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  • 8/11/2019 Applications_of GC in the Paint and Allied Industries-raw Materials-part 2

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    4 PIGMENT AND RESIN TECHNOLOGY JANUAR Y 1981

    A p p l i c a t i o n s o f gasc h r o m a to g r ap h y in t h ep a i n t a l l i e d i n d u s t r i es .R a w m a t e r i a l s : P a r t 2A n n J . Wa l t o n

    C ashe w nu t she l l l i qu i dThe l i qu id e x t r a c t ob t a ined f rom the na tu r a l

    c a s hew nu t sh e l l i s r i ch in pheno l i c subs t ances w h ic ha re de r i ved f rom a n a c a rd i c a c id C 6 H 3 ( O H ) CO 2H)(C 1 5H3 1-n) , wh ere n may have va lues of 0 , 2 , 4 or 6and represents var ious degrees of unsa tura t ion in thea l i p ha t i c C15 s i de - c ha in . I ndus t r i a l deca rboxy l a t i on o fth is mater ia l a ffords cardanol C 6 H4 (OH) (C15 H31 -n) pluso t h e r s ub s t i t u t ed pheno l s and po lymer i c r e s i dues .Ty m a n et al. ( 19 7 , 1 98 ) have s t ud i ed t he ana ly s i s o f

    a l l t h e s e p r od uc t s u s i n g GC, mo lecu l a r d i s t i l l a t i on ,TLC a nd mass sp ec t r om e t ry. Af t e r hyd rogena t i on andt he fo r m a t i on o f t he c o r r e spond ing me thy l e s t e r s , t hep r o duc t s w e re a na l y s ed by GC us ing g l a s s co lumn s(5 f t x 3 / 1 6 i n ) pa ck e d w i t h ac id wash ed and s i l an i zedD i a tom i t e a s s up po r t m a t e r i a l and wh ich was coa t e dwi t h non - po l a r s t a t i ona r y phase s such a s SE30 , SE25or APL , o r s emi - po l a r phase s such a s 0V17 , Dex i l3 0 0 o r PEGA . A l t e r n a t i ve ly, t he s amp le s we re subj ec t ed t o an ace t y l a t i on p rocedu re p r i o r t o GC examina t i o n on co l umn s c o n t a in ing Dex i l 300 , SE30 o rS E 5 2 . The G C equ i pm en t cons i s t ed o f a Pye -Un icammod e l 10 4 i n s t r um e n t ope ra t ed w i th n i t r ogen ca r r i e rgas ( f low ra te 45cm 3 m in- 1) and equ ipped w i th F ID .

    The s a tu r a t ed (1 5 :0 ) , monoene 1 5 : 1 ) , d iene( 1 5 :2 ) and t r ie ne ( 15 : 3 ) con s t i t uen t pheno l s we r e det e rm ined by m ass spe c t r om e t ry fo l l ow ing a TLC separa t i on , wh i l s t bo th T LC and GC sepa ra t i ons r eq u i r edt ha t c o r r ec t i on f a c t o r s we re app l i ed i n o rde r t oaccount for d i ffe ren t response charac ter i s t ics of thed e t ec to r sy s t e m . Th e more h igh ly -po lym er i c s amp le sw er e h and l ed by m o lecu l a r d i s t i l l a t i on t e chn iques ,w h ich g av e f r ac t i on s t ha t we re subsequen t l ye x am i ne d by G C .

    I t was co n c lu de d t ha t t he bu lk o f c a shew nu ts h e l l l i q u id w as su ff i c i en t l y vo l a t i l e t o a l l ow GCa n a l y s i s a l on g t he l i ne s i nd i ca t ed above and , s i ncethe de r i va t i ve s emp l o y ed cou ld be quan t i t a t i ve ly p r ep a r e d , t he G C p eaks c ou ld be hand l ed by s t anda rdin t e g ra t i on p roce du re s t ha t pe rmi t t ed quan t i t a t i ve det e r m ina t i on o f the com ponen t p heno l s .

    Re s in ac i d sTh e me thy l e s t e r s o f ab i e t i c and dehyd ro -

    a b i e t i c a c i d s we re s e p a ra t ed by Medyan t s ev et al.( 134 ) u s ing a co lu m n (1 .8m x 2m m d i a ) con t a in ing4 . 2 Va r n i s ch 3R-7 2 8 a s s t a t i ona ry phase t ha t ope rated a t 125C and wi th he l ium as car r ie r gas a t a f lowr a t e o f 1 0 0c m 3 m in - 1 . The me thy l e s t e r s o f l a evop i -

    ma r i c , pa lu s t r i c and neoab i e t ic a c id s , wh ich we reob t a ined by i somer i s i ng ab i e t i c a c id a t 180 unde rca rbon d iox ide o r 200 C un de r a rgon , we re ana ly sedby Fomin et al. ( 155 ) u s ing GC, i n f r a r ed and u l t r av io l e t spec t ro scopy.

    P ine ro s in ac id s i nc lud in g p im ar i c , i so p im ar i c ,l a evop imar i c , ab i e t i c and neoab i e t i c , a l ongs ide C12to C22 f a t t y a c id s we re r e so lved s imu l t aneo us ly i n aGC procedure descr ibed by Lapshina and Kosynkova(117 ) . The ac id s we re conve r t ed i n to t he i r co r r e spond ing me thy l e s t e r s u s ing d i azome thane and subsequen t l y s epa ra t ed on a co lumn packed w i th 5p o l y e t h a n e d i o ls u c c i n a t e on C h r o m a t r o n N - AW - D M C Swh ich was ope ra t ed unde r a t empe ra tu r e p rog ra mming s chedu l e be tween 150 and 230C .

    In an a l t e rna t i ve p rocedu re , sugges t ed byMahood and Roge r s ( 129 ) , t he f a t t y a c id s we re s epara t ed i n i t i a l l y f r om the r e s in a c id s by p r e l im ina ryme thy l a t i on fo l l owed by t he add i t i on o f 2 , 2 , 4 - t r i -me thy lpen t ane p r i o r t o ex t r ac t i on w i th 5 po t a s s iumhydrox ide so lu t i on i n wa t e r, whe reby t he r e s in a c id swere ca r r i ed i n to the aqueous phase . Af t e r app ly ing

    sui tab le recov ery techniq ues each of the ac id sam pleswere sub j ec t ed t o t r e a tmen t w i th d i azome thane , t oensu re t o t a l me thy l a t i on , f o l l ow ed by GC ana ly s i s ona co lumn conta in ing EGSS-X on Gas Chrom P a t175 C . A r ev i ew dea l i ng w i th t he ana ly s i s o f t helower f a t t y a c id s , w i t h up t o 18 ca rbon a tom s , bycap i l l a ry GC has been pub l i shed by Krupc ik et al( 114 ) . Amongs t t he t op i c s d i s cus sed we re t he s epa rat i on o f f r e e f a t t y a c id s a s opposed t o t he co r r e sponding me thy l e s t e r s , qua l i t a t i ve and quan t i t a t i ve a spec t si nc lu d ing t he ca l c u l a t i on o f Kova t s i nd i ce s , p lu s f e atures of the equ ipm ent suc h as oven s , de te c tors ,s ta t ionary phases and the use of suppor t -coa ted asopposed t o wa l l - coa t ed open t ubu l a r co lumns .

    M i s c e l l a n e o u s c o m p o u n d sThe l ower p r ima ry a l i pha t i c amines we re

    sepa ra t ed , a s t he i r co r r e spo nd ing f l uo r ine - con t a in ingSch i f f ba se s , on a t empe ra tu r e -p rog ram med GCco lu mn co n t a in ing T enax SE-30 a s s t a t i ona ry phaseand w i th an e l ec t ron -cap tu r e de t ec to r, a cco rd ing t oHosh ika (88 , 89 ) . Res idua l s econda ry and t e r t i a ryamines we re ana ly sed a s t he f r e e ba ses . Am ongs t t hes a m p l e s e x a m i n e d w e r e m e t h y l a m i n e , e t h y l a m i n e , na n d i s o - b u t y l a m i n e , n a n d i s o - a m y l a m i n e , d i m e t h y l -a m i n e , d i e t h y l a m i n e , d i ( n - p r o p y l ) a m i n e , t r i m e t h y l -amine and t r i e t hy l amine . Za tkove t sk i i and Sa fonova

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    JANUA RY 1981 PIGMENT AN D RESIN TECHNOLOGY 5

    ( 210 ) r ep o r t ed t he GC sepa ra t ion o f t o luene d i i soc y -a na t e an d h exa me t hy l ene d i i socyana t e u s ing s i n t e r edPTFE pow de r (P o l y ch rom 1 ) a s co lu mn pac k ingm a t e r i a l . The s ame s ubs t ances we re de t e rmined i nt h e i r r e sp ec t i v e p r e p o l ymer s o r adduc t s by J anmot( 9 6 ) wh o u s ed a s a m p le so lu t i on i n e t hy l ace t a t ew h i ch wa s i n j e c t ed o n t o a GC co lumn con t a in ings i l i co ne g um ru bb e r an d ope ra t ed a t 150C . I n t he

    la t te r proc edu re 1-chloronaphtha lene served as in te rna l s t an da rd .

    D im e th y l a ce t ami de i s p r e sen t a s an im pur i t yin conce n t r a t i on s be l ow 2 i n r egene ra t ed syn the t i cg l y c e r o l . T he f o rmer su bs t ance was de t e rmined u s inga GC c o lu m n (1 m x 3 m m i .d . ) packed w i th 20 o f a3 : 1 mix tu r e o f p o ly ( oxp yheny l ene ) and po ly ( e thy l ene -g l y c o l ) s u p p o r t e d o n C h r o m a t r o n N - AW- D M C S b ySergeeva et al. ( 16 9 ) . The co lu mn was elu ted w i thni t rogen as car r ie r gas (30cm 3 m in -1 ) and opera ted a t135 C . A f t e r t he an a l y s is t he co lu mn was c l eaned upb y h ea t i ng i t t o app r ox . 300C .

    A comprehens ive l i s t o f GC re ten t ion da ta on5 0 meth y l an d ph en y l s i l i cone co lumns , ope ra t edu n d e r t empe r a t u r e p r og ram min g , was pub l i shed byM a t t s on and Pe t e rso n (1 32 ) f o r t he t r ime thy l s i l y l der i v a t i ve s o f a roma t i c compounds such a s pheno l s ,n a p h t h o l s , a l c o h o l s , c a r b o x y l ic a c i d s , c h l o r o - c o m -poun ds , a l deh yd es and ke tones , the l a t t e r tw o be inga n a ly sed b o th a s o x i me s and O-me thy l ox imes . Anin t e rp r e t a t i on o f t he co r r e l a t i on be tween s t r uc tu r e andre t en t i on be hav iou r was g iven . A lkyp heno l s p rodu cedf r o m the o l e f i n f r a c t i o ns o f pe t ro l eum were ana ly sedacc o rd ing t o a GC me t h od deve loped by Shchego l et

    al . ( 17 0 ) . Th e t e ch n iqu e was app l i ed i n pa r t i cu l a r t othe ana lys is of p tert octyIphenol produced from2 , 4 ,4 - t r im e thy l pe n t - l - e n e . A t o t a l o f 14 impur i t i e s ,w h i c h i n c l u d e d a c e t o n e , m e t h y l a c r y l a t e , m e t h y l i s o -bu t y r a t e , e t hy l me th a c r y l a t e and me th y l 2 -h yd rox y -2 -m e thy lp rop r iona t e , we r e r e so lved in s amp le s o fm e t hy l me thac ry l a t e b y Soko lowska et al. ( 181 ) u s inga G C co lu m n pa cke d w i t h Ucon -LB-550X on C hrom o-sorb W tha t was opera ted a t 85C.

    Ac eta ldeh yd e , as a source of in te r fe ren ce inthe quant i ta t ive GC analys is of lower leve ls of v i ny lc h lo r i de , wa s e l im ina t e d u s ing a m ix tu r e o f g l a s s

    woo l a nd so d ium b i s u l p ha t e p r i o r t o t he GC co lumnp r o pe r a cco r d ing t o t h e me thod o f Kr i shen and Tucke r( 11 3 ) . W h i t e ( 2 06 ) p ro pose d t he u se o f a co lu mn o fO V- 1 on ac i d -washed D i a tom i t e , t ha t was t em pe ra tu r ep rog ra m m ed f rom 1 8 0 t o 38 0 C , in t he i den t i f i c a t i ono f w axes t ha t we re t ak en f rom museum ob j ec t s . Thepresence of f ree parent ac ids in cy c l ic anh ydr id es w asd e t e rm in ed by Haa s a n d DuBo i s ( 68 ) . Each anhyd r idesa mp le w as i n i t i a l l y r e a c t ed w i th m orpho l i ne so t ha tthe res idue of f ree carboxyl ic ac id could then be c o nv e r t ed i n to t h e co r r e s p ond ing s i l y l de r i va t i ve u s ingb i s ( t r im e th y l s i l y l ) a c e t a mid e r eagen t . The s amp le soo b t a ined w a s ana ly s e d by GC on a co lu mn o f 5S E 5 2 on Gas C hrom Q unde r t empe ra tu r e p rog ram mec o n t ro l f r o m 1 25 t o 2 5 0 C . TLC , on p l a t e s com pr i s i n g

    a mixture of s i l ica ge l and bor ic a c i d , was used tos e pa ra t e , , a n d t o c o p h e r o ls f r o m t h e u n s a p o n i -f i ab l e ma t t e r o f vege t ab l e o i l s , p r i o r t o t he i r de t e rmina t i on by a GC techn iqu e em p loy ing a s i l i cone SE-30co lumn acco rd ing t o R i e r a ( 160 ) . Squa l ane s e rved a san i n t e rna l s t anda rd and t ocophe ro l s we re measu redin sam ples of soya bean , sa ff low er and o ther o i l s . Avery s imi la r techn ique for the GC analys is of toc o

    phero ls was a l so recorded by Domper t and Ber inger(46 ) .

    D D I T I V E S

    P l a s t i c i s e r s

    A GC p rocedu re fo r t he qua l i t a t i ve and quan t it a t i ve ana ly s i s o f d i ca rboxy l i c a l i pha t i c a c id e s t e r s ,wh ich a r e f r equen t l y u sed a s p l a s t i c i s e r co mpon en t si n su r f ace coa t i ng s , ha s been r epo rt ed by B loom (2 6 ) .A 0 .5 -m ic ro l i t r e quan t i t y s amp le d i s so lved i n c a rbond i su lph ide , and equ iva l en t t o be tween 2 and 5 mic ro -gram me s of es te r, wa s in jec ted a t 26 0 C on to asp i r a l l y -wo und g l a s s co lu mn (8m x 1 .8mm i .d . )packed w i th 1 QF-1 ( a t r i f l uo rop ro py lm e t hy l s i l i conel i qu id phase ava i l ab l e commerc i a l l y f r om App l i edScience Labs . ) on 100 to 120 mesh Chromosorb Q.

    The i n s t rum en t u sed was a Hew le t t Packa rdSe r i e s 7400 , hav ing a F ID wh ich ope ra t ed a t 260C ,and wh ich p rov ided an oven t empe ra tu r e p rog rammef rom 160 t o 250 C a t a hea t i ng r a t e o f 3 deg . m i n - 1 .The car r ie r gas was n i t rog en adm i t ted a t a pressureof 29 p s i wh ich en abled a f low ra te of 16 cm 3 m i n - 1 tobe ma in t a ined . Amongs t t he e s t e r s examined we re 14alkyl ad ipa tes , 8 a lkyl aze la tes and 9 a lkyl sebaca tes

    and the i r re ten t ion t imes were compared to tha t ofme th y l a r ach ida t e wh ich wa s emp loy ed as t he i n t e rna l s tan dard . Even wh en these mater ia l s we re use das mixtures to tes t the GC technique , a t l eas t 25 oft hem cou ld be r e so lved and i den t i f i ed unequ ivoca l l y.The pre-de termined e lu t ion proper t ies of any of theabove -men t ioned compounds a l l owed t hem to ber ead i l y i den t i f i ed a s comp onen t s i n two com me rc i a lp l a s t i c i s e r s name ly Durop l az DIOA and Ad im o l l B B .Imia (91 ) de sc r i bed t he de t e rm ina t i on o f the a l coho lcomponents of es te r- type p las t ic i sers by GC in a procedure tha t requ i red a pre l imin ary es te r in te rchan ge

    reac t ion to be car r ied out on the sample us ing methan o l . D ioc ty lph tha l a t e (D O P) , 2 - e thy lhexano l ( 2EH )and o ther subs tances which arose dur ing the reac t iono f 2EH wi th ph tha l i c anhyd r ide we re s epa ra t ed byMos in ska (144 ) u s ing a GC co lum n packed w i th 5DC 200 depos i t ed on Chromoso rb G-AW-DCMS. Theco lum n was t empe ra tu r e p rog ram med f rom 110 t o25 0C a t 20 deg . m in - 1 and t he 2EH was de t e rm inedat 110 C wi t h a car r ie r gas (hydrogen ) f low ra te of6 0 c m 3 m i n - 1 w h i l s t D O P w a s d e t e r m i n e d a t 2 4 0 Cwi th a car r ie r gas f lo w ra te of 120 cm 3 m in - 1 . H y d r ochlo r ic ac id i s a poss ib le degrad at ion produ ct of PVCthat may reac t wi th the epoxy es te r added as s tab i l is e r and p l a s t i c i s e r t o f o rm ch lo rohyd r in s . A l thoughthe se wo u ld dec omp ose du r ing GC to fo rm oxo com -

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    6 PIGMENT AN D RESIN TECHNOLOGY JANU ARY 1981

    po u n ds , i t was r epo r t e d by S t a r t i n et al. ( 187 ) t ha tt he c h lo r oh yd r in s c ou l d b e conve r t ed i n to t he co r r e spond i n g t r i me thy l s i l y l e t he r de r i va t i ve s wh ich we res u ff i c i e n t l y s t ab l e t o a l l o w the i r examina t i on by GC-mass spec t rometry. Resul t s were quoted for a ser ieso f f a t t y a c id me t hy l e s t e r ch lo rohyd r in s .

    Koch e l a nd J a ro s z ynska (1 05 ) em p loyed a GCco l u m n pa cke d w i t h C hr o moso rb W and coa t ed w i th

    O W 2 5 , S E 30 o r A p iez o n L a s s t a t i ona ry phase i n t heiden t i f i c a t i on o f 13 co m m on e s t e r p l a s t i c i s e r s , i n c l ud ing t r i c r e sy l ph o s pha t e , and 17 f r equen t l y -u sed a n t ioxidants present in n i t r i le and neoprene rubbers . I tw a s found t ha t t he p l a s t i c i s e r s cou ld be examined byev a p o ra t i ng t hem d i r ec t l y f r om the s amp le s a t 480C ,pr ior to GC analys is a t 250C, and tha t no in te r fe renc e w as ev i den t f r om the deg rada t i on p roduc t s o ft he r ub be r s . Th e a n t i o x idan t s needed t o be ex t r ac t edf ro m the rubbers over a 3-hr. per io d us ing ace tone a tt he amb i en t t e mp e ra tu r e f o l l owed by GC examina t i onof the ex t rac ts .

    S u r f a c t a n t s

    S ur f ac e - ac t i v e ag en t s , de r i ved f rom the r eac t i o n o f a l ong -c ha in a l i pha t i c a l coho l w i th e thy l eneox i d e , ha ve bee n e x t en s iv e ly s t ud i ed by GC. S t anche rand Fav re t t o ( 1 86 ) r ep o r t ed t he f r a c t i o na t i on o fs am p l e s h av ing t he g en e ra l f o rmu la RO(CH 2 CH2O )1 3 H,wh ere R represents an n alkyl r ad i c a l , and found t ha tonly the com pon ents h aving n = 1 to 4 wer e capa bleo f r e s o lu t i on on a g l a s s c o lum n packed w i th 3 SE30on Ga s Ch rom Q . The v o l a t i l i t y o f t he o l i gom er s w asi mpr o v ed by co nv e r s io n t o t he co r r e spond ing t r i

    me t h y l s i l y l d e r i va t i ve s , bu t t he r e so lu t i on was nobet te r than before even wh en tempe ra tures above33 0 C w ere em p lo y ed . In o rde r t o quan t i f y t he a lky lr ad i ca l d i s t r i b u t i o n o f e t h oxy l a t ed a l coho l s , Sones etal . ( 183 ) f i r s t conve r t ed t he s amp le s i n to t he co r r e spond i ng a lk y l i od i de s p r i o r t o GC ana ly s i s .

    Fa rk a s ( 53 ) s t u d i e d t he p roduc t s ob t a ined byca t a l y t i c ox ye thy l a t i on o f l au ry l a l coho l on a GCco l u m n packed w i t h 60 -80 mesh Chromoso rb andcoa t ed w i th 7 De x s i l . I n o rde r t o e l im ina t e t a i l i ngeffec ts , the hydroxyl groups present in the samplew ere s ub j e c t ed t o ke t ene ace t y l a t i on . The s am eau tho r a l s o e xamin ed t he p roduc t d i s t r i bu t i on o f do -d e c y l a l c o h o l o l i g o m e r s a t 1 9 0 - 2 9 0 C b y G C o n 3 0 -6 0 m e s h C h r o m o s o r b W- AW- D M C S w h i c h w a scoa t e d w i th 1 0 SE3 0 1 a s l i qu id phase . Ac e ty l a t i ono r me thy l a t i on o f t h e s amp le s p r i o r t o ch roma tography led to the e l imin a t io n of peak ta i l in g , bu t i tw as foun d t h a t t he me t h y l a t ed compounds gave r i s et o s u pe r io r s ep a r a t i on pe r fo rmance . Go to et al. (65)us ed a GC c o lu m n ( 75c m x 3m m i . d .) t ha t wa sp a c k e d w i t h 2 O V- I o n C h r o m o s o r b W ( 8 0 - 1 0 0mesh ) a nd wh ic h ope r a t e d a t 232C us ing n i t r ogen a sca r r i e r ga s ( 4 0cm 3 m in-1 ) to s tudy the s ta te of s o l ut i on o f t he n on - ion i c su r f ac t an t hexaoxye thy l ene n

    l au ry l e t he r. T he t e chn i q ue was u sed i n con junc t i onw i th t he i n i t i a l GPC (ge l pe rmea t i on ch roma to

    graphic) separa t ion of the sur fac tan t so lu t ion onSephadex G -200. The resu l t s sugges ted tha t a c o nt i nuous s e l f - a s soc i a t i on o f t he su r f ac t an t ex i s t ed a tl ow conc en t r a t i ons , whe rea s a more cons t an t m ice l l a rs i z e was a s sumed a t h ighe r concen t r a t i ons . Sones etal . ( 183 ) have a l so r epo r t ed the a lky l homologue d i st r i bu t i o n i n a l ky l supha t e s and a lky l e the r su lpha t e s ,whe reby t he s amp le s we re i n i t i a l l y sub j ec t ed t o a c id

    hydrolys is pr ior to the i r convers ion in to the cor respond ing a lky l i od ide s and ana ly s i s by GC.

    Sh i l ov and Molov a (171 ) on t he o the r handp roposed t o c a l cu l a t e t he po l a r i t y i ndex o f so d iuma lky lmonosu lpha t e s amp le s f r om the i r GC r e t en t i onvo lumes and t o p lo t t h i s pa r ame te r aga in s t hyd rocarbon cha in length in order to de termine the lengthof the hydrophobic par t o f the sur fac tan t .

    Mi sce l l aneousErmi lova and Ma io rova (49 ) de s c r i bed a GC

    techn ique fo r t he de t e rmina t i on o f f o rma ldehyde i n

    fo rma l in so lu t i ons . Po lye thy l eneg lyco l ad ipa t e . ( 10w / w ) o n P o l y c h r o m 1 f o r m e d th e c o l u m n p a c k i n gmater ia l and de tec t ion of the samples was by thermalcon duc t i v i t y. Impur i t i e s such a s o l i gom er i c g ly co l s ,wh ich m ay be p r e sen t i n f o rm a l in so lu t i on s , we requan t i f i ed by Danke lman and Daeman (41 ) who s epara t ed t he co r r e spond ing s i l y l a t i on p roduc t s by GC.The r e su l t s o f t he se expe r imen t s we re co r robo ra t edus ing a 22 0M Hz NM R spec t rom e te r.

    Benzophenone and benzo t r i a zo l e , wh ich maybe used in p las t ics to abso rb UV l ight , were de termined by FID on a GC equipped wi th dual s ta in lesss t e e l co lum ns con t a in ing 10 SE-30 on Chrom oso rbW , a n d w h i c h w e r e te m p e r a t u r e p r o g r a m m e d f r o m180 t o 270 C , i n a me thod deve loped by Horacek(87 ) . The abso rbe r was i n i t i a l l y ex t r ac t ed f rom thesample of p las t ic us ing ch loroform or e thyl e ther, andsubsequen t l y app l i ed t o t he GC co lumn a s a so lu t i onin ch l o ro fo rm , e t hano l o r hep t ane . Us ing c a l i b r a t i ongraphs or in te rna l s tandards , i t was c la imed tha t 0 .1mic rog ram quan t i t i e s o f ab so rbe r cou ld be de t e rmin ed and tha t the e r ror d id not exceed 20 .

    Ac co rd ing t o a pape r pub l i shed by Uden(19 9 ) , bo th h igh pe r fo rm ance l i qu id ch roma tog raphyand GC analy t ica l techniques have been appl ied to

    the ana lys is of me ta ls . GC requ i red neut ra l mo lecu lescom bined w i t h l ow mo la r mas s and t yp i ca l l i gandss t u d i e d c o n t a i n e d - a l k y l , - a r y l , d i e n y l , c a r b o n y l o rn i t r o sy l f unc t i ona l i t y. Fo r exam p le , -d ike tona te s o fb e r y l l i u m , c h r o m i u m , a l u m i n i u m , i r o n ( I I I ) andcoba l t ( I I I ) have been used in rea l i s t ic ana ly t ica l de termin a t i ons , wh i l s t - t h ioke tona t e s we re fou nd t o beva luab l e i n t he de t e rm ina t i on o f n i cke l , coba l t , z i nc ,p a l l a d i u m , p l a t i n u m , c a d m i u m a n d l e a d . The mos tsu i ta b le de tec tor for th i s approa ch was a d i rec t curr en t a rgon p l a sma emi s s ion spec t rome te r. The s amp lewas t r an s f e r r ed f rom the ch roma tog raph v i a a hea t edl i ne w i th ann u l a r l y i n t ro duce d a rgon shea th ga s t o op -

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    10 PIGMENT AN D RESIN TECHNOLOGY JANUA RY 1981

    APPLICATIONS OF GAS CHROMATOGRAPHYContinued from Page 6t imise the form of the p lasma d ischarge , to ensure am in im um o f peak b roaden ing , and t he s ens i t i v i t y t osub -nanog ram l eve l s o f t he me t a l s . Gas number,wh ich i s a pa r ame te r f o r cha r ac t e r i s i ng t he foam ingp rope r t i e s o f b lowin g agen t s , was de t e rmine d f romthe n i t rogen con t en t o f t he t he rm a l deg rada t i on p roducts in a pyro lys is -G C approac h repor ted byM a k a g o n et al ( 130 ) Each de t e rm ina t i on t ook f ro m

    20 t o 30 minu t e s and t he r e su l t s showed a s t anda rddev i a t i on o f 0 . 012 t o 0 . 038 .