电感耦合等离子体串联质谱法测定高温合金中痕量砷  

Determination of trace arsenic in superalloys by inductively coupled plasma tandem mass spectrometry

作　　者：郭红巧 胡净宇[1,2] 侯艳霞 齐荣[2] 刘晓波 GUO Hongqiao;HU Jingyu;HOU Yanxia;QI Rong;LIU Xiaobo(Central Iron&Steel Research Institute,Beijing 100081,China;NCS Testing Technology Co.,Ltd.,Beijing 100081,China)

机构地区：[1]钢铁研究总院,北京100081 [2]钢研纳克检测技术股份有限公司,北京100081

出　　处：《冶金分析》2021年第5期35-40,共6页Metallurgical Analysis

基　　金：钢研纳克检测技术股份有限公司自立研发项目基金(ZNCS160)。

摘　　要：高温合金中Co含量较高,采用电感耦合等离子体质谱(ICP-MS)测定高温合金中As时,^(59)Co^(16)O^(+)会严重干扰As的分析,这一直是ICP-MS测定高温合金中痕量As的研究难点。在串联四极杆(MS/MS)模式下向碰撞/反应池内通入O_(2),设置一级质量过滤器(Q1)m/z=75,^(75)As+可以与O_(2)反应生成^(75)As^(16)O^(+),而干扰离子不能与O_(2)发生反应,将二级质量过滤器(Q2)设置为m/z=91,仅^(75)As^(16)O^(+)通过并被检测器检测,从而避免了^(59)Co^(16)O^(+)的质谱干扰。据此,建立了电感耦合等离子体串联质谱法(ICP-MS/MS)测定高温合金中痕量As的方法。采用As质量浓度为1.000ng/mL、Co质量浓度为1.000~1000μg/mL的系列标准溶液考察了单四极杆和MS/MS两种模式下Co对As测定的质谱干扰。结果表明,在MS/MS模式下,As的回收率均在100%左右,这说明在MS/MS质量转移模式下,采用O_(2)为反应气,通过两次质量选择,可以成功消除Co基体带来的严重干扰。对O_(2)流速进行了优化,选择O_(2)流速为0.375mL/min。方法线性范围为1.00~100ng/mL,线性相关系数为1.0000,检出限为0.0067μg/g,定量限为0.023μg/g。选择纯钴标准样品为测定对象,按照实验方法对其中As进行测定,并进行加标回收试验,回收率在96%~102%之间。采用所建立的方法对镍基高温合金标准物质和高温合金样品中As进行测定,测定结果分别与认定值或原子荧光光谱法测定值基本一致,实际样品测定结果的相对标准偏差(RSD,n=6)为1.6%~2.8%。The content of Co in superalloys is relatively high.During the determination of As in superalloys by inductively coupled plasma mass spectrometry(ICP-MS),the analysis of As will be seriously interfered by^(59)Co^(16)O^(+),which is always a research difficulty in the determination of trace As in superalloys by ICP-MS.O_(2)was introduced to the collision/reaction cell at tandem quadrupole(MS/MS)mode,and the firstlevel mass filter(Q1)was set to m/z=75.^(75)As+could react with O_(2)to generate^(75)As^(16)O^(+),while the interfering ions could not react with O_(2).The secondary mass filter(Q2)was set to m/z=91.Only^(75)As^(16)O^(+)passed through and was detected by the detector,thus avoiding the mass spectrum interference of^(59)Co^(16)O^(+).Based on this,a new method for the determination of trace As in superalloys by inductively coupled plasma tandem mass spectrometry(ICP-MS/MS)was established.A series of standard solutions with1.000ng/mL As and 1.000-1000μg/mL Co were used to investigate the mass spectrum interference of Co to As in the two modes,i.e.,single quadrupole and tandem quadrupole(MS/MS).The results showed that the recoveries of As were all about 100%at MS/MS mode.It indicated that the serious interference caused by Co could be eliminated successfully through two mass selections at MS/MS mass transfer mode,where O_(2)was used as the reactant gas.The flow rate of O_(2)was optimized,and 0.375mL/min was finally selected.The linear range of the method was 1.00-100ng/mL with the linear correlation coefficient of1.0000.The limit of detection and the limit of quantification was 0.0067μg/g and 0.023μg/g,respectively.The content of As in pure cobalt standard sample was determined according to the experimental method.Meanwhile,the standard addition recovery test was carried out.The recoveries were between96%and 102%.The established method was applied to determine As in nickel-based superalloy reference materials and superalloy samples.The found results were basically consistent with the certified values or those

关 键 词：电感耦合等离子体质谱(ICP-MS) 串联四极杆(MS/MS) 质量转移模式 高温合金 痕量砷 

分 类 号：O657.63[理学—分析化学] TF125.12[理学—化学]