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磷酸二氘钾是目前激光技术上应用很广的一种电光调制晶体。晶体中的氘含量对其性能影响很大,因此准确的测定其氘含量是一项很重要的工作。关于此类晶体中氘含量的分析,国外文献虽有报导但材料较少,国内尚未见有关报导。为配合晶体的研制,我们用干涉法、分光光度法测定过晶体中的氘含量。但用这些方法分析,条件要求比较高,必须有恒温恒湿的设备以及一套热分解和冷冻收集水的装置。还得有专门的测试仪器,同时还要用纯的重水作标准样品。为简化分析手续且能在一般的条件下进行测定,我们对磷酸二氘钾热分解的反应式作了进一步的分析,既然热分解反应生成水的氘化度与样品的氘化度一样,而生成氘化的水与生成的偏磷酸钾之间又有一定的化学计量关系,那么能否根据这种关系通过更简单的途径测定其中的氘,经反复实验最后终于建立了一种新的氘含量测定法——重量法。本文建立的方法用简单的重量法解决了一个现代工业分析问题,这对于此类材料的分析是有一定实用意义的。方法比较简便、准确、经济且便于推广使用。经分析大量样品的实践证明方法是行之有效的,分析的结果是令人满意的。
Potassium dideuterium phosphate is currently laser technology is widely used in a kind of electro-optical modulation crystal. The deuterium content in the crystal has a great influence on its performance, so accurate determination of its deuterium content is a very important task. On the analysis of deuterium content in such crystals, although foreign literature has been reported but less material, no reports have been reported in China. In line with the development of the crystal, we used interferometry, spectrophotometry to determine the amount of deuterium in the crystal. However, the analysis of these methods, the conditions require relatively high, there must be constant temperature and humidity equipment and a set of thermal decomposition and freezing water collection device. Have to have a special test equipment, but also with pure heavy water as a standard sample. In order to simplify the analysis procedure and make the determination under normal conditions, we further analyze the thermal decomposition reaction of potassium dideuterium phosphate. Since the degree of deuteration of the water produced by the thermal decomposition reaction is the same as the deuteration degree of the sample, Deuterium generated water generated potassium metaphosphate and there is a certain relationship between the stoichiometry, then according to this relationship through a more simple way to determine the deuterium, after repeated experiments and finally established a new deuterium Assay - Gravimetric method. The method established in this paper solves a modern industrial analysis problem with a simple gravimetric method, which has some practical implications for the analysis of such materials. Method is simple, accurate, economical and easy to promote the use. The analysis of a large number of samples proved that the method is effective and the result of the analysis is satisfactory.