PHN TCH THC PHM

TI: C S CA PHNG PHP AAS

GVHD: L NHT TM LP: NHM 3 SVTH: 1. PHAN HNG M
2. 3. 4. 5.

TRN TRNG NGHA HUNH TRUNG SN NGUYN T NGC HNG NGUYN TH QUYN

6.

NGUYN NGC LINH THY

I. C

s l thuyt ca php o ph hp th AAS

1. Nguyn tc ca phng php phn tch ph

hp thu nguyn t.
1.1 S xut hin ph hp th nguyn t

Trong iu kin bnh thng nguyn t khng thu v cng khng pht ra nng lng di dng cc bc x. Lc ny nguyn t tn ti trng thi c bn. l trng thi bn vng v ngho nng lng nht.

Lc ny nguyn t nhn nng lng ca cc tia bc x chiu vo n v n chuyn ln trng thi kch thch c nng lng cao hn trng thi c bn

Qu trnh c gi l qu trnh hp th nng lng ca nguyn t t do trng thi hi v to ra ph nguyn t. Ph sinh ra trong qu trnh ny c gi l ph hp th nguyn t

Hnh 1: Qu trnh pht x v hp th ca mt nguyn t Eo: Mc nng lng trng thi c bn

Em: Mc nng lng trng thi kch thch

E : Nng lng nhn vo (kch thch)

+ hv: Photon kch thch - hv : Photon pht x

1.2. Cng V Cu Trc Ca Vch Ph:

Trong

ph hp th nguyn t khi nng C nh, mi

quan h gia cng ca tia sng b hp th v nng ca nguyn t tun theo nh lut LambertBeer

I0 A = lg = Ka N L I Trong :
Ka: h s hp th nguyn t. A: hp thu quang.

N: nng nguyn t
L: b dy ca lp hp th.

Cu trc ca vch ph:

rng ca vch ph hp th c xc nh bi nhiu yu t v n l tng ca nhiu rng ring phn ca cc yu t khc nhau.

rng ton phn ca vch ph hp th: Ht = Hn + Hd + HL +Hc

Trong :

Hn: rng t nhin

Hd: rng kp HL: rng Lorentz Hc: rng ca cu trc tinh vi

2. Cc Yu T nh Hng n Php o AAS

Cc yu t v ph:

- S hp th nn:

Vch ph c chn o nm trong vng kh kin th yu t ny th hin r rng. Cn trong vng t ngoi th nh hng ny t xut hin
- S chen ln ca vch ph Yu t ny thng thy khi cc nguyn t th ba trong mu phn tch c nng ln v l nguyn t c s ca mu.

- S hp th ca cc ht rn
Cc ht ny hoc hp th hoc chn ng i ca chm sng t n HCL chiu vo mi trng hp th. Yu t ny c gi l s hp th gi. iu ny gy sai s cho kt qu o cng vch ph.

Cc yu t vt l: nht v sc cng b mt ca dung dch mu.

o v xc nh theo phng php thm chun; pha long mu bng mt dung mi hay mt nn ph hp; thm vo mu chun mt cht m c nng ln; dng bm y mu vi mt tc xc nh m chng ta mong mun.
-

Hiu ng lu li.

Khi nguyn t ho mu o cng vch ph, th mt lng nh ca nguyn t phn tch khng b nguyn t ho, chng c lu li trn b mt cuvet v c th tch t li qua mt s ln nguyn t ho mu.

S ion ho

Chn cc iu kin nguyn t ho c nhit thp, m trong iu kin nguyn t phn tch hu nh khng b ion ho; thm vo mu phn tch mt cht m cho s ion ho.

- S kch thch ph pht x :

Yu t ny xut hin thng lm gim nng ca cc

nguyn t trung ho c kh nng hp th bc x trong

mi trng hp th

Cc yu t ha hc:

Nng axit v loi axit trong dung dch mu

Trong thc t phn tch ca php o ph hp th nguyn t

ngi ta thng dng mi trng l axit HCl hay HNO3 1 hay

2%. V nng ny nh hng ca hai axit ny l khng ng k. - nh hng ca cc cation Cc cation c th lm tng, cng c th lm gim v cng c th khng gy nh hng g n cng vch ph ca nguyn t phn tch.

- nh hng ca cc anion Ni chung cc anion ca cc loi axit d bay hi thng lm gim t n cng vch ph. - Thnh phn nn ca mu

Yu t nh hng ny ngi ta quen gi l matrix effect.Nhng khng phi lc no cng xut hin m thng ch thy trong mt s trng hp nht nh. - nh hng ca dung mi hu c
S c mt ca dung mi hu c thng lm tng cng cu vch ph hp th nguyn t ca nhiu nguyn t ln nhiu ln.y l mt phng php tng nhy ca phng php phn tch ny.

II. Cc Phng Php nh Lng Ph Hp Thu AAS

1.

Phng Php ng Chun:

Nguyn tc ca phng php ny l da vo phng trnh c bn ca php o A= K.C v mt dy mu u (t nht l ba mu u) dng mt ng chun v sau nh ng chun ny v gi tr Ax xc nh nng Cx ca nguyn t cn phn tch trong mu o ph, ri t tnh c nng ca n trong mu phn tch.

A C B M

Ax

C1

C2 C3

C4 C5

C g/mL)

Hnh 7: th chun ca phng php ng chun

Phng php ny n gin, d thc hin v rt thch hp vi vic phn tch hng lot mu ca cng mt nguyn t, l u im ca phng php ny.

Khi mu phn tch c thnh phn phc tp v chng ta cha

bit chnh xc th khng th chun b c mt dy mu u

ng n nn s b nh hng ca nn, thnh phn ca mu,

l nhc im ca phng php ny.

2. Phng Php Thm Chun:

- Nguyn tc ca phng php ny l dng ngay mu phn

tch lm nn chun b mt dy mu u, bng cch ly mt lng mu phn tch nht nh v gia thm vo nhng lng nht nh ca nguyn t cn xc nh theo tng bc nng

- Sau chn cc iu kin th nghim ph hp v mt vch

ph ca nguyn t phn tch, tin hnh ghi cng hp th ca vch ph theo tt c dy mu u

M C g/mL)

C1

C2

C3

C4

C5

Hnh 3: Th Ca Phng Php Thm Chun

3. Phng Php Th Khng i:

-

Nguyn tc ca phng php ny l mun xc nh mt nguyn t no , trc ht phi dng mt ng chun nh

trong phng php ng chun. ng chun ny c

gi l ng chun c nh v c dng lu di.

C 2 cch xc nh: Cch 1: Xc nh h s chuyn k theo cng thc

Axo = k.Ax1

Cch 2: T thc t phn tch khi nghin cu cc ng chun ngi ta thy rng, trong cng mt iu kin th

nghim, i vi mt nguyn t khi o trn mt vch phn

tch, nu ng chun dng c t dy ph ca cc mu chun ghi trn cc ln khc nhau, th chng l nhng ng song song hay trng nhau T thc t ny c th suy ra cch dng ng chun phn tch mi ch nh mt mu chun m khng cn tnh k nh trn.

Hnh 4: th ca phng php th khng i

ng chun c nh (1) ng chun phn tch (2)

4. Phng Php Dng Mt Mu Chun:

- Khi c mu chun: Ta ch cn o A1 mu chun ca cht phn tch bit c nng C1 v Ax ca cht phn tch .Sau tnh Cx ca cht phn tch. Ngha l chng ta c: Vi mu phn tch: Ax = a.Cx Vi mu u: A1= a. C1
Cx = Ax.C1 / A1

-Khi khng c mu chun:Ta tin hnh tng t nh phng php thm, ch khc khng cn pha mt dy chun.Nhng mt iu cn ch l C1 thm vo v cc gi tr Cx phi nm trong vng tuyn tnh ca phng php.

5. Phng Php Vi Sai:

- xc nh mt cht bng nh sng phng php o hp th nh sng th iu kin trc tin l s hp th nh sng ca cht phi tun theo nh lut c bn v s hp th nh sng. - hp th quang ca dung dch phi t l tuyn tnh vi nng nht nh (trong khong t a1 n a2) - nhng nng nh hn a1 v ln hn a2 th s hp th nh sng khng tun theo nh lut Beer - m rng khong nng ngi ta dng php o vi sai. Phng

php vi sai o khong nng ln hn a2 gi l phng php vi sai

nng ln, nh hn a1 l phng php vi sai nng b.

u V Nhc im Ca Php o:

u im:

- Php o c nhy v chn lc cao nn c s dng

rng ri trong nhiu lnh vc xc nh vt cc kim loi, c bit trong phn tch cc nguyn t vi lng. Do c nhy cao nn trong nhiu trng hp khng cn lm giu nguyn t xc nh trc khi phn tch.

- C th xc nh ng thi hay lin tip nhiu

nguyn t trong mt mu.Cc kt qu phn tch n nh,

sai s nh.

* Nhc im:

Phi c mt h thng my t tin. V c nhy cao nn s nhim bn c th nh hng n kt qu phn tch hm lng vt. V th mi trng trong phng th nghim

phi khng c bi, cc dng c phi sch, c chnh

xc tiu chun v ho cht phi c tinh khit cao.

Phng php ch cho bit thnh phn nguyn t m

khng cho bit trng thi lin kt trong mu. V th y

ch l phng php phn tch nguyn t

CM N THY V CC BN LNG NGHE