has been reported. The sample Hg Blk BioReactor 2 Eff (1142048-06) was identified as a field blank, but had a detectable result that was comparable to the associated sample. It was also noticed that when preserved, Hg Blk BioReactor 2 Eff (1142048-06) reacted similarly to a sample and not a field blank. 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,

Lydia Greaves Project Manager lydia@brooksran.comProject ID: DUK-HV1101

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-HV1101

PM: Tiffany Stilwater Client PM: Jay Perkins Client PO: 141391



# Sample Information

Report Matrix Type Received Sampled Sample Lab ID 1142048-01 BioReactor 1 Inf 10/12/2011 10/14/2011 Sample Influent 1142048-02 Hg Blk BioReactor 1 Inf 10/12/2011 10/14/2011 Field Blank DIW 1142048-03 BioReactor 2 Inf 10/12/2011 10/14/2011 Sample Influent 1142048-04 Hg Blk BioReactor 2 Inf 10/12/2011 10/14/2011 Field Blank DIW 1142048-05 BioReactor 2 Eff 10/12/2011 10/14/2011 Sample Effluent 1142048-06 Hg Blk Bio Reactor 2 Eff 10/12/2011 10/14/2011 Field Blank DIW 

# Batch Summary

Analyte Prepared Analyzed Sequence Batch Lab Matrix Method B111723 10/21/2011 10/25/2011 1100738 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-HV1101

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 41700 T 1100738 B111723 Influent 204 76.5 1142048-01 Hg

BioReactor 2 Eff ng/L 412 T 1100738 B111723 Effluent 8.08 3.03 1142048-05 Hg

BioReactor 2 Inf ng/L 2460 T 1100738 B111723 Influent 40.8 15.3 1142048-03 Hg
Hg Blk Bio Reactor 2 Eff ng/L 527 T 1100738 B111723 DIW 4.04 1.52 1142048-06 Hg
Hg Blk BioReactor 1 Inf ng/L 0.38 T B 1100738 B111723 DIW 0.41 0.15 1142048-02 Hg
Hg Blk BioReactor 2 Inf ng/L 0.15 T U 1100738 B111723 DIW 0.41 0.15 1142048-04 Hg

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: DUK-HV1101

PM: Tiffany Stilwater Client PM: Jay Perkins Client PO: 141391



# Accuracy & Precision Summary

Batch: B111723

Analyte Result Units Native Spike REC & Limits RPD & Limits Method: EPA 1631 Lab Matrix: Water

Sample Certified Reference Material (1140052, THg ICV 1641d) B111723-SRM1 15.68 92% ng/L 85-115 Hg 14.44
Matrix Spike (1143014-01) B111723-MS2 2020 102% ng/L 71-125 Hg 2506

436.0
Matrix Spike Duplicate (1143014-01) B111723-MSD2 2020 101% ng/L 71-125 241% Hg 2473

436.0



# Method Blanks & Reporting Limits

Batch: B111723
Method: EPA 1631 Matrix: Water Analyte: Hg Result Units Sample B111723-BLK1 ng/L 0.04 B111723-BLK2 ng/L 0.0008 B111723-BLK3 ng/L 0.05 B111723-BLK4 ng/L 0.02 MDL: 0.15 Average: 0.03 Standard Deviation: 0.02 Limit: 0.10 Limit: 0.50 MRL: 0.41

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: DUK-HV1101

PM: Tiffany Stilwater Client PM: Jay Perkins Client PO: 141391



# Instrument Calibration

Sequence: 1100738 Method: EPA 1631 Instrument: THG-05 Date: 10/25/2011 Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg REC & Limits Result True Value Lab ID Units 1100738-IBL1 8.42 pg of Hg 1100738-IBL2 8.90 pg of Hg 1100738-IBL3 7.23 pg of Hg 1100738-IBL4 8.50 pg of Hg 1100738-CAL1 25.00 24.03 pg of Hg 96% 1100738-CAL2 100.0 99.48 pg of Hg 99% 1100738-CAL3 500.0 511.0 pg of Hg 102% 1100738-CAL4 2500 2549 pg of Hg 102% 1100738-CAL5 10000 10050 pg of Hg 100% 1100738-ICV1 1568 1444 pg of Hg 92% 85-115 1100738-CCB1 12.1 pg of Hg 1100738-CCV1 500.0 514.6 pg of Hg 103% 77-123 1100738-CCB2 8.55 pg of Hg 1100738-CCV2 500.0 497.9 pg of Hg 100% 77-123 1100738-CCB3 37.1 pg of Hg 1100738-CCV3 500.0 512.1 pg of Hg 102% 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-HV1101

PM: Tiffany Stilwater Client PM: Jay Perkins Client PO: 141391



# Sample Containers

Lab ID: 1142048-01 Report Matrix: Influent Sample Type: Sample Received: 10/14/2011 Sample: BioReactor 1 Inf Collected: 10/12/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71443390 30 Cooler

none n/a 250mL Bottle FLPE Hg-T
B 71443390 30 Cooler

none n/a 250 mL EXTRA_VOL

Lab ID: 1142048-02 Report Matrix: DIW Sample Type: Field Blank Received: 10/14/2011 Sample: Hg Blk BioReactor 1 Inf Collected: 10/12/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71443390 30 Cooler

none n/a 250mL Bottle FLPE Hg-T
B 71443390 30 Cooler

none n/a 250 mL EXTRA_VOL

Lab ID: 1142048-03 Report Matrix: Influent Sample Type: Sample Received: 10/14/2011 Sample: BioReactor 2 Inf Collected: 10/12/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71443390 30 Cooler

none n/a 250mL Bottle FLPE Hg-T
B 71443390 30 Cooler

none n/a 250 mL EXTRA_VOL

Lab ID: 1142048-04 Report Matrix: DIW Sample Type: Field Blank Received: 10/14/2011 Sample: Hg Blk BioReactor 2 Inf Collected: 10/12/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71443390 30 Cooler

none n/a 250mL Bottle FLPE Hg-T
B 71443390 30 Cooler

none n/a 250 mL EXTRA_VOL

Lab ID: 1142048-05 Report Matrix: Effluent Sample Type: Sample Received: 10/14/2011 Sample: BioReactor 2 Eff Collected: 10/12/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71443390 30 Cooler

none n/a 250mL Bottle FLPE Hg-T
B 71443390 30 Cooler

none n/a 250 mL EXTRA_VOL

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.comProject ID: DUK-HV1101

PM: Tiffany Stilwater Client PM: Jay Perkins Client PO: 141391



# Sample Containers

Lab ID: 1142048-06 Report Matrix: DIW Sample Type: Field Blank Received: 10/14/2011 Sample: Hg Blk Bio Reactor 2 Eff Collected: 10/12/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71443390 30 Cooler

none n/a 250mL Bottle FLPE Hg-T
B 71443390 30 Cooler

none n/a 250 mL EXTRA_VOL



# Shipping Containers

Cooler Tracking No: 472679664810 via FedEx Temperature: 3.6 °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 14, 2011 9:00

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