摘要
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 chromatography method for determination of n- butanol in waste water. Methods Factors influencing the determination such as the concentration of salt in water sample,equilibrium temperature and equilibrium time were discussed to define the best test conditions. N- butanol in water was extracted by headspace technology, then separated with 0. 32 mm × 50 m × 1 μm SE- 30 capillary column and determined by hydrogen flame ionization detector. Retention time was used for qualitative analysis and peak area was used for quantitative analysis. Results The method showed good linear relationship in the range of 0. 31 mg / L ~ 162. 0 mg / L(r = 0. 9994). The linear regression equation was Y = 1218. 5 X + 1058. 2. The detection limit was 0. 31 mg / L and the relative standard deviations of high,medium and low concentration were all less than 3. 9%. The recovery was between 97% ~ 105%. Conclusion This method can effectively separate and accurately determine n- butanol in waste water. What's more,along with the convenience,speediness,high sensitivity and wide linear range,especially the headspace technology can reduce the pollution of the chromatographic column,it is feasible for determination of n- butanol in waste water.
出处
《中国卫生检验杂志》
北大核心
2014年第9期1238-1239,共2页
Chinese Journal of Health Laboratory Technology
关键词
顶空-气相色谱法
废水
正丁醇
Headspace-gas chromatography
Waste water
N-butanol