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: J12040252

Project Name: WWTS - Biweekly (2)

Lab Contact: Jason C Perkins

Date: 5/14/2012

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

2012008883 BELEWS 25-Apr-12 8:25 AM TO FGD Purge Eff 

2012008884 BELEWS 25-Apr-12 8:19 AM TO EQ TANK EFF. 

2012008885 BELEWS 25-Apr-12 8:15 AM TO BIOREACTOR 1 INF. 

2012008886 BELEWS 25-Apr-12 TO BIOREACTOR 2 INF. 

2012008887 BELEWS 25-Apr-12 8:12 AM TO BIOREACTOR 2 EFF. 

2012008888 BELEWS 25-Apr-12 8:07 AM TO FILTER BLANK 

2012008889 BELEWS 16-Apr-12 9:50 AM CPK 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: 5/14/2012

NA

Electronic Data Deliverable (EDD) Sent Separately

Page 3 of 23
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12040252

2012008883

Collection Date: 25-Apr-12 8:25 AM

Site: FGD Purge Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

INORGANIC IONS BY IC

Bromide 92 mg/L 5 50 EPA 300.0 01-May-12 16:20 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 191 ug/L 5 100 EPA 245.1 03-May-12 14:42 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 178 mg/L 0.5 10 EPA 200.7 02-May-12 11:43 DJSULL1

Manganese (Mn) 6.57 mg/L 0.05 10 EPA 200.7 02-May-12 11:43 DJSULL1

DISSOLVED METALS BY ICP-MS

Manganese (Mn) 5450 ug/L 20 20 EPA 200.8 02-May-12 11:20 MHH7131

Selenium (Se) 156 ug/L 20 20 EPA 200.8 02-May-12 11:20 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 146 ug/L 10 10 EPA 200.8 09-May-12 13:41 DJSULL1

Chromium (Cr) 209 ug/L 10 10 EPA 200.8 09-May-12 13:41 DJSULL1

Copper (Cu) 82.0 ug/L 10 10 EPA 200.8 09-May-12 13:41 DJSULL1

Nickel (Ni) 168 ug/L 10 10 EPA 200.8 09-May-12 13:41 DJSULL1

Selenium (Se) 3430 ug/L 10 10 EPA 200.8 09-May-12 13:41 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 09-May-12 13:41 DJSULL1

Zinc (Zn) 159 ug/L 10 10 EPA 200.8 09-May-12 13:41 DJSULL1

SELENIUM SPECIATION

Vendor Parameter Complete 1 V_AS&C

TOTAL DISSOLVED SOLIDS

Vendor Parameter Complete 1 V_PACE

2012008884

Collection Date: 25-Apr-12 8:19 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) 153 ug/L 2.5 50 EPA 245.1 03-May-12 14:45 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 170 mg/L 0.5 10 EPA 200.7 02-May-12 11:47 DJSULL1

Manganese (Mn) 5.92 mg/L 0.05 10 EPA 200.7 02-May-12 11:47 DJSULL1

Page 4 of 23
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12040252

2012008884

Collection Date: 25-Apr-12 8:19 AM

Site: EQ TANK EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

DISSOLVED METALS BY ICP-MS

Manganese (Mn) 4830 ug/L 20 20 EPA 200.8 02-May-12 11:24 MHH7131

Selenium (Se) 108 ug/L 10 10 EPA 200.8 02-May-12 11:24 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 119 ug/L 10 10 EPA 200.8 09-May-12 13:44 DJSULL1

Chromium (Cr) 185 ug/L 10 10 EPA 200.8 09-May-12 13:44 DJSULL1

Copper (Cu) 75.4 ug/L 10 10 EPA 200.8 09-May-12 13:44 DJSULL1

Nickel (Ni) 153 ug/L 10 10 EPA 200.8 09-May-12 13:44 DJSULL1

Selenium (Se) 2690 ug/L 10 10 EPA 200.8 09-May-12 13:44 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 09-May-12 13:44 DJSULL1

Zinc (Zn) 131 ug/L 10 10 EPA 200.8 09-May-12 13:44 DJSULL1

2012008885

Collection Date: 25-Apr-12 8:15 AM

Site: BIOREACTOR 1 INF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

INORGANIC IONS BY IC

Bromide 81 mg/L 5 50 EPA 300.0 01-May-12 16:38 JAHERMA

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 159 mg/L 0.5 10 EPA 200.7 02-May-12 11:31 DJSULL1

Manganese (Mn) 1.02 mg/L 0.05 10 EPA 200.7 02-May-12 11:31 DJSULL1

DISSOLVED METALS BY ICP-MS

Manganese (Mn) 951 ug/L 10 10 EPA 200.8 02-May-12 11:28 MHH7131

Selenium (Se) 79.8 ug/L 10 10 EPA 200.8 02-May-12 11:28 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 09-May-12 13:47 DJSULL1

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 09-May-12 13:47 DJSULL1

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 09-May-12 13:47 DJSULL1

Nickel (Ni) 16.4 ug/L 10 10 EPA 200.8 09-May-12 13:47 DJSULL1

Selenium (Se) 72.9 ug/L 10 10 EPA 200.8 09-May-12 13:47 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 09-May-12 13:47 DJSULL1

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 09-May-12 13:47 DJSULL1

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 # J12040252

2012008886

Collection Date: 25-Apr-12

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) 167 mg/L 0.5 10 EPA 200.7 02-May-12 11:35 DJSULL1

Manganese (Mn) 2.23 mg/L 0.05 10 EPA 200.7 02-May-12 11:35 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 09-May-12 13:51 DJSULL1

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 09-May-12 13:51 DJSULL1

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 09-May-12 13:51 DJSULL1

Nickel (Ni) < 10 ug/L 10 10 EPA 200.8 09-May-12 13:51 DJSULL1

Selenium (Se) < 10 ug/L 10 10 EPA 200.8 09-May-12 13:51 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 09-May-12 13:51 DJSULL1

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 09-May-12 13:51 DJSULL1

2012008887

Collection Date: 25-Apr-12 8:12 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 01-May-12 18:43 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) < 1 ug/L 1 20 EPA 245.1 03-May-12 14:47 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 182 mg/L 0.5 10 EPA 200.7 02-May-12 11:39 DJSULL1

Manganese (Mn) 4.11 mg/L 0.05 10 EPA 200.7 02-May-12 11:39 DJSULL1

DISSOLVED METALS BY ICP-MS

Manganese (Mn) 3870 ug/L 10 10 EPA 200.8 02-May-12 11:32 MHH7131

Selenium (Se) < 10 ug/L 10 10 EPA 200.8 02-May-12 11:32 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 09-May-12 14:21 DJSULL1

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 09-May-12 14:21 DJSULL1

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 09-May-12 14:21 DJSULL1

Nickel (Ni) < 10 ug/L 10 10 EPA 200.8 09-May-12 14:21 DJSULL1

Selenium (Se) < 10 ug/L 10 10 EPA 200.8 09-May-12 14:21 DJSULL1

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 09-May-12 14:21 DJSULL1

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 09-May-12 14:21 DJSULL1

SELENIUM SPECIATION

Vendor Parameter Complete 1 V_AS&C

Page 6 of 23
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J12040252

2012008888

Collection Date: 25-Apr-12 8:07 AM

Site: FILTER BLANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

DISSOLVED METALS BY ICP-MS

Manganese (Mn) 12.9 ug/L 1 1 EPA 200.8 02-May-12 10:56 MHH7131

Selenium (Se) < 1 ug/L 1 1 EPA 200.8 02-May-12 10:56 MHH7131

2012008889

Collection Date: 16-Apr-12 9:50 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 02-May-12 11:27 DJSULL1

Manganese (Mn) < 0.005 mg/L 0.005 1 EPA 200.7 02-May-12 11:27 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 1 ug/L 1 1 EPA 200.8 09-May-12 14:12 DJSULL1

Chromium (Cr) < 1 ug/L 1 1 EPA 200.8 09-May-12 14:12 DJSULL1

Copper (Cu) < 1 ug/L 1 1 EPA 200.8 09-May-12 14:12 DJSULL1

Nickel (Ni) < 1 ug/L 1 1 EPA 200.8 09-May-12 14:12 DJSULL1

Selenium (Se) < 1 ug/L 1 1 EPA 200.8 09-May-12 14:12 DJSULL1

Silver (Ag) < 1 ug/L 1 1 EPA 200.8 09-May-12 14:12 DJSULL1

Zinc (Zn) < 1 ug/L 1 1 EPA 200.8 09-May-12 14:12 DJSULL1

SELENIUM SPECIATION

Vendor Parameter Complete 1 V_AS&C

Page 7 of 23
May 02, 2012

LIMS USE: FR - TERRY WHITNER

LIMS OBJECT ID: 92117293

92117293

Project:

Pace Project No.:

RE:

Terry Whitner

Duke Energy Carolinas, LLC

PO Box 37929

DPEHS

Charlotte, NC 28237

J12040252

Dear Terry Whitner:

Enclosed are the analytical results for sample(s) received by the laboratory on April 26, 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,

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:

92117293

J12040252

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:

92117293

J12040252

Lab ID Sample ID Method

Analytes

Analysts Reported Laboratory

92117293001 2012008883 SM 2540C LMD 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:

92117293

J12040252

Sample: 2012008883 Lab ID: 92117293001 Collected: 04/25/12 08:25 Received: 04/26/12 14:40 Matrix: Water

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

2540C Total Dissolved Solids Analytical Method: SM 2540C

Total Dissolved Solids 14500 mg/L 500 1 04/27/12 22:44

REPORT OF LABORATORY ANALYSIS

This report shall not be reproduced, except in full,

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

Date: 05/02/2012 01:39 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:

92117293

J12040252

QC Batch:

QC Batch Method:

Analysis Method:

Analysis Description:

WET/20642

SM 2540C

SM 2540C

2540C Total Dissolved Solids

Associated Lab Samples: 92117293001

Parameter Units

Blank

Result

Reporting

Limit Qualifiers

METHOD BLANK: 756724

Associated Lab Samples: 92117293001

Matrix: Water

Analyzed

Total Dissolved Solids mg/L ND 25.0 04/27/12 22:38

Parameter Units

LCS

Result

% Rec

Conc. % Rec Limits Qualifiers

LABORATORY CONTROL SAMPLE: 756725

Spike LCS

Total Dissolved Solids mg/L 250 250 100 80-120

Parameter Units

Dup

Result Result RPD Qualifiers

92117320001

SAMPLE DUPLICATE: 756726

Total Dissolved Solids mg/L 222 219 1

Parameter Units

Dup

Result Result RPD Qualifiers

92117193003

SAMPLE DUPLICATE: 756727

Total Dissolved Solids mg/L ND 29.0

REPORT OF LABORATORY ANALYSIS

This report shall not be reproduced, except in full,

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

Date: 05/02/2012 01:39 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:

92117293

J12040252

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: 05/02/2012 01:39 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:

92117293

J12040252

Lab ID Sample ID QC Batch Method QC Batch Analytical Method

Analytical

Batch

92117293001 2012008883 SM 2540C WET/20642

REPORT OF LABORATORY ANALYSIS

This report shall not be reproduced, except in full,

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

Date: 05/02/2012 01:39 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
 

May 4, 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-Wed-Sampling) (LIMS # J12040252) 

Dear Mr. Perkins, 

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

speciation analysis on April 26, 2012. The samples were received in a sealed cooler at 0.0°C on 

April 27, 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 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 (Bi-Monthly-Wed-Sampling) (LIMS # J12040252) 

May 4, 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 April 26, 2012. The samples 

were received on April 27, 2012 in a sealed container at 0.0°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 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 

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-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 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 (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 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 73.3 59.8 ND (<3.1) ND (<2.9) ND (<2.9) 0 (0)

BioReactor 1 Inf 18.4 48.4 ND (<0.77) 0.81 ND (<0.72) 0.61 (1)

BioReactor 2 Eff 0.47 ND (<0.94) ND (<0.77) ND (<0.72) ND (<0.72) 0 (0)

Metals Trip Blk ND (<0.089) ND (<0.19) ND (<0.15) ND (<0.14) ND (<0.14) 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-Wed-Sampling)

Contact: Jay Perkins

Date: May 4, 2012

LIMS #J12040252

Page 19 of 23
Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 50x eMDL 250x eMDL 1000x

Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.089 0.44 1.8

Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.19 0.94 3.8

SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.003 0.15 0.77 3.1

MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.003 0.14 0.72 2.9

SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.003 0.14 0.72 2.9

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 9.34 97.6

Se(VI) LCS 9.48 8.79 92.7

SeCN LCS 8.92 8.65 97.0

MeSe(IV) LCS 6.47 5.68 87.7

SeMe LCS 9.32 8.31 89.1

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

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

Contact: Jay Perkins

LIMS #J12040252

Date: May 4, 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) Batch QC 6.0 5.8 5.9 2.9

Se(VI) Batch QC 123.3 113.1 118.2 8.6

SeCN Batch QC ND (<3.1) ND (<3.1) NC NC

MeSe(IV) Batch QC ND (<2.9) ND (<2.9) NC NC

SeMe Batch QC ND (<2.9) ND (<2.9) 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 5560 5809 104.4 5560 5768 103.6 0.7

Se(VI) Batch QC 5045 5193 100.6 5045 5171 100.2 0.4

SeCN Batch QC 4575 4399 96.2 4575 4315 94.3 1.9

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

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

Contact: Jay Perkins

LIMS #J12040252

Date: May 4, 2012

Report Generated by: Russell Gerads

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