顶空气相色谱法测定生物柴油中的微量甲醇.pdfVIP

学兔兔 石 油 化 工 · 1196· PETR0CHEMICAL TECHN0LOGY 2012年第41卷第10期 ■ 试 顶空气相色谱法测定生物柴油中的微量甲醇 李长秀，孔翠萍 (中国石化 石油化工科学研究院，北京 100083) [摘要]建立了一种顶空气相色谱法测定生物柴油中微量甲醇的方法。确定了合适的顶空条件，即顶空进样器中试样温度 70～80℃，平衡时间15～30 rain。考察了不同类型色谱柱分离生物柴油中甲醇的情况。对于新制备的生物柴油，采用厚液膜 非极性OV—l色谱柱或强极性CP—Wax色谱柱，可满足甲醇分离的要求；对于长久储存的生物柴油，采用强极性CP—Lowox色 谱柱，甲醇可与其中的轻组分分离从而有效消除轻组分的干扰；CP—Lowox色谱柱还可用于B一5混合生物柴油中微量甲醇的测 定。建立了采用cP—Lowox色谱柱外标法定量的标准曲线，相关系数大于0．999。测定甲醇的回收率为106％～124％，该方法 具有较好的重复性，可满足一般分析的要求。 [关键词]生物柴油；甲醇；顶空气相色谱法 [文章编号]1000—8144(2012)10—1196—05 [中图分类号]TQ 223．121 [文献标识码]A Determination of Methanol Content in Biodiesel by Headspace Gas Chromatography LiChangxiu，KongCuiping (SINOPEC Research Institute ofPetroleum Processing，Beijing 100083，China) J Abstract l A test method for the determination of methanol content in biodiesel by headspace gas chromatography was established．Suitable headspace conditions were confirmed，namely the sample temperature 70—8O℃ and equilibrium time 1 5—30 min．Different kinds of columns were investigated for the separation of methanol from biodiese1．For flesh made biodiesel samples．either nonpolar OV l column with thick film or column with polar phase such as CP．WaX column could achieve the separation wel1．For long—term stored samples，light components produced during the store would interfere in the determination of methanol，which could be eliminated by using CP—Lowox column． The methanol content in B．5 mixed biodiesel fue1 could be determ ined by using CP．Low