顶空-气相色谱法测定水中6种醇类化合物

Determination of six alcohol compounds in water by headspace gas chromatography

目的建立工业污水、地表水和生活饮用水中甲醇、异丙醇、仲丁醇、异丁醇、正丁醇和异戊醇6种醇类化合物的顶空-气相色谱检测方法。方法对平衡温度和平衡时间等对测定有影响的因素进行讨论,确定最佳的检测条件。6种醇类化合物经顶空萃取、DB-WAXetr毛细管色谱柱分离、氢火焰离子化检测器测定,使用保留时间定性,使用外标法定量。结果6种化合物测定方法的线性范围为0~8.10μg/mL,相关系数为0.9993~0.9999;方法的检出限为0.0962~0.1560μg/mL;以实际样品为基体加标进行准确度和精密度实验,准确度为97.0%~100.9%,批内精密度为0.72%~3.80%,批间精密度为0.81%~2.30%。结论所建立的方法操作简便,灵敏度高,精密度好,可准确测定工业污水、地表水和生活饮用水中的甲醇、异丙醇、仲丁醇、异丁醇、正丁醇和异戊醇含量。

Objective To establish a headspace gas chromatography method for the determination of methanol,isopropyl alcohol,secondary butanol,isobutanol,n-butanol and isoamyl alcohol in industrial wastewater,surface water and drinking water.Methods The factors affecting the measurement,such as equilibrium temperature and equilibrium time,were discussed to determine the best detection conditions.Six alcohols were separated by headspace extraction,separated by DB-WAXetr capillary column,determined by hydrogen flame ionization detector,qualitative analysis was performed by retention time and quantitative analysis by external standard method.Results The linear range of the six compounds were 0-8.10μg/mL,and the correlation coefficients were0.9993-0.9999.The detection limits were 0.0962-0.1560μg/mL.The accuracy and precision experiments were carried out with actual samples as the matrix,the accuracy ranged from 97.0%to 100.9%,intra-batch precision ranged from 0.72%to 3.80%and inter-batch precision ranged from 0.81%to 2.30%.Conclusion The method is simple,sensitive and accurate,and can accurately determine the contents of methanol,isopropyl alcohol,secondary butanol,isobutanol,n-butanol and isoamyl alcohol in industrial wastewater,surface water and drinking water.