Document O13RJO3vbRdoedjBg8b4yaELX
Gril Company ASAI 6LAS5 0.170.
MR 277 Y35--
[Company sanitized ows
ACC Asai GlsCo,Lit Does not contain TSCA CBI.
ssawaursscow 10.Goikaigan, Iehibarahi, Coiba 290-8566, Japan
Characterization of a Polymeric Product (AAA) by Asahi Glass
Study director (Question to:)
To<uguh-idL e Ia scmm uraan) Senior Manager
QAunaalliyttiycAalssTuercahnncoelOofgfyicGeroup
Chemicals Company, AsahiGlassCo,Lid.
10, Goikaigan, Ichihara-shi, Chiba 290-8566 Japan
Phone: +81.436.23-3183 Fox: +81.436.23.3126 E-mail: tsuguhide-isemura@agecop
July 05D,at2e004.
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Chemicals Company, ASAHI GLASS CO.,LTD.
04705
L Substance name and TRP Identification# (for Noack shipment) ofthe polymeric product
Substance name: AAA Lot. XXX (TRP Identification #: BBB)
AAA Identification #.
Lot. XXXX was purified for biodegradation test and named AAA CCC). The purification process and characterization of AAA purified were
purified detailed
(TR in the
report"
2. Characterization of the polymeric product 2:1 Size exclusion chromatography (SEC)
SEC of the polymeric product for molecular weight analysis was conducted according to OECD gwiutihdetlhienepsu'rifiaenddpotlhyemerres.ulHtewraesthsehoanwanlytiincatlhempertehvoidousalnyd sruebsumlitttaerde ormeiptorite"d ienxccleupstivfeorofthteheiscoolmatpiaorniasnodn preparation ofhe polymer from the produc,
2-1-1 Isolationof the polymer from the product
product
At first the polymeric product was and 5 mi of isopropanol was mixed ina
shaken well for homogenization. 1 centrifuge tube and shaken well The
ml of the polymeric precipitated polymer
was separated by centrifugation (6,000 rpm, 10 min) and following decantation. The precipitate was then
dried in vacuum condition for 20 hours in room temperature. The isolated polymer was dissolved in the
mobile phase by 0.75 wi% by shaking for several minutes and stand for overnight, The solubility of the
polymer was sufficient: no precipitation or insoluble fraction was observed and the solution looks
completely transparent,
2:2 Determination ofPFOA in the polymeric product
The method validation Attachment 1of tis report,
and
determination
in
this
section
was
conducted
according
to
the
22:1 Test and control substances
standard,
"The test substance, pefluorooctancic acid (PFOA, 98.9 &-hydrohexadecafluorononanoic acid (9H-PFNA, 97.85%,
%, lot.
lo. CIT001401), and the surmogate CS8002501), were purchased from
Daikin Fine. Chemical (Osaka, Japan). Distilled water was produced in-house and checked for
contaminants by LC/MS before use. Distilled water was filtered heough a pre-column, Preclean-ORG (GL
Sciences (MeOH),
Inc. (Tokyo, reagent grade
Japan) ethanol
placed (EIOH)
between HPLC and isopropanol
pump (IPA),
and and
auto-sampler. reagent grade
HPLC grade methanol ammonium acetate were
purchased from Kanto Chemical Co. In.
ammoniumInaocretdaetretsoolauvtoiiodn cwoanstapmrienpaatrieodn,bydiwsepiogshaibnleg l1a5b4wmagreof(taubmems,onpiipuemttaec,eteattce) awnadsduissesdo.lv2inmgmionl1/1L
of distilled water,
`Chemicals Company, ASAHI GLASS CO, LTD.
oars
2:2:2 Preparation of fortification standards distilled w50au/gte/tmhiaenaonlr)d. 11000mugg//mmll 8P-F2OalAcoshoollutsioolnutwiaonswparsepparreepdaruesdinugsiangsoilsvoepnrtop(a2n/o8l ((IwPiA)) fmoirxtsuorlveenotf for the use of later section (2-3). 22:3 Preparation ofa surrogate standard ethanol). 100 ng/ml 9H-PENA solution was prepared usinag solvent (1/1 (wt) mixture of istiled wate/r
2:2:4 Preparation of calibration standards
each solut0i,o0n.a1n,0d.29,m0.o4fm1l0o0fntgh/eml1090Hu-gP/EmlNAPFsoOluAtisoonluwtaiosnmwiaxseddiilnutaedvibayl.IAPbAouutp t1om5lmo.f e1a0c0huslolouftitohne
was filtered through a 0.2 yum filler, injected twice into LC/MS conditioned
Milex-LG as follows.
(MILLIPORE,
U.S.A),
ino
an
auto-sampler
vial
and
2:2:5 ExtractionofPFOA from the polymeric product
to homogenBiezfoertehethpeoslaymmpelriicngproofdutchte.po1lmylmeorficthperpoodluyctmetrhicypwreordeucsthwaakesnpwuetllinweiatchhouotfgfeonuerrcaetnitnrgifbuugbabtlieosn
vis. Fortification of PFOA and 8-2 alcohol were conducted as listed in Table 1. Fortification of 82
alcohol was conducted fo with fortification solution
the was
use of 5 mi.
later After
section puting
(2-3). a Ji,
IPA each
was added into all of five vials (with
vials uni otal the blank) was
amount shaken
vigorously and the precipitation ws separated by centrifugationat6000 rpm for 10 minutes, About 3 ml of
each supematant was dealt out fo 8-2 alcohol determination by GC.
About
1
100 ul of ml of each
the cach solution
supernatant was filtered
and 9ml through
of the
100 0.2
ng/ml SH-PFNA solution was um fir into an aut-samplr
mixed in a vial. vial and injected
into LC/MS conditioned reproducibility.
as
follows
These
procedures
were
repeated
once
again
for
the
verification
of
the
"Table 1 FortificationofC8 precursors and PFOA
Sample
Fonification
CL 0mpmis2acol moa
Ta
ou Cow
B
soul
10001X 50 ug/ml
c
100
100 WX 100 g/m
200m
200 1 X 100 pgm
22:6 LOMS analysis LC/MS analysis ws conducted with the conditions listed below.
Chemicals Company, ASAHI GLASS CO, LTD,
040705
<Instruments>
(yLems HPLC Mass spectrometer
(2)LC column @rc (@) Software (5) LOMS vial
Agilent Technologies, Model 1100 Agilent Technologies, Model 1100MSD (SL) Imtak (Tokyo, Japan), cadenza CD-C128 mm (diameter) X 100 mm Hewlett Packard Kayak PC Workstation OS: MS-Windows NT 4.0 LC/MSD ChemStation, Rev. A. 08. 03 2m vial for auto-samplr, Chromatography-Convenience 400-C80, Tomsic (Tokyo, Japan)
<Analytical conditions> (1) Column temp. (2) Mobile phase
(3) Gradient condition
@) Flow rate (5) Injection volume (6) Retention time
sc A:2 mmol/L ammonium acetate B: Methanol time/min 05> 2 515 15015 25 BS ST3575 1005100557 557 0.3 m/min SL PFOA (4.3 min), 9H-PFNA (2.5 min)
<MS operating parameters>
(1) Tonization mode Electrospray (ESI) (negative ion mode)
(2) Fragmentor voltage ~~ 100V.
(3) Ton monitored
miz =413 (CF15C00'), 445 (CEH(CF:),C00)
(4) Desolvation temperature 350C
(5)Nebulizergas
N
(6) Desolvation
N: 12 Limin
22.7 Resulis
Of
(peak
Twocalibration curves for area of mz = 413) / (peak
standard area of
addition method m/z = 445) as a
are plotid and shown in vertical axis against the
Fig. 1 for the ratio amount of PFOA
faonrdtiftihceataimonou(nitgs) oasf aPFhoOriAzodnettaelramxiins.edThien ctoheeffpiocliyemnetsroifccporrordeulcattiaornea(reCBmIo)repptmhanan0d.9(9C9B0I)foprbpomth(cauvrevreasg,e
(CBD ppm). (CBI) ppm is equivalent to (CBI) molkg (specific gravityofAAA is (CBI).
Fig.
1.
`Two PFOA
calibration curves for is not detected (zero
PFOA count)
calibration standards are shown for 0 ug standard (blank). The
in Fig. 2 for the coefficients of
same axis with corelation are.
more thn 0.9995, and the recovery defined as (th slope for the standard addition) / (the slope for the
Chemicals Company, ASAHI GLASS CO, LTD.
040705
calibration standards) recovery satisfied the
was 955. All the criteria stipulated
linearity of the calibration in the attachment 1.
curve,
reproducibility
of
the
resul,
and
(CBI)
[C3]
Fig.1 Calibration curves for AAA by standard addition method
Fig. 2 Calibration curves for PFOA. calibration standards
Chemicals Company, ASAHI GLASS CO, LTD.
040705
2-3
Deter"Tmhienmaettihoondovfal8i-d2aatilocnoahnodldaetnedrmiCn8atpiroencwuarssocrosndiuncttehde
polymeric product according to the Attachment
1
of
his
report for 8:2 aleshol. C8 precursors other method us4cialibnratigon standards, and not
than 8:2 evaluated
alcohol were determined by by standard dition method,
absolute
calibration
2:31 Test and contol substances
further
"The test substances purification process.
used
in
ths
sction
are
listed
in
Table
2.
These
substances
were
used
without
Standards
Table 2 The test substances used in 2:3 Origin
Purity by GC
2 acon
Reagent grade, purchased from
Dakin fine chemical (A-1820 ot, A18202601)
82acrylte
Received from Seimi Chemical Co,, Lu. (Kanagawa, JAPAN)
9.71 (FID area)
820lein
Prepared in-house
99.75 (FID area)
CO th iodide
Reagent grade, purchased from Dakin fine chemical (11820 ot. 118200701)
--CH -- iodide
PPereppaerdediinn-hhooussee
8897.77((FDIDaamreaa)n
23:2 Preparation of fortificationandcalibration standards
listed
in
Mixture Table 3,
solutions
of
8-2
alcohol
and
C8
precursors
were
prepared
using
IPA
as
2
solvent
as
`Table 3 Preparation of 8-2 alcohol and C8 precursor standard solutions
Standard
_2alcohol
82acrylale
82olin
C8 ethyl iodide
g/ml IPA solution CS odide
A B
10
10
10
EY
50
50
10
1
s0
5
-- X c> 3050000 0 300000 ss30o000w 0 s3sw000e00 33m500
2:3:3 Extraction ofC8 precursors rom th polymeric product Extraction proceduresof8-2 alcohol and C8 precursors are explained in 22.5,
23:4 GC analysis GC analysis was conducted with the conditions listed below.
Chemicals Company, ASAHI GLASS CO, LTD,
00705
<Instruments> WGems
Gc Integrator (2) GC column (5) Auto-sampler vial
HP S890 series Il with auto-injector HP 3396C (CBI) 2m vial for auto-sampler, Chromatography-Convenience 400-C80, Tomsic (Tokyo, Japan)
<Analytical conditions>
(1) Injector temp.
20C
(2) Oven temp.
40C (2 min=)> 10 *Cimin 5 170 C (0 min) >30 *C/min
(3)
Transfer
line
temp.
~~
> 250C 250C
(10
min)
(4) Column top pressure 15 psi constant
(5) Split flow
50 mmin
(6) Injection volume wl
(7) Carrer gas.
He (99.995)
(8) Retention time (Rt, min)
Re: 12:2 min (8-2 alcohol) RE 14.4 min (8:2 acrylate) Ri: 5.4 min (8-2 olefin) Ri: 13.0 min (C8 ethyl iodide) RE 7.4 min (C8 iodide)
2:3:5 Results
poted andCaslihborwantiionn Fcigu.rv3e.sTfwoor dceutrevremsinfartoimondiofefr8e.n2t raulncso,howlhiicnhAiAncAludbeythsetadnidfaerrdenatddpirteitorneamtemtenhtodrunasr,e
prpreeoadkruecaptrroadu(c7i%b)lae.ndSutrhetohgoartiezosnttaanldaaxridsisisnfootrutsheedaminouthnits (seucgt)ioonf,8t-h2eraelfcoorhe,olthfeorvteirfiteidcatloatxhies mislfporolGyCmeFrIiDc.
Thre equivalent axis
calibration with Fig 3.
curves That i,
for the
8:2 alcohol calibration sandards horizontal axis of Fig. shows the
are shown amount in
in Sm
Fig 4 for the IPA, which is
eaqiubarlaitoonthceuravmeosufnotr cianlimbrlatipoonlystmaenrdiacrdpsrofdorucCt8spurpepcousrisnogrstahraet sthheowrnecionvFeirgys,is5-51,00%. In the same way,
provided
[The results are armanged in the Attachment 1.
in
Table
4.
All
the
reproducibility
and
recovery
satisfied
the
criteria
Chemicals Company, ASAHI GLASS CO, LTD.
oi70s
C2)
Fig. 3 Calibration curves of 8-2 alcoholby standard addition method
o"no [I JE O qsxmeDntOO ORS iit A |
sFES 0LT0 O cl 5oiema on
20 , E[RedtEael GeSE ] Le
or Aga
TE
rE
0 ac w cwmswoowncow ew
Fig. 4 Calibration curvesof 82 alcohol calibration standrds.
on i
os
Fy OeDImasi T aE l rR] Sma BL a
PTe an I [ELEBE e SaR rcoutem A TLE Je
g a | TwET mRY|L Ee RAA a 0p)Rd
cn
aa
0 Am 20acrwycococsenwaenuwgo5 miL1oAm) roo awe
Fig. Calibration curves of 8-2 acrylate calibration standards
9.
ChemicalsCompany, ASAHI GLASS CO,LTD,
00705
on 2" os aTseaetthme gZo gacls
y=asomo2 aor veoomRo=ue0.s99.9a95m4ount
R=099909
om
| @Stainmtei |
on 0
J
D0 wSw2owkotmwcwnc0ngoSrwtuotnoynw vo woo
Fig. 6 Calibration curvesof 2 olefin calibration standards
J Inte Ty
ao
|
.
Ln a heats aii
i
a2oo [20
0
i
EE
Sai BE
pT p F AiL thik]
data
a seam
Chalo a
et wa oA m E aS2m0 aE mHwNnE oePinw5S wH10om)
RA mo
Fig. 7Calibration curves of -2 hy ide calibration standards
L faim T 300m come
ff[0ou0F0mn8|a| HHeSRmET BR Tme e aEn me E e o Si Ysoune
ee Ta |
Som owCoitw coct1u1w5ammeaw mnge we we Fi. Calibration curvesofC8 cide calibration standards
Co.
ChemicalsCompany, ASAHI GLASS CO, LTD,
owns
E mMcEe s[esEarRer ,-- -: TT Ta Table 4 Result of determination for 8-2 alcohol and C8 precursors
2-4 WeighBett%orestohleidasnalysis, weig df fo colin ina desiccator
hin for
gb 15
ots wer rid minis, Abt
1in a0ovpeolseytmaetr12p0rodCufoc
wmsorseitghhaned3
0 mines prc,
dinetosaiwerighfoirng15bomlienutfese. Tmihxinwgeiwgehli.ngThbisoot lwaswawseipguhteid tanhdotvheensfoloird choonutresn,tansdsficesotcoo, To.2
resultwas(CBI)%.
.
Chemicals Company, ASAHI GLASS CO, LTD,
040705
2:5 Determinationoftotal inorganicfluoride
preament T2otalcoimnboursgtainoicn,Muoisriddee,tetrhmeianmedounbty ouflfilaufoirildieatcoonntaoifnitnhgeinpotlhyempeorliycmeprriocdpurcotduacntdwistuhbosuetquseuncth
determination lailation
using ion membrane.
chromatography. Afer fiation,
At 1
first, mi of
2 ml the
of the polymeric polymeric product
product was (containing
fered using practically no
polymer) was diluted by 4 ml ofdistilled water and injected nto anion chromatograph conditioned below,
2:5:1 Apparatusand conditions
Ultrafiltration
Membrane <lon Chromatography>
ADVANTEC
Ultra Filler Unit USY-1
Ton chromatograph
Dionex DX-500
Column
Ionpack AGIIHC x2
Mobile phase
KOH aq
Flow rate
1.0 ml/min
Gradient condition
time/min 0553 717205 30
Injection volume
BmM 2323603605 25 2 S01
Suppressor
ASRS
Detector
`Conductive Detector
2P:5:2roceofddeteurmirnateion
potassium
Absolute fluoride.
calibration curve Fluoride content of
of the
fluoride was generated for calibration polymeric product was determined using
standards consist of this calibration curve
by absolute calibration method.
2:5:3 Result Fluoride was determined to (CBI) ppm in AAA.
2
Chemicals Company, ASAHI GLASS CO,, LTD,
00705
2:6 Determinationoftotal organicfluorine (TOF)
by determiTnOatFiownabsyoobaninchcrdombaytocgormabpuhsyt.ioAnt-pfyirrsot,hysdbrooultys2i0,mfgluoofridteherpaoplyimnetoriacquperooduusctalwkaalsinhee,aftoeldloowneda
hot plate Se at 120 C for 30 introducedinto a combustion-F
minutes. Then, known amount ion analyzer conditioned belo,
(2-3
mg)
of
the
posymeric
product
way
< Apparatus and conditions > Instrument (cal)
Combustion conditions. (cy
Ton chromatography conditions Column Mobile phase Injection volume Suppressor Detector
Tonpack AGI2+AS12 (Dionex) 2.7mM Na.CO+, 0.3 mM-NaHCO, 10 uL. ASRS `Conductive Detector
<Procedure of determination
standards
(Calibration consist of
curve of potassium
fflluuoorriiddee. waTsOFgeonferasttaenddaursdinpgolayn(eironaicuhorroomtahtyolgnrea)phy(PTfoFrE,caplirberpaatrieodn
ofhineshetoaundsdeeat)redrwmaPisTnFeoEdb.tuasiinnegdtnhedcacloimbpraatrieodn wciutrhvhbeytahbesoroeltuitcalcavlaiblruaetioofn7m6ewtihso,d TanOdFcoofttchteepdolbyymethreicrepcroovdeurcyt
<Result>
93:5%.
TOF of standard TOF of AAA was
PTFE was 71.1%. Therefore the recovery of (CBI and comecte o (CBI usin the
the combustion was recovery of standard
ealulated to PTFE, TOR
canadlutlhetoerdetifcraolmvatlhueescowmeproesiitnigoonodofagthreeepmoelnytmefroricthperpoodulcytme(rtihceoprreotdiuccatl, amount) were (CBI, Empirical
3.
Chemicals Company, ASAHI GLASS CO, LTD.
00705
2.7 Calculationoftotal carbon of Atiachm"eTonttal2.caCrabrobnoin ctohnetepnotlyimsecrailccuplratoeddutcoi(sCeBstIi)m,ated by caleultion based on the sample calculation
2-8 Calculationof Molalityof 8-2 alcohol elutionMooflAaiayocfh$e2na3l.coMhoollaliinttyhoef8p-o2lyamlecroihcolpriosdcuacctulssteestditmoat(eCdBb)ymcaallciukl.ation based on he sample
3. References
"Purification and 07,2004, contains
characterization TSCA CBI
of
purified
Telomes
polymer
by
Asshi
Gass,
submited
to
EPA
onMay
* OECD guidelines 18 (`Determination `Weight Distribution of Polymers using Gel
of the Number.Aversge Molecular Permeation Chromatography")
Weight
and
the
Molecular
* OECD guidelines 119 (`Determination Permeation Chromatography")
of
Low
Molecular
Weight
Content
of
a
Polymer
using
Gel
* IemuraT,.et.al J. Chromatogr, Vol 1026/1-2, pp 109-116,(2004)
Se
Chemicals Company, ASAHI GLASS CO, LTD,
040705
Attachment 1 - Validation Example
Cme8tphroedcucrasAnorssbieimnepmlpepollvoyamylieedrdatpfirooodnutcmhteest,dheotdermindaeteiiomnionfeCP8FOprAeciunrstohrespaurnidfifeodrptohelydmeetrersmipnraotpioosnedo.f PEqFuOivAalaennt
`3StKannodawrnd aadmdoiutnitonomfePtFhOodAt(o5d4e)temreminiseaPdFdeOdA10intthheeppuurirfiifeidedpoploylmyemrerby addon ofp mi of mg/ml oPfFeOpxArp.eepccattrehedadnao(mlhoseuoneluttciioonnnc.tehneAtrpauzrtiiefoinesaddipinoilaolylmn.ersT.ahmeplaemoaunndttowfotshaemapdldeisticoonntsahionuilndgbveariinetdhceornacnegnetroatfion0-s5sthiomoets
For exampl, i 1 1g purified polymer.
ppm
PFOA
i
expected
in
the
purified
polymer,
00,
1.0,
20
ug
PFOA
is
added
to
the
`SoxPhFleOtAextirsacetxitornacbtyedRbOyHRmOaHy a(sMoebOeHavaoirlaEblIeO.H)Faidndailtivoonl,umuelsasfoonriaclaisoanm,pleasndmucsetntbreifiudgeanltisceapl,aration.
ceoxnaEtcxittrneadcwtasetodelruRtitOooHnpfrioesrvteihnnettrcobodaumncpdeednbsriaonttaoidoetnnhieonfLgtCih/neMtMShue/ctMHaSPt)LioCanfoceforilnutjmheenc.dtiilIounnttievomonalliufmsneteacanendsdsaarrdMyS.maDsyielnabsteiitoaindvds:eoldveinnttmoathye
The PFOA
standard addiion calibration curve is plotted area (count) or (PFOA ata (cou/inntetrn)al
aginst the added PFOA standard area (count).
weight,
The
vertical
axis
is
16 the calibration curve (ax + b) satisfied the criteria of B > 0.99, it s valid,
& PFOA content obtained fromth calibration curve where PFOA content= ba ory-ntrcept.
h. Example calculations are shown below.
15.
`Chemicals Company, ASAHI GLASS CO, LTD,
04705
PFOA added to the Ig purified polymer Im 00 10 20
aPnFdOdAilucto"inocnenbtarsaetdioonn a1f0t0er%exrteraccotvieorny emi 000 002 004
PFOA area count 30.300 68.500 113000
noonye |
-
|
=
4135000x04 2250000
R099
samo |
!
on !
|| ostundat sasion
000000200)
PROAGOoNent = O71 ugg = 071 ppm
8Reprisodruecpiebaitleditoynocfetmhoermee(t2hmodesanidn ahlo)moorgsuebsnaeompiflttehseyofputrhiefsiaedmepopluryimfeierd polymer.
n1dhehotmwoogePnFeiOtAyovfaltuheespurrcifwieidtiponlhymeer15r%eosfufftihceieenta,vearnadgethveaPluFe,OAbovtahltuee
reprodaciiy of th is the average value,
method
sFRooelucuroovcneosrn)ycnactrraittneireoicnats-eodCfaliPinFborOaLAtiMsoSno.cournvecoornttahienisntga.ndsaolrvdesnt lnk no extracted solution bot pure sandard
ihehchoantcenntreatdioninanhgeessthaonudladrdbaedciTqiuhioevnaclmoemenpttohs1oi0dtti(h0oe)n.iotafnedKamOraHd aaadnnddidtwiaaortnershiouhldebseolsveendt sbhyouslidbmeiitngse,n
Should no blank. The
be detectedo les han calibration curve for the
20% of he standards s
count ofthe plotted.
lowest
range iandard
conducted in, concntation for
The pro he solve
tRehceovcearlyibirsadtieonicunraeve t(hc*exs+lodp)e sfaotistfhiedsthaendcarridteariaionf R)>(h0e.99sliotpies fvoarlitd,he standards.
18 the recovery satisfied the criteria of 70-1209, it i valid
Example calculations are shown below,
.16.
Chemicals Company, ASAHI GLASS CO, LTD. Calibration curve for the standards>
PFOA concentration g/ml 000 oor 003 00s
oss PFOA area
count 10
27000 75,000 130.000
Joo 100000
00
nom i
(com) ofe_om0_om
. ye 26750000+ | soo
Room [--
caflobrratinoncnurdve e | 2R5 eT03sx10 93220 om ape
Recovery: 2067500 2574746
= 080 = son
Recoivsafefercteyd by bo Recovery doesnot mean the
the mati effet and extract value (PFOA determined)
ficiency: (amount of
PFOA
in
the
puri
polymers),
but
dheeivnailouen(iPFprOacArtieccaolvleyriemdp)os(sPbFeO1A0 aabddaend bietcauthseeplulriPfiOedApoilnymtehresp).rTiheedrpeocloyvemreyrsbmaudstobetximae,s
Generally the recovery is determined based on ater definition,
te
Chemicals Company, ASAHI GLASS CO, LTD.
040705
Example method details "The amount of the purified polymer: 1g Expected PFOA in the purified polymer: 1pm
`<Standard addition method>
1 2
000,0.10,0.20 ml of 0.01 mg/ml PFOA 4.80 5.00 ml B(OH is added to the each
EXOH solution polymer (total
i 5
added 0 the mi EIOH)
1
g
purified
polymer.
3 PFOA is extracted by ultrasonication and centrifugal separation
#
0:1 mi of added and
extracted ROH mixed well.
is
taken
out
into
a
vial
and
0.9
ml
of
(EtOH
water
=
1:1
(wt)
is
5 The mixturei introduced into the LOMS(MS).
The standard addition calibration vertical axis is PFOA area (count).
curv
is
plotid
against
(PFOA
weight
added)
/
1g,
The
Calibration curve for the standards>
7 b0u0t0,pu0r0e1,st0a.n0d5ar,d0s.o0l5utkigon/sm) aPrFe OinAje(ctEeOdHi:nwtoatLeCr/M=S1(:1MS()wt.) solutions (no extracted solution
8 The calibration curve s plotted.
On the same graph, standard addition curve is extracted and diluted solution as horizontal axis,
plotied
by
PFOA
concentration
for
the
10 Mthe "recovery"i 100 %, the slopes of two calibration curves are expected to be identical,
18-
Chemicals Company, ASAHI GLASS CO, LTD,
ours
Attachment 2 ~Example Calculationsof Carbon Content
[The example is based monomers used in the following
on the estimation weight percent
that
the
purified
polymer
is
based
on
sg.
4
ifeent
60% RICH.OCOCHSCH,
(the RE chain distibution average may be equivalent for fy)
35%
25%
CHOiCsHH.yO0CCOOCC(HC=HCyH),=CH,
25% HOCH;NHCOC(CHy)=CH,
Monomer type
Ri(= CyF15)C;H,0COCH=CH,
CisHyOCOCH=CH,
HHOOCC:HH:,N0HCCOOCC((CCHH;y))=~CCHH,,
Formula
CI4FIOHT02
C21H4002 C6H1003
cshno2
Mw [g/mol]
5682
3245
130,1
11531
O17n:t7h6a%t b(a2s9i.s6xth0e6C)-cfoontRenItCoHf,suOcChOaCpHo=lCymHeerfwoirlRbteaverage COF19)
27.02% (77.2x0,35) foCr isHy;0COCH=CH,
4
7.47%
1.385% (55.40,025) for
L305% (52.250.025)for Sum
HOC;H,0COC(CH;)=CH,
HOCH,NHCOC(CH,)=CH,
Cecontent 1%
206
m2 554
522
The carbon content in such a polymer will be approximately 47.5%.
19.
CK hemicals `Company, ASAHI GLASS CO, LTD.
04/07/05
keee e eTmoss moatme a cory ee os Attachment 3 ~ ExampleCalculationsofMolality of 8-2 TB alcohol in polymer
ns E a e a
7 [Mesraionto b8. 5t Atapai tpu| gs[og se m g]
lig
ey ef
I f er naa --c Te WiareJt oaedmep]
ee me
|
eegy--|emp]
i.