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: J12100064

Lab Contact: Jason C Perkins

Date: 10/16/2012

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:

Please contact the Program Manager (Jason C Perkins) with any questions regarding this report.

Data Flags & Calculations:

Any analytical tests or individual analytes within a test flagged with a Qualifier indicate a deviation from the method quality 

system or quality control requirement. The qualifier description is found at the end of the Certificate of Analysis (sample results) 

under the qualifiers heading. All results are reported on a dry weight basis unless otherwise noted. Subcontracted data 

included on the Duke Certificate of Analysis is to be used as information only. Certified vendor results can be found in the 

subcontracted lab final report. Duke Energy Analytical Laboratory subcontracts analyses to other vendor laboratories that have 

been qualified by Duke Energy to perform these analyses except where 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. 

Page 1 of 16
Sample ID's & Descriptions:

Sample ID Plant/Station

Collection 

Date and Time Collected By Sample Description

2012020952 ALLEN 28-Sep-12 9:00 AM Matt Campbell FGD Purge Eff 

2012020953 ALLEN 28-Sep-12 9:10 AM Matt Campbell EQ Tank Eff 

2012020954 ALLEN 28-Sep-12 9:15 AM Matt Campbell BioReactor 1 Inf 

2012020955 ALLEN 28-Sep-12 9:20 AM Matt Campbell BioReactor 2 Inf 

2012020956 ALLEN 28-Sep-12 9:25 AM Matt Campbell BioReactor 2 Eff 

2012020957 ALLEN 28-Sep-12 9:45 AM Matt Campbell Filter Blk 

6 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.

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

Analytical Laboratory QC Report

Chain of Custody

Reviewed By: DBA Account Date: 10/16/2012

Electronic Data Deliverable (EDD) Sent Separately

Page 3 of 16
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12100064

2012020952

Collection Date: 28-Sep-12 9:00 AM

Site: FGD Purge Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

INORGANIC IONS BY IC

Bromide 410 mg/L 50 500 EPA 300.0 10/09/2012 09:29 JAHERMA

Chloride 1100 mg/L 50 500 EPA 300.0 10/09/2012 09:29 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 16.2 ug/L 2.5 50 EPA 245.1 10/04/2012 14:48 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 28.9 mg/L 0.5 10 EPA 200.7 10/04/2012 09:49 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 2420 ug/L 10 10 EPA 200.8 10/04/2012 11:26 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 196 ug/L 10 10 EPA 200.8 10/04/2012 10:30 KRICHAR

Chromium (Cr) 172 ug/L 10 10 EPA 200.8 10/04/2012 10:30 KRICHAR

Copper (Cu) 182 ug/L 10 10 EPA 200.8 10/04/2012 10:30 KRICHAR

Nickel (Ni) 251 ug/L 10 10 EPA 200.8 10/04/2012 10:30 KRICHAR

Selenium (Se) 3650 ug/L 10 10 EPA 200.8 10/04/2012 10:30 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 10/04/2012 10:30 KRICHAR

Zinc (Zn) 240 ug/L 10 10 EPA 200.8 10/04/2012 10:30 KRICHAR

SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC)

Vendor Parameter Complete Vendor Method V_AS&C

TOTAL DISSOLVED SOLIDS

TDS 6100 mg/L 200 1 SM2540C 10/03/2012 15:30 TJA7067

2012020953

Collection Date: 28-Sep-12 9:10 AM

Site: EQ Tank Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 10.5 ug/L 2.5 50 EPA 245.1 10/04/2012 14:51 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 34.4 mg/L 0.5 10 EPA 200.7 10/04/2012 09:53 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 1790 ug/L 10 10 EPA 200.8 10/04/2012 11:29 KRICHAR

Page 4 of 16
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12100064

2012020953

Collection Date: 28-Sep-12 9:10 AM

Site: EQ Tank Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 85.1 ug/L 10 10 EPA 200.8 10/04/2012 10:33 KRICHAR

Chromium (Cr) 88.9 ug/L 10 10 EPA 200.8 10/04/2012 10:33 KRICHAR

Copper (Cu) 96.2 ug/L 10 10 EPA 200.8 10/04/2012 10:33 KRICHAR

Nickel (Ni) 172 ug/L 10 10 EPA 200.8 10/04/2012 10:33 KRICHAR

Selenium (Se) 2390 ug/L 10 10 EPA 200.8 10/04/2012 10:33 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 10/04/2012 10:33 KRICHAR

Zinc (Zn) 138 ug/L 10 10 EPA 200.8 10/04/2012 10:33 KRICHAR

2012020954

Collection Date: 28-Sep-12 9:15 AM

Site: BioReactor 1 Inf 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 38.0 mg/L 0.5 10 EPA 200.7 10/04/2012 10:04 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 1430 ug/L 10 10 EPA 200.8 10/04/2012 11:33 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 10/04/2012 10:36 KRICHAR

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 10/04/2012 10:36 KRICHAR

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 10/04/2012 10:36 KRICHAR

Nickel (Ni) < 10 ug/L 10 10 EPA 200.8 10/04/2012 10:36 KRICHAR

Selenium (Se) 1560 ug/L 10 10 EPA 200.8 10/04/2012 10:36 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 10/04/2012 10:36 KRICHAR

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 10/04/2012 10:36 KRICHAR

SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC)

Vendor Parameter Complete Vendor Method V_AS&C

2012020955

Collection Date: 28-Sep-12 9:20 AM

Site: BioReactor 2 Inf 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 46.0 mg/L 0.5 10 EPA 200.7 10/04/2012 10:08 MHH7131

Page 5 of 16
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12100064

2012020955

Collection Date: 28-Sep-12 9:20 AM

Site: BioReactor 2 Inf 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 10/04/2012 10:39 KRICHAR

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 10/04/2012 10:39 KRICHAR

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 10/04/2012 10:39 KRICHAR

Nickel (Ni) < 10 ug/L 10 10 EPA 200.8 10/04/2012 10:39 KRICHAR

Selenium (Se) 65.5 ug/L 10 10 EPA 200.8 10/04/2012 10:39 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 10/04/2012 10:39 KRICHAR

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 10/04/2012 10:39 KRICHAR

2012020956

Collection Date: 28-Sep-12 9:25 AM

Site: BioReactor 2 Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

INORGANIC IONS BY IC

Bromide 470 mg/L 50 500 EPA 300.0 10/09/2012 09:46 JAHERMA

Chloride 1400 mg/L 50 500 EPA 300.0 10/09/2012 09:46 JAHERMA

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 67.3 mg/L 0.5 10 EPA 200.7 10/04/2012 10:12 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 5 ug/L 5 5 EPA 200.8 10/04/2012 10:43 KRICHAR

Chromium (Cr) < 5 ug/L 5 5 EPA 200.8 10/04/2012 10:43 KRICHAR

Copper (Cu) < 5 ug/L 5 5 EPA 200.8 10/04/2012 10:43 KRICHAR

Nickel (Ni) < 5 ug/L 5 5 EPA 200.8 10/04/2012 10:43 KRICHAR

Selenium (Se) 10.2 ug/L 5 5 EPA 200.8 10/04/2012 10:43 KRICHAR

Silver (Ag) < 5 ug/L 5 5 EPA 200.8 10/04/2012 10:43 KRICHAR

Zinc (Zn) < 5 ug/L 5 5 EPA 200.8 10/04/2012 10:43 KRICHAR

SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC)

Vendor Parameter Complete Vendor Method V_AS&C

2012020957

Collection Date: 28-Sep-12 9:45 AM

Site: Filter Blk 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

DISSOLVED METALS BY ICP-MS

Selenium (Se) < 1 ug/L 1 1 EPA 200.8 10/04/2012 11:11 KRICHAR

Page 6 of 16
 

October 15, 2012 

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 (2010, Bi-Monthly Sampling) (LIMS #J12100064) 

Dear Mr. Perkins, 

Attached is the report associated with three (3) aqueous samples submitted for selenium 

speciation analysis on October 4, 2012. The samples were received in a sealed cooler at 0.6°C 

on October 5, 2012. Selenium speciation analysis was performed via ion chromatography 

inductively coupled plasma collision reaction cell mass spectrometry (IC-ICP-CRC-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, 

 

 Russell Gerads 

Vice President 

Applied Speciation and Consulting, LLC 

 

 

Page 7 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 (2010, Bi-Monthly Sampling) (LIMS #J12100064) 

October 15, 2012 

1. Sample Reception 

Three (3) aqueous samples in 125mL HDPE bottles (provided by Applied Speciation and 

Consulting) were submitted for selenium speciation analysis on October 4, 2012. The 

samples were received on October 5, 2012 in a sealed container at 0.6°C. 

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

and ultra-violet radiation, and were designated discrete sample identifiers. An aliquot of 

each sample was filtered (0.45μm) and each filtrate was 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 collision reaction cell 

mass spectrometry (IC-ICP-CRC-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-CRC-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 

a sample 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 8 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-CRC-MS Each sample for selenium speciation 

analysis was analyzed by ion chromatography inductively coupled plasma collision reaction 

cell mass spectrometry (IC-ICP-CRC-MS) on October 8-9, 2012. 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 (CRC) containing a reaction 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 well and no significant analytical issues were encountered. All 

quality control parameters associated with the 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 contain 

methylseleninic acid or selenomethionine due to impurities in these standards which would 

bias the results for other selenium species. 

Page 9 of 16
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 

Page 10 of 16
Sample Results

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

Unknown Se 

Species (n)

FGD Purge Eff 430 1610 20.0 ND (<1.4) ND (<1.4) 40.9 (1)

BioReactor 1 Inf 33.8 1290 ND (<0.17) 0.55 ND (<0.35) 0.0 (0)

BioReactor 2 Eff 0.64 ND (<0.57) ND (<0.17) ND (<0.35) ND (<0.35) 0.0 (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: Russell Gerads

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Allen - FGD WWTS (2010, Bi-Monthly Sampling)

Contact: Jay Perkins

Date: October 15, 2012

LIMS #J12100064

Page 11 of 16
Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 250x

Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.0012 0.30

Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.0023 0.57

SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.0007 0.17

MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.0014 0.35

SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.0014 0.35

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 8.79 98.5

MeSe(IV) LCS 6.47 6.40 99.0

SeMe LCS 9.32 8.81 94.5

LIMS #J12100064

Date: October 15, 2012

Report Generated by: Russell Gerads

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Allen - FGD WWTS (2010, Bi-Monthly Sampling)

Contact: Jay Perkins

Page 12 of 16
Quality Control Summary - Matrix Duplicates

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

Se(IV) BioReactor 1 Inf 33.83 34.21 34.02 1.1

Se(VI) BioReactor 1 Inf 1293 1298 1295 0.3

SeCN BioReactor 1 Inf ND (<0.17) ND (<0.17) NC NC

MeSe(IV) BioReactor 1 Inf 0.55 0.42 0.48 27.4*

SeMe BioReactor 1 Inf ND (<0.35) ND (<0.35) NC NC

ND = Not detected at the applied dilution

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

*Associated results were less than 10 times the MDL

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 1 Inf 1390 1526 107.4 1390 1527 107.4 0.1

Se(VI) BioReactor 1 Inf 1261 2749 115.2 1261 2568 100.9 6.8

SeCN BioReactor 1 Inf 1144 1168 102.1 1144 1175 102.7 0.6

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Allen - FGD WWTS (2010, Bi-Monthly Sampling)

Contact: Jay Perkins

LIMS #J12100064

Date: October 15, 2012

Report Generated by: Russell Gerads

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