管式炉燃烧–碘量库仑滴定法测定石油焦中总硫含量

Determination of Total Sulfur in Petroleum Coke by Tube Furnace Combustion with Ionometric Coulometry

建立一种管式炉内燃烧石油焦样品前处理,然后用自动碘量库仑滴定法测定石油焦中总硫含量的方法。探讨了影响实验结果的因素,电解液采用10 m L冰乙酸溶解于250 m L蒸馏水中,避光保存,实验环境温度为20℃以上,电解液中搅拌转子的转速为500 r/min。在优化的实验条件下,测定结果的相对标准偏差在2.36%~3.94%(n=6)之间,3种石油焦样品加标回收率在82.0%~101.5%之间。该方法可应用于石油焦中总硫含量的测定。

A method for the determination of total sulfur in petroleum coke was developed by the pretreatment of tube furnace combustion following with automatic ionometric coulometry. The factors relevant to the lab results were investigated, 10 mL acetic acid dissolved in 250 mL distilled water was used the electrolytic solution, storage conditions of electrolytic solution was kept in dark place, ambient temperature was more than 20℃ and rotor speed was approximate 500 r/min. Under the optimized conditions, the relative standard deviations of determination results were in the range of 2.36%–3.94%（n=6）, and the recoveries of 3 kinds of petroleum coke samples were in the range of 82.0%–101.5%. The method can be used for the analysis of total sulfur in petroleum coke.