粉末压片X射线荧光光谱法测定氧化铝中杂质元素

介绍了X射线荧光光谱法测定氧化铝中杂质元素的方法。研究了粉末压片法中助研剂丙二醇的选择和用量，考察了氧化铝粒度对X射线荧光强度的影响。试验表明，样品的粒度达到40 μm以下，粒度效应减弱；对于10.0 g氧化铝样品，加2滴丙二醇，研磨40 s，并用硼酸镶边垫底，制备的测量样片效果较好。用系列氧化铝标准样品作校准曲线，对样品中11个元素进行测定，其SiO₂、Fe₂O₃、Na₂O、K₂O、CaO、Ga₂O₃、ZnO测得结果的相对标准偏差（RSD）均小于8.0%，P₂O₅、TiO₂、V₂O₅、Cr₂O₃的含量在3倍检出限以上，RSD小于10%，含量在3倍检出限以下的RSD小于17%。用氧化铝标准样品验证，测量结果与标准样品的认定值基本一致。

Determination of impurity elements in alumina by pressed powder pellet X-ray fluorescence spectrometry

This paper describes X-ray fluorescence spectrometric method of impurity elements in aluminum. The selection and dosage of assistant agent propylene glycol for the pressed powder pellet method, as well as alumina particle size’s effects on X-ray fluorescence intensity were studied. Experiments showed that, when the particle size was smaller than 40 μm, the size effect weakened;good sample pellet was prepared with 10.0 g of alumina sample plus two drops of propylene glycot ground for 40 s and then packaged with boric acid before pellet pressing.Calibration curve were founded using a series of standard samples of alumina. Eleven elements in each sample were determined. The RSD of SiO₂,Fe₂O₃,Na₂O,K₂O,CaO,Ga₂O₃,ZnO were smaller than 8.0%; the RSD of P₂O₅,TiO₂,V₂O₅,Cr₂O₃ were smaller than 10% when their content was larger than three times of the detection limit; smaller than 17% when their content was smaller than three times of the detection limit. The method has been applied to the determination of those elements in alumina reference materials, and the results for these elements were in good agreement with certified values.