建立了微波消解-电感耦合等离子体质谱(ICP-MS)测定地质样品中稀土元素的方法,采用HNO3-HF体系-微波消解进行样品前处理,经赶酸后再用5 mL 1∶1 HNO3提取,整个过程安全、高效、无损失。利用ICP-MS进行测定,可以有效降低多原子离子质谱干扰,在优化仪器参数后,用内标铑(Rh)进行校正,弥补基体抑制效应和灵敏度漂移,测试结果更加准确。方法用于岩石标准物质(GBW07109,GBW07110和GBW07111)测试,其测定值与标准值相一致。结果表明,该方法的检出限低,准确度高,操作简单快捷,可同时测定多种元素,能满足批量测定地质样品中稀土元素含量的要求。
Abstract
Rare earth elements(REEs) in geological samples are of great interest,mainly because they might be considered as a primary source with the potential to resolve the global REEs supply shortage.This paper describes a method for the determination of REEs in geological samples by inductively coupled plasma mass spectrometry(ICP-MS).Samples were dissolved using distilled HNO3 and HF during microwave digestion process,in which HNO3 was added after acid-drying.The whole process was safe and efficient without any loss.In addition,the use of ICP-MS could effectively eliminate the interference of polyatomic ions.After optimizing the instrument parameters,the internal standard element rhodium(Rh) was used to compensate for matrix suppression effect and sensitivity drift so that the results were more accurate.The method was applied in the determination of REEs in the National Geochemistry Standard Reference Materials(GBW07109,GBW07110 and GBW07111).The determined values are in good agreement with the certified values.The results show that this method has the advantages of simplicity,rapidness, low detection limit and high accuracy,and could be used for the detection of many different elements at the same time.
关键词
微波消解电感耦合等离子体质谱地质样品稀土元素
Keywords
microwave digestioninductively coupled plasma mass spectrometry(ICP-MS)geological samplesrare earth elements