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选用几种常用玻璃色谱自动进样瓶(简称色谱瓶),包括硼硅玻璃、一级水解级玻璃和高白料玻璃色谱瓶,以及聚丙烯材质的色谱瓶,1%HNO3对色谱瓶浸提后用ICP-MS和HPLC-ICP-MS测定浸提液中砷的总量和形态,并研究了10%HNO3对色谱瓶的清洗效果;此外还探讨了温度及时间对玻璃色谱瓶中砷释放的影响.结果表明,玻璃色谱瓶中砷普遍存在,其中硼硅玻璃色谱瓶浸提液中砷浓度低于1μg·L-1,用10%HNO3酸泡24 h能够全部清除;而一级水解级玻璃和高白料玻璃色谱瓶浸提液中砷的浓度则高达45.67μg·L-1和70.25μg·L-1,酸泡24 h后也有较高的残留量,浓度分别为1.63μg·L-1和0.94μg·L-1.高温能促进玻璃色谱瓶中砷的释放;玻璃色谱瓶中砷的释放量随时间的延长而增加,但短时间内即达到平衡.形态分析结果表明,玻璃色谱瓶浸提液中砷形态为As(Ⅴ),没有检测到As(Ⅲ)、二甲基砷酸(DMA)和甲基砷酸(MMA).同时,聚丙烯色谱瓶浸提液中砷总量低于检测限,因而在进行砷形态测定时,建议使用聚丙烯色谱瓶或者经10%HNO3清洗后的硼硅玻璃色谱瓶,以避免玻璃色谱瓶中As(Ⅴ)的污染.
Several common glass chromatography auto-sampling vials (abbreviated as chromatographic vials) are used, including borosilicate glass, first-grade hydrolyzed glass and high-white glass chromatographic vials, polypropylene bottles, and 1% HNO3 The total amount and morphology of arsenic in the extract was determined by ICP-MS and HPLC-ICP-MS, and the cleaning effect of 10% HNO3 on the chromatographic flask was also studied. In addition, the effects of temperature and time on the arsenic release .The results showed that arsenic was common in glass chromatographic bottles, in which the concentration of arsenic in the borosilicate glass chromatographic flask was less than 1μg · L-1, and was completely eliminated with 10% The concentrations of arsenic in the leaching solution of glass grade glass and high white glass bottle were as high as 45.67μg · L-1 and 70.25μg · L-1, respectively, and the acid residues were higher after 24 h, with concentrations of 1.63μg · L-1 and 0.94μg · L-1.High temperature could promote the release of arsenic in the glass chromatographic flask.Arsenic release in the glass chromatographic flask increased with time, but reached a balance within a short time.From the results of morphological analysis, The As (Ⅴ) in As (Ⅴ), the arsenic (Ⅲ), dimethyl arsenate (DMA) and methyl arsenate (MMA) were not detected in glass bottle. , The total amount of arsenic in the polypropylene bottle extract is below the limit of detection, so it is recommended to use a polypropylene bottle or a borosilicate glass bottle after washing with 10% HNO3 for the determination of arsenic speciation in order to avoid glass chromatography Bottle of As (Ⅴ) pollution.