TP CH KHOA HC, i hc Hu, S 59, 2010

NGHIN CU S TO PHC CA Fe(III) VI 4-(3-METYL-2PYRIDYLAZO) REZOCXIN BNG PHNG PHP TRC QUANG
Nguyn nh Luyn, Nguyn Minh o, Nguyn Hu Hin Trng i hc S phm, i hc Hu

TM TT
S to phc gia Fe(III) vi 4-(3-metyl-2-pyridylazo)rezocxin (3-Me-PAR) c nghin cu bng phng php trc quang. Phc mu Fe(III)-(3-Me-PAR) c t l l 1:2 vi pH ti u t 8,28 n 10,20 v c mt cc i hp th bc sng 498 nm trong khi 3-Me-PAR hp th 418 nm. Phc bn theo thi gian, tun theo nh lut Beer trong mt gii hn rng. C th s dng phc Fe(III) (3-Me-PAR) xc nh vi lng st trong nhiu i tng.

1. M u Thuc th 4-(3-metyl-2-pyridylazo)rezocxin (3-Me-PAR) l thuc th hu c c Tritribabin tng hp nm 1918 v c dng nghin cu to phc mu vi mt s ion kim loi nh: Cu(II), Zn(II), Co(II), Ni(II)[8]. St l mt nguyn t kim loi chuyn tip, rt d to phc vi nhiu thuc th hu c nh: 1- (2-pyridylazo)-2naphtol (PAN), trioxyazobenzen (TOAB), xylen da cam (XO)...[1; 2; 3, 4]. St v hp cht ca n ng mt vai tr rt quan trng trong i sng, sinh hot ca con ngi. V vy, vic xc nh st trong cc i tng ang c s quan tm ca nhiu nh khoa hc trong v ngoi nc. Trong cng trnh ny, chng ti thng bo kt qu nghin cu s to phc gia Fe(III) vi 3-Me-PAR bng phng php trc quang v thm d kh nng s dng phc to thnh phn tch hm lng st. 2. Phn thc nghim Dung dch Fe(III) c chun b t Fe(NO3)3 pha trong nc ct vi s c mt ca HNO3. Nng ca dung dch Fe(III) c xc nh bng phng php chun complexon vi ch th l axit sunfosalixilic. Cc dung dch long hn ca Fe(III) c pha ch t dung dch gc. Dung dch 3-Me-PAR c pha ch t 4-(3-metyl-2pyridylazo)rezocxin bng cch cn mt lng chnh xc trn cn phn tch sau ho tan bng nc ct v nh mc n vch. Cc dung dch long hn c pha ch t dung dch gc. Cc ho cht khc c pha ch t ho cht tinh khit phn tch. pH ca dung dch c o trn my o pH HQ 40D ca hng HACH (M). Mt quang ca dung dch c o trn my DR 5000 ca hng HACH (M).
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3. Kt qu v tho lun 3.1. Hiu ng to phc trong h Fe(III) (3-Me-PAR) Ph hp th electron ca dung dch thuc th 3-Me-PAR v dung dch phc Fe(III) (3-Me-PAR) pH = 9,0 vi CFe(III) = 2.10-5M, C 3 Me PAR = 4.10-5 M c biu din trn hnh 1. Qua hnh 1 cho thy, dung dch 3-Me-PAR c mt quang cc i A = 0,590 ti max = 418 nm, khi to phc vi Fe(III) s hp th ca dung dch mu chuyn v sng di hn v max ca dung dch phc l 498 nm ng vi A = 0,829. Vi s chuyn max v sng di v s tng gi tr mt quang (A) chng t c s to phc n phi t gia Fe(III) vi 3-Me-PAR. Gi tr = 498 nm c chn cho cc nghin cu tip theo.
Ai

0.9 0.8 0.7 0.6 0.5 0.4 0.3 0.2 0.1 0.0

(2)

(1)

(nm)
350 400 450 500 550 600 650

Hnh 1. Ph hp th electron ca dung dch 3- Me-PAR (1) v dung dch phc Fe(III)-(3-Me-PAR) (2)

3.2. S ph thuc mt quang ca phc vo thi gian v pH Kt qu s ph thuc mt quang ca phc Fe(III) (3-Me-PAR) vo thi gian cho thy phc n nh sau 10 pht pha ch v bn theo thi gian. S ph thuc mt quang ca phc vo pH c th hin trn hnh 2, cho thy khong pH ti u cho s to phc t 8,28 - 10,20. Trong cc th nghim tip theo, chng ti thc hin pH = 9,0 v o sau 10 pht pha ch.

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0.9 0.8 0.7 0.6 0.5 0.4 0.3 0.2 4

Ai

pH
5 6 7 8 9 10 11 12

Hnh 2. S ph thuc mt quang ca phc vo pH

3.3. Xc nh thnh phn phc Fe(III) 3-Me-PAR Kt qu xc nh thnh phn phc bng phng php h ng phn t gam c biu din trn hnh 3, bng phng php t s mol trn hnh 4. Qua 2 hnh trn cho thy, t l Fe(III):(3-Me-PAR) = 1:2. Bng phng php Staric-Bacbanen [5] cho kt qu phc l n nhn. Nh vy, iu kin chn, kt qu cho thy: phc Fe(III)-(3-MePAR) c t l to phc l 1:2 v l n nhn.
Ai
0.5

0.4

0.3

0.2

0.1 0 1 9 2 8 3 7 4 6 5 5 6 4 7 3 8 2 9 1 10 VFe3+

V3-Me-PAR

Hnh 3. Xc nh thnh phn phc theo phng php h ng phn t gam

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A i
0.6 0.5 0.4 0.3 0.2 0.1 0.0 0.0

C /C e-PAR Fe 3-M
3+

0.5

1.0

1.5

2.0

2.5

3.0

Hnh 4. Xc nh thnh phn phc theo phng php t s mol

3.4. Nghin cu c ch to phc v xc nh cc tr s , , kp C ch to phc trong h Fe(III) (3-Me-PAR) c nghin cu theo [6], kt qu cho thy ion kim loi i vo phc dng Fe3+, thuc th 3-Me-PAR i vo phc dng R2-. Phng trnh phn ng to phc c th vit : Fe3+ + 2HRFeR2- + 2H+ ; kp

Vy cng thc ca phc l: FeR , ng vi cng thc cu to l: 2

Kt qu tnh , kp ca phc c ghi bng 1, sau khi x l thng k theo [7] ta c lgkp = 9,29 0,29; lg = 31,40 0,46.
Bng 1. Kt qu tnh lgKp v lg ca phc FeR2-

pH 4,75 5,22 5,98 6,43 7,02

CK.105 0,74 1,01 1,37 1,54 1,70

[ Fe3+] 4,24.10-14 1,31.10-15 4,37.10-17 1,42.10

-18

[R2-] 2,04.10-12 9,84.10-12 1,74.10-10 8,27.10

-10

[HR-].106 4,35 8,59 16,30 27,40 31,40

lgkp 9,46 9,57 9,11 9,30 9,00

lg 31,62 31,89 31,01 31,20 31,27

1,57.10-19

2,40.10-9
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3.5. Phng trnh ng chun v xc nh h s hp th phn t gam H s hp th phn t gam ca phc c xc nh theo phng php Komar [6], kt qu thu c FeR = (4,2 0,1).104 l.cm-1.mol-1. Phng trnh ng chun c 2 dng: Ai = 4,18.104 .CFe(III) - 0,01; vi C l nng mol/l. Khong nng phc Fe(III)- (3-Me-PAR) tun theo nh lut Beer l (0,5 4,0).10 M.
-5

4. Kt lun Qua nghin cu s to phc gia Fe(III) vi thuc th 4-(3-Metyl-2-pyridylazo) rezocxin bng phng php trc quang, chng ti rt ra mt s kt lun sau: 1. Phc n phi t Fe(III)-(3-Me-PAR) c cc i hp th bc sng max = 498 nm, pHti u = (8,28 10,20), phc hnh thnh sau 10 pht pha ch v n nh v sau. Bng cc phng php khc nhau xc nh c thnh phn phc Fe(III)-(3Me-PAR) c t l Fe(III): 3-Me-PAR = 1 : 2 v l phc n nhn. 2. nghin cu c ch to phc n phi t, kt qu cho thy: ion kim loi i vo phc di dng Fe3+ cn thuc th 3-Me-PAR i vo phc di dng R2- v phng trnh to phc nh sau: Fe3+ + 2HRFeR2- + 2H+ 3. xc nh c: lgkp = 9,29 0,29; lg = 31,40 0,46; = (4,2 0,1).10 l.cm-1mol-1 ; phng trnh ng chun c dng: Ai = 4,18.104.CFe(III) 0,01.
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TI LIU THAM KHO

1. Lm Ngc Th, Nguyn Phm H, L Th Vinh. Nghin cu s to phc ca Fe(III) vi PAN trong dung dch nc v ng dng. Tp ch Ha hc, tp 38, s 4, (2000), 6-9. 2. Lm Ngc Th, Nguyn Phm H, L Th Vinh. Nghin cu c ch to phc gia Fe(III) vi PAN trong dung dch nc axeton. Tp ch Ha hc, tp 40, s 3, (2002), 20 - 23. 3. Lm Ngc Th, Ng Vn T. Nghin cu s to phc ca Fe(III) vi trioxyazobenzen trong mi trng kim. Tp ch Ho hc, T.31, s 1, (1993), 15-18. 4. Nguyn nh Luyn, Phan Trung Cang. Nghin cu s to phc ca Fe(III) vi Xylen da cam bng phng php trc quang, Tp ch Khoa hc & Gio dc, Trng HSP Hu, s 01, (2007), 35-39. 5. H Vit Qu. Cc phng php phn tch quang hc trong ho hc, NXB HQG H Ni, 1999. 85

6. H Vit Qu. Phc cht trong ho hc, NXB Khoa hc v K thut, H Ni, 2000. 7. Doerffel. Thng k trong ha hc phn tch, NXB i hc v Trung hc chuyn nghip, H Ni, (1983). 8. Bottomley F, Geary W.J. Steric Hindrance effects in the use of heterocylic azodyestuffs as spectrophotometric reagents, Pergamon Press Ltd, Vol 14, (1967), 537-542

STUDY ON THE COMPLEXATION OF Fe(III) WITH 4-(3-METHYL-2PYRIDYLAZO) RESORCINOL BY SPECTROPHOTOMETRIC METHOD

Nguyen Dinh Luyen, Nguyen Minh Dao, Nguyen Huu Hien College of Pedagogy, Hue University

SUMMARY
The complexation of Fe(III) with 4-(3-methyl-2-pyridylazo)resorcinol (3-Me-PAR) has been investigated by spectrophotometric method. The coloured Fe(III)-(3-Me-PAR) complex, with the composition of 1:2, is formed most favourably at the pH value of 8,28 10,20 and has an absorption maximum at 498 nm whereas that of 3-Me-PAR is at 418 nm. It was shown that the complex of Fe(III) (3-Me-PAR) is stable with time in accordance with the Beer Law in a rather large limit interval, which could, therefore, be utilized for microdetermination of Fe from different resources.

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