### 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: J12110082 Project Name: Flex Fuel WW

L ab Contact: Jason C Perkins


### Date: 11/19/2012 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 2012023616 BELEWS 02-Nov-12 7:30 AM W. B. WORKMAN FGD Purge Eff 2012023617 BELEWS 02-Nov-12 7:35 AM W. B. WORKMAN EQ TANK 2012023618 BELEWS 02-Nov-12 7:40 AM W. B. WORKMAN BIOREACTOR 1 INF 2012023619 BELEWS 02-Nov-12 7:40 AM W. B. WORKMAN biOREACTOR 1 INF HG BLK 2012023620 BELEWS 02-Nov-12 7:50 AM W. B. WORKMAN BIOREACTOR 2 INF. 2012023621 BELEWS 02-Nov-12 7:50 AM W. B. WORKMAN BIOREACTOR 2 INF. HG BLANK 2012023622 BELEWS 02-Nov-12 8:00 AM W. B. WORKMAN BIOREACTOR 2 EFF. 2012023623 BELEWS 02-Nov-12 8:00 AM W. B. WORKMAN BIOREACTOR 2 EFF. HG BLANK 2012023624 BELEWS 02-Nov-12 8:15 AM W. B. WORKMAN FILTER BLANK 9 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: 

### 11/19/2012 Electronic Data Deliverable (EDD) Sent Separately

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



## Order # J12110082

2012023616 Collection Date: 02-Nov-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 90 mg/L EPA 300.0 11/12/2012 19:30 JAHERMA 5 50 Chloride 6300 mg/L EPA 300.0 11/12/2012 19:30 JAHERMA 100 1000 Sulfate 1100 mg/L EPA 300.0 11/12/2012 19:30 JAHERMA 100 1000 MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 124 ug/L EPA 245.1 11/08/2012 14:49 AGIBBS 5 100
DISSOLVED METALS BY ICP Manganese (Mn) 6.04 mg/L EPA 200.7 11/07/2012 10:21 MHH7131 0.05 10
TOTAL RECOVERABLE METALS BY ICP Boron (B) 167 mg/L EPA 200.7 11/14/2012 12:40 DJSULL1 0.5 10 Calcium (Ca) 4020 mg/L EPA 200.7 11/14/2012 12:40 DJSULL1 0.1 10 Iron (Fe) 117 mg/L EPA 200.7 11/14/2012 12:40 DJSULL1 0.1 10 Magnesium (Mg) 655 mg/L EPA 200.7 11/14/2012 12:40 DJSULL1 0.05 10 Manganese (Mn) 6.97 mg/L EPA 200.7 11/14/2012 12:40 DJSULL1 0.05 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 347 ug/L EPA 200.8 11/14/2012 14:46 KRICHAR 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 240 ug/L EPA 200.8 11/15/2012 11:08 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 11/15/2012 11:08 KRICHAR 10 10 Chromium (Cr) 226 ug/L EPA 200.8 11/15/2012 11:08 KRICHAR 10 10 Copper (Cu) 143 ug/L EPA 200.8 11/15/2012 11:08 KRICHAR 10 10 Nickel (Ni) 196 ug/L EPA 200.8 11/15/2012 11:08 KRICHAR 10 10 Selenium (Se) 4390 ug/L EPA 200.8 11/15/2012 11:08 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 11/15/2012 11:08 KRICHAR 10 10 Zinc (Zn) 327 ug/L EPA 200.8 11/15/2012 11:08 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 11/14/2012 16:23 SWILLI3 200 1
TOTAL SUSPENDED SOLIDS TSS 3500 mg/L SM2540D 11/06/2012 13:34 SWILLI3 250 1

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



## Order # J12110082

2012023617 Collection Date: 02-Nov-12 7:35 AM 

### Site: EQ TANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 98.5 ug/L EPA 245.1 11/08/2012 14:52 AGIBBS 2.5 50
DISSOLVED METALS BY ICP Manganese (Mn) 4.93 mg/L EPA 200.7 11/07/2012 10:24 MHH7131 0.05 10
TOTAL RECOVERABLE METALS BY ICP Boron (B) 149 mg/L EPA 200.7 11/14/2012 12:44 DJSULL1 0.5 10 Calcium (Ca) 3880 mg/L EPA 200.7 11/14/2012 12:44 DJSULL1 0.1 10 Iron (Fe) 101 mg/L EPA 200.7 11/14/2012 12:44 DJSULL1 0.1 10 Magnesium (Mg) 600 mg/L EPA 200.7 11/14/2012 12:44 DJSULL1 0.05 10 Manganese (Mn) 5.90 mg/L EPA 200.7 11/14/2012 12:44 DJSULL1 0.05 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 242 ug/L EPA 200.8 11/14/2012 14:49 KRICHAR 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 212 ug/L EPA 200.8 11/15/2012 11:12 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 11/15/2012 11:12 KRICHAR 10 10 Chromium (Cr) 210 ug/L EPA 200.8 11/15/2012 11:12 KRICHAR 10 10 Copper (Cu) 133 ug/L EPA 200.8 11/15/2012 11:12 KRICHAR 10 10 Nickel (Ni) 196 ug/L EPA 200.8 11/15/2012 11:12 KRICHAR 10 10 Selenium (Se) 3970 ug/L EPA 200.8 11/15/2012 11:12 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 11/15/2012 11:12 KRICHAR 10 10 Zinc (Zn) 290 ug/L EPA 200.8 11/15/2012 11:12 KRICHAR 10 10



### 2012023618 Collection Date: 02-Nov-12 7:40 AM 

### Site: 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 MERCURY 1631 - DISSOLVED - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND
DISSOLVED METALS BY ICP Manganese (Mn) 1.03 mg/L EPA 200.7 11/07/2012 10:28 MHH7131 0.05 10

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



## Order # J12110082

2012023618 Collection Date: 02-Nov-12 7:40 AM 

### Site: BIOREACTOR 1 INF Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF TOTAL RECOVERABLE METALS BY ICP Boron (B) 131 mg/L EPA 200.7 11/14/2012 12:48 DJSULL1 0.5 10 Calcium (Ca) 2960 mg/L EPA 200.7 11/14/2012 12:48 DJSULL1 0.1 10 Iron (Fe) < 0.1 mg/L EPA 200.7 11/14/2012 12:48 DJSULL1 0.1 10 Magnesium (Mg) 510 mg/L EPA 200.7 11/14/2012 12:48 DJSULL1 0.05 10 Manganese (Mn) 1.06 mg/L EPA 200.7 11/14/2012 12:48 DJSULL1 0.05 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 122 ug/L EPA 200.8 11/14/2012 14:52 KRICHAR 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 11/15/2012 11:15 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 11/15/2012 11:15 KRICHAR 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 11/15/2012 11:15 KRICHAR 10 10 Copper (Cu) < 10 ug/L EPA 200.8 11/15/2012 11:15 KRICHAR 10 10 Nickel (Ni) 19.3 ug/L EPA 200.8 11/15/2012 11:15 KRICHAR 10 10 Selenium (Se) 111 ug/L EPA 200.8 11/15/2012 11:15 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 11/15/2012 11:15 KRICHAR 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 11/15/2012 11:15 KRICHAR 10 10 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C



### 2012023619 Collection Date: 02-Nov-12 7:40 AM 

### Site: biOREACTOR 1 INF HG BLK 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 MERCURY 1631 - DISSOLVED - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND



### 2012023620 Collection Date: 02-Nov-12 7:50 AM 

### Site: 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

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



## Order # J12110082

2012023620 Collection Date: 02-Nov-12 7:50 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF MERCURY 1631 - DISSOLVED - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND
DISSOLVED METALS BY ICP Manganese (Mn) 1.12 mg/L EPA 200.7 11/07/2012 10:32 MHH7131 0.05 10
TOTAL RECOVERABLE METALS BY ICP Boron (B) 128 mg/L EPA 200.7 11/14/2012 12:52 DJSULL1 0.5 10 Calcium (Ca) 2920 mg/L EPA 200.7 11/14/2012 12:52 DJSULL1 0.1 10 Iron (Fe) < 0.1 mg/L EPA 200.7 11/14/2012 12:52 DJSULL1 0.1 10 Magnesium (Mg) 503 mg/L EPA 200.7 11/14/2012 12:52 DJSULL1 0.05 10 Manganese (Mn) 1.13 mg/L EPA 200.7 11/14/2012 12:52 DJSULL1 0.05 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 18.1 ug/L EPA 200.8 11/14/2012 15:14 KRICHAR 10 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 11/15/2012 11:19 KRICHAR 10 10 Cadmium (Cd) < 10 ug/L EPA 200.8 11/15/2012 11:19 KRICHAR 10 10 Chromium (Cr) < 10 ug/L EPA 200.8 11/15/2012 11:19 KRICHAR 10 10 Copper (Cu) < 10 ug/L EPA 200.8 11/15/2012 11:19 KRICHAR 10 10 Nickel (Ni) < 10 ug/L EPA 200.8 11/15/2012 11:19 KRICHAR 10 10 Selenium (Se) 12.5 ug/L EPA 200.8 11/15/2012 11:19 KRICHAR 10 10 Silver (Ag) < 10 ug/L EPA 200.8 11/15/2012 11:19 KRICHAR 10 10 Zinc (Zn) < 10 ug/L EPA 200.8 11/15/2012 11:19 KRICHAR 10 10 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C



### 2012023621 Collection Date: 02-Nov-12 7:50 AM 

### Site: BIOREACTOR 2 INF. HG BLANK 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 MERCURY 1631 - DISSOLVED - (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 # J12110082

2012023622 Collection Date: 02-Nov-12 8:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF INORGANIC IONS BY IC Bromide 78 mg/L EPA 300.0 11/12/2012 19:49 JAHERMA 5 50 Chloride 5700 mg/L EPA 300.0 11/12/2012 19:49 JAHERMA 100 1000 Sulfate 1200 mg/L EPA 300.0 11/12/2012 19:49 JAHERMA 100 1000 MERCURY 1631 - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND MERCURY 1631 - DISSOLVED - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND
DISSOLVED METALS BY ICP Manganese (Mn) 1.26 mg/L EPA 200.7 11/07/2012 10:36 MHH7131 0.05 10
TOTAL RECOVERABLE METALS BY ICP Boron (B) 126 mg/L EPA 200.7 11/14/2012 12:56 DJSULL1 0.5 10 Calcium (Ca) 2910 mg/L EPA 200.7 11/14/2012 12:56 DJSULL1 0.1 10 Iron (Fe) < 0.1 mg/L EPA 200.7 11/14/2012 12:56 DJSULL1 0.1 10 Magnesium (Mg) 507 mg/L EPA 200.7 11/14/2012 12:56 DJSULL1 0.05 10 Manganese (Mn) 1.29 mg/L EPA 200.7 11/14/2012 12:56 DJSULL1 0.05 10
DISSOLVED METALS BY ICP-MS Selenium (Se) 5.72 ug/L EPA 200.8 11/14/2012 15:17 KRICHAR 5 5
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 5 ug/L EPA 200.8 11/15/2012 11:22 KRICHAR 5 5 Cadmium (Cd) < 5 ug/L EPA 200.8 11/15/2012 11:22 KRICHAR 5 5 Chromium (Cr) < 5 ug/L EPA 200.8 11/15/2012 11:22 KRICHAR 5 5 Copper (Cu) < 5 ug/L EPA 200.8 11/15/2012 11:22 KRICHAR 5 5 Nickel (Ni) < 5 ug/L EPA 200.8 11/15/2012 11:22 KRICHAR 5 5 Selenium (Se) < 5 ug/L EPA 200.8 11/15/2012 11:22 KRICHAR 5 5 Silver (Ag) < 5 ug/L EPA 200.8 11/15/2012 11:22 KRICHAR 5 5 Zinc (Zn) < 5 ug/L EPA 200.8 11/15/2012 11:22 KRICHAR 5 5 SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC) Vendor Parameter Complete Vendor Method V_AS&C



### 2012023623 Collection Date: 02-Nov-12 8:00 AM 

### Site: BIOREACTOR 2 EFF. HG BLANK 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 # J12110082

2012023623 Collection Date: 02-Nov-12 8:00 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

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



### 2012023624 Collection Date: 02-Nov-12 8:15 AM 

### Site: FILTER BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DF DISSOLVED METALS BY ICP Manganese (Mn) < 0.005 mg/L EPA 200.7 11/07/2012 10:09 MHH7131 0.005 1
DISSOLVED METALS BY ICP-MS Selenium (Se) < 1 ug/L EPA 200.8 11/14/2012 14:27 KRICHAR 1 1

## November 14 , 201 2

Jay Perkins Duke Energy Analytical Laboratory Mail Code MGO3A2 (Building 7405) 13339 Hagers Ferry Rd. Huntersville, NC 28078 (704) 875-5 245 Project: Belews Creek (Flex Fuel) - WW (LIMS # J121100 82 )

Dear Mr. Perkins, Attached is the report associated with four (4 ) aqueous samples submitted for selenium speciation analysis on November 5 , 2012

. The samples were received in a sealed cooler at -0. 5 ° C on November 6, 2012

. Selenium speciation analysis was performed via ion chromatography 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: Belews Creek (Flex Fuel) - WW (LIMS # J12110082)

November 14 , 2012

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 5 , 2012 . The samples were received on November 6 , 201 2 in a sealed container at -0. 5 °C

. The samples were received in a laminar flow clean hood, void of trace metals contamination and ultra-violet radiation, and were designated discrete sample identifiers. An aliquot of each sample was filtered (0.45μm) and each filtrate w asstored 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 an autosampler vial. No further sample preparation was performed as any chemical alteration of a sample may shift the equilibrium of the system, resulting in changes in speciation ratios.

3. Sample Analysis All sample analysis is preceded by a minimum of a five-point calibration curve spanning the entire concentration range of interest. Calibration curves are performed at the beginning of

## each analytical day. All calibration curves, associated with each species of interest, are

standardized by linear regression resulting in a response factor. All sample results are instrument blank correctedto account for any operational biases associated with the analytical platform. Prior to sample analysis, all calibration curves are verified using second source standard s which are identified as initial calibration verification standards (ICV). Ongoing instrument performance is identified by the analysis of continuing calibration verification standards (CCV) and continuing calibration blanks (CCB) at a minimum interval of every ten analytical runs. Selenium Speciation Analysis by IC-ICP-DRC

-MS Eachsample for selenium speciation analysis w asanalyzed by ion chromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICP-DRC-MS) on November 8 , 2012

. Analiquot of each sample isinjected onto an anion exchange column and mobilized by a basic (pH > 7) gradient. The eluting selenium species are then introduced into a radio frequency (RF) plasma where energy-transfer processes cause desolvation, atomization, and ionization. The ions are extracted from the plasma through a differentially-pumped vacuum interface and travel through a pressurized chamber (DRC) containing a reaction gas which preferentially reacts with interfering ions of the same target mass to charge ratios (m/z). A solid-state detector detects ions transmitted through the mass analyzer and the resulting current is processed by a data handling system. Retention times for each eluting species are compared to known standards for species identification.

4. Analytical Issues The overall analyses went well and no significant analytical issues were encountered. The selenocyanate matrix spike and matrix spike duplicate sample recoveries (61.3% and 58.6%, respectively) were below the lower control limit of 75%. The spiking solution also contained selenite, and the spike recoveries for selenite (122.1% and 123.6%, respectively) were elevated. An acceptable mass balance of selenium species was obtained; the sum of species was calculated in each case yielding values of 92.7% and 91.7%. The apparent conversion of selenocyanate to selenite is indicative of an oxidizing matrix in the samples. Species conversion was not observed in the bracketing continuing calibration verification standards (CCV), demonstrating adequate stability of selenium species within the analytical platform. No corrective actions were required. All other quality control parameters associated with the 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 225 73.5 ND (<2.5) ND (<3.2) ND (<3.2) 0.0 (0) BioReactor 1 Inf 15.7 57.8 ND (<0.63) 2.74 ND (<0.81) 1.65 (1) BioReactor 2 Inf 1.05 ND (<0.95) ND (<0.63) ND (<0.81) ND (<0.81) 0.0 (0) BioReactor 2 Eff ND (<0.85) ND (<0.95) ND (<0.63) ND (<0.81) ND (<0.81) 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 Creek (Flex Fuel) - WW

Contact: Jay Perkins

Date: November 14, 2012 LIMS #J12110082

### Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 50x eMDL 200x Se(IV) 0.00 0.00 0.00 0.00 0.00 0.00 0.017 0.85 3.4 Se(VI) 0.00 0.00 0.00 0.00 0.00 0.00 0.019 0.95 3.8 SeCN 0.00 0.00 0.00 0.00 0.00 0.00 0.013 0.63 2.5 MeSe(IV) 0.00 0.00 0.00 0.00 0.00 0.00 0.016 0.81 3.2 SeMe 0.00 0.00 0.00 0.00 0.00 0.00 0.016 0.81 3.2 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 9.11 95.2 Se(VI) LCS 9.48 8.44 89.0 SeCN LCS 8.92 8.31 93.2 MeSe(IV) LCS 6.47 6.31 97.5 SeMe LCS 9.32 8.29 89.0 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews Creek (Flex Fuel) - WW

Contact: Jay Perkins LIMS #J12110082 Date: November 14, 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 197.4 200.7 199.1 1.6 Se(VI) Batch QC 76.7 75.5 76.1 1.6 SeCN Batch QC ND (<2.5) ND (<2.5) NC NC MeSe(IV) Batch QC ND (<3.2) ND (<3.2) NC NC SeMe Batch QC ND (<3.2) ND (<3.2) NC NC ND = Not detected at the applied dilution NC = Value was not calculated due to one or more concentrations below the eMDL

Quality Control Summary - Matrix Spike/ Matrix Spike Duplicate Analyte (μg/L) Sample ID Spike Conc MS Result Recovery Spike Conc MSD Result Recovery RPD Se(IV) Batch QC 1112 1556 122.1 1112 1574 123.6 1.1 Se(VI) Batch QC 1009 1032 94.8 1009 1013 92.8 1.9 SeCN Batch QC 915.0 560.9 61.3 * 915.0 535.8 58.6 * 4.6 *Low recovery is attributed to matrix induced species conversion Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Belews Creek (Flex Fuel) - WW

Contact: Jay Perkins LIMS #J12110082 Date: November 14, 2012 Report Generated by: Russell Gerads

### 3958 6 th

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

## November 16, 2012 Duke Energy ATTN: Jay Perkins Scientific Support-Laboratory 13339 Hagers Ferry Road Huntersville NC 28078 jcperkins@duke-energy.com labcustomer@duke-energy.com
RE: Project DUK-HV1201 Client Project: J12110082 Dear Mr. Perkins, On November 06, 2012, Brooks Rand Labs (BRL) received three (3) wastewater samples and three (3) corresponding field blanks. An aliquot was removed from each sample bottle and filtered into a separate container designed for dissolved mercury (Hg) analysis. The sample volume from the original container was logged-in for total Hg analysis. All samples were received, prepared, analyzed, and stored acco rding to BRL SOPs and EPA methodology.Data used for regulatory purposes has a 24 hour filtration holding time requirement. Nonregulatory purposed data has a 48 hour filtration holding time. The samples were received outside of the non-regulatory requirement holding time and were qualified H

. 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. Aside from concentration qualifiers, all data was reported without further qualification and all associated quality control sample results met the acceptance criteria. BRL, an accredited laboratory, certifies the reported results of all analyses for which BRL is NELAP accredited meet all NELAP requirements. For more details, see the Report Information page of the report. Please feel free to contact me if you have any questions regarding this report. Sincerely,

Lydia Greaves Mi Sun Um Project Manager Data Manager lydia@brooksrand.com misun@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: 

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### 141391



# Sample Information

Report Matrix Type Received Sampled Sample Lab ID 

### 1245003-01 BioReactor 1 Inf 11/02/2012 11/06/2012 Sample Influent 1245003-02 BioReactor 1 Inf 11/02/2012 11/06/2012 Sample Influent 1245003-03 BioReactor 1 Inf Hg Blk 11/02/2012 11/06/2012 Field Blank DIW 1245003-04 BioReactor 1 Inf Hg Blk 11/02/2012 11/06/2012 Field Blank DIW 1245003-05 BioReactor 2 Inf 11/02/2012 11/06/2012 Sample Influent 1245003-06 BioReactor 2 Inf 11/02/2012 11/06/2012 Sample Influent 1245003-07 BioReactor 2 Inf Hg Blk 11/02/2012 11/06/2012 Field Blank DIW 1245003-08 BioReactor 2 Inf Hg Blk 11/02/2012 11/06/2012 Field Blank DIW 1245003-09 BioReactor 2 EFF 11/02/2012 11/06/2012 Sample Effluent 1245003-10 BioReactor 2 EFF 11/02/2012 11/06/2012 Sample Effluent 1245003-11 BioReactor 2 EFF Hg Blk 11/02/2012 11/06/2012 Field Blank DIW 1245003-12 BioReactor 2 EFF Hg Blk 11/02/2012 11/06/2012 Field Blank DIW 

# Batch Summary

Analyte Prepared Analyzed Sequence Batch Lab Matrix Method 

### B122105 11/09/2012 11/12/2012 1200862 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: 

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# Sample Results

Sample Sequence Result MDL MRL Unit Batch

Qualifier Analyte Basis

Report Matrix BioReactor 1 Inf 

### 104 T 1200862 B122105 Influent 10.1 3.79 1245003-01 Hg ng/L 48.6 D H 1200862 B122105 Influent 2.02 0.76 1245003-02 Hg ng/L
BioReactor 1 Inf Hg Blk 

### 0.15 T U 1200862 B122105 DIW 0.41 0.15 1245003-03 Hg ng/L 0.15 D H, U 1200862 B122105 DIW 0.39 0.15 1245003-04 Hg ng/L

BioReactor 2 EFF 

### 7.18 T 1200862 B122105 Effluent 1.01 0.38 1245003-09 Hg ng/L 1.52 D H 1200862 B122105 Effluent 0.41 0.15 1245003-10 Hg ng/L
BioReactor 2 EFF Hg Blk 

### 0.16 T U 1200862 B122105 DIW 0.42 0.16 1245003-11 Hg ng/L 0.15 D H, U 1200862 B122105 DIW 0.39 0.15 1245003-12 Hg ng/L

BioReactor 2 Inf 

### 25.8 T 1200862 B122105 Influent 1.01 0.38 1245003-05 Hg ng/L 3.20 D H 1200862 B122105 Influent 0.39 0.15 1245003-06 Hg ng/L
BioReactor 2 Inf Hg Blk 

### 0.15 T U 1200862 B122105 DIW 0.40 0.15 1245003-07 Hg ng/L 0.15 D H, U 1200862 B122105 DIW 0.40 0.15 1245003-08 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: 

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# Accuracy & Precision Summary

Batch: 

### B122105

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

### EPA 1631 Lab Matrix: 

### Water

Sample Certified Reference Material (1245026, NIST 1641d 1000x dilution) B122105-SRM1 

### 15.68 100% ng/L 85-115 Hg 15.61
Matrix Spike (1245003-01) B122105-MS2 

### 505.1 109% ng/L 71-125 Hg 652.5

103.9
Matrix Spike Duplicate (1245003-01) B122105-MSD2 

### 505.1 108% ng/L 71-125 240.6% Hg 648.6

103.9
Matrix Spike (1245022-01) B122105-MS1 

### 100.2 94% ng/L 71-125 Hg 106.7

12.44
Matrix Spike Duplicate (1245022-01) B122105-MSD1 

### 99.96 94% ng/L 71-125 240.7% Hg 106.0

12.44

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

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# Method Blanks & Reporting Limits

Batch: 

### B122105
Method: 

### EPA 1631 Matrix: 

### Water Analyte: 

### Hg Result Units Sample 

### B122105-BLK1 ng/L 0.08 B122105-BLK2 ng/L 0.09 B122105-BLK3 ng/L 0.05 B122105-BLK4 ng/L 0.08 MDL: 

### 0.15 Average: 

### 0.08 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.comProject ID: 

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### Tiffany Stilwater Client PM: 

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# Instrument Calibration

Sequence: 

### 1200862 Method: 

### EPA 1631 Instrument: 

### THG-05 Date: 

### 11/12/2012 Total Mercury and Mercury Speciation by CVAFS

Analyte: 

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

### 1200862-IBL1 4.67 pg of Hg 1200862-IBL2 5.27 pg of Hg 1200862-IBL3 4.67 pg of Hg 1200862-IBL4 4.44 pg of Hg 1200862-CAL1 10.00 10.63 pg of Hg 106% 1200862-CAL2 25.00 24.16 pg of Hg 97% 1200862-CAL3 100.0 97.59 pg of Hg 98% 1200862-CAL4 500.0 497.3 pg of Hg 99% 1200862-CAL5 2500 2511 pg of Hg 100% 1200862-CAL6 10000 10010 pg of Hg 100% 1200862-ICV1 1568 1561 pg of Hg 100% 85-115 1200862-CCB1 9.36 pg of Hg 1200862-CCV1 500.0 509.7 pg of Hg 102% 77-123 1200862-CCB2 6.74 pg of Hg 1200862-CCB3 5.28 pg of Hg 1200862-CCB4 5.84 pg of Hg 1200862-CCV2 500.0 529.7 pg of Hg 106% 77-123 1200862-CCB5 6.14 pg of Hg 1200862-CCV3 500.0 533.3 pg of Hg 107% 77-123 1200862-CCB6 5.49 pg of Hg 1200862-CCV4 500.0 538.3 pg of Hg 108% 77-123 1200862-CCB7 4.90 pg of Hg 1200862-CCV5 500.0 542.2 pg of Hg 108% 77-123 1200862-CCB8 5.01 pg of Hg 1200862-CCV6 500.0 540.3 pg of Hg 108% 77-123 1200862-CCB9 5.53 pg of Hg 1200862-CCV7 500.0 546.0 pg of Hg 109% 77-123 1200862-CCBA 4.66 pg of Hg 1200862-CCV8 500.0 543.0 pg of Hg 109% 77-123 1200862-CCBB 4.75 pg of Hg 1200862-CCV9 500.0 542.5 pg of Hg 108% 77-123 1200862-CCBC 5.31 pg of Hg 1200862-CCVA 500.0 542.4 pg of Hg 108% 77-123 1200862-CCBD 4.37 pg of Hg 1200862-CCVB 500.0 541.1 pg of Hg 108% 77-123 1200862-CCBE 4.76 pg of Hg 1200862-CCVC 500.0 540.7 pg of Hg 108% 77-123 1200862-CCBF 4.20 pg of Hg 1200862-CCVD 500.0 542.3 pg of Hg 108% 77-123 1200862-CCBG 4.37 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: 

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# Instrument Calibration

Sequence: 

### 1200862 Method: 

### EPA 1631 Instrument: 

### THG-05 Date: 

### 11/12/2012 Total Mercury and Mercury Speciation by CVAFS

Analyte: 

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

### 1200862-CCVE 500.0 548.1 pg of Hg 110% 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

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# Sample Containers

Lab ID: 

### 1245003-01 Report Matrix: 

### Influent Sample Type: 

### Sample Received: 

### 11/06/2012 Sample: 

### BioReactor 1 Inf Collected: 

### 11/02/2012 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: 

### 1245003-02 Report Matrix: 

### Influent Sample Type: 

### Sample Received: 

### 11/06/2012 Sample: 

### BioReactor 1 Inf Collected: 

### 11/02/2012
Comments: 

### Qualify H Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71659890 20 Cooler

none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 

### 1245003-03 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 11/06/2012 Sample: 

### BioReactor 1 Inf Hg Blk Collected: 

### 11/02/2012 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: 

### 1245003-04 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 11/06/2012 Sample: 

### BioReactor 1 Inf Hg Blk Collected: 

### 11/02/2012
Comments: 

### Qualify H Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71659890 20 Cooler

none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 

### 1245003-05 Report Matrix: 

### Influent Sample Type: 

### Sample Received: 

### 11/06/2012 Sample: 

### BioReactor 2 Inf Collected: 

### 11/02/2012 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: 

### 1245003-06 Report Matrix: 

### Influent Sample Type: 

### Sample Received: 

### 11/06/2012 Sample: 

### BioReactor 2 Inf Collected: 

### 11/02/2012
Comments: 

### Qualify H Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71659890 20 Cooler

none n/a 250 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: 

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### 141391



# Sample Containers

Lab ID: 

### 1245003-07 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 11/06/2012 Sample: 

### BioReactor 2 Inf Hg Blk Collected: 

### 11/02/2012 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: 

### 1245003-08 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 11/06/2012 Sample: 

### BioReactor 2 Inf Hg Blk Collected: 

### 11/02/2012
Comments: 

### Qualify H Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71659890 20 Cooler

none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 

### 1245003-09 Report Matrix: 

### Effluent Sample Type: 

### Sample Received: 

### 11/06/2012 Sample: 

### BioReactor 2 EFF Collected: 

### 11/02/2012 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: 

### 1245003-10 Report Matrix: 

### Effluent Sample Type: 

### Sample Received: 

### 11/06/2012 Sample: 

### BioReactor 2 EFF Collected: 

### 11/02/2012
Comments: 

### Qualify H Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71659890 20 Cooler

none n/a 250 mL Bottle FLPE Hg-T

Lab ID: 

### 1245003-11 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 11/06/2012 Sample: 

### BioReactor 2 EFF Hg Blk Collected: 

### 11/02/2012 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: 

### 1245003-12 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 11/06/2012 Sample: 

### BioReactor 2 EFF Hg Blk Collected: 

### 11/02/2012
Comments: 

### Qualify H Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71659890 20 Cooler

none n/a 250 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: 

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### 141391



# Shipping Containers

Cooler Tracking No: 

### 535305195354 via FedEx Temperature: 

### -0.9 °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 6, 2012 9:30

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