固相萃取-高效液相色谱法测定城市污水中痕量多环芳烃的研究 |
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引用本文: | 荣楠,王靖飞,康全影,吴亦红,李洪波.固相萃取-高效液相色谱法测定城市污水中痕量多环芳烃的研究[J].安徽农业科学,2012,40(1):451-453. |
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作者姓名: | 荣楠 王靖飞 康全影 吴亦红 李洪波 |
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作者单位: | 1. 河北大学化学与环境科学学院,河北保定071002;河北省环境科学研究院河北省水环境科学实验室,河北石家庄050037 2. 河北省环境科学研究院河北省水环境科学实验室,河北石家庄,050037 |
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基金项目: | 国家水体污染控制与治理科技重大专项 |
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摘 要: | 目的]采用固相萃取-高效液相色谱法测定城市污水中痕量多环芳烃.方法]从固相萃取柱、洗脱溶剂、洗脱体积、洗脱速度等方面,对固相萃取-反相高效液相色谱法的试验条件进行优化,并检测城市污水中痕量多环芳烃。结果]优化得到的固相萃取条件为:选择SUPELCLEAN LC-18固相萃取柱;以二氯甲烷为洗脱溶剂,洗脱体积为15 ml,分3次洗脱,洗脱速度为2 ml/min;上样速度为5ml/min,上样体积为1 000 ml,并向水样添加200 ml甲醇作有机改性溶剂。在该萃取条件下,该方法的加标回收率高,为76.3%~105.2%;相对标准偏差为3.8%~6.0%,精密度好;检出限低,为0.000 8~0.048μg/L。结论]固相萃取-反相高效液相色谱法操作简便,灵敏度高,精密度好,适用于大体积水样连续测定。
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关 键 词: | 固相萃取 高效液相色谱 多环芳烃 城市污水 |
Study on the Determination of Trace Amount of Polycyclic Aromatic Hydrocarbons in Urban Sewage by Solid-phase Extraction Coupled with High Performance Liquid Chromatograph |
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Institution: | RONG Nan et al(College of Chemistry and Environmental Science,Hebei University,Baoding,Hebei 071002) |
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Abstract: | Method] The study aimed at determining trace amount of polycyclic aromatic hydrocarbons(PAHs) in urban sewage by using solid-phase extraction(SPE) coupled with high performance liquid chromatograph(HPLC).Method] From the aspects of solid-phase extraction column,elution solvent,elution volume,elution speed and so forth,the test conditions of SPE-HPLC method were optimized,and trace amounts of PAHs in urban sewage was determined by this method.Result] The optimized solid-phase extraction conditions were SUPELCLEAN LC-18 solid-phase extraction column,methylene dichloride as elution solvent,15 ml elution volume,2 ml/min elution speed,5 ml/min loading speed,1 000 ml water with 200 ml methanol loading volume.Under the optimized extraction conditions,the average recovery was high,namely 76.3%-105.2%;relative standard deviation was 3.8%-6.0%,showing good precision;detection limit was low,only 0.000 8-0.048 μg/L.Conclusion] The method is user-friendly,with high sensitivity and good precision,and suitable for continuous determination of a large volume of water. |
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Keywords: | Solid-phase extraction(SPE) High performance liquid chromatograph(HPLC) Polycyclic aromatic hydrocarbons(PAHs) Urban sewage |
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