使用液相色谱及液质联用技术建立了硅烷偶联剂 Si‐69中单质硫和化合态硫各自含量的分析方法．以C8柱为液相分离柱，采用简单的甲醇‐水流动相体系进行梯度淋洗，Si‐69各组分得到了很好的分离．Si‐69样品中鉴定出单质硫，并根据外标法测得其质量分数为16．8 mg／g ．同时，对样品中含硫化合物进行分析、鉴定，计算出化合态硫质量分数为28．26％，平均硫链长为3．55．本方法操作简单、快速，可用于Si‐69的硫质量控制分析．%In this study ,the method for analyzing the content of the elemental and the combined sulfur in silane coupling agent Si‐69 is established by liquid chromatography and liquid chromatography‐mass spectrometry .Every component in Si‐69 is well separated by using gradient elution with the simple mobile phase system of methanol‐water .Elemental sulfur is detected in Si‐69 samples ,and quantitated to be 16 .8 mg/g according to the external standard method .In addition ,the combined sulfur content is determined to be 28 .26% and the length of average sulfur chain to be 3 .55 .This method is simple and fast ,and suitable for sulfur quality control analysis of Si‐69 .
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