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: J12030290

Project Name: WWTS - Biweekly

Lab Contact: Jason C Perkins

Date: 4/9/2012

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 23
Sample ID's & Descriptions:

Sample ID Plant/Station

Collection 

Date and Time Collected By Sample Description

2012006457 BELEWS 14-Mar-12 8:00 AM T. Johnson FGD Purge Eff 

2012006458 BELEWS 14-Mar-12 8:00 AM T. Johnson EQ TANK EFF. 

2012006459 BELEWS 14-Mar-12 8:00 AM T. Johnson BIOREACTOR 1 INF. 

2012006460 BELEWS 14-Mar-12 8:00 AM T. Johnson BIOREACTOR 2 INF. 

2012006461 BELEWS 14-Mar-12 8:00 AM T. Johnson BIOREACTOR 2 EFF. 

2012006462 BELEWS 14-Mar-12 8:00 AM T. Johnson FILTER BLANK 

2012006463 BELEWS 14-Mar-12 8:00 AM T. Johnson Trip Blank 

7 Total Samples

Page 2 of 23
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: 4/9/2012

Yes

Electronic Data Deliverable (EDD) Sent Separately

Page 3 of 23
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12030290

2012006457

Collection Date: 14-Mar-12 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 160 mg/L 5 50 EPA 300.0 02-Apr-12 18:47 JAHERMA

Fluoride 12 mg/L 5 50 EPA 300.0 02-Apr-12 18:47 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 189 ug/L 5 100 EPA 245.1 21-Mar-12 07:48 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 159 mg/L 0.5 10 EPA 200.7 22-Mar-12 13:51 DJSULL1

Strontium (Sr) 9.82 mg/L 0.05 10 EPA 200.7 22-Mar-12 13:51 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 931 ug/L 10 10 EPA 200.8 22-Mar-12 11:06 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 212 ug/L 10 10 EPA 200.8 22-Mar-12 10:30 MHH7131

Chromium (Cr) 250 ug/L 10 10 EPA 200.8 22-Mar-12 10:30 MHH7131

Copper (Cu) 159 ug/L 10 10 EPA 200.8 22-Mar-12 10:30 MHH7131

Nickel (Ni) 204 ug/L 10 10 EPA 200.8 22-Mar-12 10:30 MHH7131

Selenium (Se) 4210 ug/L 10 10 EPA 200.8 22-Mar-12 10:30 MHH7131

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 22-Mar-12 10:30 MHH7131

Zinc (Zn) 340 ug/L 10 10 EPA 200.8 22-Mar-12 10:30 MHH7131

SELENIUM SPECIATION

Vendor Parameter Complete 1 V_AS&C

TOTAL DISSOLVED SOLIDS

Vendor Parameter Complete 1 V_PACE

2012006458

Collection Date: 14-Mar-12 8:00 AM

Site: EQ TANK EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

INORGANIC IONS BY IC

Bromide 150 mg/L 5 50 EPA 300.0 02-Apr-12 19:05 JAHERMA

Fluoride 12 mg/L 5 50 EPA 300.0 02-Apr-12 19:05 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 173 ug/L 2.5 50 EPA 245.1 21-Mar-12 07:51 AGIBBS

Page 4 of 23
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12030290

2012006458

Collection Date: 14-Mar-12 8:00 AM

Site: EQ TANK EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 154 mg/L 0.5 10 EPA 200.7 22-Mar-12 14:08 DJSULL1

Strontium (Sr) 9.34 mg/L 0.05 10 EPA 200.7 22-Mar-12 14:08 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 873 ug/L 10 10 EPA 200.8 22-Mar-12 11:09 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 193 ug/L 10 10 EPA 200.8 22-Mar-12 10:33 MHH7131

Chromium (Cr) 220 ug/L 10 10 EPA 200.8 22-Mar-12 10:33 MHH7131

Copper (Cu) 137 ug/L 10 10 EPA 200.8 22-Mar-12 10:33 MHH7131

Nickel (Ni) 176 ug/L 10 10 EPA 200.8 22-Mar-12 10:33 MHH7131

Selenium (Se) 3710 ug/L 10 10 EPA 200.8 22-Mar-12 10:33 MHH7131

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 22-Mar-12 10:33 MHH7131

Zinc (Zn) 280 ug/L 10 10 EPA 200.8 22-Mar-12 10:33 MHH7131

2012006459

Collection Date: 14-Mar-12 8:00 AM

Site: BIOREACTOR 1 INF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

INORGANIC IONS BY IC

Bromide 150 mg/L 5 50 EPA 300.0 02-Apr-12 20:34 JAHERMA

Fluoride 18 mg/L 5 50 EPA 300.0 02-Apr-12 20:34 JAHERMA

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 135 mg/L 0.5 10 EPA 200.7 22-Mar-12 13:39 DJSULL1

Strontium (Sr) 7.87 mg/L 0.05 10 EPA 200.7 22-Mar-12 13:39 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 715 ug/L 10 10 EPA 200.8 22-Mar-12 11:12 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 22-Mar-12 10:36 MHH7131

Chromium (Cr) 13.1 ug/L 10 10 EPA 200.8 22-Mar-12 10:36 MHH7131

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 22-Mar-12 10:36 MHH7131

Nickel (Ni) 20.5 ug/L 10 10 EPA 200.8 22-Mar-12 10:36 MHH7131

Selenium (Se) 816 ug/L 10 10 EPA 200.8 22-Mar-12 10:36 MHH7131

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 22-Mar-12 10:36 MHH7131

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 22-Mar-12 10:36 MHH7131

SELENIUM SPECIATION

Vendor Parameter Complete 1 V_AS&C

Page 5 of 23
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12030290

2012006460

Collection Date: 14-Mar-12 8:00 AM

Site: BIOREACTOR 2 INF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

INORGANIC IONS BY IC

Bromide 120 mg/L 5 50 EPA 300.0 02-Apr-12 20:52 JAHERMA

Fluoride 15 mg/L 5 50 EPA 300.0 02-Apr-12 20:52 JAHERMA

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 129 mg/L 0.5 10 EPA 200.7 22-Mar-12 13:43 DJSULL1

Strontium (Sr) 7.65 mg/L 0.05 10 EPA 200.7 22-Mar-12 13:43 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 22-Mar-12 10:39 MHH7131

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 22-Mar-12 10:39 MHH7131

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 22-Mar-12 10:39 MHH7131

Nickel (Ni) < 10 ug/L 10 10 EPA 200.8 22-Mar-12 10:39 MHH7131

Selenium (Se) 202 ug/L 10 10 EPA 200.8 22-Mar-12 10:39 MHH7131

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 22-Mar-12 10:39 MHH7131

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 22-Mar-12 10:39 MHH7131

2012006461

Collection Date: 14-Mar-12 8:00 AM

Site: BIOREACTOR 2 EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

INORGANIC IONS BY IC

Bromide 130 mg/L 5 50 EPA 300.0 02-Apr-12 21:10 JAHERMA

Fluoride 16 mg/L 5 50 EPA 300.0 02-Apr-12 21:10 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) < 1 ug/L 1 20 EPA 245.1 21-Mar-12 07:53 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 136 mg/L 0.5 10 EPA 200.7 22-Mar-12 13:47 DJSULL1

Strontium (Sr) 7.27 mg/L 0.05 10 EPA 200.7 22-Mar-12 13:47 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 5 ug/L 5 5 EPA 200.8 22-Mar-12 10:42 MHH7131

Chromium (Cr) < 5 ug/L 5 5 EPA 200.8 22-Mar-12 10:42 MHH7131

Copper (Cu) < 5 ug/L 5 5 EPA 200.8 22-Mar-12 10:42 MHH7131

Nickel (Ni) < 5 ug/L 5 5 EPA 200.8 22-Mar-12 10:42 MHH7131

Selenium (Se) < 5 ug/L 5 5 EPA 200.8 22-Mar-12 10:42 MHH7131

Silver (Ag) < 5 ug/L 5 5 EPA 200.8 22-Mar-12 10:42 MHH7131

Zinc (Zn) < 5 ug/L 5 5 EPA 200.8 22-Mar-12 10:42 MHH7131

Page 6 of 23
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12030290

2012006461

Collection Date: 14-Mar-12 8:00 AM

Site: BIOREACTOR 2 EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

SELENIUM SPECIATION

Vendor Parameter Complete 1 V_AS&C

2012006462

Collection Date: 14-Mar-12 8:00 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) 2.95 ug/L 1 1 EPA 200.8 22-Mar-12 11:03 MHH7131

2012006463

Collection Date: 14-Mar-12 8:00 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 22-Mar-12 13:35 DJSULL1

Strontium (Sr) < 0.005 mg/L 0.005 1 EPA 200.7 22-Mar-12 13:35 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 1 ug/L 1 1 EPA 200.8 22-Mar-12 09:54 MHH7131

Chromium (Cr) < 1 ug/L 1 1 EPA 200.8 22-Mar-12 09:54 MHH7131

Copper (Cu) < 1 ug/L 1 1 EPA 200.8 22-Mar-12 09:54 MHH7131

Nickel (Ni) < 1 ug/L 1 1 EPA 200.8 22-Mar-12 09:54 MHH7131

Selenium (Se) < 1 ug/L 1 1 EPA 200.8 22-Mar-12 09:54 MHH7131

Silver (Ag) 1.05 ug/L 1 1 EPA 200.8 22-Mar-12 09:54 MHH7131

Zinc (Zn) < 1 ug/L 1 1 EPA 200.8 22-Mar-12 09:54 MHH7131

SELENIUM SPECIATION

Vendor Parameter Complete 1 V_AS&C

Page 7 of 23
March 27, 2012

LIMS USE: FR - TERRY WHITNER

LIMS OBJECT ID: 92114362

92114362

Project:

Pace Project No.:

RE:

Terry Whitner

Duke Energy Carolinas, LLC

PO Box 37929

DPEHS

Charlotte, NC 28237

J12030290

Dear Terry Whitner:

Enclosed are the analytical results for sample(s) received by the laboratory on March 15, 2012. The

results relate only to the samples included in this report. Results reported herein conform to the

most current TNI standards and the laboratory's Quality Assurance Manual, where applicable, unless

otherwise noted in the body of the report.

Analyses were performed at the Pace Analytical Services location indicated on the sample analyte

page for analysis unless otherwise footnoted.

If you have any questions concerning this report, please feel free to contact me.

Sincerely,

Erin Waters for

Kevin Herring

kevin.herring@pacelabs.com

Project Manager

Enclosures

REPORT OF LABORATORY ANALYSIS

This report shall not be reproduced, except in full,

without the written consent of Pace Analytical Services, Inc..

Page 1 of 7

Pace Analytical Services, Inc.

9800 Kincey Ave. Suite 100

Huntersville, NC 28078

(704)875-9092

Pace Analytical Services, Inc.

2225 Riverside Dr.

Asheville, NC 28804

(828)254-7176

Pace Analytical Services, Inc.

205 East Meadow Road - Suite A

Eden, NC 27288

(336)623-8921

Page 8 of 23
CERTIFICATIONS

Pace Project No.:

Project:

92114362

J12030290

Asheville Certification IDs

2225 Riverside Dr., Asheville, NC 28804

Florida/NELAP Certification #: E87648

Massachusetts Certification #: M-NC030

North Carolina Drinking Water Certification #: 37712

North Carolina Wastewater Certification #: 40

South Carolina Certification #: 99030001

Virginia Certification #: 00072

West Virginia Certification #: 356

Virgina/VELAP Certification #: 460147

REPORT OF LABORATORY ANALYSIS

This report shall not be reproduced, except in full,

without the written consent of Pace Analytical Services, Inc..

Page 2 of 7

Pace Analytical Services, Inc.

9800 Kincey Ave. Suite 100

Huntersville, NC 28078

(704)875-9092

Pace Analytical Services, Inc.

2225 Riverside Dr.

Asheville, NC 28804

(828)254-7176

Pace Analytical Services, Inc.

205 East Meadow Road - Suite A

Eden, NC 27288

(336)623-8921

Page 9 of 23
SAMPLE ANALYTE COUNT

Pace Project No.:

Project:

92114362

J12030290

Lab ID Sample ID Method

Analytes

Analysts Reported Laboratory

92114362001 2012006457 SM 2540C SMW 1 PASI-A

REPORT OF LABORATORY ANALYSIS

This report shall not be reproduced, except in full,

without the written consent of Pace Analytical Services, Inc..

Page 3 of 7

Pace Analytical Services, Inc.

9800 Kincey Ave. Suite 100

Huntersville, NC 28078

(704)875-9092

Pace Analytical Services, Inc.

2225 Riverside Dr.

Asheville, NC 28804

(828)254-7176

Pace Analytical Services, Inc.

205 East Meadow Road - Suite A

Eden, NC 27288

(336)623-8921

Page 10 of 23
ANALYTICAL RESULTS

Pace Project No.:

Project:

92114362

J12030290

Sample: 2012006457 Lab ID: 92114362001 Collected: 03/14/12 08:00 Received: 03/15/12 15:20 Matrix: Water

Parameters Results Units Report Limit DF Prepared Analyzed CAS No. Qual

2540C Total Dissolved Solids Analytical Method: SM 2540C

Total Dissolved Solids 19700 mg/L 500 1 03/20/12 14:58

REPORT OF LABORATORY ANALYSIS

This report shall not be reproduced, except in full,

without the written consent of Pace Analytical Services, Inc..

Date: 03/27/2012 05:13 PM Page 4 of 7

Pace Analytical Services, Inc.

9800 Kincey Ave. Suite 100

Huntersville, NC 28078

(704)875-9092

Pace Analytical Services, Inc.

2225 Riverside Dr.

Asheville, NC 28804

(828)254-7176

Pace Analytical Services, Inc.

205 East Meadow Road - Suite A

Eden, NC 27288

(336)623-8921

Page 11 of 23
QUALITY CONTROL DATA

Pace Project No.:

Project:

92114362

J12030290

QC Batch:

QC Batch Method:

Analysis Method:

Analysis Description:

WET/20150

SM 2540C

SM 2540C

2540C Total Dissolved Solids

Associated Lab Samples: 92114362001

Parameter Units

Blank

Result

Reporting

Limit Qualifiers

METHOD BLANK: 738207

Associated Lab Samples: 92114362001

Matrix: Water

Analyzed

Total Dissolved Solids mg/L ND 25.0 03/20/12 14:57

Parameter Units

LCS

Result

% Rec

Conc. % Rec Limits Qualifiers

LABORATORY CONTROL SAMPLE: 738208

Spike LCS

Total Dissolved Solids mg/L 250 298 119 80-120

Parameter Units

Dup

Result Result RPD Qualifiers

92114107013

SAMPLE DUPLICATE: 738209

Total Dissolved Solids mg/L 408 392 4

Parameter Units

Dup

Result Result RPD Qualifiers

92114381002

SAMPLE DUPLICATE: 738210

Total Dissolved Solids mg/L 317 323 2

REPORT OF LABORATORY ANALYSIS

This report shall not be reproduced, except in full,

without the written consent of Pace Analytical Services, Inc..

Date: 03/27/2012 05:13 PM Page 5 of 7

Pace Analytical Services, Inc.

9800 Kincey Ave. Suite 100

Huntersville, NC 28078

(704)875-9092

Pace Analytical Services, Inc.

2225 Riverside Dr.

Asheville, NC 28804

(828)254-7176

Pace Analytical Services, Inc.

205 East Meadow Road - Suite A

Eden, NC 27288

(336)623-8921

Page 12 of 23
QUALIFIERS

Pace Project No.:

Project:

92114362

J12030290

DEFINITIONS

DF - Dilution Factor, if reported, represents the factor applied to the reported data due to changes in sample preparation, dilution of

the sample aliquot, or moisture content.

ND - Not Detected at or above adjusted reporting limit.

J - Estimated concentration above the adjusted method detection limit and below the adjusted reporting limit.

MDL - Adjusted Method Detection Limit.

S - Surrogate

1,2-Diphenylhydrazine (8270 listed analyte) decomposes to Azobenzene.

Consistent with EPA guidelines, unrounded data are displayed and have been used to calculate % recovery and RPD values.

LCS(D) - Laboratory Control Sample (Duplicate)

MS(D) - Matrix Spike (Duplicate)

DUP - Sample Duplicate

RPD - Relative Percent Difference

NC - Not Calculable.

SG - Silica Gel - Clean-Up

U - Indicates the compound was analyzed for, but not detected.

N-Nitrosodiphenylamine decomposes and cannot be separated from Diphenylamine using Method 8270. The result reported for

each analyte is a combined concentration.

Acid preservation may not be appropriate for 2-Chloroethylvinyl ether, Styrene, and Vinyl chloride.

Pace Analytical is TNI accredited. Contact your Pace PM for the current list of accredited analytes.

TNI - The NELAC Institute.

LABORATORIES

PASI-A Pace Analytical Services - Asheville

REPORT OF LABORATORY ANALYSIS

This report shall not be reproduced, except in full,

without the written consent of Pace Analytical Services, Inc..

Date: 03/27/2012 05:13 PM Page 6 of 7

Pace Analytical Services, Inc.

9800 Kincey Ave. Suite 100

Huntersville, NC 28078

(704)875-9092

Pace Analytical Services, Inc.

2225 Riverside Dr.

Asheville, NC 28804

(828)254-7176

Pace Analytical Services, Inc.

205 East Meadow Road - Suite A

Eden, NC 27288

(336)623-8921

Page 13 of 23
QUALITY CONTROL DATA CROSS REFERENCE TABLE

Pace Project No.:

Project:

92114362

J12030290

Lab ID Sample ID QC Batch Method QC Batch Analytical Method

Analytical

Batch

92114362001 2012006457 SM 2540C WET/20150

REPORT OF LABORATORY ANALYSIS

This report shall not be reproduced, except in full,

without the written consent of Pace Analytical Services, Inc..

Date: 03/27/2012 05:13 PM Page 7 of 7

Pace Analytical Services, Inc.

9800 Kincey Ave. Suite 100

Huntersville, NC 28078

(704)875-9092

Pace Analytical Services, Inc.

2225 Riverside Dr.

Asheville, NC 28804

(828)254-7176

Pace Analytical Services, Inc.

205 East Meadow Road - Suite A

Eden, NC 27288

(336)623-8921

Page 14 of 23
 

March 23, 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 (2010, Bi-Weekly Sampling) (LIMS # J12030290) 

Dear Mr. Perkins, 

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

speciation analysis on March 15, 2012. The samples were received in a sealed cooler at -0.4°C 

on March 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 15 of 23
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 (2010, Bi-Weekly Sampling) (LIMS # J12030290) 

March 23, 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 March 15, 2012. The 

samples were received on March 16, 2012 in a sealed container at -0.4°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 16 of 23
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 March 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. 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 17 of 23
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 18 of 23
Sample Results

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

Unknown Se 

Species (n)

FGD Purge Eff 23.5 744 ND (<0.60) 2.7 ND (<1.4) 0 (0)

BioReactor 1 Inf 9.37 682 ND (<0.15) 2.12 ND (<0.35) 0.66 (1)

BioReactor 2 Eff ND (<0.32) ND (<0.58) ND (<0.15) ND (<0.35) ND (<0.35) 0 (0)

Metals Trip Blk ND (<0.065) ND (<0.12) ND (<0.030) ND (<0.070) ND (<0.070) 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 (2010, Bi-Weekly Sampling)

Contact: Jay Perkins

Date: March 23, 2012

LIMS #J12030290

Page 19 of 23
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 0.006 0.065 0.32 1.3

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 0.003 0.030 0.15 0.60

MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.007 0.070 0.35 1.4

SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.007 0.070 0.35 1.4

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 9.77 102.0

Se(VI) LCS 9.48 9.61 101.4

SeCN LCS 8.92 9.07 101.7

MeSe(IV) LCS 6.47 6.17 95.3

SeMe LCS 9.32 8.90 95.4

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Belews - FGD WWTS (2010, Bi-Weekly Sampling)

Contact: Jay Perkins

LIMS #J12030290

Date: March 23, 2012

Report Generated by: Russell Gerads

Page 20 of 23
Quality Control Summary - Matrix Duplicates

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

Se(IV) BioReactor 2 Eff ND (<0.32) ND (<0.32) NC NC

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

SeCN BioReactor 2 Eff ND (<0.15) ND (<0.15) NC NC

MeSe(IV) BioReactor 2 Eff ND (<0.35) ND (<0.35) NC NC

SeMe BioReactor 2 Eff 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

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 278.0 256.9 92.4 278.0 252.6 90.9 1.7

Se(VI) BioReactor 2 Eff 252.3 226.7 89.9 252.3 223.6 88.7 1.4

SeCN BioReactor 2 Eff 228.8 201.4 88.1 228.8 198.1 86.6 1.7

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Belews - FGD WWTS (2010, Bi-Weekly Sampling)

Contact: Jay Perkins

LIMS #J12030290

Date: March 23, 2012

Report Generated by: Russell Gerads

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