色谱 ›› 2010, Vol. 28 ›› Issue (10): 989-992.DOI: 10.3724/SP.J.1123.2010.00989

• 技术与应用 • 上一篇    下一篇

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

娄大伟1, 孙秀云1*, 杨积学2, 李自恩1, 牛春芳1, 赵飞1, 姜国玉2, 胡春福2, 牛志蒙2, 金辉2   

  1. 1. 吉林化工学院化学系, 吉林 吉林 132022; 2. 中国石油天然气股份有限公司吉林石化分公司, 吉林 吉林 132021
  • 收稿日期:2010-07-08 修回日期:2010-08-13 出版日期:2010-10-28 发布日期:2010-10-28
  • 通讯作者: 孙秀云,教授,主要从事量化计算和催化剂的结构特征研究. E-mail: sunxiuyun1989@sina.com.
  • 基金资助:

    吉林省科技发展计划项目(No. 20095022)和中国石油天然气股份有限公司吉林石化分公司科技计划项目(No. 2008-12117).

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

LOU Dawei1, SUN Xiuyun1*, YANG Jixue2, LI Zien1, NIU Chunfang1, ZHAO Fei1, JIANG Guoyu2, HU Chunfu2, NIU Zhimeng2, JIN Hui2   

  1. 1. Department of Chemistry, Jilin Institute of Chemical Technology, Jilin 132022, China; 2. Jilin Petrochemical Branch Company, PetroChina Company Limited, Jilin 132021, China
  • Received:2010-07-08 Revised:2010-08-13 Online:2010-10-28 Published:2010-10-28
  • Contact: LOU Da-Wei

摘要: 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。

关键词: 2,4-二苯基-4-甲基-1-戊烯, 2-甲基苯并呋喃, 工业苯酚, 固相微萃取, 气相色谱

Abstract: 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.

Key words: 2,4-diphenyl-4-methyl-1-pentene, 2-methyl benzofuran, gas chromatography, industrial phenol, solid-phase microextraction