顶空气相色谱法测定富氢水中的氢气

建立顶空气相色谱法测定富氢水中氢气的方法。采用顶空的方式将水中的微量氢气转移到气相中,通过分子筛色谱柱分离,用热导检测器测定。分析条件如下:分流比为5∶1,气液体积比为1.2∶1,平衡温度为40℃,平衡时间为15 min。水中氢气的质量浓度在0.080~1.603 mg/L范围内与色谱峰面积成良好线性关系,线性相关系数为0.999,方法检出限为0.005 mg/L。样品加标回收率为91.03%~94.25%,测定结果的相对标准偏差为0.61%~2.32%(n=6)。该法可用于富氢水中氢气的测定。

Determination of Hydrogen in Hydrogen-Rich Water by Headspace Gas Chromatography

A method for determining hydrogen in hydrogen-rich water by headspace gas chromatography was established. The trace hydrogen in water was transferred to gas by the manner of headspace, then separated by the molecular sieve chromatography column, finally determined by gas chromatography with TCD. The analysis conditions were determined as the following: the split ratio was 5:1, the gas-liquid volume ratio was 1.2:1, the equilibrium temperature was 40℃ , and the equilibrium time was 15 min. The mass concentration of hydrogen in water was linear with chromatographic peak area in the range of 0.080-1.603 mg/L, and the linear correlation coefficient was 0.999. The detection limit was 0.005 mg/L. The addition recoveries of the sample were 91.03%-94.25%, and the relative standard deviations of determination results were 0.61%-2.32%(n=6). The method is suitable for the determining hydrogen in hydrogen-rich water.