### 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: J11040141

Lab Contact: Jason C Perkins


### Date: 4/26/2011 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:

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 2011007587 ALLEN 11-Apr-11 3:09 AM Matt Campbell FGD Purge Eff 2011007588 ALLEN 11-Apr-11 3:18 AM Matt Campbell EQ Tank Eff 2011007589 ALLEN 11-Apr-11 3:22 AM Matt Campbell BioReactor 1 Inf 2011007590 ALLEN 11-Apr-11 3:27 AM Matt Campbell BioReactor 2 Inf 2011007591 ALLEN 11-Apr-11 3:30 AM Matt Campbell BioReactor 2 Eff 2011007592 ALLEN 06-Apr-11 2:20 PM L. Davis Filter Blk 2011007593 ALLEN 06-Apr-11 2:20 PM L. Davis TRIP BLANK 2011007594 ALLEN 11-Apr-11 10:25 AM David Morris (Prism) BioReactor 1 Inf 2011007595 ALLEN 11-Apr-11 10:25 AM David Morris (Prism) Hg Blk BioReactor 1 Inf 2011007596 ALLEN 11-Apr-11 10:35 AM David Morris (Prism) BioReactor 2 Inf 2011007597 ALLEN 11-Apr-11 10:35 AM David Morris (Prism) Hg Blk BioReactor 2 Inf 2011007598 ALLEN 11-Apr-11 10:30 AM David Morris (Prism) BioReactor 2 Eff 2011007599 ALLEN 11-Apr-11 10:30 AM David Morris (Prism) Hg Blk BioReactor 2 Eff 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: 

### 4/26/2011 Yes

Electronic Data Deliverable (EDD) Sent Separately

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



## Order # J11040141

2011007587 Collection Date: 11-Apr-11 3:09 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) 46.9 ug/L EPA 245.1 21-Apr-11 14:55 TLINN 2.5
TOTAL RECOVERABLE METALS BY ICP Boron (B) 80.4 mg/L EPA 200.7 20-Apr-11 11:22 DJSULL1 0.5
DISSOLVED METALS BY ICP-MS Selenium (Se) 644 ug/L EPA 200.8 20-Apr-11 14:33 KRICHAR 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 145 ug/L EPA 200.8 20-Apr-11 09:50 KRICHAR 10 Chromium (Cr) 113 ug/L EPA 200.8 20-Apr-11 09:50 KRICHAR 10 Copper (Cu) 149 ug/L EPA 200.8 20-Apr-11 09:50 KRICHAR 10 Nickel (Ni) 236 ug/L EPA 200.8 20-Apr-11 09:50 KRICHAR 10 Selenium (Se) 1330 ug/L EPA 200.8 20-Apr-11 09:50 KRICHAR 10 Silver (Ag) < 10 ug/L EPA 200.8 20-Apr-11 09:50 KRICHAR 10 Zinc (Zn) 252 ug/L EPA 200.8 20-Apr-11 09:50 KRICHAR 20
SELENIUM SPECIATION Vendor Parameter Complete V_AS&C
TOTAL DISSOLVED SOLIDS TDS 13000 mg/L SM2540C 19-Apr-11 09:15 TJA7067 100 

### 2011007588 Collection Date: 11-Apr-11 3:18 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) 33.5 ug/L EPA 245.1 21-Apr-11 14:57 TLINN 2.5
TOTAL RECOVERABLE METALS BY ICP Boron (B) 72.7 mg/L EPA 200.7 20-Apr-11 11:26 DJSULL1 0.5
DISSOLVED METALS BY ICP-MS Selenium (Se) 581 ug/L EPA 200.8 20-Apr-11 14:37 KRICHAR 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) 113 ug/L EPA 200.8 20-Apr-11 09:45 KRICHAR 10 Chromium (Cr) 84.6 ug/L EPA 200.8 20-Apr-11 09:45 KRICHAR 10 Copper (Cu) 112 ug/L EPA 200.8 20-Apr-11 09:45 KRICHAR 10 Nickel (Ni) 181 ug/L EPA 200.8 20-Apr-11 09:45 KRICHAR 10

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



## Order # J11040141

2011007588 Collection Date: 11-Apr-11 3:18 AM 

### Site: EQ Tank Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst TOTAL RECOVERABLE METALS BY ICP-MS Selenium (Se) 1080 ug/L EPA 200.8 20-Apr-11 09:45 KRICHAR 10 Silver (Ag) < 10 ug/L EPA 200.8 20-Apr-11 09:45 KRICHAR 10 Zinc (Zn) 197 ug/L EPA 200.8 20-Apr-11 09:45 KRICHAR 20 

### 2011007589 Collection Date: 11-Apr-11 3:22 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) 64.2 mg/L EPA 200.7 20-Apr-11 11:30 DJSULL1 0.5
DISSOLVED METALS BY ICP-MS Selenium (Se) 762 ug/L EPA 200.8 20-Apr-11 14:42 KRICHAR 10
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 20-Apr-11 09:41 KRICHAR 10 Chromium (Cr) < 10 ug/L EPA 200.8 20-Apr-11 09:41 KRICHAR 10 Copper (Cu) < 10 ug/L EPA 200.8 20-Apr-11 09:41 KRICHAR 10 Nickel (Ni) 18.6 ug/L EPA 200.8 20-Apr-11 09:41 KRICHAR 10 Selenium (Se) 846 ug/L EPA 200.8 20-Apr-11 09:41 KRICHAR 10 Silver (Ag) < 10 ug/L EPA 200.8 20-Apr-11 09:41 KRICHAR 10 Zinc (Zn) < 20 ug/L EPA 200.8 20-Apr-11 09:41 KRICHAR 20
SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011007590 Collection Date: 11-Apr-11 3:27 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) 57.0 mg/L EPA 200.7 20-Apr-11 11:34 DJSULL1 0.5
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 10 ug/L EPA 200.8 20-Apr-11 09:36 KRICHAR 10 Chromium (Cr) < 10 ug/L EPA 200.8 20-Apr-11 09:36 KRICHAR 10 Copper (Cu) < 10 ug/L EPA 200.8 20-Apr-11 09:36 KRICHAR 10 Nickel (Ni) < 10 ug/L EPA 200.8 20-Apr-11 09:36 KRICHAR 10 Selenium (Se) 262 ug/L EPA 200.8 20-Apr-11 09:36 KRICHAR 10 Silver (Ag) < 10 ug/L EPA 200.8 20-Apr-11 09:36 KRICHAR 10 Zinc (Zn) < 20 ug/L EPA 200.8 20-Apr-11 09:36 KRICHAR 20

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



## Order # J11040141

2011007591 Collection Date: 11-Apr-11 3:30 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 21-Apr-11 15:00 TLINN 1
TOTAL RECOVERABLE METALS BY ICP Boron (B) 57.0 mg/L EPA 200.7 20-Apr-11 11:38 DJSULL1 0.5
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 5 ug/L EPA 200.8 20-Apr-11 09:21 KRICHAR 5 Chromium (Cr) < 5 ug/L EPA 200.8 20-Apr-11 09:21 KRICHAR 5 Copper (Cu) < 5 ug/L EPA 200.8 20-Apr-11 09:21 KRICHAR 5 Nickel (Ni) < 5 ug/L EPA 200.8 20-Apr-11 09:21 KRICHAR 5 Selenium (Se) 5.36 ug/L EPA 200.8 20-Apr-11 09:21 KRICHAR 5 Silver (Ag) < 5 ug/L EPA 200.8 20-Apr-11 09:21 KRICHAR 5 Zinc (Zn) < 10 ug/L EPA 200.8 20-Apr-11 09:21 KRICHAR 10
SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011007592 Collection Date: 06-Apr-11 2:20 PM 

### 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 20-Apr-11 14:46 KRICHAR 2 

### 2011007593 Collection Date: 06-Apr-11 2:20 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 20-Apr-11 11:14 DJSULL1 0.05
TOTAL RECOVERABLE METALS BY ICP-MS Arsenic (As) < 1 ug/L EPA 200.8 20-Apr-11 09:17 KRICHAR 1 Chromium (Cr) < 1 ug/L EPA 200.8 20-Apr-11 09:17 KRICHAR 1 Copper (Cu) < 1 ug/L EPA 200.8 20-Apr-11 09:17 KRICHAR 1 Nickel (Ni) < 1 ug/L EPA 200.8 20-Apr-11 09:17 KRICHAR 1 Selenium (Se) 1.53 ug/L EPA 200.8 20-Apr-11 09:17 KRICHAR 1 Silver (Ag) < 1 ug/L EPA 200.8 20-Apr-11 09:17 KRICHAR 1 Zinc (Zn) < 2 ug/L EPA 200.8 20-Apr-11 09:17 KRICHAR 2
SELENIUM SPECIATION

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



## Order # J11040141

2011007593 Collection Date: 06-Apr-11 2:20 PM 

### Site: TRIP BLANK Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst SELENIUM SPECIATION Vendor Parameter Complete V_AS&C 

### 2011007594 Collection Date: 11-Apr-11 10:25 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 

### 2011007595 Collection Date: 11-Apr-11 10:25 AM 

### Site: Hg Blk BioReactor 1 Inf Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND 

### 2011007596 Collection Date: 11-Apr-11 10:35 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 

### 2011007597 Collection Date: 11-Apr-11 10:35 AM 

### Site: Hg Blk BioReactor 2 Inf Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND 

### 2011007598 Collection Date: 11-Apr-11 10:30 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

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



## Order # J11040141

2011007599 Collection Date: 11-Apr-11 10:30 AM 

### Site: Hg Blk BioReactor 2 Eff Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result 

### Sample #:

Analyst MERCURY 1631 Vendor Parameter Complete V_BRAND

## April 22, 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 WWTS (2011, Bi -Weekly Sampling) (LIMS # J11040141)

Dear Mr. Perkins, Attached is the report associat ed with four (4) aqueous sa mples submitted for selenium speciation analysis on April 14, 2011. The sa mples were received on April 15, 2011 in a sealed cooler at -0.5 o 

## C. Selenium speciation anal ysis 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 WWTS (2011, Bi -Weekly Sampling) (LIMS # J11040141)

April 22, 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 April 14, 2011. The samples were received on April 15, 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 April 15, 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 Eff83.0657 ND (<5.1) ND (<3.8) ND (<3.8) 0 (0)BioReactor 1 Inf5.39839 ND (<1.3) ND (<0.95) ND (<0.95) 0 (0)BioReactor 2 Eff4.311.65 ND (<1.3) ND (<0.95) ND (<0.95) 0 (0)Metals Trip BlkND (<0.19) ND (<0.13) ND (<0.25) ND (<0.19) ND (<0.19) 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 WWTS (2011, Bi-Weekly Sampling)Contact: Jay PerkinsDate: April 22, 2011LIMS #J11040141Quality 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 0.019 0.19 0.95 3.8Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.013 0.13 0.64 2.6SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.025 0.25 1.3 5.1MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.019 0.19 0.95 3.8SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.019 0.19 0.95 3.8eMDL = 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 9.40 98.3Se(VI) ICV 9.48 9.02 95.2SeCN ICV 8.92 8.87 99.5MeSe(IV) ICV 6.47 5.97 92.3SeMe ICV 9.32 7.23 77.6Selenium Speciation Results for Duke EnergyProject Name: Allen - FGD WWTS (2011, Bi-Weekly Sampling)Contact: Jay PerkinsLIMS #J11040141Date: April 22, 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 216.6 212.0 214.3 2.2Se(VI) Batch QC 242.0 244.5 243.2 1.0SeCN Batch QC ND (<5.1) ND (<5.1) NC NCMeSe(IV) Batch QC 8.4 7.3 7.9 13.9SeMe Batch QC 4.7 3.9 4.3 18.4ND = 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 1294 97.1 1112 1288 96.5 0.5Se(VI)Batch QC 1009 1214 96.2 1009 1208 95.6 0.5SeCNBatch QC 915.0 801.2 87.6 915.0 792.1 86.6 0.0Selenium Speciation Results for Duke EnergyProject Name: Allen - FGD WWTS (2011, Bi-Weekly Sampling)Contact: Jay PerkinsLIMS #J11040141Date: April 22, 2011Report Generated by: Russell GeradsApplied Speciation and Consulting, LLC

### 3958 6 th 

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

## April 22, 2011
Duke Energy ATTN: Jay Perkins Scientific Support-Laboratory 13339 Hagers Ferry Road Huntersville NC 28078 jcperkins@duke-energy.com labcustomer@duke-energy.com
RE: Project DUK-HV1101 Client Project: J11040141
Dear Mr. Perkins, On April 13, 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). BRL received four samples (2 FGD samples and 2 field blanks) labeled BioReactor 1 Inf and no samples were labeled BioReactor 2 Inf . BRL matched the sample IDs using the collection date/times on the containers with those listed on the chain-of-custody form. The samples were logged-in accordingly. All samples were logged-in for total mercury (Hg) analysis and were received, prepared, analyzed, and stored acco rding 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 quality assurance criteria were satisfied. BRL, an accredited laboratory, certifies the reported results of all analyses for which BRL is NELAP accredited meet all NELAP requirements. For more details, see the Report Information page of the report. Please feel free to contact us if you have any questions regarding this report. Sincerely,

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

### 1116015-01 BioReactor 1 Inf 04/11/2011 04/13/2011 Sample FGD Wastewater 1116015-02 Hg Blk BioReactor 1 Inf 04/11/2011 04/13/2011 Field Blank DIW 1116015-03 BioReactor 2 Inf 04/11/2011 04/13/2011 QC Sample FGD Wastewater 1116015-04 Hg Blk BioReactor 2 Inf 04/11/2011 04/13/2011 Field Blank DIW 1116015-05 BioReactor 2 Eff 04/11/2011 04/13/2011 Sample FGD Wastewater 1116015-06 Hg Blk BioReactor 2 Eff 04/11/2011 04/13/2011 Field Blank DIW 

# Batch Summary

Analyte Prepared Analyzed Sequence Batch Lab Matrix Method 

### B110548 04/15/2011 04/18/2011 1100252 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 858 T 1100252 B110548 FGD Wastewater 4.04 1.52 1116015-01 Hg

BioReactor 2 Eff 

### ng/L 11.2 T 1100252 B110548 FGD Wastewater 1.58 0.59 1116015-05 Hg

BioReactor 2 Inf 

### ng/L 184 T 1100252 B110548 FGD Wastewater 4.04 1.52 1116015-03 Hg
Hg Blk BioReactor 1 Inf 

### ng/L 0.15 T U 1100252 B110548 DIW 0.40 0.15 1116015-02 Hg
Hg Blk BioReactor 2 Eff 

### ng/L 0.15 T U 1100252 B110548 DIW 0.40 0.15 1116015-06 Hg
Hg Blk BioReactor 2 Inf 

### ng/L 0.15 T U 1100252 B110548 DIW 0.40 0.15 1116015-04 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: 

### B110548

Method: 

### EPA 1631 Lab Matrix: 

### Water

Sample Certified Reference Material (1116002, NIST 1641d 1000x dilution) B110548-SRM1 

### 15.84 103% ng/L 85-115 Hg 16.25 Matrix Spike (1116015-03) B110548-MS1 

### 606.1 103% ng/L 71-125 Hg 810.8

184.0 Matrix Spike Duplicate (1116015-03) B110548-MSD1 

### 606.1 107% ng/L 71-125 242% Hg 829.8

184.0



# Method Blanks & Reporting Limits

Batch: 

### B110548
Method: 

### EPA 1631 Matrix: 

### Water Analyte: 

### Hg Result Units Sample 

### B110548-BLK1 ng/L 0.05 B110548-BLK2 ng/L 0.10 B110548-BLK3 ng/L 0.06 B110548-BLK4 ng/L 0.04 MDL: 

### 0.15 Average: 

### 0.06 Standard Deviation: 

### 0.03 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: 

### 1100252 Instrument: 

### THG-05 Date: 

### 04/18/2011 Total Mercury and Mercury Speciation by CVAFS

Analyte: 

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

### 1100252-IBL1 pg of Hg 6.05 1100252-IBL2 pg of Hg 6.81 1100252-IBL3 pg of Hg 5.76 1100252-IBL4 pg of Hg 7.30 25.00 1100252-CAL1 104% pg of Hg 26.06 100.0 1100252-CAL2 100% pg of Hg 99.96 500.0 1100252-CAL3 97% pg of Hg 484.4 2500 1100252-CAL4 98% pg of Hg 2457 10000 1100252-CAL5 101% pg of Hg 10100 1568 1100252-ICV1 103% pg of Hg 85-115 1615 1100252-CCB1 pg of Hg 13.4 500.0 1100252-CCV1 101% pg of Hg 77-123 504.9 500.0 1100252-CCV2 107% pg of Hg 77-123 534.4 500.0 1100252-CCV3 102% pg of Hg 77-123 512.5

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: 

### 1116015-01 Report Matrix: 

### FGD Wastewater Sample Type: 

### Sample Received: 

### 04/13/2011 Sample: 

### BioReactor 1 Inf Collected: 

### 04/11/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71281400 20 Cooler

None N/A 250 mL Bottle FLPE Hg-T

Lab ID: 

### 1116015-02 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 04/13/2011 Sample: 

### Hg Blk BioReactor 1 Inf Collected: 

### 04/11/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71281400 20 Cooler

None N/A 250 mL Bottle FLPE Hg-T

Lab ID: 

### 1116015-03 Report Matrix: 

### FGD Wastewater Sample Type: 

### QC Sample Received: 

### 04/13/2011 Sample: 

### BioReactor 2 Inf Collected: 

### 04/11/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71281400 20 Cooler

None N/A 250 mL Bottle FLPE Hg-T

Lab ID: 

### 1116015-04 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 04/13/2011 Sample: 

### Hg Blk BioReactor 2 Inf Collected: 

### 04/11/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71281400 20 Cooler

None N/A 250 mL Bottle FLPE Hg-T

Lab ID: 

### 1116015-05 Report Matrix: 

### FGD Wastewater Sample Type: 

### Sample Received: 

### 04/13/2011 Sample: 

### BioReactor 2 Eff Collected: 

### 04/11/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71281400 20 Cooler

None N/A 250 mL Bottle FLPE Hg-T

Lab ID: 

### 1116015-06 Report Matrix: 

### DIW Sample Type: 

### Field Blank Received: 

### 04/13/2011 Sample: 

### Hg Blk BioReactor 2 Eff Collected: 

### 04/11/2011 Ship. Cont. pH P-Lot Preservation Lot Size Container Des 

### A 71281400 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-HV1101

PM: 

### Tiffany Stilwater Client PM: 

### Jay Perkins Client PO: 

### 141391



# Shipping Containers

Cooler Tracking No: 

### 4726 7965 9421 via FedEx Temperature: 

### 3.9 °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: 

### April 13, 2011 8:45

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