Phng php phn tch quang ph

cao hc kho 19

TI: PHNG PHP PHN TCH QUANG PH

HC VIN THC HIN: L NGC THY TI N

Ni dung: 1. Phng php phn tch quang ph 2. My quang ph. 3. Cc phng php phn tch quang ph 4. Cc vng ph 5. My quang ph pht x 6. My quang ph hp th

1.

Phng php phn tch quang ph : l phng php phn tch quang hc da

trn vic nghin cu s tng tc ca bc x nh sng tr n cht kho st hoc s hp th cc bc x di mt tc ng ha l no . 2. My quang ph: My quang ph l mt dng c dng thu, phn li v ghi li ph ca mt vng ph quang hc nht nh. V ng ph ny l mt i ph ca vt mu nghi n cu t sng ngn n sng di. Ty theo b phn dng phn li nh sng trong my da theo hin tng vt l no (khc x hay nhiu x) m ngi ta chia cc my quang ph thnh hai loi. a) My quang ph lng knh. l nhng my quang ph m h tn sc ca chng c ch to t 1 hay 2 hoc 3 lng knh. S phn li nh sng y da theo hin tng khc x ca nh sng qua hai mi tr ng c chit sut khc nhau (khng kh v thy tinh hay khng kh v thch anh). b) My quang ph cch t. L nhng my quang ph m h tn sc l mt cch t phng hay lm phn x. Bn cht ca s tn sc nh sng y l s nhiu x ca tia sng qua cc k he hp.
3.

Cc phng php phn tch quang ph gm :

Ph nguyn t : Ph pht x, Ph hp th, Ph hunh quang Ph phn t : Ph pht x, Ph hp th v ng UV-VIS, Ph hp th hng ngoi, Ph tn x Raman Ph tia X : Ph pht x, Ph tn x, Ph hunh quan g Ph cng hng t in t v Ph cng hng t proton

4.

Cc vng ph : STT Tn vng ph

1

di sng
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Phng php phn tch quang ph

cao hc kho 19

1 2 3 4 5 6 7 8 9 10

Tia gama () Tia X T ngoi Kh kin Hng ngoi Sng ngn Sng Rada Sng cc ngn Tivi-FM Sng radio

< 0.1 nm 0.1+5nm 80+400nm 400+800nm 1+400m 400+1000m 0.1+1cm 0.1-50cm 1+10m 10+1500m

My quang ph pht x a) Nguyn l hot ng :

5.

Trong iu kin bnh thng, cc in t chuyn ng tr n cc qu o ng vi mc nng lng thp nht. Khi nguy n t trng thi bn vng, tr ng thi c bn, trng thi ny nguyn t khng thu v cng khng pht nng l ng. Nu cung cp nng l ng cho nguyn t th trng thi khng tn ti na. Theo quan im ca thuyt l ng t, khi trng thi kh, in t chuyn ng tp trung to thnh cc m my i n t trong nguyn t, c bit l cc in t ha tr, nu chng nhn c nng lng bn ngoi (in nng, nhit nng, ha nng,...) th in t s chuyn l n mc nng lng cao hn. Khi nguyn t tn ti trng thi kch thch (trn g thi khng b n vng). Nguyn t ch tn ti trng thi n y trong mt khong thi gian sng rt nh (nhiu nht l 10-8 giy). Sau n lun lun c xu h ng tr v trng thi c bn ban u, trng thi bn vng, v gii phng nng l ngm chng hp th c trong qu trnh trn di dng ca cc bc x quang hc. Bc x n y chnh l ph pht x ca nguyn t, tn s c tnh theo cng th c: E = (En E0 ) = h = h.c/
b) 1.

C ch thc hin:

Trc ht mu phn tch cn c chuyn thnh hi (kh) ca nguyn t hay ion t do trong mi trng kch thch, y l qu trnh ha h i v nguyn t ha mu. Sau d ng ngun nng lng ph hp kch thch m h i chng pht x, y l qu trnh kch thch ph ca mu. 2. Thu, phn 1i v ghi ton b ph pht x ca vt mu nh my quang ph. Ph c th c ghi ln knh nh hay phim nh, hoc ghi trc tip cc tn hiu c ng pht x ca mt vch ph di dng cc lc trn bng giy, hoc ch ra cc sng c ng vch ph tr n my in (printer), ghi li vo a t ca my tnh. 3. nh gi ph ghi v mt nh tnh v nh lng theo nhng yu cu t ra.
c) -

Cu to c bn :

My quang ph n knh : ch c 1 khe my li ra v cch t c quay tng th nh phn n sc s lt qua khe ra n goi v c thu nhn trn t bo quang in. - My quang ph a knh : cch t ng yn v li ra khng dng khe sng m dng CCD (hoc PDA) t mt phng ti u ca bung ti chuyn tn hiu quang phn tch thnh tn hi u in.

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Phng php phn tch quang ph

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1. Ngun sng cung cp iu kin kch thch nguy n t, phn t vt cht ca mu nghin cu pht x. Yu cu i vi ngun sng : Trong phn tch quang ph pht x nguyn t, ngun sng c gi l ngun kch thch ph v c mt vai tr ht sc quan trng. V nh ngun nng lng kch thch ngi ta c th chuyn vt liu mu phn tch th nh trng thi hi ca cc nguyn t v kch thch m hi pht sng (pht x ), ngha l ngun nng lng nh hng trc tip n kt qu ca php phn tch. V vy ngun nng l ng mun dng c vo mc ch phn tch quang ph pht x nguy n t cn phi thc hin c hai nhim v sau y: Trc ht ngun nng l ng phi ha hi, nguyn t ha v chuyn c hon ton cc nguyn li u mu phn tch vo vng phng i n (plasma). C nh th thnh phn ca m hi trong plasma m i ng nht vi th nh phn ca vt mu. ng thi ngun nng lng phi c nng l ng ln (nhit ) c th kch thch c tt nht cc nguyn t ca nguyn t cn phn tch i n pht x ra ph ca n. Song nh th vn cha hon ton . V mt phng php phn tch ch c gi tr khi n c nhy v lp li cao. Chnh v th, ngoi hai nhim v trn mt ngun sng mun dng c lm ngun kch thch ph pht x n c n cn phi tha m n mt s yu cu nht nh sau y: 1) Trc ht ngun sng phi m bo cho php phn tch c nhy cao v cng ca vch ph phi nhy vi s bin thi n nng ca nguyn t phn tch; nhng li khng nhy vi s dao ng ca iu kin l m vic. 2) Ngun nng lng phi n nh v bn vng theo thi gian, m bo cho phng php phn tch c lp li v n nh cao. Ngha l cc thng s ca ngun sng chn nht thit phi duy tr v lp li c. 3) Ngun nng lng phi khng a thm ph ph vo lm ln vi ph ca mu nghin cu. Nu khng s l m kh khn thm cng vi c nh gi nh tnh v nh lng v c khi lm sai l c c kt qu phn tch. 4) Ngun kch thch phi c s cu to khng qu phc tp; nh ng li c kh nng thay i c nhiu thng s, c th chn c nhng iu kin ph hp theo tng i tng phn tch hay tng nguy n t. 5) Yu cu cui cng l ngun nng lng kch thch phi l m tiu hao t m u phn tch v trong m t s trng hp phi khng l m h hi mu phn tch, nh trong 18

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Phng php phn tch quang ph

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Nhng ngun sng th ng gp l : ngn la, plasma cao tn, h quang, tia in, laser ... 2. H chun trc gm mt h thng thu knh ghp vi nhau hay h gng hi t v mt khe hp (khe vo ca chm sng v c th iu chnh c) t tiu c ca h thu knh ny. H chun trc c nhim v nhn v to ra chm sng song song hng vo h tn sc phn li th nh ph. 3. H tn sc l mt h thng lng knh hay cch t. H n y c nhim v phn li (tn sc) chm sng a sc phc tp c nhiu bc sng khc nhau th nh mt di ph ca chng theo tng sng ring bit lch i nhng gc khc nhau. Nu h tn sc c ch to bng lng knh th tia sng ngn s b lch nhiu, sng d i lch t, cn nu h tn sc c ch to bng cch t th ngc li. 4. H bung nh l mt h thng thu knh hay mt h g ng hi t v mt mt phng tiu ca cc chm sng. H ny c nhim v hi t cc tia sng c c ng bc sng sau khi i qua h phn li li vi nhau to ra nh ca khe my tr n mt phng tiu. chnh l cc vch ph. 5. H thu ph c th l knh nh, phim nh, t b o quang in, cc mng diode PDA hoc CCD. H ny c t mt phng ti u ca bung ti v c nhim v ghi li cc vch ph.

My quang ph hp th : a) Nguyn l hot ng :

6.

Khi nguyn t trng thi hi t do, nu ta chiu mt ch m tia sng c nhng bc sng xc nh vo m hi nguyn t , th cc nguyn t t do s hp th cc bc x c bc sng nht nh ng ng vi nhng tia bc x m n c th pht ra c trong qu trnh pht x ca n. Lc ny nguyn t nhn nng lng ca cc tia bc x chiu v o n v chuyn ln trng thi kch thch c nng lng cao hn trng thi c bn. l tnh cht c trng ca nguyn t trng thi hi, qu trnh c gi l qu trnh hp th nng lng ca nguyn t t do trng thi h i v to ra ph hp th nguyn t ca nguyn t . ng vi mi gi tr nng l ng E m nguyn t hp th ta s c mt vch ph hp th vi d i sng i c trng cho qu trnh , ngha l ph hp th ca nguyn t cng l ph vch. Nhng nguyn t khng hp th tt c cc bc x m n c th pht ra c trong qu trnh pht x. Qu trnh hp th ch xy ra i vi GVHD: T.S L V TUN HNG 4 SVTH: L NGC THU TIN

Phng php phn tch quang ph

cao hc kho 19

cc vch ph nhy, cc vch ph c trng v cc vch cui cng ca cc nguyn t. Do , mun c ph hp th nguy n t trc ht phi to ra c m hi nguyn t t do, v sau chiu vo n mt chm tia sng c nh ng bc sng nht nh ng ng vi cc tia pht x nhy ca nguyn t cn nghin cu.
b)

nh lut Lambert Beer :

Khi chm sng c c ng I0 truyn ti mi trng c b dy d th b hp th mt phn nn cng nh sng ra khi mi tr ng l I < I0. Nu I0 nh v cc hin tng phn x, tn x khng ng k th :

I = I0exp(- .C.d)
truyn qua : hp th:

T= I/I0

Trong :

A = - logT = log 10e. ( .C.d )= 0, 434. ( .C.d)

C l nng ca dng dch (mol/l hoc %) d l b dy ca lp dung dch (cm) l h s hp th c tr ng cho cu to ca cht tan trong dung dch ph thuc b c sng nh sng n sc
c)

Cu to c bn :
My quang ph 1 chm tia phi o 2 ln : 1 ln vi mu chu n (ch cha dung mi) v 1 ln vi mu cn o (cha dung dch cn phn tch) ->I0 trong 2 ln o phi khng i -> kt qu phn tch khng chnh xc

My quang ph 2 chm tia th nh sng t i c tch lm 2 chm : 1 i qua m u chun v 1 ln i qua mu cn o, sau c ng i vo my thu so snh cng ->ch phi o 1 ln -> kt qu phn tch chnh xc v tnh c ngay hp th A

Yu cu i vi ngun sng : nh sng ti mu cn n sc nn phi kt hp my n sc c knh lc i vi ngun sng c v ng ph rng vi bc sng lin tc (hoc dng ngun laser c bc sng thch hp), ngun thng dng l n Wolfram Halogen cho ph lin tc trong vng kh kin v hng ngoi, n H2 hoc D2 cho ph li n tc vng t ngoi.

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Phng php phn tch quang ph

cao hc kho 19

GVHD: T.S L V TUN HNG

SVTH: L NGC THU TIN