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Bi thu hoch - ICP-MS

ICP - MS (Inductively Coupled Plasma Mass Spectrometry)

Ph khi plasma cm ng cao tn
1. Gii thiu
ICP-MS l mt k thut phn tch c ng dng trong
nhiu lnh vc vi kh nng phn tch c hu ht cc nguyn
t trong bng h thng tun hon gm cc nguyn t kim v
kim th, cc kim loi chuyn tip v cc kim loi khc, cc
nguyn t t him, hu ht cc halogen v mt s phi kim so
vi k thut F-AAS ch xc nh c 56 nguyn t, l graphit
xc nh c 69 nguyn t, MHS ch xc nh c 8 nguyn
t.
Nu nh AAS ch c kh nng xc nh c tng thnh
phn nguyn t th ICP-MS c th xc nh c tng dng nu
nh trc khi i vo ICP mu c chy qua h thng tch. Cc k
thut ghp ni ca k thut tch u c th ghp ni c vi
ICP-MS. Vic xc nh c thnh phn cc dng rt c ngha
trong nhiu php phn tch v i khi vic ch xc nh c
tng cc thnh phn khng phn nh c y cc vn .
Ngoi ra ICP-MS cn c kh nng xc nh c cc ng
v ca nguyn t v n xc nh da trn nguyn tc ph
khi lng.
Nguyn l hot ng
Trong AAS cc cht cn phn tch c chuyn thnh cc
nguyn t t do trng thi kh, cc nguyn t t do ny c kh
nng hp th nh sng n sc c bc sng khc nhau lm hao
ht nng lng nh sng ti. Nng lng nh sng ti b hao ht t l
vi s lng nguyn t t do th hi do t l vi nng
cht cn phn tch. Trong OES s dng ngun nng lng cao
hn chuyn cc nguyn t t do ln trng thi kch thch,
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Bi thu hoch - ICP-MS

chng lun c xu hng nhy v trng thi c bn ng thi pht

ra nng lng. H thng ghi li ngun nh sng pht ra. Nhng
trong ICP-MS cc nguyn t t do b ion ha, thit b m trc
tip cc s lng ion, s lng ion m c t l vi nng cc
cht cn phn tch do gim thiu c sai s.
ng dng:
- Mi trng;
- Cng nghip bn dn (semiconductor)
- Ht nhn (nuclear)
- Lm sng, dc phm (clinical, pharma...)
- Ha du (petrochemical)
- Y php (Forensic);
- a ha (Geological);
- Nghin cu hn lm (Academia);
- Kho c
Sampl
Sample
ICPData review
e
digestio
MS
and
loggin
n
analys
reporting
Cc
qu
trnh
din
ra
trong
ICP-MS:
g
is
Liqui
d
samp
le

Archiva
l

Aroso
l
Particl
e

Molecul
e

Atom

Ion

Solid
samp
le

Mass
Spectru
m

Hay
Sng
ha mu

Kh
solv
at

Bay
hi

Nguyn
t ha

Ion
ha

B
phn
tch
khi

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Bi thu hoch - ICP-MS

Vi cc qu trnh din ra trong ICP-MS nh vy kt cu

phn cng ca thit b bao gm:
- Truyn mu
- Plasma
- Giao din
- H thng chn khng
- Hi t ion
- Bung Collision/Reaction
- B phn phn tch khi (tch khi lng, tch ion)
- Detector
2. Cu to phn cng
2.1. H thng truyn mu
H thng truyn mu l mt trong nhng cu kin quan
trng nht ca ton b h thng ICP-MS. Mc ch chnh ca
h thng truyn mu l chuyn mu lng thnh aerosol v
truyn nhng git nh hn mt cch hiu qu vo tm
plasma, trong khi nh bt nhng git ln hn v nhng git
ln hn ny khng th phn hu hon ton trong plasma.
Bung phu sng c lm mt bng k thut Peltier (khng dng
gas hay kh lng lm lnh). nhit cao c th xy ra
cc phn ng bt li, do vic gi u phun sng nhit
thp trnh hnh thnh cc polyatom gy nh hng
ng thi ngng t hi nc thi ra ngoi.
Do h thng truyn mu l i tng tip xc trc tip vi
cc cht ho hc khc nghit v s n mn c hc, dn n
c mt yu cu quan trng l phi d bo dng.
Cc loi u phun sng:
Mu i
- u
phun sng ng trc (CN): u phun sng ng
vo
trc l mt trong s nhng u phun sng ph bin nht.
3
Kh mang

Ht sng
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Bi thu hoch - ICP-MS

Mu c kh mang ko vo qua u phu sng to thnh cc

ht sng. Mt bt li ca u phun sng ng trc

l kh

nng d b tc nghn chp u phun khi nng cht rn

ha tan cao hn c truyn vo. Vn khc c th xy ra l
tnh trng r r ng kh Ar v dng mu; nu nh cc vng Oring cho ng mu khng c xit cht, c th xut hin r
r.

S u phun sng ng trc

- u phun sng High solids nebulizer: u phun sng c
dng mu lin tc chu c cht rn ha tan cao, thch hp
dng cho phn tch mu nc bin. u

phun

sng

kiu

Agilent High Solids Babington c ch to bng PEEK (polyether

ether ketone) v khng li hu ht cc loi axit, baz v dung
mi hu c. Nguyn l phun sng rt n gin: c hai l cho
ng mu v ng kh mang, mu (c phn phi bi mt
bm nhu ng) i ra khi l pha trn v kh mang i ra
khi mt l nh pha di l ht mu v nebulize ha mu.
- u phun sng dng cho
- u phun sng dng Micro
2.2. Plasma
Plasma l mt dng kh chy hnh thnh t s dao ng
cp ngu ca cc in t t do vi tn s cao. Cun cm qun
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Bi thu hoch - ICP-MS

quanh torch ni vi my pht cao tn c dng 27,12 MHz. Kh Ar

i trong ng thch anh i qua cun cm, nhng phn t tch
in dao ng, do tn s dao ng ln cc phn t kh dao
ng hn lon va chm ma st ln nhau v bc chy, pht
nhit. Tuy nhin phi iu chnh cun cm vi torch kh Ar
khng chy trong ng m ch khi i ra khi ng thch anh mi
bt u bc chy trnh chy torch.
Ar c chn lm kh chy plasma v:
- R;
- D iu ch tinh khit;
- Ar c th ion ha th nht (th cn thit nh bt 1
in t) cao hn hu ht cc nguyn t khc. Trong khi th
ion ha th hai thp hn th ion ha th 2 ca hu ht cc
nguyn t khc (tr mt s nguyn t nh Ca, Sr, Ba...). Do
khi s dng kh Ar hu ht cc nguyn t s chuyn thnh dng
tch in 1+.
Kh Ar cc ht arosol, kh b tr, kh plasma u tip
xc vi cun cm dao ng i ra khi torch v bc chy.
Cc ht arosol i theo double - pass o chiu 360 0 ,
nhng git ln va vo thnh ri xung ch cn cc git sng
nh i vo tm ca plasma v i dc theo li la. Ti y xy
ra cc qu trnh vt l bao gm sy kh, bay hi, nguyn t
ha v ion ha. Trong plasma lc ny tn ti mt lng ln cc
in t, cc ion v cc polyatom, cc ion 2+. Cc ion sau khi c hnh thnh trong plasma s c tch ra khi trung tm
plasma i vo ph khi. Vn t ra l phi nh v
chnh chnh xc knh trung tm v v tr Sampling cone
vo vng plasma c cha mt ion cao nht. N l nhng
ion s c o to ra tn hiu phn tch.
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Bi thu hoch - ICP-MS

Bn cnh cn mt yu t l su ly mu. Khong

cch t chn plasma n li la l chiu su ly mu ca
torch. Thi gian lu mu trong plasma cng di th qu trnh
phn ly, nguyn t ha v ion ha din ra cng trit . Do
cn iu chnh torch cng di cng tt. Ti chp plasma
v mt ct tit din ca Sampling cone, mt ca cc ion
nguyn t l cao nht ng thi vn tn ti cc polyaton i vo
v cc polyatom mi hnh thnh.
* Ti u iu kin plasma
- Gim lng mu i vo ngn la plasma: ngc li vi AAS,
ICP-MS cn gim thiu ti a lng mu i vo ngn la plasma
do nhy ca quarupole qu cao. gim lng mu cn iu
chnh tc ht mu ca Nebulizer, s dng tc thp
l/pht, nl/pht. Vic gim lng mu i vo ngn la plasma
cn ko theo nn gim, cc nh hng v nn cng gim theo.
- Gim hi nc i vo plasma bng cch s dng h thng
lm mt bung phun sng (Spray chamber).
- Tng thi gian mu tn ti trong plasma qu trnh
phn ly, nguyn t ha, ion ha din ra c trit . Do
cn iu chnh ngn uc plasma di nht c th (max l
13mm, thit b cn chnh ti u 8,5mm).
- S dng ngn uc rng: khi plasma ln th li la trung
tm plasma ln, qung ng mu s c di chuyn trong
plasma ln.
- Tng ti a nng lng ion ha bng cch:
+ Tng cng sut ngun pht (tnh theo W);
+ Gim lng mu i vo plasma (gim tc mu thng
qua gim tc bm nhu ng, gim tc dng kh
mang);
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+ Loi b v gim i cc nguyn t d b ion ha, hiu

ng trit thoi ion (KL kim, KL kim th, ...). Chng cnh tranh
lm mt nng lng ca plasma lm cho nng lng ca plasma
khng ion ha cc nguyn t cn phn tch.
2.3. Cone (giao din)
Sau khi i ra khi plasma m hi ion nguyn t s c
hi t thnh mt bng hp nh sampling cone v Skimmer
cone. Cone c lm t Nikel v Platium. Sampling cone khng
c in p (tip t).
Nhim v ca cone l hi t chm ion i thnh mt bng
hp. Lun c mt lp Ar khng chy bao bc xung quanh ngn
la ICP cch ly ngn la vi mi trng bn ngoi v chng
lun chuyn ng ng thi chng cn c tc dng lm mt
ngn la plasma khng tip xc vi cc thnh phn khc.
Cng do lp v Ar bao bc bn ngoi torch nn cone mc d tip
xc trc tip vi ngn la plasms cng khng b nng chy.
ng thi cone cn c lm mt bng nc.
Mt trong ca sampling cone c mt lp v Ar (nguyn t
Ar t do) bao bc vi dy nht nh. Plasma tch in (+)
do s lng ion ln, lp v phn tip gip vi sample cone tch
in (-) (do tip t), mt cn li tch in (+) to ra mt t
in ngay lp v Ar xung quanh mt bn trong ca Samlping
cone. N to ra hin tng phng in lm cho cc phn t Ar
b ion ha v cc polyatom trung ha v in b ion ha tr li
to ra cc yu t nh hng.
2.4. Thu knh
2.4.1. Thu knh chit
Thu knh chit c t ch ngay sau skimmer cone v
c gn ln b skimmer. Hai thu knh c iu khin ti
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Bi thu hoch - ICP-MS

in p m. Cc ion dng tin n gn thu knh chit v

cc ion c tng tc. Mt khc cc in t b cc thu knh
chit y v tin n tip t theo hng skimmer cone v
thnh bung chn khng.
2.4.2. Thu knh omega
Nhim v ca thu knh omega ny l tch cc
photon v cc ion v li cc ion vo Q-pole. Cc thu knh
omega gm 2 cp hnh li lim, phn trn tch in (+) v
phn di tch in (-) (v ngc li i vi cp cn li) vi cc th
khc nhau, do photon nh sng (do khng tch in) v cc
phn t trung ha khng chu tc ng ca in t trng s
i thng v c tch khi dng ion. Trong khi cc ion (+)
c to ra nh plasma i qua trng tnh in trong h thng
thu knh, chng c th b ht vi trng m in v b y
t trng dng in, do b un cong chiu chuyn ng.
Cc thu knh omega tch c cc photon nh sng v cc phn
t khng tch in, lm lch ng i ca chm ion, do
chng cn c gi l cc thu knh lch trc hay o trc (offaxis). Chm ion sau khi i ra khi cc thu knh omega thnh
mt bng hp v i vo b tch t cc.
2.5. Bung phn ng bt cc
Bung phn ng bt cc gm 8 thanh xp theo hnh bt
gic trong mt khng gian hp. Nhim v ca bung phn ng
bt cc l loi b cc nh hng v ph. Bung phn ng bt cc
c np kh H2 hoc He hoc cc kh hot ng (NH3, CH4).
Cc ch hot ng:
1. Ch hot ng thng thng: Khng c dng kh va
chm i vo bung phn ng. Lc ny bung phn ng ng
vai tr l cu dn ion, tc l cp nng lng ion i qua .
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Bi thu hoch - ICP-MS

2. Ch va chm
Mt dng kh n nh c m v bung phn ng. Vi
cc h thng multipole khi c dng mt chiu cc ion b p i
thnh mt bng hp xuyn tm.

Lc ny trong bung phn

ng c cc ion cn phn tch v cc polyatom nh hng. Cc

polyatom c cng khi lng vi cc ion cn phn tch nhng c
kch thc ln hn cc ion cn phn tch. Kh tr khi np vo
bung phn ng khng phn ng vi cc ion cn phn tch nhng s va chm vi chng. Do cc polyatom c kch thc ln hn
cc ion cn phn tch nn xc sut va chm v tn sut va
chm ca chng vi cc phn t kh tr s ln hn rt nhiu so
vi cc ion cn phn tch. Cc polyatom s mt nhiu nng lng
hn so vi cc ion cn phn tch nn khng nng lng
i n b phn tch khi t cc. Hai u octapole u c
thu knh (octa lens). Cc thu knh ny s cp nng lng b
li phn nng lng mt i nhng phn nng lng ny ch
cho cc ion cn phn tch i vo b tch t cc m khng
b li nng lng cho cc polyatom i vo b tch t cc.
Khi s dng kh tr trong ch va chm th kh tr
ch va chm vi cc polyatom v cc ion cn phn tch nhng
khi s dng kh hot ng NH3, CH4 th cc polyatom c cha
oxy l cc polyatom hot ng phn ng vi cc kh hot ng
to ra cc sn phm ph khc. Nh vy cc polyatom nh hng s
mt i nhng c th sinh ra cc polyatom khc cng c th gy
nh hng ng thi cn lm bn h thng. V vy cc kh
hot ng b hn ch s dng trong ch va chm ca
bung phn ng.
Bung np kh phn ng s c qut ng b vi t cc
chnh v c khng ch bng bng thng ng hc.
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Bi thu hoch - ICP-MS

Hiu qu tch ca bung phn ng ph thuc vo kh

nng v tn s va chm ca kh c np trong bung phn ng.
Do khng gian ca bung phn ng phi hp v di
tng tn sut v tn s va chm.
2.6. B tch t cc
Quadrupole: gm 4 thanh Mo siu tinh khit song song
(poles) c xp xp mt khong cch tng ng tnh t
trc trung tm (trc tng tng). B mt bn trong ca cc
thanh Q-pole c dng hyperbolic to ra mt in trng l tng
bn trong Q-pole. Hin nay chuyn thnh mt thanh Mo c
khoan xuyn tm. Vic pht trin ln thnh mt khi l mt
tin b ln (c gi l t cc nguyn khi monolithic).
Nguyn l hot ng:
Quadrupole l mt b lc khi (hoc c th hn l b lc
khi lng trn in tch (m/z)) tch cc ion ca nhng gi
tr m/z khc nhau. Trong b tch t cc cc cc thay i lin
tc (3 triu ln/s) lm cho cc ion dao ng theo hnh xoy
trn c xung quanh trc xuyn tm v tch ra khi nhau. i vi
mt cng v tn s c th ca in trng, ch nhng ion
c khi lng chn lc i qua (filter) b lp ghp tin n
b pht hin ion (detecto). Nhng ion c khi lng qu ln hoc
qu nh so vi ion c th i qua quadrupole s va vo cc thanh
v bin mt. Nh thay i in trng theo mt kiu nht
qun, khi lng ca tt c cc ion c to ra trong ngun c th
c qut tun t t khi lng thp n cao hoc ngc li
to ra mt ph khi.
2.7. Detector
2.7.1. Detector nhn in t

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Bi thu hoch - ICP-MS

Mt ion dng i n ming detector, n p vo dynod

u tin, dynod ny c gi ti in p m cao. Tc ng
ca ion nh ra mt vi in t t do t b mt dynod, nhng
in t ny c y khi mt trc in p m cao v va vo
dynod k tip. Mi in t va vo dynod th hai nh ra t b
mt mt vi in t v c nh th xui theo nhiu giai on
ca detecto. Theo thi gian tng in t n c dynod cui
cng, h s nhn tch lu mt xung ln c th o c
mt cch tin cy nh mt "s m" ion.
Detector nhn in t hot ng trong c hai ch
m xung v ch analog. Khi nng mu thp (s lng
ion t) detector hot ng vi ch m xung tc l cc ion
i n tn dynode cui cng. Nhng khi nng mu cao (s lng ion ln) cc ion ch i n dynode th 13 th dng li v
c o ti . Thit b t ng chuyn gia cc ch . Khi
tn hiu <106, thit b hot ng ch m xung, nhng
khi tn hiu vt qu 106-109 thit b t ng chuyn sang ch
analog. Nh tnh nng ny nn ICP-MS c di tuyn tnh
rng.
2.7.2. Detector nhn quang in
3. Loi b nh hng
3.1. nh hng v ph
Cc bin php gim thiu nh hng ph:
- S dng cc ng v khng b nh hng;
- Ti u thit b;
- Ti u iu kin plasma;
- S dng tm chn shield torch: mt tm chn c chn
vo gia ngn uc v cun RF v c tip t. Khi plasma
c hnh thnh tm kim loi tch in (+) nhng do tip t
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Bi thu hoch - ICP-MS

nn b trit tiu in th do lp Ar bn ngoi khng cn

tch in, th in p plasma c gim v 0 mt cch hiu
qu. H qu tt yu khng cn ko di hin tng phng in
th cp v cc ion poly nguyn t khng b ion ha pha sau
Sampling cone. Do t bn thn plasma cng to ra cc ion
polyatom ny nn gim cc ion polyatom hn na, nhit
plasma c gim xung. Nh h thp nhit plasma, h
thng ShieldTorch gim t ngt cc yu t nh hng ny dn
n nng cao gii hn pht hin.
3.2. nh hng nn:
Bin php hu hiu gim thiu nh hng v nn l
vic x l mu. Ngoi ra thit b cng gp phn gii quyt cc
nh hng v nn nh vic s dng tc ht mu nebulizer
thp gim lng mu ng thi cng gim nn; s dng cc
hm hiu chnh nh hng lp hm b tr s nh hng; ...
* Hiu ng tch in khng gian: Sau thu knh chit,
chm ion phn ln l tch in dng. Lc y mnh tn ti
trong phm vi chm ion c tc ng ln ion khi lng thp mnh
hn nhiu so vi ln ion khi lng cao dn n lm phn tn
phn khi thp ca chm ion. Khng kim sot c hiu ng
tch in khng gian s dn n lm mt nhy khi thp,
c bit l trong s c mt ca nn mu cao.

Hiu ng tch in khng gian

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Bi thu hoch - ICP-MS

* Hiu ng trit thoi tn hiu trong vng plasma: cc ion

d b ion ha va chm vi cc ion cn phn tch lm chng
nhn thm in tch chuyn thnh dng 2+, ngoi ra ion
phn tch cn nhn in t t mi trng in t m c
tr thnh cc phn t trung ha lm mt cc ion cn phn
tch (tc l mt mu).

Hiu ng trit thoi tn hiu trong vng plasma

4. Ni chun
Ni chun thng c s dng trong k thut sc k v
ph khi.
Ni chun l mt cht c bn cht ha hc gn ging nht
vi cc cht trong mu phn tch nhng khng c php c
mt trong mu. Vic p ng yu cu ny l rt kh nn cht
ni chun thng ch p ng c chng c bn cht ha hc,
cu trc phn t gn ging vi cc cht trong mt nhm cht
(biu hin trong k thut o lng v tch ging nhau) v d
nh thi gian lu gn trng vi mt hp cht no hay i lc gn
ging vi nhng cht xung quanh n.
Trong sc k cht ni chun thng l hp cht tng hp v
lm giu mt ng v trong hp cht . Do chng c khi

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Bi thu hoch - ICP-MS

lng khc vi khi lng ca hp cht cn phn tch, MS s tch

ring nn khng trng vi hp cht no.
Trong ICP-MS, ni chun l nguyn t m ng v ca n
khng trng vi bt k ng v no. N lm ni chun cho cc
nguyn t ng v c khi lng xung quanh n.
Hp cht ni chun c a vo mu trc khi a ln thit
b phn tch. Trong qu trnh phn tch ni chun cng vi
cht cn phn tch cng i vo h thng, do n c th b
tr nhng dao ng ca thit b v nhng dao ng ca
thit b tc ng ln cht phn tch nh th no s tc ng
ln cht ni chun tng t.
Cht ni chun c cho vo tt c cc mu t blank,
reagent blank, chun v mu mt lng nh nhau nhng dao
ng ca tn hiu ni chun trn l thuyt phi l nh nhau
gia cc mu. Tn hiu dao ng ca cht ni chun trong cc
mu s c b tr cho s s dao ng ca mu u tin.
Tuy nhin cht ni chun ch b tr cho s dao ng ca
bn thn thit b, hiu chnh dao ng ca tn hiu gy ra
bi:
- Nn: + s dao ng ca bm nhu ng,
+ Nebulizer: s xut hin bt kh,
+ ion ha: RF khng n nh, nhit khng n nh,
+ Hiu ng tch in khng gian,
- tri ca thit b
5. K thut lai ghp
Vic x l mu trc ch gip xc nh c dng tng m
khng xc nh c thnh phn v mc ng gp ca chng
trong tng thnh phn. Cc k thut lai ghp s gip gii quyt
vn ny.
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Bi thu hoch - ICP-MS

- GC-ICP-MS: ton b mu khi i ra khi GC i vo torch

ca ICP-MS. Lc ny ICP-MS ng vai tr nh mt detector. Ngn
la plasma ch dng ion ha, khng c dung mi nn khng
c nh hng, nhit ca plasma l cao nht, ton b ph
khi pha sau ch bt ng v ca mt nguyn t. Vn
t ra l

ng truyn gia GC v ICP-MS phi tr, ngn

nht mc c th v c t nng ng u n nhit

cao hn nhit cao nht ca chng trnh l ngn chn
s ngng t mu.
- LC-ICP-MS: thay v dng bm nhu ng bm mu lng
th dung mi hu c sau khi i ra khi ct s i thng vo
nebulizer ch khng i thng vo ng thch anh. Nh vy
nebulizer phi chu c dung mi hu c. i vi h thng lai
ghp GC-ICP-MS ch c kh tr i vo torch nhng vi LC-ICPMS cn c cc gradien dung mi vi thnh phn dung mi thay
i v th thit b phi thay i nhanh p ng li s
thay i ca dung mi.
* Bn nh lng: dng mt chun ca mt hoc vi ba
nguyn t cn li tt c cc nguyn t khc s dng li ng
chun nh lng. Bn nh lng c dng kho st
v n cha tuyt i chnh xc nhng vn tin cy (
chnh xc 30% so vi gi tr nh lng y ).
6. ICP-MS/GF-AAS / ICP-OES sequential / ICP-MS simultaneos
T

Ch tiu

GF-AAS

T
1.
2.
3.

ICP-OES

ICP-MS

ICP-MS

sequent simultane
LOD
Di tuyn tnh
nh hng

ppt
2-3
C mc

ial
ppb
4-6
Nhiu

15

ous
ppb
4-6
Nhiu

ppq-ppt
9
t

Trng Th Hng Hnh

4.
5.

Tc
Di nguyn t

6.
7.
8.

a nguyn t
ng thi
Th tch mu

Bi thu hoch - ICP-MS

Chm
Poor
Khng
Khng
l

Chm
Good
C
Khng
ml

Nhanh
Good

Nhanh
Excellenc

C
C
ml

e
C
C
l hoc

9.

Chi

ph

ban

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ml
***

10.

u
Chi ph

vn

***

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hnh

1. Autosampler
Khay mu: c rnh nh trn b t khay lp kht
khay mu. Khay c 89 v tr, trong c 10 v tr ln s
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Bi thu hoch - ICP-MS

dng i vi nhng mu, dung dch cn s dng lng th tch

nhiu nh blank, chun nh k (CCV), ...
Bn phi khay mu c mt v tr t l to. C hai
cht thay i cao v tr t l (tc l thay i l vi
th tch khc nhau). Khi s dng v tr ny phi b khay mu
ra trnh b vng. S dng l mu vi th tch ln nh vy khi cn
phn tch nhiu thng s trong mt mu, tc l s dng lng
th tch mu ln cho mt ln phn tch (khong 100ml). V
th v tr ny cn c gi l single sampler.
Bn phi khay ly mu c ba v tr t ba l vi th tch
ln. Thng thng y l v tr t cc dung dch ra,
dung dch tune. Chng trnh phn mm thit k cho ra ti
a vi 3 dung dch. Vic t v tr cc dung dch ra l ty
chn, sau khai bo trn phn mm. Dung dch ra sau phi
mnh hn dung dch ra trc (nng axit cao hn hoc l
cc hn hp axit mnh hn) v thi gian ra sau ngn hn thi
gian ra ln trc v nguyn tc vn hnh ca ICP-MS l tit
kim ti a thi gian vn hnh v chi ph vn hnh ICP-MS l
kh cao. Thng thng dung dch ra th 3 bao gi cng l nc
ct trong trng hp ra bng c 3 dung dch. Nhng tt nht l
ra bng 2 dung dch, dung dch ra mt l axit v dung dch
ra th hai l nc ct.
Ngoi ra cn mt v tr ra na l ra bng bm rinse
pump (bm ra). C hai ng mt ng bm dung dch ra
vo v mt ng thi. Hai ng bm c t ngc theo chiu
quay ca bm khi bm hot ng s ko dung dch ra
vo. Nguyn tc ra khi s dng rinse pump l nguyn tc
chy trn. Dung dch c ko vo ra c nh trn
autosampler. u tp cm ngp trong dung dch ra. Dung
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Bi thu hoch - ICP-MS

dch ra ko lin tc ln v chy trn qua thi ra ngoi nn

dung dch ra lun l dung dch ti mi.
Cc dung dch ra t trn v tr 1, 2, 3 ch yu l ra
bn trong u tp cn ra bng rinse pump l ra c bn trong
v bn ngoi.
Khi vn hnh my cn chy bm ra trc khi phn tch
mu u tin ht dung dch ra ln np y ng bm,
ui ht bt trong ng bm ra trnh khi bt u phn tch
dung dch ra mi c bm ln th lc ny u tp vn cha c ra.
Vn

hnh:

ca

iu

khin

Instrument

Control/ALS/Rinse vn hnh bm ra.

Sau khi phn tch cn tho cc cht ca ng bm ra, tho
cht t trn ng bm trnh ng bm b cng, chng hng.
Chnh v tr u tp: u tp khi cm vo cc mu
thng thng cch y cc mu khong 2-5mm l thch hp.
chnh u tp bng c chnh th v chnh bng phn mm.
Ban u u tp cao hn mt cht trnh thp qu
u tp khi di chuyn d va vo np khay ly mu lm cong
vnh u tp. Chnh sao cho u tp gn st khay ly mu.
Bt phn mm Instrument Control/ALS/Goto. Nhp v tr
ly mu (theo s 1001, 1002 phn bit vi 3 v tr ra 1, 2,
3). Kch Move u tp di chuyn n v tr ly mu. Sau
vn c chnh u tp cm xung ng ly mu n
v tr thch hp (cch y cc ly mu khong 2-5mm). C th
iu chnh v tr u tp bng phn mm ring bit tc l
di chuyn tnh theo bc ca tay ly mu (mt bc tng ng vi
0,125cm). cao ca cc mu v v tr ra bng rinse pump l
tng ng. V th nng cao hiu qu ra c v tr ny
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Bi thu hoch - ICP-MS

khi mu vo cc mu khng nn y m cch

1cm. Khi u tp cm vo cc mu, su so vi khi cm
vo v tr ra l t hn 1 cm do dung dch ra c th ra
sch c u tp.
2. Sample pump
Sample pump ng vai tr a mu sang thit b. Trn
sample pump c 3 knh vi rng khe khc nhau. Knh 1 l
ng ly mu, knh th 2 c khe hp hn dnh ring lp ng
bm cht ni chun v knh th 3 l ng thi. Mi ng ng c
3 mu cht c bt c nh lp vo bm v c quy
nh mu khc nhau phn bit r rng:
- ng mu (Tygon) c cht mu en v trng;
- ng ni chun (Tygon) c cht mu cam v ;
- ng thi (PharMed) c cht mu vng v xanh;
Cc ng ng c lp ngc chiu quay ca bm. ng
mu c cm vo ng bm khong 2-3mm v phi thng
xuyn kim tra xem chng c b tut ra khi nhau khng. Cc
cht gi t p ng ng c cn su hp l nhng nu
nh bm hot ng m khng thy dung dch c ko ln th
phi sit ai c cht thm p ng xung, dung dch s c ko ln. Sau khi phn tch phi tho cc cht t ln cc ng
bm trnh ng bm b t p trong thi gian di lm cng
ng bm.
s dng ng ng ni chun, mt b kit chc 3 c lp
thm pha sau sample pump. Khi chy cc php phn tch c
s dng cht ni chun th ng ng ni chun s c lp vo
kt chc 3 cn bnh thng c cht kha v tr . Cht ni
chun v mu u c bm vo chc 3 v trn vi nhau ti
ri mi c a ln nebulizer. Thng thng nng cht ni
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Bi thu hoch - ICP-MS

chun l 50ppb nhng do ng ng ca cht ni chun nh hn

ng ng ca mu l 20 ln nn khi i vo chc 3 n s b pha
long 20 ln. V th nng pha ban u ca cht ni chun
l 1ppm.
Khi bm nhu ng hot ng s to ra ma st vi ng,
trong mu sn c cc ion phng in nn to ra hin tng tch
in lm nhiu tn hiu. loi b hin tng phng in b
kt chc 3 c lp thm mt cht mu en. Bn trong cht c
mt mt si Pt. Si Pt ny cm ngp trong dung dch mu v c ni vi b phn tip t trong thit b.
3. Bung phun sng v nebulizer
C 4 b phn c tho lp v bo dng thng xuyn:
nebulizer, bung phun sng (spray chamber), torch, connector.
Cc b phn tho ra c ra bng nc sch v nc ct v
kh t nhin (khng cho vo t sy).
Tho theo th t: nebulizer khi end cap, tho ng ng
thi bung phun sng, connector, torch.
Ch :
- Khi lp nebulizer vo encap cn ch lp nh nhng.
Chp ca nebulizer khi lp vo phi ngang bng vi thnh trong
ca endcap. Do c th ly mt tm th va y nebulizer
nh nhng vo va kim tra. Vn oring cht c nh
nebulizer. Khi vn khng ng n nebulizer trnh lm dch
v tr ca nebulizer. Lp cht xanh c nh ng kh mang.
Khi lp ch cn y mnh ng ng vo kha xanh. Khi tho
ra th n u cht vo ra ko ng ng ra.
- Sau tip tc lp nebulizer vo bung phun sng.
Ch ng kh mang (carrier gas) vung gc vi bung phun sng. Lp ng ng thi vo bung phun sng.
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Bi thu hoch - ICP-MS

- Lp torch: u tin lp tm shieldtorch vo torch, lp

ng ni. Tm shieldtorch phi chm vo ming ng mi c
hiu qu tip t. Kim tra u torch phi ngang vi mt ct
ca cun cm.
- Cui cng l lp connector vo gia torch v bung phun
sng. Dng kp kp cht connnetor. Lp hai ng kh vo
torch, vn cht hai cht c nh hai ng kh. Torch c
lp ng th mt ng kh vung gc v mt ng kh song
song vi ng carrier gas.
- Lp cc np bo v torch v bung phun sng. Kim
tra xem np c t ln cc ng dy hay khng.
- p sut kh He: 20psi (kim ng h hu nh khng
nhch)
Bnh Ar (kh mang, kh carrier, auxerier, plasma, make
up): p sut 100 l/in2.
2. Phn mm
2.1. Ca s Instrument control
n vng trn thit b nhy lin tc khi thit b ang trong
thi gian chuyn gia cc ch Shutdown Standby
analysis. n s chuyn sang mu xanh v ht nhy khi thit b
chuyn ch .
- Biu tng bt v tt plasms: nh la v tt
plasma. Bn cnh n trn thit b cn c mt nt Plasma off
dng tt khn cp plasma.
- Biu tng bt tt cc ca s hin th trn mn hnh:
ti a cho php hin th 5 ca s.
Vacumm: - IF/BK Press: p sut interface Backing
- Analyzer Press: p sut vng analyzer (bao gi cng
< IF/BK Press)
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Bi thu hoch - ICP-MS

- TMP revolution: s vng quay bm chn khng

(100%)
Water: water RF/WC/IF: nhit nc lm mt 3 b phn
S/C: Spray chamber: S/C temperature: 20C
Plasma RF: RF power 1000W
Optional gas: Kh Xe ng vai tr lm kh ni chun (ni
vi GC) v mu ra khi GC l kh.
2. Ca s Maintance
- ALS (auto line sampler: b mu lng t ng):
Goto: n v tr v cm xung ng mu
Move: ch di chuyn u tp n v tr cn thit nhng
khng h xung
Rinse: bm ra, trc khi phn tch phi u tp ko
y dung dch ra ln ra u tp v ng thi loi b
ht bt trong ng ng.
Home: v v tr ban u
3. Ca s ICP-MS configination
- Auto sampler IAS/Setup: khi khi hot ch Escape
mt s v tr thit b khng cho php t mu. Trong ch
ny di chuyn u kim trn khay mu, th khay mu s di
chuyn n mt s v tr c nh trn khay mu (khng cha
mu 32, 57, 77, 89), git mu u tp khng ri vo cc
mu khc trnh lm nhim mu.
- Moscellaneous:

S/C cooling

Plasma Ignotun Mode: ch nh la plasma.

Hin ti ang dng ch Aqueous solution. Nu lp HPLC
th chuyn sang ch Organic.
Remote

Shutdown:

(Standard)
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ch

tt

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Bi thu hoch - ICP-MS

Enable Post Rotation: Xoay bm nhu ng sau

khi phn tch xong: sau khi phn tch xong hoc
tm dng thit b thay mu th bm vn quay
trnh lm ng bm.
Post carry pump: khi u tp di chuyn bm
dng li nn git mu s treo trn u tp. Nu vn
bm hot ng khi u tp di chuyn th bm
s ko kh vo ng lm tc mt s v tr trn ng di chuyn ca mu lm nhiu tn hiu.
4. ISIS
4.1. Kt ni
- Remote 1 ni vi Remote ISIS ICP
- Autosampler ni vi controller 1;
- Chems my tnh ni vi chems ISIS.
4.2. Phn mm
4.2.1. Ti u ha cc thng s: ICP-MS tuning/ISIS/Prerun
- Uptake: tnh t lc bt u ht mu n lc mu i ra khi
chc 3 th nht +2s
- stablezation time:

23