l a n r u J Teknobiolog,iI II(1 )2012 : 15 – 65 ISSN :2087– 5428
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k it il a n A a i m i K i s a i s e p S n a d n a h a s i m e P m u ir o t a r o b a L t u ti t s n I a i m i K i d u t S m a r g o r P Teknolog iBandung 2 3 1 0 4 g n u d n a B 0 1 a h s e n a G . l J E-mali :ilana_mey@yahoo.com a r t s b A c t Cr(VI )compound saret oxicandcarcinogenic ,consequenlty,t hedevelopmen to fa l a t n e m n o ri v n e n i m u i m o r h c f o s i s y l a n a e v it c e l e s e h t s a l l e w s a , d o h t e m e v it i s n e s s i e l p m a s absolutelyessenita.lAchelaitngresinAmbelrtieXAD- 61 - 51 -, Dipheny l e v it c e l e s d n a d e t a rt n e c n o c e r P . d e z ir e t c a r a h c d n a d e z i s e h t n y s n e e b s a h e d i z a b r a c H t a x e l p m o c g n i m r o f y b ) I V ( m u i m o r h c f o s i s y l a n a 2SO4 0,05M .TheCr(VI)i on D A X n o d e n i a t e r s a w - 61 -DPCmini-columnandcanbeelutedquanttiaitvelywtih O N H 3 5 M and determined by Atomic Absorpiton Specrtomerty .The effec to f H2SO4 concenrtaiton ,contac t itme ,reteniton capactiy ,eluen tconcenrtaiton were invesitgated .The research show stha treteniton capactiy o fAmbelrtie XAD- 61 s i y ti c a p a c n o it n e t e r c i m a n y d d n a d o h t e m h c t a b r o f D A X g / r C g m 4 2 . 2 s i C P D 5 . 6 1 s i n m u l o c i n i m f o d e t a r u t a s e m it h ti w d o h t e m n m u l o c r o f D A X g / r C g µ 1 7 . 4 2 n o i s i c e r p e h T . d n o c e s fort hi smethodexpresseda scoefifcien tvairaitoni s3.68% r e i n il e h T . b p p 9 6 s a w d e n i a t b o n o it c e t e d f o t i m il e h T . l e v e l e c n e d if n o c % 5 9 a t a t n e i c if f e o c n o it a l e r r o c a h ti w b p p 0 0 9 l it n u b p p 0 0 1 n e e w t e b d e n i a tt a e b n a c e g n a r o g a s a h d o h t e m s i h T . 5 8 9 . 0 s i odaccuracyaccordingt o 100%o frecovery .The , r o t c a f t n e m h c ir n e y b d e w o h s e b n a c e c n a m r o f r e p s i s y l a n A n o it c e j n I w o l F d n a , s e t u n i m / 5 . 0 , 2 s a w d e n i a t b o x e d n i e v it p m u s n o c d n a , y c n e i c if f e n o it a rt n e c n o c l F d n a l a c it y l a n a f o y d u t s e h T . y l e v it c e p s e r , L m 5 . 6 ow Injeciton Analysi s s i s y l a n a e v it c e l e s o t d e s u e b n a c d o h t e m s i h t t a h t d e w o h s e c n a m r o f r e p .l e v e l b p p a n o ) I V ( m u i m o r h C y e K words : ambe lrtie XAD-16 , chelaitng re isn , chromium(VI) , 1,5 -p , e d iz a b r a c l y n e h p i d reconcentraiton.
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m a g o l n o i il a k g n ir e S beratmasukke alrianai rkarenaai r h a l e t i d u t S . ir t s u d n i s e s o r p i a g a b r e b i r a d n a g n a u b b a b e s i d n i a l a r a t n a r e k n a k b a b e y n e p a w h a b n a k k u j n u n e m -g n a y a y a h a b r e b t a g n a s g n a y u t n e tr e t m a g o l a n e r a k n a k dapa tmeningkatkan interaksinya dengan logam lain ,d i u t a u s a i m i k k u t n e b a d a p g n u t n a g r e t t a g n a s i n i s e s o r p a n a m a y a h a b n a k a n a r a d a s e k n a t a k g n i n e p i n i g n a r a k e S . m a g o l g n u r e d n e c a y n a i m i k k u t n e b n a k r a s a d r e b t a r e b m a g o l i b e l g n a y s i s il a n a n a g n a b m e k r e p g n o r o d n e m hselekit fdan .) 7 0 0 2 , k k d n a r u D ( m a g o l i s a i s e p s Logam kromium banyak digunakan d i beberapa , t a c , ti l u k n a k a m a y n e p , g n it a l p o rt k e l e i tr e p e s i rt s u d n i m a l a i d m u i m o r K . li t s k e t n a d , r o t o m r e b n a a r a d n e k t o p l a n k d n i c l a Y ( ) I V ( r C n a d ) I I I ( r C k u t n e b m a l a d t a p a d r e t an .) 6 0 0 2 , k a p A Senyawa Cr(III )merupakan makronutiren m e m k u t n u a i s u n a m h e l o n a k h u t u b i d g n a y l a i s n e s e , k il i F ( n i e t o r p n a d , d i p il , a s o k u l g e m s il o b a t e m n a k n a h a tr e p t a g n a s n a d r e k n a k n a k b a b e y n e m ) I V ( r C n a k g n a d e S . ) 2 0 0 2 n a y a y n i s a d i s k o l a i s n e t o p a n e r a k k i s k o t g itngg i dan n a k r o p a li D . ) 6 0 0 2 , k a p A n a d n i c l a Y ( li c e k g n a y a y n n a r u k u l a j n i g n a d , r e v il , u r a p k a s u r e m t a p a d ) I V ( r C a w h a b ) I V ( r C s a t a b g n a b m a O H W t u r u n e M . ) 6 9 9 1 , k k d c e v o k B ( o k i s e r n a g n e d n a k g n i d n a b i d i g g n it u l a lr e t L / g m 5 0 , 0 t a b i k A . n a k l u b m it i d g n a y r e k n a k nya , perkembangan i d m u i m o r k n o i i s a i s e p s e d o t e m i tr e p e s f it i s n e s e d o t e m g n it n e p t a g n a s i d a j n e m n a g n u k g n il (Durandkk ,2007.) e d o t e M untuk anailsa kromium meilput i eksrtaks i n a d a m a l u t k a w n a k u lr e m e m n o i r a k u n e p n a d t u r a l e p m a s i b l e p m a s i s a l u p i n a m a y n a d a engakibatkan rusaknya . ) 4 0 0 2 , k k d n u S ( s i s il a n a n a k u k a li d m u l e b e s m u i m o r k k u t n u n a k a n u g i d h a l e t n e m u rt s n i s i s il a n a k i n k e t a p a r e b e B v u i rt e m o t o f o rt k e p s i t u p il e m m u i m o r k i s a n i m r e t e d - sviI
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n a p a r e T s ni a S h ai m lI la n r u J u ai R s a ti s r e vi n U n ai til e n e P a g a b m e L2 5 ( S A A , ) 1 9 9 1 , ll u r K ( Tunceil danTurker ,2002) ,danICP , k k d a d i m u S ( S E A 2005.) Karena konsenrtas i Cr(VI ) n a g n u d n a k n a d L / g µ m a l a d a y n a s a i b r i a l e p m a s m a l a d a k a m , i g g n it a y n s k ir t a m metode anailsi sinsrtumen pelru k u t n u i s a rt n e s n o k a r p e d o t e m n a g n e d n a k g n u b a g i d . a y n i s k e t e d t i m il i k i a b r e p m e m i s a rt n e s n o k a r p k u t n u t a l e h k g n e p n i s e r n a a n u g g n e P n a k g n u b u h i d a s i b a n e r a k n a k t a k g n it i d h i b e l g n a r a k e s n a g n e d FlowI njecitonAnaily iss(FIA )yangt erotomaitsas i . ) 5 0 0 2 , r a w a h u h K ( Keuntungannya bisa meminimalkan s e m u l o v a tr e s a n a h r e d e s h i b e l ,i s a r a p e r p u t k a w ampe ldan .) 5 0 0 2 , k k d a y r a K ( t i k i d e s h i b e l n a k a n u g i d g n a y n e g a e r D A X t il r e b m A n i s e R -16( PSDVB )dipiilhsebaga imateira l n a t u r a l m a l a d a y n n a li b a t s e k a n e r a k m o l o k i n i m i s i g n e p p u k u c g n a y n a a k u m r e p h a r e a d i a y n u p m e m , a s a b n a d m a s a i a g a b e s n a k a n u g i d k o c o c , s a u l pengis ikolomdenganeluen n a g n a li h e k u a t a i s a d a r g e d i d a jr e t a p n a t t a u k m a s a .) 6 0 0 2 , k a p A n a d n i c l a Y ( a y n a m r o f r e p 1 -,5Dfienli -n a d f it k e l e s n e g a e r i a g a b e s i u h a t e k i d ) C P D ( a d i z a b r a k . ir t e m o t o f o rt k e p s a r a c e s ) I V ( r C n a u t n e n e p k u t n u f it i s n e s u ti a n e r a k h e l O tuju an dar ipeneilitanin iuntukmengem -n a d i s a rt n e s n o k a r p k i n k e t i s a u l a v e g n e m n a d n a k g n a b s i s a b r e b ) I V ( m u i m o r k f it k e l e s s i s il a n a Flow Injeciton s is y l a n A menggunakan resin pengkhela tAmbelrtie XAD -6 1 - CD . P Metode i n idiharapkanmemiilk iakurasi ,presisi , l n a d imi tdeteksi ,setra kinejra FIA yang baik sehingga m u i m o r k f it k e l e s k i n e r s i s il a n a k u t n u n a k a n u g r e p i d t a p a d . n a ri a r e p n a g n u k g n il i d t a p a d r e t g n a y
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t a l A -ala tyang digunakan antara lain :Spekrtofotomete r R I ( r e ir u o F i s a m r o f s n a r T h a r e M a r f n I Presitge-21 Fouire r k u t n u ) u z d a m i h S r e t e m o t o h p o rt c e p S d e r a r f n I m r o f s n a r T r e t e m H p , s i s e t n i s i d g n a y n i s e r k it s ir e t k a r a k n a ij u g n e p a n n a H ( ®) , Pompa peirstalitk (Ismatec) , kolom PTFE n o g y T a p i p , m c 5 g n a j n a p , m m 2 r e t e m a i d ®diamete r0,07 -n a r u l a s k u t n u m c 0 1 , 0 sampe lpereaks ilainnya ,Atomic r e t e m o t o h p o r t c e p S n o it p r o s b A (AASDoubleBeamGBC® t a k g n a r e P , ti l a n a m a l a d ) I V ( r C r a d a k s i s il a n a k u t n u ) 2 0 9 k a n u l Powe rChrom (AD Insrtument® )yang teirntegras i l a ti g i d a r a c e s a t a d t a t a c n e p k u t n u S A A m a l a d .Bahan -g n a y n a h a b digunakan dalam peneilitan in i memiilk i : i r a d i ri d r e t n a d ) a . p ( s i s il a n a o r p n a i n r u m e k t a k g n it K2Cr2O7(s) ,CrCl3.6H2O(s) ,etanol ,aseton(aq) ,HNO3 pekat , H2SO4 pekat ,HC lpekat ,SnCl2(aq) ,NaNO2(s) ,NaOH(aq) , D A X e ti lr e b m A - 61 (s) ,KI(s) ,amlium(s) dibel idar iMerck 5 , 1 i l a u c e k -Dfieni lkarbazida (DPC)(s) dibel idar iSigma . h c ir d l A.
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. 1 . 3 Sintesi sdanKarakteirsas iResinPengkhela tAmbelrtie D A X - 61 - CD P n a k li s a h g n e m t a k e p t a rt i n m a s a n a g n e d i s k a e r e b n e z n e B a l k o c a n r a w r e b g n a y n e z n e b o rt i n tmuda secara lambat . n a g n e d n a k a n a s k a li d a k ij t a p e c h i b e l t u b e s r e t i s k a e R t a k e p t a rt i n m a s a n a r u p m a c n a g n e d n e z n e b n a k s a n a m e m u j a l n a k k i a n e m t a k e p t a fl u s m a s A . t a k e p t a fl u s m a s a n a d n o i u ti a y l if o rt k e l e h a l m u j n a k t a k g n i n e m n a g n e d i s k a e r O N ( m u i n o rt i n 2+) . Prose s reduks i nirtobenzen meng -n a k u k a li d a u t t a l k o c a n r a w r e b g n a y a n i m a li z n e b n a k li s a h l C n S m a g o l m a r a g n a u t n a b n a g n e d 2 dalam HCl ,karena n a k h a b m a ti d a g g n i h e s l C H m a l a d t u r a l r a k u s n e z n e b o rt i n e n e r a n o I . s k u lf e r s e s o r p h a l n a k u k a li d n a d l o n a t e -e m m u i n o z a i d rupakan elekrtoifilk lemah yang bisa g n e m f it k a e r g n a y k it a m o r a a w a y n e s n a g n e d i s k a e r e b -k il if o rt k e l e k it a m o r a i s u ti t s b u S . o z a a w a y n e s n a k li s a h i r a d m u i n o z a i d e n e r a n o i i s k a e R . o z a g n il p o k i s k a e r t u b e s i d D A X e ti lr e b m A -16 (PSDVB ) dengan 1,5-Dfieni l a d i z a b r a k menghaslikan resin pengkela tyang berwarna . n a h a r e m e k t a l k o c Tahapanreaks inirtasi ,reduksi ,diazot-i g il n a g n e d g n il p o k n a d , i s a s andapa tdiilha tpadaGamba r . 1 CH CH2 HNO3 SnCl2 NaNO 2 CH CH2 NH2 CH CH2 NO2 CH CH2 N2+Cl -HCl HCl H2SO4 PSDVB NHNH O NHNH N NH N NHNH O NH CH CH2 + . 1 r a b m a G Tahapan Reaks iSintesi sAmbelrtieXAD- 61 -C P D k u t n u n a k u k a li d s i s e t n i s l i s a h n i s e r i s a s ir e t k a r a K m u rt k e p s n a k r a s a d r e B . s i s e t n i s n a li s a h r e b e k i u h a t e g n e m B V D S P a w a y n e s R I - ON 2 (2a)yang diperoleh dar ihasi l m c 2 6 , 7 2 5 1 a d a p m a j a t n a p a r e s a ti p n a k k u j n u n e m i s a rt i n -1 m c 4 2 , 8 4 3 1 n a d -1 .Keduaptiaserapant ersebu tmerupakan g n a li h n a k a n a p a r e s a ti P . o rt i n s u g u g i r a d n a p a r e s a ti p l C n S n a g n e d i s k u d e r n a k u k a li d h a l e t e s 2 dalam HC lyang s u g u g i s k u d e r e m - ON 2 dar i benzen menjad i - HN 2 . B V D S P m u rt k e p S - HN 2 menunjukkan ptiaserapan sediki t 6 1 g n a b m o l e g n a g n a li b a d a p m a j a t 08,63 cm-1 yang H N s u g u g k it s ir e t k a r a k n a k a p u r e m 2 pada benzliamina . n a g n a li b a d a p n a p a r e s a ti p n a g n e d g n u k u d i d t u b e s r e t a t a D m c 8 8 , 6 7 2 1 g n a b m o l e g -1 yang merupakan karakteirsitk C n a t a k i -Npadabenzliamina( Gamba r2b) . . 2 r a b m a G Spekrtum Infra Merah PSDVB- ON 2 (a) , B V D S P - HN 2 (b) ,Ambelrtie XAD- 61 -DPC ) d ( i n r u M C P D , ) c ( . 2 5 ( S A A , ) 1 9 9 1 , ll u r K ( TunceildanTurker ,2002) ,danICP , k k d a d i m u S ( S E A 2005.) Karena konsenrtas i Cr(VI ) n a g n u d n a k n a d L / g µ m a l a d a y n a s a i b r i a l e p m a s m a l a d a k a m , i g g n it a y n s k ir t a m metode anailsi sinsrtumen pelru k u t n u i s a rt n e s n o k a r p e d o t e m n a g n e d n a k g n u b a g i d . a y n i s k e t e d t i m il i k i a b r e p m e m i s a rt n e s n o k a r p k u t n u t a l e h k g n e p n i s e r n a a n u g g n e P n a k g n u b u h i d a s i b a n e r a k n a k t a k g n it i d h i b e l g n a r a k e s n a g n e d FlowI njecitonAnaily iss(FIA )yangt erotomaitsas i . ) 5 0 0 2 , r a w a h u h K ( Keuntungannya bisa meminimalkan s e m u l o v a tr e s a n a h r e d e s h i b e l ,i s a r a p e r p u t k a w ampe ldan .) 5 0 0 2 , k k d a y r a K ( t i k i d e s h i b e l n a k a n u g i d g n a y n e g a e r D A X t il r e b m A n i s e R -16( PSDVB )dipiilhsebaga imateira l n a t u r a l m a l a d a y n n a li b a t s e k a n e r a k m o l o k i n i m i s i g n e p p u k u c g n a y n a a k u m r e p h a r e a d i a y n u p m e m , a s a b n a d m a s a i a g a b e s n a k a n u g i d k o c o c , s a u l pengis ikolomdenganeluen n a g n a li h e k u a t a i s a d a r g e d i d a jr e t a p n a t t a u k m a s a .) 6 0 0 2 , k a p A n a d n i c l a Y ( a y n a m r o f r e p 1 -,5Dfienli -n a d f it k e l e s n e g a e r i a g a b e s i u h a t e k i d ) C P D ( a d i z a b r a k . ir t e m o t o f o rt k e p s a r a c e s ) I V ( r C n a u t n e n e p k u t n u f it i s n e s u ti a n e r a k h e l O tuju an dar ipeneilitanin iuntukmengem -n a d i s a rt n e s n o k a r p k i n k e t i s a u l a v e g n e m n a d n a k g n a b s i s a b r e b ) I V ( m u i m o r k f it k e l e s s i s il a n a Flow Injeciton s is y l a n A menggunakan resin pengkhela tAmbelrtie XAD -6 1 - CD . P Metode i n idiharapkanmemiilk iakurasi ,presisi , l n a d imi tdeteksi ,setra kinejra FIA yang baik sehingga m u i m o r k f it k e l e s k i n e r s i s il a n a k u t n u n a k a n u g r e p i d t a p a d . n a ri a r e p n a g n u k g n il i d t a p a d r e t g n a y.
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t a l A -ala tyang digunakan antara lain :Spekrtofotomete r R I ( r e ir u o F i s a m r o f s n a r T h a r e M a r f n I Presitge-21 Fouire r k u t n u ) u z d a m i h S r e t e m o t o h p o rt c e p S d e r a r f n I m r o f s n a r T r e t e m H p , s i s e t n i s i d g n a y n i s e r k it s ir e t k a r a k n a ij u g n e p a n n a H ( ®) , Pompa peirstalitk (Ismatec) , kolom PTFE n o g y T a p i p , m c 5 g n a j n a p , m m 2 r e t e m a i d ®diamete r0,07 -n a r u l a s k u t n u m c 0 1 , 0 sampe lpereaks ilainnya ,Atomic r e t e m o t o h p o r t c e p S n o it p r o s b A (AASDoubleBeamGBC® t a k g n a r e P , ti l a n a m a l a d ) I V ( r C r a d a k s i s il a n a k u t n u ) 2 0 9 k a n u l Powe rChrom (AD Insrtument® )yang teirntegras i l a ti g i d a r a c e s a t a d t a t a c n e p k u t n u S A A m a l a d .Bahan -g n a y n a h a b digunakan dalam peneilitan in i memiilk i : i r a d i ri d r e t n a d ) a . p ( s i s il a n a o r p n a i n r u m e k t a k g n it K2Cr2O7(s) ,CrCl3.6H2O(s) ,etanol ,aseton(aq) ,HNO3 pekat , H2SO4 pekat ,HC lpekat ,SnCl2(aq) ,NaNO2(s) ,NaOH(aq) , D A X e ti lr e b m A - 61 (s) ,KI(s) ,amlium(s) dibel idar iMerck 5 , 1 i l a u c e k -Dfieni lkarbazida (DPC)(s) dibel idar iSigma . h c ir d l A.
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. 1 . 3 Sintesi sdanKarakteirsas iResinPengkhela tAmbelrtie D A X - 61 - CD P n a k li s a h g n e m t a k e p t a rt i n m a s a n a g n e d i s k a e r e b n e z n e B a l k o c a n r a w r e b g n a y n e z n e b o rt i n tmuda secara lambat . n a g n e d n a k a n a s k a li d a k ij t a p e c h i b e l t u b e s r e t i s k a e R t a k e p t a rt i n m a s a n a r u p m a c n a g n e d n e z n e b n a k s a n a m e m u j a l n a k k i a n e m t a k e p t a fl u s m a s A . t a k e p t a fl u s m a s a n a d n o i u ti a y l if o rt k e l e h a l m u j n a k t a k g n i n e m n a g n e d i s k a e r O N ( m u i n o rt i n 2+) . Prose s reduks i nirtobenzen meng -n a k u k a li d a u t t a l k o c a n r a w r e b g n a y a n i m a li z n e b n a k li s a h l C n S m a g o l m a r a g n a u t n a b n a g n e d 2 dalam HCl ,karena n a k h a b m a ti d a g g n i h e s l C H m a l a d t u r a l r a k u s n e z n e b o rt i n e n e r a n o I . s k u lf e r s e s o r p h a l n a k u k a li d n a d l o n a t e -e m m u i n o z a i d rupakan elekrtoifilk lemah yang bisa g n e m f it k a e r g n a y k it a m o r a a w a y n e s n a g n e d i s k a e r e b -k il if o rt k e l e k it a m o r a i s u ti t s b u S . o z a a w a y n e s n a k li s a h i r a d m u i n o z a i d e n e r a n o i i s k a e R . o z a g n il p o k i s k a e r t u b e s i d D A X e ti lr e b m A -16 (PSDVB ) dengan 1,5-Dfieni l a d i z a b r a k menghaslikan resin pengkela tyang berwarna . n a h a r e m e k t a l k o c Tahapanreaks inirtasi ,reduksi ,diazot-i g il n a g n e d g n il p o k n a d , i s a s andapa tdiilha tpadaGamba r . 1 CH CH2 HNO3 SnCl2 NaNO 2 CH CH2 NH2 CH CH2 NO2 CH CH2 N2+Cl -HCl HCl H2SO4 PSDVB NH NH O NHNH N NH N NHNH O NH CH CH2 + . 1 r a b m a G Tahapan Reaks iSintesi sAmbelrtieXAD- 61 -C P D k u t n u n a k u k a li d s i s e t n i s l i s a h n i s e r i s a s ir e t k a r a K m u rt k e p s n a k r a s a d r e B . s i s e t n i s n a li s a h r e b e k i u h a t e g n e m B V D S P a w a y n e s R I - ON 2 (2a)yang diperoleh dar ihasi l m c 2 6 , 7 2 5 1 a d a p m a j a t n a p a r e s a ti p n a k k u j n u n e m i s a rt i n -1 m c 4 2 , 8 4 3 1 n a d -1 .Keduaptia serapant ersebu tmerupakan g n a li h n a k a n a p a r e s a ti P . o rt i n s u g u g i r a d n a p a r e s a ti p l C n S n a g n e d i s k u d e r n a k u k a li d h a l e t e s 2 dalam HC lyang s u g u g i s k u d e r e m - ON 2 dar i benzen menjad i - HN 2 . B V D S P m u rt k e p S - HN 2 menunjukkan ptia serapan sediki t 6 1 g n a b m o l e g n a g n a li b a d a p m a j a t 08,63 cm-1 yang H N s u g u g k it s ir e t k a r a k n a k a p u r e m 2 pada benzliamina . n a g n a li b a d a p n a p a r e s a ti p n a g n e d g n u k u d i d t u b e s r e t a t a D m c 8 8 , 6 7 2 1 g n a b m o l e g -1 yang merupakan karakteirsitk C n a t a k i -Npadabenzliamina( Gamba r2b) . . 2 r a b m a G Spekrtum Infra Merah PSDVB- ON 2 (a) , B V D S P - HN 2 (b) ,Ambelrtie XAD- 61 -DPC ) d ( i n r u M C P D , ) c ( . 2 5 ( S A A , ) 1 9 9 1 , ll u r K ( TunceildanTurker ,2002) ,danICP , k k d a d i m u S ( S E A 2005.) Karena konsenrtas i Cr(VI ) n a g n u d n a k n a d L / g µ m a l a d a y n a s a i b r i a l e p m a s m a l a d a k a m , i g g n it a y n s k ir t a m metode anailsi sinsrtumen pelru k u t n u i s a rt n e s n o k a r p e d o t e m n a g n e d n a k g n u b a g i d . a y n i s k e t e d t i m il i k i a b r e p m e m i s a rt n e s n o k a r p k u t n u t a l e h k g n e p n i s e r n a a n u g g n e P n a k g n u b u h i d a s i b a n e r a k n a k t a k g n it i d h i b e l g n a r a k e s n a g n e d FlowI njecitonAnaily iss(FIA )yangt erotomaitsas i . ) 5 0 0 2 , r a w a h u h K ( Keuntungannya bisa meminimalkan s e m u l o v a tr e s a n a h r e d e s h i b e l ,i s a r a p e r p u t k a w ampe ldan .) 5 0 0 2 , k k d a y r a K ( t i k i d e s h i b e l n a k a n u g i d g n a y n e g a e r D A X t il r e b m A n i s e R -16( PSDVB )dipiilhsebaga imateira l n a t u r a l m a l a d a y n n a li b a t s e k a n e r a k m o l o k i n i m i s i g n e p p u k u c g n a y n a a k u m r e p h a r e a d i a y n u p m e m , a s a b n a d m a s a i a g a b e s n a k a n u g i d k o c o c , s a u l pengis ikolomdenganeluen n a g n a li h e k u a t a i s a d a r g e d i d a jr e t a p n a t t a u k m a s a .) 6 0 0 2 , k a p A n a d n i c l a Y ( a y n a m r o f r e p 1 -,5Dfienli -n a d f it k e l e s n e g a e r i a g a b e s i u h a t e k i d ) C P D ( a d i z a b r a k . ir t e m o t o f o rt k e p s a r a c e s ) I V ( r C n a u t n e n e p k u t n u f it i s n e s u ti a n e r a k h e l O tuju an dar ipeneilitanin iuntukmengem -n a d i s a rt n e s n o k a r p k i n k e t i s a u l a v e g n e m n a d n a k g n a b s i s a b r e b ) I V ( m u i m o r k f it k e l e s s i s il a n a Flow Injeciton s is y l a n A menggunakan resin pengkhela tAmbelrtie XAD -6 1 - CD . P Metodei n idiharapkanmemiilk iakurasi ,presisi , l n a d imi tdeteksi ,setra kinejra FIA yang baik sehingga m u i m o r k f it k e l e s k i n e r s i s il a n a k u t n u n a k a n u g r e p i d t a p a d . n a ri a r e p n a g n u k g n il i d t a p a d r e t g n a y.
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. 1 . 3 Sintesi sdanKarakteirsas iResinPengkhela tAmbelrtie D A X - 61 - CD P n a k li s a h g n e m t a k e p t a rt i n m a s a n a g n e d i s k a e r e b n e z n e B a l k o c a n r a w r e b g n a y n e z n e b o rt i n tmuda secara lambat . n a g n e d n a k a n a s k a li d a k ij t a p e c h i b e l t u b e s r e t i s k a e R t a k e p t a rt i n m a s a n a r u p m a c n a g n e d n e z n e b n a k s a n a m e m u j a l n a k k i a n e m t a k e p t a fl u s m a s A . t a k e p t a fl u s m a s a n a d n o i u ti a y l if o rt k e l e h a l m u j n a k t a k g n i n e m n a g n e d i s k a e r O N ( m u i n o rt i n 2+) . Prose s reduks i nirtobenzen meng -n a k u k a li d a u t t a l k o c a n r a w r e b g n a y a n i m a li z n e b n a k li s a h l C n S m a g o l m a r a g n a u t n a b n a g n e d 2 dalam HCl ,karena n a k h a b m a ti d a g g n i h e s l C H m a l a d t u r a l r a k u s n e z n e b o rt i n e n e r a n o I . s k u lf e r s e s o r p h a l n a k u k a li d n a d l o n a t e -e m m u i n o z a i d rupakan elekrtoifilk lemah yang bisa g n e m f it k a e r g n a y k it a m o r a a w a y n e s n a g n e d i s k a e r e b -k il if o rt k e l e k it a m o r a i s u ti t s b u S . o z a a w a y n e s n a k li s a h i r a d m u i n o z a i d e n e r a n o i i s k a e R . o z a g n il p o k i s k a e r t u b e s i d D A X e ti lr e b m A -16 (PSDVB ) dengan 1,5-Dfieni l a d i z a b r a k menghaslikan resin pengkela tyang berwarna . n a h a r e m e k t a l k o c Tahapanreaks inirtasi ,reduksi ,diazot-i g il n a g n e d g n il p o k n a d , i s a s andapa tdiilha tpadaGamba r . 1 CH CH2 HNO3 SnCl2 NaNO 2 CH CH2 NH2 CH CH2 NO2 CH CH2 N2+Cl -HCl HCl H2SO4 PSDVB NHNH O NHNH N NH N NHNH O NH CH CH2 + . 1 r a b m a G Tahapan Reaks iSintesi sAmbelrtieXAD- 61 -C P D k u t n u n a k u k a li d s i s e t n i s l i s a h n i s e r i s a s ir e t k a r a K m u rt k e p s n a k r a s a d r e B . s i s e t n i s n a li s a h r e b e k i u h a t e g n e m B V D S P a w a y n e s R I - ON 2 (2a)yang diperoleh dar ihasi l m c 2 6 , 7 2 5 1 a d a p m a j a t n a p a r e s a ti p n a k k u j n u n e m i s a rt i n -1 m c 4 2 , 8 4 3 1 n a d -1 .Keduaptiaserapant ersebu tmerupakan g n a li h n a k a n a p a r e s a ti P . o rt i n s u g u g i r a d n a p a r e s a ti p l C n S n a g n e d i s k u d e r n a k u k a li d h a l e t e s 2 dalam HC lyang s u g u g i s k u d e r e m - ON 2 dar i benzen menjad i - HN 2 . B V D S P m u rt k e p S - HN 2 menunjukkan ptia serapan sediki t 6 1 g n a b m o l e g n a g n a li b a d a p m a j a t 08,63 cm-1 yang H N s u g u g k it s ir e t k a r a k n a k a p u r e m 2 pada benzliamina . n a g n a li b a d a p n a p a r e s a ti p n a g n e d g n u k u d i d t u b e s r e t a t a D m c 8 8 , 6 7 2 1 g n a b m o l e g -1 yang merupakan karakteirsitk C n a t a k i -Npadabenzliamina( Gamba r2b) . . 2 r a b m a G Spekrtum Infra Merah PSDVB- ON 2 (a) , B V D S P - HN 2 (b) ,Ambelrtie XAD- 61 -DPC ) d ( i n r u M C P D , ) c ( .B V D S P n i s e r n a k i s a k i d n i g n e m i n i l i s a H - ON 2 telah B V D S P i d a j n e m i s k u d e ri d l i s a h r e b - HN 2 disetra idengan t a l k o c i d a j n e m a d u m t a l k o c i r a d n i s e r a n r a w n a h a b u r e p s e R . a u t in yang telah drieduks itersebu tsupaya dapa t 5 , 1 n a g il n a g n e d n e l a v o k a r a c e s n a t a k ir e b -dfienlikarbazida . o z a a w a y n e s n a k li s a h g n e m u l u h a d i s a s it o z a i d s u r a h a g g n i h e s C º 4 s a t a i d u h u s a d a p l i b a t s k a d it o z a a w a y n e S s ir e t k a r a k i d k a d it a y n a w a y n e s s i s e t n i s l i s a h as idenganFT -n i s e r m a l a d e k , k u t n e b r e t m u i n o z a i d m a r a g h a l e t e S . R I T F l i s a H . m a d n e ri d n a d C P D n a g il n a k h a b m a ti d - IR D A X e ti lr e b m A - 61 -DPC (Gamba r 2c ) antara lain m c 9 7 , 2 1 7 1 n a p a r e s a ti p n a k k u j n u n e m -1 ,1521,84 cm-1 , m c 5 7 , 2 4 4 1 -1 betrurut-turu t menggambarkan spekrtum n a p a r e s a ti p a t a D . H N n a d , H N C , O = C n a t a k i n a k t a k ii d l i s a h r e b h a l e t C P D n a g il a w h a b n a k t a h il r e p m e m D A X e ti lr e b m A n i s e r n a g n e d n e l a v o k a r a c e s -16 melalu i i n r u m C P D t a u k n a p a r e s a ti P . o z a a r a t n a r e p s u g u g m c 2 9 , 0 0 6 1 n a d 5 3 , 0 7 6 1 a d a p ) d 2 r a b m a G ( -1menunjukkan m c 0 9 , 2 9 4 1 , O = C -1 menunjukkan CNH yang didukung m c 0 2 , 9 3 5 1 n a p a r e s a ti p h e l o -1 .Bukitnya ptia serapan n i s e r n a g n e d n e l a v o k a r a c e s t a k ir e t h a l e t g n a y C P D D A X e ti lr e b m A -16 ,sama sepetr ipada ptia DPC murn i . H N C n a d O = C n a t a k i a y n a d a n a k k u j n u n e m u ti a y . 2 . 3 PengaruhKonsenrtas iH2SO4 terhadapRetens iCr(VI) r o l o k e d o t e m a d a p r u t a r e ti l i d u t S imert i menunjukkan m u i m o r k n a g n e d C P D s k e l p m o k n a k u t n e b m e p a w h a b r e B . ) 2 9 9 1 , m i n o n A ( 5 , 0 ± 2 H p e g n a r a d a p i d a jr e t -H i s a rt n e s n o k h u r a g n e p t u b e s r e t l a h n a k r a s a d 2SO4 i s n e t e r m u m it p o i s i d n o k n a k t a p a d n e m k u t n u i r a j a l e p i d D A X e ti lr e b m A - 61 -DPC terhadap Cr(VI) .Konsenrtas i H2SO4 yangdigunakandalampeneilitani n idar i0,005-0,1 . H i s a rt n e s n o k n a g n u b u h k if a r G 2SO4 dan kapastia sretens i ) I V ( r C s k e l p m o k n a k u t n e b m e p i s k a e r a d a p ) g / g m ( -DPC . 3 r a b m a G a d a p t a h il i d t a p a d . 3 r a b m a G Proif l kapastia sretens iXAD- CD -P Cr(VI ) m a s a i s a rt n e s n o k i s a ir a v a d a p . H i s a rt n e s n o k a d a p a w h a b i t a m a i d t a p a D 2SO4 dar i g / g m n a d t a k g n i n e m a y n i s n e t e r g / g m , i g g n it e k h a d n e r n i k a m e S . M 1 , 0 i s a rt n e s n o k a d a p n u r u n e m i a l u m i s n e t e r H i s a rt n e s n o k i g g n it 2SO4 (semakin rendah pH ) maka n a k u t n e b m e p komplek s yang tejrad ilebih besa rsetra H i s a rt n e s n o k a d a p n a n u r u n e p a y n a d a 2SO4 0,1 M (pH H i s a rt n e s n o K . ) 7 , 0 r a ti k e s 2SO4 opitmumselanjutnyaakan n a t u r a l i a g a b e s n a k a n u g i d car irer .Pengaruh konsenrtas i H2SO4 terhadapkeseitmbanganCr(VI )mengikuitr eaks i :
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H i s a rt n e s n o k a d a P + itngg i(pH relait fasam) ,Cr(VI ) r C k u t n e b r e b g n a y k a y n a b h i b e l 2O72- .Dengan semakin H a y n g n a r u k r e b + ,Cr(VI)l ebihberbentukCrO 42- . . 3 . 3 PengaruhWaktuKontakt erhadapRetens iCr(VI) p a d a h r e t k a t n o k u t k a w h u r a g n e P pembentukan komplek s ) I V ( r C -DPC dipelajar iuntuk mengetahu iseberapa lama e t e r e t t a p a d r a g a ) I V ( r C n o i h e l o n a k h u t u b i d g n a y u t k a w n -.) 4 r a b m a G ( i s . 4 r a b m a G Proif lKapastia sRetens iCr(VI)-DPC pada k a t n o K u t k a W i s a ir a V i a l u m n a k a n u g i d g n a y k a t n o k u t k a W dar i15 meni t / ) I V ( r C g m . ti n e m 0 2 1 i a p m a s gr esinAmbelrtieXAD- 61 -0 6 i a p m a s 5 1 k a t n o k u t k a w i r a d i a l u m t a k g n i n e m C P D 0 9 k a t n o k u t k a w k u t n u r a t a d n e m a r a c e s n u r u t n a d t i n e m n i s e r p a d a h r e t ) I V ( r C g m n a k i a n e k a y n a d A . ti n e m 0 2 1 n a d ti lr e b m A n i s e r n a k a n e r a k i d e XAD- 61 -DPC masih bisa i s n e t e r g / g m n a n u r u n e P . ) I V ( r C h a l m u j e s i s n e t e r e m ) I V ( r C -DPC dan mencapa ikondis ikonstan dikarenakan u p m a m k a d it n a d ) I V ( r C h a l m u j e s h e l o h u n e j h a d u s n i s e r .) I V ( r C i s n e t e r e m i g a l . 4 . 3 PengukuranKapastia sRetens iMetodeBatch a ti s a p a K sretens iresin Ambelrtie XAD- 61 -DPC adalah . ) I V ( r C i s n e t e r e m k u t n u t u b e s r e t n i s e r n a u p m a m e k n a r u k u n i k a m e s , p a r e s i d g n a y ) I V ( r C h a l m u j k a y n a b n i k a m e S e d o t e m a d a P . a y n i s n e t e r s a ti s a p a k r a s e b batch dliakukan m p p 0 3 ) I V ( r C r a d n a t s n a t u r a l i s a rt n e s n o k i s a ir a v sampa i e d o t e m a r a c e s s i s il a n a l i s a h i r a D . m p p 0 0 3 batchdiperoleh D A X e ti lr e b m A n i s e r i s n e t e r m u m it p o s a ti s a p a k - 16 a y n r a s e b m p p 9 5 1 i s a rt n e s n o k a d a p i d a jr e t ) I V ( r C p a d a h r e t . ) 5 r a b m a G ( D A X g / r C g m 4 2 , 2 r a ti k e s . 5 r a b m a G Kapastia sRetens iResinAmbelrtie XAD- 61 -e d o t e M C P D Batch g 1 p a it e s a w h a b i s a m r o f n i n a k ir e b m e m t u b e s r e t a t a D . ) I V ( r C g m 4 2 , 2 i s n e t e r e m t a p a d n i s e r Sebelummencapa i ) I V ( r C i s n e t e r e m t a p a d h i s a m n i s e r m p p 9 5 1 i s a rt n e s n o k n a k a a y n i s n e t e r s a ti s a p a k a g g n i h e s teru s mengalam i m p p 9 5 1 i r a d r a s e b h i b e l g n a y i s a rt n e s n o K . n a t a k g n i n e p 0 1 , 0 2 , 0 3 , 0 0 0,02 0,04 0,06 0,08 0,1 is net er sat is ap aK )g /g m( ) M ( m a s a i s a r t n e s n o K 0 1 , 0 2 , 0 3 , 0 0 30 60 90 120 is net er sat is ap aK )g /g m( ) ti n e m ( k a t n o k u t k a W 0 1 2 0 30 60 90120150180210240270300 s ati sa pa K )g /g m( i sn et er Konsentras iCr( ppm)4 5 ) I V ( r C a y n it r a m a j a t n a t a k g n i n e p n a k k u j n u n e m k a d it . n i s e r h e l o i s n e t e ri d i g a l u p m a m k a d it h a d u s . 5 . 3 PengukuranKapastia sRetens iDinamik a k k i a n e m k u t n u e d o t e m u t a u s h a l a d a i s a rt n e s n o k a r P n . r a d n a t s n a h a b m a n e p a y n a d a a p n a t ti l a n a u t a u s i s a rt n e s n o k i s a rt n e s n o k n a g n e d ) I V ( r C u ti a y t il a n a , i n i e d o t e m i u l a l e M i u l a l e m a y n a r a C . i s k e t e d i d t a p a d h i s a m ) b p p ( h a d n e r i r e t a m u t a u s a d a p u y n it n o k a r a c e s ) I V ( r C i s n e t e r D A X e ti lr e b m A g n u k u d n e p - 61 -DPC yang dimasukkan m e m k u t n U . ri l a m e t s i s u t a u s a d a p m o l o k i n i m m a l a d -n a k u k a li d a y n m u l e b e s , l e p m a s i s a rt n e s n o k a t a d h e l o r e p i s a rt n e s n o k i s a u l a v e n a d k i m a n i d s a ti s a p a k n a r u k u g n e p e d o t e m a d a p k i m a n i d i s n e t e r s a ti s a p a k n a r u k u g n e P . n e u l e ) I V ( r C n a t u r a l n a k a n u g i d m o l o k sebesa r 10 ppm . g n u ti h g n e m a r a c n a g n e d n a k u k a li d i s n e t e r s a ti s a p a K break t n i o p kolom .Dar iGamba r6dapa tdiilha tdar ideitkke- 0 a ri k i a p m a s -kria ke- 61 menunjukkan sinya lyangkonstan , l a y n i s i r a d l a s a r e b i n i l a y n i s car irer .Ga ir sluru stersebu t k a d n a n e m an bahwa resin masih bisa meretens i atau . ) I V ( r C n a h a n e m . 6 r a b m a G Kapastia sRetens iResin Ambelrtie XAD- 61 -m o l o K e d o t e M C P D e k k it e d h a l e t e S -16 tejrad ipeningkatan sinya lyang g n a y i s u l e i d l i s a h r e b g n a y ) I V ( r C l a y n i s n a k i s a k i d n i g n e m a d it m o l o k a y n it r a k mampu lag imeretens iCr(VI) .Tiitk t u b e s i d g n a y h a li n i break point .Penguijan menghaslikan t n i o p k a e r b kolom tejrad isetelah kolom dialri iCr(VI ) u j a l p a d a h r e t i s r e v n o k n a k u k a li d h a l e t e S . k it e d 5 , 6 1 a m a l e s i s e r t a r e b n a d r a d n a t s n a t u r a l i s a rt n e s n o k , ri l a npadakolom . D A X g / r C g µ 1 7 , 4 2 m o l o k i s n e t e r s a ti s a p a k h e l o r e p i d e d o t e m a r a t n a ) I V ( r C i s n e t e r s a ti s a p a k a li B batch dan s a ti s a p a k h e l o r e p i d a k a m n a k g n i d n a b i d m o l o k e d o t e m i n i l a H . li c e k h i b e l m o l o k e d o t e m n a g n e d ) I V ( r C i s n e t e r t n e s n o k a n o z a d a p n a k r a s a d i d ras iyang sama pada itap . i a s e l e s i s k a e r a g g n i h u g g n u n e m k a d it n a d n a r u k u g n e p e d o t e m n a g n e d a y n l a h n i a L batch yang didasarkan pada i s n e t e r t a p a d i d a g g n i h e s n a k i a u s e s i d g n a y u t k a w g n a t n e r . m u m it p o a r a c e s g n u s g n a lr e b g n a y . 6 . 3 Evaluas iKonsenrtas iEluen m o l o k e d o t e m m a l a d a y n n a r e p g n it n e p t a g n a s n e u l E n o i f it a ti t n a u k a r a c e s i s u l e g n e m u p m a m s u r a h a n e r a k D A X e ti lr e b m A n i s e r a d a p i s n e t e r e t g n a y ) I V ( r C - 61 -DPC . r o t k e t e d h e l o i s k e t e d i d a s i b a g g n i h e s Selain tiu ,min iko -n a k a n u g i d a s i b r a g a i s a r e n e g e ri d u lr e p m o l kembail .Efek . n e u l e i s a rt n e s n o k n a d s i n e j h e l o n a k u t n e ti d i s u l e s a ti v it O N H n a g n e d n a k u k a li d ) I V ( r C n a i s u l e g n e P 3 karena dida -O N H m a l a d t u r a l h a d u m g n a y r C m a g o l t a fi s a d a p n a k r a s 3 . O N H i r a d n e g o r d i h n o I 3 akanmengganggusenyawakhela t a r a t n a k u t n e b r e t g n a y resinAmbelrtieXAD- 61 -DPC den -k u t n u i s a m it p o i d u lr e p n e u l e i s a rt n e s n o K . ) I V ( r C n a g r e m k a d it g n a y ) I V ( r C n a i s u l e g n e p i s i d n o k i u h a t e g n e m u -D A X e ti lr e b m A n a t a k i k a s - 61 -DPC dalamkolom .Berda -d t a p a d ) 8 r a b m a G ( h e l o r e p i d g n a y l a y n i s l if o r p n a k r a s -i s n o k a d a p t a h il enrtas iHNO3 1-3 M itdak menunjukkan l a y n i s i g g n it n a k i a n e k i d a jr e t n a d n a k if i n g i s n a a d e b r e p O N H i s a rt n e s n o k a d a p 3 4dan5M .Semakin itngg ikonsen -k a y n a b n i k a m e s a y n it r a , k a c n u p i g g n it n i k a m e s n e u l e i s a rt O N H . i s u l e r e t g n a y ) I V ( r C 3 1-3M itdakdigunakankarena i s u l e r e t m u l e b g n a y ) I V ( r C m a g o l n o i a d a h i s a m a g u d i d O N H n a k g n a d e s , a n r u p m e s 3d iata s5Mj uga itdakdiguna i g g n it u l a lr e t g n a y m a s a i s a rt n e s n o k a n e r a k a n e r a k n a k s e s o r p a g g n i h e s m o l o k i s a r e n e g e r s e s o r p t il u s r e p m e m n a k a n a k il a b m e g n e m k u t n u i s a r e n e g e r keadaankolompada pH n e m t a p a d a g u j n a d a m a l g n u s g n a lr e b n a k a a y n m u m it p o u -n u g i d i n i n a it il e n e p m a l a d i d a J . A I F i r a d a jr e n i k n a k n u r a -O N H n a k 3 5M. . 8 r a b m a G Presis iSinya lCr(VI) . 7 . 3 Presisi i r a d ) 8 r a b m a G ( n a g n a l u h e l o b e k n a k r a b m a g g n e m i s i s e r P ti a y , n a r u k u g n e p u kedekatan antara nlia idata yang satu g n e m n a g n e d h e l o r e p i d g n a y n i a l g n a y a t a d n a g n e d -g n a y s il a n a n a d u t k a w , e d o t e m , n a t a l a r e p , n a t u r a l n a k a n u g . 5 8 6 1 , 0 n a g n u ti h r e p r a s a d r e b i s a i v e d r a d n a t s i a li N . a m a s s u g a b n i k a m e s , i s a i v e d r a d n a t s i a li n l i c e k n i k a M e k bolehulangan pengukuran .Biasanya presis idinyatakan n e s r e p i a g a b e s Relaitve Standard Deviaiton (RSD )atau n o it a i r a V f o t n e i c if f e o C (CV) .Koeifsienvairans i(%KV ) i s a rt n e s n o k k u t n u % 8 6 , 3 r a s e b e s h e l o r e p i d i n i e d o t e m a d a p t a k i d e d o t e m u t a u S . b p p 0 0 5 ) I V ( r C akan mempunya i i s if e o k i a li n a k ij k i a b g n a y i s i s e r p envairansinyal ebihkeci l i r a d 5% .Hasi lyang diperoleh menunjukkan keboleh i r a d g n a r u k g n a y V K % i a li n i r a d t a h il r e t k i a b g n a y n a g n a l u . % 5 . 8 . 3 Limi tDeteksi i m a s s a m u a t a i s a rt n e s n o k n a k a t a y n e m i s k e t e d t i m i L n -i t e m u t a u s h e l o i s k e t e d r e t t a p a d h i s a m g n a y l i c e k r e t m u m o -e D . i g g n it g n a y n a a y a c r e p e k t a k g n it n a g n e d s i s il a n a e d n -h a l m u j n a k a ri k r e p i d t a p a d i s k e t e d t i m il i u h a t e g n e m n a g u t a u s m a l a d n a k h u t u b i d g n a y m u m i n i m l e p m a s i s a rt n e s n o k m n a ir a c n e p a tr e s s i s il a n a s e s o r p etodebaruataupengem t i m il n a k g n i d n a b m e m a r a c n a g n e d a m a l e d o t e m n a g n a b k u t n u i s k e t e d t i m i L . a y n m u l e b e s e d o t e m n a g n e d i s k e t e d 0 1 , 0 2 , 0 3 , 0 0 10 20 30 40 50 60 na br os bA ) k it e d ( u t k a W 4 5 ) I V ( r C a y n it r a m a j a t n a t a k g n i n e p n a k k u j n u n e m k a d it . n i s e r h e l o i s n e t e ri d i g a l u p m a m k a d it h a d u s . 5 . 3 PengukuranKapastia sRetens iDinamik a k k i a n e m k u t n u e d o t e m u t a u s h a l a d a i s a rt n e s n o k a r P n . r a d n a t s n a h a b m a n e p a y n a d a a p n a t ti l a n a u t a u s i s a rt n e s n o k i s a rt n e s n o k n a g n e d ) I V ( r C u ti a y t il a n a , i n i e d o t e m i u l a l e M i u l a l e m a y n a r a C . i s k e t e d i d t a p a d h i s a m ) b p p ( h a d n e r i r e t a m u t a u s a d a p u y n it n o k a r a c e s ) I V ( r C i s n e t e r D A X e ti lr e b m A g n u k u d n e p - 61 -DPC yang dimasukkan m e m k u t n U . ri l a m e t s i s u t a u s a d a p m o l o k i n i m m a l a d -n a k u k a li d a y n m u l e b e s , l e p m a s i s a rt n e s n o k a t a d h e l o r e p i s a rt n e s n o k i s a u l a v e n a d k i m a n i d s a ti s a p a k n a r u k u g n e p e d o t e m a d a p k i m a n i d i s n e t e r s a ti s a p a k n a r u k u g n e P . n e u l e ) I V ( r C n a t u r a l n a k a n u g i d m o l o k sebesa r 10 ppm . g n u ti h g n e m a r a c n a g n e d n a k u k a li d i s n e t e r s a ti s a p a K break t n i o p kolom .Dar iGamba r6 dapa tdiilha tdar ideitkke- 0 a ri k i a p m a s -kria ke- 61 menunjukkan sinya lyangkonstan , l a y n i s i r a d l a s a r e b i n i l a y n i s car irer .Gair sluru stersebu t k a d n a n e m an bahwa resin masih bisa meretens i atau . ) I V ( r C n a h a n e m . 6 r a b m a G Kapastia sRetens iResin Ambelrtie XAD- 61 -m o l o K e d o t e M C P D e k k it e d h a l e t e S -16 tejrad ipeningkatan sinya lyang g n a y i s u l e i d l i s a h r e b g n a y ) I V ( r C l a y n i s n a k i s a k i d n i g n e m a d it m o l o k a y n it r a k mampu lag imeretens iCr(VI) .Tiitk t u b e s i d g n a y h a li n i break point .Penguijan menghaslikan t n i o p k a e r b kolom tejrad isetelah kolom dialri iCr(VI ) u j a l p a d a h r e t i s r e v n o k n a k u k a li d h a l e t e S . k it e d 5 , 6 1 a m a l e s i s e r t a r e b n a d r a d n a t s n a t u r a l i s a rt n e s n o k , ri l a npadakolom . D A X g / r C g µ 1 7 , 4 2 m o l o k i s n e t e r s a ti s a p a k h e l o r e p i d e d o t e m a r a t n a ) I V ( r C i s n e t e r s a ti s a p a k a li B batch dan s a ti s a p a k h e l o r e p i d a k a m n a k g n i d n a b i d m o l o k e d o t e m i n i l a H . li c e k h i b e l m o l o k e d o t e m n a g n e d ) I V ( r C i s n e t e r t n e s n o k a n o z a d a p n a k r a s a d i d ras iyang sama pada itap . i a s e l e s i s k a e r a g g n i h u g g n u n e m k a d it n a d n a r u k u g n e p e d o t e m n a g n e d a y n l a h n i a L batch yang didasarkan pada i s n e t e r t a p a d i d a g g n i h e s n a k i a u s e s i d g n a y u t k a w g n a t n e r . m u m it p o a r a c e s g n u s g n a lr e b g n a y . 6 . 3 Evaluas iKonsenrtas iEluen m o l o k e d o t e m m a l a d a y n n a r e p g n it n e p t a g n a s n e u l E n o i f it a ti t n a u k a r a c e s i s u l e g n e m u p m a m s u r a h a n e r a k D A X e ti lr e b m A n i s e r a d a p i s n e t e r e t g n a y ) I V ( r C - 61 -DPC . r o t k e t e d h e l o i s k e t e d i d a s i b a g g n i h e s Selain tiu ,min iko -n a k a n u g i d a s i b r a g a i s a r e n e g e ri d u lr e p m o l kembail .Efek . n e u l e i s a rt n e s n o k n a d s i n e j h e l o n a k u t n e ti d i s u l e s a ti v it O N H n a g n e d n a k u k a li d ) I V ( r C n a i s u l e g n e P 3 karena dida -O N H m a l a d t u r a l h a d u m g n a y r C m a g o l t a fi s a d a p n a k r a s 3 . O N H i r a d n e g o r d i h n o I 3 akanmengganggusenyawakhela t a r a t n a k u t n e b r e t g n a y resinAmbelrtieXAD- 61 -DPCden -k u t n u i s a m it p o i d u lr e p n e u l e i s a rt n e s n o K . ) I V ( r C n a g r e m k a d it g n a y ) I V ( r C n a i s u l e g n e p i s i d n o k i u h a t e g n e m u -D A X e ti lr e b m A n a t a k i k a s - 61 -DPCdalamkolom .Berda -d t a p a d ) 8 r a b m a G ( h e l o r e p i d g n a y l a y n i s l if o r p n a k r a s -i s n o k a d a p t a h il enrtas iHNO3 1-3 M itdak menunjukkan l a y n i s i g g n it n a k i a n e k i d a jr e t n a d n a k if i n g i s n a a d e b r e p O N H i s a rt n e s n o k a d a p 3 4dan5M .Semakin itngg ikonsen -k a y n a b n i k a m e s a y n it r a , k a c n u p i g g n it n i k a m e s n e u l e i s a rt O N H . i s u l e r e t g n a y ) I V ( r C 3 1-3M itdakdigunakankarena i s u l e r e t m u l e b g n a y ) I V ( r C m a g o l n o i a d a h i s a m a g u d i d O N H n a k g n a d e s , a n r u p m e s 3d iata s5Mj uga itdakdiguna i g g n it u l a lr e t g n a y m a s a i s a rt n e s n o k a n e r a k a n e r a k n a k s e s o r p a g g n i h e s m o l o k i s a r e n e g e r s e s o r p t il u s r e p m e m n a k a n a k il a b m e g n e m k u t n u i s a r e n e g e r keadaankolompadapH n e m t a p a d a g u j n a d a m a l g n u s g n a lr e b n a k a a y n m u m it p o u -n u g i d i n i n a it il e n e p m a l a d i d a J . A I F i r a d a jr e n i k n a k n u r a -O N H n a k 3 5M. . 8 r a b m a G Presis iSinya lCr(VI) . 7 . 3 Presisi i r a d ) 8 r a b m a G ( n a g n a l u h e l o b e k n a k r a b m a g g n e m i s i s e r P ti a y , n a r u k u g n e p u kedekatan antara nlia idata yang satu g n e m n a g n e d h e l o r e p i d g n a y n i a l g n a y a t a d n a g n e d -g n a y s il a n a n a d u t k a w , e d o t e m , n a t a l a r e p , n a t u r a l n a k a n u g . 5 8 6 1 , 0 n a g n u ti h r e p r a s a d r e b i s a i v e d r a d n a t s i a li N . a m a s s u g a b n i k a m e s , i s a i v e d r a d n a t s i a li n l i c e k n i k a M e k bolehulangan pengukuran .Biasanya presis idinyatakan n e s r e p i a g a b e s Relaitve Standard Deviaiton (RSD )atau n o it a ir a V f o t n e i c if f e o C (CV) .Koeifsienvairans i(%KV ) i s a rt n e s n o k k u t n u % 8 6 , 3 r a s e b e s h e l o r e p i d i n i e d o t e m a d a p t a k i d e d o t e m u t a u S . b p p 0 0 5 ) I V ( r C akan mempunya i i s if e o k i a li n a k ij k i a b g n a y i s i s e r p envairansinyal ebihkeci l i r a d 5% .Hasi lyang diperoleh menunjukkan keboleh i r a d g n a r u k g n a y V K % i a li n i r a d t a h il r e t k i a b g n a y n a g n a l u . % 5 . 8 . 3 Limi tDeteksi i m a s s a m u a t a i s a rt n e s n o k n a k a t a y n e m i s k e t e d t i m i L n -i t e m u t a u s h e l o i s k e t e d r e t t a p a d h i s a m g n a y l i c e k r e t m u m o -e D . i g g n it g n a y n a a y a c r e p e k t a k g n it n a g n e d s i s il a n a e d n -h a l m u j n a k a ri k r e p i d t a p a d i s k e t e d t i m il i u h a t e g n e m n a g u t a u s m a l a d n a k h u t u b i d g n a y m u m i n i m l e p m a s i s a rt n e s n o k m n a ir a c n e p a tr e s s i s il a n a s e s o r p etode baruataupengem t i m il n a k g n i d n a b m e m a r a c n a g n e d a m a l e d o t e m n a g n a b k u t n u i s k e t e d t i m i L . a y n m u l e b e s e d o t e m n a g n e d i s k e t e d 0 6 70 0 0 , 0 0 0 , 1 0 0 , 2 0 0 , 3 0 0 , 4 0 0 , 5 1 2 3 ka cn up i gg niT e k n a g n a l u g n e P -4 5 ) I V ( r C a y n it r a m a j a t n a t a k g n i n e p n a k k u j n u n e m k a d it . n i s e r h e l o i s n e t e ri d i g a l u p m a m k a d it h a d u s . 5 . 3 PengukuranKapastia sRetens iDinamik a k k i a n e m k u t n u e d o t e m u t a u s h a l a d a i s a rt n e s n o k a r P n . r a d n a t s n a h a b m a n e p a y n a d a a p n a t ti l a n a u t a u s i s a rt n e s n o k i s a rt n e s n o k n a g n e d ) I V ( r C u ti a y t il a n a , i n i e d o t e m i u l a l e M i u l a l e m a y n a r a C . i s k e t e d i d t a p a d h i s a m ) b p p ( h a d n e r i r e t a m u t a u s a d a p u y n it n o k a r a c e s ) I V ( r C i s n e t e r D A X e ti lr e b m A g n u k u d n e p - 61 -DPC yang dimasukkan m e m k u t n U . ri l a m e t s i s u t a u s a d a p m o l o k i n i m m a l a d -n a k u k a li d a y n m u l e b e s , l e p m a s i s a rt n e s n o k a t a d h e l o r e p i s a rt n e s n o k i s a u l a v e n a d k i m a n i d s a ti s a p a k n a r u k u g n e p e d o t e m a d a p k i m a n i d i s n e t e r s a ti s a p a k n a r u k u g n e P . n e u l e ) I V ( r C n a t u r a l n a k a n u g i d m o l o k sebesa r 10 ppm . g n u ti h g n e m a r a c n a g n e d n a k u k a li d i s n e t e r s a ti s a p a K break t n i o p kolom .Dar iGamba r6dapa tdiilha tdar ideitkke- 0 a ri k i a p m a s -kria ke- 61 menunjukkansinya lyangkonstan , l a y n i s i r a d l a s a r e b i n i l a y n i s car irer .Gair sluru stersebu t k a d n a n e m an bahwa resin masih bisa meretens i atau . ) I V ( r C n a h a n e m . 6 r a b m a G Kapastia sRetens iResinAmbelrtie XAD- 61 -m o l o K e d o t e M C P D e k k it e d h a l e t e S -16 tejrad ipeningkatan sinya lyang g n a y i s u l e i d l i s a h r e b g n a y ) I V ( r C l a y n i s n a k i s a k i d n i g n e m a d it m o l o k a y n it r a k mampu lag imeretens iCr(VI) .Tiitk t u b e s i d g n a y h a li n i break point .Penguijan menghaslikan t n i o p k a e r b kolom tejrad isetelah kolom dialri iCr(VI ) u j a l p a d a h r e t i s r e v n o k n a k u k a li d h a l e t e S . k it e d 5 , 6 1 a m a l e s i s e r t a r e b n a d r a d n a t s n a t u r a l i s a rt n e s n o k , ri l a npadakolom . D A X g / r C g µ 1 7 , 4 2 m o l o k i s n e t e r s a ti s a p a k h e l o r e p i d e d o t e m a r a t n a ) I V ( r C i s n e t e r s a ti s a p a k a li B batch dan s a ti s a p a k h e l o r e p i d a k a m n a k g n i d n a b i d m o l o k e d o t e m i n i l a H . li c e k h i b e l m o l o k e d o t e m n a g n e d ) I V ( r C i s n e t e r t n e s n o k a n o z a d a p n a k r a s a d i d ras iyang sama pada itap . i a s e l e s i s k a e r a g g n i h u g g n u n e m k a d it n a d n a r u k u g n e p e d o t e m n a g n e d a y n l a h n i a L batch yang didasarkan pada i s n e t e r t a p a d i d a g g n i h e s n a k i a u s e s i d g n a y u t k a w g n a t n e r . m u m it p o a r a c e s g n u s g n a lr e b g n a y . 6 . 3 Evaluas iKonsenrtas iEluen m o l o k e d o t e m m a l a d a y n n a r e p g n it n e p t a g n a s n e u l E n o i f it a ti t n a u k a r a c e s i s u l e g n e m u p m a m s u r a h a n e r a k D A X e ti lr e b m A n i s e r a d a p i s n e t e r e t g n a y ) I V ( r C - 61 -DPC . r o t k e t e d h e l o i s k e t e d i d a s i b a g g n i h e s Selain tiu ,min iko -n a k a n u g i d a s i b r a g a i s a r e n e g e ri d u lr e p m o l kembail .Efek . n e u l e i s a rt n e s n o k n a d s i n e j h e l o n a k u t n e ti d i s u l e s a ti v it O N H n a g n e d n a k u k a li d ) I V ( r C n a i s u l e g n e P 3 karenadida -O N H m a l a d t u r a l h a d u m g n a y r C m a g o l t a fi s a d a p n a k r a s 3 . O N H i r a d n e g o r d i h n o I 3 akanmengganggusenyawakhela t a r a t n a k u t n e b r e t g n a y resinAmbelrtieXAD- 61 -DPCden -k u t n u i s a m it p o i d u lr e p n e u l e i s a rt n e s n o K . ) I V ( r C n a g r e m k a d it g n a y ) I V ( r C n a i s u l e g n e p i s i d n o k i u h a t e g n e m u -D A X e ti lr e b m A n a t a k i k a s - 61 -DPCdalamkolom .Berda -d t a p a d ) 8 r a b m a G ( h e l o r e p i d g n a y l a y n i s l if o r p n a k r a s -i s n o k a d a p t a h il enrtas iHNO3 1-3 M itdak menunjukkan l a y n i s i g g n it n a k i a n e k i d a jr e t n a d n a k if i n g i s n a a d e b r e p O N H i s a rt n e s n o k a d a p 3 4dan5M .Semakin itngg ikonsen -k a y n a b n i k a m e s a y n it r a , k a c n u p i g g n it n i k a m e s n e u l e i s a rt O N H . i s u l e r e t g n a y ) I V ( r C 3 1-3M itdakdigunakankarena i s u l e r e t m u l e b g n a y ) I V ( r C m a g o l n o i a d a h i s a m a g u d i d O N H n a k g n a d e s , a n r u p m e s 3d iata s5Mj uga itdakdiguna i g g n it u l a lr e t g n a y m a s a i s a rt n e s n o k a n e r a k a n e r a k n a k s e s o r p a g g n i h e s m o l o k i s a r e n e g e r s e s o r p t il u s r e p m e m n a k a n a k il a b m e g n e m k u t n u i s a r e n e g e r keadaankolompadapH n e m t a p a d a g u j n a d a m a l g n u s g n a lr e b n a k a a y n m u m it p o u -n u g i d i n i n a it il e n e p m a l a d i d a J . A I F i r a d a jr e n i k n a k n u r a -O N H n a k 3 5M. . 8 r a b m a G Presis iSinya lCr(VI) . 7 . 3 Presisi i r a d ) 8 r a b m a G ( n a g n a l u h e l o b e k n a k r a b m a g g n e m i s i s e r P ti a y , n a r u k u g n e p u kedekatan antara nlia idata yang satu g n e m n a g n e d h e l o r e p i d g n a y n i a l g n a y a t a d n a g n e d -g n a y s il a n a n a d u t k a w , e d o t e m , n a t a l a r e p , n a t u r a l n a k a n u g . 5 8 6 1 , 0 n a g n u ti h r e p r a s a d r e b i s a i v e d r a d n a t s i a li N . a m a s s u g a b n i k a m e s , i s a i v e d r a d n a t s i a li n l i c e k n i k a M e k bolehulangan pengukuran .Biasanya presis idinyatakan n e s r e p i a g a b e s Relaitve Standard Deviaiton (RSD )atau n o it a ir a V f o t n e i c if f e o C (CV) .Koeifsienvairans i(%KV ) i s a rt n e s n o k k u t n u % 8 6 , 3 r a s e b e s h e l o r e p i d i n i e d o t e m a d a p t a k i d e d o t e m u t a u S . b p p 0 0 5 ) I V ( r C akan mempunya i i s if e o k i a li n a k ij k i a b g n a y i s i s e r p envairansinyal ebihkeci l i r a d 5% .Hasi lyang diperoleh menunjukkan keboleh i r a d g n a r u k g n a y V K % i a li n i r a d t a h il r e t k i a b g n a y n a g n a l u . % 5 . 8 . 3 Limi tDeteksi i m a s s a m u a t a i s a rt n e s n o k n a k a t a y n e m i s k e t e d t i m i L n -i t e m u t a u s h e l o i s k e t e d r e t t a p a d h i s a m g n a y l i c e k r e t m u m o -e D . i g g n it g n a y n a a y a c r e p e k t a k g n it n a g n e d s i s il a n a e d n -h a l m u j n a k a ri k r e p i d t a p a d i s k e t e d t i m il i u h a t e g n e m n a g u t a u s m a l a d n a k h u t u b i d g n a y m u m i n i m l e p m a s i s a rt n e s n o k m n a ir a c n e p a tr e s s i s il a n a s e s o r p etode baruataupengem t i m il n a k g n i d n a b m e m a r a c n a g n e d a m a l e d o t e m n a g n a b k u t n u i s k e t e d t i m i L . a y n m u l e b e s e d o t e m n a g n e d i s k e t e d 4 5 e k n a g n a l u g n e P
-n a g n e d ) I V ( r C n o i i s a rt n e s n o k a r p e d o t e m F -IAA AS yang r a d n a t s n a t u r a l e m u l o v k u t n u b p p 9 6 h a l a d a h e l o r e p i d . L m 1 ) I V ( r C . 9 . 3 PenentuanLiniertias a k it a m e t a m i s a u l a v e / k if a r g a r a c e s i s a u l a v e i d s a ti r e i n i L ) y u b m u s ( ti l a n a k a c n u p s a u l/ l a y n i s i g g n it a r a t n a t o l p u ti a y a s a i b g n a y ) x u b m u s ( ti l a n a i s a rt n e s n o k i r a d i s g n u f i a g a b e s i n i n a it il e n e p a d a p i s a r b il a k a v r u K . i s a r b il a k a v r u k t u b e s i d t a u b i d dengan memvairasikan konsenrtas ilarutan standa r e p h e l o r e p i d a g g n i h e s b p p 0 0 9 i a p m a s 0 0 1 i r a d ) I V ( r C r -x 7 4 0 , 0 = y s ir a g n a a m a s – 0,705dengankoeifsienkorelas i R2= 0,985 .Konsenrtas iCr(VI )dalam sampe lai ryang , O H W n a k a s a d r e B . b p p 5 8 r a s e b e s h e l o r e p i d kandungan a n e r a K . m p p 5 0 , 0 r a s e b e s ri r e l o ti d g n a y ) I V ( r C m u m i s k a m e d h e l o r e p i d g n a y n a g n a u b m e p n a r u l a s r i a a d a p ) I V ( r C n -n a g n e d f it k e l e s s i s il a n a n a d i s a rt n e s n o k a r p e d o t e m n a g A I F -AAS membeirkan hasi lyang melebih istanda ryang s a k i d n ii d a k a m , O H W n a k p a t e ti d ikantelahtejrad ipence -.t u b e s r e t n a g n a u b m e p n a r u l a s ir a d r i a n a r a m . 0 1 . 3 PerolehanKembail( %Recovery) ( i l a b m e k n a h e l o r e P % recovery )menunjukkan itngka t e k n a h e l o r e P . n a k a n u g i d g n a y e d o t e m i r a d n a i s a r u k a e k m -i s a rt n e s n o k i a li n n a k g n i d n a b m e m n a g n e d n a k u k a li d i l a b e t g n a y t il a n a i s a rt n e s n o k n a g n e d r u k u r e t g n a y t il a n a r l e p m a s ( l e p m a s e k i p s s i s il a n a n a k u k a l e m u ti a y , g n u ti h . a y n i s a rt n e s n o k i u h a t e k i d h a l e t g n a y ) n a t a u b Nlia i% % . % 5 ± 0 0 1 r a s i k r e b h a l a d a k i a b g n a y y r e v o c e r recovery l i s a H . % 0 0 1 r a s e b e s n a g n u ti h r e p l i s a h tersebu tmenunjuk t a k g n it i k il i m e m n a k u k a li d g n a y e d o t e m a w h a b n a k . k i a b g n a y i s a r u k a . 1 1 . 3 Fakto rPengayaan( Enirchmen tFactor) v it i s n e s n a t a k g n i n e p n a k a t a y n e m ) F E ( n a a y a g n e P r o t k a F -i A I F i s a rt n e s n o k a r p e d o t e m s a t -AASdibandingkandengan a p n a t n a r u k u g n e p e d o t e m prakonsenrtasi .Fakto rpengaya -n a k g n i d n a b m e m n a g n e d g n u ti h i d t a p a d n a lsope kurva a v r u k n a d g n u s g n a l a r a c e s ) I V ( r C n a r u k u g n e p i s a r b il a k h e l o r e p i D . i s a rt n e s n o k a r p e d o t e m i u l a l e m ) I V ( r C i s a r b il a k i a li n lsope 0,0234 Absorban /ppm untuk Cr(VI )tanpa t n e s n o k a r p ras idan 0,047Absorban /ppmdenganmetode e m u l o v k u t n u 2 r a s e b e s F E i a li n a g g n i h e s , i s a rt n e s n o k a r p r p e d o t e m , u ti a n e r a k h e l O . L m 1 ) I V ( r C r a d n a t s n a t u r a l a -n a k g n i d n a b i d a k ij f it i s n e s h i b e l i l a k 2 ) I V ( r C i s a rt n e s n o k t n e s n o k a r p a p n a t s i s il a n a e d o t e m n a g n e d rasi .Metodepra -F E i a li n i a y n u p m e m n a k p a r a h i d A I F n a g n e d i s a rt n e s n o k h e l o r e p i d a s i b F E i a li n n a t a k g n i n e P . n i k g n u m r a s e b e s g n a y ) I V ( r C r a d n a t s n a t u r a l e m u l o v n a k k i a n e m n a g n e d . A I F m a l a d n a k a n u g i d . 2 1 . 3 Eifsiens iKonsenrtasi( ConcentraitonEfifciency) o K i s n e i s if E nsenrtas i(CE )menyatakan rentang waktu n a k li s a h i d a g g n i h s i s il a n a i l a k u t a s k u t n u n a k u lr e p i d g n a y t i n e m 0 6 p a it l a y n i s 5 1 h e l o r e p i d i n i e d o t e m a d a P . l a y n i s a y n it r A . ti n e m / 5 , 0 r a s e b e s E C i a li n h e l o r e p i d a g g n i h e s rt n e s n o k i s n e i s if e n a k li s a h i d t i n e m p a it e s as isebesa r0,5 . a w h a b n a k k u j n u n e m m a j r e p i l a k 5 1 n a r u k u g n e p i s n e u k e r F t a p e c p u k u c i n i n a k g n a b m e k i d g n a y e d o t e m s i s il a n a u t k a w u j n a g n e d n it u r a s il a n a k u t n u n a k a n u g i d k a y a l a g g n i h e s m -. k a y n a b g n a y l e p m a s h a l . 3 1 . 3 Indek sKonsumtfi( ConsumpitveI ndex) u s n o K s k e d n I mit f(CI )menyatakaneifsiens isampe lyang e m u l o v n a g n e d t i a k r e t car irerdaneluen yangdigunakan . n a k p a r a h i d A I F n a g n e d i s a rt n e s n o k a r P mempunyai nlia i u t a S . i s k a e r e p i s n e i s if e i a p a c r e t r a g a n i k g n u m l i c e k e s I C i r a d i ri d r e t s i s il a n a i s n e u k e s i l a k car irer- as m -pelcar irer -n e u l e -car irer diperoleh nlia iC I6,5 mL .Ha lin iberatr i u t a s n a k li s a h g n e m g n a y s i s il a n a i s n e u k e s i l a k u t a s k u t n u l e p m a s e m u l o v a k ij i s k a e r e p L m 5 , 6 n a k u lr e p i d l a y n i s . L m 1 n a k a n u g i d g n a y