研究生: |
李惠美 |
---|---|
論文名稱: |
加速溶劑萃取法配合同位素稀釋氣相層析質譜法分析土壤中三十五種多苯環芳香烴化合物之分析方法研究 Application of Ase and Isotope Dilution GC-MS for the Determination of 35 PAHs in Soil Samples |
指導教授: | 吳家誠 |
學位類別: |
碩士 Master |
系所名稱: |
化學系 Department of Chemistry |
畢業學年度: | 85 |
語文別: | 中文 |
論文頁數: | 145 |
中文關鍵詞: | 加速溶劑萃取 、氣相層析火焰離子化分析儀 、同位素西式氣相層析質譜法 、多苯環芳香烴化合物 、索式萃取 |
英文關鍵詞: | ASE, GC-FID, Isotope Dilution GC-MS, PAHs, Soxhlet extraction |
論文種類: | 學術論文 |
相關次數: | 點閱:238 下載:0 |
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加速溶劑萃取法(Accelerated Solvent Extraction, ASE)是目前最新的前處理技術,它利用加高溶劑的溫度及壓力來加速萃取的進行,在ASE的萃取變數中包含了壓力、溫度、溶劑的種類及靜態萃取的時間等。本研究主要採用自組的ASE設備當作三十五種在土壤中PAHs的前處理技術,配合氣相層析火焰離子化分析儀(GC-FID)及同位素稀釋氣相層析質譜法(isotope dilution GC-MS)進行定性與定量的工作。
經過ASE萃取條件的最佳化後,實驗中所得到的最佳化條件壓力為1500psi、溫度130℃、溶劑為CH3CN 靜態萃取時間為5分鐘,整個萃取的過程只需要20分鐘左右。ASE對土壤中PAHs 具有選擇性,因此不需要經過淨化的過程,萃取的過程簡單快速且效率良好。
在實驗中,也將ASE與索式萃取做一個比較,從結果中可發現以ASE萃取土壤中的PAHs其回收率大部分都比索式萃取好。而由CRM 103-100及QCS 345分析的結果更進一步的顯示出整個分析方法的精密性與準確性皆非常的好。而在實際樣品上的偵測,由結果可看出所採樣之土壤中PAHs的含量皆非常的少。
A new technique for sample preparation, accelerated solvent extraction (ASE), that combines elevated temperature and pressure with liquid solvent is utilized in this study to pretreat soil samples for PAH analysis, The effects of various operational parameters (i.e. temperature, pressure, solvent type, extraction time) on the performance of ASE were investigated.The research aims at the development of a new sample pretreatment .technique for 35 polynuclear aromatic hydrocarbons (PAHs) in soil samples with GC-FID and isotope dilution GC-MS.
The analytes are extracted by acetonitrile at 130℃ and 1500 psi within 5 minutes of static extraction.The time for the entire extraction process is 20 minutes.Results demonstrated that the ASE extraction is selective for PAHs.Thus, a further clean-up procedure after ASE is not necessary.The procedure of the extraction is simple and fast.ASE in recovery compared with Soxhlet extraction is higher.The results from CRM 103-100 and QCS345 analyses further vrified the high precision and accuracy of the developed analytical scheme.The result from real samples demonstrated that the concentration of PAHs in soil is low.