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: J11090321

Lab Contact: Jason C Perkins

Date: 10/10/2011

Customer Address: 253 Plant Allen Road

Customer Name(s): Don Scruggs, Robbin Jolly, Ray Lidke, Bill Kennedy

Belmont, NC 28012

Phone: 980-875-5348

Report Authorized By:

(Signature)

Program Comments:

Please contact the Program Manager (Jason C Perkins) with any questions regarding this report.

Data Flags & Calculations:

Any analytical tests or individual analytes within a test flagged with a Qualifier indicate a deviation from the method quality 

system or quality control requirement. The qualifier description is found at the end of the Certificate of Analysis (sample results) 

under the qualifiers heading. All results are reported on a dry weight basis unless otherwise noted.

Data Package:

This data package includes analytical results that are applicable only to the samples described in this narrative. An estimation of 

the uncertainty of measurement for the results in the report is available upon request. This report shall not be reproduced, except 

in full, without the written consent of the Analytical Laboratory. Please contact the Analytical laboratory with any questions. The 

order of individual sections within this report is as follows:

Job Summary Report, Sample Identification, Technical Validation of Data Package, Analytical Laboratory Certificate of Analysis, 

Analytical Laboratory QC Reports, Sub-contracted Laboratory Results, Customer Specific Data Sheets, Reports & 

Documentation, Customer Database Entries, Test Case Narratives, Chain of Custody (COC)

Certification:

The Analytical Laboratory holds the following State Certifications : North Carolina (DENR) Certificate #248, South Carolina 

(DHEC) Laboratory ID # 99005. Contact the Analytical Laboratory for definitive information about the certification status of 

specific methods. 

Page 1 of 16
Sample ID's & Descriptions:

Sample ID Plant/Station

Collection 

Date and Time Collected By Sample Description

2011020491 ALLEN 26-Sep-11 8:45 AM Chris Greene FGD Purge Eff 

2011020492 ALLEN 26-Sep-11 10:15 AM Chris Greene EQ Tank Eff 

2011020493 ALLEN 26-Sep-11 10:05 AM Chris Greene BioReactor 1 Inf 

2011020494 ALLEN 26-Sep-11 9:55 AM Chris Greene BioReactor 2 Inf 

2011020495 ALLEN 26-Sep-11 10:25 AM Chris Greene BioReactor 2 Eff 

2011020496 ALLEN 20-Sep-11 10:50 AM L. Davis Filter Blk 

2011020497 ALLEN 20-Sep-11 10:50 AM L. Davis TRIP BLANK 

7 Total Samples

Page 2 of 16
COC and .pdf report are in agreement with sample totals 

and analyses (compliance programs and procedures).

All Results are less than the laboratory reporting limits.

All laboratory QA/QC requirements are acceptable.

The Vendor Laboratories have been qualified by the 

Analytical Laboratory

Yes No

Technical Validation Review

Checklist:

Yes No

Yes No

Report Sections Included:

Job Summary Report Sub-contracted Laboratory Results

Sample Identification Customer Specific Data Sheets, Reports, & Documentation

Technical Validation of Data Package Customer Database Entries

Analytical Laboratory Certificate of Analysis

Analytical Laboratory QC Report

Chain of Custody

Reviewed By: DataBase Administrator Date: 10/10/2011

Yes

Electronic Data Deliverable (EDD) Sent Separately

Page 3 of 16
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11090321

2011020491

Collection Date: 26-Sep-11 8:45 AM

Site: FGD Purge Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

INORGANIC IONS BY IC

Bromide 18 mg/L EPA 300.0 5 03-Oct-11 11:53 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 36.7 ug/L EPA 245.1 2.5 30-Sep-11 10:15 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 30.2 mg/L EPA 200.7 0.5 04-Oct-11 13:41 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 835 ug/L EPA 200.8 10 30-Sep-11 13:44 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 210 ug/L EPA 200.8 10 05-Oct-11 11:00 KRICHAR

Chromium (Cr) 98.2 ug/L 10 EPA 200.8 05-Oct-11 11:00 KRICHAR

Copper (Cu) 133 ug/L 10 EPA 200.8 05-Oct-11 11:00 KRICHAR

Nickel (Ni) 178 ug/L 10 EPA 200.8 05-Oct-11 11:00 KRICHAR

Selenium (Se) 1030 ug/L 10 EPA 200.8 05-Oct-11 11:00 KRICHAR

Silver (Ag) < 10 ug/L 10 EPA 200.8 05-Oct-11 11:00 KRICHAR

Zinc (Zn) 178 ug/L 20 EPA 200.8 05-Oct-11 11:00 KRICHAR

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

TOTAL DISSOLVED SOLIDS

TDS 7600 mg/L SM2540C 200 28-Sep-11 16:25 TJA7067

2011020492

Collection Date: 26-Sep-11 10:15 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) 13.6 ug/L EPA 245.1 2.5 30-Sep-11 10:17 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 22.8 mg/L EPA 200.7 0.5 04-Oct-11 13:45 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 152 ug/L EPA 200.8 10 30-Sep-11 13:48 KRICHAR

Page 4 of 16
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11090321

2011020492

Collection Date: 26-Sep-11 10:15 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) 55.5 ug/L EPA 200.8 10 05-Oct-11 11:03 KRICHAR

Chromium (Cr) 26.8 ug/L 10 EPA 200.8 05-Oct-11 11:03 KRICHAR

Copper (Cu) 41.7 ug/L 10 EPA 200.8 05-Oct-11 11:03 KRICHAR

Nickel (Ni) 76.2 ug/L 10 EPA 200.8 05-Oct-11 11:03 KRICHAR

Selenium (Se) 250 ug/L 10 EPA 200.8 05-Oct-11 11:03 KRICHAR

Silver (Ag) < 10 ug/L 10 EPA 200.8 05-Oct-11 11:03 KRICHAR

Zinc (Zn) 51.3 ug/L 20 EPA 200.8 05-Oct-11 11:03 KRICHAR

2011020493

Collection Date: 26-Sep-11 10:05 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) 25.4 mg/L EPA 200.7 0.5 04-Oct-11 13:53 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 75.6 ug/L EPA 200.8 10 30-Sep-11 13:51 KRICHAR

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L EPA 200.8 10 05-Oct-11 11:06 KRICHAR

Chromium (Cr) < 10 ug/L 10 EPA 200.8 05-Oct-11 11:06 KRICHAR

Copper (Cu) < 10 ug/L 10 EPA 200.8 05-Oct-11 11:06 KRICHAR

Nickel (Ni) < 10 ug/L 10 EPA 200.8 05-Oct-11 11:06 KRICHAR

Selenium (Se) 76.0 ug/L 10 EPA 200.8 05-Oct-11 11:06 KRICHAR

Silver (Ag) < 10 ug/L 10 EPA 200.8 05-Oct-11 11:06 KRICHAR

Zinc (Zn) < 20 ug/L 20 EPA 200.8 05-Oct-11 11:06 KRICHAR

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2011020494

Collection Date: 26-Sep-11 9:55 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) 27.4 mg/L EPA 200.7 0.5 04-Oct-11 13:49 MHH7131

Page 5 of 16
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11090321

2011020494

Collection Date: 26-Sep-11 9:55 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 05-Oct-11 11:09 KRICHAR

Chromium (Cr) < 10 ug/L 10 EPA 200.8 05-Oct-11 11:09 KRICHAR

Copper (Cu) < 10 ug/L 10 EPA 200.8 05-Oct-11 11:09 KRICHAR

Nickel (Ni) < 10 ug/L 10 EPA 200.8 05-Oct-11 11:09 KRICHAR

Selenium (Se) < 10 ug/L 10 EPA 200.8 05-Oct-11 11:09 KRICHAR

Silver (Ag) < 10 ug/L 10 EPA 200.8 05-Oct-11 11:09 KRICHAR

Zinc (Zn) < 20 ug/L 20 EPA 200.8 05-Oct-11 11:09 KRICHAR

2011020495

Collection Date: 26-Sep-11 10:25 AM

Site: BioReactor 2 Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

INORGANIC IONS BY IC

Bromide 27 mg/L EPA 300.0 5 03-Oct-11 12:09 JAHERMA

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) < 1 ug/L EPA 245.1 1 30-Sep-11 10:20 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 25.9 mg/L EPA 200.7 0.5 04-Oct-11 13:56 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L EPA 200.8 10 05-Oct-11 11:12 KRICHAR

Chromium (Cr) < 10 ug/L 10 EPA 200.8 05-Oct-11 11:12 KRICHAR

Copper (Cu) < 10 ug/L 10 EPA 200.8 05-Oct-11 11:12 KRICHAR

Nickel (Ni) < 10 ug/L 10 EPA 200.8 05-Oct-11 11:12 KRICHAR

Selenium (Se) < 10 ug/L 10 EPA 200.8 05-Oct-11 11:12 KRICHAR

Silver (Ag) < 10 ug/L 10 EPA 200.8 05-Oct-11 11:12 KRICHAR

Zinc (Zn) < 20 ug/L 20 EPA 200.8 05-Oct-11 11:12 KRICHAR

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

2011020496

Collection Date: 20-Sep-11 10:50 AM

Site: Filter Blk 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

Analyst

DISSOLVED METALS BY ICP-MS

Selenium (Se) < 1 ug/L EPA 200.8 1 30-Sep-11 12:59 KRICHAR

Page 6 of 16
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J11090321

2011020497

Collection Date: 20-Sep-11 10:50 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 04-Oct-11 13:33 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 1 ug/L EPA 200.8 1 05-Oct-11 10:51 KRICHAR

Chromium (Cr) < 1 ug/L 1 EPA 200.8 05-Oct-11 10:51 KRICHAR

Copper (Cu) < 1 ug/L 1 EPA 200.8 05-Oct-11 10:51 KRICHAR

Nickel (Ni) < 1 ug/L 1 EPA 200.8 05-Oct-11 10:51 KRICHAR

Selenium (Se) < 1 ug/L 1 EPA 200.8 05-Oct-11 10:51 KRICHAR

Silver (Ag) < 1 ug/L 1 EPA 200.8 05-Oct-11 10:51 KRICHAR

Zinc (Zn) < 2 ug/L 2 EPA 200.8 05-Oct-11 10:51 KRICHAR

SELENIUM SPECIATION

Vendor Parameter Complete V_AS&C

Page 7 of 16
 

October 7, 2011 

Jay Perkins 

Duke Energy Analytical Laboratory 

Mail Code MGO3A2 (Building 7405) 

13339 Hagers Ferry Rd. 

Huntersville, NC 28078 

(704) 875-5245 

Project: Allen – FGD WWTS (2010, Bi-Monthly Sampling) (LIMS # J11090321) 

Dear Mr. Perkins, 

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

speciation analysis on September 29, 2011. The samples were received on September 30, 2011 

in a sealed cooler at 0.7

oC. 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 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: Allen – FGD WWTS (2010, Bi-Monthly Sampling) (LIMS # J11090321) 

October 7, 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 September 29, 2011. The 

samples were received on September 30, 2011 in a sealed container at 0.7

oC.

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 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 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 1, 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 

sample results have been corrected in accordance with the continuing calibration verification 

standards to account for perceived instrument drift. All quality control parameters associated 

with these samples were within acceptance limits, demonstrating the suitability of these 

corrections. 

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, 

Ben Wozniak 

Project Manager 

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 ND (<1.6) 901 ND (<2.6) ND (<2.6) ND (<2.6) 0 (0)

BioReactor 1 Inf ND (<0.39) 3200 ND (<0.65) ND (<0.65) ND (<0.65) 0 (0)

BioReactor 2 Eff 2.56 ND (<0.90) ND (<0.65) ND (<0.65) ND (<0.65) 0 (0)

Metals Trip Blk ND (<0.078) ND (<0.18) ND (<0.13) ND (<0.13) ND (<0.13) 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: Allen – FGD WWTS (2010, Bi-Monthly Sampling)

Contact: Jay Perkins

Date: October 7, 2011

LIMS #J11090321

Page 12 of 16
Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 10x eMDL 50x eMDL 200x

Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.078 0.39 1.6

Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.018 0.18 0.90 3.6

SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.013 0.13 0.65 2.6

MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.013 0.13 0.65 2.6

SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.013 0.13 0.65 2.6

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 9.818 102.6

Se(VI) LCS 9.48 9.601 101.3

SeCN LCS 8.92 9.194 103.1

MeSe(IV) LCS 6.47 6.053 93.6

SeMe LCS 9.32 8.888 95.4

Selenium Speciation Results for Duke Energy

Project Name: Allen – FGD WWTS (2010, Bi-Monthly Sampling)

Contact: Jay Perkins

LIMS #J11090321

Date: October 7, 2011

Report Generated by: Ben Wozniak

Applied Speciation and Consulting, LLC

Page 13 of 16
Quality Control Summary - Matrix Duplicates

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

Se(IV) Batch QC* ND (<1.6) 3.3 NC NC

Se(VI) Batch QC* 2662 2667 2664 0.2

SeCN Batch QC* ND (<2.6) ND (<2.6) NC NC

MeSe(IV) Batch QC* ND (<2.6) ND (<2.6) NC NC

SeMe Batch QC* ND (<2.6) ND (<2.6) 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 # J11090481

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 1269 114.1 1112 1288 115.8 1.5

Se(VI) Batch QC* 1009 3644 97.1 1009 3678 100.5 0.9

SeCN Batch QC* 915.0 777.7 85.0 915.0 744.8 81.4 4.3

* Batch QC performed on sample from LIMS # J11090481

Date: October 7, 2011

Report Generated by: Ben Wozniak

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Allen – FGD WWTS (2010, Bi-Monthly Sampling)

Contact: Jay Perkins

LIMS #J11090321

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