263jafia/english/jfia/contents/10_2/jfia1993v0010… · year of publication ' - fig.1...

J. Flow Injection Anal. , Vol. 10, No .2 (1993)

O n - l i n e Column S e p a r a t i o n a n d P r e c o n c e n t r a t i o n i n Flow I n j e c t i o n

A n a l y s i s

K o i c h i Oguma

L a b o r a t o r y f o r A n a l y t i c a l C h e m i s t r y , F a c u l t y o f E n g i n e e r i n g ,

U n i v e r s i t y o f C h i b a

Y a y o i - c h o , I n a g e - k u , C h i b a , 2 6 3 J a p a n

The u s e of o n - l i n e c o l u m n s e p a r a t i o n a n d p r e c o n c e n t r a t i o n i n f l o w

i n j e c t i o n a n a l y s i s i s r e v i e w e d . The l i t e r a t u r e s u r v e y r e v e a l s t h a t t h e

d e v e l o p e d m e t h o d s f o r t h e o n - l i n e s e p a r a t i o n a n d p r e c o n c e n t r a t i o n h a v e

g r e a t e l y i m p r o v e d t h e s e n s i t i v i t y a n d s e l e c t i v i t y o f f l o w i n j e c t i o n

a n a l y s i s .

year o f publication F i g . 1 D e v e l o p m e n t o f t h e l i t e r a t u r e p u b l i s h e d ' - a b o u t o n - l i n e p r e c o n c e n t r a t i o n i n a t o m i c s p e c -

ffl, A-7 &jg^. &'BE @ t r o m e t r y ( b a s e d on t h e number o f p a p e r s h a v i n g - a p p e a r e d i n C h e m i c a l A b s t r a c t s up t o 1 9 9 0 ) ~ < 0 7 ) ~ - - 7 Â ¡ i ~ B %

aT. 4 2 9 x 9 9 3 > F i g . 2 F l o w - i n j e c t i o n m a n i f o l d f o r T h and U.

AIl/7'<Ã Â¥ >YIl//I/-Y C=3.6 H HC1; R = Z X I O - ~ N ArsenazoXII - 1 % T r i t o n X - 1 0 0 - 3 . 6 N HC1; P=pump; P C = p r e c o n c e n t r a t i o n

ofiz % 9 f^ if 7 2% 4 0 co lumn; R C = r e d u c t i o n co lumn; L l = b y - p a s s c o i l 9 > (VI)% 9 > ( 5 0 cm); L 2 = r e a c t i o n c o i l ( 5 0 cm); D = d e t e c t o r ;

W=waste. ;:3Â¤zt-5KttMO*

$ Ã ˆ f i A?:$ >-7Â¡%ff141T%-f Â¥%i-:All-7' i n j e c t i o n p o s i t i o n I= L.

4 ^ g i L k ^ L - n ^ - - --

^ ~ & - 4 i ( O j h ' ) ' ! 7 k ?I in out

1 1 Â ¥ > A O S 4 % > % i ^ 4 > S @ f i T &(TOSOH 1 C is

F f >, 12 mm x 2 . 5 om F i g . 3 Cation-exchanger column. A=PTFE f e r r u l e ;

i ' d ' b F i g ' 3 s')T'B B = f i l t e r ( p o r e s i z e 2 pm); C=Pl'FE t u b i n g ( 0 . d . L, 9 7 9 > x - T ) b f c % 1.6 am, i . d . 0 .5 MB); D=cation exchanger.

NPt-f$> TBPE(7 h 7 - 7 ' Column was composed of poly ( c h l o r o t r i f luoro- e t h y l e n e ) .

0.45 urn Piter PUMP

Sample I 1 1 t

0.075 N HCL 1.1 &HQ COI.

*%"gC>2 5cm-

mlfmln

PMT

U WASTE v

COMPUTER &

CHART RECORDER

$ ~ { ; , B & + ( o ~ ( I I ) E F i g . 4 R e a c t i o n m a n i f o l d f o r F I A - C L d e t e r m i n a t i o n o f i r o n i n s e a w a t e r .

^^ffT^tt^aSafci&l

waste

10 m knitted reaction coil in column

heater

'fJi'ET'k'* F i g . 5 FIA m a n i f o l d f o r preconcentrat ion ,LMG fc 1 7 1 BkfZ/ I^V 7 - / 8 - d e t e c t i o n o f Mn2+ i n s e a w a t e r ( u p p e r ) and

* I 1 ) V - 7 1 ' < D 3 ( 7 7 A K j : 8 - q u i n o l i n o l c o l u m n ( 1 o w e r ) .

k M L f i M % i i L T m @ S ; ? % & b T 50 ^ l O 2 HHNOs T ? & a i L 7 7

b - A A A S t z k 9 S f i T - 5 < ! t S S & S f t T b - S 0 5 ~l O % S } Â ¤ % % B U ? B ~ ^ ~ Z

b - 5 t @ f f l R g 5 ? ( 3 ( r ) Ã 1 0 n g P b / m l T f e - S $ , % J i g * O i f i H # B # l ' f S t l Â ¥ C

t3b18)o -&$. k l B H I 2 U I - 5 L 8HOQFR i: 8HOQFHQ ? ; 7 b T Ã ˆ . @ I O ? ~ i f f i i : f

S t ~ 7 b - S ~ pH 2 - 3 . 5 f c M L f i I i i S ; M B 15 m l %Mb. 5 k k M O f i 7 A

fc@B$Â¥&2IB-Â 5 0 ,u1 O 0 . 5 M H C 1 T B a i L T - 7 I / -AAAST?MF!ZT-5 k @

X M ( 3 c ) Ã 5 ngCu/ml T & a o za%&%%S;R-03@ffltt t t&l ' t ;?ft~b ^ ^ ' 9 ) 0

O b a t a 6 20)k F i g . 6 fc5-f j; -? k . ? S A 4 Ã ˆ O % ( I I I ) O i S ! % @ s h i p b o a r d

CLEANING SOLN. (MOW) WASTE

CLEANING SOW. (0.5M HO) -d -=--+% rwm 0.2M H a SOW. = I 1

I I I LUMINOL SOLN. -

I I

0.4M NH4OH SOLN. - @-, I

1 1

F i g . 6 F low c o n c e n t r a t i o n a n d C L d e t e c t i o n s y s t e m s f o r a u t o m a t i c d e t e r m i - n a t i o n o f i r o n ( I I I ) i n s e a w a t e r . P = P e r i s t a l t i c p u a p ( d a s h e d l i n e m e a n s i n t e r l o c k i n g ) ; S = s o l e n o i d v a l v e ( N O = n o m a l o p e n , NC=nomal c l o s e d , I N = i n l e t ) ; C=HAF-8HQ r e s i n c o l u ~ n ; R C = r e a c t i o n c o i l ; C L = C L d e t e c t i o n c e l l : H V = h i g h - v o l t a g e s u p p l y ; R = r e c o r d e r ; F = f l o w m e t e r .

a n a l y s i s O f t & . MAF-8HQ (8-quinolinol-innobilized f l u o r i d e c o n t a i n i n g

O M . %@OL+Y$@kT&@T&-3 k o 18 m l <OJiSM%fi(3 MAF-8HQA

= f A ( 5 0 ma x 4 mm i . d . ) t ; : M L & % & 0 . 2 H KC1 T?S@EL. @jS@iffb)I/5

I - I l / - % M & M O f k M m T Ã ˆ LT, 0 . 0 5 nM O @ f f i M - & R f i o Z

-&M 15 n l O O D s & 5 A I : %

L , i @ b T ~ 9 Y - I b T 8 k % ,

F f t % S t ^ i ' S S T * t f B X M % 5 3 ( 4 0 P l)*#A%(F<i:MBL

7 ( e l u a t e z o n e s z m p l i n g ) S B ' ? '

-SG & % t S & T b ' s o 3 m l 0% R T O M R & & H : f i 20, BffiRB %kt 0 . 8 n g C d / l , 12 n g C o / l , 1 7

n g C u / l , 6 . 5 n g P b / l . 3 6 n g N i / l

Sample Loading

'^!I8 Ãˆ*aÃ‡@ÃˆÃˆri F i g . 7 F I m a n i f o l d f o r o n - l i n e s o r b e n t T SF^ii%'S-f@T V t -5 " l o S k, e x t r a c t i o n c o l u m n p r e c o n c e n t r a t i o n .

P I , P p P u m p s ; ! = i n j e c t o r v a l v e ; C = c o n i c a l *'^^ ' A (w) c o l u m n p a c k e d w i t h C , . s o r b e n t ; W=was te ; UAO#igg%S@@&E '&He& R = r e a c t i o n c o i l ( 4 0 m m x 0 . 5 m m i . d . ) ; T=

t r a n s p o r t c o n d u i t ( 2 5 0 m m x 0.35 m m i . d . """' l 2 k n o t t e d r e a c t o r ) ; RAS=flam@ a t o m i c a b s o r p -

- h V I. Preconcentration 111. Elution

11. Derivatization IV. Washing * ^ A

E to GC b GC

: % 53 s w w L T b

M A W B w

5 M

^ ^ < k w - - - w

â‚ %- - -

T 1'9 Fig.8 Flow manifold used in on-line preconcentration-deriva-

X ^ /I/ tization of organotin compounds. B=Buffer; E=eluent; S=sample: R=derivatizing reagent; H=methanol; A=air; P=peristaltic pump;

'"}"Ã 9 @ V , ,Va=six-way valves; V 3 - V ~ = t h r e e - w a y valves; C=preconcentration

9- \) microcolumn; W = t o waste.

~ A - Â £ , R ~ ( s ~ ~ T X F J I / < ~ L s ^ , - ~ * ~ A ; & - H K ~ ~ w p2 c

T ^ m ^ ^ c } Â ¤ X % % ^ 7 1)-GCl~gfcL. B I S L f e X ~ L & Ã ˆ & - 7 - r ? a % 7 ' 7 %

~ l K T % X K c k ( H * B l t < 5 0 10- 15ml(o%Ãˆf1 25 htf-k-&

T. @XRS%O.l ng/lSjtfiE Waste

^^T^'S^ 'o Fig.9 Manifold for t h e trace enrichment of 7, f- V 2 -9 t* . /l/4 > 4Y gold using a supported liquid membrane (SLH).

PI, PZ=Peristaltic pumps; RC=reaction coil; '~@'B(Polysorb "-') I U , 1 ~ 2 = i n j e c t i o n valves; C=iicrocolumn %j@f i t t@S#2 L T, 97 packed with Polysorb MP-1; B=buffer stream;

E=elution solvent (methanol) ; O=organic phase; XbaSiaSa't' (O'*SB s=saiple stream; \=water. ~ f f i f f l S f t 7 b - S (Fig.9 %%

U S ) , ZO%&K. % Â ¥ r M H W A W f i ( l ~ 1 ) O#!llXffl?g%%gSL, M

4 . ÔffiOl%Ãˆffl*7A<0ffl

Z%o%ft/s~: kt. ?(0âKffcft!8l+!kM)8St:A !)%I, < H - f c - 5 ~ f c f i 6 . % ~ ~ M ( D ~ ~ ~ P ~ M ~ A % , % M H W T C W M V J .

-9 3 > t: F I A ~ L t 2 L ~ i g H S f t T - S o J i a n S 3 ' ) I 3 , sulphydryl c o t t o n

O ~ ~ ~ A % * H % + O Ã ˆ E B o~tksa~:?~~ L** ~ * i s a , f i 7 A i : % Ã ˆ ? f t T S n C l 2 T S Z $ t i f f l B a i $ t i k 0 - & ~ ? % ) f c % T ~ x $ f l

2 5 , ?13&izl%S$hft%+)b?K M 3 H HC1 7% 8 ,, Br-/Br03- TBSfti?

ft^(o'&z7C?ftâ*ffi&l^î:^ffi?ft-S, %~~l/*^(0!!5(%Ãˆ07Â¡~'f

B f t S 0 A 3 R i l f J T - S ' & O t ~ A S t i T b - S 0 0 0 11 D e p o s i t i o n 11

C6HgO4CCH2SH + CHaHgCl- ^ C e H g O 4 C C H 2 S H g C H s + H C 1 E l u t i o n

Sample Loading m

2 . 4 %M T b 6 33'o F i g . 1 0 M a n i f o l d f o r o n - l i n e p r e c o n c e n t r a t i o n

4ÃˆttcW@ft/+ 7 4 >(of1 o f Cr(1II) a n d C r < V I ) . V = I n j e c t o r v a l v e ; P I , P 2 = p e r i s t a l t i c pumps; C = m i c r o c o l u ~ ) n p a c k e d

. 12 @Â¥f h '1 -n-^- 9 f- w i t h a c t i v a t e d a l u ~ i n a ( a c i d i c for^)-; Ã ˆ = w a s t e

7.7 a A ~ J S B ~ ~ &bkm AAS=flame. a t o m i c a b s o r p t i o n s p e c t r o m e t e r .

1) V . C a r b o n e l l , A . S a l v a d o r , H. d e l a G u a r d i a : F r e s e n i u s ' J . A n a l .

Chem., 342, 5 2 9 ( 1 9 9 2 ) .

2) H . V a r c d r c e l , H.. Dl Luque d e C a s t r o : N o n - c h r o n a t o g r a p h i c C o n t i n u o u s

S e p a r a t i o n T e c h n i q u e s , T h e R o y a l S o c i e t y o f C h e m i s t r y ( 1 9 9 1 ) .

3 ) Z . F a n g : F low I n j e c t i o n S e p a r a t i o n a n d P r e c o n c e n t r a t i o n , VCH,

W e i n h e i a ( 1 3 9 3 ) . - >

4) H. D . Luque d e C a s t r o , H. T. T e n a : T a l a n t a , 4 0 , 21 ( 1 9 9 3 ) .

5 ) J . L. P. ~ a v o n , C . G . P i n t o , E . R . G a r c i a , B . H . C o r d e r o : A n a l .

C h i n . A c t a , 2 6 4 , 2 9 1 ( 1 9 9 2 ) .

6) Z. F a n g , 1. S u n , E. H. H a n s e n , J . E. O l e s e n , L . M. H e n r i k s e n :

T a l a n t a , 3 9 , 3 8 3 ( 1 9 9 2 ) .

7) R . K u r o d a , K . Oguna , K . K i t a d a , S . Kozuka : T a l a n t a , 38, 1 1 1 9 ( 1 9 9 1 ) .

8) H. J . S a l a c i n s k i , P. G . R i b y , S . J . H a s w e l l : A n a l . C h i n . A c t a , 2 6 9 ,

1 ( 1 9 9 2 ) .

9 ) S B ilfL * * g = : 53ftft9, 4 0 , T I 0 7 ( 1 9 9 1 ) .

1 0 ) K. Oguma, K . K i t a d a , R . K u r o d a : M i k r o c h i m . A c t a , 1 1 0 , 7 1 ( 1 9 9 3 ) .

11) E. H . P e d r a z z i , R. E. S a t e l l i : T a l a n t a , 4 0 , 5 5 1 ( 1 9 9 3 ) .

1 2 ) P. S c h r a m e l , L. Xu, G . Knapp, H. H i c h a e l i s : M i k r o c h i m . A c t a , 1 0 6 ,

1 9 1 ( 1 9 9 2 ) .

1 3 ) MM, J . W . H c L a r e n , S. S . Berman: f i f f f k q , 4 2 , 4 2 3 ( 1 9 9 3 ) .

1 4 ) B. D a i h , H . Huang: A n a l . Chim. A c t a , 2 5 8 , 245 ( 1 9 9 2 ) .

1 5 ) K. H . C o a l e , K . S . J o h n s o n , P. H. S t o u t , C . M . S a k a m o t o : A n a l . Chim.

A c t a , 2 6 6 , 3 4 5 ( 1 9 9 2 ) .

1 6 ) V. A . E l r o d , K . S . J o h n s o n , K . H. C o a l e : A n a l . Chem., 63 , 8 9 3

( 1 9 9 1 ) .

1 7 ) J . A . R e s i n g , H. J . M o t t l : A n a l . Chem., 6 4 , 2 6 8 2 ( 1 9 9 2 ) .

18) R . P u r o h i t , S . D e v i : A n a l . Chim. A c t a , 2 5 9 , 5 3 ( 1 9 9 2 ) .

1 9 ) R . P u r o h i t , S . D e v i : T a l a n t a , 3 8 , 7 5 3 ( 1 9 9 1 ) .

20) H. O b a t a , H. K a r a t a n i , E . Nakayama: A n a l . Chem., 6 5 , 1 5 2 4 ( 1 9 9 3 ) .

21) E . o l b r y c h - $ l e s z y f i s k a , K . B r a j t e r , W . H a t u s z e w s k i , H . T r o j a n o w i c z ,

W . F r e n z e l : T a l a n t a , 3 9 , 7 7 9 ( 1 9 9 2 ) .

22) P. ~ e r n g n d e z , C. P . C o n d e , A . G u t i e r r e z , C . Csmara : T a l a n t a , 3 8 ,

1 3 8 7 ( 1 9 9 1 ) .

23) H. E m t e b o r g , D. C . B a x t e r , W . F r e c h : A n a l y s t , 118, 1 0 0 7 ( 1 9 9 3 ) .

24) Z. F a n g , T. Guo, B . Welz : T a l a n t a , 3 8 , 6 1 3 ( 1 9 9 1 ) .

2 5 ) H. S p e r l i n g , X . Y i n , B. Welz: F r e s e n i u s ' J . A n a l . Chem., 3 4 3 , 7 5 4

( 1 9 9 2 ) .

26) H. S p e r l i n g , X . Y i n , B. Welz: A n a l y s t , 1 1 7 , 6 2 9 ( 1 9 9 2 ) .

27) B. W e l z , M . S p e r l i n g , X . Sun: F r e s e n i u s ' J . A n a l . Chem., 3 4 6 , 5 5 0

( 1 9 9 3 ) .

28) Y. M a d r i d , M. Wu, Q. J i n , G . M. H i e f t j e : A n a l . Chim. A c t a , 2 7 7 , 1

( 1 9 9 3 ) .

29) J . ~ z p u n a r - k o b i h s k a , M . C e u l e m a n s , R . t o b i n s k i , F. C . Adams: A n a l .

Chim. A c t a , 2 7 8 , 99 ( 1 9 9 3 ) .

3 0 ) M. J . C . T a y l o r , D. E. B a r n e s , G . D. M a r s h a l l : A n a l . Chim. A c t a ,

3 1 ) W . J i a n , C . W . McLeod: T a l a n t a , 3 9 , 1 5 3 7 ( 1 9 9 2 ) .

3 2 ) H. S p e r l i n g , S . Xu, B. Welz: A n a l . Chem., 6 4 , 3 1 0 1 ( 1 9 9 2 ) .

33) C. R . H. P e i x o t o , Y . G u s h i k e m , N. B a c c a n : A n a l y s t , 1 1 7 , 1 0 2 9 ( 1 9 9 2 ) .

3 4 ) W. Q i , X. Wu, C. Zhou , H . Wu, Y . Gao: A n a l . Chim. A c t a , 2 7 0 , 205

263jafia/english/jfia/contents/10_2/jfia1993v0010… · year of publication ' - fig.1...

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