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研究生:陳士&;#23791;
研究生(外文):Chen, Shen-Feng
論文名稱:離心分配層析單相溶劑系統中溶質延散之探討
論文名稱(外文):Examination of Solute Dispersion in Centrifugal Partition Chromatography with a Single Phase
指導教授:余艇
學位類別:碩士
校院名稱:國立交通大學
系所名稱:應用化學系碩博士班
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:2011
畢業學年度:99
語文別:中文
論文頁數:76
中文關鍵詞:離心分配層析儀單相系統溶質延散
外文關鍵詞:centrifugal partition chromatographysingle phasesolutes dispersion
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離心分配層析(centrifugal partition chromatography, CPC)和逆流層析(counter-current chromatography, CCC)都是使用液體為固定相及移動相的分離技術,但是二者流動的特性不相同。我們曾經在CCC螺旋管柱中使用單相系統,對溶質延散行為做過研究,本研究則是對CPC 在單相溶劑系統中,對於溶質延散行為之探討。
我們測試六種分子量大小迥異的溶質。在靜止的CPC 管柱中,其流析的訊號波形之理&;#63809;板數值都相當高,而且理&;#63809;板數是隨著溶質的擴散係數而增大。對個別溶質而言,理&;#63809;板數會隨著流速增加而變大,亦即樣品的延散隨著流速增加而變小。和CCC 不同之處,是在流析過程中,並未有convection peak 和diffusion peak 的出現。在轉動之下,於低流速時,溶質的延散程度隨著轉速的提高而變小,理&;#63809;板數也隨之上升。在高流速下,理&;#63809;板數先隨著轉速增加而變小,當轉速繼續上升時,理&;#63809;板數又隨之上升。探討流體之縱向(axial)和橫向(radial)延散之行為,我們認為在CPC 中之流體,並非像CCC 管柱中會形成穩定之層流(laminar flow),而是兼具層流和紊流兩種性質。
Similar to counter-current chromatography (CCC), centrifugal
partition chromatography (CPC) uses liquids as the stationary and mobile phases, although these two techniques have different hydrodynamic properties. We have investigated the solute dispersion behaviors of CCC in the previous study. In this work, we will examine the CPC solute dispersion in a single phase.
We analyzed six solutes of considerable different molecular weights. Under static conditions, the eluted signals all demonstrated very high theoretical plate numbers (n). The n values increased with the increasing solute diffusion coefficient. In addition, their n values increased as the flow rate was elevated. In other words, the solute dispersion decreased with the increasing flow rate. Contrary to CCC, there appeared no signals with double peaks, i.e. convection and diffusion peaks. Under rotation, the solute dispersion decreased as the rotation speed increased at relatively lower flow rates. Thus, the theoretical plate number also increased. However, under higher flow rates, the n value decreased first with the rotation speed; then increased as the speed became higher. After considering the axial and radial dispersions of the fluid, we concluded that the flow in the CPC apparatus should include laminar and turbulent properties, unlike the stable laminar flow in the CCC.
第一章、緒論............................................................................................ 1
1-1 前言.............................................................................................. 1
1-2 研究背景...................................................................................... 2
1-2-1 離心分配層析儀................................................................ 2
1-2-1-1 離心分配層析的運作原理...................................... 5
1-2-1-2 溶劑系統的選擇...................................................... 7
1-2-1-3 移動相及固定相的流動模式.................................. 8
1-2-1-4 影響固定相滯留量的因素...................................... 9
1-2-1-5 離心分配層析管柱內的移動相和固定相的分佈...
12
1-3 研究動機....................................................................................15
第二章、文獻回顧..................................................................................16
2-1 奈米粒子在空管中的流動訊號.................................................16
2-2 逆流層析儀中單相系統的探討.................................................20
2-3 離心分配層析儀兩相系統之流析訊號.....................................23
第三章、實驗..........................................................................................25
3-1 實驗藥品.....................................................................................25
3-2 實驗儀器.....................................................................................26
3-3 實驗步驟與方法........................................................................27
3-3-1 奈米粒子的合成方法......................................................27
3-3-2 樣品的配製方法...............................................................29
3-3-3 離心分配層析儀操作步驟...............................................29
第四章、實驗結果與討論......................................................................31
4-1 靜止CPC 管柱中固定流速下的波形討論...............................31
4-2 靜止CPC 管柱中改變流速下的波形討論...............................35
4-3 樣品在轉動管柱中的流析探討.................................................40
4-4 結論.............................................................................................63
第五章、附錄..........................................................................................65
5-1 兩種沖提模式的比較................................................................. 65
5-1-1 靜止下的溶質延散比較..................................................65
5-1-2 轉動下的溶質延散比較..................................................67
參考文獻 ..................................................................................................74
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