静态顶空-气相色谱法同时测定水中12种醚类和酮类化合物的含量  

Simultaneous Determination of 12 Ether and Ketone Compounds in Water by Gas Chromatography after Static-Headspace

作　　者：何苗 徐广洲[2] 王安祥[2] 王春蕾 HE Miao;XU Guangzhou;WANG Anxiang;WANG Chunlei(Jiangsu Vocational College of Medicine,Yancheng224005,China;Yancheng Center for Disease Control and Prevention,Yancheng224000,China)

机构地区：[1]江苏医药职业学院,盐城224005 [2]盐城市疾病预防控制中心,盐城224000

出　　处：《理化检验（化学分册）》2022年第7期830-835,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：2020年江苏省高职院校青年教师企业实践培训项目(2020QYSJ151)。

摘　　要：取10 mL已采集的水样于顶空瓶中,加入3.7 g氯化钠,立即密封,轻轻摇匀。将密封的顶空瓶直接放入自动顶空进样器中,于80℃平衡20 min。抽取顶空瓶内液体上方的气体,用DB-624毛细管色谱柱(30 m×0.32 mm,0.25μm)分离目标化合物,采用配氢火焰离子化检测器的气相色谱仪检测。结果显示:12种醚类和酮类化合物的质量浓度在一定范围内与其对应的峰面积呈线性关系,检出限(3.143s)为0.1~2.9μg·L^(-1);以空白水样为基质进行加标回收试验,回收率为75.0%~118%,测定值的相对标准偏差(n=7)为0.61%~17%;方法用于分析出厂水、管网末梢水和地表水样品,地表水样品中均检出甲基叔丁基醚,检出量为0.6~0.8μg·L^(-1),其他样品中均未检出目标化合物。10 mL of the water sample collected was put into a headspace bottle,and 3.7 g of sodium chloride was added.After sealing immediately and shaking gently,the headspace bottle sealed was placed directly into an automatic headspace sampler and balanced at 80℃for 20 min.The gas above the liquid in the headspace bottle was extracted,and the target compounds were separated on DB-624 capillary column(30 m×0.32 mm,0.25μm)and detected by gas chromatograph with hydrogen flame ionization detector.It was shown that linear relationships between values of peak area and mass concentration of the 12 ether and ketone compounds were kept in the definite ranges,with detection limits(3.143s)in the range of 0.1-2.9μg·L^(-1).Test for recovery was made by standard addition method on the blank water sample as matrix,and values of recovery were found in the range of 75.0%-118%,with RSDs(n=7)of the determined values in the range of 0.61%-17%.This method was applied to analysis of the factory water,terminal tap water and surface water samples.Methyl tert-butyl ether was detected in surface water samples with the detection amounts in the range of 0.6-0.8μg·L^(-1),and the target compounds were not detected in the other samples.

关 键 词：静态顶空 气相色谱法 水 醚类化合物 酮类化合物 

分 类 号：O657.71[理学—分析化学]