### 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: J11110301

Lab Contact: Jason C Perkins 

### Date: 12/6/2011 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 2011024807 BELEWS 12-Nov-11 8:20 AM W. B. WORKMAN FGD Purge Eff 2011024809 BELEWS 12-Nov-11 8:10 AM W. B. WORKMAN BIOREACTOR 1 INF. 2011024819 BELEWS 12-Nov-11 8:10 AM W. B. WORKMAN BIOREACTOR 1 INF. BLANK 2011024820 BELEWS 12-Nov-11 8:00 AM W. B. WORKMAN BIOREACTOR 2 EFF. 2011024821 BELEWS 12-Nov-11 8:00 AM W. B. WORKMAN BIOREACTOR 2 EFF. BLANK 2011024822 BELEWS 14-Nov-11 8:30 AM W. B. WORKMAN FILTER BLANK 2011024823 BELEWS 12-Nov-11 8:35 AM W. B. WORKMAN Trip Blank 2011024826 BELEWS 12-Nov-11 10:16 AM W. B. WORKMAN FILTER PRESS CAKE 8 Total Samples

### COC and .pdf report are in agreement with sample totals and analyses (compliance programs and procedures). All Results are less than the laboratory reporting limits. All laboratory QA/QC requirements are acceptable. 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: 

### 12/6/2011 Yes

Electronic Data Deliverable (EDD) Sent Separately

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

## Order # J11110301

2011024807 Collection Date: 12-Nov-11 8:20 AM 

### Site: FGD Purge Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst ALKALINITY (FIXED END POINT 4.5) Vendor Parameter Complete V_PRISM Carbonate, Bicarbonate, and Hydroxide Alkalinity Carbonate (CO3) Complete V_PRISM Hydroxide (OH) Complete V_PRISM Bicarbonate (HCO3) Complete V_PRISM NITRITE + NITRATE (COLORIMETRIC) Nitrite + Nitrate (Colorimetric) 14 mg-N/L EPA 353.2 16-Nov-11 14:19 BGN9034 0.25 INORGANIC IONS BY IC Bromide 86 mg/L EPA 300.0 16-Nov-11 22:13 JAHERMA 5 Chloride 5800 mg/L EPA 300.0 16-Nov-11 22:13 JAHERMA 100 Sulfate 1400 mg/L EPA 300.0 16-Nov-11 22:13 JAHERMA 100 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 196 ug/L EPA 245.1 02-Dec-11 09:01 AGIBBS 5 Mercury Dissolved (cold vapor) in Water (Filtered) Mercury (Hg) < 2.5 ug/L EPA 245.1 02-Dec-11 09:29 AGIBBS 2.5 TOTAL RECOVERABLE METALS BY ICP Boron (B) 161 mg/L EPA 200.7 29-Nov-11 11:34 MHH7131 0.5 Calcium (Ca) 3330 mg/L EPA 200.7 29-Nov-11 11:34 MHH7131 0.1 Lithium (Li) 0.133 mg/L EPA 200.7 29-Nov-11 11:34 MHH7131 0.05 Magnesium (Mg) 795 mg/L EPA 200.7 29-Nov-11 11:34 MHH7131 0.05 Potassium (K) 49.5 mg/L EPA 200.7 29-Nov-11 11:34 MHH7131 1 Sodium (Na) 42.3 mg/L EPA 200.7 29-Nov-11 11:34 MHH7131 0.5 DISSOLVED METALS BY ICP-MS Selenium (Se) 251 ug/L EPA 200.8 22-Nov-11 11:27 KRICHAR 10 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 128 ug/L EPA 200.8 22-Nov-11 11:06 KRICHAR 10 Cadmium (Cd) < 10 ug/L EPA 200.8 22-Nov-11 11:06 KRICHAR 10 Chromium (Cr) 175 ug/L EPA 200.8 22-Nov-11 11:06 KRICHAR 10 Copper (Cu) 93.5 ug/L EPA 200.8 22-Nov-11 11:06 KRICHAR 10 Nickel (Ni) 156 ug/L EPA 200.8 22-Nov-11 11:06 KRICHAR 10 Selenium (Se) 4010 ug/L EPA 200.8 22-Nov-11 11:06 KRICHAR 10 Silver (Ag) < 10 ug/L EPA 200.8 22-Nov-11 11:06 KRICHAR 10 Zinc (Zn) 166 ug/L EPA 200.8 22-Nov-11 11:06 KRICHAR 20

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

## Order # J11110301

2011024807 Collection Date: 12-Nov-11 8:20 AM 

### Site: FGD Purge Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst SELENIUM SPECIATION Vendor Parameter Complete V_AS&C TOTAL DISSOLVED SOLIDS TDS 15000 mg/L SM2540C 15-Nov-11 14:50 TJA7067 200 TOTAL SUSPENDED SOLIDS TSS 2500 mg/L SM2540D 17-Nov-11 12:11 TJA7067 250 

### 2011024809 Collection Date: 12-Nov-11 8:10 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst ALKALINITY (FIXED END POINT 4.5) Vendor Parameter Complete V_PRISM Carbonate, Bicarbonate, and Hydroxide Alkalinity Bicarbonate (HCO3) Complete V_PRISM Hydroxide (OH) Complete V_PRISM Carbonate (CO3) Complete V_PRISM NITRITE + NITRATE (COLORIMETRIC) Nitrite + Nitrate (Colorimetric) 15 mg-N/L EPA 353.2 16-Nov-11 14:21 BGN9034 0.25 INORGANIC IONS BY IC Bromide 87 mg/L EPA 300.0 16-Nov-11 22:29 JAHERMA 5 Chloride 6000 mg/L EPA 300.0 16-Nov-11 22:29 JAHERMA 100 Sulfate 1400 mg/L EPA 300.0 16-Nov-11 22:29 JAHERMA 100 MERCURY 1631 Vendor Parameter Complete V_BRAND MERCURY (COLD VAPOR) IN WATER Mercury (Hg) < 2.5 ug/L EPA 245.1 02-Dec-11 09:03 AGIBBS 2.5 TOTAL RECOVERABLE METALS BY ICP Boron (B) 157 mg/L EPA 200.7 29-Nov-11 11:38 MHH7131 0.5 Calcium (Ca) 2710 mg/L EPA 200.7 29-Nov-11 11:38 MHH7131 0.1 Lithium (Li) < 0.05 mg/L EPA 200.7 29-Nov-11 11:38 MHH7131 0.05 Magnesium (Mg) 722 mg/L EPA 200.7 29-Nov-11 11:38 MHH7131 0.05 Potassium (K) 21.3 mg/L EPA 200.7 29-Nov-11 11:38 MHH7131 1 Sodium (Na) 40.5 mg/L EPA 200.7 29-Nov-11 11:38 MHH7131 0.5

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

## Order # J11110301

2011024809 Collection Date: 12-Nov-11 8:10 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 22-Nov-11 11:09 KRICHAR 10 Cadmium (Cd) < 10 ug/L EPA 200.8 22-Nov-11 11:09 KRICHAR 10 Chromium (Cr) < 10 ug/L EPA 200.8 22-Nov-11 11:09 KRICHAR 10 Copper (Cu) < 10 ug/L EPA 200.8 22-Nov-11 11:09 KRICHAR 10 Nickel (Ni) 19.8 ug/L EPA 200.8 22-Nov-11 11:09 KRICHAR 10 Selenium (Se) 137 ug/L EPA 200.8 22-Nov-11 11:09 KRICHAR 10 Silver (Ag) < 10 ug/L EPA 200.8 22-Nov-11 11:09 KRICHAR 10 Zinc (Zn) < 20 ug/L EPA 200.8 22-Nov-11 11:09 KRICHAR 20 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011024819 Collection Date: 12-Nov-11 8:10 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND 

### 2011024820 Collection Date: 12-Nov-11 8:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst ALKALINITY (FIXED END POINT 4.5) Vendor Parameter Complete V_PRISM Carbonate, Bicarbonate, and Hydroxide Alkalinity Bicarbonate (HCO3) Complete V_PRISM Hydroxide (OH) Complete V_PRISM Carbonate (CO3) Complete V_PRISM NITRITE + NITRATE (COLORIMETRIC) Nitrite + Nitrate (Colorimetric) < 0.01 mg-N/L EPA 353.2 16-Nov-11 14:23 BGN9034 0.01 INORGANIC IONS BY IC Bromide 88 mg/L EPA 300.0 16-Nov-11 22:45 JAHERMA 5 Chloride 6300 mg/L EPA 300.0 16-Nov-11 22:45 JAHERMA 100 Sulfate 1500 mg/L EPA 300.0 16-Nov-11 22:45 JAHERMA 100 MERCURY 1631 Vendor Parameter Complete V_BRAND

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

## Order # J11110301

2011024820 Collection Date: 12-Nov-11 8:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst MERCURY (COLD VAPOR) IN WATER Mercury (Hg) < 1 ug/L EPA 245.1 02-Dec-11 09:05 AGIBBS 1 TOTAL RECOVERABLE METALS BY ICP Boron (B) 155 mg/L EPA 200.7 29-Nov-11 11:42 MHH7131 0.5 Calcium (Ca) 2880 mg/L EPA 200.7 29-Nov-11 11:42 MHH7131 0.1 Lithium (Li) < 0.05 mg/L EPA 200.7 29-Nov-11 11:42 MHH7131 0.05 Magnesium (Mg) 722 mg/L EPA 200.7 29-Nov-11 11:42 MHH7131 0.05 Potassium (K) 26.2 mg/L EPA 200.7 29-Nov-11 11:42 MHH7131 1 Sodium (Na) 41.8 mg/L EPA 200.7 29-Nov-11 11:42 MHH7131 0.5 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 5 ug/L EPA 200.8 22-Nov-11 11:12 KRICHAR 5 Cadmium (Cd) < 5 ug/L EPA 200.8 22-Nov-11 11:12 KRICHAR 5 Chromium (Cr) < 5 ug/L EPA 200.8 22-Nov-11 11:12 KRICHAR 5 Copper (Cu) < 5 ug/L EPA 200.8 22-Nov-11 11:12 KRICHAR 5 Nickel (Ni) < 5 ug/L EPA 200.8 22-Nov-11 11:12 KRICHAR 5 Selenium (Se) < 5 ug/L EPA 200.8 22-Nov-11 11:12 KRICHAR 5 Silver (Ag) 5.74 ug/L EPA 200.8 22-Nov-11 11:12 KRICHAR 5 Zinc (Zn) < 10 ug/L EPA 200.8 22-Nov-11 11:12 KRICHAR 10 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011024821 Collection Date: 12-Nov-11 8:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND 

### 2011024822 Collection Date: 14-Nov-11 8:30 AM 

### Site: FILTER BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst DISSOLVED METALS BY ICP-MS Selenium (Se) < 1 ug/L EPA 200.8 22-Nov-11 10:48 KRICHAR 1

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

## Order # J11110301

2011024823 Collection Date: 12-Nov-11 8:35 AM 

### Site: Trip Blank Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst TOTAL RECOVERABLE METALS BY ICP Boron (B) < 0.05 mg/L EPA 200.7 29-Nov-11 11:17 MHH7131 0.05 Calcium (Ca) 0.014 mg/L EPA 200.7 29-Nov-11 11:17 MHH7131 0.01 Lithium (Li) < 0.005 mg/L EPA 200.7 29-Nov-11 11:17 MHH7131 0.005 Magnesium (Mg) < 0.005 mg/L EPA 200.7 29-Nov-11 11:17 MHH7131 0.005 Potassium (K) < 0.1 mg/L EPA 200.7 29-Nov-11 11:17 MHH7131 0.1 Sodium (Na) < 0.05 mg/L EPA 200.7 29-Nov-11 11:17 MHH7131 0.05 TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 1 ug/L EPA 200.8 22-Nov-11 10:39 KRICHAR 1 Cadmium (Cd) < 1 ug/L EPA 200.8 22-Nov-11 10:39 KRICHAR 1 Chromium (Cr) < 1 ug/L EPA 200.8 22-Nov-11 10:39 KRICHAR 1 Copper (Cu) < 1 ug/L EPA 200.8 22-Nov-11 10:39 KRICHAR 1 Nickel (Ni) < 1 ug/L EPA 200.8 22-Nov-11 10:39 KRICHAR 1 Selenium (Se) < 1 ug/L EPA 200.8 22-Nov-11 10:39 KRICHAR 1 Silver (Ag) < 1 ug/L EPA 200.8 22-Nov-11 10:39 KRICHAR 1 Zinc (Zn) < 2 ug/L EPA 200.8 22-Nov-11 10:39 KRICHAR 2 SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011024826 Collection Date: 12-Nov-11 10:16 AM 

### Site: FILTER PRESS CAKE Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sam p le #:

Analyst TCLP LEACHATE Vendor Parameter Complete V_PACE

## November 20 , 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: HAP S/MACT Testing Belews Creek (LIMS # J111 10 301 )

Dear Mr. Perkins, Attached is the report associated with four (4 ) aqueous samples submitted for selenium speciation analysis on November 1 4 , 2011. The samples were received in a sealed cooler at- 0. 1 ° C on November 15, 2011. Selenium speciation analysis was performed via ionchromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICPDRC-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: HAP S/MACT Testing Belews Creek (LIMS # J111 10 301 )

November 20 , 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 November 14 , 2011 . The samples were received on November 1 5 , 2011 in a sealed container at -0. 1° C. The samples were received in a laminar flow clean hood, void of trace metals contamination and ultra-violet radiation, and 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 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 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-DRC

- MS Eachsample for selenium speciation analysis w as analyzed by ion chromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICP-DRC-MS) on November 1 5 , 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 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.

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 157 72.5 ND (<3.9) ND (<4.6) ND (<4.6) 11.4 (2) BioReactor 1 Inf 60.8 58.0 ND (<1.0) 3.0 ND (<1.1) 2.2 (2) BioRector 2 Eff ND (<1.1) ND (<1.4) ND (<1.0) ND (<1.1) ND (<1.1) 0 (0) Metals Trip Blk ND (<0.21) ND (<0.28) ND (<0.20) ND (<0.23) ND (<0.23) 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: HAPS/MACT Testing Belews Creek

Contact: Jay Perkins
Date: November 20, 2011 LIMS #J11110301

### 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 0.021 0.21 1.1 4.3 Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.028 0.28 1.4 5.5 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.020 0.20 1.0 3.9 MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.023 0.23 1.1 4.6 SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.023 0.23 1.1 4.6 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 9.80 102.4 Se(VI) LCS 9.48 10.00 105.5 SeCN LCS 8.92 9.66 108.3 MeSe(IV) LCS 6.47 6.55 101.3 SeMe LCS 9.32 9.76 104.7 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: HAPS/MACT Testing Belews Creek

Contact: Jay Perkins LIMS #J11110301 Date: November 20, 2011 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 (<1.1) ND (<1.1) NC NC Se(VI) Batch QC ND (<1.4) ND (<1.4) NC NC SeCN Batch QC ND (<1.0) ND (<1.0) NC NC MeSe(IV) Batch QC ND (<1.1) ND (<1.1) NC NC SeMe Batch QC ND (<1.1) ND (<1.1) 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 278.0 259.2 93.2 278.0 251.5 90.5 3.0 Se(VI) Batch QC 252.3 245.1 97.1 252.3 241.5 95.7 1.5 SeCN Batch QC 228.8 212.2 92.8 228.8 211.3 92.4 0.4 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: HAPS/MACT Testing Belews Creek

Contact: Jay Perkins LIMS #J11110301 Date: November 20, 2011 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 

## November 22, 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: J11110301 Dear Mr. Perkins, On November 15, 2011, Brooks Rand Labs (BRL) received two (2) wastewater samples and two (2) corresponding field blanks. Samples were logged-in 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. The concentration of sample BioReactor 1 Inf (1147018-01) was not detectable while the associated field blank BioReactor 1 Inf Hg Blk (1147018-02) had a much higher concentration. It was noted that the sample labeled BioReactor 1 Inf (confirmed with the client’s label) behaved like a blank during preparation and the sample labeled BioReactor 1 Inf Hg Blk was a darker color after being prepared, similar to an actual sample. 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 us if you have any questions regarding this report.
Sincerely,

Lydia Greaves Tiffany Stilwater Project Manager Project Manager lydia@brooksrand.com tiffany@brooksrand.com

### Project 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.com

### Project ID: 

### DUK-HV1101

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Sample Information

Report Matrix Type Received Sampled Sample Lab ID 

### 1147018-01 BioReactor 1 Inf 11/12/2011 11/15/2011 Sample Influent 1147018-02 BioReactor 1 Inf Hg Blk 11/12/2011 11/15/2011 Field Blank DIW 1147018-03 BioReactor 2 Eff 11/12/2011 11/15/2011 Sample Effluent 1147018-04 BioReactor 2 Eff Hg Blk 11/12/2011 11/15/2011 Field Blank DIW 

# Batch Summary

Analyte Prepared Analyzed Sequence Batch Lab Matrix Method 

### B111907 11/19/2011 11/21/2011 1100820 Water EPA 1631 Hg



# Sample Results

Sample Sequence Result MDL MRL Unit Batch

Qualifier Analyte Fraction

Report Matrix 

### BioReactor 1 Inf 

### ng/L 0.15 T U 1100820 B111907 Influent 0.41 0.15 1147018-01 Hg
BioReactor 1 Inf Hg Blk 

### ng/L 123 T 1100820 B111907 DIW 4.04 1.52 1147018-02 Hg

BioReactor 2 Eff 

### ng/L 76.0 T 1100820 B111907 Effluent 4.04 1.52 1147018-03 Hg
BioReactor 2 Eff Hg Blk 

### ng/L 0.15 T U 1100820 B111907 DIW 0.40 0.15 1147018-04 Hg

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

### Project ID: 

### DUK-HV1101

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Accuracy & Precision Summary

Batch: 

### B111907

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

### EPA 1631 Lab Matrix: 

### Water

Sample Certified Reference Material (1145032, NIST 1641d 1000x dilution) B111907-SRM1 

### 15.68 97% ng/L 85-115 Hg 15.18
Matrix Spike (1147017-03) B111907-MS3 

### 404.0 110% ng/L 71-125 Hg 529.4

84.89
Matrix Spike Duplicate (1147017-03) B111907-MSD3 

### 404.0 116% ng/L 71-125 245% Hg 554.1

84.89



# Method Blanks & Reporting Limits

Batch: 

### B111907
Method: 

### EPA 1631 Matrix: 

### Water Analyte: 

### Hg Result Units Sample 

### B111907-BLK1 ng/L 0.03 B111907-BLK2 ng/L 0.06 B111907-BLK3 ng/L 0.05 B111907-BLK4 ng/L 0.03 MDL: 

### 0.15 Average: 

### 0.04 Standard Deviation: 

### 0.02 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.com

### Project ID: 

### DUK-HV1101

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Instrument Calibration

Sequence: 

### 1100820 Method: 

### EPA 1631 Instrument: 

### THG-10 Date: 

### 11/21/2011 Total Mercury and Mercury Speciation by CVAFS

Analyte: 

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

### 1100820-IBL1 6.34 pg of Hg 1100820-IBL2 5.63 pg of Hg 1100820-IBL3 6.04 pg of Hg 1100820-IBL4 7.90 pg of Hg 1100820-CAL1 25.00 27.03 pg of Hg 108% 1100820-CAL2 100.0 88.78 pg of Hg 89% 1100820-CAL3 500.0 498.8 pg of Hg 100% 1100820-CAL4 2500 2706 pg of Hg 108% 1100820-CAL5 10000 9779 pg of Hg 98% 1100820-ICV1 1568 1518 pg of Hg 97% 85-115 1100820-CCB1 16.8 pg of Hg 1100820-CCV1 500.0 481.9 pg of Hg 96% 77-123 1100820-CCV2 500.0 513.2 pg of Hg 103% 77-123 1100820-CCV3 500.0 545.4 pg of Hg 109% 77-123 1100820-CCV4 500.0 527.3 pg of Hg 105% 77-123 1100820-CCV5 500.0 475.7 pg of Hg 95% 77-123

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

### Project ID: 

### DUK-HV1101

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Sample Containers

Lab ID: 

### 1147018-01 Report Matrix: 

### Influent Sample Type: 

### Sample Received: 

### 11/15/2011 Sample: 

### BioReactor 1 Inf Collected: 

### 11/12/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71470160 10 Cooler

none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 

### 1147018-02 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 11/15/2011 Sample: 

### BioReactor 1 Inf Hg Blk Collected: 

### 11/12/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71470160 10 Cooler

none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 

### 1147018-03 Report Matrix: 

### Effluent Sample Type: 

### Sample Received: 

### 11/15/2011 Sample: 

### BioReactor 2 Eff Collected: 

### 11/12/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71470160 10 Cooler

none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 

### 1147018-04 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 11/15/2011 Sample: 

### BioReactor 2 Eff Hg Blk Collected: 

### 11/12/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71470160 10 Cooler

none n/a 250 mL Bottle FLPE Hg-T



# Shipping Containers

Cooler Tracking No: 

### 4726 7966 5861 via FedEx Temperature: 

### 3.5 °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: 

### November 15, 2011 8:30

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

## November 22, 2011

LIMS USE: FR - TERRY WHITNER LIMS OBJECT ID: 92106440



## 92106440 Project: Pace Project No.: RE: Terry Whitner Duke Energy Carolinas, LLC PO Box 37929 DPEHS Charlotte, NC 28237

J11110301

Dear Terry Whitner: Enclosed are the analytical results for sample(s) received by the laboratory on November 15, 2011. 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

cc: Mr. Jay Perkins, Duke Energy



### 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 11 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: 92106440

J11110301

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 11 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: 92106440

J11110301

Lab ID Sample ID Method Analytes Reported Laboratory Analysts 92106440001 2011024826 Filter Press Cake EPA 6010 7 PASI-A JMW EPA 7470 1 PASI-A SHB



### 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 11 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

### HITS ONLY

Pace Project No.: Project: 92106440

J11110301

Parameters Analyzed Result Lab Sample ID Report Limit Qualifiers Units Method Client Sample ID

92106440001 2011024826 Filter Press Cake Cadmium 0.0084 mg/L 11/22/11 14:02 0.0050 EPA 6010 Selenium 0.34 mg/L 11/22/11 14:02 0.10 EPA 6010



### 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 11 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

### PROJECT NARRATIVE

Pace Project No.: Project: 92106440

J11110301

Method:
Client: Duke Energy

EPA 6010

Date: November 22, 2011 Description: 6010 MET ICP, TCLP

General Information: 1 sample was analyzed for EPA 6010. All samples were received in acceptable condition with any exceptions noted below.
Hold Time: The samples were analyzed within the method required hold times with any exceptions noted below. Sample Preparation: The samples were prepared in accordance with EPA 3010 with any exceptions noted below. Initial Calibrations (including MS Tune as applicable): All criteria were within method requirements with any exceptions noted below. Continuing Calibration: All criteria were within method requirements with any exceptions noted below.
Method Blank: All analytes were below the report limit in the method blank with any exceptions noted below. Laboratory Control Spike: All laboratory control spike compounds were within QC limits with any exceptions noted below. Matrix Spikes: All percent recoveries and relative percent differences (RPDs) were within acceptance criteria with any exceptions noted below. Duplicate Sample: All duplicate sample results were within method acceptance criteria with any exceptions noted below.
Additional Comments:



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Page 5 of 11 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

### PROJECT NARRATIVE

Pace Project No.: Project: 92106440

J11110301

Method:
Client: Duke Energy

EPA 7470

Date: November 22, 2011 Description: 7470 Mercury, TCLP

General Information: 1 sample was analyzed for EPA 7470. All samples were received in acceptable condition with any exceptions noted below.
Hold Time: The samples were analyzed within the method required hold times with any exceptions noted below. Sample Preparation: The samples were prepared in accordance with EPA 7470 with any exceptions noted below. Initial Calibrations (including MS Tune as applicable): All criteria were within method requirements with any exceptions noted below. Continuing Calibration: All criteria were within method requirements with any exceptions noted below.
Method Blank: All analytes were below the report limit in the method blank with any exceptions noted below. Laboratory Control Spike: All laboratory control spike compounds were within QC limits with any exceptions noted below. Matrix Spikes: All percent recoveries and relative percent differences (RPDs) were within acceptance criteria with any exceptions noted below. Duplicate Sample: All duplicate sample results were within method acceptance criteria with any exceptions noted below.
Additional Comments: This data package has been reviewed for quality and completeness and is approved for release.



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Page 6 of 11 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: 92106440

J11110301
Sample: 2011024826 Filter Press

Cake Lab ID: 92106440001 Collected: 11/12/11 10:16 Received: 11/15/11 10:35 Matrix: Solid Results reported on a "dry-weight" basis

Parameters Results Units DF Prepared Analyzed CAS No. Qual Report Limit 6010 MET ICP, TCLP Analytical Method: EPA 6010 Preparation Method: EPA 3010 Leachate Method/Date: EPA 1311; 11/21/11 14:25 Arsenic ND mg/L 1 11/22/11 14:02 7440-38-2 11/22/11 08:55 0.025 Barium ND mg/L 1 11/22/11 14:02 7440-39-3 11/22/11 08:55 0.50 Cadmium 0.0084 mg/L 1 11/22/11 14:02 7440-43-9 11/22/11 08:55 0.0050 Chromium ND mg/L 1 11/22/11 14:02 7440-47-3 11/22/11 08:55 0.025 Lead ND mg/L 1 11/22/11 14:02 7439-92-1 11/22/11 08:55 0.025 Selenium 0.34 mg/L 1 11/22/11 14:02 7782-49-2 11/22/11 08:55 0.10 Silver ND mg/L 1 11/22/11 14:02 7440-22-4 11/22/11 08:55 0.025 7470 Mercury, TCLP Analytical Method: EPA 7470 Preparation Method: EPA 7470 Leachate Method/Date: EPA 1311; 11/21/11 14:25 Mercury ND ug/L 1 11/22/11 15:06 7439-97-6 11/22/11 09:25 0.20



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Date: 11/22/2011 04:23 PM Page 7 of 11 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: 92106440

J11110301

QC Batch: QC Batch Method: Analysis Method: Analysis Description: MERP/3886 EPA 7470 EPA 7470 7470 Mercury TCLP Associated Lab Samples: 92106440001

Parameter Units Blank Result Reporting

Limit Qualifiers METHOD BLANK: 690743 Associated Lab Samples: 92106440001 Matrix: Water

Analyzed Mercury ug/L ND 0.20 11/22/11 15:01

Parameter Units LCS Result % Rec Limits Qualifiers % Rec Conc. 690744 LABORATORY CONTROL SAMPLE: LCS Spike Mercury ug/L 2.2 2.5 90 80-120

Parameter Units MS Result % Rec Limits Qualifiers % Rec Conc. 690745 MATRIX SPIKE SAMPLE: MS Spike Result 92106440001 Mercury ug/L 2.3 2.5 93 75-125 ND

Parameter Units Dup Result Qualifiers

RPD Result 92106440001 690746 SAMPLE DUPLICATE:

Mercury ug/L ND ND



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Date: 11/22/2011 04:23 PM Page 8 of 11 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: 92106440

J11110301

QC Batch: QC Batch Method: Analysis Method: Analysis Description: MPRP/9450 EPA 3010 EPA 6010 6010 MET TCLP Associated Lab Samples: 92106440001

Parameter Units Blank Result Reporting

Limit Qualifiers METHOD BLANK: 690739 Associated Lab Samples: 92106440001 Matrix: Water

Analyzed Arsenic mg/L ND 0.025 11/22/11 13:56 Barium mg/L ND 0.50 11/22/11 13:56 Cadmium mg/L ND 0.0050 11/22/11 13:56 Chromium mg/L ND 0.025 11/22/11 13:56 Lead mg/L ND 0.025 11/22/11 13:56 Selenium mg/L ND 0.10 11/22/11 13:56 Silver mg/L ND 0.025 11/22/11 13:56

Parameter Units LCS Result % Rec Limits Qualifiers % Rec Conc. 690740 LABORATORY CONTROL SAMPLE: LCS Spike

Arsenic mg/L 2.9 2.5 115 80-120 Barium mg/L 2.5 2.5 98 80-120 Cadmium mg/L 2.5 2.5 99 80-120 Chromium mg/L 2.5 2.5 100 80-120 Lead mg/L 2.4 2.5 95 80-120 Selenium mg/L 2.9 2.5 115 80-120 Silver mg/L 1.4 1.2 115 80-120

Parameter Units MS Result % Rec Limits Qual % Rec Conc. 690741 MATRIX SPIKE & MATRIX SPIKE DUPLICATE:
MS Spike Result 92106440001 690742
MSD Result MSD

% Rec RPD MSD MS Spike

Conc. Arsenic mg/L 2.5 121 75-125 123 1 2.5 ND 3.0 3.1 Barium mg/L 2.5 100 75-125 101 1 2.5 ND 2.6 2.6 Cadmium mg/L 2.5 98 75-125 98 0 2.5 0.0084 2.5 2.5 Chromium mg/L 2.5 100 75-125 99 1 2.5 ND 2.5 2.5 Lead mg/L 2.5 95 75-125 95 1 2.5 ND 2.4 2.4 Selenium mg/L 2.5 119 75-125 121 2 2.5 0.34 3.3 3.4 Silver mg/L 1.2 117 75-125 117 0 1.2 ND 1.5 1.5



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Date: 11/22/2011 04:23 PM Page 9 of 11 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: 92106440

J11110301

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. 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. 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: 11/22/2011 04:23 PM Page 10 of 11 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: 92106440

J11110301

Lab ID Sample ID QC Batch Method QC Batch Analytical Method Analytical Batch 92106440001 MPRP/9450 ICP/8734 2011024826 Filter Press Cake EPA 3010 EPA 6010 92106440001 MERP/3886 MERC/3813 2011024826 Filter Press Cake EPA 7470 EPA 7470



### REPORT OF LABORATORY ANALYSIS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc.. Date: 11/22/2011 04:23 PM Page 11 of 11 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

### This data package contains the analytical results for the project identified above and includes a Case Narrative, Sample Results and Chain of Custody. Unless otherwise noted, all samples were received in acceptable condition and processed according to the referenced methods. Data qualifiers are flagged individually on each sample. A key reference for the data qualifiers appears at the end of this case narrative. NC Certification No. 402 SC Certification No. 99012 NC Drinking Water Cert No. 37735 

# Case Narrative 11/16/2011

Duke Energy Corporation (04) Jay Perkins 13339 Hagers Ferry Road Huntersville, NC 28078 Project: HAPS/MACT Testing Belews Creek Project No.: J11110301 Lab Submittal Date: 11/14/2011 Prism Work Order: 1110366

Please call if you have any questions relating to this analytical report. Respectfully, PRISM LABORATORIES, INC.



### VP Laboratory Services Reviewed By

Data Qualifiers Key Reference: 

### HT Sample received and analyzed outside of the hold time.

Method Detection Limit MDL Below Reporting Limit BRL
Relative Percent Difference RPD


## * Results reported to the reporting limit. All other results are reported to the MDL with values between MDL and reporting limit indicated with a J.

This report should not be reproduced, except in its entirety, without the written consent of Prism Laboratories, Inc.

449 Springbrook Road - P.O. Box 240543 - Charlotte, NC 28224-0543 Phone: 704/529-6364 - Toll Free Number: 1-800/529-6364 - Fax: 704/525-0409 

### Page 1 of 8

# Sample Receipt Summary 11/16/2011 

## Prism Work Order: 1110366 Client Sample ID Matrix Lab Sample ID Date Sampled Date Received 

### 1110366-01 11/12/11 2011024807/FGD Purge Eff 11/14/11 Water 1110366-02 11/12/11 2011024809/BioReactor 1 Inf 11/14/11 Water 1110366-03 11/12/11 2011024820/BioReactor 2 Eff 11/14/11 Water Samples received in good condition at 0.5 degrees C unless otherwise noted.

This report should not be reproduced, except in its entirety, without the written consent of Prism Laboratories, Inc.

449 Springbrook Road - P.O. Box 240543 - Charlotte, NC 28224-0543 Phone: 704/529-6364 - Toll Free Number: 1-800/529-6364 - Fax: 704/525-0409 

### Page 2 of 8

# Laboratory Report 11/16/2011

Result Parameter Batch ID Report Limit Analysis Date/Time Method Dilution Factor Units MDL Analyst 

### 13339 Hagers Ferry Road Project No.: Project: HAPS/MACT Testing Belews Creek Duke Energy Corporation (04)

Huntersville, NC 28078 Attn: Jay Perkins Sample Matrix: Water Client Sample ID: Prism Sample ID: 1110366-01 Prism Work Order: 1110366 Time Collected: 11/12/11 08:20 Time Submitted: 11/14/11 16:20 2011024807/FGD Purge Eff


### J11110301

General Chemistry Parameters 7.2 *SM4500-H B P1K0309 1 11/15/11 11:00 JAB HT pH Units pH 140 *SM2320 B P1K0306 1 5.0 11/15/11 11:00 JAB mg/L 1.4 Total Alkalinity BRL *SM2320 B P1K0307 1 5.0 11/15/11 11:00 JAB mg/L 1.4 Carbonate Alkalinity 140 *SM2320 B P1K0308 1 5.0 11/15/11 11:00 JAB mg/L 1.4 Bicarbonate Alkalinity

This report should not be reproduced, except in its entirety, without the written consent of Prism Laboratories, Inc. 449 Springbrook Road - P.O. Box 240543 - Charlotte, NC 28224-0543 Phone: 704/529-6364 - Toll Free Number: 1-800/529-6364 - Fax: 704/525-0409 

### Page 3 of 8

# Laboratory Report 11/16/2011

Result Parameter Batch ID Report Limit Analysis Date/Time Method Dilution Factor Units MDL Analyst 

### 13339 Hagers Ferry Road Project No.: Project: HAPS/MACT Testing Belews Creek Duke Energy Corporation (04)

Huntersville, NC 28078 Attn: Jay Perkins Sample Matrix: Water Client Sample ID: Prism Sample ID: 1110366-02 Prism Work Order: 1110366 Time Collected: 11/12/11 08:10 Time Submitted: 11/14/11 16:20 2011024809/BioReactor 1 Inf


### J11110301

General Chemistry Parameters 6.9 *SM4500-H B P1K0309 1 11/15/11 11:00 JAB HT pH Units pH 28 *SM2320 B P1K0306 1 5.0 11/15/11 11:00 JAB mg/L 1.4 Total Alkalinity BRL *SM2320 B P1K0307 1 5.0 11/15/11 11:00 JAB mg/L 1.4 Carbonate Alkalinity 28 *SM2320 B P1K0308 1 5.0 11/15/11 11:00 JAB mg/L 1.4 Bicarbonate Alkalinity

This report should not be reproduced, except in its entirety, without the written consent of Prism Laboratories, Inc. 449 Springbrook Road - P.O. Box 240543 - Charlotte, NC 28224-0543 Phone: 704/529-6364 - Toll Free Number: 1-800/529-6364 - Fax: 704/525-0409 

### Page 4 of 8

# Laboratory Report 11/16/2011

Result Parameter Batch ID Report Limit Analysis Date/Time Method Dilution Factor Units MDL Analyst 

### 13339 Hagers Ferry Road Project No.: Project: HAPS/MACT Testing Belews Creek Duke Energy Corporation (04)

Huntersville, NC 28078 Attn: Jay Perkins Sample Matrix: Water Client Sample ID: Prism Sample ID: 1110366-03 Prism Work Order: 1110366 Time Collected: 11/12/11 08:00 Time Submitted: 11/14/11 16:20 2011024820/BioReactor 2 Eff


### J11110301

General Chemistry Parameters 7.2 *SM4500-H B P1K0309 1 11/15/11 11:00 JAB HT pH Units pH 130 *SM2320 B P1K0306 1 5.0 11/15/11 11:00 JAB mg/L 1.4 Total Alkalinity BRL *SM2320 B P1K0307 1 5.0 11/15/11 11:00 JAB mg/L 1.4 Carbonate Alkalinity 130 *SM2320 B P1K0308 1 5.0 11/15/11 11:00 JAB mg/L 1.4 Bicarbonate Alkalinity

This report should not be reproduced, except in its entirety, without the written consent of Prism Laboratories, Inc. 449 Springbrook Road - P.O. Box 240543 - Charlotte, NC 28224-0543 Phone: 704/529-6364 - Toll Free Number: 1-800/529-6364 - Fax: 704/525-0409 

### Page 5 of 8

### 11/16/11 

## Level II QC Report

13339 Hagers Ferry Road Project No: J11110301 Project: HAPS/MACT Testing Belews Creek Duke Energy Corporation (04)

Huntersville, NC 28078 Attn: Jay Perkins Prism Work Order: 1110366 Time Submitted: 11/14/2011 4:20:00PM

Result Limit

Reporting Units Level Spike Result

Source %REC %REC Limits RPD RPD Limit Notes Analyte General Chemistry Parameters - Quality Control



### Batch P1K0306 - NO PREP Blank (P1K0306-BLK1) 

### Prepared & Analyzed: 11/15/11 Total Alkalinity mg/L BRL 5.0 LCS (P1K0306-BS1) 

### Prepared & Analyzed: 11/15/11 Total Alkalinity mg/L 253 5.0 250.0 90-110 101 LCS Dup (P1K0306-BSD1) 

### Prepared & Analyzed: 11/15/11 Total Alkalinity mg/L 256 5.0 250.0 200 90-110 102 1 Duplicate (P1K0306-DUP1) 

### Prepared & Analyzed: 11/15/11 Source: 1110366-03 Total Alkalinity mg/L 128 5.0 130 20 2 

### Batch P1K0307 - NO PREP Blank (P1K0307-BLK1) 

### Prepared & Analyzed: 11/15/11 Carbonate Alkalinity mg/L BRL 5.0 LCS (P1K0307-BS1) 

### Prepared & Analyzed: 11/15/11 Carbonate Alkalinity mg/L 253 5.0 90-110 LCS Dup (P1K0307-BSD1) 

### Prepared & Analyzed: 11/15/11 Carbonate Alkalinity mg/L 256 5.0 200 90-110 1 Duplicate (P1K0307-DUP1) 

### Prepared & Analyzed: 11/15/11 Source: 1110366-03 Carbonate Alkalinity mg/L BRL 5.0 BRL 20 

### Batch P1K0308 - NO PREP Blank (P1K0308-BLK1) 

### Prepared & Analyzed: 11/15/11 Bicarbonate Alkalinity mg/L BRL 5.0

This report should not be reproduced, except in its entirety, without the written consent of Prism Laboratories, Inc.

449 Springbrook Road - P.O. Box 240543 - Charlotte, NC 28224-0543 Phone: 704/529-6364 - Toll Free Number: 1-800/529-6364 - Fax: 704/525-0409 

### Page 6 of 8

### 11/16/11 

## Level II QC Report

13339 Hagers Ferry Road Project No: J11110301 Project: HAPS/MACT Testing Belews Creek Duke Energy Corporation (04)

Huntersville, NC 28078 Attn: Jay Perkins Prism Work Order: 1110366 Time Submitted: 11/14/2011 4:20:00PM

Result Limit

Reporting Units Level Spike Result

Source %REC %REC Limits RPD RPD Limit Notes Analyte General Chemistry Parameters - Quality Control



### Batch P1K0308 - NO PREP LCS (P1K0308-BS1) 

### Prepared & Analyzed: 11/15/11 Bicarbonate Alkalinity mg/L 253 5.0 250.0 90-110 101 LCS Dup (P1K0308-BSD1) 

### Prepared & Analyzed: 11/15/11 Bicarbonate Alkalinity mg/L 256 5.0 250.0 200 90-110 102 1 Duplicate (P1K0308-DUP1) 

### Prepared & Analyzed: 11/15/11 Source: 1110366-03 Bicarbonate Alkalinity mg/L 128 5.0 130 20 2 

### Batch P1K0309 - NO PREP LCS (P1K0309-BS1) 

### Prepared & Analyzed: 11/15/11 pH pH Units 6.82 6.860 99-101 99 Duplicate (P1K0309-DUP2) 

### Prepared & Analyzed: 11/15/11 Source: 1110366-03 pH pH Units 7.19 7.20 10 0.1

This report should not be reproduced, except in its entirety, without the written consent of Prism Laboratories, Inc.

449 Springbrook Road - P.O. Box 240543 - Charlotte, NC 28224-0543 Phone: 704/529-6364 - Toll Free Number: 1-800/529-6364 - Fax: 704/525-0409 

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