闭合超声循环吹扫针捕集动态提取-气相色谱法测定地下水中的4种有机磷农药
基于针捕集适于免溶剂提取气态介质样品的特点，通过蠕动泵将针捕集与水样组成闭合循环吹扫系统，提高目标物的水样/顶空亨利系数，建立了针捕集闭合循环提取耦合气相色谱快速分析地下水中4种半挥发性有机磷农药（敌敌畏、甲拌磷、甲基对硫磷、马拉硫磷）的方法，该方法集采样、提取、净化、浓缩、色谱进样于一体。确定了针捕集提取水样最佳条件为：采样流速11.11 mL/min，水样提取温度40℃，在此条件下获得浓度均为1 mg/L的4种有机磷农药的针捕集吸附穿透体积，其中甲基对硫磷最大为600 mL。以5μg/L、50μg/L和200μg/L三个浓度水平的加标平均回收率为62.3%~103.0%，除敌敌畏低浓度水平...
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| Published in | 岩矿测试 Vol. 34; no. 4; pp. 480 - 486 |
|---|---|
| Main Author | |
| Format | Journal Article |
| Language | Chinese |
| Published |
吉林大学环境与资源学院，吉林 长春130021
2015
教育部地下水资源与环境重点实验室，吉林 长春130021%深圳出入境检验检疫局,广东深圳,518067%青州市环境监察大队,山东青州,262500 |
| Subjects | |
| Online Access | Get full text |
| ISSN | 0254-5357 |
| DOI | 10.15898/j.cnki.11-2131/td.2015.04.017 |
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| Abstract | 基于针捕集适于免溶剂提取气态介质样品的特点，通过蠕动泵将针捕集与水样组成闭合循环吹扫系统，提高目标物的水样/顶空亨利系数，建立了针捕集闭合循环提取耦合气相色谱快速分析地下水中4种半挥发性有机磷农药（敌敌畏、甲拌磷、甲基对硫磷、马拉硫磷）的方法，该方法集采样、提取、净化、浓缩、色谱进样于一体。确定了针捕集提取水样最佳条件为：采样流速11.11 mL/min，水样提取温度40℃，在此条件下获得浓度均为1 mg/L的4种有机磷农药的针捕集吸附穿透体积，其中甲基对硫磷最大为600 mL。以5μg/L、50μg/L和200μg/L三个浓度水平的加标平均回收率为62.3%~103.0%，除敌敌畏低浓度水平的RSD为26.1%外，其余组分的RSD﹤7.7%；方法检出限为0.016~0.157μg/L，接近或优于现行国标及相关研究结果。 |
|---|---|
| AbstractList | 基于针捕集适于免溶剂提取气态介质样品的特点，通过蠕动泵将针捕集与水样组成闭合循环吹扫系统，提高目标物的水样/顶空亨利系数，建立了针捕集闭合循环提取耦合气相色谱快速分析地下水中4种半挥发性有机磷农药（敌敌畏、甲拌磷、甲基对硫磷、马拉硫磷）的方法，该方法集采样、提取、净化、浓缩、色谱进样于一体。确定了针捕集提取水样最佳条件为：采样流速11.11 mL/min，水样提取温度40℃，在此条件下获得浓度均为1 mg/L的4种有机磷农药的针捕集吸附穿透体积，其中甲基对硫磷最大为600 mL。以5μg/L、50μg/L和200μg/L三个浓度水平的加标平均回收率为62.3%~103.0%，除敌敌畏低浓度水平的RSD为26.1%外，其余组分的RSD﹤7.7%；方法检出限为0.016~0.157μg/L，接近或优于现行国标及相关研究结果。 O658.2%O657.71%S482.33; 基于针捕集适于免溶剂提取气态介质样品的特点，通过蠕动泵将针捕集与水样组成闭合循环吹扫系统，提高目标物的水样/顶空亨利系数，建立了针捕集闭合循环提取耦合气相色谱快速分析地下水中4种半挥发性有机磷农药（敌敌畏、甲拌磷、甲基对硫磷、马拉硫磷）的方法，该方法集采样、提取、净化、浓缩、色谱进样于一体。确定了针捕集提取水样最佳条件为：采样流速11.11 mL/min，水样提取温度40℃，在此条件下获得浓度均为1 mg/L的4种有机磷农药的针捕集吸附穿透体积，其中甲基对硫磷最大为600 mL。以5μg/L、50μg/L和200μg/L三个浓度水平的加标平均回收率为62.3%~103.0%，除敌敌畏低浓度水平的RSD为26.1%外，其余组分的RSD﹤7.7%；方法检出限为0.016~0.157μg/L，接近或优于现行国标及相关研究结果。 |
| Abstract_FL | Based on the merits of solvent-free extraction of gaseous samples by needle trap,closed circulating purge system consisting of needle trap and water sample by peristaltic pump is established to enhance the Henry ’s law constant of analytes in the gas/liquid phase. In this study,the method for determination of dichlorvos,phorate, methyl parathion and malathion in groundwater by circulating extraction with needle trap coupled with Gas Chromatography was established. This method integrated sampling,extraction,purification,concentration,and chromatography. The optimum conditions for the extraction by needle trap include sampling flow rate of 11. 11 mL/min and extraction temperature of 40℃. Under these conditions,the maximum breakthrough volume of 1 mg/L methyl parathion is 600 mL. The recoveries range from 62. 3% to 103. 0% for 5 μg/L,50 μg/L and 200 μg/L analytes. Low level dichlorvos has a relative standard deviation of 26. 1%,and other components are lower than 7. 7%. The detection limits of the proposed method range from 0. 016 to 0. 157 μg/L,close to,or better than the results of current standard method and related study. |
| Author | 高松 邓银舟 李玉芹 刘园园 张兰英 刘娜 庞英明 |
| AuthorAffiliation | 吉林大学环境与资源学院,吉林长春130021 教育部地下水资源与环境重点实验室,吉林长春130021 深圳出入境检验检疫局,广东深圳518067 青州市环境监察大队,山东青州262500 |
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| Author_FL | DENG Yin-zhou PANG Ying-ming GAO Song LIU Yuan-yuan ZHANG Lan-ying LIU Na LI Yu-qin |
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| DOI | 10.15898/j.cnki.11-2131/td.2015.04.017 |
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| DocumentTitleAlternate | Determination of Organophosphorus Pesticides in Groundwater by Gas Chromatography Coupled with Closed Ultrasound Circulating Purge Needle Trap |
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| Keywords | 气相色谱法 针捕集 地下水 organophosphorus pesticides extraction by purge 有机磷农药 needle trap groundwater Gas Chromatography 吹扫提取 |
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| Notes | groundwater;organophosphorus pesticides;needle trap;extraction by purge;Gas Chromatography Based on the merits of solvent-free extraction of gaseous samples by needle trap,closed circulating purge system consisting of needle trap and water sample by peristaltic pump is established to enhance the Henry ’s law constant of analytes in the gas/liquid phase. In this study,the method for determination of dichlorvos,phorate, methyl parathion and malathion in groundwater by circulating extraction with needle trap coupled with Gas Chromatography was established. This method integrated sampling,extraction,purification,concentration,and chromatography. The optimum conditions for the extraction by needle trap include sampling flow rate of 11. 11 mL/min and extraction temperature of 40℃. Under these conditions,the maximum breakthrough volume of 1 mg/L methyl parathion is 600 mL. The recoveries range from 62. 3% to 103. 0% for 5 μg/L,50 μg/L and 200 μg/L analytes. Low level dichlorvos has a relative standard deviation of 26 |
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| Publisher | 吉林大学环境与资源学院，吉林 长春130021 教育部地下水资源与环境重点实验室，吉林 长春130021%深圳出入境检验检疫局,广东深圳,518067%青州市环境监察大队,山东青州,262500 |
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| Snippet | 基于针捕集适于免溶剂提取气态介质样品的特点，通过蠕动泵将针捕集与水样组成闭合循环吹扫系统，提高目标物的水样/顶空亨利系数，建立了针捕集闭合循环提取耦合气相色谱快... O658.2%O657.71%S482.33; 基于针捕集适于免溶剂提取气态介质样品的特点，通过蠕动泵将针捕集与水样组成闭合循环吹扫系统，提高目标物的水样/顶空亨利系数，建立了针捕集闭... |
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| SubjectTerms | 吹扫提取 地下水 有机磷农药 气相色谱法 针捕集 |
| Title | 闭合超声循环吹扫针捕集动态提取-气相色谱法测定地下水中的4种有机磷农药 |
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