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研究生： 梁美怡
Mei-I Leong
論文名稱： 冷凝分散液液微萃取法
A New Dispersive Liquid-Liquid Microextraction Method Based On Solidfication of Floating Organic Drop
指導教授： 黃賢達
Shang-Da Huang
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： 2008
畢業學年度： 96
語文別： 中文
論文頁數： 90
中文關鍵詞： 分散液液微萃取法 、氯苯
相關次數： 點閱：1  下載：0 
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    • 鹵素化合物是常見的環境污染物之一，如本文所檢測分析物為1,2-二氯苯、1,2,4-三氯苯、四氯乙烯、六氯丁二烯及4-溴苯基苯基醚等，此類化合物均被美國環境保護局列為初級污染物，已進行水樣測試。這些染污物的測試在大部分的環境樣品中必需達到微量分析的等級。此篇論文的目的是開發低毒性且快速分離的方法，萃取存在於自然環境水樣中各分析的含量。
    本實驗所採用冷凝分散液液微萃取 ( Dispersive liquid-liquid microextraction method based on solidfication of floating organic drop ) 是一個簡單且快速萃取的方法，其使用低密度、低毒性有機溶劑取代一般分散液液微萃取法中所使用的含氯高毒性溶劑。本實驗將挑戰分析物在溶劑被沖提前先出來，即使在萃取溶劑的干擾下仍能正常操作。選用的萃取溶劑為2-十二烷醇 ( 2-Dodecanol )，分散溶劑為丙酮，根據兩種成分的溶劑系統，透過萃取溶劑及分散溶劑注入樣品中進行快速萃取，經過離心後再進行冰浴，取出萃取液滴，再利用氣相層析儀搭配電子捕捉器及氣相層析質譜儀進行分析及比對。

    目 錄 中文摘要…………………………………………………………….…………..2 英文摘要…………………………………………………………….…………..3 目錄……………………………………………………………………….….……..4 表目錄……………………………………………………………….………….…..7 圖目錄………………………………………………………………….….……..8 一 緒論……………………………………………………………..10 1.1 前言……………………………………………………………10 1.2 水中鹵素化合物………………………………….. …………..11 1.3 各種微萃取方法探討………………….……………..………..15 1.3.1 固相微萃取法………………………………………15 1.3.2 液相微萃取法………………………………………16 1.3.3 分散液液微萃取法…………………………………19 1.3.4 冷凝液液微萃取法…………………………………19 1.3.5冷凝分散液液微萃取法……………………………20 1.4 研究目的………………………………………………………21 1.5 分析物檢測方法………………………………………………22 二 實驗部分………………………………………………………….24 2.1 實驗藥品………………………………………………………24 2.2 實驗裝置……………………………………………………25 2.3 實驗儀器……………………………………………………26 三 實驗結果 …………………………………………………………28 3.1濃縮係數率、萃取回收率及相對回收率…………………..28 3.2 DLLME-SFO萃取條件選擇………………………………..…29 3.2.1 萃取溶劑的選擇………………………………………29 3.2.2 分散溶劑的選擇………………………………………31 3.2.3 不同的分散注入方式…………………………………31 3.2.4萃取溶劑體積的影響…………………………………32 3.2.5分散溶劑體積的影響……………………………33 3.2.6 鹽類的添加……………………………………………34 3.2.7 萃取溫度的影響………………………………………36 3.2.8 萃取靜止時間的影響…………………………………37 3.3定量及環境樣品分析. ………………………………………….38 3.3.1 環境樣品分析……………………………………….38 (一) 氣相層析電子捕捉檢測器 3.3.2 偵測極限…………………………………………….40 3.3.3 回收率與再現性…………………………………….41 3.3.4 冷凝分散液液萃取法與常用液相微萃取法比較….41 (二) 氣相層析質譜儀 3.3.5 分析物離子碎片選擇……………………………….44 3.3.6 偵測極限…………………………………………….44 3.3.7 回收率與再現性…………………………………….45 3.3.8 冷凝分散液液萃取法與常用液相微萃取法比較….45 3-3-9 氣相層析電子捕捉檢測器與質譜儀之分析結果比較 ……………………………………………………….46 3.4 結論. ………………………………………………………….49 3.5 References………………………………………………51 表格索引 表一 Tetrachloroethylene 的基本資料…………………………….58 表二 1,2-Chlorobenzene 的基本資料…………………………….59 表三 1,2,4-Chlorobenzene 的基本資料…………………………..60 表四 Hexachlorobutadiene 的基本資料…………………………..60 表五 4-bromodiphenyl ether的基本資料………………………….62 表六 全國飲用水中各分析物建議標準含量.………………………63 表七 萃取溶劑的溶點、沸點及密度………………………………..64 表八 分散液液萃取法使用的高毒性有機萃取溶劑.. ……………..65 表九 其他液液萃取法對本實驗各分析物之偵測極限…………….66 表十 冷凝分散液液萃取法對各分析物的定量結果……………….67 表一 真實樣品中(自來水及河水)GC/ECD分析結果………..……68 表二 分析物滯留時間、離子碎片及掃描時間列表…………………69 表三 冷凝分散液液萃取法對各分析物的定量結果………………. 70 表四 真實樣品中(自來水及河水)GC/MS分析結果……………….71 圖片索引 圖一 固相微萃取法……………………………………………………72 圖二 懸掛液滴液液微萃取法…………………………………………73 圖三 中空纖維的兩相/三相模式的液-液/液-液-液微萃取法……… 74 圖四 溶劑棒微萃取法…………………………………………………75 圖五 分散液液微萃取法………………………………………………76 圖六 冷凝懸浮低溶點的有機液滴-液液微萃取…………………..…77 圖七 冷凝懸浮低溶點的有機液滴-液液微萃取法的層析圖譜……..77 圖八 冷凝分散液液微萃取法…………………………………………78 圖九 選擇合適的萃取溶劑……………………………………………79 圖十 選擇合適的分散溶劑進行萃取…………………………………80 圖十一 選擇合適的注射方法……………………………………….81 圖十二 萃取溶劑體積的影響……………………………………….82 圖十三 萃取溶劑體積的影響……………………………………….83 圖十四 分散溶劑體積的影響……………………………………….84 圖十五 鹽類的添加……………………………………………….…85 圖十六 萃取時間的影響…………………………………………….86圖十七 冷凝分散液液微萃取法得到的自來水氣相層析圖譜 (GC/ECD)…………………………………………………...87 圖十八 冷凝分散液液微萃取法得到的湖水氣相層析圖譜(GC/ECD)…………………………………………………...88 圖十九 冷凝分散液液微萃取法得到的自來水氣相層析圖(GC/MS). ……………………………………………………89 圖二十 冷凝分散液液微萃取法得到的湖水氣相層析圖(GC/MS)……………………………………………………..90

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