顾续盛 刘凯 王祥德

【摘要】采用电感耦合等离子体质谱法测定镍基高温合金GH4698中铅、锡、锑、铋。研究了GH4698中主要成分镍、铬对铅、锡、锑、铋含量测定产生的基体效应，考察了质谱干扰、基体、内标元素等因素对铅、锡、锑、铋含量测定的影响。结果表明：在最佳测量条件下，建立工作曲线，其相关系数在0.999以上，样品加标回收率为96.3%～101.9%，精密度RSD小于6%（n=6）。该方法操作简单，准确度较高，可用于镍基高温合金GH4698中铅、锡、锑、铋的测定。

【关键词】电感耦合等离子体质谱法；GH4698；质谱干扰

【DOI编码】10.3969/j.issn.1674-4977.2023.04.027

Determination of Lead， Tin， Antimony and Bismuth in Nickel Base Superalloy GH4698 by Inductively Coupled Plasma Mass Spectrometry

GU Xusheng， LIU Kai， WANG Xiangde

（Guohe General〔Qingdao〕Testing and Evaluation Co.， Ltd.， Qingdao 266042， China）

Abstract： Lead， tin， antimony and bismuth in nickel base superalloy GH4698 were determined by inductively coupled plasma mass spectrometry. The matrix effect of the main components nickel and chromium in GH4698 on the determination of lead， tin， antimony， and bismuth content was studied. The effects of factors such as mass spectrometry interference， matrix， and internal standard elements on the determination of lead， tin， antimony， and bismuth content were investigated. The results showed that under the optimal measurement conditions， a working curve was established with a correlation coefficient above 0.999， a sample recovery rate of 96.3%～ 101.9%， and a precision RSD of less than 6% （n=6）. This method is simple to operate and has high accuracy， and can be used for the determination of lead， tin， antimony， and bismuth in nickel based high-temperature alloy GH4698.

Key words： inductively coupled plasma mass spectrometry； GH4698； mass spectrometry interference

GH4698是Ni-Cr基沉淀硬化型高溫合金，使用温度为750～800℃。该合金是在GH4033合金基础上发展而成的。该合金中温强度高、抗蠕变性能好、塑性较高、组织稳定、成本较低。主要产品有长寿命燃气涡轮转子叶片、导向叶片及其他高温用零部件。铅、锡、锑、铋作为高温合金中的有害杂质元素，会降低材料的整体性能，严重影响GH4698合金的持久强度等力学性能。因此须要严格控制GH4698中铅、锡、锑、铋的含量，准确测定有害杂质元素铅、锡、锑、铋在GH4698合金的含量是极其重要的。由于该合金的组成成分中元素种类极其复杂且相应的元素含量差异较大，从而导致在分析测定其有害杂质元素铅、锡、锑、铋的过程中易受到基体干扰效应的影响，对测定结果的准确性和可靠性产生严重的影响。目前测定高温合金中铅、锡、锑、铋的方法通常有氢化物-原子荧光光谱法、电感耦合等离子体原子发射光谱法、原子吸收光谱法等。以上方法均存在前处理过程复杂、方法的重现性与再现性差、检测周期长、成本高、不能大批量样品检验等问题[1-2]。……