氢还原重量法测定铼酸铵制备铼粉产品中铼

发布时间：2018-05-13 12:52

  本文选题：铼粉 + 铼　； 参考：《冶金分析》2017年07期

【摘要】：通过先测定铼粉产品中杂质元素总含量,再用差减法计算铼含量的方法较为繁琐。根据低温氢还原时,除了铼氧化物Re_2O_7、ReO_2,共存金属杂质元素和他们的氧化物均被还原为金属单质而不挥发外,其余非金属元素和他们的氧化物,以及水分、铵盐均会被挥发除去这一基本原理,实验提出了采用低温氢还原样品,以氢还原前后样品质量之比计算铼的含量,最终实现了氢还原重量法测定铼酸铵制备铼粉中铼的方法。确定的实验条件如下:样品量约1.0g;采用分段升温方式进行氢还原,其程序为先室温升温至200℃,恒温30min后升温至400℃,接着恒温30min后升温至600℃,最后再恒温30min;将盛有氢还原后铼粉的石英舟置于干燥器中冷却30min,恒重1次。实验方法适用于铼粉中不挥发杂质元素总质量分数不大于0.010%时铼的测定。将实验方法用于3个铼粉管理样品、4个铼粉实际样品中99.824%~99.995%铼的测定,测定值与参考值基本一致,相对标准偏差(n=9~22)为0.001 2%~0.003 3%,加标回收率99.99%~100.01%。
[Abstract]:The method of determining the total content of impurity elements in rhenium powder and then calculating the content of rhenium by subtraction method is more complicated. According to the low temperature hydrogen reduction, in addition to the rhenium oxide Re2O7 / ReO _ 2, the metal impurity elements and their oxides are reduced to metallic elements without volatilization, the rest of the non-metallic elements and their oxides, as well as water, Based on the principle that ammonium salts can be removed by volatilization, a new method for the determination of rhenium in rhenium powder by hydrogen reduction gravimetric method is proposed, in which the samples are reduced by hydrogen at low temperature and the mass ratio of samples before and after hydrogen reduction is used to calculate the content of rhenium. The experimental conditions are as follows: sample quantity is about 1.0 g, hydrogen reduction is carried out by means of stepwise heating, which is programmed to increase temperature to 200 鈩，

本文编号：1883223