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研究生:王書信
研究生(外文):Shue Shing Wang
論文名稱:以微波輔助頂空固相微萃取分析水中多氯聯苯
論文名稱(外文):Analysis of polychlorinated biphenyls in aqueous samples by a novel microwave-assisted solid-phase microextraction
指導教授:徐永源徐永源引用關係
指導教授(外文):Youn Yuen Shu
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:93
中文關鍵詞:多氯聯苯
外文關鍵詞:polychlorinated biphenyls
相關次數:
  • 被引用被引用:16
  • 點閱點閱:433
  • 評分評分:
  • 下載下載:48
  • 收藏至我的研究室書目清單書目收藏:1
摘要
本研究為以聚焦式微波輔助頂空固相微萃取進行分析水中多氯聯苯,並與傳統水浴加熱萃取相比較,探討以微波加熱取代傳統水浴加熱應用於頂空固相微萃取的可能性。
吸附時間、樣品體積-頂空比、加鹽和甲醇效應,為實驗中尋求最佳化條件探討的參數;脫附時間、溫度和深度為固相微萃取纖維在氣相層析注射口的探討參數。實驗中以內標法,檢測20個常見的多氯聯苯 ( 18、28、33、44、52、70、101、105、118、128、138、153、170、180、187、194、195、199、206、209 )。
實驗結果顯示,吸附時間15次,每次: ( 30W,1 min,0W,3 min ),樣品體積 / 頂空體積比為1:1,不加鹽類和甲醇,脫附溫度270 oC,脫附時間3 min,脫附深度4 cm為最佳實驗條件。線性範圍80 ng/L ~ 1ng/L ,最低偵測極限介於 0.27 ~ 1.34 ng/L,其r 2 >0.99 ,RSD介於3.2 ~ 14.3 %。
Abstract
The one-step microwave-assisted headspace solid phase micro-extraction (MA-HSSPME) technique for the extraction of polychlorinated biphenyls (PCBs) in aqueous samples followed by gas chromatography with electron capture detector (GC/ECD) and mass detector (GC/MSD) determination was performed. Extraction of PCBs was done by placing the polydimethylsiloxane (PDMS) fiber in the headspace with the aid of microwave radiation to elevate temperature of the aqueous sample.
The optimized condition, 15 cycles of microwave radiation (one cycle: irradiate with 30 watts of microwave power for 1 min and stop for 3 min), 1:1 volume ratio of sample to headspace with no addition of salt and methanol, was applied on the real aqueous sample and spiked nature water. The linear range is between 80 and 1 ng/L with r2 > 0.99.
目錄
中文摘要----------------------------------------------------Ⅰ
英文摘要----------------------------------------------------Ⅱ
目錄--------------------------------------------------------Ⅲ
圖次--------------------------------------------------------Ⅳ
表次--------------------------------------------------------Ⅴ
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微波發展原理-------------------------------------------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-----------------------------------------------12
Ⅰ-3 固相微萃取----------------------------------------------14
Ⅰ-3-1固相微萃取發展簡介-------------------------------------14
Ⅰ-3-2固相微萃取和頂空相微萃取的原理-------------------------17
Ⅰ-3-3固相微萃取的特點---------------------------------------20
Ⅰ-4多氯聯苯-------------------------------------------------21
Ⅰ-4-1多氯聯苯的介紹-----------------------------------------23
Ⅰ-4-2多氯聯苯的性質-----------------------------------------24
Ⅰ-4-3多氯聯苯的毒性與中毒症狀-------------------------------27
Ⅰ-4-4多氯聯苯環境中的分佈-----------------------------------29
Ⅰ-4-5分析環境樣品中多氯聯苯的方法---------------------------30
Ⅰ-5研究目的-------------------------------------------------32
第貳章 實驗-------------------------------------------------34
Ⅱ-1實驗流程-------------------------------------------------34
Ⅱ-2藥品與試劑-----------------------------------------------34
Ⅱ-2-1溶劑---------------------------------------------------34
Ⅱ-2-2標準品-------------------------------------------------35
Ⅱ-2-3內標準物溶液-------------------------------------------37
Ⅱ-3實驗儀器設備---------------------------------------------38
Ⅱ-4分析儀器-------------------------------------------------39
Ⅱ-4-1氣相層析儀-電子捕捉偵檢器------------------------------39
Ⅱ-4-2氣相層析質譜儀-----------------------------------------39
Ⅱ-5固相微萃取纖維的活化-------------------------------------40
Ⅱ-6固相微萃取纖維最佳化條件的探討---------------------------41
Ⅱ-6-1注射口脫附溫度對分析物脫附面積的影響-------------------41
Ⅱ-6-2注射口熱脫附時間對分析物脫附面積的影響-----------------42
Ⅱ-6-3固相微萃取纖維在汽化室內深度的探討---------------------42
Ⅱ-6-4分析物在固相微萃取纖維的殘留率-------------------------42
Ⅱ-7微波輔助頂空固相微萃取分析水中多氯聯苯的探討-------------43
Ⅱ-7-1不同樣品體積與頂空體積比的探討-------------------------43
Ⅱ-7-2不同萃取時間對微波輔助頂空固相微萃取的影響-------------43
Ⅱ-7-3添加鹽類對微波輔助頂空固相微萃取的影響-----------------44
Ⅱ-7-4添加甲醇對微波輔助頂空固相微萃取的影響-----------------44
Ⅱ-8比較傳統水浴加熱萃取和微波加熱萃取的不同-----------------45
Ⅱ-9以微波輔助頂空固相微萃取的檢量線和偵測極限---------------45
Ⅱ-10真實樣品的檢測------------------------------------------46
第參章 結果與討論-------------------------------------------47
Ⅲ-1直接注射法分析多氯聯苯標準溶液---------------------------47
Ⅲ-2以微波輔助頂空固相微萃取分析多氯聯苯標準溶液-------------47
Ⅲ-3固相微萃取纖維最佳化條件的探討---------------------------50
Ⅲ-3-1脫附溫度對分析物脫附面積的影響-------------------------50
Ⅲ-3-2脫附時間對分析物脫附面積的影響-------------------------50
Ⅲ-3-3固相微萃取纖維在汽化室內深度的探討---------------------53
Ⅲ-3-4分析物在固相微萃取纖維的殘留率-------------------------53
Ⅲ-4微波輔助頂空固相微萃取分析水中多氯聯苯的探討-------------56
Ⅲ-4-1不同樣品體積與頂空空間比的探討-------------------------56
Ⅲ-4-2不同萃取時間對微波輔助頂空固相微萃取的影響-------------57
Ⅲ-4-3添加鹽類對微波輔助頂空固相微萃取的影響-----------------58
Ⅲ-4-4添加甲醇對微波輔助頂空固相微萃取的影響-----------------67
Ⅲ-5比較傳統水浴加熱萃取和微波加熱萃取的不同-----------------67
Ⅲ-6以微波輔助頂空固相微萃取的檢量線和偵測極限---------------75
Ⅲ-7 真實樣品的檢測------------------------------------------76
Ⅲ-7-1 真實樣品的空白實驗------------------------------------76
Ⅲ-7-2 內標法定量--------------------------------------------76
Ⅲ-7-3 加入內標準品檢測真實樣品------------------------------77
Ⅲ-7-4 標準添加法定量----------------------------------------78
結論---------------------------------------------------------84
參考文獻-----------------------------------------------------86
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