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Modificação no método do Thorin para determinação quantitativa rápida de tório em minérios brasileiros

机译:Thorin方法改进巴西矿石中快速定量钍的测定

摘要

The minerals controlled by CNEN have in its composition, moreover than uranium and thorium, other elements, as rare earths, bismuth, tantalum, niobium and iron. Most of these elements are a great obstacle to the analytical quantitative determination of Thorium, when modern and non-destructive techniques as Energy Dispersive X Ray Fluorescence – EDXRF, cannot be used. The present work is successful in satisfying all the CNEN parameters, and executing the job in a secure and optimized way. Through the planned and studied modifications, executed in well-know and consecrated analytical methods we hit the objective to reduce the total time of the analysis process to 3 hours. The new procedure is also versatile: it can be used in all the brazilian minerals which is responsibility to CNEN such as: ilmenite, anatase, columbite, tantalite, caldasite, zirconite, thorianite, monazite and pirochlorine with the same accurate and fast results although they have diverse chemical compositions. The foremost, modifications included in the process was the fusion with ammonium and potassium bifluorides, promoting the quantitative precipitation of thorium and allowing it's separation from uranium. So, the slowly step of precipitation with oxalate used in former processes can be eliminated. The results of the separation can be confirmed by FRX analysis. After, the thorium is separated from the rare-earth using mesytilium oxide. The thorium quantifying can be done just after, by epectrophotometry in 545 nm using thorin in a 0,24 mol L-1 HCl medium. The methodology developed and presented in this writing was compared with the classic method using the statistical test of the t pair used in the determination of Th in certified material of reference (monazite), not having been found difference between the two methodologies. The new methodology also was applied to some ores with values of concentration of Th certified presenting compatible agreement enters the results for a reliable level of 95%.
机译:CNEN所控制的矿物除了铀,or之外,还具有稀土,铋,钽,铌和铁等其他元素。当不能使用诸如能量分散X射线荧光– EDXRF的现代无损技术时,这些元素中的大多数是对Thor的定量分析的巨大障碍。当前的工作成功地满足了所有CNEN参数,并以安全和优化的方式执行了作业。通过计划和研究的修改,以熟知的和奉献的分析方法执行,我们实现了将分析过程的总时间减少到3小时的目标。新程序还具有多种用途:它可以用于对CNEN负责的所有巴西矿物中,例如:钛铁矿,锐钛矿,哥伦比,钽铁矿,钙铁矿,锆石,菱锰矿,独居石和四氯化碳,尽管它们具有相同的准确和快速的结果。具有多种化学成分该过程中最重要的修改是与铵和氟化氢钾融合,促进了the的定量沉淀并使其与铀分离。因此,可以消除以前工艺中使用草酸盐沉淀的缓慢步骤。分离结果可以通过FRX分析确认。之后,使用氧化sy将the与稀土分离。 after的定量可以立即进行,在0,24 mol L-1 HCl介质中,使用thorin在545 nm下进行分光光度法。本文中开发和介绍的方法与经典方法进行了比较,使用的是t对的统计检验,该方法用于确定参考物质(独居石)中Th的含量,尚未发现两种方法之间的差异。新方法也被应用于某些矿石,这些矿石的Th认证浓度值表示兼容,可以使结果达到95%的可靠水平。

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