摘要
高温合金中的痕量杂质元素会对高温合金的性能产生一定影响,因此高温合金中杂质含量的严格控制和准确测定尤为重要。该文基于三重四极杆电感耦合等离子体串联质谱(ICP-MS/MS)直接测定了铁镍基高温合金中的15种杂质元素。采用硝酸、盐酸、氢氟酸混合酸消解样品,定容后直接上机测试,无需萃取和分离,大大提高了前处理分析效率。在氦气碰撞模式下,实现了高纯铁镍基高温合金中干扰较小的杂质元素的测试分析。由于Mo含量较高的高温合金样品中,^(95)Mo^(16)O^(+)会对^(111)Cd的测定造成强烈质谱干扰,导致单四极杆质谱仪测试受限。基于此,该文利用ICP-MS/MS优越的反应池技术,在O_(2)原位质量模式下,通过设置一级质量过滤器(Q1)的质荷比(m/z)为111,并向碰撞反应池中加入O_(2),使^(95)Mo^(16)O^(+)与O_(2)反应生成^(95)Mo^(16)O^(16)O^(+),再设置二级质量过滤器(Q2)的m/z也为111,使^(111)Cd被通过和检测,从而避免了质谱重叠干扰,实现了Cd含量的稳定测试。该研究以铁镍基高温合金标准物质(GBW01620)为样本进行验证,结果表明,各元素的线性相关系数均大于0.999,方法检出限为0.001~1.24 mg/kg,相对标准偏差不大于3.5%,15种元素的测试值均在认定值的不确定度范围内。该方法为高纯合金样品的准确测试分析提供了思路和借鉴。
Strict control and accurate measurement of impurity content in high-temperature alloys are particularly important as the trace impurity elements in high-temperature alloys may have a certain im⁃pact on the performance of high-temperature alloys.A triple quadrupole inductively coupled plasma tandem mass spectrometry(ICP-MS/MS)was applied to the direct determination of 15 impurity ele⁃ments in Fe-Ni based superalloys.The sample was firstly digested with a mixture of nitric acid,hy⁃drochloric acid and hydrofluoric acid,then directly determined on the machine after constant vol⁃ume,without the need for extraction and separation,greatly improving the efficiency of pre-treat⁃ment analysis.In the helium collision mode,the testing and analysis of impurity elements with less interference in high-purity iron-nickel based high-temperature alloys were achieved.As^(95)Mo^(16)O^(+)in the superalloy samples with high molybdenum content will cause strong mass spectrum interference to the determination of^(111)Cd,the single quadrupole mass spectrometer test is limited.Based on this,the superior reaction cell technology of ICP-MS/MS was used in this paper to set the mass-to-charge ratio(m/z)of the primary mass filter(Q1)to 111,and add O_(2)to the collision reaction pool,so that^(95)Mo^(16)O^(+)reacted with O_(2)to generate^(95)Mo^(16)O^(16)O^(+),and then setting the m/z of the secondary mass filter(Q2)to 111,so that^(111)Cd was passed and detected,thus avoiding the overlapping interference of mass spectra,and stable testing of Cd content was achieved.This study was validated using the iron nickel based high-temperature alloy standard material(GBW01620)as a sample.The results showed that the linear correlation coefficients for each element were greater than 0.999,the detection limits of the method were 0.001-1.24 mg/kg,and the relative standard deviations were not larger than 3.5%.The test values for the 15 elements were all within the uncertainty range of the determined val⁃ues.This method provides an idea or reference for accurate testing and analysis of high-purity alloy samples.
作者
杨萌
李鹰
李剑
李维涵
刘岩
YANG Meng;LI Ying;LI Jian;LI Wei-han;LIU Yan(Hangzhou Puyu Technology Co.Ltd.,Hangzhou 311300,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2023年第7期870-875,共6页
Journal of Instrumental Analysis
基金
国家重点研发计划(2021YFF0700804)。
