利用气相色谱仪和硫化学发光检测器测定焦炉气制LNG工艺气中痕量硫化物

Determination of trace sulfur in synthetic gas by gas chromatography and sulfur chemiluminescence detector

关键词:  气相色谱仪  硫化学发光检测器  焦炉气  合成气  形态硫  总硫  LNG 

Key words:  GC  SCD  coke oven gas  synthesis gas  sulfur forms  total sulfur  LNG

摘要:

焦炉气制取LNG生产过程中需严格控制合成气中的硫含量,以期增加合成催化剂的使用寿命。采用气相色谱仪-硫化学发光检测器(GC-SCD)方法,测定了焦炉气制LNG过程中痕量形态硫化物及总硫含量,并结合实际,讨论了分析过程中需注意的问题。标准气校准,计算各种组分的检出限均低于10.00×10-9 (体积分数),总硫含量33.00×10-9。6种含硫组分的标准曲线相关性均优于0.996。相对标准偏差(RSD,N=7)均小于7%。合成气样品测定过程中,在接近检出限的情况下,相对标准偏差小于12%。本方法可很好地满足工厂生产控制的需要。

Abstract:

Because of environmental pressures and market demands, the project of making LNG from coke oven gas was applied widely. In order to increase the service life of synthesis catalysts, the contents of total sulfur in synthetic gas must be strictly controlled, which should be lower than 50×10-9(volume fraction).The GC＆SCD method was applied to determine the content of trace sulfide and total sulfur in synthesis gas,and the influence factor was explained in the process of analysis and sampling. The detection limit of the method for every sulfur form is less than 10×10-9(volume fraction),and total sulfur is 33×10-9(volume fraction). The correlation coefficient of calibration curves for every sulfur form is better than 0.996 and RSD is less than 7%. During analysis of synthesis gas, the RSD is less than 12%. The demands of process control can be satisfied well.