PHN TCH QUANG PH

ti tiu lun:
XC NH HM LNG ST TRONG NC BNG PHNG PHP TRC QUANG
GVHD: Th.s: Hunh Th Minh Hin SVTH: Nguyn Hong Hi Nguyn An H Nguyn T Nh Hnh

Ni dung ti:

Chng I: Phng php trc quang Chng II: Xc nh hm lng st trong nc dng thuc th 1_10 phenantrolin

Chng I: Phng php trc quang:

1.1. Nguyn tc ca phng php trc quang 1.2. C s nh lng 1.3. Cc phng php xc nh nng dung dch mu 1.4. Thit b trong phng php trc quang

1.1. Nguyn tc ca phng php trc quang: Mun xc nh mt cu t X no , ta chuyn n thnh hp cht c kh nng hp thu nh sng ri o s hp thu nh sng ca n v suy ra hm lng cht cn xc nh X. 1.2. C s nh lng: nh lut Bougher_Lampere_Beer: Khi chiu mt chm photon n sc qua dung dch th mc hp th ca dung dch t l thun vi cng sut chm photon v nng cc phn t hp th

A = TM.I.C

1.3. Cc phng php xc nh nng dung dch mu: - Phng php so snh - Phng php ng chun - Phng php thm - Phng php vi sai 1.4. Thit b trong phng php trc quang: - Ngun sng - B n sc - Cuvet - Detector - B phn khuych i v ghi nhn tn hiu

Chng 2 : Xc nh hm lng st trong nc dng thuc th 1,10 _ phenantrolin

2.1. Nguyn tc phn tch 2.2. Ho cht _ thit b 2.3. Cch tin hnh 2.4. Biu th kt qu 2.5. Cc cht gy nhiu

2.1. Nguyn tc phn tch:

2.1.1. Ly mu v chun b mu: - Ly mu - St tng - St (II) 2.1.2. Nguyn tc: - Thm dung dch 1,10 _ phenantrolin vo ion st (II) c trong nc thi. - Xy dng ng chun ca Fe2+ vi 1,10 _ phenantrolin vi nng bit trc - Xc nh nng ion st (II) (nu xc nh hm lng st tng bao gm: Fe2+ & Fe3+, ta kh Fe3+ xung Fe3+ sau tin hnh tng t nh xc nh Fe2+)

2.2. Ha cht - thit b:

2.2.1. Ha cht: H2SO4 HNO3 _ HCl _ m axetat _ NH2OH.HCl _ 1,10 phenol _ K2S2O8 _ st dung dch gc _ st dung dch chun 1 _ st dung dch chun 2. 2.2.2. Thit b:

Ph k _ lng knh _ cuvet _ mng lc _ bnh oxi.

2.3 Cch tin hnh

2.3.1 St tng: + Xc nh trc tip:

50 ml mu axt ha Nu c st khng tan, oxt st, phc cht st Chuyn mu n bnh un Thm 5 ml K2S2O8 un nh 40oC, chuyn vo bnh nh mc 50 ml Chuyn vo bnh 100 ml Thm 1 ml NH4OH.HCl

Trn k

Thm 2 ml 1,10_phenantrolein
trong ti 15 pht

o hp thu ca dung dch

St tng sau khi phn hu:

50 ml mu axt ho Thm 5 ml HNO3 + 10 ml HCl un 70-80 oC sau 30 pht Thm 2 ml H2SO4 Lm bay hi dung dich Lm ngui n nhit phng Thm 20 ml nc Chuyn vo bnh nh mc 50 ml, nh mc n vch

Kh thnh st II

Tin hnh o quang

2.3.2 Xc nh st ho tan: tin hnh nh qu trnh xc nh st tng sau khi kh thnh st (II). 2.3.3 Xc nh st II: tin hnh nh qu trnh xc nh st tng nhng khng thm hydroxylamoni clorua. 2.3.4 Th mu trng: thc hin chnh xc theo qui trnh i vi mu, nhng 50 ml mu bng 50 ml nc.

2.3.5 Hiu chun

+ Chun b dung dch chun: chun b dy dung dch st chun trong khong nng nh d tnh ca mu th bng cch cho mt th tch chnh xc bit dung dch Fe chun, dung dch chun 1, dung dch chun 2 vo mt lai bnh nh mc 50 ml. Thm 0.5 ml dung dch axt H2SO4 c C(1/2H2SO4) = 4.5 mol/l vo mi bnh v thm nc ti vch.

Dung dch chun st cha 0.1g st trong 1 lt: Cn 50 mg dy st (p=99.9%) Cho vo bnh nh mc 500 ml Thm 20 ml nc, 5 ml HCl Hi m t t cho ho tan, ngui v thm nc ti vch Ly 100 ml dung dch st gc cho vo bnh nh mc 500 ml v thm nc n vch.

* St dung dch chun 1 cha 20 mg st trong mt lt : Dng pipet ht

100 ml dung dch st chun gc trn cho vo bnh nh mc 500 v nh mc n vch. +*St chun dung dch 2 cha 1 mg st trong 1 lt: Dng pipet ht 100 ml dung dch chun 1 cho vo bnh nh mc 500 ml v nh mc n vch. +Sau x l lot dung dch chun nh lm vi mu, tng ng cho vi qui trnh cho mi dng st cn xc nh. + Dng ng chun: vi mi dy dung dch st chun, chun b th chun bng cch t nng dung dch st(mg/l) trn trc honh tng ng vi hp th trn trc tung. Yu cu mi ng chun ring cho mi dng st, mi mt my quang ph v mi mt chiu di quang hc ca cuvet.

2.4 Biu th kt qu

2.4.1 Tnh ton

Nng st ca mu,p, biu th bng mg/l c tnh theo cng thc f(A1-A0) Trong f : l dc ca ng cong chun tng ng A1 : l hp th ca dung dch o A0 : l hp th ca dung dch mu trng

2.4.2 Bo co kt qu
Bo co kt qu, ghi r dng xc nh. a) lm trn ti 0,001 mg/l vi nng st t 0,010 n 0,100 mg/l b) lm trn ti 0,001 mg/l vi nng st ln hn 0,100 n 10 mg/l c) lm trn ti 0,1 mg/l vi nng st ln hn 10 mg/l

2.5. Cc cht gy nhiu.

ng , coban,crom v km c mth trong dung dch vi nng cao hn nng st 10 ln s gy nhiu cho kt qu.Niken vi nng ln hn 2mg/l s nh hng ti phn tch st. iu chnh pH ti 3,5 5,5 cc nh hng ny s c loi tr. Nu bitmut, bc v thu ngn s gy nhiu nu nng ln hn 1mg/l. Nng cadimi ln hn 50 mg/l s c nh hng ti kt qu. nh hng ca xianua ln kt qu phn tch c th loi tr bng cch axit ho mu, tr mt s phc cht ca xyanua khc phn hu.