电感耦合等离子体串联质谱法测定高温合金中痕量磷和硫  

Determination of trace phosphorus and sulfur 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11期1-7,共7页Metallurgical Analysis

基　　金：钢研纳克自立研发项目基金(ZNCS160)。

摘　　要：采用电感耦合等离子体质谱法测定高温合金中痕量P和S时会受到严重的质谱干扰从而影响测定结果。采用王水-氢氟酸溶解样品,在串联四极杆(MS/MS)模式下,先分别设置一级质量过滤器(Q1)的质荷比(m/z)为31和32,接着向碰撞/反应池内通入O_(2),^(31)P^(+)和^(32)S^(+)会与O_(2)反应生成^(31)P^(16)O^(+)和^(32)S^(16)O^(+),而干扰离子不能与O_(2)发生反应,设置二级质量过滤器的质荷比分别为47和48,使得^(31)P^(16)O^(+)和^(32)S^(16)O^(+)通过并被检测器检测,从而避免了质谱干扰。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P和S的方法。对O_(2)流速进行了优化,选择O_(2)流速为0.375 mL/min。方法线性范围为1.00~100μg/L,线性相关系数不小于0.9997,P和S的检出限分别为0.075μg/g和0.086μg/g,定量限分别为0.23μg/g和0.26μg/g。选择高纯镍标准样品为测定对象,按照实验方法对其中P和S进行测定,并进行空白加标回收试验,回收率在96%~109%之间。采用所建立的实验方法对高温合金标准物质和高温合金样品中P和S进行测定,测定结果分别与认定值、电感耦合等离子体原子发射光谱法或高频燃烧红外吸收法测定值基本一致,实际样品测定结果的相对标准偏差(RSD,n=6)为2.0%~4.7%。There is serious mass spectrometry interference during the determination of trace P and S in superalloys by inductively coupled plasma mass spectrometry,thus affecting the determination results.The sample was dissolved with aqua regia-hydrofluoric acid.The mass-to-charge ratio(m/z)of the first-order mass filter(Q1)were set as 31 and 32 at the mode of tandem quadrupole(MS/MS),respectively.Then O_(2) was injected into collision/reaction cell.^(31)P^(+) and ^(32)S^(+) would react with O_(2) to generate ^(31)P^(16)O^(+) and ^(32)S^(16)O^(+),while the interfering ions could not react with O_(2).The m/z of the second-order mass filter(Q2)were set as 47 and 48,respectively.Therefore,only ^(31)P^(16)O^(+) and ^(32)S^(16)O^(+) were passed and detected by the detector,which avoided the mass spectrometry interference.Accordingly,the method for the determination of trace P and S in superalloys by inductively coupled plasma tandem mass spectrometry(ICP-MS/MS)was established.The flow rate of O_(2) was optimized to be 0.375 mL/min.The linear range of the method was 1.00-100μg/L,and the linear correlation coefficients were not less than 0.9997.The limit of detection for P and S was 0.075μg/g and 0.086μg/g,and the limit of quantification was 0.23μg/g and 0.26μg/g,respectively.The certified reference material of high-purity nickel was selected as the determination object,and the contents of P and S were determined according to the experimental method.Meanwhile,the spiked recovery tests of blank were conducted.The recoveries were between 96% and 109%.The established method was applied to the determination of P and S in superalloy certified reference materials and superalloy samples,and the found results were basically consistent with the certified values and those obtained by inductively coupled plasma atomic emission spectrometry or high frequency combustion infrared absorption method.The relative standard deviations(RSD,n=6)of the determination results of actual sample were between 2.0% and 4.7%.

关 键 词：电感耦合等离子体串联质谱法(ICP-MS/MS) 质量转移模式 高温合金 磷 硫 

分 类 号：O657.63[理学—分析化学] TF033[理学—化学]