研究生: |
陳倩雯 Chen Chien Wen |
---|---|
論文名稱: |
加速溶劑萃取系統與高效能液相層析介面在分析土壤中多苯環芳香烴化合物之方法研究 Interfacing ASE and HPLC for the determination of PAH in soil |
指導教授: |
吳家誠
Wu, Jia-Cheng |
學位類別: |
碩士 Master |
系所名稱: |
化學系 Department of Chemistry |
畢業學年度: | 87 |
語文別: | 中文 |
論文頁數: | 143 |
中文關鍵詞: | 加速溶劑萃取 、氣相層析儀 、高效率液相層析儀 、氣相質譜儀 、多苯環芳香烴化合物 、土壤 、螢光 |
英文關鍵詞: | ASE, GC, HPLC, GC, PAH, soil, Fluorescence |
論文種類: | 學術論文 |
相關次數: | 點閱:290 下載:0 |
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摘要
快速有效、方便又省溶劑的加速溶液萃取法(accelerated solvent extraction, ASE),已經藉著氣相層析(GC)、高效率液相層析(HPLC)或是氣相層析質譜法(GC-MS)運用在分析有機樣品研究上,很多種揮發或不揮發的有機化合物像是殺蟲劑及多苯環芳香烴化合物(polycyclic aromatic hydrocarbons, PAHs)更容易用HPLC來分離,因此我們設計一套連線介面將ASE連線於HPLC,使得樣品前處理的方法能保有ASE的簡單方便等各項優點,並且同時保有HPLC對揮發及不揮發的樣品中待測物的解析度。
本實驗是將ASE連線HPLC,運用於分析土壤樣品中的PAHs,從結果中發現這個方法能夠維持著HPLC的高解析度以及ASE的優點,像是操作簡單、省溶劑及良好之萃取效果等,並且因為連線減少了人為因素所造成的誤差,增加實驗速率。另外也利用標準參考物質(QCS345)樣品的多次驗證,測出的結果皆在證書的範圍內,證明這個方法能簡單有效準確的檢測土壤中之PAHs含量。這個方法也實際運用在台灣各地土壤的分析工作上,結果顯示本方法對於真實樣品也是可行的。
Abstract
As a fast, convenient, and low solvent consuming extraction method, accelerated solvent extraction (ASE) technique has been studied for the analyses of organic compounds followed by gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS). However, many classes of widely-used organic compounds today are semi- or nonvolatiles, such as pesticides, and polycyclic aromatic hydrocarbons (PAH). They are easily separated by high performance liquid chromatography (HPLC). Thus, it would be advantageous to interface ASE with an HPLC system to provide easy sample preparation as well as possess high resolving power for semi- and non-volatiles simultaneously.
A method was developed to couple an accelerated solvent extraction system (ASE) with high performance liquid chromatography (HPLC) for the analysis of PAH in soil samples. The resolution of HPLC is well maintained while the advantages of ASE, fast extraction, less solvent consumption and ease of operation, are well expressed. The precision and accuracy of this method are verified by a series of analyses of reference material (QCS345sample from ERA). And the real sample collected at different sites in Taiwan. The data shows that it is feasible to analyze real samples using this method.
參考資料
1. NIOSH (National Institute for Occupational Safety and Health), Method 5506, 1985.
2. D. A. Brikholz, R. T. Coutts and S. E. Hrudey, "Determination of Polycyclic Aromatic Compounds in Fish Tissue", J. Chromatogr., 449, 251-260, 1988.
3. G. A. Eiceman,; A. C, Viau,; F. W. Karasek, Anal. Chem. 52, 1492-1496, 1980
4. C. Golden; E. Sanwichi, Anal. Lett. A11, 1051-1062, 1978.
5. G. Chatol, M. Casteynaro, J. L. Roche,; R. Fantanges, Anal. Chim. Acta 53, 259-265, 1971.
6. R. W. Wright, C. W. Wright, R. W. Gale and R. D. Smith, "Analytical Supercritical Fluid Extraction of Adsorbent Materials ", Anal. Chem., 59, 38-44, 1987.
7. T. Paschke, S. B. Hawthorne and D. J. Miller, " Supercritical Fluid Extraction of Nitrated Polycyclic Aromatic Hydrocarbons from Diesel Exhaust Particulate Matter ", J. Chromatogr., 609, 333-340, 1992.
8. M. D. Burford, S. B. Hawthorne and D. J. Miller, "Extraction Rate of Spiked versus Native PAHs from Heterogeneous Environmental Samples Using Supercritical Fluid Extraction and Sonication in Methylene Chloride", Anal. Chem., 65, 1497-4505, 1993.
9. T. S. Oostdyk; R. L. Grob; J. L. Snyder; M. E. McNally, Anal. Chem. 65, 596-600, 1993
10. S. B. Hawthorne, Anal. Chem., 62, 633A-642A, 1990
11. T. L. Chester; J. D. Pinkston; D. Raynie, Anal. Chem. 66, 106R-130R, 1994
12. L. A. Vlorica, R. Young, "Microwave-Assisted Extraction of Organic Compounds from Standard Reference Soils and Sediments", Anal. Chem., 66, 1097-1106, 1994.
13. A. Abu-Sumra; J. S. Morris,; S. R. Koirtyohann, Anal. Chem., 47, 1475-1477, 1975.
14. R. A. Nadkarni, Anal. Chem., 56, 2233-2237, 1984
15. H. M. Kingston,; L. B. Jassie, Anal. Chem., 58, 2534-2541, 1986.
16. K. Ganzler, A. Salgo, K. Vallko, J. Chromatogr., 371, 299-306, 1986
17. B. E. Richer, J. L. Ezzell, K. A. Roberts and D. W. Later, Am. Lab., 27, 24-28, 1995
18. Test Method for Evaluating Solid Waste, Method 3545, EPA SW-846, 3rd ed., Update Ⅲ US GPO, Washington, DC. , July, 1995
19.吳家誠,李迪雯, 科儀新知 19卷2期 143-148 ,民國86年.
20. 陳倩雯,吳家誠, Chemistry (The Chinese Chem. Soc. Taipei) 56(4), 295-302, 1998 (附件二)
21. 王光遠,〝 土壤學〞,1970。
22. 李俊福 ,〝土壤中的有機毒性物質〞,科學月刊,第26 卷,第三 期, 1995。
23. J. F. Barbara and N. P. James, Atmospheric Chemistry: Fundamentals and Experimental Techniques, New York; Wiley, 1986.
24. K. W. Sigvardon and J. W. Birks, "Peroxyoxate Chemiluminescence Detection of Polycyclic Aromatic Hydrocarbons in Liquid Chromatography ", Anal. Chem., 55, 432-435, 1983.
25. A. Bjorseth and T. Ramdal, "Handbook of Polycyclic Aromatic Hydrocarbons", Vol. 1, Mercel Dekker, Inc., New York and Basel, 1983.
26. D. L. Karlesky, M. E. Rollie and I. M. Warner, "Sample Clean up Procedure for Polynuclear Aromatic Compounds in Complex Matrices”, Anal. Chem., 1187-1192, 1986.
27. 江長陵,多環芳香族烴在大氣中固氣相分布模式之研究,國立台灣大學環境工程學研究所碩士論文,李慧梅博士指導,1991。
28. M. Blumer, W. W. Youngblood, "Polycyclic Aromatic Hydro-carbons in Soil and Recent Sediments ", Science, 188, 53~55, 1975.
29. C. A. Menzie, B. B. Potocki, J. Santodonato, "Exposure to Carcinogenic PAHs in the Environment", Environ. Sci. Technol., 26(7), 1278-1284, 1992.
30. E. Benfenati et al.,” PCDD, PCDF, PCB, PAH, Cadmium and Lead in Roadside soil Relationship Between Road Distance and Concentration”, Chemise., 24(8), 1077~ 1083, 1992.
31. J. Josephson, "Polynuclear Aromatic Hydrocarbons", Environ. Sci. Technol., 18, 93A-95A, 1984.
32. J. Tuominen, S. Salomaa, H. Pyysalo, E. Skytta, Tikanen and T. Nurmela, "Polynuclear Aromatic Compounds and Genotoxicity in Particulate and Vapor Phase of Ambient Air:Effect of Traffic, Season, and Meteorological Conditions", Environ. Sci. Technol., 22, 1228-1234, 1988.
33. J. Edward Calabrese, “Multiple Chemical Interactions” 325-339, 1991.
34. R. M. Niesink; J. de Vries; M. A. Hollinger, “Toxicology Principle and Applications” 403-405, 1996.
35. A. Wallace Hayes, “Principle and Methods of Toxicology second Edition” 751-752, 1989.
36. Louis J. Casarett. pH.; John doull, MD., Ph.D. “Toxicology the Basic Science of Poisons, 336-339, 1975
37. Mary O. Amdur, Ph.D.; John Doull, Ph.D., MD.; Curtis D.Klaassen, Ph.D. “Casarett and doull’s Toxicology The Basic Science of Poisons Fourth edition” 172-175, 1991.
38. D. A. Birkholz, R. T. Coutts, S. E. Hrudey, ”Determination of Polycyclic Aromatic Compounds in Fish Tissue”, J. Chromatography, 449, 251-260, 1988.
39. S. B. Hawthorne and D. J. Miller, “directly Coupled Supercritical Fluid Extraction-Gas Chromatographic Analysis of Polycyclic Aromatic Hydrocarbons and Polychlorinated Biphyls from Environmental Solid”, J. Chromatography, 403, 63-76, 1987.
40. R. W. Wright, C. W. Wright, R. W. Gale and RD Smith, “Analytical Supercritical Fluid extraction of Adsorbent Materials”, Anal. Chem., 59,38-44, 1987.
41. J. Dachs, J. M. Bayona, C. Raoux, J. Albaiges, “Spatical, Vertical Distribution and Budget of Polycyclic Aromatic Hydrocarbons in Western Mediterranean Seawater” Environ. Sci. Technol., 31, 682-688, 1997
42. S. A. Kanga, J. S. Bonner, c. A. Page, M. A. Mills, and R. L. Auterieth, “Solubility of Naphthalene from Crude Oil Using Biosurfactants” Environ. Sci. Technol, 31, 556-561, 1997
43. W. E. May and S. A. Wise, “Liquid Chromatographic Determination of Polycyclic Aromatic Hydrocarbons in Air Particulate Extraction”, Anal. Chem. 56, 225-232, 1984.
44. M. Radke, H. Willsch, D. H.Wette, “Class Separation of Aromatic Compounds in Rock Extracts and Fossil Fuels by Liquid Chromatography” Anal. Chem. 56,2538-2546, 1984.
45. J. P. Durand, N. Petroff, “Determination of Benzo(a)Pyrene and other Polyaromatic Hydrocarbons in Petroleum oil by direct Liquid Chromatography” Journal of Chromatography, 190, 85-95, 1980
46. D. W. Grant, R. B. Meiris “Application of Thin –Layer And High-Performance Liquid Chromatography to The Separation of Polycyclic Aromatic Hydrocarbons in Bituminous Materials” Journal of Chromatography, 142, 339-351, 1977.
47. 陳揖遜,以超臨界流體萃取/同位素稀釋質譜進行土壤中的多苯環芳香烴化合物分析,國立臺灣師範大學化學研究所碩士論文,吳家誠教授指導,1996。
48. M. Ellen and P. Mcnally, "Advance in Environmental SFE", Anal. Chem., 67, 1995.
49. A. L. Blilie, T. Greibrokk, "Modifier Effect on Retention and Peak Shape in Supercritical Fluid Chromatography", Anal. Chem., 57, 2239-2242, 1985.
50. R. H. Perry, D. W. Green, J. O. Maloney, “Perry’s Chemical Engineer’s Handbook”, 6thed, Chapter 3, 1984
51. B. E. Richer,; B. A. Jones,; J. L. Ezzell, and N. L. Poter, Anal. Chem., 68, 1033, 1996
52. K. S. Pitzer, L. Brewer, Thermodynamics, 2 ed.; McGraw-Hill: New York, Chapter 18, 1961
53. T. Sekine and Y. Hassegawa, Solvent Extraction Chemistry, Marcel Dekker: New York, 1997.
54. G. C. Pimentel, A.L. McClellan, The Hydrogen Bond ; Freeman: San Francisco, 1960.
55. 李惠美,加速溶劑萃取技術配合同位素稀釋氣相層析質譜法進行土壤中三十五種多苯環芳香烴化合物之分析方法研究,國立台灣師範大學化學研究所碩士論文,吳家誠教授指導, 1997
56. 李迪雯,加速溶劑萃取技術配合同位素稀釋氣相層析質譜法進行大氣塵粒中三十五種多苯環芳香烴化合物之分析方法研究,國立台灣師範大學化學研究所碩士論文, 吳家誠教授指導, 1997
57. 許裕昌, 加速溶劑萃取技術配合同位素稀釋氣相層析質譜法分析土壤及底泥中十二種鄰苯二甲酸酯之方法研究,國立台灣師範大學化學研究所碩士論文,吳家誠教授指導, 1997
58. X. Lou,;H-G. Janssen, and C. A. Cramers, Anal. Chem., 69, 1598-1603, 1997
59. N. Saim, ; J. R. Dean,;Md. P. Abdullaah, and Zakaria, Anal. Chem., 70, 420-424, 1998
60. O. P. Heemken,; N. Theobald, and B. W. Wenclawiak, Anal. Chem., 69, 2171-2180, 1997
61. J. R. Dean, Analytical Communications, 33, 191-192, 1996
62. D. V. Kenny,;S. V. Olesik, J. Chromatagr. Science, 36, 66-72, 1998
63. D. V. Kenny, S. V. Olesik, J. Chromatogr. Science, 36, 59-65, 1998
64. H. Obana,;K. Kikuchi,;M. Okihashi,;S. Hori, Analyst, 123, 711-714, 1998
65. M. Okihashi,;H. Obana,;S. Hori, Analyst, 122, 217-220. 1997
66. E. Conte,; R. Milani,; G. Morali and F. Abballe J. Chromatogr. A, 765, 121-125, 1997
67. P. Popp,;P. Keil,;M. Moder,;A. paschke and U. Thuss, J. Chromatogr. A, 74, 203-211, 1997
68. B. E. Richer,;J. L. Ezzell,;D. E. Knowles, and F. Hoefler, Chemosphere, 34, 975-987, 1997
69. Klaus Schafer, analytical Chimica Acta, 358, 69-77, 1998
70. B. Erland,;J. Mattias,;M. Lennart,;K. Lar, ;S. J. T., E. Jonaas,;T. Arne, J. Liq. Chromatogr. Relat. Technol., 21(4), 535-549, 1998
71. Chen Chien wen (陳倩雯) ; Yun Yuan Wang (王韻媛) ; Gaston J. C. Wu (吳家誠), Journal of Chinese Chemical Society, 46, 245-251, 1999. (附件三)
72. A. Kreisselmeier,; H. W. Durbeck , J. Chromatogr. A, 765, 121-125, 1997.
73.吳家誠 空氣中揮發性有機化合物檢測方法─以高分子吸附劑採樣之GC/MS法驗証研究,環保署研究報告,EPA─86─E3S3─09─03, 1997
74. 張明吉,大氣粒狀污染物中多苯環芳香烴之分析方法研究,國立台灣師範大學化學研究所碩士論文,吳家誠教授 指導,1994。
75. 高彩萍,以超臨界流體萃取法(SFE)/索氏萃取法及高效率液相層析法-紫外光-螢光偵測器測定大氣塵粒中多環芳香烴,國立台灣師範大學化學研究所碩士論文,吳家誠教授 指導,1996。