激光溅射电离飞行时间质谱快速定量分析钛合金中的氢OA北大核心CSTPCDEI
Rapid Quantitative Analysis of Hydrogen in Titanium Alloys by Laser Sputtering Ionization Time-of-flight Mass Spectrometry
本研究使用自行搭建的激光溅射电离飞行时间质谱(LAI-TOF MS)对钛合金标准样品进行检测,建立了钛合金中氢的直接定量分析方法,得到氢元素标准曲线的线性关系良好,线性相关系数0.9913,检出限低至0.0004%,计算得到氢元素的原子化和离子化效率约为 13.4%.将该方法应用于其他钛合金样品中氢元素的分析,氢测定值相对标准偏差(RSDs)均小于 14%;将该测定结果与惰性气体熔融-红外法测定值进行对比,相对误差均在5%以内.同时,通过分析LAI-TOF MS谱图,可实现钛合金样品中Be、C、Al、Si、P、Ca、Cr、Fe、Zr、Mo、Pd、In、Sn等微量元素的定性和半定量检测.结果表明,基于LAI-TOF MS建立的钛合金中氢定量检测方法几乎无需样品前处理、操作简便、分析时间短、灵敏度高,可用于钛合金中氢元素的快速直接定量检测.
Titanium alloy is an important structural material with many advantages of high strength,excellent corrosion resistance,good biocompatibility,and good processing performance,which has been widely used in aerospace,medical devices,automobile manufacturing and various other fields.However,the presence of hydrogen in titanium alloys can lead to hydrogen embrittlement,which degrades the mechanical properties.Due to its high ionization energy,high reactivity,and high diffusivity,quantitative analysis of hydrogen in metal or alloy materials faces enormous challenge.Accurately and quickly detecting the hydrogen content in titanium alloys is of great significance for optimizing material design and controlling product quality.Traditional methods for determining the hydrogen in titanium alloys require complicated sample pretreatment,which greatly prolong the analysis time.The self-built high irradiance laser ablation and ionization time-of-flight mass spectrometry(LAI-TOF MS)has many advantages such as high sensitivity,high resolution,multi-element simultaneous detection,and simple sample pretreatment.It introduces helium into the ion source as a buffer gas to cool the high kinetic energy ions and reduce the multi-charged ion interferences,and has been successfully applied to the determination of metallic and nonmetallic elements in solid samples.In this study,a direct quantitative analysis method of LAI-TOF MS was established for detecting hydrogen in titanium alloys.The calibration curve of intensities and contents for hydrogen has a correlation coefficient of 0.991 3,the limit of detection(LOD)is calculated to be 0.000 4%,and the atomization and ionization efficiency of hydrogen can reach 13.4%.This method was applied to the analysis of hydrogen in other titanium alloy samples.The relative standard deviations(RSDs)of hydrogen signals are less than 14%.The relative errors of the quantitative results are less than 5%compared with values obtained by the pulsed heating-infrared method.The analysis time for a single titanium alloy sample is only a few minutes,significantly shorter than the 2-4 h required for the pulsed heating-infrared method.The spectrum obtained by LAI-TOF MS enables qualitative and semi-quantitative determination of trace elements of Be,C,Al,Si,P,Ca,Cr,Fe,Zr,Mo,Pd,In and Sn in the titanium alloy samples.Considering the advantages of less sample preparation,simplicity,rapidness,and high sensitivity,the method based on LAI-TOF MS can be used to the directly quantitative analysis of hydrogen in titanium alloys and can be further extended to the quantitative analysis of hydrogen in other materials,such as hydrogen storage materials,metal materials,ceramic materials and other related materials.
洪周怡;张振建;王煜兵;徐周毅;郭伟;杭纬
厦门大学化学化工学院,谱学分析与仪器教育部重点实验室,福建厦门 361005厦门大学萨本栋微米纳米科学技术研究院,福建厦门 361102中国地质大学,生物地质与环境地质国家重点实验室,湖北武汉 430078
化学
钛合金氢定量激光溅射电离飞行时间质谱(LAI-TOF MS)微量元素半定量分析
titanium alloyhydrogen quantificationlaser ablation and ionization time-of-flight mass spectrometry(LAI-TOF MS)trace elementssemi-quantitative analysis
《质谱学报》 2024 (004)
457-464 / 8
厦门市自然科学基金项目(3502Z20227013);福建省双百计划人才经费
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