### 13339 Hagers Ferry Road **H u**  **ntersville, NC 28078-7929 McGuire Nuclear Complex - MG03A2**  **Phone: 980-875-5245 Fax: 980-875-4349** 

# Order Summary Report 

# Analytical Laboratory

Order Number: J11120166

**Lab Contact: Jason C Perkins**  

### Date: **12/20/2011 C**  **us tomer Address:**  **253 Plant Allen Road Customer Name(s):**  **Don Scruggs, Robbin Jolly, Ray Lidke, Bill Kennedy**

**Belmont, NC 28012**

**P hone:**  **980-875-5348** Report Authorized By: (Signature)


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

## Sample ID's & Descriptions:

Sample ID Plant/Station C o llection Date and Time Collected By Sample Description **2011026433 A**  **LLE N 07-Dec-11 10:53 AM**  **JBW FGD Purge Eff**  **2011026434 ALLEN 07-Dec-11 11:06 AM**  **JBW EQ Tank Eff**  **2011026435 ALLEN 07-Dec-11 11:17 AM**  **JBW BioReactor 1 Inf**  **2011026436 ALLEN 07-Dec-11 2:29 PM**  **BS Hg Blk BioReactor 1 Inf**  **2011026437 ALLEN 07-Dec-11 11:43 AM**  **JBW BioReactor 2 Inf**  **2011026438 ALLEN 07-Dec-11 2:33 PM**  **BS Hg Blk BioReactor 2 Inf**  **2011026439 ALLEN 07-Dec-11 11:01 AM**  **JBW BioReactor 2 Eff**  **2011026440 ALLEN 07-Dec-11 2:30 PM**  **BS Hg Blk BioReactor 2 Eff**  **2011026441 ALLEN 07-Dec-11 1:45 PM**  **JBW Filter Blk**  **9 Total Samples**

### COC and .pdf report are in agreement with sample totals

**a n**  **d 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**



# T e chnical Validation Review Chec klist:

**Yes No** 

**Yes No** 



## R e port 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**

**R ev**  **iewed By:** 

### DataBase Administrator **Date:** 

### 12/20/2011 **Yes**

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

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



### Order # J11120166

2011026433 **Collection Date: 07-Dec-11 10:53 AM** 

### Site: **FGD Purge Eff M**  **a trix: OTHER** 

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst I N ORGANIC IONS BY IC **Bromide** 100 **m g/**  **L EPA 300.0**  **14-Dec-11 02:40 JAHERMA 5**  **Chloride** 2000 **mg/L EPA 300.0**  **14-Dec-11 02:40 JAHERMA 50**  MERCURY (COLD VAPOR) IN WATER **Mercury (Hg)** 121 **ug/ L**  **E PA 245.1**  **16-Dec-11 09:28 AGIBBS 2.5**  Mercury Dissolved (cold vapor) in Water (Filtered) **Mercury (Hg)** 66. 0 **ug/ L**  **EPA 245.1 16-Dec-11 10:39 AGIBBS**  **2.5**
TOTAL RECOVERABLE METALS BY ICP **Boron (B)** 165 **m g/**  **L EPA 200.7**  **12-Dec-11 11:01 MHH7131 0.5**  **Manganese (Mn)** 4.30 **mg/L EPA 200.7**  **12-Dec-11 11:01 MHH7131 0.05** 
DISSOLVED METALS BY ICP-MS **Selenium (Se)** 2210 **ug/ L**  **E PA 200.8**  **13-Dec-11 13:49 KRICHAR 10** 
TOTAL RECOVERABLE METALS BY ICP-MS **Arsenic (As)** 192 **ug/ L**  **E PA 200.8**  **13-Dec-11 11:45 KRICHAR 10**  **Chromium (Cr)** 244 **ug/L EPA 200.8**  **13-Dec-11 11:45 KRICHAR 10**  **Copper (Cu)** 171 **ug/L EPA 200.8**  **13-Dec-11 11:45 KRICHAR 10**  **Nickel (Ni)** 288 **ug/L EPA 200.8**  **13-Dec-11 11:45 KRICHAR 10**  **Selenium (Se)** 2240 **ug/L EPA 200.8**  **13-Dec-11 11:45 KRICHAR 10**  **Silver (Ag)** < 10 **ug/L EPA 200.8**  **13-Dec-11 11:45 KRICHAR 10**  **Zinc (Zn)** 253 **ug/L EPA 200.8**  **13-Dec-11 11:45 KRICHAR 20** 
SELENIUM SPECIATION **Vendor Parameter** C o mplete **V_AS&C**
TOTAL DISSOLVED SOLIDS **TDS** 8800 **m g/**  **L SM2540C**  **12-Dec-11 14:20 AGIBBS 200**  

### 2011026434 **Collection Date: 07-Dec-11 11:06 AM** 

### Site: **EQ Tank Eff M**  **a trix: OTHER** 

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst I N ORGANIC IONS BY IC **Bromide** 120 **m g/**  **L EPA 300.0**  **14-Dec-11 02:56 JAHERMA 5**  **Chloride** 2000 **mg/L EPA 300.0**  **14-Dec-11 02:56 JAHERMA 50**  MERCURY (COLD VAPOR) IN WATER **Mercury (Hg)** 97.6 **ug/ L**  **EPA 245.1 16-Dec-11 09:31 AGIBBS**  **2.5**

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



### Order # J11120166

2011026434 **Collection Date: 07-Dec-11 11:06 AM** 

### Site: **EQ Tank Eff M**  **a trix: OTHER** 

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst T O TAL RECOVERABLE METALS BY ICP **Boron (B)** 146 **m g/**  **L EPA 200.7**  **12-Dec-11 11:05 MHH7131 0.5**  **Manganese (Mn)** 3.56 **mg/L EPA 200.7**  **12-Dec-11 11:05 MHH7131 0.05** 
DISSOLVED METALS BY ICP-MS **Selenium (Se)** 1880 **ug/ L**  **E PA 200.8**  **13-Dec-11 13:53 KRICHAR 10** 
TOTAL RECOVERABLE METALS BY ICP-MS **Arsenic (As)** 150 **ug/ L**  **E PA 200.8**  **13-Dec-11 11:48 KRICHAR 10**  **Chromium (Cr)** 199 **ug/L EPA 200.8**  **13-Dec-11 11:48 KRICHAR 10**  **Copper (Cu)** 140 **ug/L EPA 200.8**  **13-Dec-11 11:48 KRICHAR 10**  **Nickel (Ni)** 228 **ug/L EPA 200.8**  **13-Dec-11 11:48 KRICHAR 10**  **Selenium (Se)** 1870 **ug/L EPA 200.8**  **13-Dec-11 11:48 KRICHAR 10**  **Silver (Ag)** < 10 **ug/L EPA 200.8**  **13-Dec-11 11:48 KRICHAR 10**  **Zinc (Zn)** 217 **ug/L EPA 200.8**  **13-Dec-11 11:48 KRICHAR 20**  

### 2011026435 **Collection Date: 07-Dec-11 11:17 AM** 

### Site: **BioReactor 1 Inf M**  **a trix: OTHER** 

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst I N ORGANIC IONS BY IC **Bromide** 170 **m g/**  **L EPA 300.0**  **14-Dec-11 03:12 JAHERMA 5**  **Chloride** 2100 **mg/L EPA 300.0**  **14-Dec-11 03:12 JAHERMA 50** 
MERCURY 1631 **Vendor Parameter** C o mplete **V_BRAND**
TOTAL RECOVERABLE METALS BY ICP **Boron (B)** 108 **m g/**  **L EPA 200.7**  **12-Dec-11 11:09 MHH7131 0.5**  **Manganese (Mn)** < 0.05 **mg/L EPA 200.7**  **12-Dec-11 11:09 MHH7131 0.05** 
DISSOLVED METALS BY ICP-MS **Selenium (Se)** 1620 **ug/ L**  **E PA 200.8**  **13-Dec-11 13:56 KRICHAR 10** 
TOTAL RECOVERABLE METALS BY ICP-MS **Arsenic (As)** < 10 **ug/L EPA 200.8**  **13-Dec-11 11:51 KRICHAR 10**  **Chromium (Cr)** 45.2 **ug/L EPA 200.8**  **13-Dec-11 11:51 KRICHAR 10**  **Copper (Cu)** < 10 **ug/L EPA 200.8**  **13-Dec-11 11:51 KRICHAR 10**  **Nickel (Ni)** < 10 **ug/L EPA 200.8**  **13-Dec-11 11:51 KRICHAR 10**  **Selenium (Se)** 1670 **ug/L EPA 200.8**  **13-Dec-11 11:51 KRICHAR 10**  **Silver (Ag)** < 10 **ug/L EPA 200.8**  **13-Dec-11 11:51 KRICHAR 10**  **Zinc (Zn)** < 20 **ug/L EPA 200.8**  **13-Dec-11 11:51 KRICHAR 20** 

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



### Order # J11120166

2011026435 **Collection Date: 07-Dec-11 11:17 AM** 

### Site: **BioReactor 1 Inf M**  **a trix: OTHER** 

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst S E LENIUM SPECIATION **Vendor Parameter** C o mplete **V_AS&C** 

### 2011026436 **Collection Date: 07-Dec-11 2:29 PM** 

### Site: **Hg Blk BioReactor 1 Inf M**  **a trix: OTHER** 

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst M E RCURY 1631 **Vendor Parameter** C o mplete **V_BRAND** 

### 2011026437 **Collection Date: 07-Dec-11 11:43 AM** 

### Site: **BioReactor 2 Inf M**  **a trix: OTHER** 

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst I N ORGANIC IONS BY IC **Bromide** 160 **m g/**  **L EPA 300.0**  **14-Dec-11 03:28 JAHERMA 5**  **Chloride** 2100 **mg/L EPA 300.0**  **14-Dec-11 03:28 JAHERMA 50** 
MERCURY 1631 **Vendor Parameter** C o mplete **V_BRAND**
TOTAL RECOVERABLE METALS BY ICP **Boron (B)** 91. 7 **m g/L**  **EPA 200.7 12-Dec-11 11:13 MHH7131**  **0.5 Manganese (Mn)**  0.345 **mg/L EPA 200.7**  **12-Dec-11 11:13 MHH7131 0.05** 
TOTAL RECOVERABLE METALS BY ICP-MS **Arsenic (As)** < 10 **ug/L EPA 200.8**  **13-Dec-11 11:54 KRICHAR 10**  **Chromium (Cr)** < 10 **ug/L EPA 200.8**  **13-Dec-11 11:54 KRICHAR 10**  **Copper (Cu)** < 10 **ug/L EPA 200.8**  **13-Dec-11 11:54 KRICHAR 10**  **Nickel (Ni)** < 10 **ug/L EPA 200.8**  **13-Dec-11 11:54 KRICHAR 10**  **Selenium (Se)** 205 **ug/L EPA 200.8**  **13-Dec-11 11:54 KRICHAR 10**  **Silver (Ag)** < 10 **ug/L EPA 200.8**  **13-Dec-11 11:54 KRICHAR 10**  **Zinc (Zn)** < 20 **ug/L EPA 200.8**  **13-Dec-11 11:54 KRICHAR 20** 
SELENIUM SPECIATION **Vendor Parameter** C o mplete **V_AS&C**

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



### Order # J11120166

2011026438 **Collection Date: 07-Dec-11 2:33 PM** 

### Site: **Hg Blk BioReactor 2 Inf M**  **a trix: OTHER** 

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst M E RCURY 1631 **Vendor Parameter** C o mplete **V_BRAND** 

### 2011026439 **Collection Date: 07-Dec-11 11:01 AM** 

### Site: **BioReactor 2 Eff M**  **a trix: OTHER** 

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst I N ORGANIC IONS BY IC **Bromide** 200 **m g/**  **L EPA 300.0**  **14-Dec-11 03:43 JAHERMA 5**  **Chloride** 1900 **mg/L EPA 300.0**  **14-Dec-11 03:43 JAHERMA 50** 
MERCURY 1631 **Vendor Parameter** C o mplete **V_BRAND**
TOTAL RECOVERABLE METALS BY ICP **Boron (B)** 38. 7 **m g/L**  **EPA 200.7 12-Dec-11 11:17 MHH7131**  **0.5 Manganese (Mn)**  1.07 **mg/L EPA 200.7**  **12-Dec-11 11:17 MHH7131 0.05** 
TOTAL RECOVERABLE METALS BY ICP-MS **Arsenic (As)** < 5 **ug/L EPA 200.8**  **13-Dec-11 11:57 KRICHAR 5**  **Chromium (Cr)** < 5 **ug/L EPA 200.8**  **13-Dec-11 11:57 KRICHAR 5**  **Copper (Cu)** < 5 **ug/L EPA 200.8**  **13-Dec-11 11:57 KRICHAR 5**  **Nickel (Ni)** < 5 **ug/L EPA 200.8**  **13-Dec-11 11:57 KRICHAR 5**  **Selenium (Se)** 6.38 **ug/L EPA 200.8**  **13-Dec-11 11:57 KRICHAR 5**  **Silver (Ag)** < 5 **ug/L EPA 200.8**  **13-Dec-11 11:57 KRICHAR 5**  **Zinc (Zn)** < 10 **ug/L EPA 200.8**  **13-Dec-11 11:57 KRICHAR 10** 
SELENIUM SPECIATION **Vendor Parameter** C o mplete **V_AS&C** 

### 2011026440 **Collection Date: 07-Dec-11 2:30 PM** 

### Site: **Hg Blk BioReactor 2 Eff M**  **a trix: OTHER** 

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst M E RCURY 1631 **Vendor Parameter** C o mplete **V_BRAND**

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



### Order # J11120166

2011026441 **Collection Date: 07-Dec-11 1:45 PM** 

### Site: **Filter Blk M**  **a trix: OTHER** 

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst D I SSOLVED METALS BY ICP-MS **Selenium (Se)** < 1 **ug/L EPA 200.8**  **13-Dec-11 13:25 KRICHAR 1** 3958 6 th Ave NW • Seattle, WA 98107 • T: 206-632-6206 • F: 206-632-6017 • www.brooksrand.com • brl@brooksrand.com 

### December 19, 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: J11120166 Dear Mr. Perkins, On December 9, 2011, Brooks Rand Labs (BRL) received three (3) waste water samples and three (3) 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. 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 me if you have any questions regarding this report.
Sincerely,

Tiffany Stilwater Project Manager tiffany@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 1150036-01 BioReactor 1 Inf 12/07/2011 12/09/2011 Sample Influent 1150036-02 BioReactor 1 Inf Hg Blk 12/07/2011 12/09/2011 Field Blank DIW 1150036-03 BioReactor 2 Inf 12/07/2011 12/09/2011 Sample Influent 1150036-04 BioReactor 2 Inf Hg Blk 12/07/2011 12/09/2011 Field Blank DIW 1150036-05 BioReactor 2 Eff 12/07/2011 12/09/2011 Sample Effluent 1150036-06 BioReactor 2 Eff Hg Blk 12/07/2011 12/09/2011 Field Blank DIW 

# Batch Summary

Analyte Prepared Analyzed Sequence Batch Lab Matrix Method B112082 12/09/2011 12/12/2011 1100872 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 61200 T 1100872 B112082 Influent 404 152 1150036-01 Hg
BioReactor 1 Inf Hg Blk ng/L 0.15 T U 1100872 B112082 DIW 0.40 0.15 1150036-02 Hg

BioReactor 2 Eff ng/L 16.8 T 1100872 B112082 Effluent 1.63 0.61 1150036-05 Hg
BioReactor 2 Eff Hg Blk ng/L 0.15 T U 1100872 B112082 DIW 0.40 0.15 1150036-06 Hg

BioReactor 2 Inf ng/L 538 T 1100872 B112082 Influent 4.04 1.52 1150036-03 Hg
BioReactor 2 Inf Hg Blk ng/L 0.15 T U 1100872 B112082 DIW 0.41 0.15 1150036-04 Hg

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

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



# Accuracy & Precision Summary

Batch: B112082

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

Sample Certified Reference Material (1149037, NIST 1641d 1000x dilution) B112082-SRM1 15.68 102% ng/L 85-115 Hg 16.00
Matrix Spike (1150033-01) B112082-MS1 130.8 101% ng/L 71-125 Hg 159.5

26.87
Matrix Spike Duplicate (1150033-01) B112082-MSD1 133.3 100% ng/L 71-125 240.6% Hg 160.4

26.87



# Method Blanks & Reporting Limits

Batch: B112082
Method: EPA 1631 Matrix: Water Analyte: Hg Result Units Sample B112082-BLK1 ng/L 0.05 B112082-BLK2 ng/L 0.03 B112082-BLK3 ng/L 0.03 B112082-BLK4 ng/L 0.03 MDL: 0.15 Average: 0.04 Standard Deviation: 0.01 Limit: 0.10 Limit: 0.50 MRL: 0.41

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

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



# Instrument Calibration

Sequence: 1100872 Method: EPA 1631 Instrument: THG-05 Date: 12/12/2011 Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg REC & Limits Result True Value Lab ID Units 1100872-IBL1 8.35 pg of Hg 1100872-IBL2 7.05 pg of Hg 1100872-IBL3 4.78 pg of Hg 1100872-IBL4 6.48 pg of Hg 1100872-CAL1 25.00 25.62 pg of Hg 102% 1100872-CAL2 100.0 96.45 pg of Hg 96% 1100872-CAL3 500.0 490.5 pg of Hg 98% 1100872-CAL4 2500 2573 pg of Hg 103% 1100872-CAL5 10000 10030 pg of Hg 100% 1100872-ICV1 1568 1600 pg of Hg 102% 85-115 1100872-CCB1 9.00 pg of Hg 1100872-CCV1 500.0 420.2 pg of Hg 84% 77-123 1100872-CCV2 500.0 475.8 pg of Hg 95% 77-123 1100872-CCB2 10.2 pg of Hg 1100872-CCV3 500.0 491.6 pg of Hg 98% 77-123

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

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



# Sample Containers

Lab ID: 1150036-01 Report Matrix: Influent Sample Type: Sample Received: 12/09/2011 Sample: BioReactor 1 Inf Collected: 12/07/2011 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: 1150036-02 Report Matrix: DIW Sample Type: Field Blank Received: 12/09/2011 Sample: BioReactor 1 Inf Hg Blk Collected: 12/07/2011 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: 1150036-03 Report Matrix: Influent Sample Type: Sample Received: 12/09/2011 Sample: BioReactor 2 Inf Collected: 12/07/2011 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: 1150036-04 Report Matrix: DIW Sample Type: Field Blank Received: 12/09/2011 Sample: BioReactor 2 Inf Hg Blk Collected: 12/07/2011 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: 1150036-05 Report Matrix: Effluent Sample Type: Sample Received: 12/09/2011 Sample: BioReactor 2 Eff Collected: 12/07/2011 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: 1150036-06 Report Matrix: DIW Sample Type: Field Blank Received: 12/09/2011 Sample: BioReactor 2 Eff Hg Blk Collected: 12/07/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71470160 10 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-HV1101

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



# Shipping Containers

Cooler Tracking No: 4726 7966 6629 via FedEx Temperature: 2.5 °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: December 9, 2011 8:45

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

## December 1 5 , 201 1

Jay Perkins Duke Energy Analytical Laboratory Mail Code MGO3A2 (Building 7405) 13339 Hagers Ferry Rd. Huntersville, NC 28078 (704) 875-5245
P roject: Allen

– FGD Alternative Fuels Test Burn #3 (LIMS # J11120 166 )
Dear Mr. Perkins, Attac hed is the report associated with four (4 ) a queous samples submitted for selenium speciation analysis on December 8, 2011. The samples were received in a sealed cooler at0.7 ° C on December 9, 2011. Selenium speciation analysis was performed via ion chromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICP-DRC-MS). Any issues associated with the analysis are addressed in the following report.
I f 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: Allen

– FGD Alternative Fuels Test Burn #3 (LIMS # J11120166)

De cember 1 5 , 2011

1. Sample Reception Four (4 ) a queous samples in 125mL HDPE bottles (provided by Applied Speciation and Consulting) were submitted for selenium speciation analysi s on December 8, 2011 . The samples were received on December 9 , 2011 in a sealed container at 0. 7 ° C. The samples were received in a laminar flow clean hood, void of trace metals contamination and ultra-violet radiation, and was 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. P rior 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 December 13, 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. All results have been corrected for instrument drift in accordance with the continuing calibration verification standards. All quality control parameters associated with this report were within acceptance limits signifying the applied calculations were acceptable.

## 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 ND (<2.2) 1880 ND (<1.6) ND (<1.9) ND (<1.9) 24.8 (3) BioReactor 1 Inf 9.59 1330 ND (<0.39) 2.12 ND (<0.47) 13.5 (4) BioReactor 2 Inf 30.2 127 ND (<0.39) 1.75 ND (<0.47) 0 (0) BioReactor 2 Eff 2.63 ND (<0.47) ND (<0.39) ND (<0.47) ND (<0.47) 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: Allen - FGD Alternative Fuels Test Burn #3 - Daily

Contact: Jay Perkins

Date: December 15, 2011 LIMS #J11120166

### Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 50x eMDL 200x Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.011 0.56 2.2 Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.009 0.47 1.9 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.39 1.6 MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.009 0.47 1.9 SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.009 0.47 1.9 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 3.83 4.09 106.8 Se(VI) LCS 3.79 4.18 110.1 SeCN LCS 3.57 3.83 107.3 MeSe(IV) LCS 2.59 2.52 97.4 SeMe LCS 3.73 3.77 101.1 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Allen - FGD Alternative Fuels Test Burn #3 - Daily

Contact: Jay Perkins LIMS #J11120166 Date: December 15, 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 92.5 91.2 91.8 1.4 Se(VI) Batch QC 12.4 13.6 13.0 9.3 SeCN Batch QC 5.3 4.5 4.9 15.6 MeSe(IV) Batch QC ND (<1.9) ND (<1.9) NC NC SeMe Batch QC ND (<1.9) ND (<1.9) 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 1277 114.8 1112 1320 118.7 3.4 Se(VI) Batch QC 1009 1032 102.3 1009 1031 102.2 0.0 SeCN Batch QC 915.0 859.3 93.9 915.0 824.4 90.1 4.2 Applied Speciation and Consulting, LLC Selenium Speciation Results for Duke Energy Project Name: Allen - FGD Alternative Fuels Test Burn #3 - Daily

Contact: Jay Perkins LIMS #J11120166 Date: December 15, 2011 Report Generated by: Russell Gerads