摘要
对惰性熔融红外吸收法测定高氢钛样品中氧含量的分析方法进行了研究,确定了最佳分析参数。通过步进式升温模式将样品中的大部分氢提前释放出来,避免了在高温条件下甲烷的产生。确定高温段最佳分析功率为4.8kW;最佳样品称样量为0.04~0.08g;助熔剂采用镍囊镍粒组合形式;氧最短分析时间为140s,比较器水平设为1%。使用标样502-879建立单标样校准曲线,得到回归方程y=0.7123 85x。通过对高氢钛样品的多次平行试验和加标回收试验对测定方法的可行性进行了分析,测定方法的相对标准偏差分别为2.57%,加标回收率在95%~107%,表明该测定方法可以准确测定高氢钛样品中的氧含量。
In this paper,a method was established to measure the oxygen content in titanium metal containing high hydrogen content based on the inert gas fusion and infrared absorption method.Most of the hydrogen could be released in advance at a low temperature in a step-by-step heating mode,and the generation of methane at high temperatures could be avoided.The analytical parameters were optimized,the optimally analytical power is 4.8 kW in high temperature step,sample weight is 0.04-0.08 g,fluxes are the combination of capsule nickel and nibbled nickel,minimum analysis time for oxygen is 140 s,and a comparator level is 1%.A calibration curve was built by using certified titanium standard sample(502-879)with a regression equation of y=0.712 385x.To verify the feasibility of the proposed method,a parallel test was carried out on a Ti64 sample with high hydrogen,and the oxygen recovery of standard addition was also determined on a titanium sample with high hydrogen.The relative standard deviation(RSD)was 2.57%,and the recovery of standard addition of the method was between 95%and 107%.These show that the proposed method could accurately determine the oxygen content in titanium containing high hydrogen.
作者
韩丽辉
张盈
HAN Lihui;ZHANG Ying(School of Metallurgical and Ecological Engineering,University of Science and Technology Beijing,Beijing100083,China;Institute of Process Engineering,Chinese Academy of Sciences,Beijing 100190,China)
出处
《实验室研究与探索》
CAS
北大核心
2019年第7期46-51,共6页
Research and Exploration In Laboratory
关键词
金属钛
氧
惰性熔融
红外吸收法
titanium
oxygen
inert gas fusion
infrared absorption method
