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: J11100039

Lab Contact: Jason C Perkins

Date: 10/27/2011

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 27
Sample ID's & Descriptions:

Sample ID Plant/Station

Collection 

Date and Time Collected By Sample Description

2011021606 BELEWS 12-Oct-11 11:08 AM TO FGD Purge Eff 

2011021607 BELEWS 12-Oct-11 10:56 AM TO EQ TANK EFF. 

2011021608 BELEWS 12-Oct-11 10:29 AM TO BIOREACTOR 1 INF. 

2011021609 BELEWS 12-Oct-11 10:35 AM TO BIOREACTOR 2 INF. 

2011021610 BELEWS 12-Oct-11 10:41 AM TO BIOREACTOR 2 EFF. 

2011021611 BELEWS 12-Oct-11 10:22 AM TO FILTER BLANK 

2011021612 BELEWS 12-Oct-11 10:22 AM TO Trip Blank 

2011021613 BELEWS 12-Oct-11 10:29 AM TO BIOREACTOR 1 INF. 

2011021614 BELEWS 12-Oct-11 10:29 AM TO HG BLANK BIOREACTOR 1 INF. 

2011021615 BELEWS 12-Oct-11 10:35 AM TO BIOREACTOR 2 INF. 

2011021616 BELEWS 12-Oct-11 10:35 AM TO Hg Blk BioReactor 2 Inf 

2011021617 BELEWS 12-Oct-11 10:41 AM TO BIOREACTOR 2 EFF. 

2011021618 BELEWS 12-Oct-11 10:41 AM TO Hg Blk BioReactor 2 Eff 

13 Total Samples

Page 2 of 27
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: 10/27/2011

Yes

Electronic Data Deliverable (EDD) Sent Separately

Page 3 of 27
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11100039

2011021606

Collection Date: 12-Oct-11 11:08 AM

Site: FGD Purge Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

INORGANIC IONS BY IC

Bromide 88 mg/L EPA 300.0 10 25-Oct-11 07:45 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 317 ug/L EPA 245.1 5 21-Oct-11 09:04 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 182 mg/L EPA 200.7 0.5 24-Oct-11 13:15 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 1130 ug/L EPA 200.8 10 19-Oct-11 12:01 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 159 ug/L EPA 200.8 10 19-Oct-11 12:25 KRICHAR

Chromium (Cr) 228 ug/L 10 EPA 200.8 19-Oct-11 12:25 KRICHAR

Copper (Cu) 126 ug/L 10 EPA 200.8 19-Oct-11 12:25 KRICHAR

Nickel (Ni) 188 ug/L 10 EPA 200.8 19-Oct-11 12:25 KRICHAR

Selenium (Se) 6080 ug/L 20 EPA 200.8 19-Oct-11 12:25 KRICHAR

Silver (Ag) < 10 ug/L 10 EPA 200.8 19-Oct-11 12:25 KRICHAR

Zinc (Zn) 228 ug/L 20 EPA 200.8 19-Oct-11 12:25 KRICHAR

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

TOTAL DISSOLVED SOLIDS

TDS 18000 mg/L SM2540C 200 19-Oct-11 13:25 TJA7067

2011021607

Collection Date: 12-Oct-11 10:56 AM

Site: EQ TANK EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 199 ug/L EPA 245.1 2.5 21-Oct-11 09:07 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 163 mg/L EPA 200.7 0.5 24-Oct-11 13:19 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 1150 ug/L EPA 200.8 10 19-Oct-11 12:04 KRICHAR

Page 4 of 27
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11100039

2011021607

Collection Date: 12-Oct-11 10:56 AM

Site: EQ TANK EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 113 ug/L EPA 200.8 10 19-Oct-11 11:19 KRICHAR

Chromium (Cr) 168 ug/L 10 EPA 200.8 19-Oct-11 11:19 KRICHAR

Copper (Cu) 90.2 ug/L 10 EPA 200.8 19-Oct-11 11:19 KRICHAR

Nickel (Ni) 142 ug/L 10 EPA 200.8 19-Oct-11 11:19 KRICHAR

Selenium (Se) 4110 ug/L 10 EPA 200.8 19-Oct-11 11:19 KRICHAR

Silver (Ag) < 10 ug/L 10 EPA 200.8 19-Oct-11 11:19 KRICHAR

Zinc (Zn) 160 ug/L 20 EPA 200.8 19-Oct-11 11:19 KRICHAR

2011021608

Collection Date: 12-Oct-11 10:29 AM

Site: BIOREACTOR 1 INF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 152 mg/L EPA 200.7 0.5 24-Oct-11 13:22 DJSULL1

DISSOLVED METALS BY ICP-MS

Selenium (Se) 1200 ug/L EPA 200.8 10 19-Oct-11 12:07 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L EPA 200.8 10 19-Oct-11 11:22 KRICHAR

Chromium (Cr) 11.9 ug/L 10 EPA 200.8 19-Oct-11 11:22 KRICHAR

Copper (Cu) < 10 ug/L 10 EPA 200.8 19-Oct-11 11:22 KRICHAR

Nickel (Ni) 10.8 ug/L 10 EPA 200.8 19-Oct-11 11:22 KRICHAR

Selenium (Se) 1240 ug/L 10 EPA 200.8 19-Oct-11 11:22 KRICHAR

Silver (Ag) < 10 ug/L 10 EPA 200.8 19-Oct-11 11:22 KRICHAR

Zinc (Zn) < 20 ug/L 20 EPA 200.8 19-Oct-11 11:22 KRICHAR

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2011021609

Collection Date: 12-Oct-11 10:35 AM

Site: BIOREACTOR 2 INF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 154 mg/L EPA 200.7 0.5 24-Oct-11 13:26 DJSULL1

Page 5 of 27
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11100039

2011021609

Collection Date: 12-Oct-11 10:35 AM

Site: BIOREACTOR 2 INF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L EPA 200.8 10 19-Oct-11 11:25 KRICHAR

Chromium (Cr) < 10 ug/L 10 EPA 200.8 19-Oct-11 11:25 KRICHAR

Copper (Cu) < 10 ug/L 10 EPA 200.8 19-Oct-11 11:25 KRICHAR

Nickel (Ni) 15.9 ug/L 10 EPA 200.8 19-Oct-11 11:25 KRICHAR

Selenium (Se) 191 ug/L 10 EPA 200.8 19-Oct-11 11:25 KRICHAR

Silver (Ag) < 10 ug/L 10 EPA 200.8 19-Oct-11 11:25 KRICHAR

Zinc (Zn) < 20 ug/L 20 EPA 200.8 19-Oct-11 11:25 KRICHAR

2011021610

Collection Date: 12-Oct-11 10:41 AM

Site: BIOREACTOR 2 EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

INORGANIC IONS BY IC

Bromide 78 mg/L EPA 300.0 10 25-Oct-11 08:00 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) < 1 ug/L EPA 245.1 1 21-Oct-11 09:09 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 153 mg/L EPA 200.7 0.5 24-Oct-11 13:30 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 5 ug/L EPA 200.8 5 19-Oct-11 11:28 KRICHAR

Chromium (Cr) < 5 ug/L 5 EPA 200.8 19-Oct-11 11:28 KRICHAR

Copper (Cu) < 5 ug/L 5 EPA 200.8 19-Oct-11 11:28 KRICHAR

Nickel (Ni) < 5 ug/L 5 EPA 200.8 19-Oct-11 11:28 KRICHAR

Selenium (Se) 14.2 ug/L 5 EPA 200.8 19-Oct-11 11:28 KRICHAR

Silver (Ag) < 5 ug/L 5 EPA 200.8 19-Oct-11 11:28 KRICHAR

Zinc (Zn) < 10 ug/L 10 EPA 200.8 19-Oct-11 11:28 KRICHAR

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2011021611

Collection Date: 12-Oct-11 10:22 AM

Site: FILTER BLANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

DISSOLVED METALS BY ICP-MS

Selenium (Se) 1.17 ug/L EPA 200.8 1 19-Oct-11 10:42 KRICHAR

Page 6 of 27
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11100039

2011021612

Collection Date: 12-Oct-11 10:22 AM

Site: Trip Blank 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

TOTAL RECOVERABLE METALS BY ICP

Boron (B) < 0.05 mg/L EPA 200.7 0.05 24-Oct-11 12:59 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 1 ug/L EPA 200.8 1 19-Oct-11 10:30 KRICHAR

Chromium (Cr) < 1 ug/L 1 EPA 200.8 19-Oct-11 10:30 KRICHAR

Copper (Cu) < 1 ug/L 1 EPA 200.8 19-Oct-11 10:30 KRICHAR

Nickel (Ni) < 1 ug/L 1 EPA 200.8 19-Oct-11 10:30 KRICHAR

Selenium (Se) < 1 ug/L 1 EPA 200.8 19-Oct-11 10:30 KRICHAR

Silver (Ag) < 1 ug/L 1 EPA 200.8 19-Oct-11 10:30 KRICHAR

Zinc (Zn) < 2 ug/L 2 EPA 200.8 19-Oct-11 10:30 KRICHAR

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2011021613

Collection Date: 12-Oct-11 10:29 AM

Site: BIOREACTOR 1 INF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY 1631

Vendor Parameter Complete V_BRAND

2011021614

Collection Date: 12-Oct-11 10:29 AM

Site: HG BLANK BIOREACTOR 1 INF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY 1631

Vendor Parameter Complete V_BRAND

2011021615

Collection Date: 12-Oct-11 10:35 AM

Site: BIOREACTOR 2 INF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY 1631

Vendor Parameter Complete V_BRAND

Page 7 of 27
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11100039

2011021616

Collection Date: 12-Oct-11 10:35 AM

Site: Hg Blk BioReactor 2 Inf 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY 1631

Vendor Parameter Complete V_BRAND

2011021617

Collection Date: 12-Oct-11 10:41 AM

Site: BIOREACTOR 2 EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY 1631

Vendor Parameter Complete V_BRAND

2011021618

Collection Date: 12-Oct-11 10:41 AM

Site: Hg Blk BioReactor 2 Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

MERCURY 1631

Vendor Parameter Complete V_BRAND

Page 8 of 27
 

October 21, 2011 

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 # J11100039) 

Dear Mr. Perkins, 

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

speciation analysis on October 13, 2011. The samples were received on October 14, 2011 in a 

sealed cooler at 0.7°C. 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, 

 

 Ben Wozniak

 Project Manager 

 Applied Speciation and Consulting, LLC 

 

Page 9 of 27
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 # J11100039) 

October 21, 2011 

1. Sample Reception 

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

Consulting) were submitted for selenium speciation analysis on October 13, 2011. The 

samples were received on October 14, 2011 in a sealed container at 0.7°C. 

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

and ultra-violet radiation. Upon reception, the samples were designated discrete sample 

identifiers. An aliquot of each sample was filtered (0.45μm) and these filtrates were 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 

the samples 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 10 of 27
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 minimal interval 

of every ten analytical runs. 

Selenium Speciation Analysis by IC-ICP-DRC-MS All samples for selenium speciation 

analysis were analyzed by ion chromatography inductively coupled plasma dynamic reaction 

cell mass spectrometry (IC-ICP-DRC-MS) on October 17-18, 2011. 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 these samples were within acceptance limits with 

the following exceptions: 

The recoveries associated with the matrix spike (MS) and matrix spike duplicate (MSD) 

performed on the sample identified as Batch QC were below the established control limit of 

75% for selenocyanate (54.4% and 51.2%, respectively). The MS and MSD also included 

selenite in the spiking solution which yielded elevated recoveries (139.1% and 143.3%, 

respectively). The low recoveries for selenocyanate correlate with the elevated recoveries of 

selenite suggesting that the sample matrix induces species conversion. The fact that no 

species conversion was observed in the ICV or CCVs, which contain both selenite and 

selenocyanate, demonstrates that the applied method stabilizes these selenium species in 

solution. Since the conversion of selenocyanate to selenite in the MS and MSD is a function 

of the sample matrix and the recoveries confirm a mass balance, no corrective action was 

required. The reported results are deemed representative of the supplied samples and suggest 

that selenocyanate is not stable in the spiked sample matrix. 

Page 11 of 27
The estimated method detection limits (eMDLs) for selenite, selenate, and selenocyanate are 

generated from replicate analyses of the lowest standard in the calibration curve. Not all 

selenium species are present in preparation blanks; therefore, eMDL calculations based on 

preparation blanks are artificially biased low. 

The eMDL for methylseleninic acid and selenomethionine is calculated from the average 

eMDL of selenite, selenate, and selenocyanate. The calibration does not contain 

methylseleninic acid or selenomethionine due to impurities in these standards which would 

bias the results for other selenium species. 

If you have any questions or concerns regarding this report, please feel free to contact me. 

Sincerely, 

Ben Wozniak 

Project Manager 

Applied Speciation and Consulting, LLC 

Page 12 of 27
Sample Results

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

Unknown Se 

Species (n)

FGD Purge Eff 14.9 1030 ND (<1.3) ND (<1.5) ND (<1.5) 0 (0)

BioReactor 1 Inf 16.0 1070 ND (<0.34) 1.00 ND (<0.37) 0 (0)

BioReactor 2 Eff 1.61 6.40 ND (<0.34) ND (<0.37) ND (<0.37) 0 (0)

Metals Trip Blk ND (<0.097) ND (<0.055) ND (<0.067) ND (<0.073) ND (<0.073) 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: Ben Wozniak

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

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

Contact: Jay Perkins

Date: October 21, 2011

LIMS #J11100039

Page 13 of 27
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 0.010 0.097 0.48 1.9

Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.006 0.055 0.28 1.1

SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.007 0.067 0.34 1.3

MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.007 0.073 0.37 1.5

SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.007 0.073 0.37 1.5

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 11.24 117.5

Se(VI) LCS 9.48 10.01 105.6

SeCN LCS 8.92 9.239 103.6

MeSe(IV) LCS 6.47 5.847 90.4

SeMe LCS 9.32 9.200 98.7

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

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

Contact: Jay Perkins

LIMS #J11100039

Date: October 21, 2011

Report Generated by: Ben Wozniak

Page 14 of 27
Quality Control Summary - Matrix Duplicates

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

Se(IV) Batch QC* 12.0 11.9 11.9 0.8

Se(VI) Batch QC* 973.3 1020 996.7 4.7

SeCN Batch QC* ND (<1.3) ND (<1.3) NC NC

MeSe(IV) Batch QC* ND (<1.5) ND (<1.5) NC NC

SeMe Batch QC* ND (<1.5) ND (<1.5) NC NC

ND = Not detected at the applied dilution

NC = Value was not calculated due to one or more concentrations below the eMDL

* Batch QC performed on sample from LIMS # J11100235

Quality Control Summary - Matrix Spike/ Matrix Spike Duplicate

Analyte (μg/L) Sample ID Spike Conc MS Result Recovery Spike Conc MSD Result Recovery RPD

Se(IV) Batch QC* 1112 1559 139.1** 1112 1606 143.3** 3.0

Se(VI) Batch QC* 1009 2025 101.9 1009 2077 107.1 2.6

SeCN Batch QC* 915.0 497.9 54.4** 915.0 468.2 51.2** 6.1

* Batch QC performed on sample from LIMS # J11100235

** The recovery is outside the established control limits of 75-125%; please see narrative

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

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

Contact: Jay Perkins

LIMS #J11100039

Date: October 21, 2011

Report Generated by: Ben Wozniak

Page 15 of 27
Page 16 of 27
 

3958 6th Ave NW • Seattle, WA 98107 • T: 206-632-6206 • F: 206-632-6017 • www.brooksrand.com • brl@brooksrand.com 

October 26, 2011 

Duke Energy 

ATTN: Jay Perkins 

Scientific Support-Laboratory

13339 Hagers Ferry Road 

Huntersville NC 28078 

jcperkins@duke-energy.com 

labcustomer@duke-energy.com 

RE: Project DUK-HV1101 Client Project: J11100039 

Dear Mr. Perkins, 

On October 14, 2011, Brooks Rand Labs (BRL) received three (3) flue gas desulfurization 

(FGD) wastewater samples and three (3) corresponding blank samples. Samples were loggedin for total mercury (Hg) analysis. All samples were received, prepared, analyzed, and stored 

according to BRL SOPs and EPA methodology. 

The results were blank-corrected as described in the calculations section of the applicable 

SOP(s) and may be evaluated using adjusted reporting limits to account for sample aliquot size. 

Please refer to the Sample Results page for sample-specific detection limits and other details. 

Aside from concentration qualifiers, all data was reported without qualification and all associated 

quality control sample results met the acceptance criteria. 

It should be noted that a matrix spike/matrix spike duplicate (MS/MSD) set was not analyzed on 

one of the samples from this work order. A similar sample from a different work order had a 

MS/MSD set analyzed and that has been reported. 

The sample Hg Blk BioReactor 2 Eff (1142048-06) was identified as a field blank, but had a 

detectable result that was comparable to the associated sample. It was also noticed that when 

preserved, Hg Blk BioReactor 2 Eff (1142048-06) reacted similarly to a sample and not a field 

blank. 

BRL, an accredited laboratory, certifies the reported results of all analyses for which BRL is 

NELAP accredited meet all NELAP requirements. For more details, see the Report Information

page of the report. 

Please feel free to contact me if you have any questions regarding this report. 

Sincerely, 

 

Lydia Greaves 

Project Manager 

lydia@brooksran.com 

Page 17 of 27
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Definition of Data Qualifiers

(Effective 9/23/09)

Laboratory Accreditation

BRL is accredited by the National Environmental Laboratory Accreditation Program (NELAP) through the State of Florida 

Department of Health, Bureau of Laboratories (E87982) and is certified to perform many environmental analyses. BRL is 

also certified by many other states to perform environmental analyses. For a current list of our accreditations /certifications, 

please visit our website at <http://www.brooksrand.com/default.asp?contentID=586>. Results reported relate only to the 

samples listed in the report.

Report Information

BLK

BRL

BS

CAL

CCV

CRM

D

DUP

ICV

MSD

ND

NR

PS

REC

RPD

RSD

SCV

SOP

method blank 

Brooks Rand Labs

laboratory fortified blank

calibration standard

continuing calibration verification

certified reference material

dissolved fraction

duplicate

initial calibration verification

matrix spike duplicate

non-detect

non-reportable

post preparation spike

percent recovery

relative percent difference

relative standard deviation

secondary calibration verification

standard operating procedure

MDL

MRL

MS

method detection limit

method reporting limit

matrix spike

SRM

T

COC

standard reference material

total recoverable fraction

chain of custody record 

Common Abbreviations

These qualifiers are based on those previously utilized by Brooks Rand, Ltd., those found in the EPA SOW ILM03.0, 

Exhibit B, Section III, pg. B-18, and the USEPA Laboratory Data Validation Functional Guidelines for Evaluating Inorganic 

Analyses; USEPA; July 2002. These supersede all previous qualifiers ever employed by BRL.

B Detected by the instrument, the result is > the MDL but ≤ the MRL. Result is reported and considered an estimate.

E An estimated value due to the presence of interferences. A full explanation is presented in the narrative.

H Holding time and/or preservation requirements not met. Result is estimated.

J Estimated value. A full explanation is presented in the narrative.

J-M Duplicate precision (RPD) for associated QC sample was not within acceptance criteria. Result is estimated.

J-N Spike recovery for associated QC sample was not within acceptance criteria. Result is estimated.

M Duplicate precision (RPD) was not within acceptance criteria. Result is estimated.

N Spike recovery was not within acceptance criteria. Result is estimated.

R Rejected, unusable value. A full explanation is presented in the narrative.

U Result is ≤ the MDL or client requested reporting limit (CRRL). Result reported as the MDL or CRRL.

X Result is not BLK-corrected and is within 10x the absolute value of the highest detectable BLK in the batch. 

Result is estimated.

Field Quality Control Samples

Please be notified that certain EPA methods require the collection of field quality control samples of an appropriate type 

and frequency; failure to do so is considered a deviation from some methods and for compliance purposes should only be 

done with the approval of regulatory authorities. Please see the specific EPA methods for details regarding required field 

quality control samples.

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.com

Page 18 of 27
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Sample Information

Sample Lab ID Report Matrix Type Sampled Received

BioReactor 1 Inf 1142048-01 Influent Sample 10/12/2011 10/14/2011

Hg Blk BioReactor 1 Inf 1142048-02 DIW Field Blank 10/12/2011 10/14/2011

BioReactor 2 Inf 1142048-03 Influent Sample 10/12/2011 10/14/2011

Hg Blk BioReactor 2 Inf 1142048-04 DIW Field Blank 10/12/2011 10/14/2011

BioReactor 2 Eff 1142048-05 Effluent Sample 10/12/2011 10/14/2011

Hg Blk Bio Reactor 2 Eff 1142048-06 DIW Field Blank 10/12/2011 10/14/2011

Batch Summary

Analyte Lab Matrix Method Prepared Analyzed Batch Sequence

Hg Water EPA 1631 10/21/2011 10/25/2011 B111723 1100738

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.com

Page 19 of 27
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Sample Results

Sample Analyte Report Matrix Fraction Result Qualifier MDL MRL Unit Batch Sequence

BioReactor 1 Inf

1142048-01 Hg Influent T 41700 76.5 204 ng/L B111723 1100738

BioReactor 2 Eff

1142048-05 Hg Effluent T 412 3.03 8.08 ng/L B111723 1100738

BioReactor 2 Inf

1142048-03 Hg Influent T 2460 15.3 40.8 ng/L B111723 1100738

Hg Blk Bio Reactor 2 Eff

1142048-06 Hg DIW T 527 1.52 4.04 ng/L B111723 1100738

Hg Blk BioReactor 1 Inf

1142048-02 Hg DIW T 0.38 B 0.15 0.41 ng/L B111723 1100738

Hg Blk BioReactor 2 Inf

1142048-04 Hg DIW T 0.15 U 0.15 0.41 ng/L B111723 1100738

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.com

Page 20 of 27
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Accuracy & Precision Summary

Batch: B111723

Analyte Native Spike Result Units REC & Limits RPD & Limits

Method: EPA 1631

Lab Matrix: Water

Sample

B111723-SRM1 Certified Reference Material (1140052, THg ICV 1641d)

Hg 15.68 14.44 ng/L 92% 85-115

B111723-MS2 Matrix Spike (1143014-01)

Hg 436.0 2020 2506 ng/L 102% 71-125

B111723-MSD2 Matrix Spike Duplicate (1143014-01)

Hg 436.0 2020 2473 ng/L 101% 71-125 241%

Method Blanks & Reporting Limits

Batch: B111723

Method: EPA 1631

Matrix: Water

Analyte: Hg

Sample Result Units

B111723-BLK1 0.04 ng/L

B111723-BLK2 0.0008 ng/L

B111723-BLK3 0.05 ng/L

B111723-BLK4 0.02 ng/L

Average: 0.03 Standard Deviation: 0.02 MDL: 0.15

Limit: 0.50 Limit: 0.10 MRL: 0.41

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.com

Page 21 of 27
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Instrument Calibration

Sequence: 1100738

Instrument: THG-05 Method: EPA 1631

Date: 10/25/2011

Total Mercury and Mercury Speciation by CVAFS

Analyte: Hg

Lab ID True Value Result Units REC & Limits

1100738-IBL1 8.42 pg of Hg

1100738-IBL2 8.90 pg of Hg

1100738-IBL3 7.23 pg of Hg

1100738-IBL4 8.50 pg of Hg

1100738-CAL1 25.00 24.03 pg of Hg 96%

1100738-CAL2 100.0 99.48 pg of Hg 99%

1100738-CAL3 500.0 511.0 pg of Hg 102%

1100738-CAL4 2500 2549 pg of Hg 102%

1100738-CAL5 10000 10050 pg of Hg 100%

1100738-ICV1 1568 1444 pg of Hg 92% 85-115

1100738-CCB1 12.1 pg of Hg

1100738-CCV1 500.0 514.6 pg of Hg 103% 77-123

1100738-CCB2 8.55 pg of Hg

1100738-CCV2 500.0 497.9 pg of Hg 100% 77-123

1100738-CCB3 37.1 pg of Hg

1100738-CCV3 500.0 512.1 pg of Hg 102% 77-123

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.com

Page 22 of 27
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Sample Containers

Lab ID: 1142048-01 Report Matrix: Influent

Sample: BioReactor 1 Inf Sample Type: Sample Received: 10/14/2011

Collected: 10/12/2011

Des Container Size Lot Preservation P-Lot pH Ship. Cont.

A 71443390

30

Bottle FLPE Hg-T 250mL none n/a Cooler

B 71443390

30

EXTRA_VOL 250 mL none n/a Cooler

Lab ID: 1142048-02 Report Matrix: DIW

Sample: Hg Blk BioReactor 1 Inf Sample Type: Field Blank Received: 10/14/2011

Collected: 10/12/2011

Des Container Size Lot Preservation P-Lot pH Ship. Cont.

A 71443390

30

Bottle FLPE Hg-T 250mL none n/a Cooler

B 71443390

30

EXTRA_VOL 250 mL none n/a Cooler

Lab ID: 1142048-03 Report Matrix: Influent

Sample: BioReactor 2 Inf Sample Type: Sample Received: 10/14/2011

Collected: 10/12/2011

Des Container Size Lot Preservation P-Lot pH Ship. Cont.

A 71443390

30

Bottle FLPE Hg-T 250mL none n/a Cooler

B 71443390

30

EXTRA_VOL 250 mL none n/a Cooler

Lab ID: 1142048-04 Report Matrix: DIW

Sample: Hg Blk BioReactor 2 Inf Sample Type: Field Blank Received: 10/14/2011

Collected: 10/12/2011

Des Container Size Lot Preservation P-Lot pH Ship. Cont.

A 71443390

30

Bottle FLPE Hg-T 250mL none n/a Cooler

B 71443390

30

EXTRA_VOL 250 mL none n/a Cooler

Lab ID: 1142048-05 Report Matrix: Effluent

Sample: BioReactor 2 Eff Sample Type: Sample Received: 10/14/2011

Collected: 10/12/2011

Des Container Size Lot Preservation P-Lot pH Ship. Cont.

A 71443390

30

Bottle FLPE Hg-T 250mL none n/a Cooler

B 71443390

30

EXTRA_VOL 250 mL none n/a Cooler

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.com

Page 23 of 27
Project ID: DUK-HV1101

PM: Tiffany Stilwater

Client PM: Jay Perkins

 Client PO: 141391

Sample Containers

Lab ID: 1142048-06 Report Matrix: DIW

Sample: Hg Blk Bio Reactor 2 Eff Sample Type: Field Blank Received: 10/14/2011

Collected: 10/12/2011

Des Container Size Lot Preservation P-Lot pH Ship. Cont.

A 71443390

30

Bottle FLPE Hg-T 250mL none n/a Cooler

B 71443390

30

EXTRA_VOL 250 mL none n/a Cooler

Shipping Containers

Cooler

Tracking No: 472679664810 via FedEx

Temperature: 3.6 °C

Coolant Type: Ice

Description: Cooler

Damaged in transit? No

Returned to client? No

Custody seals present? No

Custody seals intact? No

COC present? Yes

Received: October 14, 2011 9:00

3958 6th Avenue NW Seattle WA 98107 · P(206) 632-6206 · F(206) 632-6017 · brl@brooksrand.com · www.brooksrand.com

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