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: J12010230

Project Name: WWTS - Biweekly

Lab Contact: Jason C Perkins

Date: 2/8/2012

Customer Address: 3195 Pine Hall Rd

Customer Name(s): Bill Kennedy, Melonie Martin, Wayne Chapman, Tom Johnson

Mailcode: Belews Steam Station

Belews Creek, 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.

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

2012001138 BELEWS 25-Jan-12 9:00 AM dean m FGD Purge Eff 

2012001139 BELEWS 25-Jan-12 9:00 AM dean m EQ TANK EFF. 

2012001140 BELEWS 25-Jan-12 9:00 AM dean m BIOREACTOR 1 INF. 

2012001141 BELEWS 25-Jan-12 9:00 AM dean m BIOREACTOR 2 INF. 

2012001142 BELEWS 25-Jan-12 9:00 AM dean m BIOREACTOR 2 EFF. 

2012001143 BELEWS 25-Jan-12 9:00 AM dean m FILTER BLANK 

2012001144 BELEWS 25-Jan-12 9:00 AM dean m 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

Analytical Laboratory QC Report

Chain of Custody

Reviewed By: DataBase Administrator Date: 2/8/2012

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 # J12010230

2012001138

Collection Date: 25-Jan-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 89 mg/L 5 50 EPA 300.0 31-Jan-12 13:15 JAHERMA

Fluoride 8.4 mg/L 5 50 EPA 300.0 31-Jan-12 13:15 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 180 ug/L 5 100 EPA 245.1 03-Feb-12 08:48 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 173 mg/L 0.5 10 EPA 200.7 03-Feb-12 13:37 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 167 ug/L 2 2 EPA 200.8 06-Feb-12 13:26 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 200 ug/L 10 10 EPA 200.8 06-Feb-12 13:09 DJSULL1

Chromium (Cr) 220 ug/L 10 10 EPA 200.8 06-Feb-12 13:09 DJSULL1

Copper (Cu) 134 ug/L 10 10 EPA 200.8 06-Feb-12 13:09 DJSULL1

Nickel (Ni) 215 ug/L 10 10 EPA 200.8 06-Feb-12 13:09 DJSULL1

Selenium (Se) 3480 ug/L 10 10 EPA 200.8 06-Feb-12 13:09 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 06-Feb-12 13:09 DJSULL1

Zinc (Zn) 255 ug/L 20 10 EPA 200.8 06-Feb-12 13:09 DJSULL1

Arsenic Speciation

Vendor Parameter Complete 1 V_AS&C

TOTAL DISSOLVED SOLIDS

TDS 14000 mg/L 200 1 SM2540C 26-Jan-12 16:00 TJA7067

2012001139

Collection Date: 25-Jan-12 9:00 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) 120 ug/L 2.5 50 EPA 245.1 03-Feb-12 08:50 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 172 mg/L 0.5 10 EPA 200.7 03-Feb-12 13:41 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 98.4 ug/L 2 2 EPA 200.8 06-Feb-12 13:29 DJSULL1

Page 4 of 16
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12010230

2012001139

Collection Date: 25-Jan-12 9:00 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) 160 ug/L 10 10 EPA 200.8 06-Feb-12 13:12 DJSULL1

Chromium (Cr) 167 ug/L 10 10 EPA 200.8 06-Feb-12 13:12 DJSULL1

Copper (Cu) 104 ug/L 10 10 EPA 200.8 06-Feb-12 13:12 DJSULL1

Nickel (Ni) 197 ug/L 10 10 EPA 200.8 06-Feb-12 13:12 DJSULL1

Selenium (Se) 2460 ug/L 10 10 EPA 200.8 06-Feb-12 13:12 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 06-Feb-12 13:12 DJSULL1

Zinc (Zn) 210 ug/L 20 10 EPA 200.8 06-Feb-12 13:12 DJSULL1

2012001140

Collection Date: 25-Jan-12 9:00 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) 155 mg/L 0.5 10 EPA 200.7 03-Feb-12 13:33 DJSULL1

Strontium (Sr) 9.15 mg/L 0.05 10 EPA 200.7 03-Feb-12 13:33 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 88.8 ug/L 2 2 EPA 200.8 06-Feb-12 13:32 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 5 ug/L 5 5 EPA 200.8 06-Feb-12 13:58 DJSULL1

Chromium (Cr) < 5 ug/L 5 5 EPA 200.8 06-Feb-12 13:58 DJSULL1

Copper (Cu) < 5 ug/L 5 5 EPA 200.8 06-Feb-12 13:58 DJSULL1

Nickel (Ni) 50.9 ug/L 5 5 EPA 200.8 06-Feb-12 13:58 DJSULL1

Selenium (Se) 92.8 ug/L 5 5 EPA 200.8 06-Feb-12 13:58 DJSULL1

Silver (Ag) < 5 ug/L 5 5 EPA 200.8 06-Feb-12 13:58 DJSULL1

Zinc (Zn) < 10 ug/L 10 5 EPA 200.8 06-Feb-12 13:58 DJSULL1

SELENIUM SPECIATION

Vendor Parameter Complete 1 V_AS&C

2012001141

Collection Date: 25-Jan-12 9:00 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) 152 mg/L 0.5 10 EPA 200.7 03-Feb-12 13:45 DJSULL1

Page 5 of 16
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12010230

2012001141

Collection Date: 25-Jan-12 9:00 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) < 5 ug/L 5 5 EPA 200.8 06-Feb-12 14:02 DJSULL1

Chromium (Cr) < 5 ug/L 5 5 EPA 200.8 06-Feb-12 14:02 DJSULL1

Copper (Cu) < 5 ug/L 5 5 EPA 200.8 06-Feb-12 14:02 DJSULL1

Nickel (Ni) 9.86 ug/L 5 5 EPA 200.8 06-Feb-12 14:02 DJSULL1

Selenium (Se) 19.6 ug/L 5 5 EPA 200.8 06-Feb-12 14:02 DJSULL1

Silver (Ag) < 5 ug/L 5 5 EPA 200.8 06-Feb-12 14:02 DJSULL1

Zinc (Zn) < 10 ug/L 10 5 EPA 200.8 06-Feb-12 14:02 DJSULL1

2012001142

Collection Date: 25-Jan-12 9:00 AM

Site: BIOREACTOR 2 EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

INORGANIC IONS BY IC

Bromide 80 mg/L 5 50 EPA 300.0 31-Jan-12 12:59 JAHERMA

Fluoride 10 mg/L 5 50 EPA 300.0 31-Jan-12 12:59 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) < 1 ug/L 1 20 EPA 245.1 03-Feb-12 08:52 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 149 mg/L 0.5 10 EPA 200.7 03-Feb-12 13:49 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 5 ug/L 5 5 EPA 200.8 06-Feb-12 14:05 DJSULL1

Chromium (Cr) < 5 ug/L 5 5 EPA 200.8 06-Feb-12 14:05 DJSULL1

Copper (Cu) < 5 ug/L 5 5 EPA 200.8 06-Feb-12 14:05 DJSULL1

Nickel (Ni) < 5 ug/L 5 5 EPA 200.8 06-Feb-12 14:05 DJSULL1

Selenium (Se) < 5 ug/L 5 5 EPA 200.8 06-Feb-12 14:05 DJSULL1

Silver (Ag) < 5 ug/L 5 5 EPA 200.8 06-Feb-12 14:05 DJSULL1

Zinc (Zn) < 10 ug/L 10 5 EPA 200.8 06-Feb-12 14:05 DJSULL1

SELENIUM SPECIATION

Vendor Parameter Complete 1 V_AS&C

2012001143

Collection Date: 25-Jan-12 9:00 AM

Site: FILTER BLANK 

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 06-Feb-12 13:06 DJSULL1

Page 6 of 16
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12010230

2012001144

Collection Date: 25-Jan-12 9:00 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 03-Feb-12 13:25 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 1 ug/L 1 1 EPA 200.8 06-Feb-12 13:02 DJSULL1

Chromium (Cr) < 1 ug/L 1 1 EPA 200.8 06-Feb-12 13:02 DJSULL1

Copper (Cu) < 1 ug/L 1 1 EPA 200.8 06-Feb-12 13:02 DJSULL1

Nickel (Ni) < 1 ug/L 1 1 EPA 200.8 06-Feb-12 13:02 DJSULL1

Selenium (Se) < 1 ug/L 1 1 EPA 200.8 06-Feb-12 13:02 DJSULL1

Silver (Ag) < 1 ug/L 1 1 EPA 200.8 06-Feb-12 13:02 DJSULL1

Zinc (Zn) < 2 ug/L 2 1 EPA 200.8 06-Feb-12 13:02 DJSULL1

SELENIUM SPECIATION

Vendor Parameter Complete 1 V_AS&C

Page 7 of 16
 

January 31, 2012 

Jay Perkins 

Duke Energy Analytical Laboratory 

Mail Code MGO3A2 (Building 7405) 

13339 Hagers Ferry Rd. 

Huntersville, NC 28078 

(704) 875-5245 

Project: Belews – FGD WWTS Bi-Monthly Sampling) (LIMS # J12010230) 

Dear Mr. Perkins, 

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

speciation analysis on January 26, 2012. The samples were received in a sealed cooler at -0.3°C 

on January 27, 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: Belews – FGD WWTS Bi-Monthly Sampling) (LIMS # J12010230) 

January 31, 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 January 26, 2012. The 

samples were received on January 27, 2012 in a sealed container at -0.3°C. 

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

and ultra-violet radiation, and was designated a discrete sample identifier. 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 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 

each analytical day. All calibration curves, associated with each species of interest, are 

Page 9 of 16
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 Each sample for selenium speciation 

analysis was analyzed by ion chromatography inductively coupled plasma dynamic reaction 

cell mass spectrometry (IC-ICP-DRC-MS) on January 30, 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 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 well and no significant analytical issues were encountered. All 

quality control parameters associated with this sample 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 10 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 11 of 16
Sample Results

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

Unknown Se 

Species (n)

FGD Purge Eff 73.7 66.6 ND (<3.6) ND (<2.4) ND (<2.4) 0 (0)

BioReactor 1 Inf 13.5 60.9 ND (<0.91) 1.49 ND (<0.61) 0 (0)

BioReactor 2 Eff ND (<0.34) ND (<0.58) ND (<0.91) ND (<0.61) ND (<0.61) 0 (0)

Metals Trip Blk ND (<0.068) ND (<0.12) ND (<0.18) ND (<0.12) ND (<0.12) 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: Belews - FGD WWTS Bi-Monthly Sampling)

Contact: Jay Perkins

Date: January 31, 2012

LIMS #J12010230

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 0.007 0.068 0.34 1.4

Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.012 0.12 0.58 2.3

SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.018 0.18 0.91 3.6

MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.012 0.12 0.61 2.4

SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.012 0.12 0.61 2.4

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 9.39 98.1

Se(VI) LCS 9.48 9.28 97.9

SeCN LCS 8.92 8.21 92.1

MeSe(IV) LCS 6.47 6.29 97.2

SeMe LCS 9.32 9.14 98.0

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Belews - FGD WWTS Bi-Monthly Sampling)

Contact: Jay Perkins

LIMS #J12010230

Date: January 31, 2012

Report Generated by: Russell Gerads

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 ND (<0.34) ND (<0.34) NC NC

Se(VI) BioReactor 2 Eff ND (<0.58) ND (<0.58) NC NC

SeCN BioReactor 2 Eff ND (<0.91) ND (<0.91) NC NC

MeSe(IV) BioReactor 2 Eff ND (<0.61) ND (<0.61) NC NC

SeMe BioReactor 2 Eff ND (<0.61) ND (<0.61) 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 278.0 249.4 89.7 278.0 251.3 90.4 0.8

Se(VI) BioReactor 2 Eff 252.3 236.8 93.9 252.3 236.4 93.7 0.2

SeCN BioReactor 2 Eff 228.8 211.9 92.6 228.8 212.1 92.7 0.1

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Belews - FGD WWTS Bi-Monthly Sampling)

Contact: Jay Perkins

LIMS #J12010230

Date: January 31, 2012

Report Generated by: Russell Gerads

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