摘要
采用气相色谱-氢火焰离子化检测器-硫化学发光检测器(GC-FID-SCD)联用技术,建立了催化柴油中各种硫化物类型分布的分析方法.考察了色谱条件对催化柴油中各种硫化物分离的影响,定性了某催化柴油中的120多个硫化物,该方法还可以同时提供催化柴油中正构烷烃含量的分布信息.硫化物中的硫在1.5～700 mg/L时其峰面积与质量浓度呈较好的线性关系,相关系数达0.9999,响应与硫化物的类型无关.催化柴油中苯并噻吩、4-甲基苯并噻吩、二苯并噻吩、4-甲基二苯并噻吩和4,6-二甲基二苯并噻吩等主要硫化物浓度测定的相对标准偏差(RSD)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0.1 mg/L.将该方法用于不同来源柴油中各种硫化物类型分布的研究,并与气相色谱-原子发射光谱检测器(GC-AED)测硫的数据进行了对比,两种检测器的定量结果大多数具有较好的相关性,相关系数大于0.95.
A method for separation and determination of sulfur compounds in catalytic diesel oil by gas chromatography-flame ionization detector-sulfur chemiluminescence detector （GC-FID-SCD） was established. More than 120 sulfur compounds （including alkyl thiophenes, benzothiophene, alkyl benzothiophenes, dibenzothiophence, alkyl dibenzothiophenes） in one typical catalytic diesel oil were qualified based on retention time of some pure sulfur compound, retention rules of sulfur compound and qualified results by gas chromatography-atomic emission detector （GC-AED）. At the same time, distribution information of n-12 to n-C26 in diesel oil can be also provided by this method. The effects of speed of can-ier gas, oven temperature on resolution and effective plate number were discussed, Relative standard deviations of peak area of main sulfur compounds （benzothiophene, 4-benzothiophene, dibenzothiophene,4-methyl dibeazothiophene, 4,6-dimethyl dibenzothiophene） in one typical catalytic diesel oil are less than 5.0% , detection limit for sulfur is 0.1 mg/L under chosen condition. Using benzothiophene and 4,6-dimethyl dibenzothiophene solution as testing samples, it was validated that response factor was independent on the molecule structure of sulfur compound by detetlnining peak area of different concentration. The linear range was 1. 5 - 700 mg/L sulfur for each sulfur compound, correlation coefficient is 0. 999. The content of each sulfur compound in different diesel oil was determined with GC-SCD and GC-AED respectively, and correlation coefficients are over 0.95.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2005年第11期1517-1521,共5页
Chinese Journal of Analytical Chemistry
