摘要
建立一种水源水中有机磷农药的气相色谱分析方法。对程序升温条件、衬管选择及样品萃取条件进行了优化,确立了最佳检测方案。以二氯甲烷作为萃取剂对水样中的敌敌畏、乐果、甲基对硫磷、马拉硫磷、对硫磷5种有机磷农药进行萃取;采用火焰光度检测器,Elite-1701色谱柱,填料为14%氰丙基苯基(其中7%氰丙基7%苯基)二甲基聚硅氧烷(86%),载气流量为1.0 mL/min,程序升温,惰性不分流衬管。当取样量为100 mL时,5种有机磷农药的检出限在0.03~0.05μg/L之间,定量限在0.10~0.20μg/L之间。标准曲线在0.1~10 mg/L范围内线性关系良好,相关系数r在0.9991~0.9999之间,5种有机磷农药测定的相对标准偏差在3.1%~5.8%之间,加标回收率在65.8%~113.0%之间。该方法选择性好,5种有机磷农药及杂质均得到了较好的分离,同时具有良好的精密度及准确度,较宽的线性范围,较低的检出限。同时在样品前处理中采用较少的萃取剂,减少了对环境造成的二次污染。
A gas chromatographic method for determination of organophosphorus pesticides in water was established.Through optimizing the program temperature increase condition,the screened pipe selection and the sample extraction condition,the optimal detection scheme was determined.Dichloromethane was used to extract 5 kinds of organophosphorus pesticides from the water samples,including DDVP,dimethoate,parathion-methyl,malathion and parathion.The experiment adopted flame photometric detector,Elite-1701 column,program heating and inert non-shunt screened pipe,the filler was 14%cyanopropyl phenyl(7%cyanopropyl,7%phenyl)and dimethylpolysiloxane(86%),the carrier gas flow rate was 1.0 mL/min.When the sample quantity was 100 mL,the detection limits of five organophosphorus pesticides were 0.03-0.05μg/L,and the quantitative limits were 0.10-0.20μg/L.Standard curves had good linear relation in the range of 0.1-10 mg/L,the correlation coefficient r was 0.9991-0.9999,the relative standard deviation of the said 5 kinds of organophosphorus pesticides were in the range of 3.1%-5.8%,the adding standard recoveries were 65.8%-113.0%.The said method has good selectivities,which can effectively separate the 5 kinds of organophosphorus and impurities,and it also has good precision and accuracy,wide linear ranges and low detection limits.Adding lesser extractant before the treatment of the samples can reduce secondary pollution to the environment.
作者
马文娟
董凤娟
秦承刚
张勇
王旭东
闫香香
MA Wenjuan;DONG Fengjuan;QIN Chenggang;ZHANG Yong;WANG Xudong;YAN Xiangxiang(Zaozhuang Institute of Science and Technology Information,Zaozhuang,277000,China;Shandong Zaozhuang Ecological Environment Monitoring Center,Zaozhuang 277000,China)
出处
《工业用水与废水》
CAS
2022年第3期81-84,88,共5页
Industrial Water & Wastewater
关键词
有机磷农药
气相色谱法
方法优化
惰性不分流衬管
organophosphorus pesticides
gas chromatography
method optimization
inert non-shunt screened pipe
