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氢同位素核自旋异构体正-仲态比例影响氢同位素的低温物性,有必要对其比例进行测定。本文利用活性三氧化二铝多孔层开管(Porous Layer Open Tubular,PLOT)柱实现了正-仲氢同位素(氕、氘)的基线分离,发展了一种可在液氮温度下测定同核分子正-仲态比例的色谱分析技术。研究结果表明,与传统三氧化二铝填充柱相比,高效PLOT柱实现了正、仲氕(o-H_2、p-H_2)以及正、仲氘(o-D2、p-D2)的基线分离(分离度R_s大于1.5),当流量为5 m L·min-1时,分离度R_s(p-H_2,o-H_2)=6.9,R_s(o-D2,p-D2)=1.8。正仲态分离度与进样量、流量均有关系。根据峰面积的积分结果,常温(298 K)下正、仲氕比例为2.77:1,正、仲氘比例为1.78:1,与理论测算值基本符合。HD与o-H_2实现了部分分离,R_s(o-H_2,HD)=0.5,根据理论预测,实现HD与o-H_2的基线分离(R_s达到1.5),理论塔板数需要达到3.9×105。
Hydrogen isotope nuclear spin isomers of normal - s-phase ratio affect the low-temperature hydrogen isotope physical properties, it is necessary to determine the ratio. In this paper, baseline separation of n- and para-hydrogen isotopes (氕 and deuterium) was achieved by using Porous Layer Open Tubular (PLOT) columns. A new method was developed for the determination of homonuclear molecules Chromatographic analysis of positive - midrange ratio. The results show that compared with the conventional alumina packed column, the baseline of the positive, middlecrinose (o-H_2, p-H_2) and normal and secondary deuterium (o-D2, p-D2) (Resolution R_s greater than 1.5), the resolution R_s (p-H_2, o-H_2) = 6.9 and R_s (o-D2, p-D2) = 1.8 when the flow rate is 5 m L · min-1. Positive secondary state of separation and injection volume, flow are related. According to the result of integral of peak area, the ratio of positive and secondary 氕 at normal temperature (298 K) is 2.77: 1, and the ratio of positive and secondary deuterium is 1.78: 1, which is in good agreement with the theoretical value. HD and o-H 2 are partially separated with R_s (o-H 2, HD) = 0.5. According to the theoretical prediction, the baseline separation of HD and o-H 2 can be achieved (R_s reaches 1.5), and the theoretical plate number needs to reach 3.9 × 105.