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研究生: 黃戎巖
論文名稱: 以雷射剝蝕感應耦合電漿質譜分析術(LA-ICP-MS)分析土壤中之無機元素
指導教授: 王竹方
口試委員:
學位類別: 碩士
Master
系所名稱: 原子科學院 - 生醫工程與環境科學系
Department of Biomedical Engineering and Environmental Sciences
論文出版年: 2000
畢業學年度: 88
語文別: 中文
論文頁數: 89
中文關鍵詞: 雷射剝蝕感應耦合電漿質譜儀土壤
外文關鍵詞: LA-ICP-MS, Soil
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  • 目前傳統分析環境樣品的方法,多採用溼式消化的方式,將固體樣品轉化成水溶液,再以ICP-MS或ICP-AES等儀器定量分析其中的元素。但消化過程中不僅繁複費時且易造成漏失或污染。雷射剝蝕感應耦合電漿質譜儀( Laser Ablation Inductively Coupled Plasma Mass Spectrometry ; LA-ICP-MS)具有直接分析不須前處理,樣品量少,偵測極限低,線性範圍大及多元素同時分析等特性,因此可以作為環境樣品分析的最佳選擇。
    在進行LA-ICP-MS分析時,所遭遇的主要問題為標準樣品的製備,一般而言,環境樣品基質的成份相當複雜,因此很難找到與樣品基質完全相同的標準品。本研究嘗試分別以黏著劑混合標準土壤製備不同濃度的標準品,以及發展以標準溶液進樣同步校正固體樣品的定量方法來克服上述的問題。

    研究結果發現以配置之標準土壤樣品校正時,各元素撿量線線性關係不佳,但經由選擇適當的內標準元素修正後,大多數元素撿量線之線性關係可改善至0.95以上。此外以標準溶液與雷射剝蝕之氣體樣品同步進行ICP-MS偵測時,則已初步建立可以相對靈敏因子(Relatively Sensitive Factor)方式對未知樣品進行校正定量的技術。


    Traditional analytical methods for determining soil samples rely on decomposition procedure, typically through microwave or acid digestion and analysis of resulting solution by ICP-AES or ICP-MS. These analytical methods based on dissolving the sample are easily calibrated but suffer from the time and difficulty needed to bring the sample into dissolution as well as from dilution and contamination induced by the digestion procedure. Solid sample introduction into an ICP-MS by laser ablation (LA) is a very attractive alternative to the nebulization of aqueous sample solutions. In addition to the usual analytical advantages of ICP-MS, LA offers reduced sample preparation, rapid sample exchange and throughput, reduced spectral interferences and the possibility of situ spatially resolved analysis. There are also a number of concerns and problems that have prevented LA-ICP-MS from becoming a general technique for analysis of materials. Practical concerns include the difficulty of obtaining or making matrix-matched standards that contains all the elements of interest and the accuracy of the resulting calibration. We try to propose two mehtods of preparing standard for analysis of LA-ICP-MS and overcome the above problems. Standard soil samples are mixed with a polyethene-based binding agent and press into pellets for direct solid sampling by the laser. It is found that the correlation coefficient of the calibration curves based on 9 standards (10-90% of soil) in three different soil sample are better than 0.9 when appropriate elements are chosen as the internal standard. A simultaneous dried solution aerosol (supersonic nebulizer) and laser-induced aerosol introduction system is also used to investigate the calibration capabilities of dried solution for LA-ICP-MS. In most cases, the measure concentrations are within ±20% of the certified value if 208Pb as the internal standard. The lower results obtained for Sr and Ba may be partially due to matrix effects resulting from the high levels of efficiently ionized element (EIEs).

    目 錄 第一章 前言 ……………………………………………………….. 1 1.1 研究緣起 ……………………………………………………. 1 1.2 研究目的 ……………………………………………………. 2 第二章 文獻回顧 ………………………………………………….. 6 第三章 儀器原理 ………………………………………………….. 10 3.1 雷射剝蝕(Laser Ablation , LA)系統 ……………………… 12 3.2 感應耦合電漿離子源(ICP as ion source)…………………... 17 3.3 離子萃取(Ion extraction)…………………………………… 20 3.4 離子聚焦(Ion focusing)……………………………………... 20 3.5 四極柱質量分析器(Quadrupole mass analyzer)…………… 21 3.6 離子偵測(Ion detection)…………………………………….. 22 3.7 LA-ICP-MS的分析特性 …………………………………... 23 第四章 研究方法與設備 ………………………………………….. 25 4.1 實驗設備 ……………………………………………………. 25 4.2 試藥及器材 …………………………………………………. 26 4.3 容器清洗 ……………………………………………………. 26 4.4 土壤錠片樣品之製備………………………………………... 26 4.5 LA-ICP-MS分析 …………………………………………... 28 第五章 結果與討論 ……………………………………………….. 29 5.1 標準品均勻性之評估 ………………………………………. 29 5.2 LA-ICP-MS儀器最佳化條件之探討 ……………………... 31 5.3 樣品分析之探討 …………………………………………… . 35 第六章 結論 ……………………………………………………….. 45 第七章 參考文獻 ………………………………………………….. 46

    1. Houk, R.S.; Fassel,V.A.; Flesch,G.D.Anal.Chem.1980, 52 ,2283-2289.
    2. Jarvis,K.E ; Gray, A. L. ; Houk,R.S. Handbook of Inductively Coupled Plasma Mass Spectrometry, Scotland.
    3. Houk,R.S. Acc. Chem. Res. 1994, 27, 333-339
    4. Hieftje, G.M. ; Norman, L.A. Int. J. Mass Spectrom. Ion Process , 1992, 118/119,519-573
    5. Houk,R.S Anal.Chem.1986, 58 ,97A-105A
    6. Blain, L.;Salin, E.D.;Boomer, D.W., J. Anal. At. Spectrom., 1989, 4 ,271-276
    7. Hager, J.W. Anal.Chem.1989, 61 ,1243
    8.Thompson, M.; Chenery, S.; Brett. L. J. Anal. At. Spectrom., 1989, 4 ,11-15
    9.黃憲文,科儀新知,105,
    10. Park, C.J.; Hall, G.E.M. J. Anal. At. Spectrom., 1987, 17 ,34
    11.Jakubowski, D.; Feldmann, I. Spectrochim. Acta, Part B, 1995 , 110 ,551
    12. Gray , A. L. Analyst,1985, 110 , 551
    13.鄭素玲,清華大學原子科學所碩士論文,1996
    14.Gregoire, D. C.,Applied Spectroscopy,1987,41,897
    15. Durrant, S. F. Analyst,1992,117,1585
    16. Durrant, S. F.;Ward, N. I. Fresenius J. Anal. Chem.,345,512-517
    17. Denoyer, E. R. J. Anal. At. Spectrom., 1992, 7 ,1187-1193
    18. Hofffmann, E.; Ludke, C. Fresenius J. Anal. Chem.,355,900-903
    19. Cousin, H.; Magyar, B. Mikrochim. Acta ,113,313-323
    20. Perkins, T. W. J. Anal. At. Spectrom., 1991, 6 ,445-449
    21.Cromwell, E.F.;Arrowsmith, P Anal.Chem.1995, 67 ,131-138
    22. Jackson, S.E., Longerich, H.P., Dunning, G.R. and Fryer, B.J. Can. Mineral., 1992, 30, 1049.
    23.Imbert, J.L. and Telouk, P. Mikrochim. Acta, 1993, 110, 151.
    24. Perkins, W.T., Pearce N.J.G. and Jeffries, T.E. Geochim. Cosmochim. Acta, 1993, 57, 3479.
    25. Walder, A.J., Abell, I.D., Platzner, I. and Freedman, P.A. Spectrochim. Acta, 1993, 57, 475.
    26. Williams, J.G. and Jarvis, K.E. J. Anal. At. Spectrom., 1993, 8, 25.
    27.Jarvis, K.E. and Williams, J.G. Chem. Geol., 1993, 106, 251.
    28. Jenner, G.A., Foley, S.F., Jackson, S.E. and Longerich, H.P. Geochim. Cosmochim. Acta, 1994, 58, 5099.
    29. Imai, N. and Yamamoto, M. Mikrochem. J., 1994, 50, 281.
    30. Christensen, J.N., Halliday, A.N., Lee, D.C. and Hall, C.M. Earth Planet. Sci. Lett., 1995, 136, 79.
    31.Mochizuki, T., Sakashita, A., Iwata, H. and Blair, P. Anal. Sci., 1988,
    4, 403.
    32.Weijer, P. Van de, Baeten, W.L.M., Bekkers, M.H.J. and Vullings, P.J.M.G. J. Anal. At. Spectrom., 1992, 7, 599.
    33.Yasuhara, H., Okano, T. and Matsmura, Y. Analyst, 1992, 117, 395.
    34.Durrant, S.F. Braz. J. Vac. Appl., 1991, 10, 39.
    35.Raith, A., Hutton, R.C., Abell, I.D. and Crighton, J. J. Anal. At. Spectrom., 1995, 10, 591.
    36.Cromwell, E.F. and Arrowsmith P. Appl. Spectrosc., 1995, 49, 1652.
    37.Yuzefovsky, A.I. and Miser, D.E. Appl. Spectrosc., 1998, 52, 629.
    38.Jeffries, T.E., Perkins, W.T. and Pearce, N.J.G. Chem. Geol., 1995, 121, 131.
    39.Morrison, C.A., Lambert, D.D., Morrison, R.J.S. and Nicolls, I.A. Chem. Geol., 1995, 119, 13.
    40.Lichte, F.E. Anal. Chem., 1995, 67, 2479.
    41.Raith, A., Godfrey, J. and Hutton, R.C. Fresenius' J. Anal. Chem., 1996, 354, 163.
    42.Norman, M.D., Pearson, N.J., Sharma, A. and Griffin, W.L. Geostand. Newsl., 1996, 20, 247.
    43.Gunther, D., Frischknecht, R., Heinrich, C.A. and Kahlert, H.J. J. Anal. At. Spectrom., 1997, 12, 939.
    44.Shibuya, E.K., Sarkis, J.E.S., Enzweiler, J. and Figueiredo, A.M.G. J. Anal. At. Spectrom. 1998, 13, 941.
    45.Audetat, A., Gunther, D. and Heinrich, C.A. Science, 1998, 52, 629.
    46.Shuttleworth, S., Kremser, D.T. J. Anal. At. Spectrom., 1998, 13, 697.
    47. Olesik, J.W. Anal.Chem.1996, 61 ,496A

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