毛细管气相色谱法同时测定饮用水中多种微量的挥发酚  

Simultaneous Determination of Several Trace Volatile Phenols in Drinking Water by Capillary Gas Chromatograph

作　　者：孙剑奇[1] 肖国光[1] 谢宝华[1] 代军[1] 

机构地区：[1]九江学院化学化工学院,江西九江332005

出　　处：《九江学院学报（自然科学版）》2010年第1期48-51,共4页Journal of Jiujiang University：Natural Science Edition

基　　金：江西省教育厅科学技术研究项目(GJJ09351)

摘　　要：本文建立了同时测定饮用水中多种微量挥发酚：苯酚、2-氯苯酚、对甲基苯酚、2,4-二氯苯酚的毛细管气相色谱方法。水样以乙醚及硫酸的混合液萃取,经氢氧化钠溶液反萃取,调整酸度后再以乙醚萃取,利用毛细管柱气相色谱-FID检测,以外标法定量。该方法测定的苯酚、2-二氯苯酚、对甲基苯酚、2,4-二氯苯酚的标准工作曲线方程分别为y=15.275x＋2.5942（r=0.9995）、y=11.42x＋2.9701（r=0.9992）、y=15.506x＋3.6894（r=0.9996）、y=8.9453x-2.185（r=0.9991）,检出限（S/N=3）分别为9.5×10^-5μg.mL^-1、1.3×10^-4μg.mL^-1、9.4×10^-5μg.mL^-1、1.6×10^-4μg.mL^-1，线性范围分别是3.2×10^-4-15μg.mL^-1、4.3×10^-4-9.1μg.mL^-1、3.1×10^-4-16μg.mL^-1、5.3×10^-4-5.3μg.mL^-1.对标准混合物溶液进行了3个不同水平的添加,每个水平重复5次进样,苯酚、2-氯苯酚、对甲基苯酚、2,4-二氯苯酚的加标回收率分别为89%-101%、83%-93%、77%-87%、91%-100%,相对平均标准偏差分别为1.7%-2.6%、2.9%-3.7%、1.8%-3.5%、2.4%-2.9%。相同条件下,实际饮用水经富集后,检测到苯酚的平均质量浓度为0.0011μg.mL^-1，其加标回收率为89%-93%,相对标准偏差为1.7%-2.8%。实验结果表明：本方法操作简单、快速,定量准确、灵敏度高、线性范围宽,测定结果令人满意。Capillary gas chromatography was established for simultaneous determination of trace volatile phenols in drinking water,including phenol,2-chlorophenol,p-methylphenol and 2,4-dichloro phenol.The samples,extracted with mixture of sulfuric acid and ether and reextracted by sodium hydroxide,then extracted with the same mixture indicated above were quantified by external standards using a capillary column with a flame ionization detector.The equations for linear regression calibration curves of phenol,2-chlorophenol,p-methylphenol and 2,4-dichlorophenol are y=15.275x ＋2.5942（r=0.9995）,y=11.42x ＋ 2.9701（r=0.9992）,y=15.506x ＋ 3.6894（r=0.9996） and y=8.9453x–2.185（r=0.9991）,respectively,and detection limits to these phenols（S/N=3） were 9.5×10^-5μg·mL^-1.3×10^-4g·mL-1,9.4×10^-5g·mL-1 and 1.6×10^-4g·mL-1,individually.The linear ranges for measuring these phenols were 3.2×10^-415μg·mL^-1.3×10^-49.1μg·mL^-1,3.1×10^-416μg·mL^-1nd 5.3×10^-45.3μg·mL^-1eparately.Three different levels of standard additions were added individually to standard mixture solutions of volatile phenols,and at each level five replicate samples were performed on.The average recoveries from spiked samples were 89%～101% for phenol,83%～93% for 2-chlorophenol,77%～87% for p-methylphenol and 91%～100% for 2,4-dichlorophenol,with the relative standard deviation 1.7%~2.6% for phenol,2.9%~3.7% for 2-chlorophenol,1.8%~3.5% for p-methylphenol and 2.4%~2.9% for 2,4-dichlorophenol.In the same way,drinking water samples were concentrated and measured,the mass concentration of phenol was 0.0011μg·mL^-1hose average recoveries from spiked samples and relative standard deviations were 89%～93%,1.7%~2.8% respectively.The satisfying result showed the proposed method several attributes,such as,simple,less time-and labor-intensive,high sensitivity,accurate,wide linear range and so on.

关 键 词：毛细管柱气相色谱法 苯酚 2-氯苯酚 对甲基苯酚 2 4-二氯苯酚 饮用水 萃取 

分 类 号：TU991.21[建筑科学—市政工程] X832[环境科学与工程—环境工程]