用于荧光光谱测定的微量固体粉末样品制样优化*

为满足微量固体粉末荧光检测要求,采用薄层制样法,改变黏结剂种类、黏结剂的用量、涂层厚度以及后处理方法来进行其制样工艺优化。 结果表明:以聚乙烯醇做黏结剂、1∶5的固液比、在50 ℃烘干30 min、涂片次数3层的薄层制样优化工艺可满足荧光固体测样的要求。采用t检验比较固体样品池装样和薄层制样法的荧光检测结果发现两者无显著性差异,薄层制样优化工艺的需样量较样品池减少90%。

Optimization of Sample Preparation of Trace Solid Powder Detected Using Fluorescence Spectrometry

To meet the requirement of trace solid powder samples tested by fluorescence spectrometry,some process parameters of the thin-layer sample preparation were optimized including the type of binder,the amount of binder,the coating thickness and the post-treatment method.The results show that the thin-layer sample prepared with polyvinyl alcohol as binder,a solid-liquid ratio of 1∶5,drying at 50℃for 30 minutes and coating times of 3 layers can meet the test requirements.The analysis results of student’s t-test show that,even if the amount of thin-layer sample is reduced by 90%compared with the solid sample cell,there is no significant difference between the their results.