摘要
含痕量苯酚的水样与丙酮和环己烷(1+1)的混合溶剂混合,置于控温在60℃的微波炉中加热30 s,使苯酚萃取进入有机相,分取部分萃取液在pH 8～9的条件下与衍生试剂乙酸酐反应15 min,所生成的苯酚衍生物用石油醚萃取,分取部分经脱水后的有机相进样作气相色谱分析。色谱测定中采用DB-17毛细管色谱柱(30 m×0.53 mm,1.0μm)及氢火焰离子化检测器,在优化的条件下测得方法的检出限(3S/N)为0.01 mg·L-1。按所提出方法分析了8个模拟水样,根据测得苯酚的含量值算得其相对标准偏差为4.2%,并按标准加入法求得其平均回收率为94.0%。
Water sample containing phenol was extracted with mixed solvent of acetone and cyclohexane（1＋1）, heated at 60℃ in a microwave oven for 30 s. An aliquot of the extract was reacted with the derivatizing reagent, acetic anhydride for 15 rain at pH 8 - 9. The derivatized product of phenol was then extracted with petroleum ether. An aliquot of the organic phase, after dehydration, was used for GC determination. DB-17 capillary chromatographic column （30 m×0. 53 mm, 1.0 μm） and hydogen flame ionization detector were used in the gas chromatography. Detection limit （3S/N） found under the optimum condition was 0. 01 mg · L^-1. Precision and recovery were tested by analyzing 8 simulated water samples with addition of standard phenol, giving values of RSD＇s and average recovery of 4.2% and 94. 0% respectively.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2009年第1期32-34,共3页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
湖南省科技厅项目(2007FJ4156)
关键词
微波加热萃取
气相色谱法
柱前衍化法
苯酚
水样
Microwave heated solvent extraction
Gas chromatography
Pre-column derivatization
Phenol
Water sample
