Atomic Spectroscopy

Revision for Mid-Term

2016, May 2nd

Phng phap AAS la phng phap phn

tich nguyn t. Giai thich?

Cht phn tich c a v trang

thai nguyn t / ion nguyn t t do
Da vao s hp thu bc xa vach c
trng cua nguyn t inh tinh
hoc inh lng

Cac b phn va chc nng cua chung

trong mt h o AAS?
Ngun bc xa cung cp bc xa c trng (HCL,
EDL) hoc khng c trng (en Xe cao ap)
B phn nguyn t hoa (F, GF, CV, HG-AAS)
a nguyn t cn phn tich v dang nguyn
t t do
B phn tach quang ph (cach t) loc vach bc
xa cn o qua khe o
Detector (PMT n knh tun t, CCD a knh
lin tuc) ghi nhn va khuch ai tin hiu
B phn x ly va biu thi tin hiu thanh ph
(may tinh)

So sanh cu tao h may o trc quang va o ph

nguyn t? So sanh h o AAS mt chum tia va hai
chum tia?

H o trc quang co cach t nm

trc quang l, h o ph nguyn t
co cach t nm sau quang l
H o mt chum tia khng co b
phn tach chum bc xa ngun, vi vy
nhay se cao hn gp i h hai
chum tia. H hai chum tia lun co s
bu tr tc thi gia chun chay may
va mu nn se co s chinh xac cao
hn.

im khac bit cn ban cua h o AAS va

h o AES?

AAS co ngun bc xa, AES khng co

ngun bc xa
Ngun kich hoat trong AAS bng bc
xa, cung cp bc xa c trng .
Ngun kich hoat trong AES bng
nhit, cung cp dai bc xa khng c
trng

Nguyn ly vn hanh en cathode rng?

Ba bc : phun xa (sputtering), kich

hoat (activation) va phn ra (decay)
Nguyn t cua nguyn t tai anode
c Ar+ kich hoat va phat ra bc xa
c trng
Cng en phu thuc vao mt
hi nguyn t (do th ap u vao
quyt inh)

Y nghia inh lut phn b Maxwell trong

ph nguyn t?

Cho bit ng nng cac vi hat nhit

lam vic cua plasma, t o nu
ln thc trang cua cac cu t trong
plasma

Vai tro cua b phun sng trong AAS? Cac

yu t anh hng n s phun sng?

Giam kich thc va loc la nhng hat

sng co kich thc phu hp cho qua
trinh nguyn t hoa
Cac yu t anh hng:
nht dung dich
Thanh phn dung dich (chu yu la nng
mui)
Sc cng b mt
Lu lng khi mang trong spray
chamber.

inh nghia nhiu vt ly trong AAS? Khi

nao thi xay ra nhiu vt ly?
Nhiu vt ly la s anh hng cua nn mu
ln hiu sut cua qua trinh nguyn t hoa
Anh hng chu yu ln bn qua trinh :
phun sng, desolvat, hoa long hat rn
(liquefaction) va hoa hi (vaporization)
Nhiu vt ly xay ra nghim trong khi nn
mu co nhiu mui kho bay hi , sc cng
b mt ln lam nhu hoa dung dich va
nht ln can tr hiu sut phun sng.

Phat hin va khc phuc nhiu vt ly?

Ta phat hin nhiu vt ly bng s pha

loang mu. Tin hiu cht phn tich
giam khng tuyn tinh theo h s
pha loang thng bao s hin din cua
nhiu vt ly
Can thip nhiu vt ly bng:
Hiu chinh nn : thm chun hoc pha
loang mu
X ly mu loai nn (nu hiu chinh nn
khng hiu qua). Lu y tranh nhim bn
va mt mu.

inh nghia nhiu hoa hoc trong AAS? Khi

nao thi xay ra nhiu hoa hoc?

Nhiu hoa hoc la cac yu t anh hng

ln qua trinh ct t lin kt hoa hoc
tao hi nguyn t t do
Anh hng ln qua trinh nguyn t hoa
la chinh
Nhiu hoa hoc xay ra nghim trong khi
ban thn cht phn tich tao
oxide/hydroxide bn nhit hoc ngun
bc xa khng u manh a phn ln
lng mu v dang hi nguyn t t do

Phat hin va khc phuc nhiu hoa hoc?

Ta phat hin nhiu hoa hoc va s khac

bit v tin hiu cht phn tich cua mu
va chun, hoc s khng tuyn tinh va
nhay kem cua ng chun.
Mt vai phng phap khc phuc nhiu
hoa hoc:
S dung ngun bc xa co nhit thich hp
hn hoc tinh cht thich hp hn (la kh)
Thm tac nhn phong thich (vd La trong
trng hp nhiu Al khi phn tich Mg)

inh nghia nhiu ion hoa trong AAS? Khi

nao thi xay ra nhiu ion hoa?
Nhiu ion hoa la s bt tng ng v
lng hi nguyn t bi ion hoa trong chun
va mu khi phn tich bng AAS, anh hng
n chinh xac khi inh lng
Nhiu ion hoa xay ra khi :
Nhit cua plasma u ai cho qua trinh ion
hoa trong nn mu hn so vi chun.
Ban thn cht phn tich co th ion hoa thp.

Tuy nhin, iu kin lam vic cua AAS,

nhiu ion hoa thng khng anh hng
ang k

Phn bit nhiu quang ph va nhiu khng

quang ph?

Nhiu quang ph la s chng ln

vach ph cua nn mu hoc mi
trng (vd nh lo graphite) ln vach
ph cua cht phn tich
Nhiu khng quang ph anh hng
n hiu sut tao nguyn t t do
cua cht phn tich khng tng ng
gia mu va chun.

Phn loai cac loai nhiu quang ph va anh gia

phn ong gop cua chung? Nu cach khc phuc?

Co hai loai thanh phn trong nhiu

quang ph
Nhiu do bc xa vt en : lo graphite bi
nung nong, phat ra ph lin tuc. ong
gop nh phn nhiu c inh. Khc
phuc bng cach giam nhit lo va
chinh quang l sao cho detector khng
thu bc xa phat ra t lo
Nhiu do s hp thu gia: cac phn t,
nguyn t hp thu bc xa ngun lam
tng hp thu. Phn ong gop co th

Nhiu quang ph la gi? Lam th nao

khc phuc nhiu quang ph?
Nhiu quang ph xay ra do s chng ln
vach ph cua cac bc song k cn bc
xa cua cht phn tich, lam thay i
hp thu (do tinh cng cua mt quang)
Ta khc phuc nhiu quang ph bng
cach :
Dung b phn tach quang ph co phn
giai tt hn
Tinh chinh b rng khe o
Can thip hiu chinh nn bng Zeeman hoc
en D2 nu cn

Phn bit vach ph va peak hp thu cua

cht phn tich?

Vach ph cua cht phn tich la tin

hiu cua thi A= f(), biu din
cng hp thu tng i (i.e
nhay) cua cht phn tich mt bc
song xac inh.
Peak hp thu cua cht phn tich la
tin hiu cua thi A=f(t) xac
inh, biu din cng hp thu cua
cht phn tich nhng iu kin lam
vic khac nhau cua phep phn tich.

Vach ph anh hng n hp thu th

nao?

Nu vach ph la n sc (tc khng

chiu tac ng nhiu cua nhiu quang
ph) thi ng nn bin ng it phc
tap, peak hp thu it nhoe, hp thu
qua cac ln o lp co chum tt hn
Nu vach ph co cng ln (tc I o
ln), nhay se cao. Nhiu quang ph
se th hin kem ro net hn (tinh cng
mt quang) ; nhiu vt ly se th
hin ro hn qua s pha loang mu.

Nguyn ly hoat ng cua en D2 trong

vic hiu chinh nn?

en D2 c m song song vi en HCL

sao cho hai en co cung cng I0
Peak hp thu cua cht phn tich co
cng khng ang k so vi D2
nhng ang k vi HCL
Tia lo t en HCL bi hp thu bi cht
phn tich + nn, tia lo t en D2 bi hp
thu bi nn. Hiu s hai tri s nay la gia
tri I chi do ong gop cua cht phn tich.

Ngun lin tuc nao thng c dung hiu

chinh nn? Bc song lam vic ti u cua ngun?

Ngi ta dung ph phat xa cua en

Deuterium hiu chinh nn cho cac
nguyn t co vach phat xa nhay nht
nm vung UV. vung bc song
nay, s t hp thu cua cac cu t
nn gy nn nhiu quang ph
Khoang lam vic ti u cua en D2
nm trong khoang 200-400 nm, thich
hp o cac nguyn t nh As, Se.

Dong ti (dark current) la gi? Cach khc

phuc dong ti?

Dong ti la tin hiu nn i vao PMT khi

khng co cac photon. Tin hiu nn nay
thng do bc xa nhit cua cac photon
cua vt liu lam cathode phat ra.
th lam vic cua PMT cang cao (ti
a 1000V), hin tng dong ti cang ro
net. Vi vy, ta chi tng th u vao
cai thin nhay cua PMT trong nhng
trng hp ht sc cn thit.

Ky thut nguyn t hoa bng F-AAS co

nhay khng cao. Giai thich?

S pha loang mu lin tuc trong ngon

la (di tac ng cua dong khi vn
tc chay cao) lam giam nhay cua
cht phn tich.
Thm na, nhit nguyn t hoa
cua F-AAS tng i thp so vi cac
ky thut khac , nn nhay co th
giam do s nguyn t hoa khng
hoan toan.

Phn loai cac tac nhn hiu chinh nn (matrix

modifier)? Pham vi va cng dung cua mi loai
tac nhn?
Tac nhn hiu chinh nn (matrix modifier) la
cac tac nhn loai tr anh hng nn mu ma
khng cn phai qua XLM. Co ba loai:
Tac nhn phong thich (masking interfering
compounds) che nhiu bng cach tao lin kt
hoa hoc bn ; khc phuc nhiu hoa hoc trong FAAS
Cht bin tinh dung cho GF-AAS khc phuc
nhiu quang ph, co hai loai:
Tac nhn thng hoa (Sublimation agent) giup nn tro
hoa d hn. n c nh vic thm NH4NO3 vao nn co
nhiu NaCl
Tac nhn lam bn (Stabilizing agent) c inh cht phn
tich trong giai oan tro hoa bng c ch tao lin kt
(Pd) hoc by trong mang tinh th (MgO)

Cht bin tinh van nng la gi? C ch tac

ng?
Cht bin tinh van nng la hn hp cua Pd
va Mg(NO3)2, thng c phi trn di
dang mui hoa tri hai cua hai kim loai
C ch tac ng cua cht bin tinh van nng
la c ch lam bn hoa, do Pd co th tao cac
hp cht lin kim loai (vi du nh Pd 3Sn2), t
o khin cho nguyn t phn tich khng bi
mt i giai oan tro hoa mu.
Tng t, Mg(NO3)2 nhit phn cho MgO, lam
bn cht phn tich bng cach gi cht phn
tich trong mang tinh th cua no nhit
tro hoa

Ky thut nguyn t hoa GF-AAS it chiu

nhiu vt ly. Giai thich?

Chng trinh nhit cua GF-AAS co

bc tro hoa mu loai bo gn ht nn
mu, cht phn tich se khng bi
nhiu vt ly , t o cai thin nhay
cho phng phap GF-AAS.
Thm na, hiu sut ly mu cua GFAAS gn nh hoan toan, khac vi
hiu sut thp do phun sng cua
phng phap F-AAS

Phn tich Se trong nn nc dung pp nao con phn

tich Se trong hai san dung pp nao. Giai thich?

Nn mu hai san phc tap hn nn

nc nn ta cn c lp Se bng HGAAS vic phn tich tranh bi anh
hng bi nhiu vt ly
Nn nc n gian, d tro hoa va bay
hi nn ta dung GF-AAS tn dung
nhay cao cua phng phap (thay
vi s dung F-AAS phai kem thm D2BGC)

Ky thut phn tich Hg c goi la ky

thut hoa hi lanh. Giai thich?

Qua trinh hoa hi am chi qua trinh

nguyn t hoa cua nguyn t phn
tich.
Hg la nguyn t duy nht co dang hi
nguyn t nhit thng ( lanh
hn cac nguyn t khac)
Do vy, phep phn tich Hg chi cn
a tt ca dang Hg lin kt v dang
Hg t do - u vit va n gian hn so
vi cac phng phap con lai.

Phng phap ph nguyn t co cho phep phn

tich nguyn dang c khng? Giai thich?

Khng, vi ph nguyn t chi phn

tich c n nguyn t sau khi a
ct t tt ca lin kt hoa hoc
Mun phn tich c nguyn dang,
ph nguyn t phai c ghep ni
vi cac h phn tach nh GC hoc x
ly mu chon loc (SPE, chit phn
oan)

Cac thng tin nao la cn thit cho vic dng

mt ng chun cho AAS? Giai thich?

Co ba yu t: ban cht cht phn tich,

ky thut nguyn t hoa , nn mu.
Cac yu t trn anh hng n ty s
S/N cua tin hiu cht phn tich. Vi mi
ty s S/N c trng cho tng iu kin
phn tich, mi ng chun se co LOD
va LOQ khac nhau
Ngoai ra , khoang lam vic cua ng
chun con quyt inh ln vic s dung
ng chun tuyn tinh hoc phi tuyn.

Tac dung cua phng phap thm chun? Nhc

im va iu kin s dung cua thm chun?

Tac dung : bu tr / giam thiu anh hng

t nn mu cai thin nhay khi
nng cht phn tich tng i thp
Nhc im : khng can thip c vao
nhiu ion hoa va nhiu quang ph.
Ta s dung phng phap thm chun khi
phat hin ra nhiu vt ly (qua pha loang
mu). Lng thm chun cung phai
c da trn s phong oan ham lng
cht phn tich trong mu.

Vi sao trong AAS ngi ta thng dung

ng chun phi tuyn?

nng cao, s t hp thu cua cac

cu t cht phn tich lam sai lch
inh lut Lambert-Beer.
Do vy, khoang lam vic tng i
rng hoc khi phn tich cac nguyn
t kem nhay, vic s dung ng
chun phi tuyn cho kt qua phan
anh ung hin thc din ra trong
plasma hn.

Yu t quan trong nht quyt inh nhay cac

bc xa vach cua ph hp thu nguyn t?

Mt cac bc xa k cn cua bc xa
vach c quan tm. Nhiu quang
ph xay ra t iu kin t nhin nay.
Ngoai ra, banh rng ph t nhin
cung gop phn lam giam nhay
cho peak hp thu (vn be va rng
hn peak phat xa)

Nhc im ln nht cua phng phap

phn tich bng hi hydride?

S gii han cac nguyn t co th

phn tich bng HG-AAS. Chi co 8
nguyn t co th tao hi hydride,
nhng chi co 4 nguyn t c phn
tich thng dung do LOD thp va
nhay cao : As, Se, Te, Sb.
Ngoai ra, s phn huy cac hydride v
nguyn t t do din ra theo c ch
gc t do hoat tinh cao kho kim
soat va d mt mu

So sanh hiu sut cua tao hi hydride

theo me va dong lin tuc. Giai thich?

Hiu sut ly mu cua batch mode la

hoan toan, cao hn continuous flow
do lng hoa cht kh hoa s dung
thp hn
Ngc lai, phn tich bng continuous
flow tit kim hoa cht hn, s trn
mu u hn va co th t ng hoa
tt hn.