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高纯度的化学试剂是许多食品分析、制药分析、工业制造等行业中的关键性基础化工材料之一,其中微量杂质的分析是发展这类试剂产业的关键技术环节之一。建立了高纯度有机试剂中的3种阴离子的离子色谱定量分析方法,分别以5和20 mmol/L NaOH为流动相,Ionpac AS 11-HC阴离子通用分析柱进行分离,电导检测器检测,可以实现HPLC级甲醇样品中添加的Cl-、SO2-4和NO-3的含量分析。该方法3种离子的线性范围在5~100μg/L之间,3种阴离子的最低检出浓度分别为2(Cl-)、5(SO2-4)和5μg/L(NO-3),方法的回收率为93%~107%,相对标准偏差(RSD)为2.0%~3.5%。此外,我们还进一步考察了前处理方法中采用WAX固相萃取技术对色谱纯的N-甲基-2-吡咯烷酮试剂中的阴离子进行富集,可以实现该样品中上述3种阴离子的分析检测。
High-purity chemicals are one of the key basic chemical materials in many food analysis, pharmaceutical analysis and industrial manufacturing industries. Among them, the analysis of trace impurities is one of the key technical aspects in the development of such reagent industries. An ion chromatographic method for the determination of three anions in high purity organic reagent was established. The separation was performed on 5 and 20 mmol / L NaOH as mobile phase and Ionpac AS 11-HC anion analytical column, respectively. Content analysis of Cl-, SO2-4 and NO-3 added in HPLC grade methanol sample. The linear range of the three ions was between 5 and 100 μg / L. The minimum detectable concentrations of the three anions were 2 (Cl -), 5 (SO2-4) and 5 μg / L (NO 3) The recoveries ranged from 93% to 107% with relative standard deviations (RSDs) from 2.0% to 3.5%. In addition, we further investigated the pretreatment method using WAX solid phase extraction of the chromatographic purity of N-methyl-2-pyrrolidone reagent anion enrichment can be achieved in the sample analysis of the above three anions detected.