Document O14Yaqg6Z3ybr0zjgqE8dk12e
RECYCLED
AR226-2659
&> CO
V
RES E A R C H
.Precise Research. Proven Results.
AR226-2659
Analytical Report
."
Air Sampling Fluorochemical Report
DuPont Washington Works - Air Sampling Program Round 2 Exygen Research Report No. L0001308
i i / 1t s
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
Iw
I
ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH
Page 1 of 7
S j L 305i8 Research Drive
V1 m SSttaate College, PA 16801, USA T: 800.281.3219
F: 814.272.1019
luminary
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 samples were 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 was not analyzed but saved for possible future analysis. Perfluorodecanoic Acid (CIO Acid) was 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
P R e su lts S u m m a ry . y ' , - ' . ,
-, : :
" .- -
-
Request #
WWK-A-AMS1-E2 A WWK-A-AMS1-E2 B WWK-A-AMS1-E2C WWK-A-AMS1-E2 (Total)
Air Volume Sampled (L)
.
' / 1475
.-
. 1475 .- . - : .
1475
C8 Acid . (mq/m3)
<0.00007 < 0.00007
NA .... <0.00014
< G .\\
WWK-A-AMS2-E2 A
,, WWK-A-AMS2-E2 B
WWK-A-AMS2-E2 C
WWK-A-AMS2-E2 (Total)
.
1468 1468 1468
0.0009 <0.00007
NA
0.0009
O ,V
WWK-A-AMS3-E2 A
'
WWK-A-AMS3-E2 B
. WWK-A-EMS3-E2 C
WWK-A-EMS3-E2 (Total)
1462 1462 1462
-
0.0009 <0.00007
NA
0.0009
: WWK-A-AMS4-E2 A
WWK-A-AMS4-E2 B WWK-A-AMS4-E2 C
WWK-A-AMS4-2 (Total)
1437 1437 1437
:
< 0.00007 < 0.00007
NA
<0.00014
< o. A
: WWK-A-AMS5-E2 A
WWK-A-AMS5-E2 B WWK-A-AMS5-E2 C
WWK-A-AMS5-E2 (Total)
.
1456 1456 1456
<0.00007 < 0.00007
NA
<0.00014
c . }-
WWK-A-AMS6-E2 A WWK-A-AMS6-E2 B WWK-A-AMS6-E2 C
WWK-A AMS6-E2 (Total)
1422 1422 1422
.
<0.00007 < 0.00007
NA
<0.00014
. < o .K
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
Page 3 of 7
OC Data
l c s '. . . . .
- .;
Please note: One control sample was spiked with each perfluorooctanoic acid to give a final concentration of 500 ppb. Air was pulled
through the tube at a rate of 1-liter per minute for one hour (60 liters of air). The fractions were separated and analyzed. The
acceptable range for control recovery is 75-125%.
Request # Control 1
C8 Acid (amount spiked - ppb)
500
C8 Acid (amount recovered - ppb)
503
C8 Acid (percent recovery
101
Blanks
Request # WWK-A-AMSFBLK-E2 A WWK-A-AMSFBLK-E2 B
Voi. Of Air (L) 0 0
C8 Acid (uq/fraction)
: <0.10 . <0.10
ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 4 of 7
S" urrogates
:
\
.
A surrogate spike (CIO 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-AMSFBLK-E2 A WWK-A-AMSFBLK-E2 B
WWK-A-AMS1-E2 A WWK-A-AMS1-E2 B WWK-A-AMS2-E2 A WWK-A-AMS2-E2B WWK-A-AMS3-E2 A WWK-A-ANIS3-E2 B WWK-A-AMS4-E2 A WWK-A-AMS4-E2 B . WWK-A-AMS5-E2 A WWK-A-AMS5-E2 B WWK-A-AMS6-E2 A WWK-A-AMS6-E2 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) , 644
329 707 392 666;: 405 : 666 : ' 396 697 403 . ' 732 437 . , 763 -375 612 392
Percent Recovery (%) 129* ...
* CD CD
141* 78 133* 81 133* 79 139* 81 146* 87 153* 75 122 78
> Surrogate recovery outside of advisory range
) a l l DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH
Page 5 of 7
Calculations
Request #
WWK-A-AMSFBLK-E2 A WWK-A-AMSFBLK-E2 B
WWK-A-AMS1-E2 A WWK-A-AMS1-E2 B WWK-A-AMS2-E2 A WWK-A-AMS2-E2 B WWK-A-AMS3-E2 A WWK-A-AMS3-E2 B WWK-A-AMS4-E2 A WWK-A-AMS4-E2 B WWK-A-AMS5-E2 A WWK-A-AMS5-E2 B WWK-A-AMS6-E2 A WWK-A-AMS6-E2 B
Control Spike A Control Spike B
Vol. Of Air
(L) 0 0 1475 1475 1468 1468 1462 1462 1437 1437 1456 1456 1422 1422 0 0
C8 Acid (raw-ppb) .
<10 < 10 < 10 <10 1340 < 10 1266 <10 <10 < 10 49 <10 < 10 <10 454 . 49
C8 Acid (ug/fraction)
<0.10 <0.10 <0.10 <0.10
1.3 <0.10
1.3 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 0.45 <0.10
C8 Acid (mg/m3)
< 0.00007 < 0.00007
0.0009 < 0.007
0.0009 <0.00007 < 0.00007 < 0.00007 <0.00007 <0.00007 <0.00007 < 0.00007
ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 6 of 7
Example Calculation .
For sample WWK-A-AMS2-E2 A C8 Acid,
= [1340 ng/ml of C8 Acid x (1 ml) x: (1 ug / 1000 ng) x (1 mg / 1000 ug) ] / [(1468 L) x (1 m3 /
1000 L)]
/ - ::
;'
= 0.0009 mg / m3
:/ v
Signatures
Other Lab Members Contributing to Data James Miller
ALL DATA-CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 7 of 7
onn r
Table 1. Login Information / Field Data
Sample ID
Exygen ,
Lab ID
Date Received Description
WWK-A-AMSFBLK-E2 A WWK-A-AMSFBLK-E2 B WWK-A-AMSFBLK-E2 C
WWK-A-AMS1-E2 A WWK-A-AMS1-E2B WWK-A-AMS1-E2 C WWK-A-AMS2-E2 A WWK-A-AMS2-E2 B WWK-A-AMS2-E2 C WWK-A-AMS3-E2 A WWK-A-AMS3-E2 B WWK-A-AMS3-E2 C WWK-A-AMS4-E2 A WWK-A-AMS4-E2 B WWK-A-AMS4-E2 C WWK-A-AMS5-E2 A WWK-A AMS5-E2 B WWK-A-AMS5-E2 C WWK-A-AMS6-E2 A WWK-A-AMS6-E2 B WWK-A AMS6-E2 C
Control Spike A Control Spike B Control Spike C
L0001308-1 L0001308-2 L0001308-3 L0001308-4 L0001308-5 L0001308-6 LOOO1308-7 L0001308-8 LOOO1308-9 L0001308-10 L0001308-11 L0001308-12 L0001308-13 L0001308-14 L0001308-15 L0001308-16 L0001308-17 L0001308-18 L0001308-19 L0001308-20 L0001308-21 L0001308-22 L0001308-23 L0001308-24
11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 : 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03
Frit extract 1st set beads extract 2nd set beads extract Frit extract 1st set beads extract 2nd set beads extract Frit extract 1st set beads extract 2nd set beads extract Frit extract ' 1st set beads extract 2nd set beads extract Frit extract 1st set beads extract 2nd set beads extract Frit extract 1st set beads extract , 2nd set beads extract Frit extract 1st set beads extract 2nd set beads extract Frit extract . 1st set beads extract 2nd set beads extract
Air Volume Sampled (L)
0 0 0 1475 1475 . 1475 1468 , 1468 1468 1462 1462 1462 1437 1437 1437 1456 . 1456 1456 1422 1422 1422 0 0 ' 0
'
Table 2. Chain of Custody
Sample ID
WWK-A-AMSFBLK-E2 A WWK-A-AMSFBLK-E2 B WWK-A-AMSFBLK-E2 C
WWK-A-AMS1-E2 A WWK-A-AMS1-E2 B WWK-A-AMS1-E2 C WWK-A-AMS2-E2 A WWK-A-AMS2-E2 B. WWK-A-AMS2-E2 C WWK-A-AMS3-E2 A WWK-A-AMS3-E2 B WWK-A-AMS3-E2 C WWK-A-AMS4-E2 A WWK-A-AMS4-E2 B WWK-A-AMS4-E2 C WWK-A-AMS5-E2 A WWK-A AMS5-E2 B WWK-A-AMS5-E2 C WWK-A-AMS6-E2 A WWK-A-AMS6-E2 B WWK-A AMS6-E2 C
Control Spike A Control Spike B Control Spike C
Date Collected
11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03
NA NA NA
Date Received at Exygen
11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03
Date Extracted by Exyqen
Date Analyzed by Exyqen
11/20/03 11/20/03
NA 11/20/03 11/20/03
NA 11/20/03 11/20/03
NA 11/20/03 11/20/03
NA 11/20/03 11/20/03
NA 11/20/03 11/20/03
NA 11/20/03 11/20/03 , NA 11/20/03 11/20/03
NA
11/20-11/21/03 11/20-11/21/03
NA 11/20 -11/21/03 11/20-11/21/03
NA 11/20 - 11/21/03 11/20 - 11/21/03
NA 11/20 - 11/21/03 11/20 - 11/21/03
NA 11/20 -11/21/03 11/20-11/21/03
NA 11/20 -11/21/03 11/20 - 11/21/03
NA 11/20-11/21/03 11/20-11/21/03
NA 11/20-11/21/03
11/20 - 11/21/03 " N .
Project:
P0000419
/
Project Storage:
........
Submitted By:
Michael D/AUcoin .
;;
: '
Conform COC: ^ Conform Sample:
Conform Request:
Status:
Unreceived
^:
Login Type:
Immediate Receipt of Samples
^
Started: DateStart: DueDate;
T: 11/14/2003 8:43:13AM 11/28/2003
.
::
; '
.
Received Date: 11/14/2003
Received By:
AMMEERMAN, MARK1
: . ^:
v ...
.
Spread Sample:
. '^ : :
:V f :
Label:
..... -
Project Title/Type: Analysis of PFOA in OVS Tubes / ROUTINE
"
'
True True True
' ''
^ '
. Login Notes: Conform Notes:
-. ^: , :
Packages / Containers
Package Carton
Mail Date / Condition
Shipper/ ID ' Temp. Control / Temperai
PK0001882
)
11/13/2003 2:00:14PM Package & Contents. Uncompromised
FEDEX 8363913020070200
. RT
: . o.oo
,
: ...
container # Gross Weight
C0019829
7-2 g
C0019830
7.2 g
C0019831-- -- -- TS-g-
C0019832
7.2 g
C0019833
7.2 g
G0649834 --------- - 7.2 g - '
C0019835 ,
7.2 g
C0019836
7.2 g
00010837^--- --
C0019838
7.2 g
C0019839
7.2 g
<30049849------------- ?r2-g-
C0019841
7.2 g
C0019842
7.2 g
G0649843---- -------
COO19844
7.2 g
C0019845
7.2 g
60049846---- ------- 7:2 g~
C0019847
7.2 g
C0019848
7.2 g
CQ019849---------- T-g-.
COO19850
7.2 g
C0019851
7.2 g
eOO19852 ----------- 7r2-g
pH 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. Lot
Direction / Handled By RECEIVED
AMMERMAN, MARK
Mfg. ID
scellaneous Item Key
None
Description
ICOC
0 JI-,O
11/14/2003 Loqin.rpt
Report Version: Nov 13 2003 4:51PM Page 1 of 5
Instance:
R0072755 ill
I* n
.
1 Sample ID ; Matrix
' 001308-0001
GAS
_J001308-0002
GAS
-fe90430&^e03
GAS
L0001308-0004
GAS
L0001308-0005
GAS
L0001300-9000 GAS ;
L0001308-0007 , GAS
L0001308-0008
GAS
L0QQ4-3S88Q99- GAS
L0001308-0010
GAS
L0001308-0011
GAS
-teeo48s=eo42- GAS
L0001308-0013
GAS
L0001308-O14 GAS
^.0004308=8848=- . GAS
L0001308-0016 , GAS
L0001308-0017
GAS
LOOO4308*48'- GAS
L0001308-0019
GAS
. L0001308-0020
GAS
JJlQ0130ae24- GAS
L0001308-0022
GAS
L0001308-0023 . GAS
I 8064308-0024^ GAS
S a m p le s
Fraction OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes : OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes
Sample
WWK-A-AMSFBLK-E2 A
WWK-A-AMSFBLK-E2 B
WWK-A-AMSrDLK'-C2"C ;
WWK-A-AMS1-E2 A
WWK-A-AMS1-E2 B
WWK-AAMS1 C2G
.
WWK-A-AMS2-E2 A
WWK-A-AMS2-E2 B ; V ,
-WWK A AMS2 E2 C------ /
; WWK-A-AMS3-E2 A .
WWK-A-AMS3-E2 B
.
, -WWK-A-AMS3-E2 G -
.
WWK-A-AMS4-E2 A
.
. WWK-A-AMS4-E2 B
WWK-A-AMS4C2 C
WWK-A-AMS5-E2 A
WWK-A-AMS5-E2 B
WWK-A-AMG5C2 e~ .
WWK-A-AMS6-E2 A
:
WWK-A-AMS6-E2 B
-WWK-A-AMGC-C3 C-
Control 1 A
Control 1 B .
Control 1 6 ------ '
Date Sampled Date Received
yj C - s<5cf"1'oi^- .
fc jt'Tr cC~T
LS owly.
11/13/2003 11/13/2003 11/13/2003
11/13/2003
11/13/2003
11/13/2003
11/13/2003
11/13/2003
11/13/2003
11/13/2003
11/13/2003
11/13/2003
11/13/2003
11/13/2003
11/13/2003
11/13/2003
11/13/2003
11/13/2003
11/13/2003
11/13/2003
11/13/2003
11/13/2003
11/13/2003
11/13/2003
Date Due 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003
f
11/14/2003 Login.rpt
057
Report Version: Nov 13 2003 4:51PM Page 2 of 5
Instance:
R0072755
R0072755
\0 0 0 1 308-0001
~ Container
CQ019829 / Other / NONE
Bottles
Method
I' L0001308-0002
I Container C0019830/ Other /NONE
Method
L0001308-0003
K. Container
C0019831 / Other/NONE
Method
| L0001308-0004
Container
| C0019832 / Other / NONE
L0001308-0005
I Container
\ 0019833/Other/NONE
| L0001308-0006
Container
' C0019834/Other/NONE ' ' '
'
..
.
* L0001308-0007
f Container C0019835/Other/NONE
. L0001308-0008
* Container
C0019836/Other/NONE
L0001308-0009
Container
0 0 1 9 8 3 7 /Other/NONE
.
L0001308-0010
Container
C0019838 / Other / NONE
..
.
:
Method Method Method . Method Method Method Method
L0001308-0011
Container
0019839/Other/NONE
)0 0 1 308-0012
Container
11/14/2003 I Login.rpt
Method
Method
r
UGb 6
Report Version: Nov 13 2003 4:51PM Page 3 of 5
instance:
R0072755
R0072755
C0019840 / Other / NONE
0001308-0013
^ Container J0019841 /Other /NONE
,
L0Q01308-0014
Container C0019842/ Other / NONE :
;
L0001308-0015
. Container
-;
C0019843 / Other / NONE
L0001308-0016
Container
v
C0019844/ Other / NONE
,
L0001308-0017
Container C0019845/Other/NONE
-
L0001308-0018
Container ^00019846/Other/NONE
^ `
LO001308-0019
Container 00019847/Other/NONE .
L0001308-0020
Container C0019848/Other/NONE
^
L0001308-0021
Container C0019849/Other/NONE
L0001308-0022
Container C0019850/Other/NONE
L0001308-0023
Container C0019851 /Other/NONE
9001308-0024 J
Container
C0019852/Other/NONE
.
. -
11/14/2003 Login.rpt
Method ,
. : r : Method V -
. . Method
.
Method
-
- . ' Method
'
;
Method
V Method
Method
Method
Method
Method
Method
U0b i
Report Version: Nov 13 2003 4:51PM Page 4 of 5
Instance:
R0072755
R0072755
11/14/2003 Login.rpt
Report Version: Nov 13 2003 4:51PM Page 5 of 5
0 J
instance:
R0072755
R0072755
CHAIN OF CUSTODY/ANALYSIS REQUEST FORM
PROJECT INFORMATION
Client (name & address):
f r D QiYV
.
\VL.cPo.Ar \ AjiXS
Phone: ( Fax: Sampler: U M
\;
.
2\ \ q c 05O
Exygen Research Sample Receiving * 31 17 Research Drive State College, PA 1 6 80 1, USA T: 8 1 4 .2 3 1 .8 0 3 2 F: 8 1 4 .2 3 1 .1 5 8 0 exygenresearch.com
Page
of
ANALYSES REQUESTED
____
Project Manager (Name & E-mail Address):
fYft ' 1U L (Vu CJM
Project Name: ^
f\
iV s f cAX<%vO\'\ iV\. \ f QCyOXcvw
p.o. # :
A r 1 Cr
Quotation #:
Please fill out this form completely to ensure correct analysis and proper handling of your samples.
AMPLE ALYSiSExyLIMS# Client Sample Identification
Collection Collection
Date
Time
.(ad a
Oa M-QoZa-.j.E>vfd>-
uEo
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Z U Specify Matrix
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Comments
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LAB USE ONLY
OF CUSTODY
Relinquished by
Date
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tV /'7
OTHER INFORMATION b A ) ^ i l
Cooler ID # r10 cco Z
Recfliived by
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Cooler Temp. (C) /\4
Date . ' lo W /63
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PROJECT REQREMNTS
Results Deadline:
Laboratory Report Options: I I Sample results only I I Add case narrative I I Add quality control summary I I Add calibration summary [~1 Add raw data d l Other
REV. 3-02
Exygen
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Date & Time Received
' - / / # u t i l i /*
Condition o f Samples
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Initials & Date
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Comments
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May 24. 2002/3
038 Research Drivi' Siate Colli w . PA I WH) I, USA
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