Sac Ky Ion PDF

I CNG SC K ION
GII THIU H THNG IC DIONEX

NG DNG TRN MY IC
Ngi trnh by :
ThS. Phan Bch H
Cn. Nguyn Th H Linh
KHOA XT NGHIM
I CNG SC K ION
GII THIU H THNG IC DIONEX
ThS. Phan Bch H
Khoa Xt Nghim - Vin VSYTCC TP.HCM
PHNG PHP SC K
1903 Tswett (18721919) cng b tch
c cc cht mu trong cy c.
CHROMATOGRAPHY
ThS. Phan Bch H
Phn tch sc k
Nguyn l c bn
- Sc k l k thut tch cc cu t ra khi
hn hp da trn i lc khc nhau ca
mi cu t i pha tnh v pha ng
+ pha tnh: c tc dng gi cu t cn tch
(lp cht c nh)
+ pha ng: c tc dng ko cu t cn
tch ra khi ct (cht lng, kh)
ThS. Phan Bch H
PPPT sc k
+ kh nng phn tch cao, c th tch
nhng cht rt ging nhau v mt ha hc
ln vt l
+ l 1 trong nhng PPPT mnh nht
ThS. Phan Bch H
ThS. Phan Bch H
Phan loi sc k theo bn cht ca 2 pha s

dng
Pha
ng
Pha tnh
Cht rn
Cht
lng
Cht kh
ThS. Phan Bch H
Tn gi ca k
thut sc k
ng dng
Cht lng
Sc k ct, sc k
lp mng, sc k
lng cao p
Sc k lng - lng Sc k lng cao p
Cht rn
Sc k kh - rn
Cht lng
Sc k lng - rn
Sc k kh - lng
Sc k kh
Phn loi sc k theo cu hnh

Hnh hc
Phng
Ct
ThS. Phan Bch H
Cu hnh sc k
Chiu di chuyn ca pha ng
Giy
i ln, i xung, t tm lan to trn
Lp mng
i ln, i xung, t tm lan to trn
Ct h
i xung
Sc k kh
Nh vo ngoi lc
Sc k lng cao p
Nh vo ngoi lc
Ct sc k
ThS. Phan Bch H
Th t ra khi ct
Hp cht c i lc nhiu vi pha ng th c xu
hng ra khi ct trc
Hp cht c i lc nhiu vi pha tnh th b gi
li lu hn trong ct v ra sau
ThS. Phan Bch H
10
Sc k
ThS. Phan Bch H
11
SC K ION
A special application of HPLC
1975
ThS. Phan Bch H
12
So sanh vi HPLC
i tng
Pha ng
Th tich cht ngoai ct
ng kinh, chiu dai,
c ht ca ct
Chiu rng mui sc ky
ThS. Phan Bch H
HPLC
IC - CD
Phn t
trung hoa
Hn hp
dung mi
Nho hn
Ion (chu yu
anion)
Dung dch
Ion
Ln hn
Nho hn
Ln hn
Nho hn
Ln hn
13
ThS. Phan Bch H
14
INH NGHIA
Sc ky ion l ky thut tch cc cu t
anion hay cation t hn hp qua ct sc
ky da trn i lc khc nhau ca mi ion
i vi pha tnh va pha ng.
Ion cng b gi mnh bi pha tnh thi cng ra
tr.
Gradient : tng nng /in tich ca eluent.
ThS. Phan Bch H
15
Nguyn ly
Sc ky ion tch cc ion va phn t phn
cc da trn in tich ca chung.
IC-CD : Pht hin ion chu yu da trn
dn in
Dung dch ion c tinh dn in nn khi s
dng CD cn kh nn.
ThS. Phan Bch H
16
Thnh phn c bn ca sc k ion
ThS. Phan Bch H
17
S THIT BI SC K ION
ThS. Phan Bch H
18
Ion Chromatography
HCO3-/CO32- Eluent
Sample Loop
Eluant
0.0028M NaHCO
0.0022M Na CO 2
~2 ml/min flow
3
3
500 - 5,000 psi

1,000 nominal
Check for air bubbles
Pump
50 ul
Sample
Inject Valve
Sample in Syringe
or from Autosampler
Waste
Guard Column
PO 43SO 4=
Separator Column
RNR +
3
NO 3-
Cl -
RNR +
3
CO =3
SO 4=
2RNR
HCO
+
3
2RNR
Cl -
Cl +
3
SO 4=
HCO 3-
+
+
CO =3
H+
Na +
--
H 2CO
OH -
H 2O
Self Regenerating
Anion Suppressor
+
-
Conductivity Detector
ThS. Phan Bch H
Chromatogram
NO -3
- Cl
F
Conductivity (uS)
H 2O
H2
Cathode
Anode
--
Cation Exchange
Membrane
+
-
Cation Exchange
O2
HCO -3 Na +
Membrane
"R" = latex resin particle
SO 4=
PO 43-
water dip
time
Computer/Integrator
19
Ion Chromatography
OH - Eluent
Degas
Eluant
40 mM
NaOH
Degas
Eluant
DI Water
Sample Loop
500 - 5,000 psi

1,650 psi nominal
Quaternary
Pump
100 ml
Sample
Inject Valve
Sample in Syringe
or from Autosampler
Waste
Guard Column
PO43SO42-
Separator Column
RNR +
3
NO3-
OH+
3
2RNR
Cl-
Cl -
RNR +
3
SO42-
2RNR
2(OH-)
Cl +
3
SO42-
OH-
+ 2OH-
--
H2 O
H2 O
OH-
H2 O
Cathode
Anode
--
H2
Self Regenerating
Anion Suppressor
+
-
Conductivity (mS)
H+
Cation Exchange
Na+
Na+
Membrane
+
-
Cation Exchange
O2
OH-
Membrane
"R" = latex resin particle

Chromatogram
Cl-
SO42-
NO3-
F-
PO43-
CO32-
time
Computer/Integrator
ThS. Phan Bch H
20
Pump Mode
He Gas
Degas Mode
He Gas
To Pump
To Pump
Eluent
Eluent
ThS. Phan Bch H
21
Conductivity (mS)
Non-Suppressed IC
time
Conductivity (mS)
Suppressed IC
ThS. Phan Bch H
time
22
H thng sc k ion Metrohm IC850
ThS. Phan Bch H
23
H thng sc k ion Shimadzu
ThS. Phan Bch H
24
H thng sc k ion Dionex 3000
ThS. Phan Bch H
25
Sc k ion Dionex 3000 ti Vin
ThS. Phan Bch H
26
CC B PHN
ThS. Phan Bch H
27
CC B PHN
Bm SP : Single pump
EGC : Eluent genarator cartridges RFIC Reagent
Free Ion Chromatography
CT-RC : Continously Regenerated Trap Column
Injector : AS-AP
DC : Detector/Chromatography: Separation (Guard
column, column); detection(CD v ED); automation
ASRS : Anion Self-Regenerating Suppressor
H x l d liu
ThS. Phan Bch H
28
PHN LOAI SC K ION

Sc ky trao i ion. (Ion exchange)
Sc ky ghp cp ion. (Ion pair)
Khng s dng u d dn
Sc ky ui ion. (Ion exclusion)
ng dng cho acid hu c
ThS. Phan Bch H
29
Sc ky ghp cp ion
S dng ct sc ky lng pha o vi u do

thng
ThS. Phan Bch H
30
Sc ky loi ion
Phn tich acid va baz yu
R-COOH RCOO- + H+
S lu gi phu thuc
Kich c ca R.
Tng tac ca R vi cht nn pha tinh.
pKa
R tng tac vi eluent va cht nn pha tinh
ThS. Phan Bch H
31
Size exclusion chromatography
Phn
bit
ThS. Phan Bch H
32
Ion exclusion chromatography
Pha tnh trao i cation c cc nhm SO3H. Pha ng c

nc lm pha tnh b hidrat ha. Lp nc hidrat ha to
mng c bit gi l mng Donnan, mang in tch m ch
cho qua cc phn t trung ha v mt in tch.
Cc acid hu c khng phn ly, c th c lu gi trn pha
tnh, khi phn ly s b loi ra v s ra gii theo pha ng
ThS. Phan Bch H
33
Sc ky trao i ion
ThS. Phan Bch H
34
C ch trao i ion
The cation
exchange
mechanism
The anion
exchange
mechanism
ThS. Phan Bch H
35
CC AI LNG TRONG SC K ION

Tng t nh trong HPLC
Ba i lng lin quan n phn gii R :
H s lu gi : khng nn ln qua.
S a ly thuyt N : tng i ln.
chn lc : khng b nh hng nhiu bi cac
thng s pha ng ma chu nh hng do pha
tinh.
ThS. Phan Bch H
36
Retention time Thi gian lu
Dng nh tnh
ThS. Phan Bch H
37
ThS. Phan Bch H
38
Retention time Ion phn tch

Charge = valency in tch ion
Size - Kch thc
Polarizability kh nng phn cc ca ion
ThS. Phan Bch H
39
in tch ion
ThS. Phan Bch H
40
in tch ion
ThS. Phan Bch H
41
Kch thc
ThS. Phan Bch H
42
Kch thc
ThS. Phan Bch H
43
Kch thc
ThS. Phan Bch H
44
Kh nng phn cc ca ion
ThS. Phan Bch H
45
ThS. Phan Bch H
46
ThS. Phan Bch H
47
Retention time
Nng pha ng
Nhit ct
pH ca pha ng
ThS. Phan Bch H
48
ThS. Phan Bch H
49
ThS. Phan Bch H
50
ThS. Phan Bch H
51
QU TRNH PHN TCH MU BNG IC
ThS. Phan Bch H
52
ThS. Phan Bch H
53
ThS. Phan Bch H
54
Ion chromatography system configuration
ThS. Phan Bch H
55
Dionex - Ion Chromatography Product Line
ThS. Phan Bch H
56
RFIC (Reagent free Ion

chromatography) system - DIONEX
ThS. Phan Bch H
57
Bm (Pump)
Bn hn
P(IC) < P(HPLC)
SP Single Pump
ThS. Phan Bch H
PEEK (Polyether ether ketone)
DP Dual Pump
58
B TO PHA RA GII EGC

S dng
in
phn
to pha
ng
nng
chnh
xc
ThS. Phan Bch H
59
B TO PHA RA GII
EGC (phn tch Anion)
ThS. Phan Bch H
60
B TO PHA RA GII
EGC (phn tch Cation)
ThS. Phan Bch H
61
B TO PHA RA GII
EGC (phn tch Anion)
ThS. Phan Bch H
62
ThS. Phan Bch H
63
EPM (Electrolytic pH Modifier)
ThS. Phan Bch H
64
CR-TC
Continously Regenerated Trap Column
ThS. Phan Bch H
65
CR-ATC
ThS. Phan Bch H
66
CR-CTC
ThS. Phan Bch H
67

ThS. Phan Bch H
68
Injector
ThS. Phan Bch H
69
Injector
ThS. Phan Bch H
70
AUTOSAMPLER
ThS. Phan Bch H
71

ThS. Phan Bch H
72
DC MODULE
ThS. Phan Bch H
73
SEPARATION
ThS. Phan Bch H
74
Column Material
Composition of the stationary phase
Substrate:
substrate / resin carrier
Polystyrene / divinylbenzene
spacer group
Polymethacrylate
functional group
Polyvinylalcohol
Silica gel
Hydroxyethylmethacrylate (HEMA)
Spacer
Alkyl chain
ThS. Phan Bch H
Cation exchanger
Anion exchanger
sulfonates
carboxylates
quaternary
ammonium groups
alkyl amines
hydroxy-alkylamines
75
The stationary phase
ThS. Phan Bch H
76
Column Material
ion exchangers for IC
silica gels
polymer coated
polymer resins
surface
functionalized
microporous
polymer coated
Metrosep C 4
Metrosep C 2
layer
DIONEX
ThS. Phan Bch H
latex
particles
A Supp 10
A Supp 15 &16
macroporous
surface functionalized
PS/DVB
PVA
MA
A Supp 4
A Supp 5
77
Cu trc nha latex
ThS. Phan Bch H
78
OH-
Latex
Bead
OSO3-
+H N
3
NH3+
NH3+
OH-
SO42-
Cl-
OH-
ThS. Phan Bch H
79
DETECTOR
ThS. Phan Bch H
80
DETECTOR
ThS. Phan Bch H
81
SRS 300 Self-Regenerating Suppressor
ThS. Phan Bch H
82
SRS 300 Self-Regenerating Suppressor
ThS. Phan Bch H
83
Cc loi khc
ThS. Phan Bch H
84
ThS. Phan Bch H
85
ThS. Phan Bch H
86
The assembly of key SRS components
ThS. Phan Bch H
87
The electrolytic suppression processes in the ASRS
ThS. Phan Bch H
88
Self Regenerating Anion Suppressor
H2O
Na+
H2 CO3
O2
OH-
Cathode
Cation Exchange
+
-
Anode
Membrane
O2
HCO3 Na+
Cation Exchange
Membrane
From Separator Column
+
-
H2O
ThS. Phan Bch H
89
~ pH 10
Na+
OH-
+
H+
Membrane
Membrane
Na+
Cation Exchange
H2
NO3Cation Exchange
O2
+
OH-
H+
H2O
H2O
H2O
Cathode
Anode
NO3-
~ pH 3
ThS. Phan Bch H
90
ThS. Phan Bch H
91
ThS. Phan Bch H
92
ThS. Phan Bch H
93
ThS. Phan Bch H
94
TI LIU THAM KHO

1. Nguyn Kim Phi Phng (2007), Phng php
c lp hp cht hu c, Nh xut bn i hc
Quc gia TP. H Ch Minh, TP. H Ch Minh
2. Tng hp cc ti liu ca Dionex
ThS. Phan Bch H
95
NG DNG TRN MY IC
Trnh by: Cn. Nguyn Th H Linh
Phn tch trn mu nc
Phn tch cc anion
Column: ionpac As22 ( 4x250mm),

ionpac AG22 ( 4x250mm);
Eluent: 4.5mmol/L Na2CO3; 1.4mmol/L
NaHCO3
Flow rate: 1.2 mL/min
Injection volume: 2.5L
SRS suppressor: ASRS 300(2mm)
Background: 20-23L
Phn tch cc anion
><
Column: ionpac As22 ( 4x250mm),

ionpac AG22 ( 4x250mm);
Eluent: 4.5mmol/L Na2CO3; 1.4mmol/L
NaHCO3
Injection volume: 10L
SRS suppressor: asrs 300(4mm)
Background: 20-23L
Phn tch cc anion
Column: AS23, AG23

Eluent: 4.5mmol/L Na2CO3; 1.0mmol/L NaHCO3
Detection: suppressed conductivity with CRD-300
Scrubber: 0.5 mol/L KOH
Background: < 1.0L
Peak
ppb
Fluoride 10
Chlorite
10
Bromate 5
Chloride 100
Chlorate
10
Bromide
500
Nitrate
500
Sulfate
100
Phn tch cc anion
Phn tch cation
Phn tch cation
Phn tch trn mu thc phm
Phn tch trn mu thc phm

Phn tch
Phng php trn IC
Anion v c
HPIC/ Suppressed Conductivitty, DC Amperometry, UV/Vis
Kim loi kim th
HPIC/ Suppressed Conductivity
Acid hu c
HPIC/ Suppressed Conductivity; HPICE/ Suppressed

Conductivity
Amine bo
HPIC/ Suppressed Conductivity/ Pulsed Amperometry
Carbohydrates
HPIC/ Pulsed Amperometry
Alcolhols/ aldehydes
HPICE/ Pulsed Amperometry
Amino acids
HPIC/ Pulsed Amperometry
Phn tch NO2-, NO3- trong tht
Phn tch iodide trong sa bt
Phn tch polyphosphates trong

phomai
Anion trong tr
Column: ionpac
AS19(0.4x250mm and
AG19(0.4x50mm)
Eluent: KOH(EG)
Flow rate: 10L/min
Inj.volume: 0.4L
Detection: suppressed
conductivity
Phn tch phosphate v citrate trong

nc ngt
Phn tch cht hu c trong nc
Phn tch ng
Phn tch ng monosaccharides

trong cph ha tan
NG DNG TRN IC

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I CNG SC K ION

GII THIU H THNG IC DIONEX

ThS. Phan Bch H

Khoa Xt Nghim - Vin VSYTCC TP.HCM

ThS. Phan Bch H

Khoa Xt Nghim - Vin VSYTCC TP.HCM

Khoa Xt Nghim - Vin VSYTCC TP.HCM

ThS. Phan Bch H

Khoa Xt Nghim - Vin VSYTCC TP.HCM

ThS. Phan Bch H

Khoa Xt Nghim - Vin VSYTCC TP.HCM

Phan loi sc k theo bn cht ca 2 pha s

ThS. Phan Bch H

Phn loi sc k theo cu hnh

ThS. Phan Bch H

Chiu di chuyn ca pha ng

i ln, i xung, t tm lan to trn

i ln, i xung, t tm lan to trn

Khoa Xt Nghim - Vin VSYTCC TP.HCM

ThS. Phan Bch H

Khoa Xt Nghim - Vin VSYTCC TP.HCM

ThS. Phan Bch H

Khoa Xt Nghim - Vin VSYTCC TP.HCM

ThS. Phan Bch H

Khoa Xt Nghim - Vin VSYTCC TP.HCM

Khoa Xt Nghim - Vin VSYTCC TP.HCM

Khoa Xt Nghim - Vin VSYTCC TP.HCM

ThS. Phan Bch H

Khoa Xt Nghim - Vin VSYTCC TP.HCM

ThS. Phan Bch H

Khoa Xt Nghim - Vin VSYTCC TP.HCM

ThS. Phan Bch H

Khoa Xt Nghim - Vin VSYTCC TP.HCM

Thnh phn c bn ca sc k ion

ThS. Phan Bch H

Khoa Xt Nghim - Vin VSYTCC TP.HCM

ThS. Phan Bch H

Khoa Xt Nghim - Vin VSYTCC TP.HCM

500 - 5,000 psi

ThS. Phan Bch H

Khoa Xt Nghim - Vin VSYTCC TP.HCM

"R" = latex resin particle

500 - 5,000 psi

"R" = latex resin particle

ThS. Phan Bch H

Khoa Xt Nghim - Vin VSYTCC TP.HCM

ThS. Phan Bch H

Khoa Xt Nghim - Vin VSYTCC TP.HCM

ThS. Phan Bch H

Khoa Xt Nghim - Vin VSYTCC TP.HCM

H thng sc k ion Metrohm IC850

ThS. Phan Bch H

Khoa Xt Nghim - Vin VSYTCC TP.HCM

H thng sc k ion Shimadzu

ThS. Phan Bch H

Khoa Xt Nghim - Vin VSYTCC TP.HCM

H thng sc k ion Dionex 3000

ThS. Phan Bch H

Khoa Xt Nghim - Vin VSYTCC TP.HCM

Sc k ion Dionex 3000 ti Vin

ThS. Phan Bch H

Khoa Xt Nghim - Vin VSYTCC TP.HCM

ThS. Phan Bch H