摘要
酚类化合物在土壤中含量低，且性质活泼，提取与分析比较困难。利用二氯甲烷-正己烷混合溶剂（v／V=2）作为溶剂，超声20rain提取了土壤中的有机成分。再利用酚类化合物中酚羟基的弱酸性，在提取液中加入pH〉12的强碱性水溶液，使得酚类化合物与强碱反应生成对应的盐而溶于水，从而与有机相分离。在分离后的水相中加入二氯甲烷-正己烷混合溶剂（v／V=2）进行净化，进一步将碱性水溶液中的有机干扰组分除去。然后将溶液调至酸性（pH〈3），用二氯甲烷／乙酸乙酯混合溶剂（v／V=4）萃取酚类化合物。最终，采用气相色谱-质谱法（GC-MS）对样品中的苯酚、2-氯酚、2-硝基酚、2，4-二甲基酚、2，4-二氯酚、4-氯-3-甲基酚、2，4，6-三氯酚共7种酚类化合物进行了测定。方法检出限为O．O3～O．48mg／kg。将方法应用于实际样品中7种酚类化合物的检测，结果的相对标准偏差（RSD，n=7）为1．6％～7．9％，加标回收率为82％～111％。
The content of phenols in soil was low.Moreover,their chemical properties were active.As a result,the extraction and analysis of phenols in soil were relatively difficult.The organic components in soil were extracted by ultrasonic for 20 min using dichloromethane and n-hexane(V/V=2)as mixed solvent.The strongly alkaline aqueous solution(pH>12)was added into extracting solution.The phenols could react with alkali to form corresponding water-soluble slats due to the weak acidity of phenolic hydroxyl groups.Therefore,the phenols could be separated from the organic phase.The dichloromethane and nhexane(V/V=2)mixed solvent was added into water phase after separation for purification.The interference organic components in alkaline aqueous solution were further removed.Then,the solution was adjusted to acid(pH<3).The phenolic compounds were extracted with dichloromethane/n-hexane(V/V=4)mixed solvent.Finally,seven types of phenols(including phenol,2-chlorophenol,2-nitrophenol,2,4-dimethylolphenol,2,4-dichlorophen,4-chlor-3-methylolphenol and 2,4,6-trichlorophenol)in sample were determined by gas chromatography-mass spectrometry(GC-MS).The detection limit of method was 0.03-0.48mg/kg.The proposed method was applied to the detection of seven phenols in actual samples.The relative standard deviations(RSD,n=7)were between 1.6% and 7.9%,and the recoveries were between82% and 111%.
出处
《冶金分析》
CAS
CSCD
北大核心
2016年第2期27-32,共6页
Metallurgical Analysis
