TP CH KHOA HC V CNG NGH, I HC NNG - S 3(26).

2008

IU KIN TI U XC NH HM LNG ION ORTHOPHT PHT TRONG NC BNG PHNG PHP QUANG PH HP TH PHN T UV-VIS
OPTIMAL CONDITIONS FOR DETERMINING THE AMOUNT OF NO3-, PO43- IN SURFACE WATER BY SPECTROPHOTOMETER ABSORBANCE UV-VIS MOLECULE METHOD PHM TH H
Trng i hc S phm, i hc Nng
TM TT Bi bo trnh by kt qu xc nh cc iu kin ti u, phng php loi b cc yu t nh hng n php o v lp dng quy trnh phn tch hm lng ion 3orthophotphat PO4 trong nc bng phng php quang ph hp th phn t UV-VIS. ABSTRACT The report presents the results from the determination of optimal conditions, a method for eliminating the affective factors to measure and establish a suitable 3process for analyzing the concentration of ion orthophosphate PO4 in the surface water by spectrophotometer absorbance molecule method UV-VIS.

1. M u Phng php quang ph hp th phn t UV-VIS l phng php phn tch dng c nhanh, chnh xc v khng qu t tin xc nh hm lng ion orthophotphat PO43- trong nc. C s cho php phn tch ion orthophotphat trong nc l cho ion ny kt hp vi amoni molipdat trong mi trng axit to ra hp cht d a axit photphoromolypdat, n lt hp cht ny c th b kh bng nhiu thuc th khc nhau nh thic(II), ng, hidroquynon... to ra phc mu mnh gi l Xanh molipden, m mu ca dung dch t l vi hm lng ion orthophotphat trong mu. Xanh molipden thng c coi l mt polime phc tp, cu to t hn hp ca Mo(V) v Mo(VI), qu trnh to thnh phc thng to ra cc sn phm ph khng mong mun, do phn ng phi c tin hnh v quan st cn thn trong cc iu kin thch hp m bo tin cy ca kt qu phn tch. Cng vi phng php dng SnCl2 lm tc nhn kh, phng php dng ng kh cng thng c s dng, tuy nhin phn ng xy ra chm, phi un nng mt thi gian nht nh nhit khong 60oC n 70oC phc to mu n nh, ngoi ra kt qu o thng b nh hng ca cc ion st v asen. Di y l kt qu kho st, tm cc iu kin ti u cho hai quy trnh phn tch ny.

106

TP CH KHOA HC V CNG NGH, I HC NNG - S 3(26).2008

2. Nguyn liu v phng php 2.1. Thit b, dng c v v ha cht 2.1.1. Dng c v thit b My quang ph hp th phn t UV- VIS: Jasca V- 530; Cn phn tch Precisa XT 220- A v cc dng c thy tinh 2.1.2. Ha cht Dung dch thuc th sunfomolipic A v dung dch thuc th sunfomolipic B; Dung dch H2SO4 5N; Dung dch thic clorua SnCl2 0.05M (chun b ngay khi s dng); Dung dch FeCl3 0.1g/l; Dung dch NaF 0.1g/l; Dung dch gc photphat 0.1g/l (100ppm) v cc dung dch lm vic. 2.2. Phng php nghin cu Quy trnh phn tch c thc hin trn cc mu gi l cc dung dch cha ion PO43- c hm lng chnh xc, t chng ti tm cc iu kin ti u, cc yu t nh hng cng nh cch loi b cc yu t nh hng . Trong quy trnh xc nh ion orthophotphat PO43- vi tc nhn kh l thic clorua, chng ti kho st chn thi gian to phc v lng cc thuc th ph hp. Quy trnh xc nh ion orthophotphat PO43- vi tc nhn kh l ng li thng b nh hng bi s c mt ca ion Fe3+ , nn ngoi vic kho st chn thi gian to phc ph hp, chng ti tin hnh kho st s nh hng ny v tm cch loi b nh hng bng cch thm vo mu 1 lng ion F-, nhm to phc bn vi ion Fe3+ nu c mt trong mu. 3. Kt qu v tho lun 3.1. iu kin ti u phn tch theo phng php dng thic(II) clorua 3.1.1. Kt qu kho st thi gian n nh phc mu kho st thi gian thch hp cho qu trnh, chun b 9 0.25 dung dch chun PO43- c nng 0.2 0.5mg/l, thm mt lng thuc 0.15 th amoni molipdat v SnCl2, phn ng to phc mu gia 0.1 thuc th v ion phn tch xy ra 0.05 trong khong t 5 n 45 pht, o 0 mt quang bc sng max 0 10 20 30 40 50 l 690nm. Kt qu o ca cc Thi gian, pht mu c th hin hnh 1. Kt qu thc nghim cho Hnh 1. S ph thuc mt quang thy, xanh molypden c thi gian ca dung dch vo thi gian to phc n nh mu t 10 n 30 pht. Vi cc mu c thi gian ln hn 30 pht th mu dung dch thay i, ng thi
Mt quang D

107

TP CH KHOA HC V CNG NGH, I HC NNG - S 3(26).2008

dung dch khng thu quang nn khng ph hp cho php o mt quang. Thi gian to phc mu cho cc th nghim sau c chn l 20 pht. 3.1.2. Kt qu kho st lng thuc th amoni molipdat kho st lng thuc 0.2 th amoni molypdat thch hp 0.15 cho qu trnh, chun b 7 dung 3dch chun PO4 c nng 0.1 0.5mg/l, thm SnCl2 v cc lng 0.05 amoni molipdat khc nhau, 20 pht phn ng to phc mu 0 0 0.2 0.4 0.6 0.8 1 xy ra hon ton gia thuc th 3Lng thuc th, ml v ion PO4 , o mt quang bc sng max = 690nm. Kt qu o c th hin hnh 2. Hnh 2. S ph thuc mt quang ca Kt qu thc nghim cho dung dch mu vo lng thuc thy, nu ly lng thuc th qu th Amonimolipdat t, mt quang o c nh, nguyn nhn l thiu thuc th. Tuy nhin vi lng ln hn nhiu th gi tr mt quang o c cng gim, ng thi mu dung dch khng n nh. Lng ph hp vi 10 ml nc mu l 0.5ml Amonimolipdat, tng ng vi hm lng 0.025g/l. 3.1.3. Kt qu kho st lng thuc th thic diclorua kho st lng thuc 0.3 th SnCl2 thch hp cho qu trnh, 0.25 chun b 7 dung dch chun PO430.2 c nng 0.5mg/l, thm 0.5ml 0.15 Amonimolipdat v thm cc 0.1 0.05 lng SnCl2 khc nhau, 20 0 pht cho phn ng to phc mu 0 0.05 0.1 0.15 0.2 0.25 xy ra hon ton gia thuc th Lng thuc th, ml v ion phn tch, o mt quang bc sng max = 690nm. Kt Hnh 3. S ph thuc mt quang ca qu thc nghim trnh by hnh dung dch mu vo lng thic iclorua 3. Mt quang ca mu o c rt thp nu ly lng SnCl2 t hn 0.05ml. Vi lng thuc th t 0.1ml SnCl2 th mu ca dung dch mu khng i, cc gi tr o c n nh. Do la chn lng ph hp nht ly vi 10 ml nc mu l 0.15ml SnCl2, tng ng vi nng 0.14g/l. Qua cc kt qu kho st, quy trnh phn tch xut nh sau: (1). Ly 10 ml mu nc cn phn tch (nu hm lng PO43- trong dung dch ln hn 6mg/l phi pha long);(2).Thm 0.5ml dung dch amonimolipdat. (3). Lc u v yn trong vng 5 pht. (4). Thm 0.15ml dung dch SnCl2. (5). khong 15 pht ri
Mt quang D
Mt quang D

108

TP CH KHOA HC V CNG NGH, I HC NNG - S 3(26).2008

o mt quang ca dung dch bc sng 690nm. Da vo ng chun xc nh nng ca octhophotphat trong dung dch. 3.2. iu kin ti u phn tch theo phng php dng ng 3.2.1. Kt qu kho st thi gian n nh phc mu kho st thi gian thch hp cho qu trnh to phc 0.8 mu, chun b 6 dung dch chun 0.6 PO43- c nng 1mg/l. Sau khi 0.4 thm thuc th, cc dung dch c un cch thy cc thi 0.2 gian l: 20, 25, 30, 35, 40 v 45 0 pht ri o mt quang bc 0 10 20 30 40 sng max = 600nm. Kt qu o Thi gian, pht c th hin hnh 4. Hnh 4. S ph thuc mt quang ca Qua kt qu kho st, dung dch mu vo thi gian to phc chn thi gian un mu l 30 pht cho cc th nghim tip theo.
Mt quang D

50

3.2.2. Kt qu kho st nh hng v s che nh hng ca Fe3+ trong mu a) Kho st nh hng ca Fe3+ kho st nh hng ca ion Fe3+ n qu trnh xc nh PO43-, chun b 6 dung dch chun PO43- c nng 1mg/l. Thm lng thuc th sunphomolypdic bng nhau, mu th nht nguyn cn cc dung dch mu tip theo b sung ion Fe3+ vi lng tng dn t mu s 2 n mu s 6. un cch thy 30pht, ngui, o mt quang bc sng max = 600nm. Kt qu o c th hin trong hnh hnh 5. Kt qu kho st cho thy: 0.8 s c mt ca ion Fe3+ nh hng rt mnh n kt qu o mt 0.6 Mu i chng quang ca phc xanh Molypden. 0.4 3+ Mu o c C th cho rng ion Fe to c 30.2 phc vi ion PO4 lm gim nng 0 ion orthophotphat t do trong 1 2 3 4 5 6 mu, tuy nhin cng khng th S mu loi tr cc nguyn nhn khc v nh qu trnh to thnh hp cht Hnh 5. Biu so snh mt quang ca d a axit molypdophosphoric ri dung dch mu khi c mt b kh n xanh Molypden l rt Fe3+ cc nng khc phc tp. Nh vy trong qu trnh phn tch cn phi loi tr nh hng ca ion nhau Fe3+. Mt trong cc phng php loi tr l che nh hng ca ion Fe3+ bng cch a ion Fe3+ v dng hp cht phc rt bn, ion Fe3+ khng tn ti dng
Mt quang D

109

TP CH KHOA HC V CNG NGH, I HC NNG - S 3(26).2008

t do trong dung dch. Qua mt s phn ng thc hin, chng ti s dng F- to hp cht phc rt bn FeF63-. b) Kho st loi tr nh hng ca Fe3+ bng cch to phc FeF63Chun b 10 dung dch chun PO43- cng nng 1mg/l. Mu s 1 nguyn lm mu i chng, thm vo cc mu cn li cng mt lng dung dch Fe3+. T mu s 3, b sung dung dch F- c nng tng dn, tin hnh o mt quang. Cc kt qu o c trnh by hnh 6. Kt qu cho thy: khi a 0.8 ion F vo dung dch phn tch 3cha hm lng ion PO4 nhng 0.6 Mu i chng c b sung ion Fe3+ th gi tr 0.4 Mu o c mt quang o c gn nh tng ng vi hm lng ion 0.2 PO43-, iu ny c th l gii rng s c mt ca Fe3+ t nh 0 1 2 3 4 5 6 7 8 9 10 hng n gi tr o l do ion S mu Fe3+ c trong dung dch i vo phc bn vi ion F . Thc Hnh 6. Biu so snh mt quang nghim cng cho thy nu lng ca dung dch mu khi c mt Fe3+ ion F b sung vo qu nhiu th v c loi tr bng Fgi tr mt quang o c li gim v khng n nh. Nh vy vi hm lng ion PO43- trong mu khong vi mg/l, s c mt ion Fe3+ s nh hng n kt qu o v nu b sung vo dung dch phn tch mt lng ion F- thch hp c th coi nh loi tr c nh hng ca Fe3+. Cc thc nghim cho thy, vi hm lng Fe3+ nh hn 0.05mg/l th s nh hng l khng ng k. Qua cc kt qu kho st, quy trnh phn tch xut nh sau: (1). Ly 30 ml mu nc cn phn tch. (2). Thm 2ml dung dch thuc th sunfomolypic A. (3). Thm 1ml dung dch thuc th sunfomolypic B. (4). Thm 7ml dung dch Fnng 0.1 g/l. (5). un cch thy 30 pht. (6). ngui ri tin hnh o mt quang bc sng 600 nm. Da vo ng chun xc nh nng PO43-. 4. Kt lun 1. xc nh cc iu kin ti u cho hai quy trnh phn tch PO43- trong nc. 2. Cc quy trnh c lp dng theo phng php dng SnCl 2, Cu p dng dng trong phn tch cc mu thc cho kt qu c tin cy cao, ph hp vi vic nh gi hm lng ion Orthophotphat trong cc mu nc mt.
Mt quang D

110

TP CH KHOA HC V CNG NGH, I HC NNG - S 3(26).2008

TI LIU THAM KHO [1] Hong Minh Chu, T Vn Mc, T Vng Nghi (2002), C s ha hc phn tch, NXB KH&KT, H Ni [2] R.A. Lidin, V.A. Molosco, L.L. Andreeva (2001), Tnh cht l ha hc cc cht v c, NXB KH&KT, H Ni [3] H Vit Qu (2000), Phn tch ha l, NXB Gio dc, H Ni [4] J. H. Kennedy (1990), Analytical Chemmitry Principles, Sauders Cllege Publishing, New York [5] Standar methods for the examination of water end wastewater, American Public Health Association.

111