无机盐工业
主管:中海油天津化工研究设计院有限公司
主办:中海油天津化工研究设计院有限公司
   中海油炼油化工科学研究院(北京)有限公司
   中国化工学会无机酸碱盐专业委员会
ISSN 1006-4990 CN 12-1069/TQ

无机盐工业 ›› 2016, Vol. 48 ›› Issue (4): 72-.

• 论文 • 上一篇    下一篇

X射线荧光光谱法测定 白炭黑中主、次、微量成分

钟坚海1,陈金凤1,张奇勋1,谭玉泉2,陈章捷1,张艳燕1,刘明健1,林亚妹1   

  1. 1.龙岩出入境检验检疫局,福建龙岩 364000;2.福建正盛无机材料股份有限公司
  • 出版日期:2016-04-10 发布日期:2016-04-27

Determination of major,minor,and micro components in white carbon black by X-ray fluorescence spectrometry

Zhong Jianhai1,Chen Jinfeng1,Zhang Qixun1,Tan Yuquan2,Chen Zhangjie1, Zhang Yanyan1,Liu Mingjian1,Lin Yamei1   

  1. 1.Longyan Entry-Exit Inspection and Quarantine Bureau of P.R.C,Longyan 364000,China;
    2.Fujian Zhengsheng Inorganic Materials Co.,Ltd.
  • Published:2016-04-10 Online:2016-04-27

摘要: 采用偏硼酸锂熔融制样的方法,建立了白炭黑中二氧化硅、三氧化二铝、氧化钠、氧化钾、三氧化二铁、氧化钙、氧化镁、二氧化钛、氧化锰的X射线荧光光谱分析方法。熔融实验结果表明,以碘化铵作为脱模剂,熔剂和样品质量比为5∶1,在1 100 ℃下熔融10 min可得到较好的熔样效果。选用与白炭黑基体类似的硅质砂岩标准物质,同时将其与光谱纯二氧化硅按不同比例混合配制成组分含量有一定梯度的校准样品,有效地解决了白炭黑XRF测定的校准样品缺失的问题,并采用变化的理论α影响系数法对基体效应进行了考察。精密度实验结果表明,各组分的相对标准偏差(RSD,n=11)在0.33%~7.71%。用本方法对实际样品中上述成分进行测定,与湿法化学分析法结果一致。

关键词: 熔融制样, X射线荧光光谱法, 白炭黑, 主、次、微量成分

Abstract: A X-ray fluorescence spectrometry for the determination of SiO2,Al2O3,Na2O,K2O,Fe2O3,CaO,MgO,TiO2,and MnO in white carbon black by fusion sample preparation with lithium metaborate(LiBO2) as fusing agent was established.It was showed that the glass bead obtained was optimal when the sample was fused at 1 100 ℃ for 10 min with the sample to fusing agent mass ratio of 1∶5 and ammonium iodide(NH4I) as release agent.The siliceous sandstone with similar matrix to white carbon black was adopted as standard sample,and a series of calibration sample with gradient content was prepared by mixing the standard sample and silicon dioxide with spectroscopically pure in different ratios,and the matrix effect was investigated by variable theoretical α-influence coefficient method.The precision test demonstrated that the relative standard deviations(RSD,n=11) of components were 0.33%~7.71%.By analyzing the actual sample,it was found that the results were consistent with those of chemical analysis methods.

Key words: fusion sample preparation;X-ray fluorescence spectrometry;white carbon black;major, minor, and micro components

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