电感耦合等离子体原子发射光谱法测定硼钛复合材料中硼

硼钛复合材料中硼含量多少关系到增强相(BTi)占比,直接影响硼钛复合材料各项机械性能。故硼测定结果对硼钛复合材料研究有重要意义。实验提出采用硫酸(1+1)分解样品,选择B 208.890nm作为分析线,采用基体匹配法绘制校准曲线消除基体效应的影响,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定硼钛复合材料中硼。通过条件试验优化仪器的工作条件为发生器功率1.2kW和雾化气压力0.23MPa。硼质量浓度在5.00~50.0μg/mL范围内与其发射强度呈线性关系,线性相关系数大于0.999;方法检出限为0.00045%,测定下限为0.0015%。按照实验方法分别测定5种硼钛复合材料中硼,其结果的相对标准偏差(RSD,n=11)为0.44%~0.68%,加标回收率为94%~103%。

Determination of boron in boron-titanium composite material by inductively coupled plasma atomic emission spectrometry

The content of boron in boron-titanium composite material concerns the proportion of reinforcement phase (BTi), which directly influences on the mechanical properties of boron-titanium composite material. Therefore, the determination of boron has important significance on the research of boron-titanium composite material.The sample was decomposed by sulfuric acid (1∶1). B 208.890nm was selected as the analytical line. The calibration curve was prepared by matrix matching method to eliminate the influence of matrix effect. Consequently, the content of boron in boron-titanium composite material was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The working conditions of instrument were optimized by conditional tests and listed as below: the radio frequency power of generator was 1.2kW and the atomization gas pressure was 0.23MPa. The mass concentration of boron in range of 5.00-50.0μg/mL was linear to the corresponding emission intensity. The linear correlation coefficient was higher than 0.999. The detection limit of method was 0.00045%, and the low limit of determination was 0.0015%. The content of boron in five kinds of boron-titanium composite material was determined according to the experimental method. The relative standard deviations (RSD, n=11) of determination results were between 0.44% and 0.68%. The recoveries were between 94% and 103%.