高分辨ICP-MS测定涂料中痕量砷形态分布的研究

为建立高分辨率电感耦合等离子体质谱法(HR-ICP-MS)测定涂料中砷化合物形态分布的分析方法,应用离子交换树脂和溶剂萃取相结合的分离技术分离涂料中As(Ⅲ)、As(Ⅴ)、MMA(甲基胂酸)、DMA(二甲基胂酸)等4种砷化合物,试液直接用HR-ICP-MS法同时测定上述4种砷化合物,在高分辨质谱测量模式下避免了大量的质谱干扰,考察了采用内标元素对基体效应的校正,应用标准加入法进行定量分析,确定了实验的最佳测定条件。结果表明,方法的检出限为0.002μg/g,样品的加标回收率为98.2%～104.2%,相对标准偏差为0.72%～2.61%。该法具有简单、快速、准确等优点,应用涂料中砷化合物的4种不同形态砷的测定,结果满意。

Study on Determination of Arsenic Speciation in Paint by High Resolution ICP-MS

A rapid method of static adsorption of ion exchange resin and solvent extraction for seperation and high resolution inductively coupled plasma mass spectrometry （HR - ICP - MS） determination has developed for analysis of As （III ）, As （ V ）, MMA and DMA in paint. Most of the spectral interferences could be avoided by measuring in the high resolution mode. The correction for matrix effects was tried using internal standard elements. The standard addition method was employed for quantitative analysis. The optimum conditions for the determination was tested and discussed. The results show that the detection limit of As is 0. 002 μg/g, the recovery ratio is 98.2% - 104. 2%, and the RSD is less than 2.61%. The method is accurate, quick and convenient. It is used in the analysis of arsenic speciation in paint with satisfactory results.