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脉冲红外和热导检测法测定钌粉和钌靶中氧、氮含量
引用本文:刘 伟,刘 文,韩守礼,贺小塘,谭志龙,方 卫,王应进,杨晓滔,甘建壮,唐发静.脉冲红外和热导检测法测定钌粉和钌靶中氧、氮含量[J].贵金属,2013,34(4):53-56.
作者姓名:刘 伟  刘 文  韩守礼  贺小塘  谭志龙  方 卫  王应进  杨晓滔  甘建壮  唐发静
作者单位:贵研资源易门有限公司,云南 易门 651100;贵研资源易门有限公司,云南 易门 651100;贵研资源易门有限公司,云南 易门 651100;贵研资源易门有限公司,云南 易门 651100;贵研铂业股份有限公司 稀贵金属综合利用新技术国家重点实验室,昆明 650106;贵研铂业股份有限公司 稀贵金属综合利用新技术国家重点实验室,昆明 650106;贵研铂业股份有限公司 稀贵金属综合利用新技术国家重点实验室,昆明 650106;贵研铂业股份有限公司 稀贵金属综合利用新技术国家重点实验室,昆明 650106;贵研铂业股份有限公司 稀贵金属综合利用新技术国家重点实验室,昆明 650106;贵研资源易门有限公司,云南 易门 651100
基金项目:国家高技术研究发展计划(863计划)项目(2012AA063203)、国家自然科学基金(51262015)、云南省自然科学重点基金(2010ZC261)和云南省自然科学基金(2010ZC55)。
摘    要:建立了钌粉和钌靶中氧、氮含量的测定方法。研究了样品前处理、仪器条件、助熔剂选择、方法准确度和精密度等。以锡-碳作助熔剂,在选定条件下,采用脉冲红外和热导检测法,测定50×10-6氧时RSD<10%,测定40×10-6氮时RSD<25%;加标回收率:氧100%~102%,氮91%~101%。测定范围:氧0.002%~0.4%,氮0.0001%~0.02%。方法简便、快速、精密度和准确度满足质量控制要求。

关 键 词:分析化学  钌粉  钌靶  氧、氮含量
收稿时间:2013/1/22 0:00:00

Determination of Oxygen and Nitrogen Content in Ru Powder and Target by Pulsed Infrared and Thermal Conductivity Detection Method
LIU Wei,LIU Wen,HAN Shouli,HE Xiaotang,TAN Zhilong,FANG Wei,WANG Yingjin,YANG Xiaotao,GAN Jianzhuang and TANG Fajing.Determination of Oxygen and Nitrogen Content in Ru Powder and Target by Pulsed Infrared and Thermal Conductivity Detection Method[J].Precious Metals,2013,34(4):53-56.
Authors:LIU Wei  LIU Wen  HAN Shouli  HE Xiaotang  TAN Zhilong  FANG Wei  WANG Yingjin  YANG Xiaotao  GAN Jianzhuang and TANG Fajing
Affiliation:Sino-Platinum Metals Resources Yimen Co.Ltd., Yimen 651100, Yunnan, China;Sino-Platinum Metals Resources Yimen Co.Ltd., Yimen 651100, Yunnan, China;Sino-Platinum Metals Resources Yimen Co.Ltd., Yimen 651100, Yunnan, China;Sino-Platinum Metals Resources Yimen Co.Ltd., Yimen 651100, Yunnan, China;State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals, Sino-Platinum Metals Co.Ltd., Kunming 650106, China;State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals, Sino-Platinum Metals Co.Ltd., Kunming 650106, China;State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals, Sino-Platinum Metals Co.Ltd., Kunming 650106, China;State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals, Sino-Platinum Metals Co.Ltd., Kunming 650106, China;State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals, Sino-Platinum Metals Co.Ltd., Kunming 650106, China;State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals, Sino-Platinum Metals Co.Ltd., Kunming 650106, China
Abstract:A method using the pulsed infrared-thermal conductivity detection has been established to determine O and N content in Ru powder and target. Pre-treatment of the samples, testing condition of the equipment, choice of the accelerators, accuracy and precision of the method were investigated. Under the optimized conditions with Sn-C as an accelerator, the RSD (Relative standard deviation, n=7) was found to be <10% for oxygen analysis when its content did not exceed 50×10-6, and <25% for nitrogen analysis when its content was no more than 40 ×10-6. The recovery for standard addition test was 100%~102% for oxygen and 91%~101% for nitrogen. The measuring ranges were 0.002%~0.4% for oxygen and 0.0001%~0.02% for nitrogen. The accuracy and precision of the method are satisfactory.
Keywords:analytic chemistry  ruthenium powder  ruthenium target  content of oxygen and nitrogen
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