高分辨电感耦合等离子体质谱法测定高纯镍中25种痕量元素  

Determination of twenty-five trace elements in high purity nickel by high resolution inductively coupled plasma mass spectrometry

作　　者：高颂 张艳 庞晓辉 牛木森 梁钪 陈靖 GAO Song;ZHANG Yan;PANG Xiaohui;NIU Musen;LIANG Kang;CHEN Jing(AECC Beijing Institute of Aeronautical Materials,Beijing 100095,China;Beijing Key Laboratory of Aeronautical Materials Testing and Evaluation,Beijing 100095,China;Beijing Tongzhou District Quality Inspection and Inspection of Agricultural Products,Beijing 101149,China)

机构地区：[1]中国航发北京航空材料研究院,北京100095 [2]航空材料检测与评价北京市重点实验室,北京100095 [3]北京市通州区农产品质量检验检测站,北京101149

出　　处：《冶金分析》2021年第6期35-43,共9页Metallurgical Analysis

摘　　要：镍基高温合金广泛应用于航空发动机的热端部件,其主要原材料高纯镍的纯度对其性能有着重要影响,因此需要测定和控制高纯镍中痕量元素的含量。通过选择合适的同位素克服质谱干扰,选择标准加入法绘制校准曲线克服基体效应,对辅助气流量进行了优化,在高分辨率模式下测定钙和砷,在中分辨率模式下测定其余元素,建立了高分辨电感耦合等离子体质谱法测定高纯镍中镁、铝、磷、钙、锰、铁、铜、锌、镓、锗、砷、硒、银、镉、铟、锡、锑、碲、金、汞、铊、铅、铋、钍、铀共25种痕量元素的方法。在优化的实验条件下,校准曲线线性相关系数均在0.999以上,各元素的方法检出限在0.003~0.15μg/L之间,定量限在0.010~0.50μg/L之间。选择3个高纯镍样品(纯度为99.99%),按实验方法对其中25种痕量元素进行测定,同时对同一高纯镍样品进行不同梯度的加标回收试验,结果表明,测定结果的相对标准偏差(RSD,n=8)为3.5%~9.7%,回收率为90%~110%。采用实验方法测定纯镍标准物质,测定值与标准值基本一致。按照实验方法对高纯镍样品中25种杂质元素进行测定,同时采用辉光放电质谱法进行方法比对,结果表明,两种分析方法测定结果吻合度较高。Nickel-based high temperature alloys were widely used in hot end components of aero-engines.The purity of main raw material(high-purity nickel)had important influence on the properties of alloys.Therefore,the content of trace elements in high-purity nickel should be determined and controlled.Proper isotopes were selected to overcome the mass spectral interference.The calibration curves were prepared by standard addition method to eliminate the matrix effect.The flow rate of auxiliary gas was optimized.The contents of calcium and arsenic were determined at high resolution mode,while the contents of other elements were determined at middle resolution mode.The determination method of 25 trace elements(magnesium,aluminum,phosphorus,calcium,manganese,iron,copper,zinc,gallium,germanium,arsenic,selenium,silver,cadmium,indium,tin,antimony,tellurium,gold,mercury,thallium,lead,bismuth,thorium and uranium)in high-purity nickel by high resolution inductively coupled plasma mass spectrometry was established.Under the optimized experimental conditions,the linear correlation coefficients of calibration curves were all higher than 0.999.The limits of detection of method ranged from 0.003μg/L to 0.15μg/L.The limits of quantification were in range of 0.010-0.50μg/L.The contents of trace elements in three high-purity nickel samples(purity of 99.99%)were determined according to the experimental method.Meanwhile,the recovery test with different gradients was conducted with one high-purity nickel sample.The results showed that relative standard deviations(RSD,n=8)of determination values were between 3.5%and 9.7%.The recoveries were between 90%and 110%.The certified reference material of pure nickel was determined according to the experimental method,and the results were basically consistent with the standard values.The contents of 25 impurity elements in high-purity nickel sample were determined according to the experimental method,and the results were compared with the glow discharge mass spectrometry.It was found that the determi

关 键 词：高分辨电感耦合等离子体质谱法(HR-ICP-MS) 高纯镍 痕量元素 质谱干扰 

分 类 号：O657.63[理学—分析化学]