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环境化学  2015 

雪冰中痕量高氯酸盐的在线富集方法

Keywords: 高氯酸盐,在线富集,离子色谱,南极雪冰

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Abstract:

利用一维离子色谱建立了高氯酸盐的在线富集方法,以期为建立定量检测南极雪冰中痕量高氯酸盐的离子色谱-串联质谱法奠定基础.选用高容量、强亲水性的IonPacAS20阴离子交换柱进行分离,以淋洗液自动发生器在线产生的KOH作为淋洗液,等梯度淋洗.考虑到南极雪冰样品量十分有限,选定5mL为富集体积,对应的富集时间为10min.高氯酸盐质量浓度在0.5—50μg·L-1范围内,方法具有良好的线性(相关系数为0.9995),检出限(以S/N=3计)为0.05μg·L-1.将浓度为0.5μg·L-1的标准溶液连续11次富集进样,所得峰面积的相对标准偏差(RSD)为4.7%.以人工配制的仅含有高氯酸盐的溶液实施了加标回收实验,回收率在85%—108%之间.

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