催化柴油中硫化物的气相-原子发射光谱分析方法及应用

 建立了催化柴油馏分中各种硫化物类型分布的气相 原子发射光谱分析方法,考察了条件对各种硫化物分离的影响,定性(或归类)了催化柴油中的130多个硫化物,计算了程序升温条件下各种硫化物的保留指数,为不同实验室的定性比较和方法的转让提供了依据。硫化物中的硫在2mg/L～1000mg/L时其质量浓度与峰面积呈较好的线性关系,相关系数达0 997。几种硫化物(苯并噻吩、4 甲基苯并噻吩、二苯并噻吩、4 甲基二苯并噻吩、4,6 二甲基二苯并噻吩)6次测定所得峰面积的相对标准偏差均小于5 0%。当信噪比(S/N)为3时,测得苯并噻吩硫的检出限为0 1mg/L。

Determination of Sulfur Compounds in Catalytic Diesel Oil by Gas Chromatography with Atomic Emission Detector and Its Applications

The method for separation and determination of sulfur compounds in catalytic diesel oil by gas chromatography with atomic emission detector (GC-AED) was established. More than 130 sulfur compounds (including alkyl thiophenes, benzothiophene, alkyl benzothiophenes, dibenzothiophene, alkyl dibenzothiophenes) in catalytic diesel oil were qualified based on the retention time of some pure sulfur compounds and the retention indexes of sulfur compounds. The effects of oven temperature, heating rate and sample amount on resolution and effective plate number were investigated. Retention indexes of different sulfur compounds under temperature programmed condition were calculated. The relative standard deviations of peak areas of main sulfur compounds in catalytic diesel oil were no more than 5.0%, detection limit for sulfur was 0.1 mg/L under chosen conditions. Because response factor was independent on the molecule structure of the sulfur-containing compound, the content of each sulfur compound was determined quantitatively using thiophene as sulfur standard sample. The linear range was 2 mg/L-1,000 mg/L sulfur, and the correlation coefficient was 0.997. The method is successfully applied for the determination of the contents of sulfur compounds in six different catalytic diesel oils (Fujian catalytic diesel oil, Yanshan catalytic diesel oil, Zhongdong diesel oil, Zhenhai catalytic diesel oil, Zhenhai Changsan oil and Zhenhai Changer oil). Distributions of sulfur compounds in different catalytic diesel oils were obtained by GC-AED.