HomeMy WebLinkAboutNC0001422_ATT 5 - Speciation - J15060166F_2015080513339 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: J15060166
Project Name:SUTTON - AB GW ASSESSMENT SPECIATION
Lab Contact:Peggy Kendall
Date:7/2/2015
Customer Address:
Customer Name(s):Perry Waldrep, Tim Hunsucker, 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
2015017417 Sutton 02-Jun-15 11:23 AM Synterra MW24C
2015017418 Sutton 02-Jun-15 9:50 AM Synterra MW24B
2015017419 Sutton 02-Jun-15 Synterra MW23C
2015017420 Sutton 02-Jun-15 9:46 AM Synterra MW12
4 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.
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:7/2/2015
Electronic Data Deliverable (EDD) Sent Separately
Page 3 of 27
Certificate of Laboratory Analysis
This report shall not be reproduced, except in full.
Order # J15060166
2015017417
Collection Date: 02-Jun-15 11:23 AM
Site: MW24C
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 # J15060166
2015017418
Collection Date: 02-Jun-15 9:50 AM
Site: MW24B
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 5 of 27
Certificate of Laboratory Analysis
This report shall not be reproduced, except in full.
Order # J15060166
2015017419
Collection Date: 02-Jun-15
Site: MW23C
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 6 of 27
Certificate of Laboratory Analysis
This report shall not be reproduced, except in full.
Order # J15060166
2015017420
Collection Date: 02-Jun-15 9:46 AM
Site: MW12
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
3958 6th Ave NW • Seattle, WA 98107 • T: 206-632-6206 • F: 206-632-6017 • www.brooksrand.com • brl@brooksrand.com
July 2, 2015
Peggy Kendall
Duke Energy Analytical Laboratory
Mail Code MGO3A2 (Building 7405)
13339 Hagers Ferry Rd.
Huntersville, NC 28078
980-875-5848
Project: Duke Sutton Wilmington (LIMS# J15060166)
Mr. Perkins,
Attached is the report associated with four (4) aqueous samples submitted for hexavalent
chromium, selenium speciation, arsenic speciation, iron speciation, and manganese speciation
analyses on June 2, 2015. The samples were received in a sealed cooler at -0.1°C on June 3,
2015. Hexavalent chromium analysis was performed by ion chromatography inductively
coupled plasma dynamic reaction cell mass spectrometry (IC-ICP-DRC-MS). Selenium
speciation and arsenic speciation analyses were performed via ion chromatography inductively
coupled plasma collision reaction cell mass spectrometry (IC-ICP-CRC-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 8 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: Duke Sutton Wilmington (LIMS# J15060166)
July 2, 2015
1. Sample Reception
Four (4) aqueous samples were submitted for hexavalent chromium, selenium speciation,
arsenic speciation, iron speciation, and manganese speciation analyses on June 2, 2015. All
samples were received in acceptable condition on June 3, 2015 in a sealed container at
-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. Sample fractions
requesting hexavalent chromium, selenium speciation, arsenic speciation, and iron speciation
analyses were field filtered by the client. Two containers were submitted for each client
sample requesting manganese speciation, one field filtered fraction and one unfiltered
fraction. 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.
An aliquot of each sample requiring selenium speciation evaluation was decanted into a
polypropylene centrifuge tube and each filtrate was stored in a secure, monitored cryofreezer
(maintained at a temperature of -80°C) until selenium speciation analysis could be
performed. The original bottles were then stored in a secure, monitored refrigerator
(maintained at a temperature of ≤6oC).
An aliquot of each sample submitted for arsenic speciation analysis was decanted into a
polypropylene centrifuge tube; all fractions were then stored in a secure, monitored
refrigerator (maintained at a temperature of ≤6oC) 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.
Page 9 of 27
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
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.
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.
Arsenic Speciation Analysis by IC-ICP-CRC-MS An aliquot of each sample was filtered
directly into a sealed autosampler vial. No further sample preparation was performed as a
buffered EDTA solution was provided by Brooks Rand Labs for field-preservation of the
submitted samples.
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).
Page 10 of 27
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 June 5-6, 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.
Retention times for each eluting species are compared to known standards for species
identification.
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 June 4-5, 2015. 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.
Page 11 of 27
Arsenic Speciation Analysis by IC-ICP-CRC-MS Each sample was analyzed for arsenic
speciation via ion chromatography inductively coupled plasma collision reaction cell mass
spectrometry (IC-ICP-CRC-MS) on June 4, 2015. Aliquots of each sample are injected onto
an anion exchange column and eluted isocratically. The eluting arsenic 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 specific collision gas. Polyatomic interferences, due to their inherently larger
size, collide more frequently with the collision gas and therefore may be separated from the
analyte of interest via kinetic energy discrimination (KED). 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.
Retention times for each eluting species are compared to known standards for species
identification.
Iron Speciation Analysis by Spectrophotometry All sample fractions submitted for iron
speciation were analyzed for Fe(II) quantification on June 3, 2015. All sample fractions
submitted for iron speciation were analyzed for Fe(III) quantification on June 25, 2015. The
samples were analyzed for iron speciation 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 June 5, 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.
Page 12 of 27
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 June 30, 2015 and July 1, 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.
4. Analytical Issues
No significant analytical issues were encountered. All quality control parameters associated
with the samples were within acceptance limits.
Preparation blanks were not analyzed for Fe(II) analysis. The preparation blanks were
analyzed or Fe(III) analysis. No iron was detected in any of the total iron preparation blanks,
demonstrating the absence of iron contamination due to the containers or the preservative
employed. One non-detect result was reported for Fe(II), demonstrating the absence of any
significant iron contamination due to the equipment used to collect and filter 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 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 values for methylseleninic acid and selenomethionine are 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.
The eMDL values for arsenite, arsenate, and dimethylarsinic acid are generated using the
standard deviation of replicate analyses of the lowest standard in the calibration curve. The
Page 13 of 27
eMDL for monomethylarsonic acid is calculated from the average eMDL of the three arsenic
species contained in the calibration (i.e., arsenite, arsenate, and dimethylarsinic acid); the
calibration and CCVs do not contain monomethylarsonic acid due to impurities in this
standard which would bias the results for other arsenic species.
The eMDL values for iron speciation results have been generated from replicate analyses of
the lowest standard in the calibration curve.
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.
The fourth preparation blank for total manganese analysis was determined to be a statistical
outlier according to the Grubb’s Test. The blank was not used for the eMDL calculations
presented in this report.
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 14 of 27
Sample Results (1)
Sample ID Cr(VI)Se(IV)Se(VI)SeCN MeSe(IV)SeMe
Unknown Se
Species (n)
MW24C 0.019 ND (< 0.080)ND (< 0.065)ND (< 0.098)ND (< 0.081)ND (< 0.081)0 (0)
MW24B 0.098 0.267 0.288 ND (< 0.098)ND (< 0.081)ND (< 0.081)0 (0)
MW23C 0.022 ND (< 0.080)ND (< 0.065)ND (< 0.098)ND (< 0.081)ND (< 0.081)0 (0)
MW12 0.013 ND (< 0.080)ND (< 0.065)ND (< 0.098)ND (< 0.081)ND (< 0.081)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: Jeremy Maute
Brooks Rand Labs, LLC
Speciation Results for Duke Energy
Project Name: Duke Sutton Wilmington
Contact: Peggy Kendall
Date: July 2, 2015
LIMS# J15060166
Page 15 of 27
Sample Results (2)
Sample ID As(III)As(V)MMAs DMAs
Unknown As
Species
MW24C 1.74 0.30 ND (< 0.054)ND (< 0.038)ND (< 0.054)
MW24B ND (< 0.018)ND (< 0.11)ND (< 0.054)ND (< 0.038)ND (< 0.054)
MW23C 0.039 ND (< 0.11)ND (< 0.054)ND (< 0.038)ND (< 0.054)
MW12 0.037 ND (< 0.11)ND (< 0.054)ND (< 0.038)ND (< 0.054)
All results reflect the applied dilution and are reported in µg/L
ND = Not detected at the applied dilution
MMAs = monomethylarsonic acid
DMAs = dimethylarsinic acid
Unknown As Species = Total concentration of all unknown As species observed by IC-ICP-MS
Brooks Rand Labs, LLC
Speciation Results for Duke Energy
Project Name: Duke Sutton Wilmington
Contact: Peggy Kendall
LIMS# J15060166
Date: July 2, 2015
Report Generated by: Jeremy Maute
Page 16 of 27
Sample Results (3)
Sample ID Fe(II)Fe(III)*Mn (II)Mn(IV)**
MW24C 1820 600 270 ND (< 0.088)
MW24B ND (< 8.3)14.2 34.8 ND (< 0.088)
MW23C 138 ND (< 41)269 37.3
MW12 4330 1570 795 ND (< 0.088)
All results reflect the applied dilution and are reported in µg/L
ND = Not detected at the applied dilution
*Fe(III) 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: Duke Sutton Wilmington
Contact: Peggy Kendall
LIMS# J15060166
Date: July 2, 2015
Report Generated by: Jeremy Maute
Page 17 of 27
Quality Control Summary - Preparation Blank Summary (1)
Analyte (µg/L)PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL*eMDL 5x RL 5x eMDL 50x RL 50x
Cr(VI)0.002 0.005 0.001 0.005 0.003 0.002 0.001 0.007 0.050 --
Se(IV)0.000 0.000 0.000 0.000 0.000 0.000 0.002 --0.080 0.50
Se(VI)0.000 0.000 0.000 0.000 0.000 0.000 0.001 --0.065 0.50
SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.002 --0.098 0.46
MeSe(IV)0.000 0.000 0.000 0.000 0.000 0.000 0.002 --0.081 0.49
SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.002 --0.081 0.49
eMDL = Estimated Method Detection Limit; RL = Reporting Limit
*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
As(III)0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.018 0.20
As(V)0.00 0.00 0.00 0.00 0.00 0.00 0.011 0.11 0.20
MMAs 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.054 0.20
DMAs 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.038 0.21
eMDL = Estimated Method Detection Limit; RL = Reporting Limit
*Please see narrative regarding eMDL calculations
Brooks Rand Labs, LLC
Speciation Results for Duke Energy
Project Name: Duke Sutton Wilmington
Contact: Peggy Kendall
LIMS# J15060166
Date: July 2, 2015
Report Generated by: Jeremy Maute
Page 18 of 27
Quality Control Summary - Preparation Blank Summary (3)
Analyte (µg/L)PBW1*PBW2*PBW3*PBW4*Mean StdDev eMDL**eMDL 2x RL 2x eMDL 10x RL 10x
Fe(II)****4.1 8.3 40 41 200
Total Fe 0.0 0.0 0.0 0.0 0.0 0.0 4.1 8.2 40 41 200
eMDL = Estimated Method Detection Limit; RL = Reporting Limit
*Preparation blanks for Fe(II) were not analyzed. See narrative.
**Please see narrative regarding eMDL calculations
Quality Control Summary - Preparation Blank Summary (3)
Analyte (µg/L)PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL*eMDL 10x RL 10x eMDL 25x RL 25x
Mn (II)-0.66 -0.79 -0.66 -0.75 -0.70 0.07 0.086 0.86 5.0 --
Total Mn 0.104 0.093 0.108 ***0.101 0.008 0.001 --0.023 1.0
Diss Mn -0.035 0.007 -0.035 0.022 -0.021 0.029 0.004 --0.088 1.0
eMDL = Estimated Method Detection Limit; RL = Reporting Limit
*Please see narrative regarding eMDL calculations
***Preparation blank is a statistical outlier according to the Grubb's Test. Please see narrative.
Speciation Results for Duke Energy
Brooks Rand Labs, LLC
Project Name: Duke Sutton Wilmington
Contact: Peggy Kendall
LIMS# J15060166
Date: July 2, 2015
Report Generated by: Jeremy Maute
Page 19 of 27
Quality Control Summary - Certified Reference Materials (1)
Analyte (µg/L)CRM True Value Result Recovery
Cr(VI)LCS 2.002 1.781 89.0
Se(IV)LCS 10.00 10.03 100.3
Se(VI)LCS 10.00 10.32 103.2
SeCN LCS 8.92 8.821 98.9
MeSe(IV)LCS 6.47 6.709 103.7
SeMe LCS 9.32 9.547 102.4
Quality Control Summary - Certified Reference Materials (2)
Analyte (µg/L)CRM True Value Result Recovery
As(III)LCS 5.00 5.824 116.5
As(V)LCS 5.00 5.244 104.9
MMAs LCS 5.07 5.657 111.5
DMAs LCS 3.63 3.700 102.1
Quality Control Summary - Certified Reference Materials (3)
Analyte (µg/L)CRM True Value Result Recovery
Fe(II)ICV 500.0 394.1 78.8
Total Fe TMDA-70.2 376 388.9 103.4
Mn (II)LCS 1.00 1.053 105.3
Total Mn TMDA-70.2 312 315.3 101.1
Diss Mn TMDA-70.2 312 310.5 99.5
Report Generated by: Jeremy Maute
Brooks Rand Labs, LLC
Speciation Results for Duke Energy
Project Name: Duke Sutton Wilmington
Contact: Peggy Kendall
LIMS# J15060166
Date: July 2, 2015
Page 20 of 27
Quality Control Summary - Matrix Duplicates (1)
Analyte (µg/L)Sample ID Rep 1 Rep 2 Mean RPD
Cr(VI)Batch QC 0.059 0.060 0.059 0.9
Se(IV)MW12 ND (< 0.080)ND (< 0.080)NC NC
Se(VI)MW12 ND (< 0.065)ND (< 0.065)NC NC
SeCN MW12 ND (< 0.098)ND (< 0.098)NC NC
MeSe(IV)MW12 ND (< 0.081)ND (< 0.081)NC NC
SeMe MW12 ND (< 0.081)ND (< 0.081)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 Duplicates (2)
Analyte (µg/L)Sample ID Rep 1 Rep 2 Mean RPD
As(III)Batch QC ND (< 0.018)ND (< 0.018)NC NC
As(V)Batch QC ND (< 0.11)ND (< 0.11)NC NC
MMAs Batch QC ND (< 0.054)ND (< 0.054)NC NC
DMAs Batch QC ND (< 0.038)ND (< 0.038)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: Duke Sutton Wilmington
Contact: Peggy Kendall
LIMS# J15060166
Date: July 2, 2015
Page 21 of 27
Quality Control Summary - Matrix Duplicates (3)
Analyte (µg/L)Sample ID Rep 1 Rep 2 Mean RPD
Fe(II)MW24C 1819 1681 1750 7.9
Total Fe Batch QC 7.1 4.7 5.9 40.0*
Mn (II)Batch QC 51.73 50.31 51.02 2.8
Total Mn Batch QC 1069 1106 1088 3.4
Diss Mn Batch QC 1073 1079 1076 0.5
ND = Not detected at the applied dilution
NC = Value was not calculated due to one or more concentrations below the eMDL
*Associated results were less than the RL
Report Generated by: Jeremy Maute
Brooks Rand Labs, LLC
Speciation Results for Duke Energy
Project Name: Duke Sutton Wilmington
Contact: Peggy Kendall
LIMS# J15060166
Date: July 2, 2015
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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 4.824 95.3 5.000 5.180 102.4 7.1
Se(IV)MW12 251.0 263.3 104.9 251.0 265.6 105.8 0.9
Se(VI)MW12 250.0 260.7 104.3 250.0 260.8 104.3 0.1
SeCN MW12 228.8 236.1 103.2 228.8 236.8 103.5 0.3
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
As(III)Batch QC 20.00 21.09 105.5 20.00 21.05 105.3 0.2
As(V)Batch QC 20.00 21.07 105.4 20.00 20.99 104.9 0.4
DMAs Batch QC 20.98 22.06 105.2 20.98 22.04 105.0 0.1
Quality Control Summary - Matrix Spike/ Matrix Spike Duplicate (3)
Analyte (µg/L)Sample ID Spike Conc MS Result Recovery Spike Conc MSD Result Recovery RPD
Fe(II)MW24C 2500 4271 100.9 2500 3968 88.7 7.4
Total Fe Batch QC 500.0 488.5 96.5 500.0 486.1 96.0 0.5
Mn (II)Batch QC 50.00 98.35 94.7 50.00 101.7 101.3 3.3
Total Mn Batch QC 1000 2046 95.8 1000 2069 98.1 1.1
Diss Mn Batch QC 1000 2051 97.5 1000 2072 99.6 1.0
Report Generated by: Jeremy Maute
Brooks Rand Labs, LLC
Speciation Results for Duke Energy
Project Name: Duke Sutton Wilmington
Contact: Peggy Kendall
LIMS# J15060166
Date: July 2, 2015
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