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本文利用二维色谱技术,开发了一种新的总硫分析方法。本方法以CuO作陷阱,在650℃—700℃温度下,捕捉样品中经氧化生成的SO_2,SO_3。然后使其在900—950℃温度下变为SO_2释放出来。被释放的SO_2用载气携入色谱柱,用火焰光度鉴定器(FPD)测定。同时,CuO起预分离柱的作用,使样品主体成分及其它杂质与含硫化合物分离。由于CuO的富集和分离作用,分析时可以加大进样量,提高了方法的灵敏度和准确性。文中还报道了丙烯中加入硫化氢、硫氧碳:乙醇中加入二硫化碳、噻吩、乙硫醚等六种化合物的测定结果。实验表明,气体样品进样量为100ml,液体样品进样量为100μl时,最低检测限可达到ppb级,偏差小于10％。
In this paper, a new method of total sulfur analysis has been developed using two-dimensional chromatographic techniques. In this method, CuO is used as a trap to trap the SO_2 and SO_3 generated in the sample after being oxidized at a temperature of 650 ° C to 700 ° C. It is then released at a temperature of 900-950 ° C as SO2. The released SO2 is carried into the column with a carrier gas and measured with a flame photometric detector (FPD). At the same time, CuO acts as a pre-separation column to separate the main components of the sample from other sulfur-containing compounds. Due to the enrichment and separation of CuO, the injection volume can be increased during the analysis, which improves the sensitivity and accuracy of the method. The article also reported the addition of hydrogen sulfide in propylene, sulfur and oxygen: ethanol added carbon disulfide, thiophene, ethyl sulfide and other six compounds measured results. Experiments show that the gas sample injection volume of 100ml, the liquid sample injection volume of 100μl, the minimum detection limit can reach ppb level, the deviation is less than 10%.