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: J12110239

Project Name: WWTS - Biweekly (2)

Lab Contact: Jason C Perkins

Date: 12/4/2012

Customer Address: 253 Plant Allen Road

Customer Name(s): BillK-RonL--RobnJ-DonS-RayL

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

2012024485 ALLEN 13-Nov-12 11:47 AM Chris Williams FGD Purge Eff 

2012024486 ALLEN 13-Nov-12 11:55 AM Chris Williams EQ Tank Eff 

2012024487 ALLEN 13-Nov-12 11:58 AM Chris Williams BioReactor 1 Inf 

2012024488 ALLEN 13-Nov-12 12:02 PM Chris Williams BioReactor 2 Inf 

2012024489 ALLEN 13-Nov-12 12:07 PM Chris Williams BioReactor 2 Eff 

2012024490 ALLEN 13-Nov-12 12:40 PM Chris Williams Filter Blk 

2012024491 ALLEN 18-Oct-12 8:30 AM J. TALLENT 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.

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: 12/4/2012

Electronic Data Deliverable (EDD) Sent Separately

Page 3 of 16
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12110239

2012024485

Collection Date: 13-Nov-12 11:47 AM

Site: FGD Purge Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

INORGANIC IONS BY IC

Bromide 1000 mg/L 20 200 EPA 300.0 11/20/2012 09:23 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 30.3 ug/L 2.5 50 EPA 245.1 11/15/2012 14:44 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 24.3 mg/L 0.5 10 EPA 200.7 11/27/2012 09:11 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 752 ug/L 10 10 EPA 200.8 11/29/2012 12:09 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 289 ug/L 10 10 EPA 200.8 11/28/2012 11:19 KRICHAR

Chromium (Cr) 238 ug/L 10 10 EPA 200.8 11/28/2012 11:19 KRICHAR

Copper (Cu) 348 ug/L 10 10 EPA 200.8 11/28/2012 11:19 KRICHAR

Nickel (Ni) 322 ug/L 10 10 EPA 200.8 11/28/2012 11:19 KRICHAR

Selenium (Se) 7260 ug/L 20 20 EPA 200.8 11/28/2012 11:19 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 11/28/2012 11:19 KRICHAR

Zinc (Zn) 411 ug/L 10 10 EPA 200.8 11/28/2012 11:19 KRICHAR

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

Vendor Parameter Complete Vendor Method V_AS&C

TOTAL DISSOLVED SOLIDS

TDS 9900 mg/L 200 1 SM2540C 11/20/2012 15:27 SWILLI3

2012024486

Collection Date: 13-Nov-12 11:55 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) 25.9 ug/L 2.5 50 EPA 245.1 11/15/2012 14:47 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 23.9 mg/L 0.5 10 EPA 200.7 11/27/2012 09:14 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 319 ug/L 10 10 EPA 200.8 11/29/2012 12:12 DJSULL1

Page 4 of 16
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12110239

2012024486

Collection Date: 13-Nov-12 11:55 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) 217 ug/L 10 10 EPA 200.8 11/28/2012 11:23 KRICHAR

Chromium (Cr) 199 ug/L 10 10 EPA 200.8 11/28/2012 11:23 KRICHAR

Copper (Cu) 297 ug/L 10 10 EPA 200.8 11/28/2012 11:23 KRICHAR

Nickel (Ni) 302 ug/L 10 10 EPA 200.8 11/28/2012 11:23 KRICHAR

Selenium (Se) 6210 ug/L 20 20 EPA 200.8 11/28/2012 11:23 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 11/28/2012 11:23 KRICHAR

Zinc (Zn) 375 ug/L 10 10 EPA 200.8 11/28/2012 11:23 KRICHAR

2012024487

Collection Date: 13-Nov-12 11:58 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) 27.7 mg/L 0.5 10 EPA 200.7 11/27/2012 09:18 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 974 ug/L 10 10 EPA 200.8 11/29/2012 12:15 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 11/28/2012 10:45 KRICHAR

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 11/28/2012 10:45 KRICHAR

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 11/28/2012 10:45 KRICHAR

Nickel (Ni) < 10 ug/L 10 10 EPA 200.8 11/28/2012 10:45 KRICHAR

Selenium (Se) 1130 ug/L 10 10 EPA 200.8 11/28/2012 10:45 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 11/28/2012 10:45 KRICHAR

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 11/28/2012 10:45 KRICHAR

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

Vendor Parameter Complete Vendor Method V_AS&C

2012024488

Collection Date: 13-Nov-12 12:02 PM

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) 29.7 mg/L 0.5 10 EPA 200.7 11/27/2012 09:22 MHH7131

Page 5 of 16
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12110239

2012024488

Collection Date: 13-Nov-12 12:02 PM

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 11/28/2012 10:49 KRICHAR

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 11/28/2012 10:49 KRICHAR

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 11/28/2012 10:49 KRICHAR

Nickel (Ni) < 10 ug/L 10 10 EPA 200.8 11/28/2012 10:49 KRICHAR

Selenium (Se) 23.9 ug/L 10 10 EPA 200.8 11/28/2012 10:49 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 11/28/2012 10:49 KRICHAR

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 11/28/2012 10:49 KRICHAR

2012024489

Collection Date: 13-Nov-12 12:07 PM

Site: BioReactor 2 Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

INORGANIC IONS BY IC

Bromide 730 mg/L 10 100 EPA 300.0 11/20/2012 09:42 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) < 1 ug/L 1 20 EPA 245.1 11/15/2012 14:49 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 27.4 mg/L 0.5 10 EPA 200.7 11/27/2012 09:26 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 5 ug/L 5 5 EPA 200.8 11/28/2012 10:52 KRICHAR

Chromium (Cr) < 5 ug/L 5 5 EPA 200.8 11/28/2012 10:52 KRICHAR

Copper (Cu) < 5 ug/L 5 5 EPA 200.8 11/28/2012 10:52 KRICHAR

Nickel (Ni) < 5 ug/L 5 5 EPA 200.8 11/28/2012 10:52 KRICHAR

Selenium (Se) 9.36 ug/L 5 5 EPA 200.8 11/28/2012 10:52 KRICHAR

Silver (Ag) < 5 ug/L 5 5 EPA 200.8 11/28/2012 10:52 KRICHAR

Zinc (Zn) < 5 ug/L 5 5 EPA 200.8 11/28/2012 10:52 KRICHAR

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

Vendor Parameter Complete Vendor Method V_AS&C

2012024490

Collection Date: 13-Nov-12 12:40 PM

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 11/29/2012 11:43 DJSULL1

Page 6 of 16
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12110239

2012024491

Collection Date: 18-Oct-12 8:30 AM

Site: TRIP BLANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

TOTAL RECOVERABLE METALS BY ICP

Boron (B) < 0.05 mg/L 0.05 1 EPA 200.7 11/27/2012 09:07 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 1 ug/L 1 1 EPA 200.8 11/28/2012 10:35 KRICHAR

Chromium (Cr) < 1 ug/L 1 1 EPA 200.8 11/28/2012 10:35 KRICHAR

Copper (Cu) < 1 ug/L 1 1 EPA 200.8 11/28/2012 10:35 KRICHAR

Nickel (Ni) < 1 ug/L 1 1 EPA 200.8 11/28/2012 10:35 KRICHAR

Selenium (Se) < 1 ug/L 1 1 EPA 200.8 11/28/2012 10:35 KRICHAR

Silver (Ag) < 1 ug/L 1 1 EPA 200.8 11/28/2012 10:35 KRICHAR

Zinc (Zn) < 1 ug/L 1 1 EPA 200.8 11/28/2012 10:35 KRICHAR

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

Vendor Parameter Complete Vendor Method V_AS&C

Page 7 of 16
 

November 27, 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 #J12110239) 

Dear Mr. Perkins, 

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

speciation on November 15, 2012. The samples were received in a sealed cooler at -0.1°C on 

November 16, 2012. 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, 

 

 Russell Gerads 

Vice President 

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 (2010, Bi-Monthly Sampling) (LIMS #J12110239) 

November 27, 2012 

1. Sample Reception 

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

Consulting) were submitted for selenium speciation analysis on November 15, 2012. The 

samples were received on November 16, 2012 in a sealed container at -0.1°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 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 an 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 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 minimum interval 

of every ten analytical runs. 

Selenium Speciation Analysis by IC-ICP-DRC-MS Each sample for selenium speciation 

analysis was analyzed by ion chromatography inductively coupled plasma dynamic reaction 

cell mass spectrometry (IC-ICP-DRC-MS) on November 19, 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 (DRC) 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. 

The selenocyanate matrix spike and matrix spike duplicate sample recoveries (35.8% and 

39.5%, respectively) were below the lower control limit of 75%. The spiking solution also 

contained selenite, and the spike recoveries for selenite (169.0% and 167.1%, respectively) 

were greater than the upper control limit of 125%. An acceptable mass balance of selenium 

species was obtained; the sum of species was calculated in each case yielding values of 

103.6% and 104.6%. The apparent conversion of selenocyanate to selenite is indicative of an 

oxidizing matrix in the samples. Selenium species conversion was not observed in the 

bracketing continuing calibration verification standards (CCV), demonstrating adequate 

stability of selenium species within the analytical platform. No corrective actions were 

required. 

All other quality control parameters associated with the samples were within acceptance 

limits. 

Page 10 of 16
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, 

Russell Gerads 

Vice President 

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 500 112 116 25.5 ND (<1.6) 14.5 (2)

BioReactor 1 Inf 713 247 ND (<0.49) 32.1 ND (<0.40) 10.1 (2)

BioReactor 2 Eff ND (<0.25) ND (<0.45) ND (<0.49) ND (<0.40) ND (<0.40) 0.84 (1)

Metals Trip Blk ND (<0.050) ND (<0.091) ND (<0.097) ND (<0.079) ND (<0.079) 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

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: November 27, 2012

LIMS #J12110239

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 0.0050 0.050 0.25 1.0

Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.0091 0.091 0.45 1.8

SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.0097 0.097 0.49 1.9

MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.0079 0.079 0.40 1.6

SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.0079 0.079 0.40 1.6

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 9.74 101.8

Se(VI) LCS 9.48 9.48 100.1

SeCN LCS 8.92 8.98 100.6

MeSe(IV) LCS 6.47 6.43 99.3

SeMe LCS 9.32 9.09 97.5

LIMS #J12110239

Date: November 27, 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 13 of 16
Quality Control Summary - Matrix Duplicates

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

Se(IV) Batch QC 23.9 20.9 22.4 13.4

Se(VI) Batch QC 73.8 72.2 73.0 2.1

SeCN Batch QC ND (<1.9) ND (<1.9) NC NC

MeSe(IV) Batch QC 3.5 3.3 3.4 5.5

SeMe Batch QC ND (<1.6) ND (<1.6) 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) Batch QC 1112 1902 169.0 * 1112 1880 167.1 * 1.1

Se(VI) Batch QC 1009 1142 106.0 1009 1155 107.3 1.2

SeCN Batch QC 915.0 327.2 35.8 * 915.0 361.5 39.5 * 10.0

*Low/high recovery is attributed to matrix induced species conversion

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

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

Contact: Jay Perkins

LIMS #J12110239

Date: November 27, 2012

Report Generated by: Russell Gerads

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