vxEPA
United States
Environmental Protection
Agency
Results of the Analyses of
Screening Surface and Well
Water Samples from Decatur,
Alabama for Selected
Perfluorinated Compounds
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EPA 600/C-09-004
May 2009
www.epa.gov
Results of the Analyses of
Screening Surface and Well
Water Samples from Decatur,
Alabama for Selected
Perfluorinated Compounds
Original Report Date: April 16, 2009
Revised Report Date: April 22, 2009
Andrew B. Lindstrom, Mark J. Strynar, Amy D. Delinsky, Larry McMillan
Human Exposure and Atmospheric Sciences Division
National Exposure Research Laboratory
U. S. Environmental Protection Agency
Research Triangle Park, NC 27711
Shoji F. Nakayama
Land Remediation and Pollution Control Division
National Risk Management Research Laboratory
U. S. Environmental Protection Agency
Research Triangle Park, NC 27711
U.S. Environmental Protection Agency
Office of Research and Development
Washington, DC 20460
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Results of the Analyses of Screening Surface and Well Water Samples from
Decatur, Alabama for Selected Perfluorinated Compounds
Original Report Date: April 16, 2009
Revised Report Date: April 22, 2009
Principle Investigators: Mike Neill, EPA/Region 4/SESD
Field Sampling: Mike Neill, EPA/Region 4/SESD
Sample Analysis: Andrew B. Lindstrom, Ph.D., Mark J.Strynar, Ph.D., Amy D. Delinsky, Ph.D.,
Larry McMillan, EPA/ORD/NERL; Shoji F. Nakayama, Ph.D. EPA/ORD/NRMRL
Disclaimer: The United States Environmental Protection Agency through its Office of
Research and Development funded and managed the work described here. It has been
subjected to the Agency's administrative review and approved for publication
Introduction
EPA has conducted testing of agricultural sites in Alabama where sewage sludge was applied from
a local wastewater treatment plant that receives wastewater from numerous industrial sources,
including facilities that manufacture and use perfluorooctanoic acid (PFOA) and other
perfluorinated chemicals (PFCs). The results from the initial limited testing indicated elevated
levels of PFCs in the sewage sludge and the soil that received the sewage sludge. As a result, EPA
conducted sampling of public drinking water, private wells, springs, ponds, and soil in the area. In
January 2009, EPA developed drinking water Provisional Health Advisories for PFOA and
perfluorooctane sulfonate (PFOS) (Reference No. 1) to provide information in response to an
urgent and rapidly developing situation. These short term Provisional Health Advisories reflect
reasonable, health-based hazard concentrations above which action should be taken to reduce
exposure to unregulated contaminants in drinking water. The Provisional Health Advisories are
0.4 ppb (400 ng/L) for PFOA and 0.2 ppb (200 ng/L) for PFOS. The levels of PFOA and PFOS
recently analyzed in community water systems in Lawrence and Morgan Counties were all lower
than 0.04 ppb (2).
EPA conducted a small scale reconnaissance screening level study in which Region 4 staff
collected a limited number of groundwater and surface water samples during the period of
February 16-19, 2009. A total of 51 samples collected from surface and potable water sources
were submitted for PFC analysis. Analyses were performed in EPA's Office of Research and
Development (ORD) laboratory to assess if perfluorochemicals have migrated into private
drinking water supplies, ponds, and streams in the affected area. The purpose for collection and
analyses of these 51 samples was to determine if the concentrations of PFOA and PFOS were at
or above the Provisional Health Advisory levels. These analyses were not intended to measure
low levels of the PFCs that may be present at concentrations below the calibration range discussed
in this document.
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This report provides a description of the methods used for the collection and analyses,
documentation of the quality control samples, and the resulting measured concentrations of the
selected perfluorinated chemicals, including PFOA and PFOS, measured in the 51 water samples
submitted by EPA Region 4 for analysis.
Methods
Sample Collection
The field portion of this study was conducted by USEPA Region 4 personnel following the
procedures established in their Quality Assurance Project Plan (QAPP) entitled "Land Application
Site Near Decatur, Alabama - Private Wells Perfluorinated Compounds Study" (3). The
Perfluorinated Chemicals (PFC) laboratory in the National Exposure Research Laboratory
(NERL) of ORD, located in Research Triangle Park, NC, prepared and sent Region 4 personnel the
materials used for the collection of these samples. Sampling materials were shipped to Region 4
personnel on February 11, 2009. The shipment consisted of five individual shipping containers,
with each container holding one prepared field blank, two prepared field spikes (one with each
target analyte listed in Table 1 at 200 ng/L and another with each target analyte at 400 ng/L), and
12 pre-cleaned (triple rinsed with methanol and dried) 1-L FtDPE (Nalgene) sampling bottles. A
few additional wide-mouth containers were also included for use as water transfer vessels in cases
where source access might make direct filling of the narrow-mouth sampling bottles difficult.
The selection of sampling locations and the collection of the surface and well water samples were
the responsibility of Region 4 personnel. Methods used for sample collection are outlined in the
NERL/HEASD SOP No. EMAB-113-0 entitled "Sample Collection Protocol for PFCs in Surface
and Well Water (4). The specific sampling method was dependent on the source of water being
sampled; however, the basic process involved rinsing the collection bottle with three volumes of
water followed by filling on the fourth iteration and adding 5 mL of 35% nitric acid as a
preservation agent. Duplicate samples were collected at a rate of 10%. Samples were labeled with
unique codes as well as the appropriate information providing time, date, location and water
source type. Samples were maintained at ambient temperature after collection. All samples were
shipped on February 20, 2009 to the RTF PFC laboratory for analysis, with chain of custody (CoC)
forms recording collection, shipment, and receipt (Appendix 1).
Sample Analysis
Analysis of samples was conducted by the RTF PFC team following the procedures established in
the NERL/FIEASD Quality Assurance Project Plan entitled "The Analysis of Screening Surface
and Well Water Samples for Selected Perfluorinated Compounds from Decatur, Alabama" (5).
The chemical analyses were performed using the method outlined in SOP # EMAB 114.0
"Improved Method for the Extraction and Analysis of Perfluorinated Compounds (PFCs) from
Surface and Well Water by Ultra-High Performance Liquid Chromatography (UPLC)-Tandem
Mass Spectrometry (MS/MS)" (6).
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Actual water volumes were determined, sample containers were rinsed with methanol and the
rinsate combined with the original water sample. The sample was then spiked with an internal
standard mixture. Waters Oasis WAX solid phase extraction (SPE) cartridges were used for the
retention and purification of the target PFCs. After capture and washing, the target PFCs were
eluted from the SPE cartridges and the eluates were analyzed using a UPLC-MS/MS operated in
negative electrospray ionization (ESI) mode.
For the analyses of these water samples, a method previously developed for trace level analysis (7)
was modified to measure midlevel concentrations (10 -1000 ng/L) of the target analytes to allow
for more accurate comparison with the Provisional Health Advisories for PFOA and PFOS (400
ng/L and 200 ng/L, respectively). To achieve this purpose, it was necessary to calibrate the
LC/MS/MS over a range of concentrations from 10 to 1000 ng/L. Quantitation was performed
using a multipoint calibration curve and internal standard calculation. The Limit of Quantitation
(LOQ) of the modified method, defined as the lowest point on the standard curve which
back-predicted within ±30% of the theoretical value, was determined to be 10 ng/L (0.01 ppb) for
all compounds except the C7 and CIO acids, which were 50 ng/L (0.05 ppb). It should be noted
that the LOQ for these 51 water samples is much higher than the LOQ of 0.2 ng/L determined for
the previously developed trace level method (7) and was based on the lowest calibration standard.
The limit of detection (LOD) and LOQ have been defined in a number of ways in the scientific
community, including EPA's Occupational and Residential Exposure Test Guidelines (8). The
EPA Office of Prevention, Pesticides and Toxic Substances' (OPPTS') preferred procedure is to
define LOD as the concentration having a signal-to-noise ratio of 3, and LOQ as 3.3 times the
LOD. These are considered typical and acceptable definitions for LOD and LOQ. However, for
the purposes of these analyses to identify samples with concentrations at or above 200 ng/L, the
use of the higher LOQ was reasonable and most expeditious for reporting the measurement results.
Table 2 is a summary of the LC/MS/MS parameters used in this assessment.
Analyte concentrations were determined using the stable-isotope internal standard method using
the response of the analyte (peak area counts) divided by the response of the internal standard to
calculate unknown concentrations. Appendix 2 contains the standard curves used to calculate the
concentrations of the samples measured in this survey.
Quality Control
The collection and analytical processes included prescribed quality control (QC) procedures to
document data quality and assay performance. These QC procedures included the following:
Field Blanks
Field blanks were used to monitor for potential contamination in all steps of the process, to include
the purity of all reagents used, possible contamination of sample storage bottles, potential
contamination associated with shipping and sample collection procedures, and possible
contamination during sample preparation and analysis in the laboratory. Field blanks were
prepared in the RTF PFC laboratory by filling pre-cleaned 1 L collection bottles with deionized
laboratory grade water, previously determined to be PFC-free. The samples were preserved with
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the addition of 5 mL of 35% nitric acid, and shipped into the field with the empty containers
designated for collection of field samples. The field blanks were included at a rate of 10% of all
planned samples.
Field Spikes
Field spikes were used to monitor how sample preparation, collection, storage, and analysis
procedures potentially influence target analyte recovery. Field spikes were prepared at low (200
ng/L) and high (400 ng/L) levels of all of the compounds on the target list (Table 1). These
samples were preserved with the addition of 5 mL of 35% nitric acid and shipped into the field
with the empty containers designated for collection of field samples. Both low and high level field
spikes were included at a rate of 10% of all planned field samples (e.g., 5 low level and 5 high level
spikes).
Field Duplicates
Field duplicates were used to document precision (repeatability) of the entire process, to include
potential variability in reagents, sample storage bottles, differences in sample collection
technique, and possible variation in sample processing in the laboratory during analysis.
Duplicate surface and well water samples were collected at a rate of 10% of all planned field
samples.
As part of the laboratory analysis, QC procedures included:
Matrix Blank
Field samples that have high concentrations of the target analytes may need to be diluted before
they can be accurately measured in the laboratory. It is therefore necessary to determine that this
diluent (blank matrix) is free of potential contamination. A matrix blank sample was prepared in
the RTF PFC laboratory by filling a pre-cleaned 1 L collection bottle with deionized laboratory
grade water, previously determined to be PFC-free, and adding 5 mL of 35% nitric acid. After
addition of the internal standard mix, this material was analyzed and determined to be free of
potential contaminants before it was used as a diluent for samples that had concentrations of PFOA
that exceeded 1000 ng/L in the preliminary screening analysis.
Solvent Blanks
Solvent blanks containing unprocessed methanol (MEOH) and 2 mM ammonium acetate at a ratio
of 1:3 were analyzed to assure that the primary solvents used in the LC mobile phase were not
contaminated with any of the target PFCs.
Fortified Water Samples
Water samples fortified with target analytes (standard addition) were prepared at a rate of 10% of
all field samples. After successful analysis of the first 500 mL portion of selected 1 L samples, the
remaining portion received a spike of the native standard solution containing all target analytes
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equivalent to 400 ng/L for each of the individual analytes. These samples were prepared to
provide assurance that retention times, quantitiation and qualification ions, and calibration
procedures were consistent between unknown and fortified samples.
Quantitiation and Qualification Ion Ratios
For each target analyte in the field samples, quantitiation and qualification ions were monitored
and compared with the quantitiation and qualification ion ratios observed in the standards used to
construct the standard curves. If the quantitiation/qualification ion ratio of the field samples
differed by more than 2 standard deviations from the standard curve points, the sample was
flagged and examined for potential errors associated with inappropriate peak integration, retention
time, or ion suppression/enhancement. (Sufficient quantities of qualification ions were not
produced for the C4 and C5 acids to allow for this analysis).
Method Deviations
The analytical procedures outlined in SOP # EMAB 114.0 "Improved Method for the Extraction
and Analysis of Perfluorinated Compounds (PFCs) from Surface and Well Water by Ultra-High
Performance Liquid Chromatography (UPLC)-Tandem Mass Spectrometry (MS/MS)" (6) were
followed, with minor changes to improve performance.
Modification to SPE Elution
The original analytical protocol (single elution method) was designed to measure comparatively
low levels (< 50 ng/L) of the target PFCs in surface water. The elution step was tailored to extract
low levels of the target compounds from the SPE cartridge without removing other compounds
that interfere with target ion ionization. Because this application of the analytical method focused
on comparatively high levels of the PFCs, avoiding low levels of co-eluting interferences was not
a substantial concern in this case and after an initial analysis of the extracts, it was observed that
ion counts for the internal standards and native standards for some of the samples were lower than
expected, possibly adversely impacting the precision and accuracy. It was decided, therefore, to
use a more aggressive extraction procedure to increase signal, thereby improving sample accuracy
and precision. Operating on the hypothesis that analyte recovery from the SPE cartridge was
lower than expected, each cartridge was re-eluted with an additional 4 mL of elution solvent
described in section 10.4.5 of the analytical SOP. This additional extract was combined with the
initial extract, and the combined total was concentrated to a volume of 3 mL. This combined and
concentrated extract was mixed with buffer and reanalyzed, giving greater ion counts and a
corresponding increase in precision and accuracy.
Sample Batch Size
Samples were prepared and analyzed as a single batch containing all samples, QC samples, and
calibration standards. This served to eliminate batch to batch variability, thereby improving
precision of the analytical process.
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Results
Sample Completeness
As indicated in Table 3, all field samples were collected by Region 4 field personnel and analyzed
by the RTF PFC analytical team. (Note: Fifty samples were scheduled for collection; however, a
total of 51 samples were received from the field. The additional sample was collected in one of the
water transfer bottles. It was also analyzed and reported.) All of the proposed field duplicates,
field blanks, low level field spikes, high level field spikes, and laboratory spikes (n = 5 for each)
were prepared and analyzed as planned.
Standard Curve Back-Prediction
Before the standard curves were applied to the sample data, an analysis was conducted to
determine how well each standard point back-predicted its own theoretical value. Acceptable
back-prediction is within ± 20 % for all but the lowest standard point, where ± 30 % is acceptable.
Given these criteria, the LOQs were determined to be 10 ng/L for each compound except the CIO
and C7 acids, which were assigned LOQs of 50 ng/L. Table 4 summarizes the mean
back-predicted values for all standard curve points used in this analysis. After adjustment of the
LOQ for CIO and C7, the mean back-prediction criteria were satisfied for all calibration points.
The standard curves for each of the target compounds are included in Appendix 2.
Quality Control Samples
Table 5 contains a summary of the results from the field blank and spike samples. All of the field
blank samples had concentrations of all of the target compounds that were less than the LOQ. The
mean accuracy of the low (200 ng/L) and high level (400 ng/L) field spikes was in all cases within
± 25% of the theoretical spiked concentration.
Field Duplicates
The results of the duplicate field samples are presented in Table 6. Of the five duplicate samples
that were collected, three of the samples had analyte concentrations that were near, or below the
LOQ. The duplicate samples with low concentrations near, or below, the LOQs were in good
agreement. Samples W36SW and W36SW Dup, for which most of the target analytes were in the
measureable range, had relative percent difference values in most cases of < 20%. Duplicate
values for PFOS in this duplicate set had a relative difference of 42%, but the concentrations were
at the lowest portion of the calibration curve.
Fortified Water Sample (Standard Addition)
To help evaluate the response of the analytical assay at the midrange of the calibration curves,
standard addition was performed on five selected field samples. After the initial analyses were
performed, 40 jiL of a mixed standard solution containing all of the native standards at 5 ng/|iL
was added to the remaining portion of each sample (500 mL) in order to provide an additional 400
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ng/L of each analyte to the samples. The samples were then reanalyzed to determine the response
due to the addition of 400 ng/L of each analyte.
As summarized in Table 7, the average % recovery of standard addition at this level was within ±
12 % of the theoretical value for all compounds except CIO and PFOS, which showed 188% and
157% recovery, respectively. With the exception of the CIO and the PFOS, the results indicate
good general performance of the assay at the 400 ng/L level, providing additional evidence of the
accuracy of the analytical procedures. The reason for the higher than expected recoveries for CIO
and PFOS has not been conclusively determined. However, considering the good performance of
CIO and PFOS in the field spike tests, it appears that some other process influenced the results of
this specific analysis. In reviewing the data from this set of standard addition samples, it was noted
that the internal standards for PFOS and CIO had approximately 50% of their response recorded in
the original analysis. This diminished recovery could explain the apparently elevated recoveries
for these target compounds in this part of the evaluation. It should be noted that the higher
recovery noted in these analyses, which would contribute to a positive bias for these compounds,
suggests that the concentrations of the CIO and PFOS compounds reported for the field samples
may be somewhat higher their actual "true" concentration. However, PFOS was not measured
above 200 ng/L in any of the field samples and CIO was measureable above the LOQ in only six
of the 51 samples.
Field Samples
Table 8 summarizes all of the data from the field samples. Samples W01PW, Wl 1PW, W22PW,
W54PW, W62PW, and W14PW were identified by Region 4 personnel as samples from wells
used for drinking water (indicated in Table 8). Of the 51 unique field samples collected (duplicates
excluded), PFOA was detected in 29 (57%) of the samples. The PFOA concentrations ranged
from < LOQ to a high of 11,000 ng/L, with 11 samples out of 51 (22%) above 400 ng/L and two
samples had concentrations (389 ng/L and 397 ng/L), which are not significantly different from
the 400 ng/L Provisional Health Advisory level. PFOA occurred in two drinking water samples:
W54PW at 2,070 ng/L and WP14PW at 594 ng/L. PFOS was measured in 15 samples (29%) at
concentrations ranging from < LOQ to a high of 151 ng/L; all PFOS concentrations were below
the 200 ng/L Provisional Health Advisory level. PFOS was measured in two drinking water
samples: Wl 1PW at 12.0 ng/L and W14PW at 14.1 ng/L. Of the 51 samples, 42 (82%) had at least
one target compound at concentrations above the LOQ. Five of the target compounds were
measured in more than half of the samples, with C4 in 39 samples (77%), both C6 and PFOA in
29 (57%), PFBS in 27 (53%), and C5 in 26 (51%). The C9 acid was detected in 10 (20%) samples
with the highest concentration being 286 ng/L. The CIO acid was detected in 6 (12%) samples
with a high value of 838 ng/L. Neither compound was measured in the drinking water samples.
It should be noted again that this method was optimized for performance in the 200 ng/L to 400
ng/L range to allow for accurate comparison with the Provisional Health Advisories for PFOS and
PFOA. Concentrations of PFCs in samples listed as being below the LOQ have not been reported,
but should not be assumed to be zero.
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Chromatographic Profiles
As an indicator of chromatographic conditions and instrument response, Appendix 3 contains
examples of mass spectral data from three blank samples, three spiked samples, and three field
samples. The first three chromatograms are from field blank samples which contain only
mass-labeled internal standards. The following three examples are field samples which have
received the mass-labeled internal standards and standard addition of 400 ng/L of each of the
target analytes. The final three chromatograms are field samples which have received only
mass-labeled internal standards.
Discussion
Results of field blanks, field spikes, field duplicates, standard curve back-prediction, and standard
addition indicate that the methods used in this assessment generally provide data of acceptable
precision and accuracy. As shown in Table 8, PFOA was measured at concentrations exceeding
388 ng/L in 13 of the 51 samples. PFOS was not measured at concentrations exceeding 200 ng/L
in any of the samples. All 10 target compounds were measurable above the LOQ in one or more
samples. Nine of the samples contained none of the target compounds at concentrations above the
LOQ.
References
(1) Provisional Health Advisories for Perfluorooctanoic Acid (PFOA) and Perfluorooctane
Sulfonate (PFOS), USEPA Office of Water, January 8, 2009.
(2) Analytical Data Report: Perfluorinated Compounds in Water Samples Collected from Public
Water Supplies Near Decatur, Alabama. National Exposure Research Laboratory, Office of
Research and Development, USEPA, November 25, 2008.
(3) Quality Assurance Project Plan "Land Application Site Near Decatur, Alabama - Private Wells
Perfluorinated Compounds Study," Science and Ecosystem Support Division, USEPA Region 4,
February 11,2009.
(4) Standard Operating Procedure EMAB-113-0. "Sample Collection Protocol for PFCs in Surface
and Well Water," Human Exposure and Atmospheric Sciences Division, National Exposure
Research Laboratory, Office of Research and Development, USEPA, February 12, 2009.
(5) Quality Assurance Project Plan "The Analysis of Screening Surface and Well Water Samples
for Selected Perfluorinated Compounds from Decatur, Alabama," Human Exposure and
Atmospheric Sciences Division, National Exposure Research Laboratory, Office of Research and
Development, USEPA, March 13, 2009.
(6) Standard Operating Procedure EMAB 114.0 "Improved Method for the Extraction and
Analysis of Perfluorinated Compounds (PFCs) from Surface and Well Water by Ultra-High
Performance Liquid Chromatography (UPLC)-Tandem Mass Spectrometry (MS/MS)," Human
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Exposure and Atmospheric Sciences Division, National Exposure Research Laboratory, Office of
Research and Development, USEPA, March 13, 2009.
(7) S. Nakayama, M. Strynar, L. Helfant, P. Egeghy, X.Ye, and A.B. Lindstrom, (2007)
Perfluorinated Compounds in the Cape Fear Drainage Basin in North Carolina. Environmental
Science and Technology, 41(16):5271-5276.
(8) EPA's Occupational and Residential Exposure Test Guidelines: OPPTS 875.2000 - Part B -
Chapter 1; Background - General Provisions Guideline, USEPA, Office of Prevention, Pesticides
and Toxic Substances, 1998. This document is available at
http://www.epa.gov/scipoly/sap/1998/march/chapb-l.pdf
List of Tables
Table 1. Perfluorinated analytes, abbreviations, internal standards, LC/MS/MS transitions,
confirmation ions, and ion ratios monitored
Table 2. Summary of the LC/MS/MS method including target and qualifier ions
Table 3. Proposed, Collected, and Analyzed Samples Summarizing Completeness
Table 4. Mean Back-Predicted Values for all Standard Curve Points
Table 5. Summary of Field Blanks, Low Level Field Spikes, and High Level Field Spikes in ng/L
Table 6. Summary of Duplicate Field Samples in ng/L
Table 7. Standard Addition of 400 ng/L of Each Analyte to Selected Field Samples
Table 8. Perfluorinated Compound Concentrations in Surface and Well Water Samples in ng/L
List of Appendices
Appendix 1. Chain of custody forms (CoC) for water samples collected, shipped and received by
the analytical laboratory.
Appendix 2. Calibration curves for all target analytes X's correspond to standard points, O's
correspond to quality controls samples at either 200 or 400 ng/L
Appendix 3. Mass spectral data from 3 blank samples, 3 spiked samples, and 3 field samples.
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Table 1. Perfluorinated analytes, abbreviations, internal standards, LC/MS/MS transitions,
confirmation ions, and ion ratios monitored in analysis
Target Analyte
Perfluorobutanoic acid (C4)
Perfluoropentanoic acid (C5)
Perfluorohexanoic acid (C6)
Perfluoroheptanoic acid (C7)
Perfluorooctanoic acid (C8)
Perfluorononanoic acid (C9)
Perfluorodecanoic acid (CIO)
Perfluorobutane sulfonate (PFBS)
Perfluorohexane sulfonate (PFHS)
Perfluorooctane sulfonate (PFOS)
1,2-13C2- Perfluorohexanoic acid (13C2-C6)
18O2-Sodium perfluorohexanesulfonate (18O2-PFHS)
l,2,3,4,5,6,7,8-13C2-Perfluorooctanoic (13C8-C8)
18O2-Ammonium perfluorooctanesulfonate (18O2-PFOS)
13C2Perfluoroundecanoic acid (13C2-C11)
Quantitation
transition
212.80^168.75
262.85^218.75
312.70^268.70
362.65^318.70
412.60^368.65
462.60^418.60
512.60^468.55
298.70 -> 98.80
398.65 -> 98.80
498.65 -> 98.80
314.75^269.75
402.65^83.90
429.65^375.75
502.60^83.90
564.60^519.65
Confirmation
transition
*NA
NA
312.70^118.70
362.65 -> 168.65
412.60 -> 168.70
462.60^218.75
512.60^468.55
298.70 -> 79.90
398.65^79.90
498.65 -> 79.90
IS
13C2-C6
13C8-C8
13C2-C11
18O2-PFHS
18O2-PFOS
fion ratio
(mean)
NA
16.26
4.81
3.63
3.89
6.31
0.62
1.15
0.62
ion ratio
(SD)
NA
2.05
0.23
0.26
0.27
0.50
0.04
0.10
0.03
LOQ
(ng/L)
10
10
10
50
10
10
50
10
10
10
{Internal Standards (IS)
* Mass spectrometer conditions did not produce secondary qualification ions that can be used for compound confirmation
f Ratio of quantisation ion to confirmation ion, used to help confirm the identity of target compounds
{ Parameters not used with internal standards
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Table 2. Summary of the LC/MS/MS method including target and qualifier ions
Reservoirs: A: 2 mM ammonium acetate in deionized water with 5% methanol, B: 2 mM ammonium acetate in 100%
methanol
Column: BEH CIS reverse phase, 2.1x50 mm, 1.7 |im particle size
Flow rate: 500 jiL/min
Column temperature: 50°C
Injection Volume: 40 jiL
Gradient mobile phase program:
Time
0.00
0.50
3.50
3.60
4.50
4.60
6.00
A
75
75
10
0
0
75
75
B
25
25
90
100
100
25
25
curve
initial
6
6
6
6
6
6
The Quatro Premier mass spectrometer is operated in the multiple reaction monitoring (MRM) mode using negative-ion-spray
ionization under the following conditions:
Instrument Parameters
Capillary (kV) -0.40
Source temperature 150°C
Desolvation temperature 350°C
Cone gas flow 2 L/hr
Desolvation gas flow 1200 L/hr
Cone voltage Optimized for
Collision energy each compound
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Table 2. (Continued) Compound specific parameters for Quatro Premier XE (MS/MS)
Compound
PFBS
PFHS
PFOS
C4
C5
C6
C7
PFOA or C8
C9
CIO
Internal
Standards
18O2-PFHS
13C2-PFOS
13C2-C6
13C8-PFOA
13C2-C11
Quantitation MRM
298. 70 > 98. 80
398. 65 > 98. 80
498. 65 > 98. 80
212.80 > 168. 75
262.85 > 218. 75
312.70 > 268. 70
362.65 > 318. 70
412.60 > 368. 65
462.60 > 418. 60
512.60 > 468. 55
402.65 > 83.90
502.65 > 83.90
314.75 > 269.75
420.65 > 375. 75
564.60 > 519.65
Qualification
MRM
298.70 > 79.90
398.65 > 79.90
498.65 > 79.90
312.70 > 118.70
362.65 > 168.65
412.60 > 168.70
462.60 > 218.75
512.60 > 218.75
Cone
Voltage
40
50
60
15
15
13
14
15
15
16
50
60
13
15
17
Collision
Energy
28 (30)
32 (38)
38 (48)
10
9
10(21)
10(17)
11(18)
11(17)
12(18)
38
48
9
11
12
Note: Collision energies for qualification ions are in parenthesis
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Table 3. Proposed, Collected, and Analyzed Samples Summarizing Completeness
Sample Type
Field Samples
Field Duplicates
Field Blanks
Low Level Field Spikes
High Level Field Spikes
Laboratory Spikes
Proposed
50
5
5
5
5
5
Collected/prepare
d
51*
5
5
5
5
5
Analyzed
51*
5
5
5
5
5
*One additional sample was collected in a bottle intended for water transfer.
This sample was analyzed and is noted in Table 8 below.
Table 4. Mean Back-Predicted Values for all Standard Curve Points
10 ng/L standard
50 ng/L standard
100 ng/L standard
200 ng/L standard
400 ng/L standard
600 ng/L standard
800 ng/L standard
1000 ng/L standard
CIO
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50.8
100
199
389
574
873
959
C9
9.09
51.0
103
213
410
574
771
1030
PFOA
9.34
52.0
101
208
400
593
784
1010
C7
___
48.9
98.7
210
398
599
786
1010
C6
9.40
52.1
103
199
407
591
788
1010
C5
7.17
63.8
102
215
345
629
797
1000
C4
9.40
52.4
101
202
401
601
779
1010
PFOS
9.51
54.9
92.5
206
408
580
807
1000
PFHS
9.06
55.7
96.1
203
412
594
764
1030
- 13 -
-------
Table 5. Summary of Field Blanks, Low Level Field Spikes, and High Level Field Spikes in ng/L
Sample Type
*Trip Blanks
* Low Level
Trip Spike (SD)
Percent Accuracy
(RSD)
* High Level
Trip Spike (SD)
Percent Accuracy
(RSD)
CIO
<50
210 (17)
105 (8.2)
448 (56.8)
112(12.7)
C9
<10
156 (45)
78.1 (28.8)
301 (59.7)
75.2(19.9)
PFOA
<10
162 (36)
80.9 (22.5)
318(51.1)
79.4(16.1)
C7
<50
171(31)
85.5(18.3)
339 (58.0)
84.7(17.1)
C6
<10
195 (23)
97.3 11.9)
388(29.3)
97.1(7.6)
C5
<10
217(33)
108 (15.4)
393 (41.5)
98.3 (10.6)
C4
<10
218 (60)
109 (27.5)
382 (19.2)
95.4 (5.0)
PFOS
<10
172 (39)
86.1 (22.7)
364 (30.9)
90.9 (8.5)
PFHS
<10
198(18)
98.9(9.1)
386 (26.5)
96.6 (6.9)
PFBS
<10
205 (22)
103 (10.6)
387 (24.2)
96.8 (6.2)
* Mean of 5 determinations; Low Level Field Spikes prepared at 200 ng/L; High Level Field Spikes prepared at 400 ng/L
- 14-
-------
Table 6. Summary of Duplicate Field Samples in ng/L
W06PW
W06PW dup
Rel % Diff
W53SW
W53SWdup
Rel % Diff
W24SW
W24SW dup
Rel % Diff
W36SW
W36SW dup
Rel % Diff
W17PW
WlTPWdup
Rel % Diff
CIO
-------
Table 7. Standard Addition (SAT) of 400 ng/L of Each Analyte to Selected Field Samples (ng/L)
W06PW-SAT
W63PW-SA1
W02PW-SA1
W13SW-SAT
W34SW-SAT
W06PW
W63PW
W02PW
W13SW
W34SW
(W06PW-SA1) - (W06PW)
(W63PW-SAT> (W63PW)
(W02PW-SAT)- (W02PW)
(W13SW-SA1)- (W13SW)
(W34SW-SA1)- (W34SW)
% recovery
Ave % Recovery
SD % Recovery
CIO
614
677
1029
628
805
*
*
*
*
*
614
677
1029
628
805
153
169
257
157
201
188
43.2
C9
433
412
301
403
318
*
*
*
27.7
16.2
433
412
301
375
302
108
103
75
94
76
91.1
15.4
PFOA
477
471
339
653
559
*
*
*
321
204
477
471
339
332
355
119
118
85
83
89
98.8
18.2
C7
460
489
347
731
512
*
*
*
234
73.6
460
489
347
498
439
115
122
87
124
110
112
15.1
C6
386
405
392
515
451
*
*
*
182
103
385
405
392
333
348
96
101
98
83
87
93.2
7.7
C5
369
427
459
480
520
*
*
*
76.4
162
369
427
459
403
358
92
107
115
101
90
101
10.3
C4
393
412
444
426
558
*
*
*
62.5
234
393
412
444
364
324
98
103
111
91
81
96.9
11.5
PFOS
551
646
688
595
663
*
*
*
*
*
551
646
688
595
663
138
161
172
149
166
157
13.8
PFHS
450
485
420
422
396
*
*
*
*
*
450
485
420
422
396
113
121
105
105
99
109
8.5
PFBS
420
504
401
450
426
*
*
*
13.4
*
420
504
401
437
426
105
126
100
109
107
109
9.8
SA1' = Sample received laboratory spike equivalent to 400 ng/L of each compound
* Values below the limit of quantitation, assumed to be 0 for the calculation of difference
- 16-
-------
Table 8. Perfluorinated Compound Concentrations in Surface and Well Water Samples in ng/L
Sample Name
W06PW
W06PW dup
W51SW
W27SW
W10SW
W28SW
PWHPW
W46SW
W42SW
W43SW
W32SW
W53SW
W53SWdup
|W03SW
W33SW
W63PW
W07PW
W101PW
W61SW
W52SW
W58PW
W09PW
W24SW
W24SW dup
W102SW
W02PW
W64SW
|3W54PW
W15PW
PW62PW
PW22PW
PW1 1PW
W60PW
W36SW
W36SW dup
W12PW
W29SW
W31SW
W30SW
W08PW
W35SW
CIO
*
*
*
*
*
*
*
838
*125
68.0
230
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
54.2
*
*
*
*
*
*
*
C9
*
*
*
*
*
*
25.7
286
93.3
54.4
70.9
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*12.4
21.8
*
*
*
*
*
*
PFOA
*
*
29.5
134
13.6
94.8
594
1100
993
396
750
18.3
14.8
*
*
*
*
*
*
2230
*
*
*
33.7
*
*
758
2070
*
*
*
*
149
389
397
6410
*
30.1
24.1
*
*
C7
*
*
*
81.5
*
127
619
491
777
216
839
*
*
*
*
*
*
*
*
3180
*
*
*
*
*
*
1200
2100
*
*
*
*
77.2
393
407
5220
*
*
*
*
*
C6
*
*
12.0
65.9
20.2
153
570
205
729
201
961
*
*
*
*
*
9.72
*
*
3750
*
*
22.1
18.7
*
*
1730
2150
*15.8
*
*
*
150
505
511
3970
*
*
13.7
*
*
C5
*
*
*
68.4
20.8
91.1
333
192
434
180
571
*
*
*
*
*
*
*
*
1970
*
*
56.6
72.0
*
*
1060
1180
12.2
*
*
*
57.2
333
369
2330
*
*
*
*
*
C4
*
*
*
72.7
52.7
70.8
180
188
303
152
439
*
*
19.4
30.4
*
45.8
14.6
*
1030
*
10.4
62.6
77.9
*
*
825
680
42.6
*
*
34.6
98.1
236
274
1260
*
44.6
40.0
*
14.4
PFOS
*
*
*
:11.6
*
*
:14.1
83.9
*16.5
h4.6
:66.3
51.1
56.1
13.2
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
12.0
151
*30.3
19.8
*
^1.1
31.7
31.5
*
*
PFHS
*
*
*
*
*
*
20.7
*
17.5
*
20.6
*
*
*
*
*
*
*
*
12.1
*
*
*
*
*
*
12.3
46.4
*
*
*
12.7
56.5
16.7
17.7
87.5
*
*
*
*
*
PFBS
*
*
*
*
30.9
15.6
25.4
10.4
40.8
10.0
90.2
*
*
ho.9
23.9
*
*
22.9
*
91.3
*
*
*
*
*
*
56.7
56.5
*
*
*
26.4
33.9
38.2
41.2
76.6
14.8
26.0
13.5
*
9.51
- 17-
-------
Sample Name
^WOIPW
W48SW
W13SW
W34SW
W26SW
W17PW
WlTPWdup
W57SW
W47SW
W50SW
W44SW
W45SW
W41SW
W49SW
W19PW
CIO
*
*
*
*
*
*
*
*
*
*
*
129
*
*
*
C9
*
*
27.7
16.2
*
*
*
*
*
40.0
*
26.4
*
*
*
PFOA
*
26.0
321
204
67.9
*
*
32.2
1250
1160
11000
176
90.5
35.7
*
C7
*
*
234
73.6
30.0
*
*
*
1360
715
8250
61.0
*
*
*
C6
*
16.4
182
103
141
*
*
*
1310
762
6710
69.4
50.6
42.3
*
C5
*
17.2
76.4
162
305
*
*
*
478
354
3770
143
90.7
28.3
*
C4
24.1
33.0
62.5
234
394
13.2
13.8
10.7
330
199
1750
194
102
29.4
11.6
PFOS
*
*
*
*
*
*
*
*
*
*
*
38.2
*
*
*
PFHS
*
*
*
*
*
*
*
*
40.6
*
218
*
*
*
*
PFBS
:10.1
*
13.4
*
:11.2
*
*
*
63.9
54.5
208
*
*
*
*
* Values below the limit of quantitation (LOQ) - cannot be assumed to be zero.
J Values flagged for having confirmatory/quantification ion ratios more than 2 standard deviations
away from mean values determined for standards
t W03SW sample collected in a container intended for water transfer only
P indicates sample from a well used for drinking water
dup indicates duplicate sample
- 18-
-------
Appendix 1.
Chain of custody forms (CoC) for water samples collected, shipped and received by the analytical laboratory
- 19-
-------
USEPA Contract Laboratory Program /7/: >"7 / /- /
\f Generic Chain of Custody U? ' / /l/L
Region: 4
Project Code: fteuv»7
Account Code: 09-0227
CERCLIS ID:
Spill ID:
Site Name/state: LAS Near Decatur AL Private Well PFC
Project Leader: Mike Neill
Action:
Sampling Co: PL-SESD
MATRIX/ CONCS ANALYSIS/
SAMPLE No SAMPLER TYPE TURNAROUND
W01-PW Groundwater/ L/G PFCs (0)
Kevin Simmons
W02-PW Groundwater/ L/G PFCs(O)
Kevin Simmons
W06-PW Groundwater/ L/G PFCs(O)
Marty Allen
W06-PW-DU Groundwater/ L/G PFCs(O)
P Marty Allen
W07-PW Groundwater/ UG PFCs(O)
Kevin Simmons
W08-PW Groundwater/ L/G PFCs(O)
Art Masters
W09-PW Groundwater/ L/G PFCs (0)
Art Masters
W101-PW Groundwater/ L/G PFCs(O)
Kevin Simmons
W102-SW Surface Water/ L/G PFCs(O)
Kevin Simmons
W10-SW Surface Water/ L/G PFCs (0)
Marty Allen
W11-PW Groundwater/ L/G PFCs(O)
Kevin Simmons
Date Shipped:
Carrier Name:
Airbill:
Shipped to:
2/19/2009 Chain
865935737060 R8"nc"
NERL RTP 1
1 09 TW Alexander Dr
Building E, Room E-1 78 2
purnam No z/711
(919) 541-3706 3
4.
TAG No./ STATION
PRESERVATIVE/ Bottles LOCATION
1(HN03)(1)
2(HN03)(1)
4(HNO3)(1)
5(HN03)(1)
6 (HNO3) (1)
7 (HNO3) (1)
8 (HN03) (1)
10(HNO3)(1)
11 (HNO3)(1)
9 (HN03) (1)
12(HNO3)(1)
W01-PW
W02-PW
W06-PW
W06-PW-DUP
W07-PW
W08-PW
W09-PW
W101-PW
W102-SW
W10-SW
W11-PW
Reference Case: D
Client No:
Of Custody Record Sampler
Signature:
jished By (Data / Time) Received By (Date / Time)
C-^ ^^^^^^^/^ //
/ / I /
SAMPLE COLLECT QC
DATE/TIME Type
S: 2/19/2009 13:12
S: 2/18/2009 10:48
S: 2/17/2009 17:00
S: 2/17/2009 17:00
S: 2/19/2009 13:44
S: 2/18/2009 9:05
S: 2/19/2009 11:49
S: 2/18/2009 14:05
S: 2/18/2009 14:23
S: 2/18/2009 9:35
S: 2/17/2009 15:57
Shipment for Case
Complete? Y
Analysis Key:
Sample(s) to b« used for laboratory QC:
AddTObnalJIamplar Slgnature(sj: / / //
scx^. Tfafrt^ 6^W
Concentration: L = Low, M = Low/Medium, H = High Type/Designate: Composite = C, Grab = G
Chain of Custody Seal Number:
Shipment Iced?
HP us - PertiuorinaterJ uompounds
TR Number: 4-043013577-021909-0001
PR provides preliminary results. Requests for preliminary results will increase analytical costs.
Send Copy to: Sample Management Office, Attn: Heather Bauer, CSC, 15000 Conference Center Dr., Chantilly, VA 20151-3819; Phone 703/818-4200; Fax
TAO/O'IO
F2V5.1.047 Page 1 of 6
-------
USEPA Contract Laboratory Program
\f Generic Chain of Custody
Region: 4
Project Code: nO-fm
Account Code: 09-0227
CERCLIS ID:
Spill ID:
Site name/State: LAS Near Decatur AL Private Well PFC
Projsct Leader: Mike Ne'j||
Action:
Sampling Co: PL-SESD
MATRIX/ CONC/ ANALYSIS/
SAMPLE NO SAMPLER TYPE TURNAROUND
W12-PW Groundwater/ L/G PFCs (0)
Art Masters
W13-SW Surface Water/ L/G PFCs(O)
Art Masters
W14-PW Groundwater/ L/G PFCs (0)
Marty Allen
W15-PW Groundwater/ L/G PFCs(O)
Kevin Simmons
W17-PW Groundwater/ L/G PFCs(O)
Marty Allen
W17-PW-DU Groundwater/ L/G PFCs(O)
P Marty Allen
W19-PW Groundwater/ L/G PFCs(O)
Marty Allen
Date shipped: 2/19/2009 Chair
Carrier Name: FedEx
Airbill: 865935737060 Relinq
Shipped to: NERLRTP 1
109TW Alexander Dr
Building E, Room E-178 2
(919) 541-3706 3
4.
TAG NoJ STATION
PRESERVATIVE/ Bottles LOCATION
1 3 (HNO3) (1 ) W1 2-PW
14(HN03)(1) W13-SW
15(HNO3)(1) W14-PW
Reference Case: D
Client No: *
Of Custody Record Sampler
Signature:
jished By (Date / Time) Received By , (Date / Time)
/ ' ' ''/?// <'.-' '' /".-*"}
/ /
SAMPLE COLLECT QC
DATE/TIME Type
S: 2/18/2009 11:50
S: 2/18/2009 11:20
S: 2/18/2009 14:15
16(HN03)(1) W15-PW 5:2/17/2009 16:38
17(HNO3)(1) W17-PW 3:2/19/2009 11:16
18(HNO3){1) W17-PW-DUP 3:2/19/2009 11:16
19(HNO3)(1) W19-PW 3:2/19/2009 13:10
W22-PW Groundwater/ L/G PFCs(O) 20(HNO3)(1) W22-PW 3:2/18/2009 10:00
Kevin Simmons
W24-SW Surface Water/ L/G PFCs (0) 21(HN03)(1) W24-SW 3:2/19/2009 9:05
Kevin Simmons
W24-SW-DU Surface Water/ L/G PFCs (0) 22(HNO3)(1) W24-SW-DUP 8:2/19/2009 9:05
3 Kevin Simmons
W26-SW Surface Water/ L/G PFCs (0) 23(HNO3)(1) W26-SW 3:2/18/2009 14:00
Art Masters
Shipment (or Case
Complete? Y
Analysis Kay:
Sample(s) to b« used for laboratory QC:
Additional Sampler Slgnatureja): / ' tfjflf //
i J ' //, , y/jf '«trfcs'
K' , "-- ___ * f ^ ' f
t,,, ^^^^ /-,^ -.- t
Concentration: L = Low, M = Low/Medium, H = High Type/Designate: Composite = 0 Crab = C
Chain of Custody Seal Number:
Shipment Iced?
PFCs = Perfluorinated Compounds
TR Number: 4-043013577-021909-0001
PR provides preliminary results. Requesta for preliminary results will increase analytical costs.
Send Copy to: Sample Management Office, Attn: Heather Bauer, CSC, 15000 Conference Center Dr., Chantilly, VA 20151-3819; Phone 703/818-4200; Fax
F2V5.1.047 Page 2 of 6
-------
tSi USEPA Contract Laboratory Program
W Generic Chain of Custody
Region: 4
ft**** og_Q227
Account Code: 09-0227
CERCLIS ID:
Spill ID:
Site Name/state: tAS Near Decatur AL Private Well RFC
Project Leader: Mike Neill
Action:
Sampling Co: PL-SESD
MATRIX/ CONC/ ANALYSIS/
SAMPLE NO. SAMPLER TYPE TURNAROUND
Marty Allen
W28-SW Surface Water/ L/G PFCs (0)
Marty Allen
W29-SW Surface Water/ L/G PFCs (0)
Art Masters
W30-SW Surface Water/ L/G PFCs(O)
Art Masters
W31-SW Surface Water/ UG PFCs (0)
Art Masters
W32-SW Surface Water/ L/G PFCs (0)
Marty Allen
W33-SW Surface Water/ L/G PFCs(O)
Art Masters
W34-SW Surface Water/ L/G PFCs (0)
Art Masters
Date Shipped: 2/19/2009 Chain of Custody R
Carrier Name: FedEx
Airbill: 865935737060 Relinquished By
Shipped to: NERL RTP 1
Building E, Room E-178 2
Durham Mf* 0771 1 _ -
(919) 541-3706 3.
4,
Reference Case: O
Client No: * ^
ecord Sampler
Signature:
(Date / Time) Received By (Date / Time)
' * ,'' ' ./.-. 'S;
/
TAG No J STATION SAMPLE COLLECT QC
PRESERVATIVE/ Bottles LOCATION DATE/TIME Type
24 (HN03) (1) W27-SW S: 2/19/2009
25(HNO3)<1) W28-SW 5:2/18/2009
26(HN03)(1) W29-SW 8:2/17/2009
27(HNO3)(1) W30-SW 8:2/17/2009
28(HN03)(1) W31-SW 3:2/17/2009
29 (HNO3) (1) W32-SW S: 2/17/2009
30(HNO3)(1) W33-SW 8:2/18/2009
31 (HNO3) (1) W34-SW S: 2/18/2009
W35-SW Surface Water/ L/G PFCs (0) 32 (HNO3) (1) W35-SW 3:2/18/2009
Art Masters
W36-SW Surface Water/ L/G PFCs (0) 33{HNO3)(1) W36-SW 8:2/18/2009
Art Masters
W36-SW-DU Surface Water/ L/G PFCs (0) 34{HNO3)(1) W36-SW-DUP 5:2/18/2009
P Art Masters
13:15
10:05
15:54
16:35
16:11
15:55
14:55
10:05
9:20
9:35
9:35
Shipment for Case
Complete? Y
Analysis Key:
Sample(s) to be used for laboratory QC:
Additional Sam pier Sigrtature(s): f 1 n
V^^ - . - - /W#C-r^
^ ^^-' ^^:^^
Concentration: L » Low, M = Low/Medium, H = High Type/Designate: Composite = C, Grab = G
Chain of Custody Seal Number:
Shipment teed?
PFCs = Perfluorinated Compounds ' ' ! ' -
4-043013577-021909-0001
PR provides preliminary results. Reqyests for preliminary results will Increase analytical costs.
Send Copy to: Sample Management Office, Attn: Heather Bauer, CSC, 15000 Conference Center Dr., Chantilly, VA 20151-3819; Phone 703/818-4200; Fax
F2V8.1.M7 Page 3 of 8
-------
& USEPA Contract Laboratory Program
\f Generic Chain of Custody
Project Code:
Account Code: 09-0227
CERCLIS ID:
Split ID:
Site Name/state: LAS Near Decatur AL Private Well PFC
Project Leader: Mike Netll
Action:
Sampling Co: PL-SESD
MATRIX/ CONC/ ANALYSIS/
SAMPLE No. SAMPLER TYPE TURNAROUND
Marty Allen
W42-SW Surface Water/ UG PFCs(O)
Marty Alten
W43-SW Surface Water/ UG PFCs(O)
Marty Allen
W44-SW Surface Water/ L/G PFCs{0)
Marty Allen
W45-SW Surface Water/ UG PFCs(O)
Marty Alien
Dute Shipped: 2/19/2009 Cham of Custody R
Carrier Name: FedEx
Airbill: 865935737060 Ralinqu.stwd By
Shipped to: NERL RTP 1
Building E, Room E-1 78 2
Durham WP 97711
(919) 541-3706 3.
4
Reference Case: D
Client No: * *
ecord Sampler
Signature:
(Date / Time) Received By ^ (Date /Time)
^ /? j '/" /^ s* ? / '
TAG No./ STATION SAMPLE COLLECT QC
PRESERVATIVE/ Bottles LOCATION DATE/TIME Type
35(HNO3)(1) W41-SW 8:2/18/2009
36(HNO3)(1) W42-SW 8:2/18/2009
37(HN03)(1) W43-SW 8:2/18/2009
38(HNO3)(1) W44-SW 8:2/18/2009
39(HN03)(1) W45-SW 8:2/18/2009
W46-SW Surface Water/ UG PFCs(O) 40(HNO3)(1) W46-SW 3:2/18/2009
Marty Allen
I/V47-SW Surface Water/ UG PFCs(O) 41(HNO3){1) W47-SW 8:2/18/2009
Marty Allen
W48-SW Surface Water/ UG PFCs(O) 42(HNO3)(1) W48-SW 8:2/18/2009
Art Masters
W49-SW Surface Water/ UG PFCs(O) 43{HNO3)(1) W49-SW S' 2/19/2009
Marty Allen
W50-SW Surface Water/ UG PFCs(O) 44(HN03)(1) W50-SW S' 2/19/2009
Marty Alten
/V51-SW Surface Water/ UG PFCs(O) R4-56(HNO3)(1) W51-SW 8:2/19/2009
Marty Allen
11:25
11:35
11:10
14:35
13:35
13:20
12:55
10:50
14:25
14:50
15:15
Complete? Y
Analysis Key:
Sample(s) to b« used for laboratory QC:
Additional Sampler Slgnaturefs): / / ^flff /L^-~
Concentration: L = Low, M = Low/Medium, H = High Type/Designate: Composite = C,' Grab = G
PFCs =* Perfluorinated Cyiiipouiius - '
Chain of Custody Seal Numtaer:
Shipment teed?
TR Number: 4-04301 3677-021 909-0001
PR provides preliminary results. Requests for preliminary results will Increase analytical costs.
Send Copy to: Sample Management Office, Attn: Heather Bauer, CSC, 15000 Conference Center Dr., Chantilly, VA 20151-3819; Phone 703/818-4200- Fax
"TnO/CMO ^ICAI
F2VS.1.047 Page 4 of 6
-------
USEPA Contract Laboratory Program
Generic Chain of Custody
Region: 4
***** <)M227
Account Code: 09-0227
CERCLIS ID:
Spill 10:
Site Name/state: LAS Near Decalur AL Private Well RFC
Protect Loator. Mike Ne ill
Action:
Sampling Co: PL-SESD
MATRIX/ CONC/ ANALYSIS/
SAMPLE NO. SAMPLER TYPE TURNAROUND
Art Masters
W53-SW Surface Water/ UG PFCs(O)
Art Masters
W53-SW-DU Surface Water/ UG PFCs(O)
P Art Masters
Date Shipped:
Canter Mama:
Airbill:
Shipped to:
2/19/2009 Chain
FedEx
865935737060 R*"nq
NERL RTP 1
Buifdircg E, Room E-178 2
ntirham MP 977-11 -
(919)541-3706 3.
4.
TAG No./ STATION
PRESERVATIVE/ Botttes LOCATION
46(HNO3)(1)
47(HN03)(1)
W54-PW Groundwater/ UG PFCs(O) 48(HNO3)(1)
Kevin Simmons
W57-SW Surface Water/ UG PFCs (0) 49(HNO3)(1)
Marty Allen
W58-PW Groundwater/ L/G PFCs(O) 50(HNO3)(1)
Art Masters
W60-PW Groundwater/ L/G PFCs(O) 51(HNO3)(1)
Kevin Simmons
W61-SW Surface Water/ L/G PFCs(O) 52(HNO3)(1)
Art Masters
W62-PW Groundwater/ L/G PFCs(O) 53(HNO3)(1)
Kevin Simmons
I/V63-PW Groundwater/ L/G PFCs(O) 54(HNO3)(1)
Kevin Simmons
iA/64-SW Surface Water/ L/G PFCs (0) 55(HNO3)(1)
Kevin Simmons
W52-SW
Reference Case: O
Client No: * ^
Of Custody Record Sampler
Signature;
jlshedBy (Date (Time) Received By (Oate/Ttme)
'- ,
SAMPLE COLLECT QC
DATE/TIME Type
S: 2/18/2009 14:15
W53-SW S: 2/19/2009 10:25
W53-SW-DUP S: 2/19/2009 10:25
W54-PW S: 2/18/2009 9:25
W57-SW S: 2/19/2009 9:55
W58-PW S: 2/19/2009 10:45
W60-PW S: 2/17/2009 17:25
W61-SW S: 2/19/2009 13:30
W62-PW S: 2/18/2009 15:16
W63-PW S: 2/19/2009 11:10
W64-SW S: 2/19/2009 10:10
Complete? Y
An a ty sis Kay;
Sample(s) to be ussd for laboratory QC:
AdditkJIUiLgampler Si9nature(a}: / / j\A
': y" ^~~~- ' . i _^f**~*~/ I y\ ^e**^**
\'~~^* "" v f*'^\^j-^/ ^"^^r
Concentration: i = tow. M = Low/Medium. H = High Typa/Deslgnata: Composite = C. Grab = G
PFCs - Peifluuimaled Compounds ' -_ »^__ ,
Chain of Custody Seal Number:
Shipment lead?
TR Number: 4-043013577-021909-0001
PR provides preliminary results. Requests for preliminary results will Increase analytical coats.
Send Copy to: Sample Management Office, Attn: Heather Bauer, CSC, 15000 Conference Center Dr., Chantilly, VA 20151-3819; Phone 703/818-4200; Fax
FZV5.1.047 Page 5 of 6
-------
&EPA
Region:
Profact Code:
Account Code:
CERCLIS ID:
Spill ID:
Site Nime/Sfata:
Project Leaden
Action:
Sampling Co:
SAMPLE No.
USEPA Contract Laboratory Program
Generic Chain of Custody
4
09-0227
09-0227
LAS Near Decatur AL Private Well PFC
Mike Ne'ill
PL-SESD
Date Shipped:
Canter Name:
Airbill:
Shipped to:
Reference Case: D
Client No: ' ^
2/1 9/2009
FedEx
865935737060
NERL RTP
109TW Alexander Or
Building E, Room E-178
Durham NC 2771 1
(919) 541-3706
Chain of Custody Record
Relinquished By (Date / Urns)
1
2.
3.
4,
Samplar
Signature:
Received By (Date / Time)
* ' . /
' f !
/
MATRIX; CONG; ANALYSE TAGNOJ STATION SAMPLE COLLECT QC
SAMPLER TYPE TURNAROUND PRESERVATIVE; Bottles LOCATION DATE/TIME Type
Kevin Simmons
W03-SW S: 2/19/2009 14:00
Complete? ₯
Analysis Key:
Sample(s) to be uisd for laboratory QC:
AdditioaaLSajnplerSlgnature(a}: / ) 7. M
\^3\ ^^ ^ M^f(^=^
Concentration: L * Low, M = Low/Medium, H » High Type/Designate: Composrte - C, Grab = G '
Chain of CysttKiy SssS Nuni^r:
Shipment Iced?
PFCs - PerfluGiiitaled Compounds ' "~ ~~~ rrr"n" ' ' ; ___ _____
PR provides preliminary results. Raqurets tor preliminary resyfte will increass analytical costs.
Send Copy to: Sample Management Office, Attn: Heather Bauer, CSC, 15000 Conference Center Dr., Chantilly, VA 20151-3819: Phone 703/818-4200- Fax
"WVJWM 0 XCA*>
F2V5.1.M7 Page 6 of 6
-------
Appendix 2.
Calibration curves for all target analytes
X's correspond to standard points, O's correspond to Quality Control samples at the 200 or 400 ng/L levels
-20-
-------
.BOH
,r
50 100 150 200
300
350
400
450
500
r
550
600
650
700
800
850
900
950
-, ng/|
1000
-------
1 .70-;
1.60-
1 .50-i
1.40-i
1 ,30-j
1.20-i
LID-
1 ,00-i
o.eo
0.50-:
0.40-i
0.30-i
0.20-i
0.1 Oi
0.00
0
50 100 150 200 250 300 350
400
450
500 550 600 650 700 750 800 850 900 950 1000"
ng/l
-------
3.40-:
3.20-!
3.00-i
2.80-:
2.60-;
2.40-i
2.20-:
2.00-!
1.80:
1.60-i
1.40-!
1.20:
1.00^
O.BO-i
0.60-:
0.4 OH
0.20^
0.00J
0
50 100 150 200 ' 250 300
350
400
450
500
550
600
650
TTT^ np
' 700 750 800 850 ' 900 ' 950 1000
-------
5.00-;
4.50:
4.00-
3.50:
ce
0 50 100 150 200 250 300 350
400
450
500 550 600 650 700 750 BOO 850 900 950 1000
-------
2.00:
1.60:
1.40:
1.20:
1.00-
0.80-
0.60-
0.40:
0.20-
0 . D 0'" ~TTTyTTTT«pj*T"^^
0 50 100 150 200 ' 250 300 350 400
450
500
550
BOO
np
650 ' 700 750 800 850 ' 900 ' 950 1000
-------
2.80-
2.6Q-;
2.40-:
2.20-i
2.00^
1 .GO-!
1.60-:
1.40^
1.20-i
1.00-1
O.BO-i
O.BDH
0.40^
0.20-;
0 . D 0 ^^V
0
150 200 ' 250 300 350 400
450
np
500 550 BOO B50 ' 700 750 800 850 ' 900 ' 950 1000
-------
2.60-
2.40-
2.20-
2.00
DC
50
^
100 150 200 ' 250 300 350 400
450
np
500 550 BOO B50 ' 700 750 800 850 ' 900 ' 950 1000
-------
50
100
150
TT~rr?^
200 250 ' 300 350 400
450
500
550
600
650
700
750 800 850 900 950 1000
-------
Compound name: PFHS
Coefficient of Determination: RA2 = 0.997949
Calibration curve: 2.053696-007*^2 + 0.001082B1 * x + 0.00381447
Response type: Internal Std ( Ref 14 ), Area * (IS Cone. / IS Area )
Curve type: 2nd Order, Origin: Exclude, Weighting: 1/x, Axis trans: None
1.30:
1.20-
1.10-:
1.00-
I.70J
Dt
O.BO-i
0.40-
0.30-
0.10-
0 50 100 150 200 250 300 350
400
450
500
550
BOO
B50
700
750
800
850
900
950
i ng/l
1000
-------
50 100 150 200 250 ' 300 350 400
450
500 550 600
^
-------
Appendix 3. Mass spectral data from 3 blank samples, 3 spiked samples, and 3 field samples
-21 -
-------
Trip Blank #1
100n
3.04
PFOS-I.S.
2: MRM of 11 Channels ES-
502.6 > 83.9
3.56e5
0-1
0.60 0.80
032609 #1
100n PFOS
1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80
3.00 3.20
3.04
o
3.40 3.60 3.80 4.00
2: MRM of 11 Channels ES-
498.65 > 98.8
7.90e3
2.322.43
0.60 0.80 1.00
032609 #1
100-
1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60
o
PFOA-I.S.
2.80
2.78
3.00 3.20 3.40
3.60 3.80 4.00
2: MRM of 11 Channels ES-
420.65 > 375.75
9.07e5
0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00
032609 #1 2: MRM of 11 Channels ES-
2.78 412.6 > 368.65
1.99e4
100
PFOA
0
0.60 0.80 1.00 1.20 1.40
032609 #1
100q
Total Ion Chromatograph #3
2.25 2.39 2.572.68 2.92 3.05 3.323.42
o-
1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40
3.41
3.24
3.60 3.80 4.00
3: MRM of 15 Channels ES-
TIC
2.49e5
0.60 0.80 1.00 1.20 1.40
032609 #1
100n
1.60 1.80 2.00 2.20 2.40 2.60 2.80
2.78
o
Total Ion Chromatograph #2
3.00 3.20
3.04
3.40 3.60 3.80 4.00
2: MRM of 11 Channels ES-
TIC
9.37e5
0.60 0.80 1.00 1.20 1.40
032609 #1
1001 Total Ion Chromatograph #1
1.60 1.80
2.00 2.20
2.06
2.40 2.60 2.80 3.00 3.20
2-?2
3.40 3.60 3.80 4.00
1: MRM of 12 Channels ES-
TIC
1.44e6
Time
0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00
-------
Trip Blank #2
100n
3.03
PFOS-I.S.
2: MRM of 11 Channels ES-
502.6 > 83.9
3.37e5
0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00
032609 #15 2: MRM of 11 Channels ES-
3.03 498.65 > 98.8
100n
0
0.60 0.80 1.00
032609 #15
10(h PFOA-I.S.
3.15
2.29
2.49
2.83
3.30
1-3163
1.20 1.40 1.60
1.80 2.00 2.20 2.40 2.60 2.80
2.77
3.00 3.20 3.40
3.60 3.80 4.00
2: MRM of 11 Channels ES-
420.65 > 375.75
1.04e6
0
0.60
032609 #15
100
0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20
2.78
3.40 3.60 3.80 4.00
2: MRM of 11 Channels ES-
412.6 > 368.65
9.16e3
2.37 2.56 2.70
q no
1 1 2.87 | 3.15
3.28
\_Wj
3.46
0
0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00
032609 #15 3: MRM of 15 Channels ES-
3.40 TIC
100n
Total Ion Chromatograph #3
2.08e5
3-54
0.60 0.80 1.00 1.20 1.40
032609 #15
100n
1.60 1.80 2.00 2.20 2.40 2.60 2.80
2.77
Total Ion Chromatograph #2
0
0.60 0.80 1.00 1.20 1.40
032609 #15
1 Total Ion Chromatograph #1
3.00 3.20
3.03
A
3.40 3.60 3.80 4.00
2: MRM of 11 Channels ES-
.04e6
1.60
1.80 2.00 2.20 2.40 2.60 2.80
2.05 2.51
3.00 3.20 3.40 3.60 3.80 4.00
1: MRM of 12 Channels ES-
TIC
1.19e6
Time
0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00
-------
Trip Blank #3
100n
3.03
PFOS-I.S.
2: MRM of 11 Channels ES-
502.6 > 83.9
3.48e5
U i i i i i | i i i i | i i i i | i i i i | i i i i | i i i
0.60 0.80 1.00
032609 #29
100n pFOS
0
0.60 0.80 1.00
032609 #29
100^ PFOA-I.S.
1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40
2.36
2.27 2.43 2.67
3.03
2.86
i .A
3.60 3.80 4.00
2: MRM of 11 Channels ES-
498.65 > 98.8
1.13e3
3.38 3-49
1.20 1.40 1.60
o
1.80 2.00 2.20 2.40 2.60 2.80
2.77
3.00 3.20 3.40
3.60 3.80 4.00
2: MRM of 11 Channels ES-
420.65 > 375.75
1.15e6
0.60 0.80
032609 #29
100q PFOA
0 1111111111111111111111111111111111111111111111111
0.60 0.80 1.00 1.20 1.40
032609 #29
100n
1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20
2.77
2'35
2.52 2.66
3.40 3.60 3.80 4.00
2: MRM of 11 Channels ES-
412.6 > 368.65
8.53e3
2.88
3'3
3.16 3.33
1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40
3.40
o-
Total Ion Chromatograph #3
3.60 3.80 4.00
3: MRM of 15 Channels ES-
TIC
1.90e5
0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00
032609 #29 2: MRM of 11 Channels ES-
2.77 TIC
100n
Total Ion Chromatograph #2
1.1 6e6
3.03
0
0.60 0.80 1.00 1.20 1.40
032609 #29
1001 Total Ion Chromatograph #1
1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20
2.05
i\
2.51
3.40 3.60 3.80 4.00
1: MRM of 12 Channels ES-
TIC
1.27e6
Time
0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00
-------
Sample W63PW + 400 ng/L of each target compound
100n
3.04
PFOS-I.S.
2: MRM of 11 Channels ES-
502.6 > 83.9
2.08e5
0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80
032609 W63PW-SA #22
0
3.00 3.20 3.40 3.60 3.80 4.00
2: MRM of 11 Channels ES-
3.04 498.65 > 98.8
1.73e5
0.60 0.80 1.00
032609 W63PW-SA #22
100-
0
PFOA-I.S.
1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80
2.77
3.00 3.20 3.40 3.60 3.80 4.00
2: MRM of 11 Channels ES-
420.65 > 375.75
7.59e5
0.60 0.80 1.00
032609 W63PW-SA #22
100-
1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80
2.77
0
0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80
032609 W63PW-SA #22
100n
3.00 3.20 3.40 3.60 3.80 4.00
2: MRM of 11 Channels ES-
412.6 > 368.65
1.14e6
3.00
3.20
3.23
Total Ion Chromatograph #3
3.40 3.60 3.80 4.00
3: MRM of 15 Channels ES-
TIC
3.62e5
3.41
0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80
032609 W63PW-SA #22
100, 2'77
0
Total Ion Chromatograph #2
3.00 3.20
3.03
A
3.40 3.60 3.80 4.00
2: MRM of 11 Channels ES-
TIC
2.25e6
0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80
032609 W63PW-SA #22
2.05 2.47
Total Ion Chromatograph #1
100
0.65
1.43
A
/ V
1.61
3.00 3.20 3.40 3.60 3.80 4.00
1: MRM of 12 Channels ES-
TIC
2.06e6
Time
0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00
-------
Sample W06PW + 400 ng/L of each target compound
100n
3.03
PFOS-I.S.
2: MRM of 11 Channels ES-
502.6 > 83.9
2.35e5
U I i i i i | i i i i | i i i i | i i i i | i i i i | i i i
0.60 0.80 1.00
032609 W06PW-SA #4
1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80
0
3.00 3.20
3.03
3.40 3.60 3.80 4.00
2: MRM of 11 Channels ES-
498.65 > 98.8
1.85e5
0.60 0.80 1.00
032609 W06PW-SA #4
100^ RFOA-I.S.
1.20 1.40 1.60
0
1.80 2.00 2.20 2.40 2.60 2.80
2.77
3.00 3.20 3.40
3.60 3.80 4.00
2: MRM of 11 Channels ES-
420.65 > 375.75
8.24e5
0.60 0.80 1.00
032609 W06PW-SA #4
1.20 1.40 1.60 1.80 2.00 2.20 2.40
100
PFOA
2.60 2.80
2.77
3.00 3.20 3.40
3.60 3.80 4.00
2: MRM of 11 Channels ES-
41 2.6 > 368.65
1 .26e6
0
0.60 0.80 1.00 1.20 1.40
032609 W06PW-SA #4
100q
Total Ion Chromatograph #3
1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40
3.23
3.41
3.60 3.80 4.00
3: MRM of 15 Channels ES-
TIC
3'12e5
0.60 0.80 1.00 1.20 1.40
032609 W06PW-SA #4
100n
1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20
0
Total Ion Chromatograph #2
2.77
(I
3.40 3.60 3.80 4.00
2: MRM of 11 Channels ES-
TIC
2.39e6
3.03
A
0.60 0.80 1.00
032609 W06PW-SA #4
100
1.20 1.40 1.60
Total Ion Chromatograph #1
1.80 2.00 2.20 2.40 2.60 2.80
2.05 2.51
0.65
1.42
3.00 3.20 3.40 3.60 3.80 4.00
1: MRM of 12 Channels ES-
TIC
2.30e6
Time
0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00
-------
Sample W02PW + 400 ng/L of each target compound
100n
3.03
PFOS-I.S.
2: MRM of 11 Channels ES-
502.6 > 83.9
1.55e5
0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80
032609 W02PW-SA #35
0
3.00
3.03
3.20 3.40 3.60 3.80 4.00
2: MRM of 11 Channels ES-
498.65 > 98.8
1.63e5
0.60 0.80 1.00
032609 W02PW-SA #35
100-
0
PFOA-I.S.
1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80
2.77
3.00 3.20 3.40 3.60 3.80 4.00
2: MRM of 11 Channels ES-
420.65 > 375.75
9.13e5
0.60 0.80 1.00
032609 W02PW-SA #35
100
1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80
2.77
3.00 3.20 3.40 3.60 3.80 4.00
2: MRM of 11 Channels ES-
412.6 > 368.65
1.02e6
0
0.60 0.80 1.00 1.20 1.40
032609 W02PW-SA #35
100q
Total Ion Chromatograph #3
1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00
3.20 3.40 3.60 3.80 4.00
3: MRM of 15 Channels ES-
3.23 TIC
3.14e5
3.41
0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80
032609 W02PW-SA #35
100, 2'77
0
Total Ion Chromatograph #2
3.00 3.20
3.03
A
3.40 3.60 3.80 4.00
2: MRM of 11 Channels ES-
TIC
2.22e6
0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80
032609 W02PW-SA #35
2.51
100
Total Ion Chromatograph #1
2.05
0.64
1.42
A
1.61
3.00 3.20 3.40 3.60 3.80 4.00
1: MRM of 12 Channels ES-
TIC
2.12e6
Time
0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00
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Sample W27SW
100n
3.04
PFOS-I.S.
2: MRM of 11 Channels ES-
502.6 > 83.9
3.09e5
U i i i i i | i i i i | i i i i | i i i i | i i i i | i i i
0.60 0.80 1.00
032609 #7
100n
1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00
2: MRM of 11 Channels ES-
3.04 498.65 > 98.8
8.35e3
,n
2.98,
2.30 2.44 2.66 2.80
3.17
3.49
0.60 0.80 1.00
032609 #7
PFOA-I.S.
1.20 1.40 1.60
1.80 2.00 2.20 2.40 2.60 2.80
2.77
3.00 3.20 3.40
o
3.60 3.80 4.00
2: MRM of 11 Channels ES-
420.65 > 375.75
9.12e5
0.60 0.80
032609 #7
100^ PFOA
1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40
2.60 2.80
2.77
3.00 3.20 3.40
o
3.60 3.80 4.00
2: MRM of 11 Channels ES-
412.6 > 368.65
3.69e5
0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00
032609 #7 3: MRM of 15 Channels ES-
3.41 TIC
100n
Total Ion Chromatograph #3
3-23
1 .69e5
0.60 0.80 1.00 1.20 1.40
032609 #7
Total Ion Chromatograph #2
3.61 3.83
1.60
1.80 2.00 2.20 2.40 2.60 2.80
2.77
o
3.00 3.20
3.04
A
3.40 3.60 3.80 4.00
2: MRM of 11 Channels ES-
TIC
1.38e6
0.60 0.80 1.00 1.20 1.40 1.60
032609 #7
1 Total Ion Chromatograph #1
1.80
2.00 2.20
2.06
2.40 2.60 2.80 3.00 3.20
0.66
1.43
2 1
3.40 3.60 3.80 4.00
1: MRM of 12 Channels ES-
TIC
1.51e6
Time
0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00
-------
Sample W14PW
100n
3.03
PFOS-I.S.
U I i i i i i i i i i i i i i i i i i i i i i i i i i i i i
0.60 0.80 1.00
032609 #10
100n
2: MRM of 11 Channels ES-
502.6 > 83.9
4.56e5
1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80
3.00 3.20
3.03
3.40
2.32 2.48 2.63 2.77
2.96
A
3.60 3.80 4.00
2: MRM of 11 Channels ES-
498.65 > 98.8
8.47e3
3.23
3.40
0.60 0.80 1.00
032609 #10
100^ RFOA-I.S.
1.20 1.40 1.60
1.80 2.00 2.20 2.40 2.60 2.80
2.77
3.00 3.20 3.40
3.60 3.80 4.00
2: MRM of 11 Channels ES-
420.65 > 375.75
8.48e5
0.60 0.80
032609 #10
PFOA
1.00 1.20 1.40 1.60
1.80 2.00 2.20 2.40 2.60 2.80
2.77
3.00 3.20 3.40
3.60 3.80 4.00
2: MRM of 11 Channels ES-
41 2.6 > 368.65
1 .58e6
0.60 0.80 1.00 1.20 1.40
032609 #10
100^
Total Ion Chromatograph #3
1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20
3.40 3.60 3.80 4.00
3: MRM of 15 Channels ES-
3.41 TIC
I 2.73e5
3.23
0.60 0.80 1.00 1.20 1.40
032609 #10
1 Total Ion Chromatograph #2
1.60 1.80 2.00 2.20 2.40 2.60 2.80
2.77
3.00 3.20
3.40 3.60 3.80 4.00
2: MRM of 11 Channels ES-
TIC
2.88e6
3.03
A
0.60 0.80 1.00 1.20 1.40 1.60
032609 #10
1001 Total Ion Chromatograph #1
0.66 1^,3
1.80 2.00 2.20 2.40 2.60 2.80
2.47
2.06
3.00 3.20 3.40 3.60 3.80 4.00
1: MRM of 12 Channels ES-
TIC
2.72e6
A
Time
0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00
-------
Sample W42SW
100n
3.03
PFOS-I.S.
2: MRM of 11 Channels ES-
502.6 > 83.9
3.03e5
U i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i
0.60 0.80 1.00 1.20 1.40 1.60
032609 #12
1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20
3.03
2.961
2'25 2'39 A56 2^69 ^-9
Fff
2.20 2.40 2.60 2.80 3.00 3.20
2.77
3.40 3.60 3.80 4.00
2: MRM of 11 Channels ES-
498.65 > 98.8
7.33e3
3.43
0.60 0.80 1.00
032609 #12
100^ PFOA-I.S.
1.20 1.40 1.60 1.80 2.00
3.40 3.60 3.80 4.00
2: MRM of 11 Channels ES-
420.65 > 375.75
8.46e5
0.60
032609 #12
100n
0.80 1.00 1.20 1.40 1.60
1.80 2.00 2.20 2.40 2.60 2.80
2.77
3.00 3.20 3.40 3.60 3.80 4.00
2: MRM of 11 Channels ES-
412.6 > 368.65
2.93e6
0.60 0.80 1.00 1.20 1.40
032609 #12
100^
Total Ion Chromatograph #3
U I i i i i | i i i i | i i i i | i i i i | i i i i | i i i i | i i i i | i i i i | i i i i | i i i
0.60 0.80 1.00 1.20 1.40
032609 #12
100n
1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20
3.23
3.40 3.60 3.80 4.00
3: MRM of 15 Channels ES-
3.40 TIC
1.43e5
3.76 3.94
1.60 1.80 2.00 2.20 2.40 2.60 2.80
2.77
3.00 3.20
Total Ion Chromatograph #2
3.40 3.60 3.80 4.00
2: MRM of 11 Channels ES-
TIC
4.58e6
3.03
0.60 0.80 1.00 1.20 1.40 1.60
032609 #12
1 Total Ion Chromatograph #1
1.80 2.00 2.20 2.40 2.60 2.80
2.47
2.05
0.65
1.43
3.00 3.20 3.40 3.60 3.80 4.00
1: MRM of 12 Channels ES-
TIC
3.71 e6
Time
0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00
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vvEPA
United States
Environmental Protection
Agency
Office of Research and Development
(8101R)
Washington, DC 20460
Official Business
Penalty for Private Use
$300
EPA 600/C-09/004
May 2009
www.epa.gov
Recycled/Recyclable
Printed with vegetable-based ink on paper that
contains a minimum of 50% post-consumer
fiber and is processed chlorine free.
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