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| 研究生： |
熊思媛 Szu-yuan Hsiung |
|---|---|
| 論文名稱： |
以PFPH衍生試劑搭配氣相層析質譜儀檢測大氣中醛酮化合物 |
| 指導教授： |
王家麟
Jia-lin Wang |
| 口試委員: | |
| 學位類別： |
碩士 Master |
| 系所名稱： |
理學院 - 化學學系 Department of Chemistry |
| 畢業學年度： | 99 |
| 語文別： | 中文 |
| 論文頁數： | 101 |
| 中文關鍵詞： | 衍生法 、醛酮化合物 |
| 外文關鍵詞： | carbonyl compounds, derivatization |
| 相關次數： | 點閱：4 下載：0 |
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本研究建立一套常見氣態醛酮化合物檢測方法，針對甲醛、乙醛、丙酮、丙醛、丙烯醛、2-丁酮六種常見醛酮類化合物進行實驗方法設計，並利用自製滲透管配製標準樣品作為定量依據。嘗試自行製作以矽膠(silica gel)作為吸附介質之吸附管，將衍生試劑PFPH (pentafluorophenyl hydrazine)塗佈於Silica gel中，採樣同時進行空氣樣品之捕捉以及衍生化工作，再以熱脫附系統搭配氣相層析質譜儀(GC/MS)進行分析，相較於傳統分析方法以2,4-DNPH (2,4-dinitrophenylhydrazine)衍生物之高效能液相層析測定法，採樣後需經過萃取濃縮等樣品前處理步驟，並且需使用有機溶劑作為沖提液，本研究分析方法不需經過樣品前處理，且商業熱脫附儀具有自動進樣的功能，簡化了分析程序，並節省吸附劑成本的開銷。
採樣管內含100 mg之Silica gel，並於其上塗佈6 μmol PFPH衍生劑，以流速30/min採集六種醛酮化合物，採集效率可達93%以上，經過分析方法評估後，表現穩定性佳，且檢量線線性關係R2亦可達0.990以上。在實際應用於大氣量測上，同時與現行公告之標準方法進行分析方法比對，比對結果具有同調性，相關係數R2大於0.8，成功驗證了本實驗以PFPH採樣管搭配GC/MS的分析方法，展現對於大氣中醛酮化合物之檢測潛力。
The conventional method for the determination of gaseous carbonyls is to collect air onto a solid sorbent cartridge coated with 2,4-dinitrophenyl hydrazine (2,4-DNPH), followed by solvent extraction and HPLC/UV analysis. A new approach of coupling on-sorbent derivatization with thermal desorption was demonstrated. This method involves collection of carbonyls, such as formaldehyde, acetaldehyde, acetone, propionaldehyde, acrolein, and 2-butanone, onto pentafluorophenyl hydrazine (PFPH) coated Silica gel sorbent packed in a tube, followed by thermal desorption and GC/MS analysis of the PFPH-derivatives. Carbonyls are shown to be effectively collected (>93% collection efficiency) onto sampling tubes which were loaded with 6μmol PFPH per 100 mg Silica gel and operated at a sampling flow rate of 30 mLmin-1.
The method was field-tested and compared with the most commonly used HPLC/UV method. Good agreement (correlation coefficient >0.8) between two methods was found. The incorporation of derivative agent in the solid sorbent coupled with thermal desorption techniques was established, demonstrating feasibility of this analytical approach for carbonyls measurements.
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