Document LK8oZyJJyvo7XBKdeJpyqG3Db
AR226-2666
01
RE.S EARCH
. Precise Research. Proven Results.
AR226-2666 l/^
Analytical Report
Air Sampling Fluorochemical Report
DuPont Washington Works-Air Sampling Program Round 11
Exygen Research Report No. L0001668
\/\c^
Testing Laboratory
Exygen Research , 3058 Research Drive State College, PA 16801
Requester
Michael D Aucoin URS Corporation
Barley Mill Plaza
Building 27 Room 1260 Lancaster Pike and Rt 141
Wilmington, DE, 19805
ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH
Paw 1 of 7
3058 Research Drive State College, PA 16801, USA
T: 800.281.3219 F: 814.272.1019
V
Summary
' /.
.
'..
Seven solid media samples were received by Centre Analytical Laboratories, Inc. (dba Exygen Research) (Exygen) from DuPont Corporation. The media represent samples of air collected on OVS tubes. Please see Table 1 for a completed listing of samples received and field air volumes
collected.
'
The
s
a
. . ' -t;
mples
w'
e
r
e
' .
.
analyzed
for
.
Perfluorooctanoic
Acid
(C8
'. -.
Acid)
using
liquid
chromatography
/ mass spectrometry (LCMS). The method employed is entitled "Method of Analysis for the
Determination of Perfluorooctanoic Acid (PFOA) in OVS Airtubes by LCMS" (James Miller,
Exygen Research, February 17, 2003).
The OVS tubes were separated into three fractions for specific fluorochemical analysis. Fraction A consisted of the filter, backing material and plastic ring. Fraction B contained the
first bed of XAD resin and the PUF backing. Fraction C contained the second bed of XAD resin and PUF backing. Fractions A and B were extracted with 1 mL of methanol. Fraction C lll'Yas 'not analyzed but saved for possible future analysis. Perfluorodecanoic Acid (C 10 Acid)
^as added as a surrogate spike to each fraction prior to extraction.
Instrument operating conditions can be found at the beginning of each analytical run. Raw instrument data is given in Appendix A. Chain-of-custody information can be found in Appendix B.
ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH
Page 2 of 7
' t
'esults Smnmarv
'
Request #
Air Volume Sampled (L)
C8Acid (mg/m3)
WWK-A-AMS1-E11 A
.
WWK-A-AMS1-E-11B
WWK-A-AMS1-E11C
WWK-A-AMS1-E11 (Total)
1398 1398 1398
< 0.00007 < 0.00007
NA
< 0.0,00,14
WWK-A-AMS2-E11 A ,, WWK-A-AMS2-E11 B
WWK-A-AMS2-E11 C WWK-A-AMS2-E11 (Total)
WWK-A-AMS3-E11A WWK-A-AMS3-E11 B WWK-A-EMS3-E11 C WWK-A-EMS3-E11 (Total)
1448 1448 : 1448
. 931 .
931 931
< 0.00007
.
< 0.00007 NA
< 0.00014
< 0.0001 < 0.0001
NA < 0.0002
:
WWK-A-AMS4-E11 A
WWK-A-AMS4-E11B
WWK-A-AMS4-E11C
WWK-A-AMS4-E11 (Total)
: ,
WWK-A-AMS5-E11 A
.
WWK-A-AMS5-E11 B
.
:
WWK-A-AMS5-E11C
WWK-AAMS5-E11 (Total)
1424
;
1424
1424
1402 1402 1402
<0.00007
< 0.00007 NA
< 0.00014
0.0003 < 0.00007
NA 0.0003
WWK-A-AMS6-E11A WWK-A-AMS6-E11 B WWK-A-AMS6-E11 C WWK-AAMS6-E11 (Total)
1434 1434 1434
< 0.00007 < 0.00007
NA
< 0.00014
NA - Not Analyzed. B fraction was below the quantitation limit, therefore the backup fraction does not require analysis.
1. ."<" is defined as not detected at or above the reported level.
2. Sample results have not been corrected for blank results or control spike recoveries. 3. Please note the following descriptions of the OVS sample tube fractions:
Fraction A B C
Fraction Description Frit Extract 1st set beads extract 2nd set beads extract
(not analyzed)
ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH
z; ^
-. ^
^-.2,
^
0.^
Page 3 of 7
OCData
\
,,
;
'
"
!
--- ,' 1
11
1
,
^
.
'
.!
; .
;
,
11
'
' ' Lcs .
'
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' !
''
.
! '
.
1. 11"
1 '
' 1" 11
''
.
11 ''11
.
,
Please note: One control sample was spiked with each perfluorooctanoic acid to give a final concentration of 500 p
through the tube at a rate of 1-liter per minute for one hour (60 liters of air). The fractions were separated and ana
acceptable range for control recovery is 75-125%.
Request # Control 1
CSAcid (amount spiked - ppb)
500
C8 Acid (amount recovered -
509
ppb)
CSAcid (percent recovery
102
^ A(L<U<fM^
Blanks
Requests WWK-A-AMSFBLK-E9 A WWK-A-AMSFBLK-E9 B
Vol. Of Air (L)
0
-1 -'0 ...
.", .
CSAcid (ug/fraction)
<0.10 <0.10
ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH
Page 4 of 7
. . . ; . ' surrogates '
'.
.
.
.
A surrogate spike (C 10 Acid) was added to all OVS tubes to give a final concentration of 500 ppb in the extract.
Surrogate spike recoveries are given in the following table. There are no set criteria for surrogate spike
recoveries. Advisory ranges are 75-125%.
Sample #
. WWK-A-AM8FBLK-E11 A WWK-A-AMSFBLK-E11 B WWK-A-AMS1-E11 A WWK-A-AMS1-E11 B
.
WWK-A-AMS2-E11 A
'
WWK-A-AMS2-E11 B WWK-A-AMS3-E11 A WWK-A-AMS3-E11 B WWK-A-AMS4-E11 A WWK-A-AMS4-E11 B WWK-A-AMS5-E11 A WWK-A-AMS5-E11 B WWK-A-AMS6-E11 A WWK-A-AMS6-E11 B
Control Spike A Control Spike B
Amount Spiked (PPb)
500 500 500 500
. '500
500 500 500 , 500 . 500 500 500 500 .
.
500 500 500
Amount Recovered (PPb)
479
360
498
:.
564
497 ,
:
583
517
'
580
519
;
569
520
> 592
-: ,
524
'584
532
347
Percent Recovery (%)
96
72*:
100
113
99
117 -
.
103
116
.
104
114 104 : 118
105..:
117
106
69*
* Surrogate recovery outside of advisory range.
ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH
Page 5 of 7
*vssy
SB
Calculations
Request #
WWK-A-AMSFBLK-E11 A .
WWK-A-AMSFBLK-E11 B WWK-A-AMS1-E11 A WWK-A-AMS1-E11 B
''WWK-A-AMS2-E11 A WWK-A-AMS2-E11 B WWK-A-AMS3-E11 A WWK-A-AMS3-E11 B WWK-A-AMS4-E11 A WWK-A-AMS4-E11 B WWK-A-AMS5-E11 A WWK-A-AMS5-E11 B WWK-A-AMS6-E11 A WWK-A-AMS6-E11 B Control Spike A Control Spike B
Vol. Of Air
(L)
0
0
1398 1398 1448 1448 931 931 1424 1424 1402 . 1402 1434 1434
0
0
C8 Acid (raw-ppb)
<10 <10 <10 <10 <10 <10
10
<10 <10 <10
434
<:10
<10 <10
509
<10
C8 Acid (ug/fraction)
<0.10 <0;10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10
<:0.10 <0.10 0.43 ; <0.10
<0.10 <0.10
0.51
<0.10
C8Acid (mg/m3)
< 0.00007 < 0.00007 < 0.00007 < 0.00007 <0.0001 < 0.0001 < 0.00007 < 0.00007
0.0003 < 0.00007 < 0.00007 < 0.00007
ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH
Page 6 of 7
I*
Example Calculation
For sample WWK-A-AMS5-E11 A C8 Acid, " .
'
.
,;;.:
, ' =
[434 ng/ml of C8 Acid x (1ml) x (lug/1000 ng)x(l-mg/1000 ug)] / [(1402 L) x (1 m3 /
"1000L)} ' /
'
''
'
'.';. ^ '. ,: ,
:,
.:- :"
.
.
; /
'
.'
-
.
,
.
.
0.0003 mg / m3
Signatures
iAj \ ] ^ . P^ulConnolly,'tlCMSTeam Leader
(7.//v/^/^ /Oohn M. Flaherty, Vice President
Other Lab Members Contributing to Data James Miller
^wl
Date
^?/^
Date
ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BYEXYGEN RESEARCH
Page 7 of 7
-ogin Project:
P0000419 .
Project Storage:
Company Name: Submitted By: Login Type: Started: Date Start:
DuPont de Nemours & Co, Inc.
Michael D. Aucoin
Immediate Receipt of Samples
T. '
01/19/2004
'
-
'"
.
Due Date: Received Date:
02/02/2004 01/17/2004
Received By:
AMMERMAN, MARK
Spread Sample:
Label:
Project Title/Type: Analysis ofPFOAin OVS Tubes / ROUTINE ExygenSD/PI: MILLER, JAMES
Login Notes:
Conform Notes:
COC True %nform Sample: :^iaSS^S8^S:SS;^TM;^;S^^j^S;^!5ia5a=^^^ga^<^SS^^ja
Conform COC:
True
Conform Sample:
True
Conform Request:
True
PK0002257 Carton
Packages / Containers
Mail Date / Condition
' Shipper /IP
1/17/2004 12:00:56PM Package & Contents Uncompromised
FEDEX 8363912984560200
Temp. Control/Temp.
None 23.3
Direction / Handled By
RECEIVED AMMERMAN. MARK
Sir ,ainer#
C0026159 C0026160 C0026161 C0026162 C0026163 C0026164 C0026165 C0026166 C0026167 'C0026168 C0026169 C0026170 C0026171 C0026172 C0026173 C0026174 C0026175 C0026176 C0026177 C0026178 C0026179 C0026180 C0026181 C0026182
Gross Weight
6.3 g 6.3 g 6.3 g 6.1 g 6.1 g 6.1 g. 6:3 g 6.3 g 6.3 g
6.1 g 6.1 g 6.1 g 6.2 g
6.2 g 6.2 g 6.2 g 6.2 g 6.2 g 6.1 g 6.1 g. 6.1 g 6.3 g 6.3 g 6.3 g
Container Type
Other Other Other Other Other Other Other Other Other Other Other Other . Other Other Other Other Other Other Other Other Other Other Other Other
Preservative NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE . NONE
Mfg.J-ot
|,gTM|||f "cellaneous
1181- <.em Key
None
1/19/2004 Login.rpt
Description
ICOC
U054
Report Version: Dec 22 2003 10:44AM Page 1 of 4
Instance:
R0080976
83623131323120
ogin
llfttn Sample ID .
"W 668-0001
01668-0002 L0001668-0003 L0001668-0004 LOO01668-0005 L0001668-0006 L0001668-0007 L0001668-0008 LOO01668-0009 L0001668-0010 L0001668-0011 L0001668-0012 L0001668-0013 L0001668-0014 'L0001668-0015 L0001668-0016 L0001668-0017 L0001668-0018 L0001668-0019 L0001668-0020 L0001668-0021 L0001668-0022 L0001668-0023 LOO01668-0024
Matrix GAS GAS GAS GAS GAS GAS GAS GAS GAS
.
GAS GAS GAS GAS
GAS. GAS GAS GAS . GAS GAS GAS GAS GAS GAS GAS
Samples
Fraction
Sample
OVS Tubes
WWK-A-AMSFBLK-E11.A
'':
"
.'-','
' .
OVS Tubes . OVS Tubes OVS Tubes
WWK-A-AMSFBLK-EH B " '
WWK-A-AMSFBLK-Eire :'. WWK-A-AMS1-E11 A-' ../ :
;'.', '. ''.
.
;' '
:."' '.
. , '
,
'
DateSamplecI Date Received 01/16/2004 01/17/2004 01/16/2004 01/17/2004 01/16/2004 : 01/17/2004 01/16/2004 01/17/2004
OVS Tubes
WWK-A-AMS1-E11 B .; ''': .. .' ' "
01/16/2004 01/17/2004
OVS Tubes : ..WWK-A-AMS1-E11.C ''' : .
01/16/2004 01/17/2004
/.- OVS Tubes . WWK-A-AMS2-E11A.
:\:
01/16/2004 .01/17/2004
. . :. . OVS Tubes
OVS Tubes
/' OVS Tubes
OVS Tubes
WWK-A-AMS2-E11 B
.:., ^ - '
.
" : .
01/16/2004
WWK-A-AMS2-E11 C
';
..
..-'-- ''.::':
'
./
.01/16/2004
WWK-A-AMS3-E11 A:
'',.
.. :,,
.
.. ,;- \
01/16/2004
WWK-A-AMS3-E11 B.
'.::' "
'
. 01/16/2004
01/17/2004 01/17/2004 01/17/2004 01/17/2004
OVS Tubes .
'
OVS Tubes
'
WWK-A-AMS3-E11 C
;:-',
'
'
WWK-A-AMS4-E11 A ' :; .
,' ".' ;
"
''.
'
01/16/2004 01/16/2004
51/17/2004 01/17/2004
OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes '' OVS Tubes OVS Tubes OVS Tubes OVS Tubes
WWK-A-AMS4-E11 ^ WWK-A-AMS4-E11 C WWK-A-AMS5-E11 A WWK-A-AMS5-E11 B WWK-A-AMS5-E11. C WWK-A-AMS6-E11 A WWK-A-AMS6-E11 B WWK-A-AMS6-E11 C Control 1 A -
'
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.''' ',~.:'"'' "
'.'
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:'. ;. ;; ! -
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''' .', ' -. :
\ .' .' " '
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01/16/2004 01/16/2004 01/16/2004 01/16/2004 01/16/2004 01/16/2004 01/16/2004 01/16/2004
01/17/2004
01/17/2004 01/17/2004
'
01/17/2004 : 01/17/2004
01/17/2004 01/17/2004 01/17/2004 01/17/2004
OVS Tubes . Control 1 B
\ 01/17/2004
OVS Tubes
Control 1 C
. '
'
'
'
" /-
' '
'
.
" .
01/17/2004
Date Due 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004
1/19/2004 Login, rpt
:
U U "^'D
Report Version: Dec 22.2003 10:44AM Page 2 of 4
Instance:
R0080976
^
J0001668-0001
Container ^026159/Other/NONE
L0001668-0002
Container C0026160 / Other/NONE
L0001668-0003
Container . C0026161/Other/NONE
L0001668-0004
Container C0026162 / Other / NONE
L0001668-0005
Container C0026163 / Other / NONE
L0001668-0006
Container C0026164 / Other / NONE
W ,01668-0007 ' .
Container C0026165 / Other /NONE
L0001668-0008
'..
Container
: C0026166/Other/NONE
L0001668-0009
l
Container
C0026167 / Other / NONE
] L0001668-0010
Container C0026168 / Other / NONE
L0001668-0011
Container . C0026169/Other/NONE
L0001668-0012
il\
Container
ill 1026170/Other/NONE
1/19/2004 Login.rpt
ogin
Bottles
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
ij0o6
Report Version: Dec 22 2003 10:44AM Page 3 of 4
Instance:
R0080976
33291750178
Container C0026171 /Other /NONE
1^01668-0014
Container C0026172/Other/NONE
L0001668-0015
Container C0026173 / Other / NONE
L0001668-0016
Container C0026174 / Other / NONE
L0001668-0017
Container C0026175 / Other / NONE
L0001668-0018
Container C0026176/Other/NONE
L0001668-0019
aiy JM26177 / Other / NONE
L0001668-0020
Container C0026178/Other/NONE
L0001668-0021
Container C0026179 / Other /NONE
L0001668-0022
Container C0026180 / Other / NONE
L0001668-0023
Container C0026181 /Other/NONE
L0001668-0024
Container
C0026182 / Other / NONE
1/19/2004 Login.rpt
Method Method 'Method Method Method Method Method
Method Method Method Method
JUS7
Report Version: Dec 22 2003 10:44AM Page 4 of 4
Instance:
R0080976
93491758178
CHAIN OF CUSTODY/ANALYSIS RE
RESEARCH
Exygen Research Sample Receiving * 3117 Research Drive State College, PA 16801, U T: 814.231.8032 F: 814.231.1580 exygenresearch'.com
I^Wj<^"l^ll*^it'jt^
'
Client (name & address):
( M ^ ^ Phone:
(^^ma-IU^ Fax:
'^,.Pn^
\
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.
\A)a^A^A\/v}<^rte \j
Sampler: R.\<-(L(YWI L.,^^u
Piease fill out this form completely to ensure
fTV;V^fW^ Project Manager (Name & E-mail Address):
^oject Name:
n-^c ^(k'rA^v\Ap\
P.O. #:
.\ ^J
Quotati on i^.
^
ArQ^-ri?^^.
<^
.
corr ect anal^/sis cand proper handling of your samples.
W W I E ExyLIMS# Client Sample Identification
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Date
Time
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Date
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^(T/T^i .S^>>ACLM.
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Cooler ID #
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Received by
^V,^y^/a/(H.
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'
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LAB USE ONLY
' ' .
Cooler Temp. (0 ^yf Date (^is ^Time
Di/i^e^'"Ok'OO ^/y^ /<;^
'.:"'11
''^iii^
Sampler(s):
SO,RK, LK
DuPont Washington Works Air Sampling Program
FedEx Airbill #: 836391298456
Event Number
Pump#
669842 669908 669901 669890 669796 669865 Hours
0 1
2 3 4 ,
Station #^
AMS-1 AMS-2 AMS-3 AMS-4 AMS-5 AMS-6 Minutes
0
60 120 180 240
^^ iExygwID^piisE' WWK-A-AMS1-E11 WWK-A-AMS2-E11 WWK-A-AMS3-E11 WWK-A-AMS4-E11 WWK-A-AMS5-E11 WWK-A-AMS6-E11 Hours .
5
6
7 8
9
;Calibration-(pre) 0.9970 1.0160 1.0200 1.0180 1.0210 1.0150 Minutes 300 360 420 480 540
Dafe% 15-Jan 15-Jan 15-Jan 15-Jan 15-Jan 15-Jan Hours
10 11 12 13 14
IJStaiirti'Time?iaQate^
0700
16-Jan
0625 16-Jan
0627
16-Jan
0632
16-Jan
0638
16-Jan
0647
16-Jan
Minutes Hours
600
15
660
16
720
17
780
18
840
19
sSfo'p'aime,.
^0620 .
0635 0637 0658 0645 0722
Minutes 900 960 1020 1080 1140
;<RaHBration(pbst)
0.9794 0.9739 1.0130 1.0140 0.9687 1.0330 Hours
20
21 22 23
24
Field Blank:
yes yes or no
WWK-K-AMSFBLK-E11
Weather: 1/15Cold, about 27 F, snow flurries, windy
1/16 Cold, about 18 F, clear, breezy
SAFER operational:!
yes yes or no
Comments: Total minutes column is the reading from the monitor counter.
* AMS-3 was still running when we collected the sample after about 1410 minutes, but the counter only read 931 min
1/16/2f"<
Page-'1 of 2
-
'
DuPont Washington Works Air Sampling Program
Sampler(s):
SO,RK,
LK
FedEx Airbill #: 836391298456
Event Number
669842 669908 669901 669890 669796 669865
Hours
0 1
'
2 3 4
Field Blank:
AMS-1 AMS-2 AMS-3 AMS-4 AMS-5 AMS-6 Minutes
0
60 120 180 240
yes yes or no
WWK-A-AMS1-E11 WWK-A-AMS2-E11 WWK-A-AMS3-E11 WWK-A-AMS4-E11 WWK-A-AMS5-E11 WWK-A-AMS6-E11
Hours
5 6 7 8
:.9
0.9970 1.0160 1.0200 1.0180 1.0210 1.0150 Minutes
300
. 3 64020
480 540
WWK-K-AMSFBLK-E11
^Ss^^^: liiiilis^
15-Jan
0700
15-Jan
0625
15-Jan
0627
15-Jan
0632
15-Jan
0638
15-Jan
0647
Hours Minutes
10
600
"660 11
12
720
--13
780
14
840
IMMII^I lii|l;iiW|iENW
16-Jan
0620
0.9794
16-Jan 0635
'0.9739 .
16-Jan 16-Jan
0637 0658
1.0130 1.0140
16-Jan
0645
0.9687
16-Jan
0722
1.0330
Hours Minutes
Hours
15
900
20
16
960
21
17
1020
22
18
1080
23
19
1140
.
24.
,
.'
Weather: 1/15 Cold, about 27 F, snow flurries, windy
1/16 Cold, about 18 F, clear, breezy
SAFER operational:!
yes yes or no
Comments; Total minutes column is the reading from the monitor counter. * AMS-3 was still running when we collected the sample after about 1410 minutes, but the counter only read 931 min
1/28/2004
R ES EAR.C H
^ Precise Research. Proven Results.
Sample "Condition Upon Receipt" Form
Protocols . Exygen Study #
^ac^a^lf t^W /G>Cf
Date & Time Received Condition of Samples
0///7/^/ /z
^f^t-yy/^^--. f-
Temporary Storage Location
pi.w t}^_r
Initials & Date Waybill #
M(4 ^/^ r^c.5 9/^9 ^w
Comments:
--^. --^.f--//--^--/--L--fir--'---e^----^/-^^----e^--. --/i--f^--r^
May 24. 2002/3
Q:AVORD priK-cs^-lo^in.SLimpleCundiiioiionRcceipt.tiuc
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THIS IS AN EXACT COPY OF
W?| . HE ORIGINAL DOCUMENT ,
iY __AA----_ DATE
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