PHNG PHP PH HP TH UV-VIS

Sinh vin thc hin: 1. o Vn Hot 2. Phan Tun Hng 3. Phan Vn Ha A GII THIU CHUNG I Ph hp th UV_VIS 1. c im th biu din A = f( ) (hoc =f( ) hoc lg = f( )) gi l ph hp th nh sng ca dung dch. Ph hp th thng c biu din di dng mt ng cong cho thy s ph thuc hp th ca mt cht bt k trng thi dung dch vo bc sng ca nh sng chiu ti. Ph hp th ca mt cht c c trng bi bc sng max m ti s hp th l ln nht 2. Nguyn l ca ph hp th Khi chiu mt chm bc x in t tc ng ln khi vt cht th s hp th ca khi vt cht ph thuc vo bn cht ca n, nh vy o lng tia bc x b hp th ta c th xc nh c tnh cht ca vt liu. Ph hp th ng dng tt nht i vi nhng nguyn t hoc phn t nh. Khi nh sng tng tc vi cc phn t kh xy ra 3 qu trnh khc nhau: - Qu trnh hp th - Qu trnh pht x t pht - Qu trnh pht x kch thch. i vi ph hp th chng ta ch xt 2 qu trnh: Hp th v pht x t pht. II Cc nh lut c bn 1. nh lut Lambert

Ta c:

di = - k.i.dx

di k .dx b qua phn nng lng tn x, phn x, ly tch phn hai v: Suy ra i

di i (k ).dx ln I ln( I0 ) k.l I0 0

suy ra:

I I 0 .e k .l
Ni dung: Khi dy ca lp mi trng tng theo cp s cng th cng sng gim theo cp s nhn. 2. nh lut Beer k = a.C v ln = 2,3 lg

log (I0/I) = a.b.C

Kortum v Sieler cho thy nh lut Beer ch p dng c khi nng thp. H s hp th ring a ph thuc vo chit sut mi trng v nng .

a a0

n (n 2 2) 2

Ti C=10exp (-3) chit sut khng thay i. Nh vy, khi phn tch dung dich nng cao cn c hiu chnh. III chnh xc khi o ph hp th Cp chnh xc cho bit kt qu o gn bng gi tr chp nhn, cn sai s m t tnh lp li ca php o Cp chnh xc thng c xc nh bng php so snh thng nng dI qua khu gn vo mu v c ng m ti cc im khc nhau trong qu trnh hiu chnh. Cc thng s ca h o nh hng ti cp chnh xc l: + rng khe: Nu khe qu rng th gii khe s rng hn gi tr thc, cn qu hp s kh phn bit c tn hiu mu. + Tc qut qu nhanh cng gy ra li, nh ph s b dch v vng bc sng thp. + Cp chnh xc ca bc sng, cn phi hiu chnh trc khi o t bc sng tiu chun. + S lch chm sng l nguyn nhn chnh gy mt chnh xc c bit l khi chm sng yu. Nguyn nhn l do nh sng b tn x do bi hoc m mc b mt cc dng c quang hc. H s hp th thc khi khng c hin tng lch tia sng c xc nh nh sau:

Aapperent log

I0 I S I IS

IS l cng nh sng b hp th bi mu chun. IV Sai s php o Sai s ca h truyn qua: T Sai s ca cng nh sng: I
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Sai s ca nng : C Cc sai s ny xut hin khi b nhiu khi o. Gi tr ca sai s trong khong 0,01 0,002 trn ton b thang o. C s l thuyt Sai s tng i ca nng : Theo nh lut Beer:
C I A 1 T log 0 lg ab ab I ab 0, 434 dI dC 0, 434 ( ) v ab I dT Tab

=>

dC 0, 434 dI ( ) C A I

V Cc phng php nh lng 1. Phng php so mu bng mt C cc cch nh lng theo phng php so mu bng mt l: Lp dy mu chun, chun so snh mu v cn bng mu. Phng php cho kt qu vi chnh xc khng cao, tuy nhin rt n gin khng cn my o ph. Phng php thch hp trong vic kim tra ngng cho php ca cht no trong mt sn phm c th xem c t hay khng. 2. Phng php ng chun Phng trnh c bn ca php o nh lng theo ph UV_VIS l: A = .l.C (.l = const vy A=f(C) l hm bc nht) Bng cch chun b mt dy dung dch mu c nng tng dn v bit chnh xc trc C1, C2, C3, thng l 5-7 nm trong vng tuyn tnh ca mi quan h A-C v dung dch mu ca cht cn xc nh nng trong cng iu kin phn tch nh dy dung dch chun. Nghin cu chn iu kin thch hp nht o ph ca cc mu chun v mu phn tch nh cc thng s v thi gian, mi trng, loi cuvet o hp th quang ca cc dung dch chun, dng ng chun theo ta A-C sau o hp th quang ca dung dch cht mu cn xc nh (gi s l Ax), ri p dng vo ng chun ta s c nng Cx tng ng vi nng cn xc nh. Phng php rt tin li
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phn tch hng lot mu ca cng mt cht trong mt i tng nghin cu, nhanh chng, hiu sut cao. 3. Phng php thm chun Nguyn tc: Ly cng mt lng dung dch cn phn tch vo 2 bnh nh mc 1 v 2. Thm vo bnh 2 mt lng dung dch chun ca cht phn tch (C). Thc hin phn ng hin mu c hai bnh trong iu kin th nghim thch hp hon ton nh nhau. em o D ca hai dung dch max. Theo nh lut Lambert-Beer vi D v Dx ta c:

Cx

C .Dx D Dx

Trong : Dx l mt quang ca dung dch khng thm. D l mt ca dung dch sau khi thm. Dng phng php ny c th loi tr c nh hng ca cc cht l, ng thi c th kim tra c chnh xc ca cc php phn tch. B H O PH UV_VIS 1. Nguyn l

S nguyn l thit b o quang 1/ Ngun sng: cung cp bc x nh sng vng trng thy th dng n si Vonfram; vng t ngoi: dng n hydro, deteri, thu ngn t
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2/ H tn sc: h tn sc c nhim v bin chm tia a sc thnh chm tia n sc (cung cp bc x n sc). Vi cc my th h c s dng t 10 ti 12 knh lc nh sng cho di ph hp ch khng cho h n sc. Cc my hin i hn th s dng lng knh cho nh sng n sc. Cc my UV-Vis th h mi s dng cch t (12001800 vch/mm c khi ti 2400 vch/mm) c phn gii cao t 1 ti 0,2nm. 3/ Mu phn tch: cht phn tch c th cho tc dng vi mt thuc th trong mi trng thch hp nhm to phc cht c nhy m bo tnh nh lng ca phng php. Nu cht phn tch l cht kh th phi cha mu vo cuvet ng kn. Cuvet dng cho ph UV phi l cuvet thch anh. Cuvet dng cho ph Vis c th l cuvet nha hoc cuvet thu tinh. 4/ Detector: trong cc my n gin dng t bo quang in chuyn tn hiu quang thnh tn hiu in ri cho qua b khuch i hin th kt qu o. Trong cc my th h mi c nhy cao thng dng detector dng ng nhn quang hoc loi chui diot (DAD). Detector chui diot thch hp cho vic o ng thi nhiu cu t vi nhiu bc sng khc nhau, thit b kh bn. 2. Nguyn tc Ph hp th UV -VIS l ph hp th ca cc cht tan trng thi dung dch ng th ca mt dung mi nht nh nh : nc, metanol, benzen, toluen, cloroform V th, mun thc hin php o ph ny ta phi : t phn tch trong mt dung mi ph hp u vo dung dich mu cha hp cht cn phn tch 1 chm bc x n sc c nng lng ph hp cho cht phn tch hay sn phm ca n hp th bc x to ra ph hp th UV -VIS ca n. o cng ca chm sng sau khi qua dung dch mu nghin cu.

C - NG DNG CA PHNG PHP PH HP TH UV-VIS Kim tra tinh khit: Vt ca tp cht trong cht hu c c pht hin d dng khi n c cng hp th ln. Nhn bit cht v nghin cu cu trc: Bng cch so snh ph hp th ca cht so vi ph hp th ca cht trong thin nhin hoc vi mu chun c th cho kt lun v mt sn phm tng hp. Phn tch hn hp: Cc my quang ph uv-vis hin i c kh nng xc nh cc nng ring r trong hn hp gm n cu t. My s dng tnh cht cng hp th gii h phng trnh v cho kt qu nng tng cu t trong hn hp phn tch. Xc nh khi lng phn t Xc nh hng s phn ly acid-bazo: Xc nh hng s phn ly acid-bazo l mt trong nhng phng php quan trng nghin cu cu trc cc hp cht hu c. Ni dung ca phng php l o ph hp thu ca cc cht hu c cha cc nhm c tnh cht acid-bazo ph thuc vo PH ca mi trng Xc nh thnh phn ca phc cht: Thnh phn ca phc cht trong dung dch c th c xc nh bng quang ph hp thu t ngoi v kh kin theo mt trong cc phng php khc nhau phng php bin s lin tc, phng php t l mol.

M t thit b: My quang ph hp th nguyn t (AAS) 6800 do hng Shimazdu - Nht Bn ch to l loi thit b chuyn s dng phn tch hm lng cc kim loi nng trong mi trng khng kh, t, nc, phn bn v cc sn phm nng nghip. Thit b s dng h iu hnh Windows XP iu khin gip ngi vn hnh d dng s dng vi cc giao din thn thin.