摘要
采用SE-30(50 m×0.25 mm×0.5 μm)石英毛细管柱,建立了用无分流进样法分析异戊二烯中痕量环戊二烯的方法.经优化,确定了适宜的色谱条件为:汽化温度140℃,柱室温度30℃,进样量1.0μL,不分流时间0.5～0.6 min.上述条件下,可分析出异戊二烯中质量分数为0.5mg/kg以下的环戊二烯,最小检出限为0.1 mg/kg,环戊二烯质量分数为1 mg/kg左右的样品重复性实验的平均相对标准偏差为4.1%,最大为6%,每次分析时间约8 min,完全满足聚合级异戊二烯生产的纯品检验要求.
The method for analysis of trace cyclopentadiene impurity in isoprene was established by GC using splitless injection and capillary column SE-30 (50 m × 0.25 mm × 0.5 μm). The optimum operation conditions were found as follows: injection temperature is 140°C; column temperature is 30°C; volume of sample is 1.0 μL; splitless period is 0.5-0.6 minutes. The results show that the concentration of cyclopentadiene in isoprene by this method is less than 0.5 mg/kg. The minimum detectable limit is about 0.1 mg/kg. The average relative standard deviation for a isoprene sample with about of 1 mg/kg cyclopentadiene is 4.1% and the maximum deviation is 6.0% in the revision test. The time for one run is about 8 minutes. The method meets the expectation of the identification of polymerization grade isoprene.
出处
《石油化工高等学校学报》
EI
CAS
2005年第3期46-49,共4页
Journal of Petrochemical Universities
关键词
无分流进样
异戊二烯
环戊二烯
痕量分析
毛细管色谱
Splitless injection
Isoprene
Cyclopentadiene
Trace analysis
Capillary chromatography
