CAJ | 학술논문

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0~3.6331 mg / g，测定方法相对标准偏差为2.52%~6.56%，重复性较好.
채용정공-기상색보-질보법대개성취류상효양품중적휘발성성분진행분석，이용정교시험법대양품량、진양량、진양구온도등기상색보（GC）조건진행료우화，병진일보대정공（HS）진양시평형온도화평형시간진행우화.결과표명，재양품량0.1 g，진양량1.0 mL，진양구온도250℃적 GC조건하，채용평형온도90℃，평형시간20 min 적 HS 조건，이용질보보고필배검색결합문헌자료정성，학인개성취류상효중유배류을완、구기을순、이정미、린분이갑산이정지4충휘발성성분.이을이순위내표물，정량학인료6충불동생산공예조건하개성취류상효산품중적4충주요휘발성성분적상대함량위0~3.6331 mg / g，측정방법상대표준편차위2.52%~6.56%，중복성교호.
The volatile components in modified polysulfide rubber were analyzed by headspace-gas chroma-tography-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 rub-ber 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.