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本文研究了利用磷钼酸晶体与浓硝酸铵直接作用,制备的大颗粒(大于80筛目)磷钼酸铵(简称 AMP),对于卤水低含量(10~(-4)%以下)铷、铯的分离和富集以及4-仲-丁基-2(α-甲苄基)酚(简称 BAMBP)萃取的条件。实验证明:AMP 采用磷钼酸与浓硝酸铵直接作用的制备方法,具有简单、快速、颗粒大、透水性好等优点。在柱上交换条件下,铷和铯的吸附量分别为0.2和0.5毫克当量/克。其分配系数分别为:钾0.11、铷21.2、铯>2000。用于组分复杂的卤水以及矿物中铷和铯的分离、富集是一个比较好的交换剂。试验还证明:不用硝酸铵溶液洗脱,仅在试样中预先加入定量的硝酸铵和硝酸混合溶液,可直接将大量的钾、镁等元素分离而铷和铯得到满意的富集。富集了的铷、铯,用碱溶的方法进行溶解,然后采用4-仲-丁基-2(α-甲苄基)酚萃取,原子吸收法测定。为了使整个分析方法更加简化,将一般的交换柱改用经过改制的25毫升梨形分液漏斗,可使交换、分离、碱溶,萃取均在一个容器中进行,试验证明,这个方法是可行的。经过以上几个方面的研究和探讨,解决了 AMP 所存在的缺点,使 AMP 用于分析上的分离更加快速,广泛。从而使一个繁杂、冗长的铷、铯分析,变成了简单,快速,应用较为广泛的分析方法。方法的标准偏差为±0.25。
In this paper, ammonium phosphomolybdate (AMP for large size) (larger than 80 mesh) prepared by direct interaction between phosphomolybdic acid crystals and concentrated ammonium nitrate and rubidium for low content of brine (10-4%) were studied. Separation and enrichment of cesium and extraction of 4-sec-butyl-2 (α-methylbenzyl) phenol (BAMBP). Experiments show that: AMP using phosphomolybdate and concentrated ammonium nitrate direct effect of preparation, with simple, fast, large particles, good water permeability and so on. The adsorption of rubidium and cesium on column exchange was 0.2 and 0.5 meq / g, respectively. The distribution coefficients were: potassium 0.11, rubidium 21.2, cesium> 2000. For the complex components of brine and minerals in the separation of rubidium and cesium, enrichment is a better exchange agent. The test also proves that: without the ammonium nitrate solution elution, only the quantitative sample of ammonium nitrate and nitric acid mixed solution can be directly separated a large number of potassium, magnesium and other elements and rubidium and cesium obtained satisfactory enrichment. The enriched rubidium and cesium are dissolved in an alkaline solution and then extracted with 4-sec-butyl-2 (α-methylbenzyl) phenol and determined by atomic absorption spectrometry. In order to simplify the whole analysis method, the common exchange column was switched to a modified 25 ml pear-shaped separating funnel to exchange, separate, dissolve and extract in a container. The experiment proved that this method is feasible of. After the above several aspects of research and discussion, to solve the shortcomings of the existence of AMP, AMP for the separation of the analysis more quickly and widely. So that a complicated, lengthy rubidium, cesium analysis, into a simple, fast, widely used analytical methods. The standard deviation of the method is ± 0.25.