NC0038377_Revised J15070470F_20171101

13339 Hagers Ferry Road
Huntersville, NC 28078-7929
McGuire Nuclear Complex - MG03A2
Phone: [phone] Fax: [phone]
Order Summary Report
Analytical Laboratory
Order Number: J15070470
Project Name:MAYO STEAM - AB GW ASSESSMENT SPECIATION
Lab Contact:Peggy Kendall
Date:8/17/2015
Customer Address:
Customer Name(s):Tim Hunsucker, Jerry Wylie, Kathy Webb, John Toepfer
Phone:
Report Authorized By:
(Signature)
Program Comments:
Please contact the Program Manager (Peggy Kendall) with any questions regarding this report.
Data Flags & Calculations:
Any analytical tests or individual analytes within a test flagged with a Qualifier indicate a deviation from the method quality
system or quality control requirement. The qualifier description is found at the end of the Certificate of Analysis (sample results)
under the qualifiers heading. All results are reported on a dry weight basis unless otherwise noted. Subcontracted data
included on the Duke Certificate of Analysis is to be used as information only. Certified vendor results can be found in the
subcontracted lab final report. Duke Energy Analytical Laboratory subcontracts analyses to other vendor laboratories that have
been qualified by Duke Energy to perform these analyses except where noted.
Data Package:
This data package includes analytical results that are applicable only to the samples described in this narrative. An estimation of
the uncertainty of measurement for the results in the report is available upon request. This report shall not be reproduced, except
in full, without the written consent of the Analytical Laboratory. Please contact the Analytical laboratory with any questions. The
order of individual sections within this report is as follows:
Job Summary Report, Sample Identification, Technical Validation of Data Package, Analytical Laboratory Certificate of Analysis,
Analytical Laboratory QC Reports, Sub-contracted Laboratory Results, Customer Specific Data Sheets, Reports &
Documentation, Customer Database Entries, Test Case Narratives, Chain of Custody (COC)
Certification:
The Analytical Laboratory holds the following State Certifications : North Carolina (DENR) Certificate #248, South Carolina
(DHEC) Laboratory ID # 99005. Contact the Analytical Laboratory for definitive information about the certification status of
specific methods.
Peggy Kendall
Page 1 of 27
Sample ID's & Descriptions:
Sample ID Plant/Station
Collection
Date and Time Collected By Sample Description
2015023354 MAYO STEAM 07-Jul-15 12:25 PM Synterra EB1
2015023358 MAYO STEAM 07-Jul-15 10:05 AM Synterra CW-2
2015023359 MAYO STEAM 07-Jul-15 2:15 PM Synterra S-05
2015023360 MAYO STEAM 07-Jul-15 1:17 PM Synterra BG-2
2015023361 MAYO STEAM 07-Jul-15 9:47 AM Synterra CW-2D
5 Total Samples
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COC and .pdf report are in agreement with sample totals
and analyses (compliance programs and procedures).
All Results are less than the laboratory reporting limits.
All laboratory QA/QC requirements are acceptable.
Yes No
Technical Validation Review
Checklist:
Yes No
Yes No
Report Sections Included:
Job Summary Report Sub-contracted Laboratory Results
Sample Identification Customer Specific Data Sheets, Reports, & Documentation
Technical Validation of Data Package Customer Database Entries
Analytical Laboratory Certificate of Analysis
Analytical Laboratory QC Report
Chain of Custody
Reviewed By:Peggy Kendall Date:8/5/2015
Electronic Data Deliverable (EDD) Sent Separately
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Certificate of Laboratory Analysis
This report shall not be reproduced, except in full.
Order # J15070470
2015023354
Collection Date: 07-Jul-15 12:25 PM
Site: EB1
Matrix: GW_WW
Analyte Analysis Date/TimeMethodUnits Qualifiers RDLResult
Sample #:
AnalystDF
Speciation of an Element - (Analysis Performed by Brooks Rand Labs LLC)
Vendor Parameter Complete Vendor Method V_BRAND
Page 4 of 27
Certificate of Laboratory Analysis
This report shall not be reproduced, except in full.
Order # J15070470
2015023358
Collection Date: 07-Jul-15 10:05 AM
Site: CW-2
Matrix: GW_WW
Analyte Analysis Date/TimeMethodUnits Qualifiers RDLResult
Sample #:
AnalystDF
Speciation of an Element - (Analysis Performed by Brooks Rand Labs LLC)
Vendor Parameter Complete Vendor Method V_BRAND
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Certificate of Laboratory Analysis
This report shall not be reproduced, except in full.
Order # J15070470
2015023359
Collection Date: 07-Jul-15 2:15 PM
Site: S-05
Matrix: GW_WW
Analyte Analysis Date/TimeMethodUnits Qualifiers RDLResult
Sample #:
AnalystDF
Speciation of an Element - (Analysis Performed by Brooks Rand Labs LLC)
Vendor Parameter Complete Vendor Method V_BRAND
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Certificate of Laboratory Analysis
This report shall not be reproduced, except in full.
Order # J15070470
2015023360
Collection Date: 07-Jul-15 1:17 PM
Site: BG-2
Matrix: GW_WW
Analyte Analysis Date/TimeMethodUnits Qualifiers RDLResult
Sample #:
AnalystDF
Speciation of an Element - (Analysis Performed by Brooks Rand Labs LLC)
Vendor Parameter Complete Vendor Method V_BRAND
Page 7 of 27
Certificate of Laboratory Analysis
This report shall not be reproduced, except in full.
Order # J15070470
2015023361
Collection Date: 07-Jul-15 9:47 AM
Site: CW-2D
Matrix: GW_WW
Analyte Analysis Date/TimeMethodUnits Qualifiers RDLResult
Sample #:
AnalystDF
Speciation of an Element - (Analysis Performed by Brooks Rand Labs LLC)
Vendor Parameter Complete Vendor Method V_BRAND
This is a revised report and supersedes the initial report dated 8/4/15. The report has been revised to correct date
analyzed values and significant figures that were reported incorrectly in the initial report.
-- Additional Information --
Page 8 of 27

3958 6th Ave NW • Seattle, WA 98107 • T: 206-632-6206 • F: 206-632-6017 • www.brooksrand.com • [e-mail]

August 14, 2015

Peggy Kendall
Duke Energy Analytical Laboratory
Mail Code MGO3A2 (Building 7405)
13339 Hagers Ferry Rd.
Huntersville, NC 28078
980-875-5848

Project: Mayo (LIMS# J15070470)

Ms. Kendall,

Attached is the revised report associated with five (5) aqueous samples submitted for hexavalent
chromium, iron speciation, and manganese speciation analyses on July 7, 2015. The samples
were received in a sealed cooler at -0.1°C on July 8, 2015. This report has been revised to
correct date analyzed values and significant figures that were reported incorrectly in the initial
report. Fe(III) results for the client samples CW-2, S-05, and CW-2D were altered. These
results were calculated incorrectly in the initial report. The EDD format has been corrected to
conform to the EDD design requested. No other changes have been made to this report.

Hexavalent chromium analysis was performed by ion chromatography inductively coupled
plasma dynamic reaction cell mass spectrometry (IC-ICP-DRC-MS). All samples requesting iron
speciation analysis were analyzed by spectrophotometry. Mn(II) analysis was performed via IC-
ICP-CRC-MS. Mn(IV) analysis were performed via digestion and subsequent analysis by
inductively coupled plasma triple quadrupole mass spectrometry (ICP-QQQ-MS). Any issues
associated with the analyses are addressed in the following report.

If you have any questions, please feel free to contact me at your convenience.

Sincerely,
Jeremy Maute
Project Manager
Brooks Rand Labs, LLC
Page 9 of 27
Brooks Rand Labs, LLC

Report prepared for:

Peggy Kendall
Duke Energy Analytical Laboratory
Mail Code MGO3A2 (Building 7405)
13339 Hagers Ferry Rd.
Huntersville, NC 28078

Project: Mayo (LIMS# J15070470)

August 14, 2015

1. Sample Reception

Five (5) aqueous samples were submitted for hexavalent chromium, iron speciation, and
manganese speciation analyses on July 7, 2015. The samples were received in acceptable
condition on July 8, 2015 in a sealed container at a temperature of -0.1°C.

All samples were received in a laminar flow clean hood, void of trace metals contamination
and ultra-violet radiation, and were designated discrete sample identifiers. An aliquot of
each sample submitted for hexavalent chromium analysis was decanted into a clean
polypropylene tube. All hexavalent chromium sample fractions were stored in a secure
refrigerator maintained at a temperature of 4oC, until the analyses could be performed.

The sample fractions requesting iron speciation analysis were stored in a secure, monitored
refrigerator (maintained at a temperature of ≤6oC) until the analyses could be performed.

An aliquot of each filtered sample submitted for manganese speciation analysis was decanted
into a polypropylene centrifuge tube for Mn(II) analysis. These fractions were stored in a
secure, monitored refrigerator (maintained at a temperature of ≤6oC) until the analyses could
be performed. Subsequently, the original bottles (filtered and unfiltered fractions) intended
for Mn speciation were preserved to pH < 2 with concentrated HNO3 and then stored in a
secure polyethylene container, known to be free from trace metals contamination, until the
digestion could be performed.

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.

Hexavalent Chromium 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
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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.

Iron Speciation Analysis by Spectrophotometry No sample preparation was required as a de-
gassed HCL solution was provided by Brooks Rand Labs for field-preservation of the
submitted samples.

Manganese Mn(II) Analysis by IC-ICP-CRC-MS An aliquot of each sample was filtered
(0.45µm) directly into an autosampler vial for Mn(II) analysis. No additional sample
preparation was performed as any chemical alteration of the samples may shift the
equilibrium of the system resulting in changes in speciation ratios.

Manganese Mn(IV) Analysis by ICP-QQQ-MS Each filtered and unfiltered sample submitted
for Mn speciation analysis was preserved with 1% HNO3 (v/v) upon sample receipt. Each
sample fraction was then further digested on a hotblock apparatus with aliquots of 50%
HNO3 (v/v) and 50% HCl (v/v), in accordance with the digestion procedure specified in EPA
Method 200.8. All resulting sample digests were analyzed for total manganese via
inductively coupled plasma triple quadrupole mass spectrometry (ICP-QQQ-MS).

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
standardized by linear regression resulting in a response factor. All sample results are
instrument blank corrected to account for any operational biases associated with the
analytical platform.

Prior to sample analysis, all calibration curves are verified using second source standards
which are identified as initial calibration verification standards (ICV).

Ongoing instrument performance is identified by the analysis of continuing calibration
verification standards (CCV) and continuing calibration blanks (CCB) at a minimum interval
of every ten analytical runs.

Hexavalent Chromium Analysis by IC-ICP-DRC-MS Each sample for hexavalent chromium
analysis was analyzed by ion chromatography inductively coupled plasma dynamic reaction
cell mass spectrometry (IC-ICP-DRC-MS) on July 15, 2015. An aliquot of each sample is
injected onto an anion exchange column and mobilized by a basic (pH > 7) gradient. The
eluting chromium 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.

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Retention times for each eluting species are compared to known standards for species
identification.

Iron Speciation Analysis by Spectrophotometry All samples submitted for Fe speciation
quantification were analyzed on July 8, 2015 and July 9, 2015 and in accordance with the
scientifically accepted method outlined by:

Stookey, L.L., (1970). “Ferrozine - A new spectrophotometric reagent for iron”,
Anal.Chem., 42:779-81.

Manganese Mn(II) Analysis by IC-ICP-CRC-MS All samples for Mn(II) analysis were
analyzed by ion chromatography inductively coupled plasma collision reaction cell mass
spectrometry (IC-ICP-CRC-MS) on July 13, 2015. Aliquots of each sample are injected onto
an anion exchange column and mobilized by an acidic (pH < 7) gradient. An ion pairing
agent provides a dynamic ion exchange mechanism for the cationic manganese species on the
chromatographic column. The differences in the affinity of manganese species towards the
ion pair agent and the column results in separation. 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.

Manganese Mn(IV) Analysis by ICP-QQQ-MS All samples submitted for Mn speciation
quantitation were analyzed by inductively coupled plasma triple quadrupole mass
spectrometry (ICP-QQQ-MS) on July 23, 2015. Aliquots of each sample digest are
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 an initial quadrupole (Q1), which
filters the target masses prior to their entrance into a second chamber. The second chamber
contains specific reactive gasses or collision gasses that preferentially react either with
interfering ions of the same target mass to charge ratios (m/z) or with the target analyte,
producing an entirely different mass to charge ratio (m/z) which can then be differentiated
from the initial interferences. The ions then exit the collision/reaction cell into and additional
quadrupole (Q2). A solid-state detector detects ions transmitted through the mass analyzer,
on the basis of their mass-to-charge ratio (m/z), and the resulting current is processed by a
data handling system.

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4. Analytical Issues

No significant analytical issues were encountered. All quality control parameters associated
with the samples were within acceptance limits.

The preparation blanks associated with the iron speciation samples were not analyzed. The
equipment blank sample EB1 yielded non-detect results for both Fe(II) and total iron,
demonstrating the absence of significant iron contamination due to the containers, the
preservative employed, and the equipment used to collect the samples.

Mn(IV) is quantified by analyzing the water samples for total Mn and dissolved Mn. Mn(IV)
is operationally defined as the difference between the filtered and unfiltered total Mn
concentrations, since it is thermodynamically favored to be in the form of a precipitate.

The estimated method detection limit (eMDL) for hexavalent chromium is generated from
replicate analyses of the lowest standard in the calibration curve.

The eMDL values for Fe(II) and total recoverable Fe were set at 5 based on the sensitivity of
the instrument.

The eMDL for Mn(II) has been generated from replicate analyses of the lowest standard in
the calibration curve.

The eMDL values for Mn(IV) been calculated using the standard deviation of the method
blanks prepared and analyzed concurrently with the submitted samples.

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

Sincerely,
Jeremy Maute
Project Manager
Brooks Rand Labs, LLC

Page 13 of 27
Sample Results (1)
Sample ID Cr(VI)
EB1 ND (< 0.021)
CW-2 0.100
S-05 0.612
BG-2 ND (< 0.021)
CW-2D 0.084
All results reflect the applied dilution and are reported in µg/L
ND = Not detected at the applied dilution
Contact: Peggy Kendall
LIMS# J15070470
Date: August 14, 2015
Report Generated by: Jeremy Maute
Brooks Rand Labs, LLC
Speciation Results for Duke Energy
Project Name: Mayo
Page 14 of 27
Sample Results (2)
Sample ID Fe(II)Fe(III)*Mn (II)Mn(IV)**
EB1 ND(<5.0)ND(<5.0)ND(<0.46)ND(<0.39)
CW-2 ND(<5.0)7.0 347 19.3
S-05 ND(<5.0)11.6 6.78 32.0
BG-2 331 ND(<5.0)141 8.53
CW-2D ND(<5.0)7.0 7.00 77.7
All results reflect the applied dilution and are reported in µg/L
ND = Not detected at the applied dilution
*Fe(III) operationally defined as the difference between total recoverable Fe and Fe(II)
*Mn(IV) operationally defined as the difference between total and dissolved Mn
Brooks Rand Labs, LLC
Speciation Results for Duke Energy
Project Name: Mayo
Contact: Peggy Kendall
LIMS# J15070470
Date: August 14, 2015
Report Generated by: Jeremy Maute
Page 15 of 27
Quality Control Summary - Preparation Blank Summary (1)
Analyte (µg/L)PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL*eMDL 5x RL 5x
Cr(VI)0.002 0.000 0.001 0.002 0.001 0.001 0.004 0.021 0.050
eMDL = Estimated Method Detection Limit; RL = Reporting Limit
*Please see narrative regarding eMDL calculations
Contact: Peggy Kendall
LIMS# J15070470
Date: August 14, 2015
Report Generated by: Jeremy Maute
Brooks Rand Labs, LLC
Speciation Results for Duke Energy
Project Name: Mayo
Page 16 of 27
Quality Control Summary - Preparation Blank Summary (2)
Analyte (µg/L)PBW1*PBW2*PBW3*PBW4*Mean StdDev eMDL**eMDL 1x RL 1x
Fe(II)****5.0 5.0 20
Total Fe ****5.0 5.0 20
eMDL = Estimated Method Detection Limit; RL = Reporting Limit
*Preparation blanks for Fe speciation were not analyzed. See narrative.
**Please see narrative regarding eMDL calculations
Quality Control Summary - Preparation Blank Summary (2)
Analyte (µg/L)PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL*eMDL 10x RL 10x eMDL 25x RL 25x
Mn (II)-0.60 -0.60 -0.60 -0.60 -0.60 0.00 0.046 0.46 5.0 --
Total Mn 0.16 0.21 0.15 0.14 0.17 0.03 0.004 --0.10 1.0
Diss Mn 0.32 0.08 0.07 0.03 0.16 0.13 0.016 --0.39 1.0
eMDL = Estimated Method Detection Limit; RL = Reporting Limit
*Please see narrative regarding eMDL calculations
Report Generated by: Jeremy Maute
Brooks Rand Labs, LLC
Speciation Results for Duke Energy
Project Name: Mayo
Contact: Peggy Kendall
LIMS# J15070470
Date: August 14, 2015
Page 17 of 27
Quality Control Summary - Certified Reference Materials (1)
Analyte (µg/L)CRM True Value Result Recovery
Cr(VI)LCS 2.002 1.983 99.0
Quality Control Summary - Certified Reference Materials (2)
Analyte (µg/L)CRM True Value Result Recovery
Fe(II)ICV 500.0 468.0 93.6
Total Fe TMDA-70 369.0 394.0 106.8
Mn (II)LCS 10.00 10.35 103.5
Total Mn TMDA-70.2 312 302.6 97.0
Diss Mn TMDA-70.2 312 308.2 98.8
Report Generated by: Jeremy Maute
Brooks Rand Labs, LLC
Speciation Results for Duke Energy
Project Name: Mayo
Contact: Peggy Kendall
LIMS# J15070470
Date: August 14, 2015
Page 18 of 27
Quality Control Summary - Matrix Duplicates (1)
Analyte (µg/L)Sample ID Rep 1 Rep 2 Mean RPD
Cr(VI)Batch QC ND (< 0.021)ND (< 0.021)NC NC
ND = Not detected at the applied dilution
NC = Value was not calculated due to one or more concentrations below the eMDL
Report Generated by: Jeremy Maute
Brooks Rand Labs, LLC
Speciation Results for Duke Energy
Project Name: Mayo
Contact: Peggy Kendall
LIMS# J15070470
Date: August 14, 2015
Page 19 of 27
Quality Control Summary - Matrix Duplicates (2)
Analyte (µg/L)Sample ID Rep 1 Rep 2 Mean RPD
Fe(II)CW-2 ND (< 5.0)ND (< 5.0)NC NC
Total Fe CW-2 7.0 ND (< 5.0)NC NC
Mn (II)Batch QC 344.9 336.9 340.9 2.3
Total Mn Batch QC 0.32 0.42 0.37 26.3*
Diss Mn Batch QC ND(<0.39)ND(<0.39)NC NC
NC = Value was not calculated due to one or more concentrations below the eMDL
*Results associated with RPD outlier are less than the Reporting Limit
Report Generated by: Jeremy Maute
Brooks Rand Labs, LLC
Speciation Results for Duke Energy
Project Name: Mayo
Contact: Peggy Kendall
LIMS# J15070470
Date: August 14, 2015
Page 20 of 27
Quality Control Summary - Matrix Spike/ Matrix Spike Duplicate (1)
Analyte (µg/L)Sample ID Spike Conc MS Result Recovery Spike Conc MSD Result Recovery RPD
Cr(VI)Batch QC 5.000 4.857 97.1 5.000 4.917 98.3 1.2
Quality Control Summary - Matrix Spike/ Matrix Spike Duplicate (2)
Analyte (µg/L)Sample ID Spike Conc MS Result Recovery Spike Conc MSD Result Recovery RPD
Fe(II)CW-2 500.0 519.8 104.0 500.0 558.5 111.7 7.2
Total Fe CW-2 500.0 472.8 94.6 500.0 472.8 94.6 0.0
Mn (II)Batch QC 50.0 390.8 99.8 50.0 398.1 114.4 0.8
Total Mn Batch QC 1000 1060 105.9 1000 960.4 96.0 9.8
Diss Mn Batch QC 1000 914.4 91.4 1000 927.9 92.8 1.5
Report Generated by: Jeremy Maute
Brooks Rand Labs, LLC
Speciation Results for Duke Energy
Project Name: Mayo
Contact: Peggy Kendall
LIMS# J15070470
Date: August 14, 2015
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