### 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: J11030084

Lab Contact: Jason C Perkins


### Date: 3/21/2011 Customer Address: 253 Plant Allen Road Customer Name(s): Don Scruggs, Robbin Jolly, Ray Lidke, Bill Kennedy

Belmont, NC 28012

Phone: 980-875-5348 Report Authorized By: (Signature)


### Program Comments: Test Burn - Day 1 Data Flags & Calculations: Any analytical tests or individual analytes within a test flagged with an "X" or "1" indicate a deviation from the method quality system or quality control requirement. All results are reported on a dry weight basis unless otherwise noted. Data Package: This data package includes analytical results that are applicable only to the samples described in this narrative. An estimation of the uncertainty of measurement for the results in the report is available upon request. This report shall not be reproduced, except in full, without the written consent of the Analytical Laboratory. Please contact the Analytical laboratory with any questions. The order of individual sections within this report is as follows: Job Summary Report, Sample Identification, Technical Validation of Data Package, Analytical Laboratory Certificate of Analysis, Analytical Laboratory QC Reports, Sub-contracted Laboratory Results, Customer Specific Data Sheets, Reports & Documentation, Customer Database Entries, Test Case Narratives, Chain of Custody (COC)
Certification: The Analytical Laboratory holds the following State Certifications : North Carolina (DENR) Certificate #248, South Carolina (DHEC) Laboratory ID # 99005. Contact the Analytical Laboratory for definitive information about the certification status of specific methods.

## Sample ID's & Descriptions:

Sample ID Plant/Station Collection Date and Time Collected By Sample Description 2011004957 ALLEN 02-Mar-11 9:12 AM Chris Williams FGD Purge Eff 2011004958 ALLEN 02-Mar-11 8:33 AM Chris Williams EQ Tank Eff 2011004959 ALLEN 02-Mar-11 8:38 AM Chris Williams BioReactor 1 Inf 2011004960 ALLEN 02-Mar-11 8:36 AM Chris Williams BioReactor 2 Inf 2011004961 ALLEN 02-Mar-11 8:41 AM Chris Williams BioReactor 2 Eff 2011004962 ALLEN 02-Mar-11 11:25 AM illegible BioReactor 1 Inf BLANK 2011004963 ALLEN 02-Mar-11 11:40 AM illegible BioReactor 2 Inf BLANK 2011004964 ALLEN 02-Mar-11 11:30 AM illegible BioReactor 2 Eff BLANK 2011004965 ALLEN 02-Mar-11 7:59 AM Chris Williams Filter Blk 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. The Vendor Laboratories have been qualified by the Analytical Laboratory Yes No



# Technical Validation Review C hecklist:

Yes No

Yes No



## Report Sections Included:

Job Summary Report Sub-contracted Laboratory Results Sample Identification Customer Specific Data Sheets, Reports, & Documentation Technical Validation of Data Package Customer Database Entries Analytical Laboratory Certificate of Analysis Test Case Narratives Analytical Laboratory QC Report Chain of Custody

Reviewed By: 

### DataBase Administrator Date: 

### 3/21/2011 Yes

Electronic Data Deliverable (EDD) Sent Separately

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



## Order # J11030084

2011004957 Collection Date: 02-Mar-11 9:12 AM 

### Site: FGD Purge Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 63.1 ug/L EPA 245.1 17-Mar-11 10:15 2.5 MHH7131 Mercury Dissolved (cold vapor) in Water (Filtered) Mercury (Hg) 37.6 ug/L EPA 245.1 17-Mar-11 10:29 1 MHH7131
TOTAL RECOVERABLE METALS BY ICP Boron (B) 62.0 mg/L EPA 200.7 14-Mar-11 12:55 0.5 DJSULL1
DISSOLVED METALS BY ICP-MS Selenium (Se) 1560 ug/L EPA 200.8 11-Mar-11 10:19 10 KRICHAR
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 142 ug/L EPA 200.8 14-Mar-11 13:31 10 KRICHAR Chromium (Cr) 109 ug/L EPA 200.8 14-Mar-11 13:31 10 KRICHAR Copper (Cu) 163 ug/L EPA 200.8 14-Mar-11 13:31 10 KRICHAR Nickel (Ni) 223 ug/L EPA 200.8 14-Mar-11 13:31 10 KRICHAR Selenium (Se) 1660 ug/L EPA 200.8 14-Mar-11 13:31 10 KRICHAR Silver (Ag) < 10 ug/L EPA 200.8 14-Mar-11 13:31 10 KRICHAR Zinc (Zn) 267 ug/L EPA 200.8 14-Mar-11 13:31 20 KRICHAR
SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011004958 Collection Date: 02-Mar-11 8:33 AM 

### Site: EQ Tank Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY (COLD VAPOR) IN WATER Mercury (Hg) 40.4 ug/L EPA 245.1 17-Mar-11 10:20 2.5 MHH7131
TOTAL RECOVERABLE METALS BY ICP Boron (B) 50.6 mg/L EPA 200.7 14-Mar-11 12:59 0.5 DJSULL1
DISSOLVED METALS BY ICP-MS Selenium (Se) 1090 ug/L EPA 200.8 11-Mar-11 10:23 10 KRICHAR
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 95.9 ug/L EPA 200.8 14-Mar-11 13:26 10 KRICHAR Chromium (Cr) 78.5 ug/L EPA 200.8 14-Mar-11 13:26 10 KRICHAR Copper (Cu) 112 ug/L EPA 200.8 14-Mar-11 13:26 10 KRICHAR Nickel (Ni) 150 ug/L EPA 200.8 14-Mar-11 13:26 10 KRICHAR Selenium (Se) 1110 ug/L EPA 200.8 14-Mar-11 13:26 10 KRICHAR

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



## Order # J11030084

2011004958 Collection Date: 02-Mar-11 8:33 AM 

### Site: EQ Tank Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst TOTAL RECOVERABLE METALS BY ICP-MS Silver (Ag) 12.2 ug/L EPA 200.8 14-Mar-11 13:26 10 KRICHAR Zinc (Zn) 174 ug/L EPA 200.8 14-Mar-11 13:26 20 KRICHAR 

### 2011004959 Collection Date: 02-Mar-11 8:38 AM 

### Site: BioReactor 1 Inf Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND
TOTAL RECOVERABLE METALS BY ICP Boron (B) 46.1 mg/L EPA 200.7 14-Mar-11 13:03 0.5 DJSULL1
DISSOLVED METALS BY ICP-MS Selenium (Se) 726 ug/L EPA 200.8 11-Mar-11 10:27 10 KRICHAR
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 14-Mar-11 13:21 10 KRICHAR Chromium (Cr) < 10 ug/L EPA 200.8 14-Mar-11 13:21 10 KRICHAR Copper (Cu) < 10 ug/L EPA 200.8 14-Mar-11 13:21 10 KRICHAR Nickel (Ni) 17.7 ug/L EPA 200.8 14-Mar-11 13:21 10 KRICHAR Selenium (Se) 781 ug/L EPA 200.8 14-Mar-11 13:21 10 KRICHAR Silver (Ag) < 10 ug/L EPA 200.8 14-Mar-11 13:21 10 KRICHAR Zinc (Zn) < 20 ug/L EPA 200.8 14-Mar-11 13:21 20 KRICHAR
SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011004960 Collection Date: 02-Mar-11 8:36 AM 

### Site: BioReactor 2 Inf Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND
TOTAL RECOVERABLE METALS BY ICP Boron (B) 49.4 mg/L EPA 200.7 14-Mar-11 13:07 0.5 DJSULL1
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 14-Mar-11 13:17 10 KRICHAR Chromium (Cr) < 10 ug/L EPA 200.8 14-Mar-11 13:17 10 KRICHAR Copper (Cu) < 10 ug/L EPA 200.8 14-Mar-11 13:17 10 KRICHAR Nickel (Ni) 11.5 ug/L EPA 200.8 14-Mar-11 13:17 10 KRICHAR

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



## Order # J11030084

2011004960 Collection Date: 02-Mar-11 8:36 AM 

### Site: BioReactor 2 Inf Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst TOTAL RECOVERABLE METALS BY ICP-MS Selenium (Se) < 10 ug/L EPA 200.8 14-Mar-11 13:17 10 KRICHAR Silver (Ag) 18.1 ug/L EPA 200.8 14-Mar-11 13:17 10 KRICHAR Zinc (Zn) < 20 ug/L EPA 200.8 14-Mar-11 13:17 20 KRICHAR
SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011004961 Collection Date: 02-Mar-11 8:41 AM 

### Site: BioReactor 2 Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND
TOTAL RECOVERABLE METALS BY ICP Boron (B) 58.6 mg/L EPA 200.7 14-Mar-11 13:11 0.5 DJSULL1
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 5 ug/L EPA 200.8 14-Mar-11 13:02 5 KRICHAR Chromium (Cr) < 5 ug/L EPA 200.8 14-Mar-11 13:02 5 KRICHAR Copper (Cu) < 5 ug/L EPA 200.8 14-Mar-11 13:02 5 KRICHAR Nickel (Ni) < 5 ug/L EPA 200.8 14-Mar-11 13:02 5 KRICHAR Selenium (Se) < 5 ug/L EPA 200.8 14-Mar-11 13:02 5 KRICHAR Silver (Ag) < 5 ug/L EPA 200.8 14-Mar-11 13:02 5 KRICHAR Zinc (Zn) < 10 ug/L EPA 200.8 14-Mar-11 13:02 10 KRICHAR
SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011004962 Collection Date: 02-Mar-11 11:25 AM 

### Site: BioReactor 1 Inf BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND 

### 2011004963 Collection Date: 02-Mar-11 11:40 AM 

### Site: BioReactor 2 Inf BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631

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



## Order # J11030084

2011004963 Collection Date: 02-Mar-11 11:40 AM 

### Site: BioReactor 2 Inf BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND 

### 2011004964 Collection Date: 02-Mar-11 11:30 AM 

### Site: BioReactor 2 Eff BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND 

### 2011004965 Collection Date: 02-Mar-11 7:59 AM 

### Site: Filter Blk Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst DISSOLVED METALS BY ICP-MS Selenium (Se) < 2 ug/L EPA 200.8 11-Mar-11 10:30 2 KRICHAR

### March 11, 2011

Duke Energy ATTN: Jay Perkins 13339 Hagers Ferry Road Huntersville NC 28078 jperkins@duke-energy.com

RE: Project DUK-HV1101 Dear Jay Perkins, This report contains results for the 6 samples received by Brooks Rand Labs (BRL) on March 04, 2011. The samples were logged-in for the contracted analyses according to the chain-of-custody form(s). The samples were received, prepared, analyzed, and stored according to BRL SOPs and EPA methodology.
The results were method blank corrected as described in the calculations section of the relevant BRL SOP(s) and may have been evaluated using reporting limits that have been adjusted to account for sample aliquot size. Please refer to the 

### Sample Results page for sample-specific MDLs, MRLs, and other details. All data is reported without qualification and all associated quality control sample results meet the acceptance criteria. BRL, an accredited laboratory, certifies that the reported results of all analyses for which BRL is NELAP accredited meet all NELAP requirements. For more details, please see the 

### Report Information page in your report. Please feel free to contact me if you have any questions regarding this report.
Sincerely,

Tiffany Stilwater Project Manager tiffany@brooksrand.com

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

### DUK-HV1101

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



### Definition of Data Qualifiers

(Effective 9/23/09) 

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

# Report Information

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

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



### method detection limit method reporting limit matrix spike

SRM T COC



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

### Common Abbreviations

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

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

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

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

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

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

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

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

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

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

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

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

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

### DUK-HV1101

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Sample Information

Report Matrix Type Received Sampled Sample Lab ID 

### 1110038-01 BioReactor 1 Inf 03/02/2011 03/04/2011 Sample FGD Wastewater 1110038-02 BioReactor 1 Inf Hg Blk 03/02/2011 03/04/2011 Field Blank DIW 1110038-03 BioReactor 2 Inf 03/02/2011 03/04/2011 Sample FGD Wastewater 1110038-04 BioReactor 2 Inf Hg Blk 03/02/2011 03/04/2011 Field Blank DIW 1110038-05 BioReactor 2 Eff 03/02/2011 03/04/2011 Sample FGD Wastewater 1110038-06 BioReactor 2 Eff Hg Blk 03/02/2011 03/04/2011 Field Blank DIW 

# Batch Summary

Analyte Prepared Analyzed Sequence Batch Lab Matrix Method 

### B110275 03/07/2011 03/09/2011 1100153 Water EPA 1631 Hg

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

### DUK-HV1101

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Sample Results

Sample Sequence Result MDL MRL Unit Batch

Qualifier Analyte Fraction

Report Matrix BioReactor 1 Inf 

### ng/L 265 T 1100153 B110275 FGD Wastewater 80.8 30.3 1110038-01 Hg
BioReactor 1 Inf Hg Blk 

### ng/L 0.15 T U 1100153 B110275 DIW 0.40 0.15 1110038-02 Hg

BioReactor 2 Eff 

### ng/L 11.0 T 1100153 B110275 FGD Wastewater 0.41 0.15 1110038-05 Hg
BioReactor 2 Eff Hg Blk 

### ng/L 0.15 T U 1100153 B110275 DIW 0.41 0.15 1110038-06 Hg

BioReactor 2 Inf 

### ng/L 24.7 T 1100153 B110275 FGD Wastewater 0.80 0.30 1110038-03 Hg
BioReactor 2 Inf Hg Blk 

### ng/L 0.15 T U 1100153 B110275 DIW 0.40 0.15 1110038-04 Hg

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

### DUK-HV1101

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Accuracy & Precision Summary

Analyte Result Units

Native Spike REC & Limits RPD & Limits Batch: 

### B110275
Method: 

### EPA 1631 Lab Matrix: 

### Water

Sample Certified Reference Material (1107115, NIST 1641d 1000x dilution) B110275-SRM1 

### 15.68 107% ng/L 16.83 85-115 Hg Matrix Spike (1110038-01) B110275-MS1 

### 1010 103% ng/L 1306 71-125 265.0 Hg Matrix Spike Duplicate (1110038-01) B110275-MSD1 

### 1010 107% ng/L 1348 71-125 243% 265.0 Hg



# Method Blanks & Reporting Limits

Batch: 

### B110275
Method: 

### EPA 1631 Matrix: 

### Water Analyte: 

### Hg Result Units Sample 

### B110275-BLK1 0.06 ng/L B110275-BLK2 0.18 ng/L B110275-BLK3 0.07 ng/L B110275-BLK4 0.25 ng/L MDL: 

### 0.15

Average: 

### 0.14 Standard Deviation: 

### 0.09 Limit: 

### 0.10 Limit: 

### 0.50 MRL: 

### 0.40

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

### DUK-HV1101

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Instrument Calibration

Method: 

### EPA 1631 Sequence: 

### 1100153 Instrument: 

### THG-05 Date: 

### 03/09/2011 Total Mercury and Mercury Speciation by CVAFS

Analyte: 

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

### 1100153-IBL1 pg of Hg 9.93 1100153-IBL2 pg of Hg 9.40 1100153-IBL3 pg of Hg 10.13 1100153-IBL4 pg of Hg 7.10 25.00 1100153-CAL1 99% pg of Hg 24.72 100.0 1100153-CAL2 97% pg of Hg 96.80 500.0 1100153-CAL3 102% pg of Hg 509.2 2500 1100153-CAL4 100% pg of Hg 2497 10000 1100153-CAL5 103% pg of Hg 10280 1568 1100153-ICV1 107% pg of Hg 85-115 1683 1100153-CCB1 pg of Hg 11.9 500.0 1100153-CCV1 104% pg of Hg 77-123 521.3 500.0 1100153-CCV2 102% pg of Hg 77-123 507.5 500.0 1100153-CCV3 104% pg of Hg 77-123 520.7

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

### DUK-HV1101

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Sample Containers

Lab ID: 

### 1110038-01 Report Matrix: 

### FGD Wastewater Sample Type: 

### Sample Received: 

### 03/04/2011 Sample: 

### BioReactor 1 Inf Collected: 

### 03/02/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71284002 0 Cardboard Box None N/A 250-mL Bottle FLPE Hg-T

Lab ID: 

### 1110038-02 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 03/04/2011 Sample: 

### BioReactor 1 Inf Hg Blk Collected: 

### 03/02/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71284002 0 Cardboard Box None N/A 250-mL Bottle FLPE Hg-T

Lab ID: 

### 1110038-03 Report Matrix: 

### FGD Wastewater Sample Type: 

### Sample Received: 

### 03/04/2011 Sample: 

### BioReactor 2 Inf Collected: 

### 03/02/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71284002 0 Cardboard Box None N/A 250-mL Bottle FLPE Hg-T

Lab ID: 

### 1110038-04 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 03/04/2011 Sample: 

### BioReactor 2 Inf Hg Blk Collected: 

### 03/02/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71284002 0 Cardboard Box None N/A 250-mL Bottle FLPE Hg-T

Lab ID: 

### 1110038-05 Report Matrix: 

### FGD Wastewater Sample Type: 

### Sample Received: 

### 03/04/2011 Sample: 

### BioReactor 2 Eff Collected: 

### 03/02/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71284002 0 Cardboard Box None N/A 250-mL Bottle FLPE Hg-T

Lab ID: 

### 1110038-06 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 03/04/2011 Sample: 

### BioReactor 2 Eff Hg Blk Collected: 

### 03/02/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71284002 0 Cardboard Box 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-HV1101

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Shipping Containers

Cardboard Box Tracking No: 

### 472679658138 via FedEx Temperature: 

### ambient Coolant Type: 

### None Description: 

### Cardboard Box Damaged in transit? 

### No Returned to client? 

### No Custody seals present? 

### No Custody seals intact? 

### No COC present? 

### Yes Received: 

### March 4, 2011 8:50

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

## March 14, 2011 Jay Perkins Duke Energy Analytical Laboratory Mail Code MGO3A2 (Building 7405) 13339 Hagers Ferry Rd. Huntersville, NC 28078 (704) 875-5245 Project: Allen – FGD Alternative Fuels Test Burn #3 - Daily) (LIMS # J11030084)

Dear Mr. Perkins, Attached is the report associat ed with four (4) aqueous sa mples submitted for selenium speciation analysis on March 3, 2011. The sa mples were received on March 4, 2011 in a sealed cooler at 1.0 o 

## C. Selenium speciation analysis was performed via ion chromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICP-DRC-MS). Any analytical issues asso ciated with the analysis are addressed in the following report. If you have any questions, please feel fr ee 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: Allen – FGD Alternative Fuels Test Burn #3 - Daily) (LIMS # J11030084)

March 14, 2011

1. Sample Reception Four (4) aqueous samples in 125mL HDPE bottles (provided by Applied Speciation and Consulting) were submitted for selenium speciation analysis on March 3, 2011. The samples were received on March 4, 2011 in a sealed container at 1.0 o 

## C. The samples were received in a lamina r flow clean hood void of trace metals contamination and ultra-violet radiat ion. Upon reception, the samples were designated discrete sample identifiers. An aliquot of each sample was filtered (0.45μm) and these filtrates were stored in a secure, monitored cryofreezer (maintained at a temperature of -80 o 

## C) until selenium speciat ion analysis could be performed via ion chromatography inductive ly 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 a pplied water for dilutions and sample preservatives are monitored for contamina tion 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 filt er (0.45μm) and inject ed directly into a sealed autosampler vial. No further sa mple preparation was performed as any chemical alteration of the samples may shift the equilibrium of the system resulting in changes in speciation ratios.

## 3. Sample Analysis All sample analysis is precluded by a minimum of a five-poi nt calibration curve spanning the entire concentrati on range of interest. Calibration curves are performed at the beginning of each analytical day. All calibration curves, associated with each species of interest, are sta ndardized by linear regression re sulting 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 ve rified using second source standards which are identified as initial calibration verification standards (ICV). Ongoing instrument performance is iden tified 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 Anal ysis by IC-ICP-DRC-MS All samples for selenium speciation analysis were analyzed by ion chromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICP-DRC-MS) on March 4, 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-tr ansfer 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 whic h 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 very well and no analytical issues were encountered. All quality control parameters associated with these samples were within acceptance limits. The estimated method detection limits (eMDLs) for selen ite, selenate, and selenocyanate are generated from replicate analyses of the lowest standard in the calibration curve. Not all selenium speci es are present in preparation blanks; therefore, eMDL calculations based on preparat ion 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, LLCSample ResultsSample IDSe(IV) Se(VI) SeCN MeSe(IV) SeMeUnknown SeSpecies (n)FGD Purge EffND (<3.8) 1570 ND (<1.5) ND (<2.2) ND (<2.2) 0 (0)BioReactor 1 Inf6.87670 ND (<0.37) 0.71 ND (<0.55) 0 (0)BioReactor 2 Inf1.47 ND (<0.34) ND (<0.37) ND (<0.55) ND (<0.55) 0 (0)BioReactor 2 Eff1.33 ND (<0.34) ND (<0.37) ND (<0.55) ND (<0.55) 0 (0)All results reflect the applied dilution and are reported in μg/LND = Not detected at the applied dilutionSeCN = SelenocyanateMeSe(IV) = Methylseleninic acidSeMe = SelenomethionineUnknown Se Species = Total concentration of all unknown Se species observed by IC-ICP-MSn = number of unknown Se species observedReport Generated by: Russell GeradsApplied Speciation and Consulting, LLCSelenium Speciation Results for Duke EnergyProject Name: Allen - FGD Alternative Fuels Test Burn #3 - DailyContact: Jay PerkinsDate: March 14, 2011LIMS #J11030084Quality Control Summary - Preparation Blank SummaryAnalyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 50x eMDL 200xSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.019 0.95 3.8Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.007 0.34 1.4SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.007 0.37 1.5MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.011 0.55 2.2SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.011 0.55 2.2eMDL = Estimated Method Detection Limit*Please see narrative regarding eMDL calculationsQuality Control Summary - Certified Reference MaterialsAnalyte (μg/L) CRM True Value Result RecoverySe(IV) ICV 9.57 9.52 99.5Se(VI) ICV 9.48 9.07 95.6SeCN ICV 8.92 8.95 100.3MeSe(IV) ICV 6.47 5.75 88.9SeMe ICV 9.32 8.65 92.8LIMS #J11030084Date: March 14, 2011Report Generated by: Russell GeradsApplied Speciation and Consulting, LLCSelenium Speciation Results for Duke EnergyProject Name: Allen - FGD Alternative Fuels Test Burn #3 - DailyContact: Jay PerkinsQuality Control Summary - Matrix DuplicatesAnalyte (μg/L) Sample ID Rep 1 Rep 2 Mean RPDSe(IV) BioReactor 2 Eff 1.33 1.27 1.30 4.7Se(VI) BioReactor 2 Eff ND (<0.34) ND (<0.34) NC NCSeCN BioReactor 2 Eff ND (<0.37) ND (<0.37) NC NCMeSe(IV) BioReactor 2 Eff ND (<0.55) ND (<0.55) NC NCSeMe BioReactor 2 Eff ND (<0.55) ND (<0.55) NC NCND = Not detected at the applied dilutionNC = Value was not calculated due to one or more concentrations below the eMDLQuality Control Summary - Matrix Spike/ Matrix Spike DuplicateAnalyte (μg/L)Sample ID Spike Conc MS Result Recovery Spike Conc MSD Result Recovery RPDSe(IV)BioReactor 2 Eff 278.0 275.4 98.6 278.0 282.9 101.3 2.7Se(VI)BioReactor 2 Eff 252.3 247.1 97.9 252.3 243.5 96.5 1.5SeCNBioReactor 2 Eff 228.8 219.6 96.0 228.8 215.5 94.2 0.0LIMS #J11030084Date: March 14, 2011Report Generated by: Russell GeradsApplied Speciation and Consulting, LLCSelenium Speciation Results for Duke EnergyProject Name: Allen - FGD Alternative Fuels Test Burn #3 - DailyContact: Jay Perkins