Quantitative Analysis of Antioxidants from High - Virginia Tech

69 Pages·1997·0.33 MB·English

Quantitative Analysis of Antioxidants from High Density Polyethylene (HDPE)
by off-line Supercritical Fluid Extraction Coupled High Performance Liquid
Chromatography
otn i .PaMlegnA
d neatutits ncIinhcetyl oaPinigr ieV h ftyotluc aeF h otdtett i m b u ss is e hT
feoerg eed hrt osftnemeriuq eer h fttonemllifl ulfaitr a npyitisrevi neUtatS
Master of Science
in
Chemistry
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semaJ ellivnalG
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August 25, 1997
ainigri V,grubskcalB
Keywords: ,)EPD He(nelyhteyl oyPtisn ehDg i,Hnoitcart x,Elacitircr ep uS xonahtE (cid:226) 330,
xonahtE (cid:226) ,893 ,EFS ,CLPH ss a,Myr tteemlonrIt-ctecpeSr ieDborP)PID(
otn i.aPMleg n,A79 9t1hgirypoC
Quantitative Analysis of Antioxidants from High Density Polyethylene (HDPE)
by off-line Supercritical Fluid Extraction Coupled High Performance Liquid
Chromatography
otn i .PaMlegnA
(ABSTRACT)
,stra pelibomotu amor fgnigna r,ytilibacilpp arieh tn iyra vyeh tdn ades uyledi wer ascitsalP
.str acpinortce lodeto omfo rgfnihtyre vr eogfnigakc ad pn,asgnidli ud bnsaesu or hosftnenopmoc
,enerytsyl o sphac u,sscitsa l fpsonoitacilp peasrev iedhT odtetide re cr,aretseyl od pnsanifeloylop
remyl orpeh td onease hfetocnamrofr ee phetvorp msievit i.d sdeAvitid dfnaooitaroproc neiht
elpma xr eo,fsevitid dhac ufnsooitaroproc ne ihttuo h.t sinWiser xonahtE (cid:226) scitsa lepm o,s033
eviti dtfndnoaau odmeaific e epths ateh rt.ue s monriTe etgrvnooissec ogrnpi reuddar gdelduow
d i, psaasrec onropisur t exrheet trfeam yo l taodnpeitaropro c ensrieaviti dnfdooaitanib mrooc
sriemyl oep h nt)is(evitid d fanooitatitn a. udQeriuq e srdioht elmacityla neataruc cdana
e hetcneulf nni a)cs(evitid d fatonuo mea hdt neadarg eyd a)ms(evitid dea hetcn i,syrassecen
hc u,s)s(evitid draemyl orp osfeuqinhc entoitcart xleanoitnev n. orCemyl oep h fteorut alnacisyhp
e hdt n,aevisnep x,egnimusn oecm i,tevisnet nriob ael rnaoitatipice rn/poituloss i rdtoelhx o,Ssa
hc ut,snevl o fstonuo meagr a,alnoitid d. natInecr e 0pn9a hsts eylltnacifing i ssyirevoc elramitpo
sa eneulot ro ortoi replpm ae shettartnecn oorcted rndoietanimi letebs u,mnilaced
.noitar acpiehspargotamorhc
remyl oepvitanret l na sadaeyolp mnee esb a)hEF Sn(oitcart xdEiu llFacitircrepuS
noitarape replpm alsacityla nsauoir arv osfna eemlbarov a s afEi. FeSuqinhc entoitaraperp
noitcar t ex rhe EotsFfySol phmcerae s.ses ireh mTniotitcar ttxre o shdotsetitid e,rscnoitacilppa
tnadixoit ne ahfto xonahtE (cid:226)VU/CL P yHdbewoll o)fEPD He(nelyhteyl oyptisn ehdg imho r0f 33
.detagitsev neir enwoitartnecn orceifid odm n,aep yrteifid o,merutarepm e ftsotcef fe.e hsTisylana
ycneicif fneoitcart xee h,tdenimret eedr eswnoitidn oncoitcart xleamit peo hetcnO
fo xonahtE (cid:226) feocnese rep h ntdi neavitid dealgn i sas0a 33 e rEe PwmD oHsrefvitidda-oc
rdoefnia te b r%one 0awr9hett a seferoigr e.vdo ecteaRgitsevni xonahtE (cid:226) yradno c neaes h0 w33
.E P eDtnhHnites e srtapnwadixoitna
Acknowledgments
dpniahsdne i,rtfrop pruis eeh v toaehglwp oeesp okhn t aeo hktdtill uroowh teuhaT
,trop p,uescnad itungats n s ori,cohrfosi v,ydrmaol yy.arT Tr .saorkLtDn alha ti.cs erpeSyarp
rie heetmv ao ghpwuo rrGoly ae Thnetinoyre vo,etyldn o.c eecSnedifn od cntanemegaruocne
,yldri h .Tretro Pyelleh Sdn aleinaDc Miro L,sbmo Cleahci M.r D,yllaicep s .Epihsdneir fdn aemit
,htr u. oeFcnadi udg neam irtie hrt osfrebm eemettimm o ycomt ,eg unooRt a.Bp (reolCrameblA
,ylht f. isFelpm aEsP DdHerape rdp nsadradna tes h ftyolpp ues h,ttropp ulsaicnan irfie hrt o)f.AL
mi K;hce Tainigri Vt asrebme mffat sgniwollo feh tot n,.h)ronDJoitatnemur thSscMni(IraH
m i,J)po heSnihca Mr(ia ldBe r,F).tp eyDrtsero Fr(elieS )c pidonnhoaSrt creeltEl(uoC aizeK
,stner ayfhpmot oo,btylh t.x )i.Stp eyDrtsimeh Cr(ecipS ,ev orlie hr tooftn iePs od JneadlinoeL
ne hewre hytlpm iesr etwa hstdnei rdf nsarebm eymlim aefso h ot,to s. leAcnarussa edr ntaroppus
teolnp oree phe.tst o osdlohinl ttrAashu C s d, eoryyJtolmLh t m.n oeeedt hbveted SeIen
.uo yknah t;yllacificep sevob adenoitnem
vi
Table of Contents
Page
Abstract ii
Acknowledgements vi
List of Figures iv
List of Tables xi
I. Introduction 1
sremylo Pn isevitid d .AA 1
noitcart xdEiu llFacitircr e.p BuS 9
sremylo Pn isevitidd Af osisyla n .AC 14
II. Quantitative Analysis of Ethanox(cid:226)(cid:226) 330 in High Density Polyethylene 18
A. Introduction 18
latnemire p. xBE 18
noissucs idD nsatlu s. eCR 20
noisulc n. oDC 43
III. Mass Spectrometric Determination of Degradate Peak 44
A. Introduction 44
latnemire p. xBE 44
s idD nsatlu s. eCR noissuc 45
noisulc n. oDC 56
References 57
Vita 59
v
List of Figures
Figure Description Page
1 .slone hdperedn i fhsoerutcur tlsacimehC 3
2 .slone hdperedn i fhnooit c famosinahceM 4
3 erutcur tlsacimehC fso .setihpsohp 7
4 f onoitc af omsinahceM .setihpsohp 8
5 lacitircrepu slacitylan aenil-ff on af ostnenopmo ccisaB 12
.rotcar tdxieulf
6 .selbair anvoitcart xeev irf otfo lsptcef fneiaM 21
7 00 1gniniatno celpma sEPD Hdelli maf oCSD mpp0 24
xonahtE (cid:226) 330.
8 nfCaoLPH xonahtE (cid:226) tcar trxeemy l 0o3p3 28
(20 m .)noitcej nLi
9 lonaht edmradna tmspp00 0h1se rrdfoe gnfCaaoLPH 29
fnooitulos xonahtE (cid:226) 330 (20 m .)noitcej nLi
10 dn a nsdoeki pnse esb ahhci hewrutarepm e fttoceffE . 30

iv
11 nfCaoLPH xonahtE (cid:226) 0t2c(ar trxeemy l0o3p3 m .)noitcej nLi 31
12 gniniatn oeclpm adsetcart x feeoudis efaCroLPH 34
mpp0001 xonahtE (cid:226) mpp 0 /000313 xonahtE (cid:226) mpp 0/ 08593
.sremog i elnhoith tdiewpp aTrHtD

13 mpp0 0g5niniatn oeclpm arsemyl odpetcart x ne faCoLPH 36
xonahtE (cid:226) mpp 0 /000313 sofagrI (cid:226) mpp 0/ 08561 CaSt.
14 mpp0 0g5niniatn oeclpm arsemyl odpetcart x ne faCoLPH 37
xonahtE (cid:226) mpp 0 /000313 sofagrI (cid:226) mpp 0/ 08161 xonagrI (cid:226)
/6701 %2OCaC .
3
15 HPLC o deta ed hndaeta et hoenlpm arsemyl odpetcart xfe 41
.sisyla n C aoLrtoirp
16 + SfMoISL xonahtE (cid:226) .xirta mlorecyl gan i03 3 47
17 +IE fo xonahtE (cid:226) 330. 48
18 +fIoC xonahtE (cid:226) 330. 50
19 +fIoC .n oeittacdaarrfged 51
20 +fIoC n ofeiohttc ar thenbthouitiswt ceatrafdarged 52
.9 0z5 / fmno orialucelom
21 gniniat ntoc ca +r fItE oCxPaeDH xonahtE (cid:226) 0de3nh3at 53
.sei cdeeptsarged
iiv
22 .sdn oeblbu odd nsagn i frroebm uen hrt osfnoitalucl aaclumroF 54
23 feorutcur tlsacimehC elbiss oepht degradate. 55
iiiv
List of Tables
Table Description Page
I sloneh pderedni helbaliav ayllaicremmo cf oselpmaxE 2
.stnadixoit nyarami r spdae ssueni mdaeredn idhna
II aicremmo cf oselpmaxE elbaliav ayll d nsaetihpsohp 6
.stnadixoit nyaradnoc esdsae ssudnuopmocoiht
III .E FrS odfe ssudiu lnfomm o fcsoretemar alpacitirC 10
IV .selpm arsemyl orp osfeuqinhc estisyla nda nnaoitcartxE 15
V ehT atadrof .selbair anvoitcart xeev if 22
VI s efiorev otcneercreP xonahtE (cid:226) 033 mor fEPDH ta 25
.evitid dmapp001
VII y rfeov otcneercreP xonahtE (cid:226) tnereff itEdaP DmHo r0 f33 26
.sleve levitidda
VIII .lev eelvitid dda nnaoitisopm oeclpm aEsPDH 33
IX y rfeov olcaetroT xonahtE (cid:226) remyl oEpP DmHo r0f 33 35
.selpmas
X .lev eelvitid dda nnaoitisopm oeclpm aEsPDH 39
XI fyorevoceR xonahtE (cid:226) .selpm arsemyl oEpP DmHo r0f 33 40
ix
XII fyorevoc e frnooisirapmoC xonahtE (cid:226) E mP0oD3rH3f 42
f oecneser peh tn iselpma sremylop sofagrI (cid:226) d nhat i8 w61
.regnev adc istcuaohtiw
x