高纯四氯化锗测试样品的采集和制备方法研究

针对光纤级高纯四氯化锗(99.999999%)中痕量含氢杂质吸收峰红外透过率检测(FTIR)用试样的采集,以及痕量金属杂质的电感耦合等离子体质谱法(ICP-MS)测定用试样的制备方法进行了系统研究。设计开发了用于检测痕量含氢杂质吸收峰红外透过率的样品采集实验装置,实现了含氢杂质(如—OH、—CH、HCl等)吸收峰的红外透过率在线连续测试,试样采集过程全密闭进行,避免了采样过程的二次污染,采样过程流程简短,操作简便;实验优选了在制备ICP-MS法测定痕量金属杂质用的试样过程中消除四氯化锗基体干扰、防止砷等易挥发杂质损失以及防止样品处理过程污染试样的制样方法,实现了试样制备过程二次污染源的有效控制,制样过程试剂消耗量少,制备时间短,待测元素无损失。

Study on sampling and preparation of high pure germanium tetrachloride test samples

In this paper,the sample collection for trace hydrogen impurity absorption peak infrared transmittance(FTIR)of high purity tetrachloride germanium(99.999999%)and the preparation of sample for determination of trace metal impurity by ICP-MS are studied systematically.A testing device of samples for detecting the infrared transmittance of absorption peak of trace hydrogen impurity was designed and developed,which implements the infrared absorption peak transmittance online continuous testing of hydrogen impurity(e.g.—OH,—CH,HCl,etc.).The sample collection process is fully airtight,to avoid the secondary pollution insampling process.In addition,this process is brief and easy to operate.The method of sample preparation for ICP-MS determination of trace metal impurities was optimized,which can eliminate the interference of germanium tetrachloride matrix,prevent the loss of volatile impurities such as arsenic and prevent the contamination of samples in the process of sample treatment.The effective control of secondary pollution source in sample preparation process is realized,meanwhile,less reagent consumption,shorter preparation time and no loss of elements to be measured during sample preparation process.