惰气熔融-热导/红外法测定钛合金中氧氮氢  

Determination of oxygen,nitrogen and hydrogen in titanium alloy by inert gas fusion-thermal conductivity/infrared method

作　　者：李延珍 霍艳 姜辰 史丹丹 LI Yanzhen;HUO Yan;JIANG Chen;SHI Dandan(Hangxin Material Technology Co.,Ltd.,Yantai 265706,China;National Pressure Processing Engineering Technology Research Center,Yantai 265713,China)

机构地区：[1]航鑫材料科技有限公司,山东烟台265706 [2]国家压力加工工程技术研究中心,山东烟台265713

出　　处：《冶金分析》2021年第6期87-93,共7页Metallurgical Analysis

摘　　要：钛合金中氧、氮和氢的含量对其力学性能影响很大,因此,需要对其准确测定。采用氢氟酸和硝酸体积比为1∶3的酸洗液清洗样品后再用无水乙醇浸泡的方法处理样品,测氧和氮时样品质量选择0.10 g,测氢时样品质量选择0.20 g,以镍篮为助熔剂,实现了惰气熔融-热导/红外法对钛合金中氧、氮和氢的测定。试验表明,样品放置4 h与放置1 d,检测结果差异不明显;随着放置时间的继续增加,氧的检测结果增加显著,氮和氢略有升高,故选择在样品处理完成后1 d内进行测定。在选定的实验条件下,氧、氮和氢的线性相关系数均大于0.999,方法检出限为0.48~0.69μg/g,定量限为1.6~2.3μg/g。选取两个钛合金样品,按照实验方法对氧、氮、氢进行测定,同时按照标准方法GB/T 4698.7—2011测定氧、氮,GB/T 4698.15—2011测定氢进行方法比对试验,实验方法与标准方法测定结果基本一致。按实验方法对3种钛合金样品中氧、氮、氢进行11次平行测定,测得结果的相对标准偏差(RSD,n=11)为0.54%~5.7%。The content of oxygen,nitrogen and hydrogen in titanium alloy had great influence on its mechanical properties.Therefore,their contents should be accurately determined.The sample was washed with mixed acid(the volume ratio of hydrofluoric acid to nitric acid was 1∶3)and then immersed in anhydrous ethanol.0.10 g of sample was used for the determination of oxygen and nitrogen,while 0.20 g of sample was used for the determination of hydrogen.Thus,a determination method of oxygen,nitrogen and hydrogen in titanium alloy was developed by inert gas fusion-thermal conductivity/infrared method with tin basket as flux.It was found that the determination results of samples after placing for 4 h and 1 d had no significant difference.As the placing time continued to increase,the determination results of oxygen increased significantly,and the determination results of nitrogen and hydrogen increased slightly.Therefore,the determination was carried out within 1 day after sample treatment.Under the selected experimental conditions,the linear correlation coefficients of oxygen,nitrogen and hydrogen were all higher than 0.999.The limits of detection of method were between 0.48μg/g and 0.69μg/g,and the limits of quantification were in range of 1.6-2.3μg/g.The contents of oxygen,nitrogen and hydrogen in two titanium alloy samples were determined according to the experimental method.Meanwhile,the comparison tests were also conducted:oxygen and nitrogen were determined according to standard method of GB/T 4698.7-2011,and hydrogen was determined according to standard method of GB/T 4698.15-2011.The determination results of proposed method were basically consistent with those obtained by the standard method.The contents of oxygen,nitrogen and hydrogen in three titanium alloy samples were determined according to the experimental method.The relative standard deviations(RSD,n=11)were between 0.54% and 5.7%.

关 键 词：钛合金 氧 氮 氢 惰气熔融 热导法 红外法 

分 类 号：O659.2[理学—分析化学]