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: J11070314

Lab Contact: Jason C Perkins

Date: 8/9/2011

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:

FGD BiMonthly

No bottles were received for Br. The COC had Br checked.

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

2011015795 ALLEN 25-Jul-11 8:22 AM Jeff Womack FGD Purge Eff 

2011015796 ALLEN 25-Jul-11 8:37 AM Jeff Womack EQ Tank Eff 

2011015797 ALLEN 25-Jul-11 8:33 AM Jeff Womack BioReactor 1 Inf 

2011015798 ALLEN 25-Jul-11 8:50 AM Jeff Womack BioReactor 2 Inf 

2011015799 ALLEN 25-Jul-11 8:41 AM Jeff Womack BioReactor 2 Eff 

2011015800 ALLEN 19-Jul-11 9:30 AM L. Davis Filter Blk 

2011015801 ALLEN 19-Jul-11 9:30 AM L. Davis Metals Trip Blank 

7 Total Samples

Page 2 of 16
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: DataBase Administrator Date: 8/9/2011

Yes

Electronic Data Deliverable (EDD) Sent Separately

Page 3 of 16
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11070314

2011015795

Collection Date: 25-Jul-11 8:22 AM

Site: FGD Purge Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 60.5 ug/L EPA 245.1 2.5 28-Jul-11 14:14 MHH7131

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 55.1 mg/L EPA 200.7 0.5 29-Jul-11 11:27 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 222 ug/L EPA 200.8 10 01-Aug-11 11:47 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 185 ug/L EPA 200.8 10 03-Aug-11 11:29 MHH7131

Chromium (Cr) 121 ug/L 10 EPA 200.8 03-Aug-11 11:29 MHH7131

Copper (Cu) 132 ug/L 10 EPA 200.8 03-Aug-11 11:29 MHH7131

Nickel (Ni) 154 ug/L 10 EPA 200.8 03-Aug-11 11:29 MHH7131

Selenium (Se) 1350 ug/L 10 EPA 200.8 03-Aug-11 11:29 MHH7131

Silver (Ag) < 10 ug/L 10 EPA 200.8 03-Aug-11 11:29 MHH7131

Zinc (Zn) 167 ug/L 20 EPA 200.8 03-Aug-11 11:29 MHH7131

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

TOTAL DISSOLVED SOLIDS

TDS 13000 mg/L SM2540C 200 28-Jul-11 15:15 TJA7067

2011015796

Collection Date: 25-Jul-11 8:37 AM

Site: EQ Tank Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 48.8 ug/L EPA 245.1 2.5 28-Jul-11 14:17 MHH7131

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 62.0 mg/L EPA 200.7 0.5 29-Jul-11 11:31 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 222 ug/L EPA 200.8 10 01-Aug-11 11:50 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 161 ug/L EPA 200.8 10 03-Aug-11 11:32 MHH7131

Chromium (Cr) 105 ug/L 10 EPA 200.8 03-Aug-11 11:32 MHH7131

Copper (Cu) 119 ug/L 10 EPA 200.8 03-Aug-11 11:32 MHH7131

Nickel (Ni) 144 ug/L 10 EPA 200.8 03-Aug-11 11:32 MHH7131

Page 4 of 16
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11070314

2011015796

Collection Date: 25-Jul-11 8:37 AM

Site: EQ Tank Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

TOTAL RECOVERABLE METALS BY ICP-MS

Selenium (Se) 1150 ug/L EPA 200.8 10 03-Aug-11 11:32 MHH7131

Silver (Ag) < 10 ug/L 10 EPA 200.8 03-Aug-11 11:32 MHH7131

Zinc (Zn) 151 ug/L 20 EPA 200.8 03-Aug-11 11:32 MHH7131

2011015797

Collection Date: 25-Jul-11 8:33 AM

Site: BioReactor 1 Inf 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 70.2 mg/L EPA 200.7 0.5 29-Jul-11 11:35 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 351 ug/L EPA 200.8 10 01-Aug-11 11:53 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L EPA 200.8 10 03-Aug-11 11:35 MHH7131

Chromium (Cr) < 10 ug/L 10 EPA 200.8 03-Aug-11 11:35 MHH7131

Copper (Cu) < 10 ug/L 10 EPA 200.8 03-Aug-11 11:35 MHH7131

Nickel (Ni) < 10 ug/L 10 EPA 200.8 03-Aug-11 11:35 MHH7131

Selenium (Se) 343 ug/L 10 EPA 200.8 03-Aug-11 11:35 MHH7131

Silver (Ag) < 10 ug/L 10 EPA 200.8 03-Aug-11 11:35 MHH7131

Zinc (Zn) < 20 ug/L 20 EPA 200.8 03-Aug-11 11:35 MHH7131

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2011015798

Collection Date: 25-Jul-11 8:50 AM

Site: BioReactor 2 Inf 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 69.7 mg/L EPA 200.7 0.5 29-Jul-11 11:39 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L EPA 200.8 10 03-Aug-11 11:38 MHH7131

Chromium (Cr) < 10 ug/L 10 EPA 200.8 03-Aug-11 11:38 MHH7131

Copper (Cu) < 10 ug/L 10 EPA 200.8 03-Aug-11 11:38 MHH7131

Nickel (Ni) < 10 ug/L 10 EPA 200.8 03-Aug-11 11:38 MHH7131

Selenium (Se) 15.3 ug/L 10 EPA 200.8 03-Aug-11 11:38 MHH7131

Silver (Ag) < 10 ug/L 10 EPA 200.8 03-Aug-11 11:38 MHH7131

Zinc (Zn) < 20 ug/L 20 EPA 200.8 03-Aug-11 11:38 MHH7131

Page 5 of 16
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11070314

2011015799

Collection Date: 25-Jul-11 8:41 AM

Site: BioReactor 2 Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) < 1 ug/L EPA 245.1 1 28-Jul-11 14:19 MHH7131

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 76.0 mg/L EPA 200.7 0.5 29-Jul-11 11:43 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 5 ug/L EPA 200.8 5 03-Aug-11 11:41 MHH7131

Chromium (Cr) < 5 ug/L 5 EPA 200.8 03-Aug-11 11:41 MHH7131

Copper (Cu) < 5 ug/L 5 EPA 200.8 03-Aug-11 11:41 MHH7131

Nickel (Ni) < 5 ug/L 5 EPA 200.8 03-Aug-11 11:41 MHH7131

Selenium (Se) < 5 ug/L 5 EPA 200.8 03-Aug-11 11:41 MHH7131

Silver (Ag) < 5 ug/L 5 EPA 200.8 03-Aug-11 11:41 MHH7131

Zinc (Zn) < 10 ug/L 10 EPA 200.8 03-Aug-11 11:41 MHH7131

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2011015800

Collection Date: 19-Jul-11 9:30 AM

Site: Filter Blk 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

DISSOLVED METALS BY ICP-MS

Selenium (Se) < 2 ug/L EPA 200.8 2 01-Aug-11 11:34 KRICHAR

2011015801

Collection Date: 19-Jul-11 9:30 AM

Site: Metals Trip Blank 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

TOTAL RECOVERABLE METALS BY ICP

Boron (B) < 0.05 mg/L EPA 200.7 0.05 29-Jul-11 11:19 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 1 ug/L EPA 200.8 1 03-Aug-11 11:23 MHH7131

Chromium (Cr) < 1 ug/L 1 EPA 200.8 03-Aug-11 11:23 MHH7131

Copper (Cu) < 1 ug/L 1 EPA 200.8 03-Aug-11 11:23 MHH7131

Nickel (Ni) < 1 ug/L 1 EPA 200.8 03-Aug-11 11:23 MHH7131

Selenium (Se) < 1 ug/L 1 EPA 200.8 03-Aug-11 11:23 MHH7131

Silver (Ag) < 1 ug/L 1 EPA 200.8 03-Aug-11 11:23 MHH7131

Zinc (Zn) < 2 ug/L 2 EPA 200.8 03-Aug-11 11:23 MHH7131

SELENIUM SPECIATION

Page 6 of 16
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11070314

2011015801

Collection Date: 19-Jul-11 9:30 AM

Site: Metals Trip Blank 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

Page 7 of 16
 

August 8, 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 (Bi-Weekly Sampling) (LIMS # J11070314) 

Dear Mr. Perkins, 

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

speciation analysis on July 28, 2011. The samples were received in a sealed cooler at -0.3

oC on 

July 29, 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. 

If you have any questions, please feel free to contact me at your convenience. 

 Sincerely, 

 

 Ben Wozniak

 Project Manager 

 Applied Speciation and Consulting, LLC 

 

Page 8 of 16
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 (Bi-Weekly Sampling) (LIMS # J11070314) 

August 8, 2011 

1. Sample Reception 

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

Consulting) were submitted for selenium speciation analysis on July 28, 2011. The samples 

were received on July 29, 2011 in a sealed container at -0.3oC.

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 -80oC) 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. 

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 

Page 9 of 16
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 August 2, 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 very well and no significant analytical issues were encountered. 

All sample results have been corrected in accordance with the continuing calibration 

verification recoveries to account for perceived instrument bias. All quality control 

parameters associated with these samples were within acceptance limits with the following 

exceptions: 

The recoveries associated with the matrix spike (MS) and matrix spike duplicate (MSD) 

performed on the sample identified as BioReactor 2 Eff were below the established control 

limit of 75% for selenocyanate (0.0% for both). The MS and MSD also included selenite in 

the spiking solution which yielded elevated recoveries (168.2% and 166.0%, respectively). 

The low recoveries for selenocyanate correlate with the elevated recoveries of selenite 

suggesting that the sample matrix induces species conversion. The fact that no species 

conversion was observed in the ICV or CCVs, which contain both selenite and 

selenocyanate, demonstrates that the applied method stabilizes these selenium species in 

solution. Since the conversion of selenocyanate to selenite in the MS and MSD is a function 

of the sample matrix and the recoveries confirm a mass balance, no corrective action was 

Page 10 of 16
required. The reported results are deemed representative of the supplied samples and suggest 

that selenocyanate is not stable in the spiked sample matrix. 

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. 

If you have any questions or concerns regarding this report, please feel free to contact me. 

Sincerely, 

Ben Wozniak 

Project Manager 

Applied Speciation and Consulting, LLC 

Page 11 of 16
Sample Results

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

Unknown Se 

Species (n)

FGD Purge Eff 62.2 163 ND (<1.9) 7.4 ND (<4.4) 0 (0)

BioReactor 1 Inf 7.93 254 ND (<0.49) ND (<1.1) ND (<1.1) 0 (0)

BioReactor 2 Eff 3.70 ND (<1.9) ND (<0.49) ND (<1.1) ND (<1.1) 0 (0)

Metals Trip Blk ND (<0.17) ND (<0.38) ND (<0.10) ND (<0.22) ND (<0.22) 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: Ben Wozniak

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Allen - FGD WWTS (Bi-Weekly Sampling)

Contact: Jay Perkins

Date: August 8, 2011

LIMS #J11070314

Page 12 of 16
Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 10x eMDL 50x eMDL 200x

Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.017 0.17 0.87 3.5

Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.038 0.38 1.9 7.7

SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.010 0.10 0.49 1.9

MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.022 0.22 1.1 4.4

SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.022 0.22 1.1 4.4

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 9.57 9.48 99.0

Se(VI) LCS 9.48 9.42 99.4

SeCN LCS 8.92 9.10 102.0

MeSe(IV) LCS 6.47 6.53 100.9

SeMe LCS 9.32 8.74 93.7

Selenium Speciation Results for Duke Energy

Project Name: Allen - FGD WWTS (Bi-Weekly Sampling)

Contact: Jay Perkins

LIMS #J11070314

Date: August 8, 2011

Report Generated by: Ben Wozniak

Applied Speciation and Consulting, LLC

Page 13 of 16
Quality Control Summary - Matrix Duplicates

Analyte (μg/L) Sample ID Rep 1 Rep 2 Mean RPD

Se(IV) BioReactor 2 Eff 3.70 3.78 3.74 2.0

Se(VI) BioReactor 2 Eff ND (<1.9) ND (<1.9) NC NC

SeCN BioReactor 2 Eff ND (<0.49) ND (<0.49) NC NC

MeSe(IV) BioReactor 2 Eff ND (<1.1) ND (<1.1) NC NC

SeMe BioReactor 2 Eff ND (<1.1) ND (<1.1) 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) BioReactor 2 Eff 278.0 471.4 168.2* 278.0 465.3 166.0* 1.3

Se(VI) BioReactor 2 Eff 252.3 225.8 89.5 252.3 222.5 88.2 1.5

SeCN BioReactor 2 Eff 228.8 ND (<0.49) 0.0* 228.8 ND (<0.49) 0.0* NC

* The recovery is outside the established control limit of 75-125%; please see narrative

NC = Value was not calculated due to one or more concentrations below the eMDL

Date: August 8, 2011

Report Generated by: Ben Wozniak

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Allen - FGD WWTS (Bi-Weekly Sampling)

Contact: Jay Perkins

LIMS #J11070314

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