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[目的]建立石油醚中硫酸盐的高效阴离子交换色谱抑制型电导检测方法。[方法]选用去离子水、石油醚按照1︰1的体积比进行萃取后,取下清液水相过前处理小柱和过滤后进样分析。色谱条件为:高容量氢氧化物选择性色谱柱IonPacAS18阴离子分析柱,30mmol/L氢氧化钾(KOH)淋洗液等度淋洗,配有连续自动再生微膜抑制器的电导检测器。[结果]方法检出限为0.03mg/L,线性范围为0.2～20mg/L和5～500mg/L(可根据样品浓度选取不同的线性范围),相关系数r=0.9998以上。平均加标回收率为91.2%～101.3%,连续进样重现性RSD小于2.2%。[结论]本方法操作简单、快速、灵敏,结果准确,选择性好,适用于石油醚中硫酸根离子的测定。
[Objective] The research aimed to establish a high performance anion exchange chromatography inhibition conductivity detection method for petroleum sulfates in petroleum ether. [Method] After deionized water and petroleum ether were extracted according to the volume ratio of 1︰1, the aqueous phase of the supernatant was removed and the sample was filtered and injected for analysis. Chromatographic conditions were: IonPacAS18 anion column with high capacity hydroxide column, isocratic rinse with 30 mmol / L potassium hydroxide (KOH) eluent, and conductivity detector with continuous automatic regeneration of micro-membrane suppressor. [Result] The detection limit of the method was 0.03mg / L, linear range was 0.2 ~ 20mg / L and 5 ~ 500mg / L (the linear range could be chosen according to the sample concentration). The correlation coefficient was above 0.9998. The average spiked recoveries ranged from 91.2% to 101.3%. The reproducibility RSD of continuous injection was less than 2.2%. [Conclusion] The method is simple, rapid, sensitive, accurate and selective. It is suitable for the determination of sulfate ion in petroleum ether.