X-射线荧光光谱法测定地质样品中氯元素含量

Determination of Chlorine in Geological Samples by X-ray Fluorescence Spectrometry

X射线荧光法检测地质样品中氯元素含量时普遍存在同一个样片随着检测次数的增加检测结果增高的现象,因此检测数据报出结果只能报初次检测的结果,对于产生这一现象原因的研究很少有报道,本实验通过诸多实验研究得出:105℃、200℃烘干、300~800℃灼烧处理的样品制片后检测,氯元素检测值仍然随着检测次数的增加而增高,表明这种增高并不是因为水分子由样片内向样片检测面扩散引起的;真空环境和X射线照射环境对检测结果都会产生影响,在相同时间条件下X射线照射时间越长氯元素检测值越高;研究还表明一般情况下样品中氯元素含量越低,随着检测次数增加检测结果增高趋势越明显,氯元素含量越高,这种增高的趋势越不明显,样品含量在1000~7000µg/g时检测12次后其增高的量才能使检测结果和实际参考值之间产生较大差异,当氯元素含量超过7000µg/g时,多次检测结果几乎没有变化;镶边衬底材料低压聚乙烯粉及硼酸对氯的检测结果没有影响;样品在不同存储环境(干燥器、仪器间、常量金前处理工作间)下存储56小时后,检测结果和参考值间没有明显差异。

When X-ray fluorescence method is used to detect the content of chlorine elements in geological samples,it is common for the same sample to have an increase in detection results with the increase of detection times.Therefore,the reported results of the detection data can only be the results of the initial detection.There are few reports on the reasons for this phenomenon.Through many experimental studies,this experiment found that samples dried at 105℃,200℃,and burned at 300~800℃are tested after being prepared,The detection value of chlorine element still increases with the increase of detection times,indicating that this increase is not caused by the diffusion of water molecules from the sample to the detection surface of the sample;Both vacuum environment and X-ray irradiation environment have an impact on the detection results.Under the same time conditions,the longer the X-ray irradiation time,the higher the chlorine element detection value;Research also shows that in general,the lower the chlorine content in the sample,the more obvious the increasing trend of the test results as the number of tests increases.The higher the chlorine content,the less obvious the increasing trend.The amount of increase in the sample content after 12 tests at 1000~7000µg/g can make a significant difference between the test results and the actual reference value.When the chlorine content exceeds 7000µg/g,the results of multiple tests show almost no change;Low pressure polyethylene powder and boric acid have no effect on the detection results of chlorine in the edge substrate material;After storing the samples in different storage environments(dryer,instrument room,constant gold pre-treatment workshop)for 56 hours,there was no significant difference between the test results and reference values.