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作 者:王佳 朱伶俐 舒露 郭洪壮 刘永林 WANG Jia;ZHU Lingli;SHU Lu;GUO Hongzhuang;LIU Yonglin(Development Research Institute of Testing and Certification Technology,Jiangxi General Institute of Testing and Certification,Nanchang Jiangxi 330000,China)
机构地区:[1]江西省检验检测认证总院检测认证技术发展研究院,江西南昌330000
出 处:《江西化工》2025年第2期26-31,共6页Jiangxi Chemical Industry
基 金:江西省检验检测认证总院科研项目(ZYK202214)。
摘 要:镍铬基高温合金中钼、铌、锆、钛的含量对其性能的影响至关重要,准确分析这些元素的含量具有极其重要的现实意义。现行的国家标准多为化学分析方法,存在干扰多、流程长等问题,且目前尚无同时测定钼、铌、锆、钛元素含量的仪器分析方法。基于此,通过盐酸、硝酸和氢氟酸(15+5+0.5)溶解试样,优化仪器参数,分别选择202.031 nm、313.079 nm、339.197 nm、337.279 nm作为钼、铌、锆、钛的分析谱线,确定待测元素不受共存元素和基体的谱线干扰,用内标Y(2.0 mg/L)消除基体的其他干扰,用电感耦合等离子体发射光谱法(ICP-AES)同时测定镍铬基高温合金中的钼、铌、锆、钛的分析方法。各元素的校准曲线线性相关系数r均大于0.9999,方法检出限为0.0002%~0.0021%,定量限为0.0005%~0.0069%。按照实验方法测定镍铬基高温合金中的钼、铌、锆、钛,回收率为90%~110%,相对标准偏差(RSD,n=7)均小于5%;镍铬基高温合金标准物质中钼、铌、锆、钛的测定结果与认定值无显著差异。The influence of molybdenum,niobium,zirconium and titanium on the properties of nickel-chromium based superalloys is very important.Accurate analysis of the content for molybdenum,niobium,zirconium and titanium has great practical significance.The current national standard methods are mostly chemical analysis methods,which have a lot of interference and a long process,and there is no instrument analysis method for simultaneously determining the content of molybdenum,niobium,zirconium and titanium elements.Based on this,dissolve the sample with hydrochloric acid,nitric acid and hydrofluoric acid(15+5+0.5),optimize the instrument parameters,select 202.031 nm,313.079 nm,339.197 nm and 337.279 nm as the analytical spectral lines of molybdenum,niobium,zirconium and titanium,determine that the elements to be tested are not affected by the spectral lines of co-existing elements and matrix,and other matrix interference is eliminated by using internal standard Y(2.0 mg/L),with analytical method for simultaneously testing molybdenum,niobium,zirconium and titanium in nickel-chromium based superalloys by Inductively Coupled Plasma-Atomic Emission Spectrometry(ICPAES).The linear correlation coefficient r of the calibration curve of each element is 0.9999,the detection limit of the method is 0.0002%~0.0021%,and the quantitation limit is 0.0005%~0.0069%.The recoveries of molybdenum,niobium,zirconium and titanium in nickel-based superalloys are 90%~110%and the relative standard deviations(RSD,n=7)are all less than 5%.There is no significant difference between the determination results of molybdenum,niobium,zirconium and titanium in the standard material of nickel-chromium based superalloy and the certified values.
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