Sac Ky Ion

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 Khoa Xt Nghim - Vin VSYTCC TP.HCM 4
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 Tn gi ca k thut sc k
Sc k lng - rn
ng dng
Cht rn Cht lng
Cht lng Cht rn
Sc k ct, sc k lp mng, sc k lng cao p Sc k lng - lng Sc k lng cao p Sc k kh - rn Sc k kh - lng

Cht kh
Cht lng
Sc k kh
ThS. Phan Bch H
Phn loi sc k theo cu hnh

Hnh hc Cu hnh sc k Giy Phng Chiu di chuyn ca pha ng i ln, i xung, t tm lan to trn
Lp mng
i ln, i xung, t tm lan to trn
Ct h
i xung
Ct
Sc k kh
Nh vo ngoi lc
Sc k lng cao p
Nh vo ngoi lc
ThS. Phan Bch H
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
So sanh vi HPLC
HPLC IC - CD
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
Phn t trung hoa Hn hp dung mi Nho hn

Nho hn Nho hn
Ion (chu yu anion) Dung dch Ion Ln hn

Ln 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
Eluant 0.0028M NaHCO 0.0022M Na CO 2 ~2 ml/min flow
3 3
Sample Loop 50 ul Sample Inject Valve Sample in Syringe or from Autosampler Waste Guard Column
Pump
500 - 5,000 psi 1,000 nominal Check for air bubbles
3PO 4 = SO 4 NO 3
Separator Column
RNR + 3
2RNR
+ 3
HCO
+ +
Cl = SO 4
RNR + 3
2RNR
+ 3
Cl = SO 4
+ +
HCO 3
Cl -
CO = 3
CO = 3
"R" = latex resin particle Chromatogram NO 3 - Cl F

Conductivity (uS)
Cation Exchange
Membrane
O2
HCO 3 Na + Na +
H2 OH -
H+ +
Anode
Cation Exchange
+ -
Self Regenerating Anion Suppressor + -
= SO 4
3PO 4
Membrane
Cathode
water dip
H2 O
H 2CO
H2 O
time Computer/Integrator
Conductivity Detector
ThS. Phan Bch H
19
Ion Chromatography
OH - Eluent
Degas Eluant DI Water Degas Eluant 40 mM NaOH
Sample Loop 100 ml Sample Inject Valve Sample in Syringe or from Autosampler Waste Guard Column
Quaternary Pump
500 - 5,000 psi 1,650 psi nominal
PO43SO42NO3Cl-
Separator Column
RNR + 3
2RNR
+ 3
OH2(OH-)
+ +
Cl SO42-
RNR + 3
2RNR
+ 3
Cl SO42-
OH+ 2OH-
"R" = latex resin particle Conductivity (mS) Chromatogram

ClFCO32NO3SO42PO43Cation Exchange
O2
OH-
Na+ Na+
Membrane
H2 OH-
H+ +
Anode
Cation Exchange
+ -
Self Regenerating Anion Suppressor + -
Membrane
Cathode
H2 O
H2 O
H2 O
time Computer/Integrator
ThS. Phan Bch H
20
Pump Mode
Degas Mode
He Gas
He Gas
To Pump
To Pump
Eluent Eluent
ThS. Phan Bch H
21
Non-Suppressed IC
Conductivity (mS)
time
Suppressed IC
Conductivity (mS)
time
ThS. Phan Bch H
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
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
Sc ky trao i ion
ThS. Phan Bch H
34
C ch trao i ion
The cation exchange mechanism
The anion exchange mechanism

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 PEEK (Polyether ether ketone)
DP Dual Pump
ThS. Phan Bch H
58
B TO PHA RA GII EGC

S dng in phn to pha ng nng chnh xc
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: Polystyrene / divinylbenzene Polymethacrylate Polyvinylalcohol Silica gel Hydroxyethylmethacrylate (HEMA) substrate / resin carrier spacer group
functional group
Spacer Alkyl chain Cation exchanger Anion exchanger
sulfonates
carboxylates
quaternary ammonium groups

alkyl amines hydroxy-alkylamines
75
ThS. Phan Bch H
The stationary phase
ThS. Phan Bch H
76
Column Material
ion exchangers for IC silica gels polymer resins
polymer coated
surface functionalized
microporous
macroporous
Metrosep C 4 Metrosep C 2
polymer coated
surface functionalized
layer
latex particles
PS/DVB
PVA
MA
DIONEX
A Supp 10 A Supp 15 &16
A Supp 4 A Supp 5
ThS. Phan Bch H
77
Cu trc nha latex
ThS. Phan Bch H
78
OH-
OH-
Latex Bead
OSO3-
+H N 3
NH3+ NH3+
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

From Separator Column
Membrane
Membrane
HCO3 Na+ Na+
O2 +
O2
Cation Exchange
Cation Exchange
+ H2O
H2 CO3
H2O
Cathode
+ -
Anode
OH-
+ -
ThS. Phan Bch H
89
~ pH 10
OHO2 NO3Cation Exchange
Na+ H2
Membrane
Na+
H+
Cation Exchange
+
OH-
Membrane
+
Anode
Cathode
H+ NO3H2O H2O H2O
~ pH 3 Conductivity Detector
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 Khoa Xt Nghim - Vin VSYTCC TP.HCM
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 Flow rate: 1.2 mL/min 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 Flow rate: 1.0 mL/min 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 Anion v c Kim loi kim th Acid hu c Amine bo Carbohydrates Alcolhols/ aldehydes Amino acids Phng php trn IC HPIC/ Suppressed Conductivitty, DC Amperometry, UV/Vis HPIC/ Suppressed Conductivity HPIC/ Suppressed Conductivity; HPICE/ Suppressed Conductivity HPIC/ Suppressed Conductivity/ Pulsed Amperometry HPIC/ Pulsed Amperometry HPICE/ Pulsed Amperometry 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

Sac Ky Ion

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I CNG SC K ION

GII THIU H THNG IC DIONEX NG DNG TRN MY IC

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.

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

Phan loi sc k theo bn cht ca 2 pha s dng

Cht rn Cht lng

Cht lng Cht rn

Sc k ct, sc k lp mng, sc k lng cao p Sc k lng - lng Sc k lng cao p Sc k kh - rn Sc k kh - lng

ThS. Phan Bch H

Phn loi sc k theo cu hnh

i ln, i xung, t tm lan to trn

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

ThS. Phan Bch H

Khoa Xt Nghim - Vin VSYTCC TP.HCM

i tng Pha ng Th tich cht ngoai ct

Phn t trung hoa Hn hp dung mi Nho hn

Ion (chu yu anion) Dung dch Ion Ln hn

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 1,000 nominal Check for air bubbles

"R" = latex resin particle Chromatogram NO 3 - Cl F

Self Regenerating Anion Suppressor + -

ThS. Phan Bch H

Khoa Xt Nghim - Vin VSYTCC TP.HCM

500 - 5,000 psi 1,650 psi nominal

"R" = latex resin particle Conductivity (mS) Chromatogram

Self Regenerating Anion Suppressor + -

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