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Ic_sampl_prep_26062003_e.ppt 1 IC Metrohm inline sample preparation Techniques for analytical success Metrohm Ion Chromatography Bart Cleeren, Metrohm

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ic_sampl_prep_26062003_e.ppt 1 IC Metrohm inline sample preparation Techniques for analytical success Metrohm Ion Chromatography Bart Cleeren, Metrohm Belgi Slide 2 ic_sampl_prep_26062003_e.ppt 2 IC Metrohm Ion Chromatography Inline sample preparation Ultra filtration Stop flow dialysis Pre concentration technique Matrix elimination Matrix neutralization In- line calibration Slide 3 ic_sampl_prep_26062003_e.ppt 3 IC Metrohm Ion Chromatography Inline sample preparation Ultra filtration Stop flow dialysis Pre concentration technique Matrix elimination Matrix neutralization In- line calibration Slide 4 ic_sampl_prep_26062003_e.ppt 4 IC Metrohm Ion Chromatography Ultrafiltration Inline sample preparation Ultrafiltration cell EMobile phase: eluent P1High pressure pump Injection valve A CAnalytical column MSM Suppressor DConductivity detector SSample P2Peristaltic pump A position fill C P1 ED 2 Slide 5 ic_sampl_prep_26062003_e.ppt 5 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 Slide 6 ic_sampl_prep_26062003_e.ppt 6 IC Metrohm Ion Chromatography Ultrafiltration Inline sample preparation # 1 Sample filtration EMobile phase: eluent P1High pressure pump Injection valve A CAnalytical column MSM Suppressor DConductivity detector SSample P2Peristaltic pump A position fill C P1 ED 2 Slide 7 ic_sampl_prep_26062003_e.ppt 7 IC Metrohm Ion Chromatography Ultrafiltration Inline sample preparation # 2 Sample injection EMobile phase: eluent P1High pressure pump Injection valve A CAnalytical column MSM Suppressor DConductivity detector SSample P2Peristaltic pump A position inject C P1 ED 2 Slide 8 ic_sampl_prep_26062003_e.ppt 8 IC Metrohm Ion Chromatography Ultrafiltration: vegetable juice Inline sample preparation A Supp 4 250 1Organicsn.q. 2Organicsn.q. 3Cl 4141 4NO 3 102 5HPO 4 2 577 6SO 4 2 842 7Oxalaten.q. ppt NaHCO 3 /Na 2 CO 3 ; 1.7/1.8 mmol/L; dilution 1:100; 0.15 m rec. cellul. Slide 9 ic_sampl_prep_26062003_e.ppt 9 IC Metrohm Ion Chromatography Inline sample preparation Ultra filtration Stop flow dialysis Pre concentration technique Matrix elimination Matrix neutralization In- line calibration Slide 10 ic_sampl_prep_26062003_e.ppt 10 IC Metrohm Ion Chromatography Inline sample preparation Dialysis cell, acceptor solution EMobile phase: eluent P1High pressure pump Injection valve A CAnalytical column MSM Suppressor DConductivity detector P2Peristaltic pump P3Peristaltic pump (2 Ch.) Dialysis cell AAcceptor solution Dialysis C P1 ED 2 A E P2 P3 A D C X X Slide 11 ic_sampl_prep_26062003_e.ppt 11 IC Metrohm Ion Chromatography Inline sample preparation # 2 Stopped flow dialysis EMobile phase: eluent P1High pressure pump Injection valve A CAnalytical column MSM Suppressor DConductivity detector P2Peristaltic pump Injection Valve B Dialysis cell AAcceptor solution Dialysis C P1 ED 2 A P3 P2 A P1 C DE X Slide 12 ic_sampl_prep_26062003_e.ppt 12 IC Metrohm Ion Chromatography Dialysis cell Inline sample preparation Continuous flow dialysis Exclusion diameter 0.2 m Ions can pass Oil droplets, fat micelles, particles are excluded Strong concentration gradient No equilibrium concentration Cellulose acetate membrane Slide 13 ic_sampl_prep_26062003_e.ppt 13 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 Slide 14 ic_sampl_prep_26062003_e.ppt 14 IC Metrohm Ion Chromatography Dialysis: milk Inline sample preparation Metrosep Dual 1 70 1Chloride938 2Nitraten.q. 3Phosphaten.q 4Sufate103 ppm NaHCO 3 /Na 2 CO 3 ; 2.4/2.0 mmol/L; dilution 1:5; 0.2 m cellul. acetat Slide 15 ic_sampl_prep_26062003_e.ppt 15 IC Metrohm Ion Chromatography Dialysis: cutting oil emulsion Inline sample preparation Metrosep Dual 2 1Chloride74.7 2Nitrite20.5. 3Nitrate23.9 4n. det.- 5Phosphate25.2 6Sulfate192.7 7n. det.- NaHCO 3 /Na 2 CO 3 ; 2.0/1.3 mmol/L; dilution 1:5; 0.2 m cellul. acetat Slide 16 ic_sampl_prep_26062003_e.ppt 16 IC Metrohm Ion Chromatography Inline sample preparation Ultra filtration Stop flow dialysis Pre concentration technique Matrix elimination Matrix neutralization In- line calibration Slide 17 ic_sampl_prep_26062003_e.ppt 17 IC Metrohm Ion Chromatography Inline sample preparation # 1 Sample preconcentration EMobile phase: eluent P1High pressure pump Injection valve A CAnalytical column MSM Suppressor DConductivity detector P2Peristaltic pump C P1 D P32 S Inline pre concentration E C P1 P 2 D Slide 18 ic_sampl_prep_26062003_e.ppt 18 IC Metrohm Ion Chromatography Inline sample preparation # 2 Sample analysis EMobile phase: eluent P 1High pressure pump Injection valve A CAnalytical column MSM Suppressor DConductivity detector P 2Peristaltic pump C P1 ED P32 S Inline preconcentration E C D P1P 2 Slide 19 ic_sampl_prep_26062003_e.ppt 19 IC Metrohm Ion Chromatography Inline preconcentration: ultra pure water Inline sample preparation Metrosep A Supp 5 150 1Acetate2.3 2Formate22.0 3Chloride13.0 4Carbonaten.q. 5Nitrate4.5 6Phosphate16.0 7Sulfate8.5 8Oxalate12.0 ppt NaHCO 3 /Na 2 CO 3 ; 1.0/3.2 mmol/L; 20 mL preconc, Slide 20 ic_sampl_prep_26062003_e.ppt 20 IC Metrohm Ion Chromatography Inline preconcentration: ultra pure water Inline sample preparation Metrosep Dual 2 1Fluoride45 150 2Chloride100 210 3Bromide0 100 4Nitrate10 112 5Sulfate40 145 ppt NaHCO 3 /Na 2 CO 3 ; 2.0/3.2 mmol/L; 10 mL preconc, spiked 100 ppt Slide 21 ic_sampl_prep_26062003_e.ppt 21 IC Metrohm Ion Chromatography Inline sample preparation Ultra filtration Stop flow dialysis Pre concentration technique Matrix elimination Matrix neutralization In- line calibration Slide 22 ic_sampl_prep_26062003_e.ppt 22 IC P3 Metrohm Ion Chromatography Inline sample preparation Transfer solution T EMobile phase: eluent P1High pressure pump Injection valve A CAnalytical column MSM Suppressor DConductivity detector P2Peristaltic pump Injection Valve B P3Peristaltic pump TTransfer solution A position fill, B position fill C P1 ED 2 T Matrix elimination Slide 23 ic_sampl_prep_26062003_e.ppt 23 IC P3 Metrohm Ion Chromatography Inline sample preparation # 1 Preconcentrator column inline EMobile phase: eluent P1High pressure pump Injection valve A CAnalytical column MSM Suppressor DConductivity detector P2Peristaltic pump Injection Valve B P3Peristaltic pump TTransfer solution A position fill, B position fill C P1 ED 2 T Matrix elimination Slide 24 ic_sampl_prep_26062003_e.ppt 24 IC P3 Metrohm Ion Chromatography Inline sample preparation # 2 Sample transfer, matrix elim. EMobile phase: eluent P1High pressure pump Injection valve A CAnalytical column MSM Suppressor DConductivity detector P2Peristaltic pump Injection Valve B P3Peristaltic pump TTransfer solution A position fill, B position inject C P1 ED 2 T Matrix elimination Slide 25 ic_sampl_prep_26062003_e.ppt 25 IC P3 Metrohm Ion Chromatography Inline sample preparation # 3 Sample inject EMobile phase: eluent P1High pressure pump Injection valve A CAnalytical column MSM Suppressor DConductivity detector P2Peristaltic pump Injection Valve B P3Peristaltic pump TTransfer solution A position inject, B position inject C P1 ED 2 T Matrix elimination Slide 26 ic_sampl_prep_26062003_e.ppt 26 IC Metrohm Ion Chromatography Matrix elimination: organic solvents Inline sample preparation 50 L iPrOH Bwith matrix elimination Awithout matrix elimination ppt FF Ac 443 Cl 30 NO 3 28 SO 4 2 425 Cl 24 NO 3 17 SO 4 2 Slide 27 ic_sampl_prep_26062003_e.ppt 27 IC Metrohm Ion Chromatography Matrix elimination: 35 % H 2 O 2 Inline sample preparation left: without m.e. Loop 20 L right: with m.e. Loop 20 L transfer vol. 2 mL Slide 28 ic_sampl_prep_26062003_e.ppt 28 IC Metrohm Ion Chromatography Inline sample preparation Ultra filtration Stop flow dialysis Pre concentration technique Matrix elimination Matrix neutralization In- line calibration Slide 29 ic_sampl_prep_26062003_e.ppt 29 IC P3 Metrohm Ion Chromatography Inline sample preparation 833.0030 IC Sample Prep. Unit EMobile phase: eluent P1High pressure pump Injection valve A CAnalytical column MSM Suppressor DConductivity detector P2, 3Peristaltic pumps Injection Valve B TTransfer solution 833 IC Sample Prep A position inject, B position fill C P1 ED 2 T Matrix neutralization Slide 30 ic_sampl_prep_26062003_e.ppt 30 IC P3 Metrohm Ion Chromatography Inline sample preparation # 1 Preconcentrator column inline EMobile phase: eluent P1High pressure pump Injection valve A CAnalytical column MSM Suppressor DConductivity detector P2, 3Peristaltic pumps Injection Valve B TTransfer solution 833 IC Sample Prep A position fill, B position fill C P1 ED 2 T Matrix neutralization Slide 31 ic_sampl_prep_26062003_e.ppt 31 IC P3 Metrohm Ion Chromatography Inline sample preparation # 2 Sample transfer/neutralization EMobile phase: eluent P1High pressure pump Injection valve A CAnalytical column MSM Suppressor DConductivity detector P2, 3Peristaltic pumps Injection Valve B TTransfer solution 833 IC Sample Prep A position fill, B position inject C P1 ED 2 T Matrix neutralization Slide 32 ic_sampl_prep_26062003_e.ppt 32 IC P3 Metrohm Ion Chromatography Inline sample preparation # 4 Sample inject EMobile phase: eluent P1High pressure pump Injection valve A CAnalytical column MSM Suppressor DConductivity detector P2, 3Peristaltic pumps Injection Valve B TTransfer solution 833 IC Sample Prep A position inject, B position inject C P1 ED 2 T Matrix neutralization Slide 33 ic_sampl_prep_26062003_e.ppt 33 IC 0.74 F 3.6 Cl 0.97 NO 3 0.98 HPO 4 2 1.1 SO 4 2 Metrohm Ion Chromatography Matrix neutraliza