作　　者： ; ; ; ; ; ; ; ;

机构地区： 广东出入境检验检疫局

出　　处： 《现代化工》 2011年第9期90-92,共3页

摘　　要： 建立了顶空-气相色谱法,对生物柴油副产物粗甘油中的甲醇含量进行测定。将粗甘油样品用水溶解,加入1,4-二氧六环作内标,90℃下顶空平衡45 min,在HP-INNOWax柱上进行分离和测定。实验结果表明,甲醇溶液的质量浓度在0.8～40.0 g/L范围内呈良好的线性关系,相关系数r>0.999,样品中甲醇质量分数的测定低限为0.005%。对实际样品进行测定,相对标准偏差在0.9%～1.6%(n=8),加标回收率在94.0%～106.0%。该方法操作简便,精密度好,结果准确,对仪器系统污染小,适用于粗甘油中甲醇含量的测定。 A headspace-gas chromatography method is developed for determination of methanol in crude glycerine, the by-product of biodiesel. The sample is dissolved by pure water with 1,4-dioxane as internal standard, and equalized at 90℃ for 45 min in head-space sampler, then separated and determined by gas-chromatography through HP-INNOWax capillary column. The linear range is from 0. 8 g/L to 40 g/L for methanol with good correlation coefficient （ r 〉 0. 999 ）. The lower limit of quantitation is O. 005 % （ S/N = 10）. The relative standard deviations （ n = 8 ） are between O. 9% and 1.6%. The recoveries are between 94. 0% and 106%. The method is simple, accurate and sensitive for determination of methanol in crude glycerine. In addition, it brings no contaminant to gas chromatograph.

关 键 词： 粗甘油 甲醇 顶空 气相色谱

领　　域： [农业科学] [农业科学]