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作 者:马晓敏 杨军红 李茂 MA Xiaomin;YANG Junhong;LI Mao(Xi’an Hantang Analysis and Testing Co.,Ltd.,Xi’an 710201,China)
机构地区:[1]西安汉唐分析检测有限公司,陕西西安710201
出 处:《中国测试》2024年第9期143-149,共7页China Measurement & Test
基 金:科技开放共享平台(2021PT-024,2017KTPT-08)。
摘 要:作为高品质钛合金制造时的关键原料,钒铝中间合金中的痕量杂质金属元素的含量会对钛合金的使用性能产生重要影响。该文采用盐酸-硝酸混酸体系溶解样品,优化电感耦合等离子体质谱仪的工作参数,选择各待测元素的同位素,用钪、铥内标校正非质谱干扰,建立氧气反应模式-电感耦合等离子体质谱法测定钒铝中间合金中砷、镉、铬、铜、镁、锰、镍、铅、硼、钼、铌、磷、钽、钨、锆、钇、锡、汞18种痕量杂质元素的方法。其中砷元素采用氧气-反应池技术(O_(2)-DRC)在氧气流量为0.5 mL/min条件下对质谱干扰进行消除。18种待测元素测定结果的相对标准偏差(RSD,n=7)均小于3.2%,加标回收率92.7%~109.2%。As the key raw material of high-quality titanium alloy,the quality of vanadium aluminum master alloy has an important impact on the performance of titanium alloy.In this paper,the mixed hydrochloric acid nitric acid system was used to dissolve the sample,and the working parameters of the inductively coupled plasma mass spectrometer were also optimized.Then the isotopes of the elements to be measured were selected,and the internal standard of scandium and thulium was used to correct the non-mass spectrum interference.Finally,the oxygen reaction mode inductively coupled plasma mass spectrometry were established for the determination 18 kind impurity elements in the vanadium aluminum master alloy,including arsenic,cadmium,chromium,copper,magnesium,manganese,nickel,lead,boron,molybdenum,niobium,phosphorus,tantalum,tungsten,zirconium,yttrium,tin and mercury.The testing result indicated that the arsenic element uses the oxygen reaction cell technology(O2-DRC)to eliminate the mass spectrum interference at the oxygen flow rate of 0.5 mL/min and the relative standard deviations(RSD,n=7)of the determination results of 18 elements to be determined were all less than 3.2%,and the recoveries were 92.7%-109.2%.
关 键 词:反应池技术 电感耦合等离子体质谱法(ICP-MS) 钒铝中间合金 杂质元素
分 类 号:TB9[一般工业技术—计量学]
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