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目的建立顶空-气相色谱法测定废水中正丁醇的含量。方法本文对水中含盐量,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。将废水中的正丁醇经顶空技术提取后,在优化色谱条件下,采用0.32 mm×50 m×1μm SE-30毛细管柱分离,氢火焰离子化检测器检测,以保留时间定性,峰高或峰面积定量。结果正丁醇浓度在0.31 mg/L~162.0 mg/L的范围内呈良好的线性关系,回归方程为Y=1218.5X+1058.2,相关系数r为0.9994,方法检出限为0.31 mg/L,高、中、低浓度的标准重复测定的相对标准偏差均<3.9%,加标回收率在97%~105%之间。结论该方法能够有效分离、测定废水中正丁醇的含量,同时该方法具有简便、快速、灵敏度高,线性范围宽等优点,特别是顶空技术很大程度上减少了色谱柱的污染,适用于废水中正丁醇的测定。
Objective To establish a headspace-gas chromatographic method for the determination of n-butanol in waste water. Methods In this paper, salt content in the water, the equilibrium temperature and equilibrium time to determine the factors that affect the discussion to determine the best detection conditions. The n-butanol in waste water was extracted by headspace technique, and then was separated by SE-30 capillary column of 0.32 mm × 50 μm × 1 μm and detected by hydrogen flame ionization detector under optimized chromatographic conditions. The retention time was qualitative and the peak height Or peak area. Results The n-butanol concentration showed a good linearity in the range of 0.31 mg / L to 162.0 mg / L, the regression equation was Y = 1218.5X + 1058.2, the correlation coefficient was 0.9994, the detection limit was 0.31 mg / L, The relative standard deviations (RSDs) of high, medium and low concentrations were all less than 3.9% and the recoveries were between 97% and 105%. Conclusion This method can effectively separate and determine the content of n-butanol in waste water. Meanwhile, the method has the advantages of simple, rapid, high sensitivity and wide linear range. Especially, the headspace technology greatly reduces the pollution of the column and is suitable for Determination of n-butanol in wastewater.