色谱

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高效液相色谱法测定水性酚醛树脂中残留的甲醛和苯酚

刘秀玲,张武畏,隋国红,宁强

  

  1. Qingdao DIC Finechemicals Co., Ltd., Qingdao 266101, China
  • 收稿日期:2007-01-25 修回日期:2007-05-17 出版日期:2007-07-30 发布日期:1985-06-25
  • 通讯作者: 刘秀玲

Determination of Phenol and Formaldehyde in Resol Resins
by High Performance Liquid Chromatography

LIU Xiuling, ZHANG Wuwei, SUI Guohong, NING Qiang   

  1. Qingdao DIC Finechemicals Co., Ltd., Qingdao 266101, China
  • Received:2007-01-25 Revised:2007-05-17 Online:2007-07-30 Published:1985-06-25

摘要:

采用高效液相色谱法同时测定了水性酚醛树脂粘稠液体中残留的甲醛和苯酚,用2,4-二硝基苯肼对甲醛进行衍生化,然后进行色谱分离。色谱柱:Waters Symmetry C18 (5 μm,4.6 mm × 250 mm);柱温:30 ℃;流动相:甲醇-水(体积比为43∶57);检测波长:苯酚270 nm,甲醛360 nm;运行时间:45 min;流速:0.8 mL/min。方法的相对标准偏差小于5%,检测限小于1 μg/L,加标回收率为96%~105%。使用该分析方法可对该类树脂的质量性能进行有效监控。

关键词: 苯酚, 高效液相色谱法, 甲醛, 水性酚醛树脂 , 衍生化

Abstract:

A high performance liquid chromatographic (HPLC) method was developed for the separation of formaldehyde and phenol from the other components of resol resins. The sample was dissolved in methanol and treated with 2,4-dinitrophenylhydrazine in order that formaldehyde was derivatized to form 2,4-dinitrophenylhydrazone with high UV absorbance. The separation was carried out on a Waters Symmetry C18 column (5 μm,4.6 mm × 250 mm) with methanol-water (43∶57, v/v) as the mobile phase at a flow rate of 0.8 mL/min. The detection wavelength was 270 nm for phenol and 360 nm for the derivative of formaldehyde. The results showed that derivatization had no effect on the determination of phenol. The relative standard deviations (RSDs) of the contents of phenol and formaldehyde were below 5%, the limits of detection (LODs) were below 1 μg/L, and the recoveries were between 96% and 105%. With this method, formaldehyde and phenol in the resol resins can be determined by only one injection. As a result, this method would meet effective control for quality of this kind of resol resins.

Key words: derivatization, formaldehyde, phenol, resol resins , high performance liquid chromatography (HPLC)