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研究生:林世宗
研究生(外文):Shih - Tsung Lin
論文名稱:以微波輔助萃取飛灰中戴奧辛及呋喃之研究
論文名稱(外文):Microwave-Assisted Extraction of Polychlorinated Dioxins and Furans from Fly Ash
指導教授:徐永源徐永源引用關係張簡國平張簡國平引用關係
指導教授(外文):Youn Yuen ShuGuo Ping Chang Chien
學位類別:碩士
校院名稱:國立高雄師範大學
系所名稱:化學系
學門:自然科學學門
學類:化學學類
論文種類:學術論文
論文出版年:2002
畢業學年度:90
語文別:中文
論文頁數:117
中文關鍵詞:戴奧辛微波輔助萃取毒性當量
外文關鍵詞:Dioxin(PCDDs)Furan(PCDFs)Microwave - Assisted ExtractionToxicity Equivalency Quantity
相關次數:
  • 被引用被引用:5
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本研究利用微波輔助萃取(microwave-assisted extraction, MAE)飛灰中戴奧辛及呋喃(PCDDs/PCDFs),微波輔助萃取方法已廣泛使用在檢測有機氯農藥、多環芳香碳氫化合物、酚類化合物、多氯聯苯等,它優點為縮短萃取時間(10-30 min)、降低溶劑使用量(10-50 mL)以及可同時對三∼十二個樣品進行萃取,可達到快速、高效率及低溶劑需求的優點,並已被加拿大環境部與美國環保署公告為標準方法。
戴奧辛及呋喃之檢測方法傳統上均以索氏萃取法為主,由瑞典Umeå大學主辦之第五屆2000年國際戴奧辛實驗室比測資料統計檢測飛灰共計五十七實驗室,除了八家使用加速溶劑萃取法(ASE)其餘皆使用索氏萃取法,顯示檢測戴奧辛及呋喃使用微波輔助萃取方法尚未被廣泛使用,本研究樣品來源使用上述比測飛灰樣品。
本研究利用微波輔助萃取及參考USEPA Method 1613B 分析方法,經萃取、濃縮及淨化完全後,利用13C-同位素標幟稀釋法(Isotope Dilution Method),再以高解析氣相層析/高解析質譜儀(HRGC/HRMS)為定量分析儀器。所進行的實驗使用密閉式微波萃取方式,以不同溶劑組成的變化作探討,並以索氏萃取法之測出值作為比較,驗證其方法可行性,實驗所得戴奧辛及呋喃總毒性當量濃度值在該比測公布值可接受範圍內。
Microwave-Assisted Extraction (MAE) has been used as a sample preparation technique and applied in the extraction of polychlorinated biphenyls (PCBs), polycyclic aromatic hydrocarbons (PAHs), and organochlorine pesticides (OCPs) from variety of environmental samples. This study deals with using of MAE technique to extract Polychlorinated Dioxins and Furans (PCDDs / PCDFs) from fly ash samples provided by Umeå University used for the 5th Round of the International Intercalibration Study in the year or 2000.
The extraction conditions were carried out at 100 oC under pressure in closed vessels with 20 ml of 20%, 40%, 60% and 80% toluene-acetone for 10 and 20 minutes. The extracts were concentrated under reduced pressure, column cleaned, and quantified by high resolution gas chromatograph-high resolution mass spectrometer. Comparison between MAE and a 24-hour Soxhlet extraction showed that both methods provided acceptable results within a range of one standard deviation of the intercalibration study result. The quantity of PCDDs/PCDFs extracted by MAE with 60% toluene-acetone is higher than that obtained from Soxhlet method in this laboratory. MAE has advantages over Soxhlet technique due to a faster extraction time and lower quantity of solvent used, and bulletined as a standard method by Environment Canada and Environmental Protection Agency of the United States.
目 錄
中文摘要 ……………………………………………………….. I
英文摘要 ……………………………………………………….. II
目錄 ……………………………………………………………… III
表目錄 …………………………………………………………... VII
圖目錄 …………………………………………………………... X
相關名詞及單位符號 ………………………………………. XI
第壹章 緒論 ………………………………………………… 1
1-1前言 …………………………………………………………… 1
1-2研究目的 ……………………………………………………… 2
第貳章 文獻回顧 ………………………………………… 6
2-1戴奧辛的性質與特性 ………………………………………… 6
2-2戴奧辛產生的來源 …………………………………………… 8
2-3戴奧辛的毒性計量 …………………………………………… 10
2-4戴奧辛之危害及影響 ………………………………………… 12
2-5飛灰中的戴奧辛 ……………………………………………… 14
2-6微波技術的應用與原理 ……………………………………… 19
2-6-1微波化學 ………………………………………………… 21
2-6-2微波加熱 ………………………………………………… 21
2-6-3微波特性 ………………………………………………… 26
2-6-4黏度(viscosity)對偶極旋轉
(Dipalar Rotation)的影響 …………………………… 28
2-6-5樣品体積大小的影響 …………………………………… 28
2-6-6溫度對介電損失因數的影響 …………………………… 29
2-6-7樣品形狀的影響 ………………………………………… 30
2-6-8微波反應 ………………………………………………… 30
2-6-9微波萃取機制 …………………………………………… 31
2-6-10密閉式微波萃取 .……………………………………… 32
2-7環境樣品中戴奧辛的分析方法 ……………………………… 34
第參章 研究方法與設備 ……………………………... 41
3-1研究流程規劃 ………………………………………………… 41
3-2實驗試劑與藥品………………………………………………. 41
3-2-1實驗溶劑 ………………………………………………… 41
3-2-2藥品配製 ………………………………………………… 43
3-3實驗儀器設備 ………………………………………………… 44
3-4實驗條件之設計 ……………………………………………… 45
3-5器皿之清洗 …………………………………………………… 46
3-6樣品前處理 …………………………………………………… 48
3-6-1微波萃取條件的探討 …………………………………… 48
3-6-2微波萃取步驟 …………………………………………… 49
3-6-3索氏萃取步驟 ……………………………………………46 50
3-6-4硫酸酸洗 ………………………………………………… 51
3-6-4-1硫酸酸洗步驟 ……………………………………… 51
3-6-5多層矽膠管柱淨化 ……………………………………… 52
3-6-5-1多層矽膠管柱淨化步驟 …………………………… 53
3-6-6酸性氧化鋁管柱淨化 …………………………………… 54
3-6-6-1酸性氧化鋁管柱淨化步驟 ………………………… 55
3-6-7活性碳管柱淨化 ………………………………………… 56
3-6-7-1活性碳管柱淨化步驟 ……………………………… 56
3-7高解析氣層析/高解析質譜儀分析條件 ……………………… 57
3-8檢量線之建立與品保品管規範 ……………………………… 58
3-8-1滯流時間窗建立 ………………………………………… 58
3-8-2建立檢量線 ……………………………………………… 61
3-8-3檢量線查核 ……………………………………………… 61
3-8-4檢量線績效查核 ………………………………………… 62
3-8-5層析管柱解析度查核 …………………………………… 62
3-8-6訊譟比 …………………………………………………… 67
3-8-7查核樣品分析 …………………………………………… 68
3-8-8最低可偵測極限 ………………………………………… 69
3-8-9樣品鑑定準則 …………………………………………… 69
3-9計算方法 ……………………………………………………… 72
3-9-1檢量校正標準品待測物相對於內標準品之相
對感應因子…………………………………………… 72
3-9-2檢量校正標準品內標準相對於回收標準品之相
相對感應因子………………………………………… 72
3-9-3檢量校正標準品淨化標準相對於回收標準品之之相
之相對感應因子……………………………………… 73
3-9-4最低可偵測極限 ………………………………………… 73
3-9-5 PCDD/Fs之濃度 ………………………………………… 73
3-9-6內標準品之回收率 ……………………………………… 74
3-9-7淨化標準品之回收率 …………………………………… 74
3-9-8樣品中PCDD/Fs的總毒性當量濃度 …………………… 71
第肆章結果與討論 ………………………………………. 76
4-1不同比例溶劑混合微波萃取之探討 ………………………… 76
4-2索氏萃取檢測數據 …………………………………………… 77
4-3微波萃取與索氏萃取之比較 ………………………………… 88
4-4微波萃取時間的比較 ………………………………………… 93
4-5內標準品及淨化標準品回收率 ……………………………… 96
4-6結果 …………………………………………………………… 98
第伍章 結論與建議………………………………………議…………………………………………………… 101
第陸章 參考文獻 ………………………………………… 104
附 錄 …………………………………………………………… 111
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