Metrohm Ion Chromatography IC ICIC Metrohm inline sample
- Slides: 47
Metrohm Ion Chromatography IC ICIC Metrohm inline sample preparation Techniques for analytical success Bart Cleeren, Metrohm België ic_sampl_prep_26062003_e. ppt 1
Metrohm Ion Chromatography Inline sample preparation Ultra filtration Stop flow dialysis Pre concentration technique Matrix elimination Matrix neutralization In- line calibration ic_sampl_prep_26062003_e. ppt 2 IC ICIC
Metrohm Ion Chromatography Inline sample preparation Ultra filtration Stop flow dialysis Pre concentration technique Matrix elimination Matrix neutralization In- line calibration ic_sampl_prep_26062003_e. ppt 3 IC ICIC
Metrohm Ion Chromatography IC ICIC Inline sample preparation Ultrafiltration cell E Mobile phase: eluent P 1 High pressure pump Injection valve «A» C C Analytical column » MSM» Suppressor D Conductivity detector S Sample P 2 Peristaltic pump P 1 2 E A position fill ic_sampl_prep_26062003_e. ppt 4 D
Metrohm Ion Chromatography Inline sample preparation Ultrafiltration Cell 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 ic_sampl_prep_26062003_e. ppt 5 IC ICIC
Metrohm Ion Chromatography IC ICIC Inline sample preparation Ultrafiltration # 1 Sample filtration E Mobile phase: eluent P 1 High pressure pump Injection valve «A» C C Analytical column » MSM» Suppressor D Conductivity detector S Sample P 2 Peristaltic pump P 1 2 E A position fill ic_sampl_prep_26062003_e. ppt 6 D
Metrohm Ion Chromatography IC ICIC Inline sample preparation Ultrafiltration # 2 Sample injection E Mobile phase: eluent P 1 High pressure pump Injection valve «A» C C Analytical column » MSM» Suppressor D Conductivity detector S Sample P 2 Peristaltic pump P 1 2 E A position inject ic_sampl_prep_26062003_e. ppt 7 D
Metrohm Ion Chromatography Inline sample preparation Ultrafiltration: vegetable juice A Supp 4 – 250 1 Organics n. q. 2 Organics n. q. 3 Cl– 4 NO 3– 102 5 HPO 42– 577 6 SO 42– 842 7 Oxalate n. q. 4141 ppt Na. HCO 3/Na 2 CO 3; 1. 7/1. 8 mmol/L; dilution 1: 100; 0. 15 µm rec. cellul. ic_sampl_prep_26062003_e. ppt 8 IC ICIC
Metrohm Ion Chromatography Inline sample preparation Ultra filtration Stop flow dialysis Pre concentration technique Matrix elimination Matrix neutralization In- line calibration ic_sampl_prep_26062003_e. ppt 9 IC ICIC
Metrohm Ion Chromatography IC ICIC Inline sample preparation Dialysis cell, acceptor solution E Mobile phase: eluent P 1 High pressure pump X Injection valve «A» C P 3 C X Analytical column » MSM» Suppressor D Conductivity detector P 2 Peristaltic pump P 3 Peristaltic pump (2 Ch. ) P 1 P 1 2 P 2 A Dialysis cell A Acceptor solution ic_sampl_prep_26062003_e. ppt C 10 A E E D D
Metrohm Ion Chromatography IC ICIC Inline sample preparation Dialysis # 2 Stopped flow dialysis E Mobile phase: eluent P 1 High pressure pump P 3 Injection valve «A» Analytical column » MSM» Suppressor D Conductivity detector P 2 Peristaltic pump Injection Valve «B» A Acceptor solution ic_sampl_prep_26062003_e. ppt C P 1 P 1 2 P 2 Dialysis cell A C X C 11 A E E DD
Metrohm Ion Chromatography Inline sample preparation Dialysis cell 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 ic_sampl_prep_26062003_e. ppt 12 IC ICIC
Metrohm Ion Chromatography Inline sample preparation Dialysis cell Stopped flow dialysis Dialysis time 2. . . 8 min Sample volume 10 m. L 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 ic_sampl_prep_26062003_e. ppt 13 IC ICIC
Metrohm Ion Chromatography Inline sample preparation Dialysis: milk Metrosep Dual 1 – 70 1 Chloride 938 2 Nitrate n. q. 3 Phosphate n. q 4 Sufate 103 ppm Na. HCO 3/Na 2 CO 3; 2. 4/2. 0 mmol/L; dilution 1: 5; 0. 2 µm cellul. acetat ic_sampl_prep_26062003_e. ppt 14 IC ICIC
Metrohm Ion Chromatography Inline sample preparation Dialysis: cutting oil emulsion Metrosep Dual 2 1 Chloride 74. 7 2 Nitrite 20. 5. 3 Nitrate 23. 9 4 n. det. - 5 Phosphate 6 Sulfate 7 n. det. 25. 2 192. 7 - Na. HCO 3/Na 2 CO 3; 2. 0/1. 3 mmol/L; dilution 1: 5; 0. 2 µm cellul. acetat ic_sampl_prep_26062003_e. ppt 15 IC ICIC
Metrohm Ion Chromatography Inline sample preparation Ultra filtration Stop flow dialysis Pre concentration technique Matrix elimination Matrix neutralization In- line calibration ic_sampl_prep_26062003_e. ppt 16 IC ICIC
Metrohm Ion Chromatography IC ICIC Inline sample preparation Inline pre concentration # 1 Sample preconcentration E Mobile phase: eluent P 1 High pressure pump Injection valve «A» C CC Analytical column » MSM» Suppressor D Conductivity detector P 2 Peristaltic pump P 3 P 22 S ic_sampl_prep_26062003_e. ppt P 1 E 17 D D
Metrohm Ion Chromatography IC ICIC Inline sample preparation Inline preconcentration # 2 Sample analysis E Mobile phase: eluent P 1 High pressure pump Injection valve «A» C CC Analytical column » MSM» Suppressor D Conductivity detector P 2 Peristaltic pump P 3 2 P 2 S ic_sampl_prep_26062003_e. ppt P 1 P 1 EE 18 DD
Metrohm Ion Chromatography Inline sample preparation Inline preconcentration: ultra pure water 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 7 Sulfate 8. 5 8 Oxalate 12. 0 16. 0 ppt Na. HCO 3/Na 2 CO 3; 1. 0/3. 2 mmol/L; 20 m. L preconc, ic_sampl_prep_26062003_e. ppt 19 IC ICIC
Metrohm Ion Chromatography Inline sample preparation Inline preconcentration: ultra pure water Metrosep Dual 2 1 Fluoride 45 – 150 2 Chloride 100 – 210 3 Bromide 0 – 100 4 Nitrate 10 – 112 5 Sulfate 40 – 145 ppt Na. HCO 3/Na 2 CO 3; 2. 0/3. 2 mmol/L; 10 m. L preconc, spiked 100 ppt ic_sampl_prep_26062003_e. ppt 20 IC ICIC
Metrohm Ion Chromatography Inline sample preparation Ultra filtration Stop flow dialysis Pre concentration technique Matrix elimination Matrix neutralization In- line calibration ic_sampl_prep_26062003_e. ppt 21 IC ICIC
Metrohm Ion Chromatography IC ICIC Inline sample preparation Matrix elimination Transfer solution «T» E Mobile phase: eluent P 1 High pressure pump Injection valve «A» C C Analytical column » MSM» Suppressor D Conductivity detector P 2 Peristaltic pump 2 Injection Valve «B» P 3 Peristaltic pump T Transfer solution A position fill, B position fill ic_sampl_prep_26062003_e. ppt 22 P 3 P 1 T E D
Metrohm Ion Chromatography IC ICIC Inline sample preparation Matrix elimination # 1 Preconcentrator column inline E Mobile phase: eluent P 1 High pressure pump Injection valve «A» C C Analytical column » MSM» Suppressor D Conductivity detector P 2 Peristaltic pump 2 Injection Valve «B» P 3 Peristaltic pump T Transfer solution A position fill, B position fill ic_sampl_prep_26062003_e. ppt 23 P 1 T E D
Metrohm Ion Chromatography IC ICIC Inline sample preparation Matrix elimination # 2 Sample transfer, matrix elim. E Mobile phase: eluent P 1 High pressure pump Injection valve «A» C C Analytical column » MSM» Suppressor D Conductivity detector P 2 Peristaltic pump 2 Injection Valve «B» P 3 Peristaltic pump T Transfer solution A position fill, B position inject ic_sampl_prep_26062003_e. ppt 24 P 3 P 1 T E D
Metrohm Ion Chromatography IC ICIC Inline sample preparation Matrix elimination # 3 Sample inject E Mobile phase: eluent P 1 High pressure pump Injection valve «A» C C Analytical column » MSM» Suppressor D Conductivity detector P 2 Peristaltic pump 2 Injection Valve «B» P 3 Peristaltic pump T Transfer solution A position inject, B position inject ic_sampl_prep_26062003_e. ppt 25 P 3 P 1 T E D
Metrohm Ion Chromatography IC ICIC Inline sample preparation Matrix elimination: organic solvents 50 µL i. Pr. OH B with matrix elimination A without matrix elimination 443 Cl– F–Ac– ppt ic_sampl_prep_26062003_e. ppt 425 Cl– 26 30 NO 3– 28 SO 42– 24 NO 3– 17 SO 42–
Metrohm Ion Chromatography Inline sample preparation Matrix elimination: 35 % H 2 O 2 left: without m. e. Loop 20 µL right: with m. e. Loop 20 µL transfer vol. 2 m. L ic_sampl_prep_26062003_e. ppt 27 IC ICIC
Metrohm Ion Chromatography Inline sample preparation Ultra filtration Stop flow dialysis Pre concentration technique Matrix elimination Matrix neutralization In- line calibration ic_sampl_prep_26062003_e. ppt 28 IC ICIC
Metrohm Ion Chromatography IC ICIC Inline sample preparation Matrix neutralization 833. 0030 IC Sample Prep. Unit E Mobile phase: eluent P 1 High pressure pump Injection valve «A» C C Analytical column » MSM» Suppressor D Conductivity detector P 2, 3 Peristaltic pumps 2 Injection Valve «B» T Transfer solution 833 IC Sample Prep A position inject, B position fill ic_sampl_prep_26062003_e. ppt 29 P 3 P 1 T E D
Metrohm Ion Chromatography IC ICIC Inline sample preparation Matrix neutralization # 1 Preconcentrator column inline E Mobile phase: eluent P 1 High pressure pump Injection valve «A» C C Analytical column » MSM» Suppressor D Conductivity detector P 2, 3 Peristaltic pumps 2 Injection Valve «B» T Transfer solution 833 IC Sample Prep A position fill, B position fill ic_sampl_prep_26062003_e. ppt 30 P 3 P 1 T E D
Metrohm Ion Chromatography IC ICIC Inline sample preparation Matrix neutralization # 2 Sample transfer/neutralization E Mobile phase: eluent P 1 High pressure pump Injection valve «A» C C Analytical column » MSM» Suppressor D Conductivity detector P 2, 3 Peristaltic pumps 2 Injection Valve «B» T Transfer solution 833 IC Sample Prep A position fill, B position inject ic_sampl_prep_26062003_e. ppt 31 P 3 P 1 T E D
Metrohm Ion Chromatography IC ICIC Inline sample preparation Matrix neutralization # 4 Sample inject E Mobile phase: eluent P 1 High pressure pump Injection valve «A» C C Analytical column » MSM» Suppressor D Conductivity detector P 2, 3 Peristaltic pumps 2 Injection Valve «B» T Transfer solution 833 IC Sample Prep A position inject, B position inject ic_sampl_prep_26062003_e. ppt 32 P 3 P 1 T E D
Metrohm Ion Chromatography IC ICIC Inline sample preparation Matrix neutralization: caustic soda 30 % Na. OH, 20 µL loop B with matrix elimination A without matrix elimination 3. 6 Cl– 0. 74 F– ppm ic_sampl_prep_26062003_e. ppt 33 0. 97 NO 3– 0. 98 HPO 42– 1. 1 SO 42–
Metrohm Ion Chromatography Inline sample preparation Matrix neutralization: caustic soda Metrosep Dual 2 1 Chloride 2 Carbonate 3 Chlorate 4 Sulfate 25. 08 n. q. 4. 76 10. 43 ppm Na. HCO 3/Na 2 CO 3; 1. 7/1. 8 mmol/L; 50 % Na. OH, 20 µL loop ic_sampl_prep_26062003_e. ppt 34 IC ICIC
IC ICIC Metrohm Ion Chromatography Inline sample preparation Matrix neutralization: ammonia Metrosep A Supp 4 – 250 1 Formate n. q. 2 Chloride 0. 03 3 Nitrite 4 Bromide 0. 95 5 Nitrat 0. 04 6 Carbonate 7 Sulfate 4 n. q. 0. 13 1 ppm Na. HCO 3/Na 2 CO 3; 1. 7/1. 8 mmol/L; 26 % NH 3, 20 µL loop ic_sampl_prep_26062003_e. ppt 35 2 3 5 6 7
Metrohm Ion Chromatography IC ICIC Inline sample preparation Matrix neutralization OH cartridge E Mobile phase: eluent P 1 High pressure pump Injection valve «A» C » MSM» Suppressor D Conductivity detector P 2, 3 Peristaltic pumps 2 Injection Valve «B» T Transfer solution Cartridge A position fill, B position fill ic_sampl_prep_26062003_e. ppt C Ctr Analytical column 36 P 3 P 1 T E D
Metrohm Ion Chromatography Inline sample preparation Matrix neutralization: HCl 10 µL HCl direct injection ppm Metrosep C 2 – 250 ic_sampl_prep_26062003_e. ppt 37 IC ICIC
Metrohm Ion Chromatography IC ICIC Inline sample preparation Matrix neutralization: HCl Metrosep C 2 – 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 2 ppm 3 1 Tartaric-/dipicolinic acid; 4. 0/0. 75 mmol/L; 7 mol HCl, 10 µL loop ic_sampl_prep_26062003_e. ppt 38 4 5 6
Metrohm Ion Chromatography Inline sample preparation Ultra filtration Stop flow dialysis Pre concentration technique Matrix elimination Matrix neutralization In- line calibration ic_sampl_prep_26062003_e. ppt 39 IC ICIC
Metrohm Ion Chromatography IC ICIC Inline sample preparation Inline calibration Standard S, flow path E Mobile phase: eluent P 1 High pressure pump Injection valve «A» C C Analytical column » MSM» Suppressor D Conductivity detector P 3 2 P 1, 2, 3 Peristaltic pumps Injection Valve «B» S S E Standard A position inject, B position fill ic_sampl_prep_26062003_e. ppt 40 D
Metrohm Ion Chromatography IC ICIC Inline sample preparation Inline calibration # 1 Measurement of standard E Mobile phase: eluent P 1 High pressure pump Injection valve «A» C C Analytical column » MSM» Suppressor D Conductivity detector P 3 2 P 1, 2, 3 Peristaltic pumps Injection Valve «B» S S E Standard A position inject, B position fill ic_sampl_prep_26062003_e. ppt 41 D
Metrohm Ion Chromatography IC ICIC Inline sample preparation Inline calibration # 2 Preconcentrator inline E Mobile phase: eluent P 1 High pressure pump Injection valve «A» C C Analytical column » MSM» Suppressor D Conductivity detector P 3 2 P 1, 2, 3 Peristaltic pumps Injection Valve «B» S S E Standard A position fill, B position fill ic_sampl_prep_26062003_e. ppt 42 D
Metrohm Ion Chromatography IC ICIC Inline sample preparation Inline calibration # 3 Transfer of standard E Mobile phase: eluent P 1 High pressure pump Injection valve «A» C C Analytical column » MSM» Suppressor D Conductivity detector P 3 2 P 1, 2, 3 Peristaltic pumps Injection Valve «B» S S E Standard A position fill, B position inject ic_sampl_prep_26062003_e. ppt 43 D
Metrohm Ion Chromatography IC ICIC Inline sample preparation Inline calibration # 4 Inject of standard E Mobile phase: eluent P 1 High pressure pump Injection valve «A» C C Analytical column » MSM» Suppressor D Conductivity detector P 3 2 P 1, 2, 3 Peristaltic pumps Injection Valve «B» S S E Standard A position inject, B position inject ic_sampl_prep_26062003_e. ppt 44 D
Metrohm Ion Chromatography Inline sample preparation Inline calibration # 1: Transfer of 2 m. L ultrapure water to the preconcentrator Blank value # 2: Transfer of 2 m. L ultrapure water to the preconcentrator. Valve B is thrown from fill to inject and back once Calibration level 1 # 3: Transfer of 2 m. L ultrapure water to the preconcentrator. Valve B is thrown from fill to inject and back twice Calibration level 2 # 4: Transfer of 2 m. L ultrapure water to the preconcentrator. Valve B is thrown from fill to inject and back three times Calibration level 3, etc ic_sampl_prep_26062003_e. ppt 45 IC ICIC
Metrohm Ion Chromatography Inline sample preparation Inline calibration 100 ppt ic_sampl_prep_26062003_e. ppt 100. . . 400 ppt 46 IC ICIC
Metrohm Ion Chromatography inline sample preparation ? Metrohm can do that ic_sampl_prep_26062003_e. ppt 47 IC ICIC