全二维气相色谱分析直馏柴油中含硫化合物

Determination of Sulfur-containing Compounds in Straight Run Diesel Oil by Comprehensive Two Dimensional Gas Chromatography

采用全二维气相色谱-硫化学发光检测器,以直馏柴油为研究对象,考察了一维色谱柱初始温度、升温速率及两维柱温温差等条件对含硫化合物分离的影响,建立了直馏柴油中含硫化合物的分析方法。本方法对基质复杂的直馏柴油中含硫化合物的分离,并定性分析或归类了直馏柴油中的主要含硫化合物。以苯并噻吩为测试样,以峰面积对浓度作图,硫的浓度在1～100mg/kg范围内,峰面积与硫的浓度呈线性关系,相关系数大于0.999。与传统一维气相色谱相比,全二维气相色谱技术除可检测到苯并噻吩类、二苯并噻吩类等含硫化合物外,还可检测到直馏柴油中的硫醚类化合物;苯并噻吩类和二苯并噻吩类化合物也可得到较好分离。

A method was established for separating,identifying and quantitating sulfur-containing compounds in straight run diesel oil by comprehensive two-dimensional gas chromatography coupled with a sulfur chemiluminescence detector.The effects of main chromatographic conditions(oven temperature of the first dimensional column,modulation time,initial oven temperature of the second dimensional column) on separation of sulfur compounds were discussed.Sulfur compounds(including alkyl thiophenes,benzothiophene,alkyl benzothiophenes,dibenzothiophene,alkyl dibenzothiophenes and sulfides) in one straight run diesel oil were qualified based on some standard sulfur compounds by one-dimensional gas chromatography-sulfur selective detector.Some sulfides in straight run diesel oil can be separated and detected.The information was useful for processing diesel oil.Because response factor was independent on the molecule structure of sulfur compounds,using benzothiophene solution as external standard sample,the quantitative analysis on major sulfur compounds was carried out based on the linear response of sulfur chemiluminescence detector.The linear range was 1.0 100 mg/kg sulfur for each sulfur compound,and the correlation coefficient is 0.999.The method could be used to investigate the sulfur-containing compounds in different straight run diesel oil.