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研究生:歐詠喆
論文名稱:水浴加熱與微波輔助加熱頂空固相微萃取水樣品多環芳香烴碳氫化合物之研究
指導教授:徐永源徐永源引用關係
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:2003
畢業學年度:91
語文別:中文
論文頁數:107
中文關鍵詞:多環芳香烴固相微萃取
相關次數:
  • 被引用被引用:3
  • 點閱點閱:498
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  • 下載下載:42
  • 收藏至我的研究室書目清單書目收藏:2
本研究為利用固相微萃取技術(Solid-phase microextraction,簡稱SPME)及磁轉子吸附萃取(Stir bar sorptive extraction,簡稱SBSE)以傳統水浴與微波加熱吸附吸附的方法(water- bath microwave-assisted sorptive extraction):水浴頂空固相微取萃(water- bath headspace solid-phase microwave extraction, WB-HSSPME)、微波頂空固相微取萃(microwave-assisted headspace solid-phase microwave extraction, MA-HSSPME)、水浴頂空磁轉子吸附取萃(water-bath headspace solid-phase microwave extraction, WB-HSSBSE)、微波頂空磁轉子吸附取萃(microwave-assisted headspace solid-phase microwave extraction, MA-HSSBSE),探討用以分析水中多環芳香烴化合物的可能性。萃取時間、萃取溫度、加鹽種類、添加氯化鈉比例,為實驗中尋找最佳化條件探討的參數。實驗結果發現,WB-HSSBSE在100oC、添加4克NaCl、60分鐘時為實驗最佳條件。線性範圍100∼0.01ng/L,最低偵測極限0.000247∼0.077769ng/L,其r2>0.99。並以此方法檢驗真實水樣品。
The one-step microwave-assisted headspace stir bar sorptive extraction ( MA-HSSBSE ) technique for the extraction of polynuclear aromatic hydrocarbons ( PAHs ) in aqueous sample followed by gas chromatography with mass detector ( GC/MSD ). In HSSBSE enrichment is performed on a thick film of polydimethylsiloxane ( PDMS ) coated onto a stir bar incorporated in a glass jacket. Sampling is done by placing the PDMS stir bar in the headspace to absorb the analyte in the gas phase on the top of the aqueous sample.The stir bar is then thermally desorbed on-line with capillary GC-MS.
The optimized condition for obtaining extraction efficiency, such as extraction time, extraction temperature, addition of salt were investigated. Experimental result indicate that the optimized MA-HSSBSE technique is 60 min at 100 °C with addition of 4g NaCl,was applied on the real aqueous sample and spiked nature water. The linear range is between 100 and 0.01 ng/l with r2>0.99.The limit of detection is between 0.000247 and 0.077769 ng/l.
目錄
中文摘要--------------------------------------------------------------------------Ⅰ
英文摘要--------------------------------------------------------------------------II
目錄--------------------------------------------------------------------------------III
圖次------------------------------------------------------------------------------VIII
表次-------------------------------------------------------------------------------XI
第壹章 緒論-----------------------------------------------------------------------1
Ⅰ-1前言---------------------------------------------------------------------1
Ⅰ-2微波---------------------------------------------------------------------2
Ⅰ-2-1微波發展簡介-------------------------------------------------2
Ⅰ-2-2微波加熱原理-------------------------------------------------3
Ⅰ-2-3微波特性-------------------------------------------------------7
Ⅰ-2-4影響微波的因素----------------------------------------------8
Ⅰ-2-5微波萃取機制-----------------------------------------------10
Ⅰ-2-6微波加熱法與傳統加熱法的比較-----------------------11
Ⅰ-2-7微波裝置圖--------------------------------------------------12
Ⅰ-3固相微萃取-----------------------------------------------------------15
Ⅰ-3-1固相微萃取發展簡介--------------------------------------15
Ⅰ-3-2固相微萃取和頂空固相微萃取的原理-----------------18
Ⅰ-3-3固相微萃取的特點-----------------------------------------20
Ⅰ-4多環芳香烴化合物--------------------------------------------------21
Ⅰ-4-1 多環芳香烴化合物簡介----------------------------------21
Ⅰ-4-2 多環芳香烴化合物的性質-------------------------------24
Ⅰ-4-3 環境中多環芳香烴化合物之分佈情況----------------27
Ⅰ-4-4 環境樣品中多環芳香烴化合物分析之相關文獻----28
Ⅰ-5研究目的---------------------------------------------------------------35
第貳章 實驗---------------------------------------------------------------------37
Ⅱ-1實驗流程---------------------------------------------------------------37
Ⅱ-2實驗溶劑及標準品---------------------------------------------------38
Ⅱ-2-1藥品與試劑----------------------------------------------------38
Ⅱ-2-2 標準品---------------------------------------------------------38
Ⅱ-2-3 內標準品溶液------------------------------------------------39
Ⅱ-3 實驗儀器設備----------------------------------------------------------40
Ⅱ-3-1 實驗儀器裝置圖---------------------------------------------40
Ⅱ-4 分析儀器----------------------------------------------------------------42
Ⅱ-4-1氣相層析質譜儀(GC-MS)---------------------------------42
Ⅱ-4-2熱脫附冷凝系統氣相層析質譜儀(TDS-CIS-GC-MS)------------------------------------------------------------------43
Ⅱ-4-3氣相層析質譜儀選擇離子監測模式----------------------44
Ⅱ-5 固相微萃取相纖維的活化-------------------------------------------45
Ⅱ-6 固相微萃取磁轉子的活化-------------------------------------------45
Ⅱ-7 微波輔助頂空固相微萃取萃取分析水中多環芳香烴的探討
--------------------------------------------------------------------------46
Ⅱ-7-1萃取時間對微波輔助頂空固相微萃取的影響----------46
Ⅱ-7-2萃取溫度對微波輔助頂空固相微萃取的影響----------46
Ⅱ-7-3 添加鹽類對微波輔助頂空固相微萃取的影響---------47
Ⅱ-7-4 添加不同鹽類對微波輔助頂空固相微萃取的影------47
Ⅱ-8 微波輔助頂空磁轉子吸附萃取分析水中多環芳香烴的探討
--------------------------------------------------------------------------48
Ⅱ-8-1萃取時間對微波輔助頂空磁轉子吸附萃取的影-------48
Ⅱ-8-2萃取溫度對微波輔助頂空磁轉子吸附萃取的影響----49
Ⅱ-8-3 添加不同比例氯化鈉對微波輔助頂空磁轉子吸附萃取的影響--------------------------------------------------------49
Ⅱ-8-4 添加不同鹽類對微波輔助頂空磁轉子吸附萃取的影響-----------------------------------------------------------------50
Ⅱ-9 比較傳統水浴加熱萃取和微波加熱萃取的不同----------------50
Ⅱ-10 以微波輔助頂空磁轉子吸附萃取的檢量線和偵測極限-----51
Ⅱ-11 真實樣品的檢測-----------------------------------------------------51
第參章 結果與討論-----------------------------------------------------------53
Ⅲ-1 直接注射法分析多環芳香烴標準溶液氣相層析圖-------------53
Ⅲ-2 微波輔助頂空固相微萃取分析水中多環芳香烴的探討-------53
Ⅲ-2-1 以微波輔助頂空固相微萃取分析多環芳香烴標準溶液氣相層析圖---------------------------------------------------53
Ⅲ-2-2 萃取時間對微波輔助頂空固相微萃取萃取的影-------56
Ⅲ-2-3 萃取溫度對微波輔助頂空磁轉子吸附萃取的影響----57
Ⅲ-2-4 添加氯化鈉對微波輔助頂空固相微萃取萃取的影響------------------------------------------------------------------57
Ⅲ-2-5 添加不同鹽類對微波輔助頂空磁轉子吸附萃取的影響------------------------------------------------------------------65
Ⅲ-3 直接注射法分析多環芳香烴標準溶液熱脫附冷凝系統氣相層析圖---------------------------------------------------------------------68
Ⅲ-4 微波輔助頂空磁轉子吸附萃取分析水中多環芳香烴的探討---------------------------------------------------------------------------68
Ⅲ-4-1 以微波輔助頂空磁轉子吸附萃取分析多環芳香烴標準溶液熱脫附冷凝系統氣相層析圖------------------------68
Ⅲ-4-2萃取時間對微波輔助頂空磁轉子吸附萃取的影--------71
Ⅲ-4-3萃取溫度對微波輔助頂空磁轉子吸附萃取的影響-----71
Ⅲ-4-4 添加氯化鈉對微波輔助頂空磁轉子吸附萃取的影響------------------------------------------------------------------72
Ⅲ-4-5 添加不同鹽類對微波輔助頂空磁轉子吸附萃取的影響------------------------------------------------------------------79
Ⅲ-5 比較傳統水浴加熱和微波加熱頂空磁轉子吸附萃取的不同---------------------------------------------------------------------------82
Ⅲ-6 比較微波輔助頂空磁轉子吸附萃取和微波輔助頂空固相微萃取萃取的不同---------------------------------------------------------89
Ⅲ-7 以微波輔助頂空磁轉子吸附萃取的檢量線和偵測極限-------91
Ⅲ-8 真實樣品的檢測-------------------------------------------------------93
第四章 結論---------------------------------------------------------------------96
參考文獻--------------------------------------------------------------------------98
圖次
圖 Ⅰ-2-1 電磁波波長圖譜----------------------------------------------------5
圖 Ⅰ-2-2分子與電磁場作用圖-----------------------------------------------8
圖 Ⅰ-2-3 微波和傳統水浴加熱比較圖------------------------------------11
圖 Ⅰ-2-4 微波阻斷循環器作用圖------------------------------------------12
圖 Ⅰ-2-5 密閉式微波萃取裝置圖------------------------------------------13
圖 Ⅰ-2-6 開放式微波萃取裝置圖------------------------------------------14
圖 Ⅰ-2-7 聚焦式微波萃取裝置圖------------------------------------------14
圖 Ⅰ-3-1 固相微萃取之流程圖---------------------------------------------16
圖 Ⅰ-3-2 商業化的固相微萃取裝置---------------------------------------17
圖 Ⅰ-3-3 固相微萃取的分配示意圖---------------------------------------19
圖 Ⅰ-3-4頂空固相微萃取裝置簡圖----------------------------------------21
圖 Ⅱ-3-1微波輔助頂空固相微萃取裝置圖-------------------------------40
圖 Ⅱ-3-2 頂空固相微萃取裝置圖------------------------------------------41
圖 Ⅱ-3-3 頂空磁轉子吸附裝置圖-----------------------------------------41
圖 Ⅱ-3-4 熱脫附-冷凝系統儀器裝置圖-----------------------------------42
圖 Ⅲ-1:以直接注入法注入GC-MS分析標準溶液層析圖-------------54
圖 Ⅲ-2:以微波輔助頂空固相微萃取分析多環芳香烴標準溶液層析圖---------------------------------------------------------------------55
圖 Ⅲ-3:萃取時間對微波輔助頂空固相微萃取的影響-----------------59
圖 Ⅲ-4:萃取時間對傳統水浴加熱頂空固相微萃取的影響-----------60
圖 Ⅲ-5:萃取溫度對微波輔助頂空固相微萃取的影響-----------------61
圖 Ⅲ-6:萃取溫度對傳統水浴加熱頂空固相微萃取的影響-----------62
圖 Ⅲ-7:添加氯化鈉對微波輔助頂空固相微萃取的影響--------------63
圖 Ⅲ-8:添加氯化鈉對傳統水浴加熱頂空固相微萃取的影響--------64
圖 Ⅲ-9:添加不同鹽類對微波輔助頂空固相微萃取的影響-----------66
圖 Ⅲ-10:添加不同鹽類對傳統水浴加熱頂空固相微萃取的影響---67
圖 Ⅲ-11:以直接注入法注入TDSCIS GC-MS分析標準溶液層析圖-----------------------------------------------------------------------69
圖 Ⅲ-12:以微波輔助頂空磁轉子吸附萃取分析多環芳香烴標準溶液層析圖--------------------------------------------------------------70
圖 Ⅲ-13:萃取時間對微波輔助頂空磁轉子吸附萃取的影響----------73
圖 Ⅲ-14:萃取時間對傳統水浴加熱頂空磁轉子吸附萃取的影-------74
圖 Ⅲ-15:萃取溫度對微波輔助頂空磁轉子吸附萃取的影響----------75
圖 Ⅲ-16:萃取溫度對傳統水浴加熱頂空磁轉子吸附萃取的影響---76
圖 Ⅲ-17:添加氯化鈉對微波輔助頂空磁轉子吸附萃取的影響-------77
圖 Ⅲ-18:添加氯化鈉對傳統水浴加熱頂空磁轉子吸附萃取的影響-----------------------------------------------------------------------78
圖 Ⅲ-19:添加不同鹽類對微波輔助頂空磁轉子吸附萃取的影響---80
圖 Ⅲ-20:添加不同鹽類對傳統水浴加熱頂空磁轉子吸附萃取的影響-----------------------------------------------------------------------81
圖 Ⅲ-21-a:微波和傳統水浴15min頂空磁轉子吸附萃取的比較-----83
圖 Ⅲ-21-b:微波和傳統水浴30min頂空磁轉子吸附萃取的比較-----84
圖 Ⅲ-21-c:微波和傳統水浴45min頂空磁轉子吸附萃取的比較-----85
圖 Ⅲ-21-d:微波和傳統水浴60min頂空磁轉子吸附萃取的比較-----86
圖 Ⅲ-21-e:微波和傳統水浴75min頂空磁轉子吸附萃取的比較-----87
圖 Ⅲ-21-f:微波和傳統水浴90min頂空磁轉子吸附萃取的比較-----88
圖 Ⅲ-22 比較微波輔助頂空磁轉子吸附萃取和微波輔助頂空固相微
萃取萃取的不同-----------------------------------------------------90
圖 Ⅲ-23:以微波輔助頂空磁轉子吸附萃取檢量線----------------------92
圖 Ⅲ-24 以微波輔助頂空磁轉子吸附萃取真實樣品層析圖----------95
表次
表Ⅰ-2-1 工業、科學及醫學使用的微波範圍 ( ISM Bands )------------5
表Ⅰ-2-2 於3 GHz和25Oc下,各物質之介電常數與散逸係數---------7
表Ⅰ-4-1 十六種列管多環芳香碳氫化合物之結構圖-------------------22
表Ⅰ-4-2 PAHs之物化性質--------------------------------------------------26
表Ⅲ-1 多環芳香烴的線性相關係數和偵測極限-------------------------90
表Ⅲ-2 多環芳香烴真實樣品中的含量-------------------------------------93
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