摘要
通过熔融制样低温预处理技术和高温熔融制样,建立了X射线荧光光谱法测定成分复杂的水渣铁粒、富集磁粉、氧化铁皮等返生产利用资源中的主次成分的工作曲线,探讨了不同氧化剂、熔融温度、熔融时间对检测结果的影响,解决了部分试样中金属颗粒物腐蚀铂金坩埚的难题,实现了对返生产利用资源中的全铁、S、SiO_2、Al_2O_3、CaO、MgO等元素的快速检测.试验采用(1∶14)的试样熔剂稀释比,采用氧化钴作内标,在1 020℃熔融处理试样,样品熔解完全,且对铂金坩埚无明显腐蚀.试验结果表明,采用熔融法制样-X射线荧光光谱法测定返生产利用资源样品,有效消除了基体效应和粒度效应对检测结果的影响,具有良好的精密度和准确度,已经应用于生产检测.
The working curve by X ray fluorescence spectrometry determination has been established through the samples prepared by fusing pretreatment at low temperature and fusing at high temperature,which can measure the major and minor components of complex composition of slag iron particles,enrichment of magnetic powder,iron oxide scale etc. for the recycled resources. The effect of different oxidants,melting temperature,and melting time is discussed in order to solve the problem of corrosion of metal particles in the platinum crucible part of the sample for having the ability to determine the total iron,S,SiO_2,Al_2O_3,CaO,MgO and other elements contained in the recycled resources rapidly. The flux dilution ratio of the sample( 1: 14) was used for the tests,and the cobalt oxide was used as the internal standard reference. The samples were melted at 1020 ℃,and the samples were completely melted. The results show that the determination of production resource utilization by returned sample melting method-X ray fluorescence spectrometry,it can effectively eliminate the matrix effect and the effect of particle size on the results with good precision and accuracy,and has been applied in production.
引文
[1]罗学辉,陈占生,陈雪,等.X射线荧光光谱法测定铁矿石中主次成分[J].黄金科学技术,2010,18(5):123-124.
[2]崔黎黎.X射线荧光光谱法测定铁矿石中主次成分[J].冶金分析.2009,29(12):21-24.
[3]许鸿英,张继丽,张艳萍,等.X射线荧光光谱分析多矿源铁矿石中9种成分[J].冶金分析,2009,29(10):24-27.
[4]程进.钴内标玻璃熔片X射线荧光光谱法分析铁矿石中的主、次元素[J].福建分析测试,2009,18(1):46-49.
[5]杨新能,谢冲明.X射线荧光光谱法测定铁矿石中化学成分[J].云南冶金,2008,37(6):58-64.
[6]罗学辉,张勇,艾晓军,等.熔融玻璃片-波长色散X射线荧光光谱法测定铁矿石中全铁及其它多种元素的分析进展[J].中国无机分析化学,2011,1(3):23-26.
[7]王一凌,曲月华,邓军华.X射线荧光光谱分析法熔融制样技术的探讨与应用[J].冶金分析,2010,30(12):10-13.
[8]程志中,顾铁新,范永贵,等.九个铁矿石标准物质研制[J].岩矿测试,2010(3):305-308.
[9]邢文青,吴超超,王岩,等.X射线荧光熔融法测定锰系合金中硅、锰和磷含量[J].南方金属,2016(3):8-10.