Document pmJYdEjveYdxgELYKOpXpgoJD
AR226-2658
48
RES EARC H
Precise Research. . Proven Results.
AR226-2658
AnaBytical Report
Air Sampling Fluorochemical Report DuPont Washington Works - Air Sampling Program Round 1
Exygen Research Report No. L0001277
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
Page 1 of 7
3058 Research Drive State College, PA 16801, USA
T: 800.281.3219 F: 814.272.1019
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 samplesWere 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.- The fractions were extracted with 1 mL of methanol.
Perfluorodecanoic Acid (C10 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
iResults Summary
. Request #
WWK-A-AMS1-E1 A WWK-A-AMS1-E1 B WWK-A-AMS1-E1 C WWK-A-AMS1-E1 (Total)
WWK-A-AMS2-E1 A WWK-A-AMS2-E1 B :
,
WWK-A-AMS2-E1 C
WWK-A-AMS2-E1 (Total)
WWK-A-AMS3-E1 A WWK-A-AMS3-E1 B WWK-A-EMS3-E1 C
,
WWK-A-EMS3-E1 (Total)
WWK-A-AMS4-E1 A
.
WWK-A-AMS4-E1 B WWK-A-AMS4-E1 C WWK-A-AMS4-E1 (Total)
f
WWK-A-AMS5-E1 A
WWK-A-AMS5-E1 B WWK-A-AMS5-E1 C
WWK-A-AMS5-E1 (Total)
WWK-A-AMS6-E1 A WWK-A-AMS6-E1 B WWK-A-AMS6-E1 C WWK-AAMS6-E1 (Total)
Air Volume Sampled (L)
1407 1407 1407
1410 1410 1410
1418 1418 1418
1397 1397 1397
1418 1418 1418
1482 1482 1482
.
:
C8Acid (mg/m3)
<0.00007 < 0.00007 < 0.00007
<O.OQ.O.,14
0.00007 < 0.00007 < 0.00007
0.0.0.007
0.00008 < 0.00007 < 0.00007 0.00008
.
< 0.00007
< 0.00007
< 0.00007
< 0.00014
< 0.00007 < 0.00007 < 0.00007
< 0.00014
< 0.00007 < 0.00007 < 0.00007 < 0.00014
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
ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 3 of 7
. OC Data
,'
'
!
^
!
11
''1/
; !1
.
,
,.
1
1,
.,....'' LCS
'
'
.
'
'
; 1- 11
' '.' ".. ." ' "
.
'.
.
11
'
'
'
.
. . . ' Please note: One control sample was spiked with each perfluorooctanoic acid to give a final concentration of 500 ppb
through the tube at a rate of 1-liter per minute for one hour (480 liters of air). The fractions were separated and analy
acceptable range for control recovery is 75-125%. ,,
Request # Control 1
CBAcid (amount spiked - ppb)
500
C8 Acid
(amount recovered 509
ppb)
C8 Acid
(percent recovery 102
Blanks
Request # WWK-A-AMSFBLK-E1 A WWK-A-AMSFBLK-E1 B WWK-A-AMSFBLK-E1 C
Vol. Of Air (L)
.
0
0
1:.' '.0 . . !' . -
CSAcid . (ug/fraction)
<0.10 <0.10 <0.10
ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH
Page 4 of 7
Surrogates
.
'
,
''.
.
: ''
.
A surrogate spike (C10 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-E1 A WWK-A-AMSFBLK-E1 B WWK-A-AMSPBLK-E1 C
WWK-A-AMS1-E1 A WWK-A-AMS1-E1 B ... WWK-A-AMS1-E1 C WWK-A-AMS2-E1 A 'WWK-A-AMS2-E1 B WWK-A-AMS2-E1 C WWK-A-AMS3-E1 A .WWK-A-AMS3-E1 B WWK-A-AMS3-E1 C WWK-A-AMS4-E1 A WWK-A-AMS4-E1 B WWK-A-AMS4-E1 C WWK-A-AMS5-E1 A WWK-A-AMS5-E1 B WWK-A-AMS5-E1 C j WWK-A-AMS6-E1 A WWK-A-AMS6-E1 B WWK-A-AMS6-E1 C
Control Spike A Control Spike B Control Spike C
Amount Spiked (Ppb)
500
500
500
500 500
500
500
500
500
500 500 500
.500
.
500
500
500
500
500
500 500
500 1000 *
500
500
Amount Recovered (PPb)
663 -
345
:
393
561
384 '
359
668
423
411
:. .
..
691:-
-
417 418
..
774
384
382
643
358
407
825
397 .
442
'
1196
349
385
Percent Recovery ' (%)
133** 69**
79
11.2
77
72**
134**
:
85
82
:
138**
;... '.' S3-'- ;,
84
. .155**. 77
76
129**
; -72**'
81
;
165**:
79 .
88 120 70 **
77
* The control spike A Fraction was inadvertently spiked twice with surrogate. The surrogate concentration for this sample is therefore 1000 ppb.
** Surrogate recovery outside of advisory range.
ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH
Page 5 of 7
Calculations
Request #
WWK-A-AMSFBLK-E1 A WWK-A-AMSFBLK-E1 B WWK-A-AMSFBLK-E1 C
WWK-A-AMS1-E1 A ,WWK-A-AMS1-E1 B WWK-A-AMS1-E1 C
WWK-A-AMS2-E1 A WWK-A-AMS2-E1 B WWK-A-AMS2-E1 C WWK-A-AMS3-E1 A WWK-A-AMS3-E1 B WWK-A-AMS3-E1 C WWK-A-AMS4-E1 A WWK-A-AMS4-E1 B WWK-A-AMS4-E1 C WWK-A-AMS5-E1 A WWK-A-AMS5-E1 B WWK-A-AMS5-E1 C ; WWK-A-AMS6-E1 A WWK-A-AMS6-E1 B WWK-A-AMS6-E1 C
Control Spike A Control Spike B Control Spike C
Vol. Of Air (L)
0
0
0
1407 1407 1407 1410 1410 1410 1418 1418 1418 1397 1397 1397 1418 1418 1418 1482 1482 1482
0
0
0
. C8 Acid
(raw-ppb)
<10 <10 <10 <10 . <10 <10
101
<10 <10
105
<10 <10 <10 : <10 <10 <10 <10 <10 <10 <10 <10
509
<10 <10
C8 Acid (ug/fraction)
<0.10 <0.10 <0.10 <0.10 <0.10 <0.10
0.10
<0.10 <0.10
0.11
<0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10
0.51
<0.10 <0.10
C8 Acid (mg/m3)
< 0.00007 < 0.00007 < 0.00007 0.00007 < 0.00007 < 0.00007 0.00008 < 0.00007 < 0.00007 < 0.00007 < 0.00007 < 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-E1 A C8 Acid,
[101 ng/mlofC8Acidx(l ml) x (I ug/ lOOOng) x (1 mg/ lOOO.ug) ] / [(1410 L) x (1 m3 /
WOOL)]
: :: ,',
' ,
/
0.00007 mg/m3
,
/' ,
Signatures
Paul Connolly, LCMSTeam Leader ^.
^ / / ^ ^ y /dohn M. Flaherty, Vice President
Other Lab Members Contributing to Data James Miller
Z)tS/Ot-i
Date
-K
Date
ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 7 of 7
able 1. Login Information / Fieid Data
Sample ID
Exygen Lab ID
WWK-A-AMSFBLK-E1 A WWK-A-AMSFBLK-E1 B WWK-A-AMSFBLK-E1 C
WWK-A-AMS1-E1 A WWK-A-AMS1-E1 B WWK-A-AMS1-E1 C WWK-A-AMS2-E1 A WWK-A-AMS2-E1 B WWK-A-AMS2-E1 C WWK-A-AMS3-E1 A WWK-A-AMS3-E1 B WWK-A-AMS3-E1 C WWK-A-AMS4-E1 A WWK-A-AMS4-E1 B WWK-A-AMS4-E1 C WWK-A-AMS5-E1 A WWK-AAMS5-E1 B WWK-A-AMS5-E1 C WWK-A-AMS6-E1 A WWK-A-AMS6-E1 B WWK-A AMS6-E1 C
Control Spike A Control Spike B Control Spike C
L0001277-1 LOOO1277-2 L0001277-3 L0001277-4 L0001277-5 L0001277-6 L0001277-7 L0001277-8 L0001277-9 L0001277-10 LOO01277-11 L0001277-12 LOO01277-13 L0001277-14 L0001277-15 L0001277-16 L0001277-17 L0001277-18 L0001277-19 L0001277-20 LOO01277-21 LOO01277-22 L0001277-23 L0001277-24
Date Received Description
Air Volume Sampled (L)
11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03
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 1 st 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
0
0 0 ,
1407 1407 1407 1410 1410 1410 : 1418 1418 1418' 1397 1397 1397 1418 1418 1418 1482 1482 , 1482
0
0
0
.' ".'
.
ogin
Login #:
LOG01277 > 1,387
:
--
,
Conform COC Sample: true
Project:
P0000419 .
: ;
"
--
^
? Conform COC:
True
Project Title/Type: Analysis of PFOA in. OVS Tubes / ROUTINE
.
Conform Sample:
True
.
Project Storage:.
:: ;
;
Conform Request:
True
Submitted By:
Michael D.Aucoin
Status:
Unreceived
Login Type:
Immediate Receipt of Samples
Started: Date Start:
T'
.
'
.,-
11/7/2003 2:41:35PM
Due Date:
11/21/2003
Received Date: 11/07/2003
Received By:
ROBB, SHAWM
Spread Sample:
Label:
Login Notes: Conform Notes: "
Package
Carton
Mail Date / Condition
Packages / Containers
. Shipper/ID
Temp. Control / Temperat
PK0001842
lass.
i^';?A
,
"
'
'
'
' . 11/7/2003 10:40:51 PM
Package & Contents Uncompromised
'
..'
'
.
FEDEX
8363913020300200
-
-
.
NONE
container #
1018656 C0018657
C0018658 C0018659 C0018660 C0018661 C0018662 C0018663 C0018664 C0018665 C0018666 C0018667 C0018668 C0018669 C0018670 C0018671 C0018672 C0018673 C0018674 C0018675 C0018676 C0018677 C0018678 C0018679
Gross Weight
7.2 g 7.1 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g
jgH
'
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 ROBB.SHAWN
Illllpiscellaneous
Item Key None
11/7/2003 Login.rpt
ICOC
Description
0066
Report Version: Oct 23 2003 9:55AM Page 1 of 5
Instance:
R0072027
^ 8561113935
ogin
Sample ID L.0001277-0001
1-0001277-0002 001277-0003
1.0001277-0004 L0001277-0005 L0001277-0006 L0001277-0007 L0001277-0008 L0001277-0009 L0001277-0010 L0001277-0011 L0001277-0012 L0001277-0013 L0001277-0044 L0001277-0015 L0001277-0016 L0001277-0017 L0001277-0018 L0001277-0019 L0001277-0020 L0001277-0021 L0001277-0022 L0001277-0023 L0001277-0024
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
Fraction OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes , OVS Tubes OVS Tubes OVS Tubes
OVSTubes OVS Tubes OVS Tubes OVSTubes OVSTubes OVSTubes OVS Tubes OVSTubes OVS Tubes OVSTubes OVSTubes OVSTubes OVSTubes OVS Tubes OVSTubes
Samples
Sample
WWK-A-AMSFBLK-E1 A
WWK-A-AMSFBLK-E1 B
WWK-A-AMSFBLK-E1 C
WWK-A-AMS1-E1 A
WWK-A-AMS1-E1 B
:
.
WWK-A-AMS1-E1 C
;
"
WWK-A-AMS2-E1 A
WWK-A-AMS2-E1 B
WWK-A-AMS2-E1 0 .
. .
WWK-A-AMS3-E1 A
WWK-A-AMS3-E1 B
WWK-A-AMS3-E1 C
WWK-A-AMS4-E1 A
WWK-A-AMS4-E1 B
WWK-A-AMS4-E1 C
WWK-A-AMS5-E1 A
WWK-A-AMS5-E1 B
WWK-A-AMS5-E1 C
WWK-A-AMS6-E1 A
:
WWK-A-AMS6-E1 B
WWK-A-AMS6-E1 C
CONTROL A
CONTROLS
CONTROL C
Date Sampled Date Received 11/07/2003
Date Due 11/21/2003
11/07/2003
11/21/2003
11/07/2003 . 11/21/2003
11/07/2003
11/21/2003
11/07/2003
11/21/2003
11/07/2003
11/21/2003
'
11/07/2003
11/21/2003
11/07/2003
11/21/2003
11/07/2003
11/21/2003
11/07/2003
11/21/2003
11/07/2003
11/21/2003
11/07/2003
11/21/2003
:
;
11/07/2003
11/21/2003
11/07/2003
11/21/2003
11/07/2003
11/21/2003
11/07/2003
11/21/2003
11/07/2003
11/21/2003
11/07/2003
11/21/2003
11/07/2003
11/21/2003
11/07/2003
11/21/2003
11/07/2003 . 11/21/2003
11/07/2003 11/07/2003
11/21/2003 : 11/21/2003
11/07/2003
11/21/2003
11/7/2003 Login.rpt
.' U067
Report Version: Oct 23 2003 9:55AM Page 2 of 5
Instance:
R0072027
^
J001277-0001
Contaiher "0018656 /Other /NONE
L0001277-0002
Container C0018657/Other/NONE
L0001277-0003
Container C0018658 / Other /NONE
L0001277-0004
: Container
C0018659 / Other / NONE
L0001277-0005
Container C0018660 / Other/ NONE
L0001277-0006
4lgg||t' Container
(IS||;001866/ 1Other / NONE
'^^
-
-
.
.
.
I 01277-0007
Container C0018662 / Other / NONE
L0001277-0008
Container C0018663 / Other / NONE
L0001277-0009
Container C0018664 / Other / NONE
L0001277-0010
Container
C0018665 / Other / NONE
L0001277-0011
Container C0018666 / Other / NONE
'lUlo 1277-0012
Container
11/7/2003 Login.rpt
ogin
Bottles
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Report Version: Oct 23 2003 9:55AM Page 3 of 5
U 0 6 Q
Instance:
R0072027
^ 037942312834
C0018667 / Other / NONE
1001277-0013
Container C0018668 / Other / NONE
L0001277-0014
Container C0018669/Other/NONE
L0001277-0015
Container C0018670 / Other / NONE
L0001277-0016
Container C0018671 / Other / NONE
L0001277-0017
Container C0018672 / Other / NONE
L0001277-0018 '^(Kiii\ljC O! OC^oynS/taOitnheerr / NONE
' W1277-0019
i
Container
C0018674 /Other / NONE
L0001277-0020
Container C0018675/Other/NONE
L0001277-0021
Container C0018676/Other/NONE
L0001277-0022
Container C0018677/Other/NONE
L0001277-0023
Container C0018678 / Other / NONE
|||001277-0024
Container
11/7/2003 Login.rpt
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Report Version: Oct 23 2003 9:55AM Page 4 of 5
u06^
Instance:
R0072027
22126412
C0018679 / Other / NONE
11/7/2003 Login.rpt
Report Version: Oct 23 2003 9:55AM Page 5 of 5
U070
Instance:
R0072027
R0072027
CHAIN
OF
tUSTODY/ANALYSIS . .V^y
.
.
REQU
RESEARCH
PROJECT INFORAAATION
Exygen Research Sample Receiving 3117 Research Drive State College, PA 16801, USA
'
T: 814.231.8032 F: 814.231.1580 exygenresearch.com
-
ANA
Client (name & address):
ADa.AA B.jgA-t-- Wt>ii^-^
^vat-^^
Phone: Fax:
[3^) ^a-Wi^
Sampler: .^So^^J^M^IPrAP;
Project Manager (Name & E-mail Address):
. /Wk: A^toiA
Project Name:
_____/\^r
RO. #: Quotation #:
1
5^^'/-)<i-i--^)-
h
rfoif^d^
Please fill out this form completely to ensure correct analysis and proper handling of your samples.
DuPon^Washington Works Air Sampling Program
Sampler(s):
SO, AC RK.L.K
FedEx Airbill #: ^3W\W30
Event Number
iiW^iffitlp^il 669842 669908
669878 , 669831 669769 669865 Hours
0
1
2
3
4
AMS-1 AMS-2 AMS-3 AMS-4 AMS-5 AMS-6 Minutes
0
60 120 180 240
WWK-A-AMS1-E1 WWK-A-AMS2-E1 WWK-A-AMS3-E1 WWK-A-AMS4-E1 WWK-A-AMS5-E1 WWK-A-AMS6-E1
Hours
5 6 7
8 9
^IiiMpiS|l
j.OOT
n-5-rf5
l.oil
1.01%.
ii-^17
(<-5'->
1.011
LOli
I. e>f>
Minutes
K-J-0^ ll-J-0^ I(-5-^ Hours
300
10
360
11
420
12
480
13
540
14
w^ QC.Q1
n<oA?
QW^
0w&M^3
Minutes 600 660 720 780
840
|S|@M IBili^BillWI
Jl^kl. o^n^ o 3.\\\
o^^/ o.^^lS
o5^ O^WO
OufO'^ O^^Q .
0531
o^("4'^-oA
-
^
<nbL ^
ft.l<eoo0
He3urs Minutes
Hours
15
900
20
16
960
21
17
1020 ;
22
18
1080
23 :
19
1140
24
<
Field Blank:
1^
yes or no
WWK-K-AMSFBLK-E1
Weather: f ^ Clo^y CxfeM tilu^Ws> ^^0
"' - ' '.' "' .. ''' '
1'',
SAFER operational:
Comments:
c.
Q
'<! (-V-.
^
yes or no
''
'
'
'
'. . ,' " '' .
'
.
11/4/2003
Page 1 of 1
Washington Works No Charge Shipper
Ship to:
Exygen Research '3058 Research Drive State College, PA 16801
Attn: Shawn Robb or John 814-272-1039
Flaherty
Phone Number;
Date: 10/27/2003
NCS #: 38-200304715
Routing; FED EX ( SEE ABOVE ACCT)
F. 0. B.; COLLECT
Date Shipped:
B/L;
,
, '' ... .
Quantity
1
Product Code / Description
Box containing glass sample tubes for analysis
Weight
10
Units
Ibs.
Freight Class: TUBES, GLASS, N01. Originator; Crane, Alison A Cost Code; 7035-507483-862200 Purchase Order #; Value for Customs;
Dimensions; Ship From; Stores
Status;
Phone:4448
Hazardous Shipment? No 0
MSDS Sheets Required? No
Material Class: D Corrosive D
D Toxic
D
Shipping #;
Yes
0 Yes
Flammable Other
u07 5
Special Instructions; This N-C-S will cover 6 shipments beginning 10/30/03.
Will deliver package to Stores with completed FEDEX Bill.
> Weekend samples will be delivered directly to FEDEX.
Comments;
"''''.^:':"^'/\:. '.. "'^
CRG Account Number 2230-5551-6.
'.' ' ' '.
U074
.g fk^USAMrbill
1 Fi-rom
,
631,3^^050:30
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it^V Next business moming ;
,
Pac
. OeJiverycQmmilme
_i~_l FedEx Standard Overnight
--' Men business afternoon
HI FedE
I--J Easie delive
'
Sender's Name
Company
Address
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