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有机化合物中氢的测定方法已很成熟,但其中氘的测定,至今国内未见报导。国外的报导涉及重水体系中氢、氘的测定较多,对有机化合物中氘的测定未见详细资料。为解决有机晶体材料中氘的分析,我们通过反复试验建立了燃烧——分光光度法。方法是将样品中的氢、氘定量的氧化成H_2O和D_2O,再用近红外分光光度法测定其中的氚。关于样品中干扰元素的消除以及析出水的定量收集我们分别采用无水碳酸钠和无水硫酸钠来完成。实验证明无水碳酸钠是一种较好的除氮、除硫剂而无水硫酸钠用作水的吸收剂不仅有利于水的提纯,而且使水更易集中。水经无水碳酸钠、无水硫酸钠的提纯后可完全满足光度法测定的要求。方法用于氘化的硫酸三苷酞(简称DTGS)等材料的分析,都得到了令人满意的结果。
Determination of hydrogen in organic compounds has been very mature, but the deuterium determination, so far no reports. Foreign reports involving heavy water system hydrogen, deuterium determination more, no determination of organic compounds in deuterium for detailed information. To solve the deuterium analysis of organic crystalline materials, we established a combustion-spectrophotometry by trial and error. Method is the sample of hydrogen, deuterium quantitative oxidation of H_2O and D_2O, and then use near-infrared spectrophotometry tritium. About the elimination of interfering elements in the sample and quantitative collection of precipitated water, we used anhydrous sodium carbonate and anhydrous sodium sulfate respectively. Experiments show that anhydrous sodium carbonate is a better nitrogen removal, desulfurization agent and anhydrous sodium sulfate as water absorbent is not only conducive to water purification, but also to make water easier to concentrate. Water by anhydrous sodium carbonate, anhydrous sodium sulfate purification can fully meet the photometric determination of the requirements. Methods The deuterated tributylsulfate (DTGS) and other materials analysis, have been satisfactory results.