### 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: J11030102 Project Name: WWTS - Biweekly

L ab Contact: Jason C Perkins


### Date: 3/23/2011 Customer Address: 3195 Pine Hall Rd Customer Name(s): Bill Kennedy, Melonie Martin, Wayne Chapman, Tom Johnson

Mailcode: Belews Steam Station Belews Creek, NC 28012

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



### Program Comments: FGD BiMonthly Sampling
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 2011005006 BELEWS 09-Mar-11 8:00 AM ILLEGIBLE FGD Purge Eff 2011005007 BELEWS 09-Mar-11 8:05 AM ILLEGIBLE EQ TANK EFF. 2011005008 BELEWS 09-Mar-11 8:10 AM ILLEGIBLE BIOREACTOR 1 INF. 2011005009 BELEWS 09-Mar-11 8:15 AM ILLEGIBLE BIOREACTOR 2 INF. 2011005010 BELEWS 09-Mar-11 8:20 AM ILLEGIBLE BIOREACTOR 2 EFF. 2011005011 BELEWS 03-Mar-11 1:00 PM L.DAVIS Trip Blank 2011005012 BELEWS 03-Mar-11 1:00 PM L.DAVIS FILTER BLANK 2011005017 BELEWS 09-Mar-11 12:50 PM DAVID MORRIS BIOREACTOR 1 INF. 2011005018 BELEWS 09-Mar-11 12:50 PM DAVID MORRIS BIOREACTOR 1 INF. HG BLANK 2011005019 BELEWS 09-Mar-11 1:00 PM DAVID MORRIS BIOREACTOR 2 INF. 2011005020 BELEWS 09-Mar-11 1:00 PM DAVID MORRIS BIOREACTOR 2 INF. HG BLANK 2011005021 BELEWS 09-Mar-11 12:55 PM DAVID MORRIS BIOREACTOR 2 EFF. 2011005022 BELEWS 09-Mar-11 12:55 PM DAVID MORRIS BIOREACTOR 2 EFF. HG BLANK 13 Total Samples

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

and analyses (compliance programs and procedures). All Results are less than the laboratory reporting limits. All laboratory QA/QC requirements are acceptable. The Vendor Laboratories have been qualified by the Analytical Laboratory Yes No



# Technical Validation Review C hecklist:

Yes No

Yes No



## Report Sections Included:

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

Reviewed By: 

### DataBase Administrator Date: 

### 3/23/2011 Yes

Electronic Data Deliverable (EDD) Sent Separately

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



### Order # J11030102

2011005006 Collection Date: 09-Mar-11 8:00 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) 309 ug/L EPA 245.1 17-Mar-11 10:22 5 MHH7131
TOTAL RECOVERABLE METALS BY ICP Boron (B) 193 mg/L EPA 200.7 15-Mar-11 11:47 0.5 DJSULL1
DISSOLVED METALS BY ICP-MS Selenium (Se) 107 ug/L EPA 200.8 11-Mar-11 10:34 10 KRICHAR
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 231 ug/L EPA 200.8 15-Mar-11 14:02 10 KRICHAR Chromium (Cr) 256 ug/L EPA 200.8 15-Mar-11 14:02 10 KRICHAR Copper (Cu) 216 ug/L EPA 200.8 15-Mar-11 14:02 10 KRICHAR Nickel (Ni) 257 ug/L EPA 200.8 15-Mar-11 14:02 10 KRICHAR Selenium (Se) 6200 ug/L EPA 200.8 15-Mar-11 14:02 20 KRICHAR Silver (Ag) 15.4 ug/L EPA 200.8 15-Mar-11 14:02 10 KRICHAR Zinc (Zn) 393 ug/L EPA 200.8 15-Mar-11 14:02 20 KRICHAR
SELENIUM SPECIATION Vendor Parameter Complete V_AS&C
TOTAL DISSOLVED SOLIDS TDS 16000 mg/L SM2540C 15-Mar-11 13:30 10 CLEEMAN 

### 2011005007 Collection Date: 09-Mar-11 8:05 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) 236 ug/L EPA 245.1 17-Mar-11 10:25 2.5 MHH7131
TOTAL RECOVERABLE METALS BY ICP Boron (B) 196 mg/L EPA 200.7 15-Mar-11 11:55 0.5 DJSULL1
DISSOLVED METALS BY ICP-MS Selenium (Se) 84.9 ug/L EPA 200.8 11-Mar-11 10:37 10 KRICHAR
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 206 ug/L EPA 200.8 15-Mar-11 13:58 10 KRICHAR Chromium (Cr) 228 ug/L EPA 200.8 15-Mar-11 13:58 10 KRICHAR Copper (Cu) 190 ug/L EPA 200.8 15-Mar-11 13:58 10 KRICHAR Nickel (Ni) 235 ug/L EPA 200.8 15-Mar-11 13:58 10 KRICHAR Selenium (Se) 5140 ug/L EPA 200.8 15-Mar-11 13:58 20 KRICHAR

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



### Order # J11030102

2011005007 Collection Date: 09-Mar-11 8:05 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) 17.7 ug/L EPA 200.8 15-Mar-11 13:58 10 KRICHAR Zinc (Zn) 343 ug/L EPA 200.8 15-Mar-11 13:58 20 KRICHAR 

### 2011005008 Collection Date: 09-Mar-11 8:10 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst TOTAL RECOVERABLE METALS BY ICP Boron (B) 178 mg/L EPA 200.7 15-Mar-11 11:59 0.5 DJSULL1
DISSOLVED METALS BY ICP-MS Selenium (Se) 68.2 ug/L EPA 200.8 11-Mar-11 10:41 10 KRICHAR
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 15-Mar-11 13:23 10 KRICHAR Chromium (Cr) < 10 ug/L EPA 200.8 15-Mar-11 13:23 10 KRICHAR Copper (Cu) < 10 ug/L EPA 200.8 15-Mar-11 13:23 10 KRICHAR Nickel (Ni) 61.9 ug/L EPA 200.8 15-Mar-11 13:23 10 KRICHAR Selenium (Se) 82.6 ug/L EPA 200.8 15-Mar-11 13:23 10 KRICHAR Silver (Ag) < 10 ug/L EPA 200.8 15-Mar-11 13:23 10 KRICHAR Zinc (Zn) < 20 ug/L EPA 200.8 15-Mar-11 13:23 20 KRICHAR
SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011005009 Collection Date: 09-Mar-11 8:15 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst TOTAL RECOVERABLE METALS BY ICP Boron (B) 177 mg/L EPA 200.7 15-Mar-11 12:03 0.5 DJSULL1
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 15-Mar-11 13:18 10 KRICHAR Chromium (Cr) < 10 ug/L EPA 200.8 15-Mar-11 13:18 10 KRICHAR Copper (Cu) < 10 ug/L EPA 200.8 15-Mar-11 13:18 10 KRICHAR Nickel (Ni) 12.8 ug/L EPA 200.8 15-Mar-11 13:18 10 KRICHAR Selenium (Se) 18.1 ug/L EPA 200.8 15-Mar-11 13:18 10 KRICHAR Silver (Ag) < 10 ug/L EPA 200.8 15-Mar-11 13:18 10 KRICHAR Zinc (Zn) < 20 ug/L EPA 200.8 15-Mar-11 13:18 20 KRICHAR

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



### Order # J11030102

2011005010 Collection Date: 09-Mar-11 8:20 AM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY (COLD VAPOR) IN WATER Mercury (Hg) < 1 ug/L EPA 245.1 17-Mar-11 10:27 1 MHH7131
TOTAL RECOVERABLE METALS BY ICP Boron (B) 168 mg/L EPA 200.7 15-Mar-11 12:07 0.5 DJSULL1
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 5 ug/L EPA 200.8 15-Mar-11 13:04 5 KRICHAR Chromium (Cr) < 5 ug/L EPA 200.8 15-Mar-11 13:04 5 KRICHAR Copper (Cu) < 5 ug/L EPA 200.8 15-Mar-11 13:04 5 KRICHAR Nickel (Ni) < 5 ug/L EPA 200.8 15-Mar-11 13:04 5 KRICHAR Selenium (Se) < 5 ug/L EPA 200.8 15-Mar-11 13:04 5 KRICHAR Silver (Ag) 5.05 ug/L EPA 200.8 15-Mar-11 13:04 5 KRICHAR Zinc (Zn) < 10 ug/L EPA 200.8 15-Mar-11 13:04 10 KRICHAR
SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011005011 Collection Date: 03-Mar-11 1:00 PM 

### Site: Trip Blank Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst TOTAL RECOVERABLE METALS BY ICP Boron (B) < 0.05 mg/L EPA 200.7 15-Mar-11 11:43 0.05 DJSULL1
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 1 ug/L EPA 200.8 15-Mar-11 12:59 1 KRICHAR Chromium (Cr) < 1 ug/L EPA 200.8 15-Mar-11 12:59 1 KRICHAR Copper (Cu) < 1 ug/L EPA 200.8 15-Mar-11 12:59 1 KRICHAR Nickel (Ni) < 1 ug/L EPA 200.8 15-Mar-11 12:59 1 KRICHAR Selenium (Se) < 1 ug/L EPA 200.8 15-Mar-11 12:59 1 KRICHAR Silver (Ag) < 1 ug/L EPA 200.8 15-Mar-11 12:59 1 KRICHAR Zinc (Zn) < 2 ug/L EPA 200.8 15-Mar-11 12:59 2 KRICHAR
SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011005012 Collection Date: 03-Mar-11 1:00 PM 

### Site: FILTER BLANK 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 10:45 2 KRICHAR

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



### Order # J11030102

2011005017 Collection Date: 09-Mar-11 12:50 PM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND 

### 2011005018 Collection Date: 09-Mar-11 12:50 PM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND 

### 2011005019 Collection Date: 09-Mar-11 1:00 PM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND 

### 2011005020 Collection Date: 09-Mar-11 1:00 PM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND 

### 2011005021 Collection Date: 09-Mar-11 12:55 PM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND 

### 2011005022 Collection Date: 09-Mar-11 12:55 PM 

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

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND

## March 21, 2011 Jay Perkins Duke Energy Analytical Laboratory Mail Code MGO3A2 (Building 7405) 13339 Hagers Ferry Rd. Huntersville, NC 28078 (704) 875-5245 Project: Belews – FGD WWTS (2010, Bi-Weekly Sampling) (LIMS # J11030102)

Dear Mr. Perkins, Attached is the report associat ed with four (4) aqueous sa mples submitted for selenium speciation analysis on March 10, 2011. The samples were rece ived on March 11, 2011 in a sealed cooler at -0.5 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: Belews – FGD WWTS (2010, Bi-Weekly Sampling) (LIMS # J11030102)

March 21, 2011

1. Sample Reception Four (4) aqueous samples in 125mL HDPE bottles (provided by Applied Speciation and Consulting) were submitted for seleni um speciation analysis on March 10, 2011. The samples were received on March 11, 2011 in a sealed container at -0.5 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 11, 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 regardi ng 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 Eff28.670.8 ND (<3.0) ND (<3.0) ND (<3.0) 0 (0)BioReactor 1 Inf5.8760.9 ND (<0.76) 0.89 ND (<0.75) 0 (0)BioReactor 2 Eff ND (<0.60) ND (<0.90) ND (<0.76) ND (<0.75) ND (<0.75) 0 (0)Metals Trip BlkND (<0.12) ND (<0.18) ND (<0.15) ND (<0.15) ND (<0.15) 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: Belews - FGD WWTS (2010, Bi-Weekly Sampling)Contact: Jay PerkinsDate: March 21, 2011LIMS #J11030102Quality Control Summary - Preparation Blank SummaryAnalyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 10x eMDL 50x eMDL 200xSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.012 0.12 0.60 2.4Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.018 0.18 0.90 3.6SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.015 0.15 0.76 3.0MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.015 0.15 0.75 3.0SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.015 0.15 0.75 3.0eMDL = 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 9.59 100.2Se(VI) ICV 9.48 9.05 95.4SeCN ICV 8.92 8.87 99.5MeSe(IV) ICV 6.47 5.73 88.6SeMe ICV 9.32 8.42 90.4Selenium Speciation Results for Duke EnergyProject Name: Belews - FGD WWTS (2010, Bi-Weekly Sampling)Contact: Jay PerkinsLIMS #J11030102Date: March 21, 2011Report Generated by: Russell GeradsApplied Speciation and Consulting, LLCQuality Control Summary - Matrix DuplicatesAnalyte (μg/L) Sample ID Rep 1 Rep 2 Mean RPDSe(IV) Batch QC 343.7 343.4 343.6 0.1Se(VI) Batch QC 245.9 241.2 243.5 1.9SeCN Batch QC ND (<3.0) ND (<3.0) NC NCMeSe(IV) Batch QC 4.8 6.1 5.45 22.7SeMe Batch QC ND (<3.0) ND (<3.0) 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)Batch QC 1112 1646 117.1 1112 1638 116.4 0.5Se(VI)Batch QC 1009 1291 103.8 1009 1276 102.3 1.2SeCNBatch QC 915.0 790.0 86.3 915.0 771.4 84.3 0.0Selenium Speciation Results for Duke EnergyProject Name: Belews - FGD WWTS (2010, Bi-Weekly Sampling)Contact: Jay PerkinsLIMS #J11030102Date: March 21, 2011Report Generated by: Russell GeradsApplied Speciation and Consulting, LLC3958 6 th Ave NW • Seattle, WA 98107 • T: 206

- 632

- 6206 • F: 206

- 632

- 6017 • www.brooksrand.com • brl@brooksrand.com 

### March 20, 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

- HV100 1 Client P roject : J1 1 030 102
Dear Mr. Perkins, O n March 11 , 2011 , Brooks Rand Labs ( BRL ) received three ( 3 ) flue gas desulfurization ( FGD ) waste water samples and three (3) field blanks (one from each related FGD sample site)

. All samples were logged

- in for total mercury (Hg) analysis and 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 a ll quality assurance criteria were satisfied. The analysis of the low calibration standard s (1100171

- CAL1 & 1100171

- CAL2) recovered ab ove acceptance limits . The low calibration standard s w ere re - analyzed as 1100171

- CAL 7 and 1100171

- CAL8, respectively. The re

- analyses were reported and no additional corrective action was required. The analysis of method blank B1 10374

- BLK1 produced a result that was determined to be a Grubb’s Outlier ( 0.19 ng/L). This blank result was omitted and not used in any calculations. Therefore, the results were blank

- corrected with the average of the three remaining method blank result s. BRL, an acc redited laboratory, certifies the reported results of all analyses for which BRL is NELAP accredited meet all NELAP requirements. For more details , see the Report Information page of the report. Please feel free to contact us if you have any questions rega rding this report. Sincerely,

Tiffany Stilwater Lydia Greaves Project Manager Project Coordinator tiffany @brooksrand.com l y dia @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 1111043-01 BioReactor 1 Inf 03/09/2011 03/11/2011 Sample FGD Wastewater 1111043-02 Hg Blk BioReactor 1 Inf 03/09/2011 03/11/2011 Field Blank DIW 1111043-03 BioReactor 2 Inf 03/09/2011 03/11/2011 QC Sample FGD Wastewater 1111043-04 Hg Blk BioReactor 2 Inf 03/09/2011 03/11/2011 Field Blank DIW 1111043-05 BioReactor 2 Eff 03/09/2011 03/11/2011 Sample FGD Wastewater 1111043-06 Hg Blk BioReactor 2 Eff 03/09/2011 03/11/2011 Field Blank DIW 

# Batch Summary

Analyte Prepared Analyzed Sequence Batch Lab Matrix Method B110374 03/15/2011 03/17/2011 1100171 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 74.3 T 1100171 B110374 FGD Wastewater 4.04 1.52 1111043-01 Hg

BioReactor 2 Eff ng/L 4.70 T 1100171 B110374 FGD Wastewater 1.60 0.60 1111043-05 Hg

BioReactor 2 Inf ng/L 43.0 T 1100171 B110374 FGD Wastewater 1.62 0.61 1111043-03 Hg
Hg Blk BioReactor 1 Inf ng/L 0.15 T U 1100171 B110374 DIW 0.41 0.15 1111043-02 Hg
Hg Blk BioReactor 2 Eff ng/L 0.15 T U 1100171 B110374 DIW 0.40 0.15 1111043-06 Hg
Hg Blk BioReactor 2 Inf ng/L 0.15 T U 1100171 B110374 DIW 0.40 0.15 1111043-04 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: B110374

Method: EPA 1631 Lab Matrix: Water

Sample Certified Reference Material (1111049, NIST 1641d 1000x dilution) B110374-SRM1 15

. 68 108% ng/L 85-115 Hg 16

. 86 Matrix Spike (1111043-03) B110374-MS1 121.0 96% ng/L 71-125 Hg 159.2

42.95 Matrix Spike Duplicate (1111043-03) B110374-MSD1 123.1 105% ng/L 71-125 248% Hg 172.1

42.95



# Method Blanks & Reporting Limits

Batch: B110374

Method: EPA 1631 Matrix: Water Analyte: Hg Result Units Sample B110374-BLK1 0.04 ng/L B110374-BLK2 0.07 ng/L B110374-BLK3 0.06 ng/L MDL: 0.15

Average: 0.06 Standard Deviation: 0.02 Limit: 0.10 Limit: 0.50 MRL: 0.41

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

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



# Instrument Calibration

Method: EPA 1631 Sequence: 1100171 Instrument: THG-05 Date: 03/17/2011 Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg REC & Limits Result True Value Lab ID Units 1100171-IBL1 pg of Hg 7.43 1100171-IBL2 pg of Hg 6.70 1100171-IBL3 pg of Hg 5.44 1100171-IBL4 pg of Hg 6.06 500.0 1100171-CAL3 104% pg of Hg 517.9 2500 1100171-CAL4 105% pg of Hg 2625 10000 1100171-CAL5 100% pg of Hg 9967 1568 1100171-ICV1 108% pg of Hg 85-115 1686 1100171-CCB1 pg of Hg 29.6 100.0 1100171-CAL7 92% pg of Hg 92.45 1100171-CCB2 pg of Hg 14.2 1100171-CCB3 pg of Hg 7.34 25.00 1100171-CAL8 100% pg of Hg 25.07 500.0 1100171-CCV1 93% pg of Hg 77-123 463.2 500.0 1100171-CCV2 97% pg of Hg 77-123 485.6

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: 1111043-01 Report Matrix: FGD Wastewater Sample Type: Sample Received: 03/11/2011 Sample: BioReactor 1 Inf Collected: 03/09/2011
Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71281400 20 Cardboard Box None N/A 250 mL. Bottle FLPE Hg-T

Lab ID: 1111043-02 Report Matrix: DIW Sample Type: Field Blank Received: 03/11/2011 Sample: Hg Blk BioReactor 1 Inf Collected: 03/09/2011
Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71138980 50 Cardboard Box None N/A 250 mL. Bottle FLPE Hg-T

Lab ID: 1111043-03 Report Matrix: FGD Wastewater Sample Type: QC Sample Received: 03/11/2011 Sample: BioReactor 2 Inf Collected: 03/09/2011
Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71281400 20 Cardboard Box None N/A 250 mL. Bottle FLPE Hg-T

Lab ID: 1111043-04 Report Matrix: DIW Sample Type: Field Blank Received: 03/11/2011 Sample: Hg Blk BioReactor 2 Inf Collected: 03/09/2011
Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71138980 50 Cardboard Box None N/A 250 mL. Bottle FLPE Hg-T

Lab ID: 1111043-05 Report Matrix: FGD Wastewater Sample Type: Sample Received: 03/11/2011 Sample: BioReactor 2 Eff Collected: 03/09/2011
Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71281400 20 Cardboard Box None N/A 250 mL. Bottle FLPE Hg-T

Lab ID: 1111043-06 Report Matrix: DIW Sample Type: Field Blank Received: 03/11/2011 Sample: Hg Blk BioReactor 2 Eff Collected: 03/09/2011
Ship. Cont. pH P-Lot Preservation Lot Size Container Des A 71138980 50 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: 4726 7965 8377 via FedEx Temperature: ambient Coolant Type: None Description: Cardboard Box Damaged in transit? No Returned to client? No Custody seals present? Yes Custody seals intact? Yes COC present? Yes Received: March 11, 2011 8:30

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