摘要
采用熔融玻璃片法制备样品,通过波长色散X射线荧光光谱法测定萤石中氟化钙、二氧化硅、磷、硫的含量,分析了熔剂类型、稀释比、称样量、熔融温度、熔融时间等因素对测定结果的影响,确定了最佳实验条件。同时采用标准样品及自制控制样品进行了各成分工作曲线的绘制,其相关系数均达到0.999以上。精密度实验表明萤石中氟化钙、二氧化硅、磷、硫含量测定结果的相对标准偏差(RSD,n=10)为0.23%~4.80%,准确度实验表明萤石标准样品及湿法化学分析对照样品中氟化钙、二氧化硅、磷、硫含量的测定值与标准值、化学分析值的差值均在GB/T 5195.5—2017、GB/T 5195.6—2006、GB/T 5195.1—2017、GB/T 5195.8—2006方法允许差范围内。与湿法化学分析相比,该方法分析流程短,灵敏度高,具有一定的推广应用价值。
The samples are prepared with fused bead method,contents of calcium fluoride,silicon dioxide,phosphorus and sulfur in fluorite are determined with wavelength dispersion X-ray fluorescence spectrometry as well as effects of such factors as type of flux,dilution ratio,weighing sample,melting temperature and melting time on determination results are analyzed so that optimal experimental conditions are determined.Meanwhile,the working curves of each element are drawn using standard samples and self-made control samples as well as correlation coefficients all reach over 0.999.The precision experiment showed that the relative standard deviation(RSD,n=10)of determination results for contents of calcium fluoride,silicon dioxide,phosphorus and sulfur in fluorite was 0.23%~4.80%,the accuracy experiment showed that the difference values of measured values,standard values and chemical analysis values for contents of calcium fluoride,silicon dioxide,phosphorus and sulfur in standard sample of fluorite and control sample of wet chemical analysis were within the range of allowable deviation for the methods of GB/T 5195.5—2017,GB/T 5195.6—2006,GB/T 5195.1—2017 and GB/T 5195.8—2006.The method is with shorter analysis process,higher sensitivity and certain promotion and application value compared with wet chemical analysis.
作者
郝丽荣
胡月
孙志峰
杨瑞霞
梁艳芳
Hao Lirong;Hu Yue;Sun Zhifeng;Yang Ruixia;Liang Yanfang(Chemical Inspection Center of Inner Mongolia Baotou Steel Union Co.,Ltd.,Baotou 014010,Inner Mongolia Autonomous Region,China)
出处
《包钢科技》
2025年第3期81-85,共5页
Science & Technology of Baotou Steel
关键词
X射线荧光光谱分析
萤石
熔融玻璃片制样
X-ray fluorescence spectrum analysis
fluorite
sample preparation with fused bead
