脉冲红外和热导检测法测定钌粉和钌靶中氧、氮含量

摘要

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.%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。