气相色谱法测定粗甘油中的游离甘油含量.docVIP

气相色谱法测定粗甘油中的游离甘油含量 李丹，周明辉，刘莹峰，翟翠萍，郑建国 本文档由【中文word文档库】提供，转载分发敬请保留本信息； 中文word文档库免费提供海量范文、教育、学习、政策、报告和经济类word文档。 (广东出入境检验检疫局，广州，510623) 摘 要：建立了用气相色谱法直接测定生物柴油副产物粗甘油中甘油含量的方法，无需进行繁琐的衍生化步骤。采用四氢呋喃:水=3:1(v/v)的混合溶剂溶解粗甘油样品，加入二乙二醇二乙醚作内标，直接在HP-5柱上进行GC法分离，内标法定量。通过对溶剂、内标物、色谱柱、进样量等参数进行优化，得到了适当的样品前处理条件和GC法检测条件。标准曲线的线性范围从5%到100%，线性相关系数大于0.999。对实际样品进行8次平行样测定，相对标准偏差均不大于1%。对样品进行高、中、低三个不同水平的加标回收试验，回收率均在95%～105%之间。对实际样品的测定结果普遍较使用传统的高锰酸钾滴定法低，表明该方法对游离甘油的测定可能更为准确。该方法操作简便，分析迅速，结果准确，适用于粗甘油中游离甘油的测定。 关键词：粗甘油，游离甘油，气相色谱 Determination of free glycerol in crude glycerine with gas chromatography Li Dan Zhou Minghui Liu Yingfeng Zhai Cuiping Zheng Jianguo (Guangdong Entry-Exit Inspection Quarantine Bureau，Guangzhou 510623, China) Abstract: A gas chromatography method was developed for determination of free glycerol in crude glycerine without any derivative pretreatment. The sample was added with diethylene glycol diethyl ether as internal standard, and resolved with mixed solvents (THF : water =3 : 1, v/v), and was directly separated on GC by HP-5 column (30 m?.32 mm?.25 祄sep). The influence of some important factors such as solvent, internal standard, capillary column, and injection volume were all carefully investigated, and the pretreatment method and GC parameters were optimized. The standard curve of glycerol was linear in the concentration range from 5% to 100%, with correlation coefficient of 0.99994. Taking parallel determinations for each sample, the relative standard deviations (RSD) were in the range of 0.68% ～ 0.91% (n=8). Making standard addition test for 6 sample and each with 3 different addition levels, the recoveries ranged from 95% to 105%. Comparing with results from titration method by KMnO4，all results from GC method were all lower than that from titration method, this implied that the results from GC were more accurate. This method showed good simplicity, repeatability and stability, and was suitable for quantitatively analysis of the content of glycerol in crude glycerine