固相微萃取-气相色谱法测定工业苯酚中的2-甲基苯并呋喃和2,4-二苯基-4-甲基-1-戊烯

建立了工业苯酚中有机杂质的固相微萃取-气相色谱(SPME-GC)分析方法。实验考察了SPME萃取温度和萃取时间的影响,同时也优化了热解吸时间。优化后的萃取温度为20 ℃,萃取时间为10 min,热解吸时间为30 s。使用此法对工业苯酚样品中的两种主要有机杂质进行了分析检测,结果表明: 2-甲基苯并呋喃和2,4-二苯基-4-甲基-1-戊烯分别在0.05～1.06 mg/L和0.05～0.99 mg/L范围内线性关系良好(r2分别为0.990和0.992),检出限分别为0.5和1.6 μg/L。在0.1 mg/L的添加水平下,2-甲基苯并呋喃和2,4-二苯基-4-甲基-1-戊烯的回收率分别为104%和113%。该方法具有简单、快速、灵敏度高等优点,适合于工业苯酚中这两种主要痕量有机杂质的准确定量分析。

Determination of 2-methyl benzofuran and 2,4-diphenyl-4-methyl-1-pentene in industrial phenol by solid-phase microextraction coupled with gas chromatography

An analytical method based on solid-phase microextraction (SPME) coupled with gas chromatography for the determination of organic impurities (2-methyl benzofuran and 2,4-diphenyl-4-methyl-1-pentene) in industrial phenol was developed. The SPME parameters such as extraction temperature, extraction time, and the desorption time were optimized. The optimized parameters were as follows: extraction temperature was 20 ℃, extraction time was 10 min, and desorption time was 30 s. The results demonstrated that the linearities of calibration curves were good in the ranges of 0.05~1.06 mg/L and 0.05~0.99 mg/L with the correlation coefficients of 0.990 and 0.992 for 2-methyl benzofuran and 2,4-diphenyl-4-methyl-1-pentene, respectively. The limits of detection (LODs) were 0.5 and 1.6 μg/L for 2-methyl benzofuran and 2,4-diphenyl-4-methyl-1-pentene, respectively. The relative recoveries were 104% and 113% for 2-methyl benzofuran and 2,4-diphenyl-4-methyl-1-pentene at the spiked level of 0.1 mg/L with triplicate determination. The method is simple, rapid and sensitive for the quantitative analysis of trace organic impurities in industrial phenol.