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中国无机分析化学:2020,10(1):16-19
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高纯四氯化锗测试样品的采集和制备方法研究
(云南临沧鑫圆锗业股份有限公司)
Study on sampling and preparation of high pure germanium tetrachloride test samples
Pu Shikun1, Lin Zuoliang2, Wu Wangchang2, Li Zhengmei2, Luo Guoli2, Wang Xianqin2
(1.Yunnan Lincang Xinyuan Germanium Industry Co., Ltd.;2.YUNNAN LINCANG XINYUAN GERMANIUM INDUSTRIAL CO.,LTD.)
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投稿时间:2019-07-01    修订日期:2019-07-01
中文摘要: 本文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发射光谱法(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试验装置,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;试验优选了在制备ICP-MS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。 本方法的成功应用为光纤级高纯四氯化锗产品的质量检验提供了可靠的分析试样采集和制备方法,解决了光纤级高纯四氯化锗中痕量含氢杂质吸收峰红外透过率检测及痕量金属杂质测定用试样的采集和制备的关键技术难题,具有广阔的应用前景和显著的经济社会效益。
Abstract: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 sample’s test device 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 of sampling 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. The successful application of this method provides a reliable analytical sample collection and preparation method for quality inspection of fiber grade high purity germanium tetrachloride products. This work solves the key technical problems of infrared transmittance detection of trace hydrogen impurity and sample collection and preparation for determination of trace metal impurity in high purity tetrachloride germanium of fiber. Therefore it has broad application prospect and remarkable economic and social benefits.
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引用文本:
普世坤,林作亮,吴王昌,李正美,罗国利,王仙琴.高纯四氯化锗测试样品的采集和制备方法研究[J].中国无机分析化学,2020,10(1):16-19.
Pu Shikun,Lin Zuoliang,Wu Wangchang,Li Zhengmei,Luo Guoli,Wang Xianqin.Study on sampling and preparation of high pure germanium tetrachloride test samples[J].Chinese Journal of Inorganic Analytical Chemistry,2020,10(1):16-19.

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