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研究生： 陳仲強
論文名稱： 以液相微萃取法配合高效能液相層析儀偵測水中苯乙酸除草劑
指導教授： 黃賢達
口試委員:
學位類別： 碩士
Master
系所名稱： 理學院 - 化學系
Department of Chemistry
論文出版年： 2005
畢業學年度： 93
語文別： 中文
論文頁數： 69
中文關鍵詞： 液相微萃取法
相關次數： 點閱：3  下載：0 
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    • 本篇論文是以液相微萃取法結合高效能液相層析儀來偵測自然界水樣中的苯乙酸除草劑,本實驗所分析的五種除草劑分別為: Phenoxyacetic acid, o-chlorophenoxyacetic acid,
    p-chlorophenoxyacetic acid, 2,4- dichlorophenoxyacetic acid, 2,4,5-trichlorophenoxyacetic acid◦
    液相微萃取法(LPME)只需微量的有機溶劑及便宜的中空纖維,所以是一種因應環保潮流且符合經濟效益並且快速方便的前處理方法◦利用此萃取法濃縮樣品中苯乙酸除草劑,再以液相層析儀進行分離與定量,探討各種可能影響萃取效率的變因,包括:有機溶劑的選擇、萃取時間、樣品攪拌速度、鹽析效應及濃縮效率,以達到最佳萃取效果(溶劑種類:正八醇、萃取時間:60分鐘、樣品攪拌速度:750rpm、鹽析效應:1.5g氯化鈉、濃縮效率:130~260倍),並將此偵測方法應用於真實樣品(柯子湖)◦
    實驗結果發現,此分析方法的偵測極限可達ng/ml的層級,且再現性佳,線性相關係數(R2)在25∼2000ng/ml的濃度範圍內介於0.9956~0.9996之間,應用於河水分析時,相對回收率都有不錯效果(86.8%~100.7%,concentration:Phen:100 ng/ml; o-,p-,2,4-D:30 ng/ml; 2,4,5-T:50 ng/ml),表基質干擾不嚴重◦

    目錄 第一章 緒論……………………………………………………………1 1-1 前言……………………………………………………………1 1-2 苯乙酸除草劑…………………………………………………2 1-3 傳統有機污染物的前處理方法………………………………3 1-4 目前有機污染物的前處理方法………………………………5 1-5 液相微萃取法…………………………………………………9 1-5-1 液相微萃取原理……………………………………………12 第二章 實驗部分………………………………………………………14 2-1 試藥……………………………………………………………14 2-2 標準溶液和真實樣品…………………………………………14 2-3 儀器裝置………………………………………………………15 2-4 實驗步驟………………………………………………………16 第三章 結果與討論……………………………………………………17 3-1 各種影響變因探討……………………………………………17 3-1-1 有機溶劑的選擇……………………………………………17 3-1-2 萃取時間……………………………………………………17 3-1-3 攪拌速率……………………………………………………18 3-1-4 添加鹽類對萃取之影響……………………………………19 3-1-5 濃縮倍率……………………………………………………19 3-2 各種液液微萃取的比較………………………………………21 3-3 方法偵測極限、精密度和線性………………………………22 3-4 環境樣品的測試………………………………………………23 第四章 結論……………………………………………………………24 第五章 參考文獻………………………………………………………25 表目錄 表一、Phenoxyacetic acid 的基本資料……………………………32 表二、o-chlorophenoxyacetic acid 的基本資料…………………33 表三、p-chlorophenoxyacetic acid 的基本資料…………………34 表四、2,4-dichlorophenoxyacetic acid (2,4-D)的基本資料….35 表五、2,4,5-trichlorophenoxyacetic acid (2,4,5-T)的基本資料……………………………………………………………………… 36 表六、纖維液相微萃取(Hollow fiber LPME)的應用………………37 表七、流動相梯度沖提(gradient mode)……………………………40 表八、濃縮倍率……………………………………………………… 41 表九、方法偵測極限、精密度和線性……………………………… 42 表十、真實樣品(柯子湖溪水)的添加回收率...................43 表十一、自然界水體中苯乙酸除草劑的相關萃取方式………………44 表十二、LPME、SPME及SDME的比較…………………………………45 圖目錄 圖一、環境樣品的分析流程……………………………………………46 圖二、有機污染物的分析流程…………………………………………47 圖三、固相微萃取纖維與固定器………………………………………48 圖四、固相微萃取裝置…………………………………………………49 圖五、單滴微萃取………………………………………………………50 圖六、兩相及三相液液微萃取法………………………………………51 圖七、單滴微萃取(drop-in-drop system)…………………………52 圖八、單滴微萃取(Solvent microextraction into a single drop)53 圖九、注射針管壁形成薄膜層…………………………………………54 圖十、單滴微萃取(Back extraction)………………………………55 圖十一、液相微萃取的原理……………………………………………56 圖十二、利用中空纖維取代單滴微萃取的液相微萃取法……………57 圖十三、五種苯乙酸除草劑的直接注射層析圖………………………58 圖十四、液相微萃取裝置....................................59 圖十五、有機溶劑的影響………………………………………………60 圖十六、萃取時間的影響………………………………………………61 圖十七、攪拌速率的影響………………………………………………62 圖十八、離子強度的影響………………………………………………63 圖十九、動態三相微萃取法……………………………………………64 圖二十、濃縮倍率的比較………………………………………………65 圖二十一、動態三相微萃取法 (LLLME/automated movement of the acceptor phase)……………66 圖二十二、動態三相微萃取法 (LLLME/enhancement of extraction enrichment)…………………67 圖二十三、直接萃取湖水………………………………………………68 圖二十四、添加標準品在湖水中………………………………………69

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