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inline sample preparation.ppt
1. ic_sampl_prep_26062003_e.ppt 1
IC IC
IC IC
IC
Metrohm inline sample preparation
Techniques for analytical success
Metrohm Ion Chromatography
Bart Cleeren, Metrohm België
2. ic_sampl_prep_26062003_e.ppt 2
IC IC
IC IC
IC
Metrohm Ion Chromatography
Inline sample preparation
Ultra filtration
Stop flow dialysis
Pre concentration technique
Matrix elimination
Matrix neutralization
In- line calibration
3. ic_sampl_prep_26062003_e.ppt 3
IC IC
IC IC
IC
Metrohm Ion Chromatography
Inline sample preparation
Ultra filtration
Stop flow dialysis
Pre concentration technique
Matrix elimination
Matrix neutralization
In- line calibration
4. ic_sampl_prep_26062003_e.ppt 4
IC IC
IC IC
IC
Metrohm Ion Chromatography
Ultrafiltration
Inline sample preparation
Ultrafiltration cell
E Mobile phase: eluent
P1 High pressure pump
Injection valve «A»
C Analytical column
»MSM» Suppressor
D Conductivity detector
S Sample
P2 Peristaltic pump
A position fill
C
P1
E D
2
5. ic_sampl_prep_26062003_e.ppt 5
IC IC
IC IC
IC
Metrohm Ion Chromatography
Ultrafiltration Cell
Inline sample preparation
No particles on the acceptor side
Big particles are flushed away
and do not clog the membrane
High flow on the sample side
Low flow on the acceptor side
6. ic_sampl_prep_26062003_e.ppt 6
IC IC
IC IC
IC
Metrohm Ion Chromatography
Ultrafiltration
Inline sample preparation
# 1 Sample filtration
E Mobile phase: eluent
P1 High pressure pump
Injection valve «A»
C Analytical column
»MSM» Suppressor
D Conductivity detector
S Sample
P2 Peristaltic pump
A position fill
C
P1
E D
2
7. ic_sampl_prep_26062003_e.ppt 7
IC IC
IC IC
IC
Metrohm Ion Chromatography
Ultrafiltration
Inline sample preparation
# 2 Sample injection
E Mobile phase: eluent
P1 High pressure pump
Injection valve «A»
C Analytical column
»MSM» Suppressor
D Conductivity detector
S Sample
P2 Peristaltic pump
A position inject
C
P1
E D
2
8. ic_sampl_prep_26062003_e.ppt 8
IC IC
IC IC
IC
Metrohm Ion Chromatography
Ultrafiltration: vegetable juice
Inline sample preparation
A Supp 4 – 250
1 Organics n.q.
2 Organics n.q.
3 Cl– 4141
4 NO3
– 102
5 HPO4
2– 577
6 SO4
2– 842
7 Oxalate n.q.
ppt
NaHCO3/Na2CO3; 1.7/1.8 mmol/L;
dilution 1:100; 0.15 µm rec. cellul.
9. ic_sampl_prep_26062003_e.ppt 9
IC IC
IC IC
IC
Metrohm Ion Chromatography
Inline sample preparation
Ultra filtration
Stop flow dialysis
Pre concentration technique
Matrix elimination
Matrix neutralization
In- line calibration
10. ic_sampl_prep_26062003_e.ppt 10
IC IC
IC IC
IC
Metrohm Ion Chromatography
Inline sample preparation
Dialysis cell, acceptor solution
E Mobile phase: eluent
P1 High pressure pump
Injection valve «A»
C Analytical column
»MSM» Suppressor
D Conductivity detector
P2 Peristaltic pump
P3 Peristaltic pump (2 Ch.)
Dialysis cell
A Acceptor solution
Dialysis
C
P1
E D
2
A E
P1
P2
P3
A D
C
X
X
11. ic_sampl_prep_26062003_e.ppt 11
IC IC
IC IC
IC
Metrohm Ion Chromatography
Inline sample preparation
# 2 Stopped flow dialysis
E Mobile phase: eluent
P1 High pressure pump
Injection valve «A»
C Analytical column
»MSM» Suppressor
D Conductivity detector
P2 Peristaltic pump
Injection Valve «B»
Dialysis cell
A Acceptor solution
Dialysis
C
P1
E D
2
A
P3
P2
A
P1
C
D
E
12. ic_sampl_prep_26062003_e.ppt 12
IC IC
IC IC
IC
Metrohm Ion Chromatography
Dialysis cell
Inline sample preparation
Continuous flow dialysis
Exclusion diameter 0.2 µm
Ions can pass
Oil droplets, fat micelles, particles
are excluded
Strong concentration gradient
No equilibrium concentration
Cellulose acetate membrane
13. ic_sampl_prep_26062003_e.ppt 13
IC IC
IC IC
IC
Metrohm Ion Chromatography
Dialysis cell
Inline sample preparation
Stopped flow dialysis
Dialysis time 2 ... 8 min
Sample volume 10 mL
No loss of concentration on the
sample side
Equilibrium concentration
Dialysis rate > 99 %
No filtration, no pre concentration
Unique technique, that had
significantly improves the field of
application for IC
14. ic_sampl_prep_26062003_e.ppt 14
IC IC
IC IC
IC
Metrohm Ion Chromatography
Dialysis: milk
Inline sample preparation
Metrosep Dual 1 – 70
1 Chloride 938
2 Nitrate n.q.
3 Phosphate n.q
4 Sufate 103
ppm
NaHCO3/Na2CO3; 2.4/2.0 mmol/L;
dilution 1:5; 0.2 µm cellul. acetat
15. ic_sampl_prep_26062003_e.ppt 15
IC IC
IC IC
IC
Metrohm Ion Chromatography
Dialysis: cutting oil emulsion
Inline sample preparation
Metrosep Dual 2
1 Chloride 74.7
2 Nitrite 20.5.
3 Nitrate 23.9
4 n. det. -
5 Phosphate 25.2
6 Sulfate 192.7
7 n. det. -
NaHCO3/Na2CO3; 2.0/1.3 mmol/L;
dilution 1:5; 0.2 µm cellul. acetat
16. ic_sampl_prep_26062003_e.ppt 16
IC IC
IC IC
IC
Metrohm Ion Chromatography
Inline sample preparation
Ultra filtration
Stop flow dialysis
Pre concentration technique
Matrix elimination
Matrix neutralization
In- line calibration
17. ic_sampl_prep_26062003_e.ppt 17
IC IC
IC IC
IC
Metrohm Ion Chromatography
Inline sample preparation
# 1 Sample preconcentration
E Mobile phase: eluent
P1 High pressure pump
Injection valve «A»
C Analytical column
»MSM» Suppressor
D Conductivity detector
P2 Peristaltic pump
C
P1
D
P3 2
S
Inline pre concentration
E
C
P1
P 2
D
18. ic_sampl_prep_26062003_e.ppt 18
IC IC
IC IC
IC
Metrohm Ion Chromatography
Inline sample preparation
# 2 Sample analysis
E Mobile phase: eluent
P 1 High pressure pump
Injection valve «A»
C Analytical column
»MSM» Suppressor
D Conductivity detector
P 2 Peristaltic pump
C
P1
E D
P3 2
S
Inline preconcentration
E
C
D
P1
P 2
19. ic_sampl_prep_26062003_e.ppt 19
IC IC
IC IC
IC
Metrohm Ion Chromatography
Inline preconcentration: ultra pure water
Inline sample preparation
Metrosep A Supp 5 – 150
1 Acetate 2.3
2 Formate 22.0
3 Chloride 13.0
4 Carbonate n.q.
5 Nitrate 4.5
6 Phosphate 16.0
7 Sulfate 8.5
8 Oxalate 12.0
ppt
NaHCO3/Na2CO3; 1.0/3.2 mmol/L;
20 mL preconc,
20. ic_sampl_prep_26062003_e.ppt 20
IC IC
IC IC
IC
Metrohm Ion Chromatography
Inline preconcentration: ultra pure water
Inline sample preparation
Metrosep Dual 2
1 Fluoride 45 – 150
2 Chloride 100 – 210
3 Bromide 0 – 100
4 Nitrate 10 – 112
5 Sulfate 40 – 145
ppt
NaHCO3/Na2CO3; 2.0/3.2 mmol/L;
10 mL preconc, spiked 100 ppt
21. ic_sampl_prep_26062003_e.ppt 21
IC IC
IC IC
IC
Metrohm Ion Chromatography
Inline sample preparation
Ultra filtration
Stop flow dialysis
Pre concentration technique
Matrix elimination
Matrix neutralization
In- line calibration
22. ic_sampl_prep_26062003_e.ppt 22
IC IC
IC IC
IC
P3
Metrohm Ion Chromatography
Inline sample preparation
Transfer solution «T»
E Mobile phase: eluent
P1 High pressure pump
Injection valve «A»
C Analytical column
»MSM» Suppressor
D Conductivity detector
P2 Peristaltic pump
Injection Valve «B»
P3 Peristaltic pump
T Transfer solution
A position fill, B position fill
C
P1
E D
2
T
Matrix elimination
23. ic_sampl_prep_26062003_e.ppt 23
IC IC
IC IC
IC
P3
Metrohm Ion Chromatography
Inline sample preparation
# 1 Preconcentrator column inline
E Mobile phase: eluent
P1 High pressure pump
Injection valve «A»
C Analytical column
»MSM» Suppressor
D Conductivity detector
P2 Peristaltic pump
Injection Valve «B»
P3 Peristaltic pump
T Transfer solution
A position fill, B position fill
C
P1
E D
2
T
Matrix elimination
24. ic_sampl_prep_26062003_e.ppt 24
IC IC
IC IC
IC
P3
Metrohm Ion Chromatography
Inline sample preparation
# 2 Sample transfer, matrix elim.
E Mobile phase: eluent
P1 High pressure pump
Injection valve «A»
C Analytical column
»MSM» Suppressor
D Conductivity detector
P2 Peristaltic pump
Injection Valve «B»
P3 Peristaltic pump
T Transfer solution
A position fill, B position inject
C
P1
E D
2
T
Matrix elimination
25. ic_sampl_prep_26062003_e.ppt 25
IC IC
IC IC
IC
P3
Metrohm Ion Chromatography
Inline sample preparation
# 3 Sample inject
E Mobile phase: eluent
P1 High pressure pump
Injection valve «A»
C Analytical column
»MSM» Suppressor
D Conductivity detector
P2 Peristaltic pump
Injection Valve «B»
P3 Peristaltic pump
T Transfer solution
A position inject, B position inject
C
P1
E D
2
T
Matrix elimination
26. ic_sampl_prep_26062003_e.ppt 26
IC IC
IC IC
IC
Metrohm Ion Chromatography
Matrix elimination: organic solvents
Inline sample preparation
50 µL iPrOH
B with matrix elimination
A without matrix elimination
ppt
F–
Ac–
443 Cl–
30 NO3
– 28 SO4
2–
425 Cl–
24 NO3
– 17 SO4
2–
27. ic_sampl_prep_26062003_e.ppt 27
IC IC
IC IC
IC
Metrohm Ion Chromatography
Matrix elimination: 35 % H2O2
Inline sample preparation
left:
without m.e.
Loop 20 µL
right:
with m.e.
Loop 20 µL
transfer vol . 2 mL
28. ic_sampl_prep_26062003_e.ppt 28
IC IC
IC IC
IC
Metrohm Ion Chromatography
Inline sample preparation
Ultra filtration
Stop flow dialysis
Pre concentration technique
Matrix elimination
Matrix neutralization
In- line calibration
29. ic_sampl_prep_26062003_e.ppt 29
IC IC
IC IC
IC
P3
Metrohm Ion Chromatography
Inline sample preparation
833.0030 IC Sample Prep. Unit
E Mobile phase: eluent
P1 High pressure pump
Injection valve «A»
C Analytical column
»MSM» Suppressor
D Conductivity detector
P2, 3 Peristaltic pumps
Injection Valve «B»
T Transfer solution
833 IC Sample Prep
A position inject, B position fill
C
P1
E D
2
T
Matrix neutralization
30. ic_sampl_prep_26062003_e.ppt 30
IC IC
IC IC
IC
P3
Metrohm Ion Chromatography
Inline sample preparation
# 1 Preconcentrator column inline
E Mobile phase: eluent
P1 High pressure pump
Injection valve «A»
C Analytical column
»MSM» Suppressor
D Conductivity detector
P2, 3 Peristaltic pumps
Injection Valve «B»
T Transfer solution
833 IC Sample Prep
A position fill, B position fill
C
P1
E D
2
T
Matrix neutralization
31. ic_sampl_prep_26062003_e.ppt 31
IC IC
IC IC
IC
P3
Metrohm Ion Chromatography
Inline sample preparation
# 2 Sample transfer/neutralization
E Mobile phase: eluent
P1 High pressure pump
Injection valve «A»
C Analytical column
»MSM» Suppressor
D Conductivity detector
P2, 3 Peristaltic pumps
Injection Valve «B»
T Transfer solution
833 IC Sample Prep
A position fill, B position inject
C
P1
E D
2
T
Matrix neutralization
32. ic_sampl_prep_26062003_e.ppt 32
IC IC
IC IC
IC
P3
Metrohm Ion Chromatography
Inline sample preparation
# 4 Sample inject
E Mobile phase: eluent
P1 High pressure pump
Injection valve «A»
C Analytical column
»MSM» Suppressor
D Conductivity detector
P2, 3 Peristaltic pumps
Injection Valve «B»
T Transfer solution
833 IC Sample Prep
A position inject, B position inject
C
P1
E D
2
T
Matrix neutralization
33. ic_sampl_prep_26062003_e.ppt 33
IC IC
IC IC
IC
0.74 F–
3.6 Cl–
0.97 NO3
–
0.98 HPO4
2–
1.1 SO4
2–
Metrohm Ion Chromatography
Matrix neutralization: caustic soda
Inline sample preparation
30 % NaOH, 20 µL loop
B with matrix elimination
A without matrix elimination
ppm
34. ic_sampl_prep_26062003_e.ppt 34
IC IC
IC IC
IC
Metrohm Ion Chromatography
Matrix neutralization: caustic soda
Inline sample preparation
Metrosep Dual 2
1 Chloride 25.08
2 Carbonate n.q.
3 Chlorate 4.76
4 Sulfate 10.43
ppm
NaHCO3/Na2CO3; 1.7/1.8 mmol/L;
50 % NaOH, 20 µL loop
35. ic_sampl_prep_26062003_e.ppt 35
IC IC
IC IC
IC
1
Metrohm Ion Chromatography
Matrix neutralization: ammonia
Inline sample preparation
Metrosep A Supp 4 – 250
1 Formate n.q.
2 Chloride 0.03
3 Nitrite n.q.
4 Bromide 0.95
5 Nitrat 0.04
6 Carbonate n.q.
7 Sulfate 0.13
ppm
NaHCO3/Na2CO3; 1.7/1.8 mmol/L;
26 % NH3, 20 µL loop
2
3
4
5 6
7
36. ic_sampl_prep_26062003_e.ppt 36
IC IC
IC IC
IC
P3
Metrohm Ion Chromatography
Inline sample preparation
OH cartridge
E Mobile phase: eluent
P1 High pressure pump
Injection valve «A»
C Analytical column
»MSM» Suppressor
D Conductivity detector
P2, 3 Peristaltic pumps
Injection Valve «B»
T Transfer solution
Cartridge
A position fill, B position fill
C
P1
E D
2
T
Matrix neutralization
Ctr
37. ic_sampl_prep_26062003_e.ppt 37
IC IC
IC IC
IC
Metrohm Ion Chromatography
Matrix neutralization: HCl
Inline sample preparation
10 µL
HCl direct injection
ppm
Metrosep C2 – 250
38. ic_sampl_prep_26062003_e.ppt 38
IC IC
IC IC
IC
Metrohm Ion Chromatography
Matrix neutralization: HCl
Inline sample preparation
Metrosep C2 – 250
1 Nickel n.q.
2 Sodium 5.4
3 Ammonium 1.3
4 Potassium 0.8
5 Magnesium 1.5
6 Calcium 0.8
ppm
Tartaric-/dipicolinic acid; 4.0/0.75
mmol/L; 7 mol HCl, 10 µL loop
1
2
3
4 5 6
39. ic_sampl_prep_26062003_e.ppt 39
IC IC
IC IC
IC
Metrohm Ion Chromatography
Inline sample preparation
Ultra filtration
Stop flow dialysis
Pre concentration technique
Matrix elimination
Matrix neutralization
In- line calibration
40. ic_sampl_prep_26062003_e.ppt 40
IC IC
IC IC
IC
Metrohm Ion Chromatography
Inline sample preparation
Standard S, flow path
E Mobile phase: eluent
P1 High pressure pump
Injection valve «A»
C Analytical column
»MSM» Suppressor
D Conductivity detector
P1,2,3 Peristaltic pumps
Injection Valve «B»
S Standard
A position inject, B position fill
Inline calibration
C
P1
E D
P3 2
S
41. ic_sampl_prep_26062003_e.ppt 41
IC IC
IC IC
IC
Metrohm Ion Chromatography
Inline sample preparation
# 1 Measurement of standard
E Mobile phase: eluent
P1 High pressure pump
Injection valve «A»
C Analytical column
»MSM» Suppressor
D Conductivity detector
P1,2,3 Peristaltic pumps
Injection Valve «B»
S Standard
A position inject, B position fill
C
P1
E D
P3 2
S
Inline calibration
42. ic_sampl_prep_26062003_e.ppt 42
IC IC
IC IC
IC
Metrohm Ion Chromatography
Inline sample preparation
# 2 Preconcentrator inline
E Mobile phase: eluent
P1 High pressure pump
Injection valve «A»
C Analytical column
»MSM» Suppressor
D Conductivity detector
P1,2,3 Peristaltic pumps
Injection Valve «B»
S Standard
A position fill, B position fill
C
P1
E D
P3 2
S
Inline calibration
43. ic_sampl_prep_26062003_e.ppt 43
IC IC
IC IC
IC
Metrohm Ion Chromatography
Inline sample preparation
# 3 Transfer of standard
E Mobile phase: eluent
P1 High pressure pump
Injection valve «A»
C Analytical column
»MSM» Suppressor
D Conductivity detector
P1,2,3 Peristaltic pumps
Injection Valve «B»
S Standard
A position fill, B position inject
C
P1
E D
P3 2
S
Inline calibration
44. ic_sampl_prep_26062003_e.ppt 44
IC IC
IC IC
IC
Metrohm Ion Chromatography
Inline sample preparation
# 4 Inject of standard
E Mobile phase: eluent
P1 High pressure pump
Injection valve «A»
C Analytical column
»MSM» Suppressor
D Conductivity detector
P1,2,3 Peristaltic pumps
Injection Valve «B»
S Standard
A position inject, B position inject
C
P1
E D
P3 2
S
Inline calibration
45. ic_sampl_prep_26062003_e.ppt 45
IC IC
IC IC
IC
Metrohm Ion Chromatography
Inline sample preparation
# 1: Transfer of 2 mL ultrapure
water to the preconcentrator
Blank value
# 2: Transfer of 2 mL ultrapure
water to the preconcentrator.
Valve B is thrown from fill to inject
and back once
Calibration level 1
# 3: Transfer of 2 mL ultrapure
water to the preconcentrator.
Valve B is thrown from fill to inject
and back twice
Calibration level 2
# 4: Transfer of 2 mL ultrapure
water to the preconcentrator.
Valve B is thrown from fill to inject
and back three times
Calibration level 3, etc
Inline calibration
