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 trn 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 nghin
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 khe hp.
3.

Cc phng php phn tch quang ph gm :

4.

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

Cc vng ph :
STT
Tn vng ph

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di sng
1

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Phng php phn tch quang ph

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cao hc kho 19

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 nguyn t trng thi bn vng, tr ng thi c bn, trng
thi ny nguyn t khng thu v cng khng pht nng lng. 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 in 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 ln mc nng lng cao hn.
Khi nguyn t tn ti trng thi kch thch (trn g thi khng bn vng). Nguyn t
ch tn ti trng thi ny trong mt khong thi gian sng rt nh (nhiu nht l 10-8
giy). Sau n lun lun c xu hng tr v trng thi c bn ban u, trng thi bn
vng, v gii phng nng lngm 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 thc:
E = (En E0 ) = h = h.c/
b)

C ch thc hin:

1. 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 hi v nguyn t ha mu. Sau dng
ngun nng lng ph hp kch thch m hi 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 trn 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 thnh

phn n sc s lt qua khe ra ngoi 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 tiu ca bung ti chuyn tn hiu quang phn
tch thnh tn hiu in.

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Phng php phn tch quang ph

cao hc kho 19

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 lng 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 lng phi ha hi, nguyn t ha v chuyn c hon
ton cc nguyn liu mu phn tch vo vng phng in (plasma). C nh th thnh
phn ca m hi trong plasma mi ng nht vi thnh phn ca vt mu. ng thi
ngun nng lng phi c nng lng 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 mn 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 lm kh khn thm cng vi c nh gi nh tnh v nh
lng v c khi lm sai lc 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 nguyn t.
5) Yu cu cui cng l ngun nng lng kch thch phi lm tiu hao t mu
phn tch v trong mt s trng hp phi khng lm h hi mu phn tch, nh trong
18

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Phng php phn tch quang ph

cao hc kho 19

Nhng ngun sng thng 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 thnh 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 thnh 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 di 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 trn mt phng tiu. chnh l
cc vch ph.
5. H thu ph c th l knh nh, phim nh, t bo quang in, cc mng diode PDA hoc
CCD. H ny c t mt phng tiu ca bung ti v c nhim v ghi li cc vch
ph.

6.
a)

My quang ph hp th :
Nguyn l hot ng :

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 hi 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
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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 nguyn t trc ht phi to ra c m hi nguyn t t do,
v sau chiu vo n mt chm tia sng c nhng 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 cng 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 :

T= I/I0
hp th:

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

Trong :
C l nng ca dng dch (mol/l hoc %)
d l b dy ca lp dung dch (cm)
l h s hp th c trng 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 ti c tch lm 2 chm : 1 i qua mu

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 lin tc vng t ngoi.

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Phng php phn tch quang ph

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cao hc kho 19

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