氢化物发生电感耦合等离子体发射光谱法测定钢中微量砷  

Determination of trace arsenic in steel by hydride generation inductively coupled plasma emission spectrometry

作　　者：刘攀[1,2] 李治亚 杜米芳[1] 高灵清[1,3] 李景滨[1] LIU Pan;LI Zhiya;DU Mifang;GAO Lingqing;LI Jingbin(Luoyang Ship Material Research Institute,Luoyang 471023,China;National New Material Production and Application Demonstration Platform(Advanced Marine Engineering and High-tech Ship Materials),Luoyang 471023,China;Henan Key Laboratory of Technology and Application of Structural Materials for Ship and Marine Equipment,Luoyang 471023,China)

机构地区：[1]中国船舶重工集团公司第七二五研究所(洛阳船舶材料研究所),河南洛阳471023 [2]国家新材料生产应用示范平台(先进海工与高技术船舶材料),河南洛阳471023 [3]河南省船舶及海工装备结构材料技术与应用重点实验室,河南洛阳471023

出　　处：《中国测试》2021年第1期76-81,95,共7页China Measurement & Test

基　　金：国家新材料生产应用示范平台建设项目(TC180A6MR/2)。

摘　　要：该文研究氢化物发生-电感耦合等离子体发射光谱法测定非合金钢(碳素钢)和低合金钢中微量砷的分析方法,考察高频功率、雾化压力、辅助气流量、泵速等仪器工作条件与消解用酸及用量、硼氢化钠浓度对光谱强度的影响,并讨论王水、铁基体、共存离子对测定结果的背景干扰与消除方法。确定的最佳工作条件为:高频功率为1 350 W,雾化压力为22 psi(1 psi=6.895 kPa),辅助气流量为0.5 L/min,泵速为100 r/min。称取0.500 g试样,采用15 mL盐酸和5 mL硝酸加热消解制备待测试液,并加入硫脲—抗坏血酸混合溶液做掩蔽剂。将待测溶液和硼氢化钠溶液(2%)导入氢化物发生器和电感耦合等离子体发射光谱仪,选用As 189.04 nm分析谱线,采用基体匹配法消除背景干扰,以铁基体溶液建立系列校准曲线,其线性相关系数达0.999。方法的定量限为0.000 12%。按实验方法测定钢铁合成样品与有证标准样品,测定结果与理论值或认定值相符。Working conditions of the inductively coupled plasma-emission spectrometer for determination of trace arsenic in non-alloy steel(carbon steel) and low-alloy steel were optimized, such as high-frequency power, atomization pressure, auxiliary gas flow and pump speed. The effect of digestion acid, sodium borohydride, and the background interference of aqua regia, iron matrix and coexisting ions on the measurement results were studied. The optimal conditions were as follows: high-frequency power of 1 350 W, atomization pressure of 22 psi, auxiliary gas flow of 0.5 L/min, and pump speed of 100 r/min. The sample solution was prepared with 0.500 g steel sample, dissolved by 15 mL hydrochloric acid and 5 mL nitric acid. Then the solution, containing thiourea-ascorbic acid mixed solution, and sodium borohydride solution(2%) were introduced into hydride generator and inductively coupled plasma emission spectrometer to be measured, with the analysis line of As 189.04 nm. The matrix matching method was used to eliminate background interference,and a calibration curve was established with a series of iron matrix solutions. The linear correlation was 0.999.The limit of quantification was 0.000 12%. Synthetic samples and standard samples were determined, and the results were consistent with the theoretical or certified values.

关 键 词：氢化物发生 电感耦合等离子体 发射光谱法 非合金钢 碳素钢 砷 

分 类 号：O657.31[理学—分析化学] TG115.33[理学—化学]