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: J10120227

Lab Contact: Jason C Perkins

Date: 12/31/2010

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:

Se Speciation - 12/8

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. 

Analytical Laboratory 

Page 1 of 13
Sample ID's & Descriptions:

Sample ID Plant/Station

Collection 

Date and Time Collected By Sample Description

2010013394 ALLEN 08-Dec-10 8:50 AM Chuck Moose FGD Purge Eff 

2010013395 ALLEN 08-Dec-10 9:15 AM Jeff Womack BioReactor 1 Inf 

2010013396 ALLEN 08-Dec-10 9:21 AM Jeff Womack BioReactor 2 Eff 

2010013397 ALLEN 22-Nov-10 1:45 PM L. Davis TRIP BLANK 

4 Total Samples

Analytical Laboratory 

Page 2 of 13
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

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: 12/31/2010

Yes

Electronic Data Deliverable (EDD) Sent Separately

Analytical Laboratory 

Page 3 of 13
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J10120227

2010013394

Collection Date: 08-Dec-10 8:50 AM

Site: FGD Purge Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2010013395

Collection Date: 08-Dec-10 9:15 AM

Site: BioReactor 1 Inf 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2010013396

Collection Date: 08-Dec-10 9:21 AM

Site: BioReactor 2 Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2010013397

Collection Date: 22-Nov-10 1:45 PM

Site: TRIP BLANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

Analytical Laboratory 

Page 4 of 13
 

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 # J10120227) 

Dear Mr. Perkins, 

Attached is the report associated with four (4) aqueous samples submitted for selenium 

speciation analysis on December 9, 2010. The samples were received on December 10, 

2010 in a sealed cooler at -0.4o

C. Selenium speciation analysis was performed via ion 

chromatography inductively coupled plasma dynamic reaction cell mass spectrometry 

(IC-ICP-DRC-MS). Any analytical issues associated 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 

Analytical Laboratory 

Page 5 of 13
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 # J10120227) 

December 19, 2010 

1. Sample Reception 

Four (4) aqueous samples in 125mL HDPE bottles (provided by Applied Speciation 

and Consulting) were submitted for selenium speciation analysis on December 9, 

2010. The samples were received on December 10, 2010 in a sealed container at -

0.4o

C. 

The samples were received in a laminar flow clean hood void of trace metals 

contamination and ultra-violet radiation. 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 -80o

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 the samples may shift the equilibrium of the system resulting in 

changes in speciation ratios. 

Analytical Laboratory 

Page 6 of 13
3. Sample Analysis 

All sample analysis is precluded 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. 

Prior to sample analysis, all calibration curves are verified using second source 

standards 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 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 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 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 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 

Analytical Laboratory 

Page 7 of 13
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, LLC 

Analytical Laboratory 

Page 8 of 13
Sample Results

Sample ID Se(IV) Se(VI) SeCN MeSe(IV) SeMe

Unkn

Spec

FGD Purge Eff 247 94.7 ND (<0.77) 6.0 ND (<1.2) 0 

BioReactor 1 Inf 12.0 70.3 ND (<0.19) 2.45 0.69 0 

BioReactor 2 Eff 0.80 ND (<0.48) ND (<0.19) ND (<0.29) ND (<0.29) 0 Metals Trip Blk ND (<0.039) ND (<0.097) ND (<0.038) ND (<0.058) ND (<0.058) 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 observed

Report Generated by: Russell Gerads

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Allen - FGD Alternate Fuels Test Burn #2 - Se

Contact: Jay Perkins

Date: December 19, 2010

LIMS #J10120227
Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 10x eSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.039 Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.097 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.038 MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.006 0.058 SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.006 0.058 eMDL = 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 96.5

LIMS #J10120227

Date: December 19, 2010

Report Generated by: Russell Gerads

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Allen - FGD Alternate Fuels Test Burn #2 - Se

Contact: Jay Perkins
Quality Control Summary - Matrix Duplicates

Analyte (μg/L) Sample ID Rep 1 Rep 2 Mean RPDSe(IV) BioReactor 2 Eff 0.803 0.554 0.678 36.7*Se(VI) BioReactor 2 Eff ND (<0.48) ND (<0.48) NC NCSeCN BioReactor 2 Eff ND (<0.19) ND (<0.19) NC NCMeSe(IV) BioReactor 2 Eff ND (<0.29) ND (<0.29) NC NCSeMe BioReactor 2 Eff 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) BioReactor 2 Eff 278.0 450.3 161.7 278.0 492.7 177.0 9.0Se(VI) BioReactor 2 Eff 252.3 279.8 110.9 252.3 285.5 113.2 2.0SeCN BioReactor 2 Eff 228.8 1.5 0.6** 228.8 0.8 0.4** 57.9**The low recovery is attributed to sample induced species conversion

LIMS #J10120227

Date: December 19, 2010

Report Generated by: Russell Gerads

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Allen - FGD Alternate Fuels Test Burn #2 - Se

Contact: Jay Perkins
Analytical Laboratory 

Page 12 of 13
Analytical Laboratory 

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