摘要:
采用顶空-气相色谱-质谱法对改性聚硫橡胶样品中的挥发性成分进行分析,利用正交试验法对样品量、进样量、进样口温度等气相色谱(GC)条件进行了优化,并进一步对顶空(HS)进样时平衡温度和平衡时间进行优化.结果表明,在样品量0.1 g,进样量1.0 mL,进样口温度250℃的GC条件下,采用平衡温度90℃,平衡时间20 min的HS条件,利用质谱谱库匹配检索结合文献资料定性,确认改性聚硫橡胶中有环硫乙烷、巯基乙醇、二丁醚、邻苯二甲酸二丁酯4种挥发性成分.以乙二醇为内标物,定量确认了6种不同生产工艺条件下改性聚硫橡胶产品中的4种主要挥发性成分的相对含量为0~3.633 1 mg/g,测定方法相对标准偏差为2.52%~6.56%,重复性较好.
Abstract:
The volatile components in modified polysulfide rubber were analyzed by headspace-gas chromatography-mass spectrometry. The sample amount,injection volume, inlet temperature of gas chromatography(GC) conditions were optimized using the orthogonal test method, and the equilibrium temperature and equilibrium time of the headspace(HS) sampling were optimized. The results showed that under such GC conditions as sample amount of 0.1 g,injection volume of 1.0 mL, the inlet temperature of 250℃, using such HS conditions as equilibrium temperature of 90℃, equilibrium time of 20 min,and combination of NIST MS Library search and literature retrieva, 4 kinds of volatile compounds, which recognized as the thiirane, mercaptoethanol, two butyl ether and dibutyl phthalate were idetified. Using ethylene glycol as the internal standard, the 4 kinds of main volatile components relative content of the modified polysulfide rubber products from 6 different production conditions were located in 0~3.633 1 mg/g with the relative standard error(RSD) was 2.52%~6.56%. This method had good repeatability.
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