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: J13030340

Project Name: WWTS - Biweekly (2)

Lab Contact: Jason C Perkins

Date: 4/22/2013

Customer Address: 3195 Pine Hall Rd

Customer Name(s): BIll K, Wayne C, Melonie M, and T. THORNTON

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. 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. 

Jason C Perkins

Page 1 of 16
Sample ID's & Descriptions:

Sample ID Plant/Station

Collection 

Date and Time Collected By Sample Description

2013006360 BELEWS 28-Mar-13 8:00 AM ILLEGIBLE FGD Purge Eff 

2013006361 BELEWS 28-Mar-13 8:05 AM ILLEGIBLE EQ TANK EFF. 

2013006362 BELEWS 28-Mar-13 8:10 AM ILLEGIBLE BIOREACTOR 1 INF. 

2013006363 BELEWS 28-Mar-13 8:15 AM ILLEGIBLE BIOREACTOR 2 INF. 

2013006364 BELEWS 28-Mar-13 8:20 AM ILLEGIBLE BIOREACTOR 2 EFF. 

2013006365 BELEWS 28-Mar-13 8:25 AM ILLEGIBLE FILTER BLANK 

2013006366 BELEWS 21-Mar-13 7:30 AM C.KNOX 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: 4/22/2013

Electronic Data Deliverable (EDD) Sent Separately

Page 3 of 16
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13030340

2013006360

Collection Date: 28-Mar-13 8:00 AM

Site: FGD Purge Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

INORGANIC IONS BY IC

Bromide 220 mg/L 5 50 EPA 300.0 04/16/2013 02:45 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 205 ug/L 5 100 EPA 245.1 04/04/2013 13:08 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 288 mg/L 0.5 10 EPA 200.7 04/12/2013 13:24 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 358 ug/L 10 10 EPA 200.8 04/08/2013 14:07 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 276 ug/L 10 10 EPA 200.8 04/10/2013 13:56 KRICHAR

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 04/10/2013 13:56 KRICHAR

Chromium (Cr) 310 ug/L 10 10 EPA 200.8 04/10/2013 13:56 KRICHAR

Copper (Cu) 149 ug/L 10 10 EPA 200.8 04/10/2013 13:56 KRICHAR

Nickel (Ni) 291 ug/L 10 10 EPA 200.8 04/10/2013 13:56 KRICHAR

Selenium (Se) 5170 ug/L 20 20 EPA 200.8 04/10/2013 13:56 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 04/10/2013 13:56 KRICHAR

Zinc (Zn) 271 ug/L 10 10 EPA 200.8 04/10/2013 13:56 KRICHAR

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

Vendor Parameter Complete Vendor Method V_AS&C

TOTAL DISSOLVED SOLIDS

TDS 35000 mg/L 200 1 SM2540C 04/08/2013 12:43 TJA7067

2013006361

Collection Date: 28-Mar-13 8:05 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) 116 ug/L 2.5 50 EPA 245.1 04/04/2013 13:11 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 263 mg/L 0.5 10 EPA 200.7 04/12/2013 13:27 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 343 ug/L 10 10 EPA 200.8 04/08/2013 14:10 KRICHAR

Page 4 of 16
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13030340

2013006361

Collection Date: 28-Mar-13 8:05 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) 178 ug/L 10 10 EPA 200.8 04/10/2013 13:00 KRICHAR

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 04/10/2013 13:00 KRICHAR

Chromium (Cr) 229 ug/L 10 10 EPA 200.8 04/10/2013 13:00 KRICHAR

Copper (Cu) 113 ug/L 10 10 EPA 200.8 04/10/2013 13:00 KRICHAR

Nickel (Ni) 253 ug/L 10 10 EPA 200.8 04/10/2013 13:00 KRICHAR

Selenium (Se) 3400 ug/L 10 10 EPA 200.8 04/10/2013 13:00 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 04/10/2013 13:00 KRICHAR

Zinc (Zn) 207 ug/L 10 10 EPA 200.8 04/10/2013 13:00 KRICHAR

2013006362

Collection Date: 28-Mar-13 8:10 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) 231 mg/L 0.5 10 EPA 200.7 04/12/2013 13:31 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 200 ug/L 10 10 EPA 200.8 04/08/2013 14:14 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 04/10/2013 13:03 KRICHAR

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 04/10/2013 13:03 KRICHAR

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 04/10/2013 13:03 KRICHAR

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 04/10/2013 13:03 KRICHAR

Nickel (Ni) 54.9 ug/L 10 10 EPA 200.8 04/10/2013 13:03 KRICHAR

Selenium (Se) 190 ug/L 10 10 EPA 200.8 04/10/2013 13:03 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 04/10/2013 13:03 KRICHAR

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 04/10/2013 13:03 KRICHAR

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

Vendor Parameter Complete Vendor Method V_AS&C

2013006363

Collection Date: 28-Mar-13 8:15 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) 221 mg/L 0.5 10 EPA 200.7 04/12/2013 13:35 DJSULL1

Page 5 of 16
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13030340

2013006363

Collection Date: 28-Mar-13 8:15 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 04/10/2013 13:07 KRICHAR

Cadmium (Cd) < 10 ug/L 10 10 EPA 200.8 04/10/2013 13:07 KRICHAR

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 04/10/2013 13:07 KRICHAR

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 04/10/2013 13:07 KRICHAR

Nickel (Ni) < 10 ug/L 10 10 EPA 200.8 04/10/2013 13:07 KRICHAR

Selenium (Se) 18.0 ug/L 10 10 EPA 200.8 04/10/2013 13:07 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 04/10/2013 13:07 KRICHAR

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 04/10/2013 13:07 KRICHAR

2013006364

Collection Date: 28-Mar-13 8:20 AM

Site: BIOREACTOR 2 EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

INORGANIC IONS BY IC

Bromide 160 mg/L 5 50 EPA 300.0 04/16/2013 03:04 JAHERMA

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 206 mg/L 0.5 10 EPA 200.7 04/12/2013 13:39 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 5 ug/L 5 5 EPA 200.8 04/10/2013 13:10 KRICHAR

Cadmium (Cd) < 5 ug/L 5 5 EPA 200.8 04/10/2013 13:10 KRICHAR

Chromium (Cr) < 5 ug/L 5 5 EPA 200.8 04/10/2013 13:10 KRICHAR

Copper (Cu) < 5 ug/L 5 5 EPA 200.8 04/10/2013 13:10 KRICHAR

Nickel (Ni) < 5 ug/L 5 5 EPA 200.8 04/10/2013 13:10 KRICHAR

Selenium (Se) < 5 ug/L 5 5 EPA 200.8 04/10/2013 13:10 KRICHAR

Silver (Ag) < 5 ug/L 5 5 EPA 200.8 04/10/2013 13:10 KRICHAR

Zinc (Zn) < 5 ug/L 5 5 EPA 200.8 04/10/2013 13:10 KRICHAR

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

Vendor Parameter Complete Vendor Method V_AS&C

2013006365

Collection Date: 28-Mar-13 8:25 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 04/08/2013 13:53 KRICHAR

Page 6 of 16
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13030340

2013006366

Collection Date: 21-Mar-13 7:30 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 04/12/2013 13:16 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 1 ug/L 1 1 EPA 200.8 04/10/2013 12:50 KRICHAR

Cadmium (Cd) < 1 ug/L 1 1 EPA 200.8 04/10/2013 12:50 KRICHAR

Chromium (Cr) < 1 ug/L 1 1 EPA 200.8 04/10/2013 12:50 KRICHAR

Copper (Cu) < 1 ug/L 1 1 EPA 200.8 04/10/2013 12:50 KRICHAR

Nickel (Ni) < 1 ug/L 1 1 EPA 200.8 04/10/2013 12:50 KRICHAR

Selenium (Se) < 1 ug/L 1 1 EPA 200.8 04/10/2013 12:50 KRICHAR

Silver (Ag) < 1 ug/L 1 1 EPA 200.8 04/10/2013 12:50 KRICHAR

Zinc (Zn) < 1 ug/L 1 1 EPA 200.8 04/10/2013 12:50 KRICHAR

Page 7 of 16
 

April 18, 2013

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 #J13030340) 

Dear Mr. Perkins, 

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

speciation on April 2, 2013. The samples were received in a sealed cooler at -0.5°C on April 3, 

2013. 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 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 #J13030340) 

April 18, 2013 

1. Sample Reception 

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

Consulting) were submitted for selenium speciation analysis on April 2, 2013. The samples 

were received on April 3, 2013 in a sealed container at -0.5°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 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-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 April 17, 2013. 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 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 284 49.0 ND (<2.1) 8.3 ND (<2.1) 0.0 (0)

BioReactor 1 Inf 116 43.6 ND (<0.52) 8.30 ND (<0.53) 2.34 (1)

BioReactor 2 Eff ND (<0.72) ND (<0.35) ND (<0.52) ND (<0.53) ND (<0.53) 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: Belews - FGD WWTS (Bi-Monthly Sampling)

Contact: Jay Perkins

Date: April 18, 2013

LIMS #J13030340

Page 12 of 16
Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 250x eMDL 1000x

Se(IV) -0.003 0.013 0.007 0.010 0.007 0.007 0.003 0.72 2.9

Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.35 1.4

SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.52 2.1

MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.53 2.1

SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.53 2.1

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 4.79 4.530 94.7

Se(VI) LCS 4.74 4.269 90.1

SeCN LCS 4.46 4.095 91.8

MeSe(IV) LCS 3.24 3.009 93.0

SeMe LCS 4.66 4.226 90.7

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

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

Contact: Jay Perkins

LIMS #J13030340

Date: April 18, 2013

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) Batch QC 1.46 1.69 1.58 14.6

Se(VI) Batch QC ND (<0.35) ND (<0.35) NC NC

SeCN Batch QC 0.94 1.07 1.00 12.8

MeSe(IV) Batch QC ND (<0.53) ND (<0.53) NC NC

SeMe Batch QC ND (<0.53) ND (<0.53) 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 1390 1570 112.9 1390 1584 113.9 0.9

Se(VI) Batch QC 1261 1235 97.9 1261 1237 98.1 0.1

SeCN Batch QC 1144 914.5 79.9 1144 921.2 80.5 0.7

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

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

Contact: Jay Perkins

LIMS #J13030340

Date: April 18, 2013

Report Generated by: Russell Gerads

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