直接进样-硫化学发光检测器-气相色谱法测定有机硫

采用硫化学发光检测器(SCD)-气相色谱仪,建立了甲硫醇、乙硫醇、甲硫醚、乙硫醚、二甲基二硫5种有机硫化合物的分析方法。优化色谱柱种类、进样管线材质、配气方式、样品保存时间等参数,考察方法性能指标。结果表明:在最优条件下,5种有机硫化合物线性回归方程相关系数均为0.998以上。定量环进样为1.0 m L时,方法检出限为0.005~0.016 mg/m3;相对标准偏差为0.7%~3.8%。中、高浓度准确度较好,适用于有机硫化合物的测定。

Determination of Organic Sulfurin by Direct Injection-Gas Chromatography with Sulfur Chemiluminescence Detector

The analytical method for five kinds of organic sulfur compounds, including methyl mercaptan, ethyl mercaptan, methyl sulfide, ethyl sulfide and dimethyl disulfide, was established by using sulfur chemiluminescence detector (SCD)-gas chromatography. Performance indicators of the method were studied by optimizing the chromatographic column type, the material of injection pipeline, the selection of gas and the retention time of sample. The results indicated that the linear regression correlation coefficients of the five organic sulfur compounds were all above 0.998 under the optimal conditions. When injecting 1.0 mL by quantitative ring, the method detection limit was 0.005-0.016 mg/m³, and the relative standard deviation (RSD)were in the range of 0.7%-3.8%. The accuracy in detecting samples of medium and high concentration levels were better and the method was suitable for the determination of organic sulfur compounds.