建立了一种测定酒石酸中痕量阴离子的离子色谱柱切换技术分析方法.使用Dionex IonPac ICE-AS6离子排斥柱将所需分析的痕量NO3-、PO43-、SO42-离子从酒石酸溶液中分离出来,再将被分离组分通过Dionex IonPacAG23(4 mm×50 mm)离子交换浓缩柱进行浓缩,最后将浓缩柱的组分通过Dionex IonPac AG22(4 mm×50 mm)和Dionex IonPac AS22(4 mm×250 mm)色谱柱进行分离,抑制型电导器进行检测.方法所得回收率在88.7%~114.1%,且具有较好的重现性和较低的检出限,根据3∶1的信噪比3种离子的检测限分别达到9.692、31.275、1.762μg.L-1,线性良好,范围从检测限到1 000 mg.L-1.本文方法可以应用于其它有机酸中痕量无机阴离子的检测.
A method for the simultaneous determination of trace anions(NO-3,PO3-4,SO2-4) in pure tartaric acid with column-switching ion chromatography was described.An ion excluding column Dionex IonPac ICE-AS6 was used for the separation of these three anions from tartaric ion.A pre-concentration column Dionex IonPac AG23(4 mm×50 mm) was used to enrich the trace anions.After being switched to analytical system,the separation was performed on Dionex ICS1500 using Dionex IonPac AG22(4 mm×50 mm) as guard column,Dionex IonPac AS22(4 mm×250 mm) as analytical column.The detection limit(signal to noise of 3∶1) of this method can reach 9.692 μg·L-1,31.275 μg·L-1,1.762 μg·L-1,respectively.The RSDs of retention time and peak area were good.Analyte calibration curves of analytes were linear(r0.99) in the range between the LODs and 1 000 mg·L-1.The recoveries of these anions were between 88.7%-114.1%.This simple way can be applied to detect the anions in other organic acid.