Phn tch As bng phng php AAS

Bch khoa ton th m Wikipedia

Bc ti: menu, tm kim

Bi hoc on ny cn c wiki ha theo cc quy cch nh dng v vn
phong Wikipedia.
Xin hy gip pht trin bi ny bng cch lin kt trong n cc mc t thch hp khc.

Thng tin trong bi (hay on) ny khng th kim chng c do khng

c ch gii t bt k ngun tham kho no.
Xin bn hy ci thin bi vit ny bng cch b sung ch thch ti cc ngun uy tn. Nu bi
c dch t Wikipedia ngn ng khc th hy chuyn ngun tham kho t phin bn cho
bi ny.
Nu khng, nhng cu hay on vn khng c ch gii ngun gc c th b thay th hoc xa
i bt c lc no.

Phng php AAS c vit tt t phng php ph hp thu nguyn t (Atomic

Absorption Spectrophotometric). Cc nguyn t trng thi bnh thng th chng khng
hp thu hay bc x nng lng nhng khi chng trng thi t do di dng nhng m
hi nguyn t th chng hp thu v bc x nng lng. Mi nguyn t ch hp thu nhng
bc x nht nh tng ng vi nhng bc x m chng c th pht ra trong qu trnh pht
x ca chng. Khi nguyn t nhn nng lng chng chuyn ln mc nng lng cao
hn gi l trng thi kch thch. Qu trnh gi l qu trnh hp thu nng lng ca
nguyn t t do trng thi hi v to ra ph ca nguyn t . Ph sinh ra trong qu
trnh ny gi l ph hp thu nguyn t.
Do As v hp cht ca n c nhit nng chy v nhit si thp nn ta thng chn
h thng nguyn t ha mu bng phng php ngn la n kh Ar-H2 c nhit
nguyn t ha mu khong 3700 C, vi nhy cao khong 0.5g/ml, gii hn pht
hin 0.2g/ml, khong xc nh 1-50g/ml.

Mc lc
[n]

1 Cc bc chun b phn tch bng AAS

2 Chun b dung dch mu
3 Thit b v qui trnh phn tch bng AAS
o 3.1 Ngun pht ra bc x n sc
o 3.2 H thng nguyn t ha mu
4 Quy trnh phn tch
o 4.1 Ha cht
o 4.2 M my
o 4.3 Xc nh ng chun
o 4.4 Chun b mu v chun Asen
o 4.5 Xc nh Asen bng NaBH4

o 4.6 Tnh ton kt qu

5 Nguyn t ha bng nhit in
o 5.1 Vn hnh my
o 5.2 Chun ha thit b
o

5.3 Xc nh As bng AAS vi l nhit in

[sa] Cc bc chun b phn tch bng AAS

Chun b:

H thng n pht ra ngun sng hp thu

H thng nguyn t ha mu
H thng gng lc sc
B n sc
B pht hin
Computer
Dung dch mu

[sa] Chun b dung dch mu

Ly mu

Mu nc ging c ly v c bo qun trong bnh nh mc bng thy tinh c

ra bng HCl 2M, c y kn trnh mu tip xc vi xy khng kh to ra kt ta
FeAsO4 v cc hp cht bay hi, cc ion kim loi nh hng trong sut qu trnh bo
qun v x l mu khc nh hng n kt qu phn tch.

Bo qun mu

Mu c bo qun ngay sau khi ly mu bng cch axt ha mu phn tch bng dung
dch HNO3 m c n pH<2 mc ch l ha tan cc hp cht kh tan ca mu nh
As2O3 v dng tan H3AsO3 hay H3AsO4, thun tin trong qu trnh bo qun mu. Mu
c bo qun trong t gi mu.

X l mu.

Do mu c cha nhng phn t l lng hoc cc hp cht hu c do cn phi c x

l trc khi phn tch gm: lc mu, axt ha bng HNO3 n pH<2 ri em o trn php
o AAS. Nu mu c cha cc hp cht kh tan ca kim loi cn phn tch th ta cn ph
mu trc khi lc nhm m bo kt qu phn tch.

[sa] Thit b v qui trnh phn tch bng AAS

[sa] Ngun pht ra bc x n sc

Chn h thng n catot rng (HCl). n ny c cu to gm ba phn chnh:

Thn n v ca s
Cc in cc catot v anot
Kh trong n. l kh tr He, Ar, N2

Anot c cu to bng kim loi tr v bn nhit nh W hay Pt. Catot c ch to c

dng hnh xylanh hay hnh ng rng c ng knh t 3-5 mm. Di 5-6 mm v chnh
bng kim loi cn phn tch vi tinh khit cao (t nht 99.9%). Dy dn ca catot cng
l kim loi W hay Pt. c hai in cc c gn cht trn b ca thn n v cc catot
phi nm ng trc xuyn tm ca n. Ngun nui l ngun mt chiu c th 220-240
V.
Nguyn tc lm vic
Khi n lm vic, catot c nung , gia catot v anot xy ra s phng in lin tc.
Do s phng in m mt s phn t kh b ion ha. Cc ion va c sinh ra s tn
cng vo catot lm b mt catot nng v mt s nguyn t kim loi trn b mt catot
b ha hi v n tr thnh nhng nguyn t kim loi t do. Khi di tc dng ca
nhit trong n HCl ang c t nng , cc nguyn t kim loi ny b kch thch
v pht ra ph pht x ca n. chnh l ph vch ca chnh kim loi lm catot rng.
Nhng v trong iu kin lm vic c bit ca mi trng kh tr c p sut thp, nn
ph pht x ch bao gm cc vch nhy ca kim loi .

[sa] H thng nguyn t ha mu

Qu trnh nguyn t ha trong ngn la gm hai bc k tip nhau.

Bc 1 l chuyn dung dch mu phn tch thnh th cc ht nh nh sng m

trn u vi kh mang v kh chy. Qu trnh ny c gi l qu trnh aerosol
ha hay nebulize ha.
Bc 2 l dn hn hp aerosol cng hn hp kh t vo n nguyn t ha.
H thng ny gi l Nebulizer system, n gm hai phn chnh:
n nguyn t ha mu (burner head)
Bung aerosol ha mu theo hai loi k thut:
o Aerosol ha mu theo k thut pneumatic-mao dn: K thut ny ngi ta
dung h thng Nebulize v kh mang to ra th sol kh ca mu phn
tch nh hin tng mao dn. Trc ht nh ng mao dn S v dng kh
mang K m dung dch mu c dn vo bung aerosol ha. Trong bung
ny, dung dch mu c nh tung thnh th bi nh qu bi E v cnh
qut Q, ri c trn u vi hn hp kh t v c dn ln n nguyn
t ha.

Aerosol ha mu bng siu m: Theo k thut ny, aerosol ha mu

phn tch ngi ta dung h thng siu m c tn s 1-4.5MHz. Di tc
dng ca lc siu m, mu dung dch c phn tn thnh nhng ht rt
nh v trn u vi hn hp kh dn ln n nguyn t ha.

[sa] Quy trnh phn tch

[sa] Ha cht
Dung dch NaBohydrua (NaBH4): ho tan 8g NaBH4 trong 20ml NaOH 0.1N pha ch
hng ngy. Dung dch NaI ha tan 50g NaI trong 100ml nc ct, pha ch hng ngy, c
th thay bng KI cng lng tng ng H2SO4 18N ( ng vi H2SO2 t l 1:1) H2SO4
2.5N: rt cn thn 35ml H2SO4 vo 400ml nc ct, ngui, nh mc n 800ml.
Dung dch K2S2O8 5%: ha tan 25g K2S2O8 trong 800ml nc ct ng trong bnh thy
bo qun trong t lnh, pha ch hng tun. Acid Nitric HNO3 m c Acid percloric
HClO4 Acid clohidric HCl Kh Ar/N2, Ar/He

Dung dch chun As v c:

o Dung dch chun gc As(III) ha tan 1.32g As2O3 trong mu nc ct c
cha 4g NaOH. nh mc ti 1000ml (1ml cha 1mg As(III)).
o Dung dch chun lm vic As(III): pha long 10ml dd chun gc As(III)
ti 1000ml bng nc ct c pha long 5ml HCl (1ml cha 10mg
As(III))
o Dung dch chun As(III) pha long 10ml dd chun ti 1000ml bng nc
ct c cha 2-5ml HNO3 (1ml cha 0.1mg As(III)).
Dung dch chun As(V):
o Dung dch gc: Ha tan 1.534g As2O5 trong mu nc ct cha 4g NaOH
pha long n 1000ml(1ml cha 1mg As(V)).
o Dung dch chun lm vic As(V) : pha long dd gc 100 ln (1ml cha
10mg As(V))
o Pha dung dch chun: pha long dung dch chun lm vic 100 ln (1ml
cha 0.1mg As(V))
Dung dch chun As hu c:

Ha tan 1.842g (CH3)2AsOOH (acid dimethylarsenic) trong nc cha 4g NaOH pha

long n 1000ml (1ml cha 1mg As). Ch kim tra tinh khit ca acid theo dung
dch As tiu chun (50-100mg/l) bng quang ph hp thu nguyn t. Dung dch chun
lm vic As hu c: Pha ch nh trn (1ml cha 10mg As). Dung dch chun As hu c:
Pha ch nh trn (1ml cha 0.1mg As)

[sa] M my
Lp my theo ti liu hng dn dng my, ni bnh phn ng vi st kh. iu chnh tc
dng kh l 2 l/pht. Nu c ng lm kh ni gia bnh phn ng v ng nguyn t
ha mu th dng CaCl2 thay v s dng CaSO4 v n gi SeH4 li. Trc khi dng h

sinh kh hydrua phi xc nh thong s my ti u. Phun dung dch cha Asen vo ngn
la iu chnh v tr ng nguyn t ha sao cho t mt quang cc i. Phun dung
dch trng cho n khi loi hon ton dung dch lu li. Xc nh tc kh mang, nng
v tc nh git NaBH4, th tch dung dch v tc khuy t c tc
hydrua ha cc i nu s dng dung dch ng thch anh cn chn nhit ti u. Vic
nh git NaBH4 qu nhanh hydrua thot ra nhanh s lm mt cn bng h. Khi tc kh
mang qu ln th tnh hiu hp thu s gim. Nn dng bc sng 193.7 nm cho Asen.

[sa] Xc nh ng chun
Ly 0.00; 1.0; 2.0; 10; 15; 20 dung dch lm vic Asen (III) pha long n 100ml bng
dung dch HNO3 (2-5ml HNO3 c trong 1l nc ct) ta thu dy chun vi nng t 0,
1, 2, 5, 10, 15, 20mg Asen (III)/l pha dung dch chun hng ngy.

[sa] Chun b mu v chun Asen

xc nh li ti hin hon ton ca Asen lm theo hai bc trn. Trong bnh
Berzelin dung tch 200ml, trong 50ml mu chun thm vo 7ml mu chun bng
Asen(III) (dung dch chun c pha ch bng cch ly 10ml dung dch lm vic vo cc
c m v pha ch thnh 50ml thm vo 7ml H2SO4 18N v 5ml HNO3 c. Sau
em c cho n khi xut hin kh SO3. Duy tr iu kin oxy ha bng cch thm vo lin
tc HNO3 vo trnh cho dung dch khng b m mu. Khi phn hy hon ton dung
dch s c mu sng. ngui thm vo 25ml nc ct v 1 ml HClO4 v li c tip
loi ht kh oxit nit (cho n khi bc khi SO3). Ch cn thn khi tip xc vi
HClO4. Kim tra hiu qu qu trnh phn hy bng cch cho thm 5ml dung dch chun
Asen hu c vo 50ml mu v xc nh tc ti hin. X l cc mu chun theo ton b
quy trnh nh gi ti hin tng s v ti hin trung bnh ca Asen trong axit
clohydric phi trn 80%. Mt cch khc c th dng bnh kjeldahl phn hy trong vic
xc nh ti hin tng s ca Asen bng cch nng cao hiu sut mu. Sau ln c cui
cng pha long mu bng nc ct ti 50ml.

Chun b mu v dy chun o tng Asen

Ly 50ml dung dch mu hoc chun cho vo bnh Berzelin 200ml thm vo 1ml H2SO4
2.5N v 5ml dung dch K2S2O8 5% c nh trn bp cch ct khi cn khong 30-40 pht
khng c dung dch c cn. Cch khc c th un dung dch trong autoclave
120oC trong 1 gii. Sau khi phn hy xong pha long ti 50ml o asen kim tra hiu
sut phn hy bng cch xc nh ti hin ca acid cacolodic nu thp th phi phn
hy li v dung lng K2S2O8 gp i.

[sa] Xc nh Asen bng NaBH4

Thm 5ml HCl c vo 50ml chun hoc mu b phn hy trong bnh Berzelin 200ml
v khuy u thm tip 5ml NaI v khuy tip t nht 30 pht, ly ng sc kh, phu nh
git v ng thot kh vo bnh berzelin, m my ghi cho n khi ng nn n nh.
Trong lc sc kh ui tt c kim loi ra khi bnh phn ng, thm 0.5ml NaBH4 vo

bnh. Tn hiu tng nhanh v ri gim. Khi tn hiu tr li nn, ly bnh ra, ra ng phun
bng nc ri tip tc lm vi chun kim tra tn hiu, kim tra cc cht gy nh
hng ha hc lm gim tn hiu ca Asen bng cch x l mu phn hy vi dung
dch Asen (III) c nng 10mg/l. ti hin trung bnh phi t 90%.

[sa] Tnh ton kt qu

Dng ng chun cao ca pic theo nng chun. Xc nh nng mu theo
ng chun nu mu c pha long trc khi phn hy th phn kt qu o c vi h
s pha long. Tm tc qui trnh xc nh Asen bng AAS vi h to kh hydrua:

Nguyn tc

Asen c kh mt cch nh lng v trng thi kh hydrua AsH3 bng NaBH4 v kh

to thnh i theo dng kh tr vo b phn nguyn t ha ca my AAS (ng thch anh
trn ngn la dng kh O2/N2).

Thit b

H thng to kh hydrua, my AAS, n catod rng Asen, n teri hiu chnh.

Thuc th

Kh mang Ar hoc N2 HCl 12N; KI 20%; tinh th NaBH4 Dung dch chun gc Asen 1
g/l. Pha long 100 ln asen 10 mg/l v pha long tip 100 ln asen 0.1 mg/l

Dng ng chun

Dy chun c chun b trong bnh dnh mc 100 ml theo th t sau:

S bnh nh mc

Trng 2

Dung dch chun 0.1 mg/l Asen (ml) 0

10 20 40

Nc ct nh mc n vch

100

100 100 100

Nng Asen tng ng (mg/l)

10 20 40

[sa] Nguyn t ha bng nhit in

K thut ny rt thch hp phn tch cc nguyn t c hm lng vi lng 5ppm v

siu vi lng nh As
Nu phn tch nc b mt, nc tinh khit th l graphic c iu chnh trng trnh
nhit gm ba bc v mu cha hm lng nh cc cht ha tan. i vi nc mui
nc bin, nc thi cha nhiu cc cht khc th s dng trng trnh gia nhit trn 7
bc. Cn dng ng graphic c gn tm g gim cc loi nhiu nn v tng nhy.
Mt s ha cht v dung dch thng dng bng l graphic:

Nc ct khng cha kim loi

Acid chloclohydric, HCl (1:1) m c
Acid HNO3 (1:1) m c
Dung dch ch th hiu chnh nn

iu ch thuc th

Mg(NO3)2 10000mg/l: ha tan 10.57 Mg(NO3)2.6H2O trong nc v pha long ti

100ml
Ni(NO3)2 10000mg/l: ha tan 4.96g Ni(NO3)2.6H2O trong nc pha long ti
100ml
H3PO4 10%: cho 10ml H3PO4 vo nc thnh 100ml
Pd(NO3)2 4000mg/l: ha tan 8.89g Pb(NO3)2.H2O trong nc v pha long ti
1000ml
HNO3 4%: 40ml HNO3 pha long bng nc vi bnh nh mc 100ml.

X l mu: Tt c cc dng c thy tinh dng cha mu ha cht v chun b mu phi

c ra bng HNO3(1:1) v phi trng bng nc ct. Cng vic x l mu v o c
thc hin trong phng th nghim sch khng bi trnh nhim mu.
Phn tch As ha tan: cho 1ml H2O2 vo 100ml mu v 1ml th tch dd Ni(NO3)2 d tr
thch hp trc khi em o. Nhng kim loi cn li khng cn cho dd hiu chnh nn.
Phn tch tng s As: Cho vo cc 100ml mu 1ml HNO3 v 2ml H2O2 30%. un nh
trn bp 70-80 C n th tch cn khong 50ml- ngui cho mt lng thch hp
mui Ni l cht hiu chnh nn. nh mc 100ml. ng thi chun b mu trng.

[sa] Vn hnh my
t cc thong s vn hnh thit b theo hng dn ca nh sn xut. S dng hiu chnh
nn khi xc nh cc nguyn t ti cc bc sng ngn hoc mu cha hm lng cht
tan cao, thng khng s dng bc sng ln hn 350nm.

Chn tc kh tr thch hp.

giai on lm kh t nhit ln cn di nhit si ca dung mi.
Chn nhit nguyn t ha.

[sa] Chun ha thit b

Dng dung dch chun d tr pha cc dung dch chun c nng d kin. Loi dy
chun c chun b hng ngy. Cn chun b mu trng v dy dung dch chun t nht
c ba nng khc nhau nm trong khon phn tch ph hp vi thit b v vi nng
cht cn phn tch trong dung dch o.
Ch : Thnh phn c trong chun cng tng t vi mu chun cng tt. V vy c th
thm lng acid tng ng. Tim vo l mt lng dung dch chun v mu, sau vi
ln tim mu phi tim cht chun kim tra lp li ca phng php. Ngi ta c
th s ding phng php o trc tip vi xy dng ng chun hoc phng php
thm chun, phng php ny ch c gi tr khi nng nm trong vng tuyn tnh.

[sa] Xc nh As bng AAS vi l nhit in

Nguyn tc: Mu c a vo l ti y mu c nung ra nng chy v sau

mui As c phn li thnh trng thi As nguyn t.
Thit b: L nguyn t, my AAS, n catot rng AAS v n tri hiu chnh
nn, my ghi.
Thuc th: dd Ni(NO3)2 2%. Chun gc As 1g/l pha long 100ln- 10mg/l, tip
tc pha long 100 ln- 0.1mg/l.
Dng ng chun:

Dy chun c chun b trong bnh nh mc 100ml theo th t sau:

Bnh nh mc Trng 2

Chun As 0.1mg/l 0

10 20 40

Ni(NO3)2 2ml

10 10 10

10

Nc ct n vch 100

100 100 100

Nng As(mg/l) 0

10 20 40

Tim 10ml cc bnh vo l v tip tc nh phn sau:

o Tin hnh phn tch: Trn 10ml mu vi 1ml Ni(NO3)2. Tim 10ml vo l
loi nc 130 C trong vng 60s. Nung chy 850 C trong 40s v
tip tc nguyn t ha 2500 C trong 30s. o hp thu bc sng
193.7nm.

Kt qu c tnh theo mg/l. Ch ca phngphp ny l 2 g/l.