使用化学抑制的离子色谱法进行阴离子分析

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ICSpak是JASCO开发的阴离子色谱抑制技术。该填料具有磺酸基团，该磺酸基团与苯乙烯-二乙烯基苯多孔聚合物化学结合，并填充在PEEK柱中。抑制器用于阴离子色谱法，以减少洗脱液的背景信号，并将样品变为具有高等效电导率的离子对。该抑制器可以使用再生和洗涤步骤进行再循环。硝酸根和亚硝酸根离子的更灵敏检测是使用紫外线检测器进行的。Application Note 2/4Analysis of Anions using IC with chemical suppression Analysis of Anions using IC with chemical suppression I ntroduction ICSpak i s a suppressor technology for anion chromatography developed by JASCO. The packing material has a sulfonic acid group chemically bonded to a styrene-divinylbenzene porous polymer and packed in a PEEK column. T he suppressor is used in anion chromatography to decrease the background s i gnal f rom the eluent and to change the sample to an ion-pair with high equivalent conductivity. This suppressor can be re-cycled using regeneration and washing steps. The more sensi t ive detection of nitrate and nitrite ions is m ade using a UV detector. This report descr i bes the analysis of anions using inert system and ICSpak. Keyword： Chemical suppressor ， anion， Shodex IC SI-90 4E， ICSpak， inert Experimental [Equipmen t ][Con d itions]Pump： PU-4080i Column：Shodex IC SI-90 4E(4.6mml .D.x250mmL)Pump option： DG unit Suppressor：ICSpak (4.6mml .D.x100mmL)Autosampler： AS-4050i Eluent：1.8mM Na2C03+1.7mM NaHCO3Column oven： CO-4060Flow rate：1.0mL/min Detector： UV-4075 (I nert Cell)Column temp.：25°℃Shodex CD-5Wave length：215nm Injection volume：100 pL Sta n d ar d Sample：Anion Mixture (Descr i bed below) Table 1 T h e concentration of anion stand a rd sol u t i on mixt u re Fig.1 The f l o w path diagram Results Fig.2 Chromatograms o f anion standard solution mixture. 7-component anions. Figure 2. Chromatograms of a n ion standard solution mixture usi n g Shodex IC SI -90 4E and che m ical suppressor ICSpak Top： UV detector ， Bottom：Conduct i v it y detector 1： F -， 2：CI-，3： NO2-， 4： Br-， 5： NO3-，6： PO43-， SO42- Table 2 Detec t ion limit for a range of anions. Table 2 Detection limit values for anions Anions Concentration [mg/L] Injection volume [ng] UV S/N=3 [mg/L] CD-5 S/N=3[mg/L] NO， 0.5 50 0.89 1.46 Br" 1 100 8.39 1.50 NO。 1 100 1.33 1.34 F- 0.2 20 0.32 CI 0.3 30 0.40 PO 3- 1.5 150 3.67 SO2 1.5 150 1.45 The CO-4065 can be equ i pped with two optional valves. Analysis and regenerating /washing can be performed i n parallel by using the CO-4065 with two 2-position/6-port switching valves with two ICSpak suppressor columns and a multi -so l vent regenerating/washing pump (e.g.， the PU-4180 fitted with a low-pressure gradient unit) as shown in the f i g.3. Part No. Model Description 7002-JO11A PU-4180i Inert HPLC Pump 7006-H003A DG-4000-04 4-channel Degasser Unit， for Analytical 7018-J002A AS-4050i Inert Autosampler 7021-J002A CO-4060 Column Oven 7026-J002A UV-4075 UV-Visible Detector 7025-H136A UV-4000 Inert flow cell unit 0507-1334 *CD-200 Conductivity Detector 7058-J011A BS-4000-1 Bottole Stand 0507-2330 F6995244 Shodex IC SI-90 4E 0509-0457A ICSpak Suppressor 6688-H564W LC-Net CG LC-Net Cable CG (x3) ChromNAVV2 Chromatography Data System 7001-H402A HPLC PEEK Start Up Kit for LC-4000 7001-H405A Maintenance Tool Kit Part No. Model Description 7002-J004A PU-4180 RHPLC Pump (Base Unit) 7006-H003A DG-4000-04 4-channel Degasser Unit， for Analytical 7007-H002A LG-4080 Low Pressure Gradient Unit， w/o Tera mixer 7012-J002A R-PU-4080i Expand pump unit 7018-J002A AS-4050i Inert Autosampler 7023-J002A CO-4065 Column Oven， Valve mountable model 9999 2 way 6 port x2 7026-J002A UV-4075 UVNIS detector 7025-H136A UV-4000 Inert flow cell unit 0507-1334 *CD-200 Conductivity Detector 7058-J011A BS-4000-1 Bottle Stand 0507-2330 F6995244 Shodex IC SI-90 4E 0509-H169A ICSpak supressor 6688-H564W LC-NetCG LC-Net cable CG (3 pieces) ChromNAV V2 Chromatography Data System 7001-H402A HPLC PEEK Start Up Kit for LC-4000 7001-H405A Maintenance Tool Kit