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Mobile phase
Detector
t1
t2
t3
t4
Detector
signals
t0
t0
t1
t2
t3
t4
Time
Chng 4:
1. Sc k kh ghp khi ph
Phng php ph khi lng (Mass Spectrometry - MS) l mt
phng php phn tch cng c quan trng trong phn tch
thnh phn, cu trc cht
Bt u t cui th k XIX, Goldstein (1886) v Wein (1898) thy
rng mt chm tia ion dng c th tch ra khi nhau di tc
dng ca mt in trng v t trng
1913, Thomson thy kh neon t nhin gm 2 loi c khi lng
nguyn t khc nhau (isotope) l 20 v 22 (g/mol), ng cng s
dng my ph khi lng trong phn tch ha hc, xc nh khi
lng phn t v nguyn t
1940 MS c s dng trong pht hin du m v trong phn
tch hormon/steroid (1950). S kt hp GC/MS thc hin nm
1960 v LC/MS nm 1970. Sau nhiu k thut mi trong MS
nhanh chng pht trin nh FAB, TS, t cc, TOF, MALDI
C phm vi ng dng rt rng ln trong cc ngnh ha hu c,
ha sinh, v c v nguyn t ng v
ABCD+
+ 2e
> 95%
ABCD2+ + 3e
ABCD-
2. C s k thut ca MS
Thit b khi ph u tin c J. Thomson (Anh) ch to nm
1912 v c hon thin hn vo nm 1932. S chung:
Np mu
Ha kh
mu
Ion ha
Phn tch
ion theo
s khi
Bm ht
detctor
X l s
liu
1. Np mu v ha kh mu:
2. Ion ha:
cc phn t dng kh phi c ion ha bng cc pp thch hp.
Phng php va chm electron (Electron impact - EI): Phng php ph
bin, dng kh ca mu i vo bung ion ha, va chm vi dng electron
t mt si t (catod) chuyn ng vung gc vi dng phn t mu. p
sut bung ion ha t 0,005 torr, to 200 0,25oC.
Cc e va chm vi pt trung
ho to cc mnh ion, mnh
gc hay pt trung ha nh. Sau
cc ion i qua mt in
trng 400 4000V tng
tc, vn tc ion t l vi khi
lng ca chng.
H2
CH4
H2O
CH3OH
i-C4H10
NH3
(CH3)2CO
H3+
CH4+, CH3+, CH5+, C2H5+, C3H7+
H+, (H2O)n
H+, (CH3OH)n
C4H9+, C3H3+
H+, (NH3)n
(CH3)2CO+
CH4 + e CH4+ + 2e
CH4+ + CH4 CH5+ + CH3+
CH4+ CH3+ + H
CH4+ CH2+ + H2
CH3+ + CH4 C2H5+ + H2
CH2+ + CH4 C2H4+ + H2
CH2+ + CH4 C2H3+ + H2 + H
(MH l mu cht)
Thng thng nht l dng thit b t trng hnh qut (sectorfield spectrometer) tch cc ion theo khi lng
Cc ion trc khi ra khi bung ion ha c tng tc nh
mt in trng c th U, i qua nam chm hnh ng c t
trng H. Cc ion s chuyn ng theo hnh vng cung bn knh
r trong t trng ny. Vi r:
Trong K: hng s,
V: in p tn s cao,
r: khong cch 2 in
cc i nhau, f: tn
s dao ng ion
phn
gii ph k
t
cc
thng
thng t
t 500
1000, mun
nng
cao
Rs, ni 2
3 b t cc
vi
nhau
nh
hnh
di (Rs c
th t ti
20.000):
4. Detector:
Sau khi ion hnh thnh v tch khi nhau theo s khi, chng cn
c pht hin v ghi nhn nhim v ca detector. Cc loi
detector trong MS gm c cc Faraday, nhn electron th cp, tm
knh nh nhy ion, h thng m ion.
5. phn gii ca MS:
phn gii l kh nng tch 2 s khi lin nhau m v m + m.
phn gii R ca MS c tnh theo:
3. Sc k kh ghp MS
Cc mu cht trong phn tch MS phi nm dng hi do hn
hp kh mang v mu cht t GC c th a vo bung ion ha
ca MS nhng phi gim tc kh mang t ct i ra khong <
2ml/min
Turbo
pump
Rotary pump