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: J10120147

Lab Contact: Jason C Perkins

Date: 12/20/2010 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:

Allen Test Burn #2, Se Speciation - 12/6

Data Flags & Calculations:
Any analytical tests or individual analytes within a test flagged with an "X" or "1" indicate a deviation from the method quali ty system or quality control requirement. All results ar e 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 estimatio n of the uncertainty of measurement for the re sults in the report is available upon requ est. This report shall not be reproduced, ex cept in full, without the written consent of the Analytical Laborator y. 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 Labor atory Certificate of Analysis, Analytical Laboratory QC Reports, Sub-contracted Laborator y 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 Certificati ons : North Carolina (DENR) Certificate #248, South Carolina (DHEC) Laboratory ID # 99005. Contact the Analytical Laborator y 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
2010013161 ALLEN 06-Dec-10 9:30 AM Chris Williams FGD Purge Eff

2010013163 ALLEN 06-Dec-10 9:17 AM Chris Williams BioReactor 1 Inf

2010013164 ALLEN 06-Dec-10 9:35 AM Chris Williams BioReactor 2 Eff
2010013165 ALLEN 22-Nov-10 1:45 PM L. Davis Metals Trip Blank

4 Total SamplesCOC 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

Checklist:

Yes No

Yes No



### Report Sections Included:

Job Summary Report Sub-contracted Laboratory Results

Sample Identification Customer Specific Data Sheets, Reports, & Documentation

Technical Validation of Data Package Customer Database Entries

Analytical Laboratory Certificate of Analysis Test Case Narratives

Analytical Laboratory QC Report Chain of Custody

Reviewed By: Jenny A Herman Date: 12/20/2010 Yes

Electronic Data Deliverable (EDD) Sent Separately

## Certificate of Laboratory Analysis

This re p ort shall not be re p roduced, exce p t in full.
Order # J10120147

2010013161
Collection Date: 06-Dec-10 9:30 AM Site: FGD Purge Eff

Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sam p le #:

Analyst

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2010013163
Collection Date: 06-Dec-10 9:17 AM Site: BioReactor 1 Inf

Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sam p le #:

Analyst

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2010013164
Collection Date: 06-Dec-10 9:35 AM Site: BioReactor 2 Eff

Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sam p le #:

Analyst

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2010013165
Collection Date: 22-Nov-10 1:45 PM Site: Metals Trip Blank

Matrix: OTHER

Analyte Analysis Date/Time Method Units Qualifiers RDL Result Sam p le #:

Analyst

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

### December 19, 2010

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

Project: Allen – FGD Alternate Fuels Test Burn #2 - Se (LIMS # J10120147)

Dear Mr. Perkins,

Attached is the report associat ed with four (4) aqueous sa mples submitted for selenium speciation analysis on December 9, 2010. Th e samples were received on December 10, 2010 in a sealed cooler at -0.4 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 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 Alternate Fuels Test Burn #2 - Se (LIMS # J10120147)

December 19, 2010

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 December 9, 2010. The samples were received on Decem ber 10, 2010 in a sealed container at - 0.4 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 December 15, 2010. 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 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 ID Se(IV) Se(VI) SeCN MeSe(IV) SeMeUnknown SeSpecies (n)FGD Purge Eff 25.8 100 ND (<0.77) 2.8 ND (<1.2) 0 (0)BioReactor 1 Inf 12.4 64.8 ND (<0.19) 0.97 ND (<0.29) 0 (0)BioReactor 2 Eff 1.09 ND (<0.48) ND (<0.19) ND (<0.29) ND (<0.29) 0 (0)Metals Trip Blk ND (<0.039) ND (<0.097) ND (<0.038) ND (<0.058) ND (<0.058) 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 Alternate Fuels Test Burn #2 - SeContact: Jay PerkinsDate: December 19, 2010LIMS #J10120147Quality 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 0.004 0.039 0.20 0.78Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.097 0.48 1.9SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.038 0.19 0.77MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.006 0.058 0.29 1.2SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.006 0.058 0.29 1.2eMDL = Estimated Method Detection Limit*Please see narrative regarding eMDL calculationsQuality Control Summary - Certified Reference MaterialsAnalyte (μg/L) CRM True Value Result RecoverySe(IV) ICV 9.57 9.24 96.5Se(VI) ICV 9.48 8.59 90.6SeCN ICV 8.92 8.35 93.7MeSe(IV) ICV 6.47 5.51 85.2SeMe ICV 9.32 9.00 96.5LIMS #J10120147Date: December 19, 2010Report Generated by: Russell GeradsApplied Speciation and Consulting, LLCSelenium Speciation Results for Duke EnergyProject Name: Allen - FGD Alternate Fuels Test Burn #2 - SeContact: Jay PerkinsQuality Control Summary - Matrix DuplicatesAnalyte (μg/L) Sample ID Rep 1 Rep 2 Mean RPDSe(IV) Batch QC 0.803 0.554 0.678 36.7*Se(VI) Batch QC ND (<0.48) ND (<0.48) NC NCSeCN Batch QC ND (<0.19) ND (<0.19) NC NCMeSe(IV) Batch QC ND (<0.29) ND (<0.29) NC NCSeMe Batch QC ND (<0.29) ND (<0.29) NC NCND = Not detected at the applied dilutionNC = Value was not calculated due to one or more concentrations below the eMDL*Sample concentration is within 10x 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 278.0 450.3 161.7 278.0 492.7 177.0 9.0Se(VI) Batch QC 252.3 279.8 110.9 252.3 285.5 113.2 2.0SeCN Batch QC 228.8 1.5 0.6** 228.8 0.8 0.4** 57.9**The low recovery is attributed to sample induced species conversionLIMS #J10120147Date: December 19, 2010Report Generated by: Russell GeradsApplied Speciation and Consulting, LLCSelenium Speciation Results for Duke EnergyProject Name: Allen - FGD Alternate Fuels Test Burn #2 - SeContact: Jay Perkins