超轻水中氘含量的气相色谱分析

Determination of Deuterium Content of Deuterium Depleted Water by Gas Chromatography

  • 摘要: 通过实验研究建立了测定超轻水中氘含量的气相色谱分析方法。用金属镁在500 ℃高温下将超轻水分解为气体,然后在常温下以高纯H2为载气,5A分子筛作为色谱柱,进行超轻水中氘含量的检测。用金属镁法分解水样,避免了传统铀法可能带来的放射性危害,且同位素效应远小于金属锌法。采用色谱在常温下检测氢气中氘的含量,也克服了普遍采用液氮低温法操作复杂,且H2、HD和D2的校正因子难以测定的缺点。研究结果表明,以极低重水标准样绘制的HD峰面积与对应氘含量的标准曲线能反向延长到天然丰度以下,能用于不同氘含量的超轻水样品检测。该分析方法精密度高,同一样品经多次分解进样,检测的相对标准偏差<5%,在3个添加水平下的回收率为96.6%~99.9%,合成相对不确定度为0.166。测量结果精密度和准确度较高,完全能满足超轻水生产过程中氘含量定量分析的要求。

     

    Abstract: An applicable deuterium analysis method of deuterium depleted water was experimentally studied by used H2 carrier and the chromatogram columniation with 5A molecular sieve at natural temperature after decompounding the deuterium depleted water by magnesium at 500 ℃. Decompounding the water using the magnesium instead of uranium can avoid the radioactive danger and the isotope effect was smaller than zinc. Determination by chromatograph at natural temperature can overcome the operation complexity at liquid nitrogen and the difficulty of determining the emend factor of the H2, HD, D2. The results showed that standard curved using standard sample of super low heavy water can reversely extend to below the natural deuterium abundance,deuterium content of deuterium depleted water can be calculated. The relative standard deviation of the method<5%, recovery rate with added specimen with three addition level was 96.6%-99.9%, the combined relative uncertainty was 0.166. It can meet the need of quantitative analysis during the deuterium depleted water manufacturing.

     

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