超级微波消解-电感耦合等离子体发射光谱法测定滑石粉纯度及其重金属含量

Determination of the purity and heavy metal content of talc powder by ultra microwave digestion-ICP-OES

基于超级微波消解结合电感耦合等离子体发射光谱(ICP-OES)技术,建立了一种简单高效、重现性好的滑石粉纯度及其重金属含量分析方法。在50mg滑石粉样品中加入1mL纯水、2mL硝酸、2mL盐酸以及3mL氟硼酸后,使用超级微波消解进行样品前处理,在保证彻底消解效果的前提下,基于预加压技术(预加压3.5MPa),获得了较高的微波消解效率,1h(程序升温至240℃)即可得到彻底的滑石粉消解效果。在最佳化的运行条件下,本方法获得各元素的方法检出限(LOD,3σ)在0.2~20μg·kg^(-1),加标回收率在90%~110%,相对标准偏差RSD在0.1%~1.0%,方法准确度及精密度可以满足多元素同时测定的需求,本方法能够充分应用于大批量滑石粉样品的纯度及其重金属含量分析。

After adding 1mL of pure water,2mL of nitric acid,2mL of hydrochloric acid,and 3mL of Fluoroboric acid to 50mg talc powder sample,the sample was pretreated by ultra-microwave digestion.Based on the pre-pressurization technology(pre-pressurization 3.5MPa),a complete talc powder digestion effect could be obtained in 1 hour(programmed heating to 240℃).Under the optimal operating conditions,the method detection limit(LOD,3σ)for each element obtained by this method was 0.2-20μg·kg^(-1),the recovery rate of standard addition was 90%-110%,and the relative standard deviation RSD was 0.1%-1.0%.The accuracy and precision of the method could meet the needs of simultaneous determination of multiple elements.The method is simple,efficient,and has good reproducibility,and can be applied to the analysis of the purity and heavy metal content of large batches of talc samples.