研究生: |
楊勝雄 YANG.SHENG-HSIUNG |
---|---|
論文名稱: |
運用熱裂解氣相層析質譜分析法對於車漆成分定量之研究 The Application of Pyrolysis-Gas Chromatography/Mass Spectrometry for the Quantification of Vehicle Paint Components |
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 |
論文出版年: | 2005 |
畢業學年度: | 93 |
語文別: | 中文 |
中文關鍵詞: | 熱裂解氣相層析質譜儀 |
論文種類: | 學術論文 |
相關次數: | 點閱:927 下載:0 |
分享至: |
查詢本校圖書館目錄 查詢臺灣博碩士論文知識加值系統 勘誤回報 |
複雜的車漆樣品雖可藉由傅立葉轉換紅外線光譜儀(FTIR)、熱裂解氣相層析質譜儀(Pyrolysis-GC/MS)等方式加以定性,而定量的目標似乎遙不可及,最主要的原因在於變數多不易掌握,尤其是固體且經聚合後的高分子樣品,基質複雜性高,增加了困難度。本研究嘗試針對樣品量的多寡設計出二種不同的定量方式;當樣品量多時以熱重分析法(Thermogravimetry,TG)結合熱效應質譜分析法(Evolved Gas Analysis-Mass Spectrometry,EGA-MS),得到不同受熱區間分佈圖的型態和各區間所佔重量百分比。當樣品量少時,則針對車漆內最常見的成分-聚苯乙烯加以定量,除了解聚苯乙烯在熱作用下的性質外,並考慮基質所帶來定量上的影響;最後再以上述方法分析能力測試樣品(Proficiency analytical test,PAT sample)以及實際樣品,並配合國內現行車禍肇事案件鑑定流程,評估在實務上的應用性。
本研究係針對現今車禍肇事案刑事鑑定,有突破之作法,在有限的證物下除可提供一般車漆成分比對外,更可以將分析資料數據化,而對於肇事逃逸案中肇事者責任之釐清與認定應有更進一步之助益。
Qualitative analysis of complicated paint samples from traffic accident case could be usually dealt with by Fourier Transform Infrared Spectroscopy(FTIR)or Pyrolysis-Gas Chromatography/Mass Spectrometry(Pyrolysis-GC/MS), however quantification of them were still difficult owing to many factors to be controlled , especially for solid and cured polymer. The study tried to design two quantification methods based on the amount of sample and operational pattern of instrument t. When the amount is adequate enough , we can get spectral patterns and relative mass ratio by thermogravimetry(TG)and evolved gas analysis(EGA)with temperature-program pyrolysis coupled with MS via a deactivated capillary metal tube. Polystyrene(PS)is the most commonly used component in paint recipes quantitated by Pyrolysis-GC/MS when the amount is limited . Not only the characteristics of PS during the continuous heating process are examined , but also discuss the matrix effects on quantification are discussed . We than access the applications on actual cases by joining round robin test and analyzing actual samples before fitting the method to civil operation-procedure finally.
This study offers quantification technique by comparing data obtained from standard paints with those from the tiny paint chips on the limited sample for the actual forensic identification of traffic accident cases. With the developed method we can solve more suspected hit-and-run cases with good reliability.
1.Thomas P.Wampler,Gregory A.Bishea,William J.Simonsick,
,The effects of structure on the thermal degradation of polyester resins,J.Anal.Apply.Pyrolysis, Volume 40-41(1997)79-89
2.T. J. Allen,The examination of thin sections of coloured paints by light microscopy ,Forensic Science International , Volume 57, Issue 1 , November 1992, 5-16
3.Beryl Beattie , R. J. Dudley and K. W. Smalldon,The use of morin staining for the microscopic characterisation of multilayered white paint flakes, Forensic Science International , Volume 13 , 1979, 41-49
4.D. K. Laing , R. J. Dudley and M. D. J. Isaacs,Colorimetric measurements on small paint fragments using microspectrophotometry, Forensic Science International, Volume 16, Issue 2 , September-October 1980, 159-171
5.Nowicki J, Patten R,Examination of U.S. Automotive Paints: I. Make and Model Determination of Hit-Vehicles by REflectance Microspectrophotometry , J. Forensic Science ,Volume 31, Issue 2 ,April 1986
ISSN: 0022-1198
6.D. K. Laing , R. J. Dudley , Janet M. Home and M. D. J. Isaacs, The discrimination of small fragments of household gloss paint by microspectrophotometry Forensic Science International, Volume 20, Issue 2 , September-October 1982, 191-200
7.D. R. Cousins , C. R. Platoni and L. W. Russell ,The use of microspectrophotometry for the identification of pigments in small paint samples ,Forensic Science International, Volume 24, Issue 3 , 1984, 183-196
8.N. A. Fuller, Analysis of thin-layer chromatograms of paint pigments and dyes by direct microspectrophotometry,Forensic Science International ,Volume 27, Issue 3 , March 1985, 189-204
9.Patrick Buzzini , Genevive Massonnet, Stphane Birrer, Nicole M. Egli, Williams Mazzella and Annarita Fortini, Survey of crowbar and household paints in burglary cases—population studies, transfer and interpretation ,Forensic Science International Article in Press , Available online 26 November 2004.
10.Ryland S, Bishea G, Brun-Conti L, Eyring M, Flanagan B, Jergovich T, MacDougall D, Suzuki E,Discrimination of 1990s original automotive paint systems: a collaborative study of black nonmetallic base coat/clear coat finishes using infrared spectroscopy, J. Forensic Science, Volume 46, Issue 1 (January 2001) ISSN: 0022-1198
11.Suzuki EM, Marshall WP,Infrared spectra of U.S. automobile original topcoats (1974–1989): IV. Identification of some organic pigments used in red and brown nonmetallic and metallic monocoats quinacridones, J. Forensic Science ,Volume 43, Issue 3 (May 1998) ISSN: 0022-1198
12.Suzuki EM,Infrared Spectra of U.S. Automobile Original Topcoats (1974–1989): II. Identification of Some Topcoat Inorganic Pigments Using an Extended Range (4000~220 cm-1) Fourier Transform Spectrometer, J. Forensic Science, Volume 41, Issue 3 (May 1996) ISSN: 0022-1198
13.Suzuki EM,Infrared Spectra of U.S. Automobile Original Topcoats (1974–1989): I. Differentiation and Identification Based on Acrylonitrile and Ferrocyanide C≣N Stretching Absorptions, J. Forensic Science ,Volume 41, Issue 3 (May 1996) ISSN: 0022-1198
14.Suzuki EM ,Infrared spectra of U.S. automobile original topcoats (1974-1989): VI. Identification and analysis of yellow organic automotive paint pigments—isoindolinone yellow 3R, isoindoline yellow, anthrapyrimidine yellow, and miscellaneous yellows, J. Forensic Science , Volume 44, Issue 6 (November 1999) ISSN: 0022-1198
15.Suzuki EM, Marshall WP, Infrared spectra of U.S. automobile original topcoats (1974–1989): III. In situ identification of some organic pigments used in yellow, orange, red, and brown nonmetallic and brown metallic finishes—benzimidazolones, J. Forensic Science ,Volume 42, Issue 4 (July 1997) ISSN: 0022-1198
16.Suzuki EM ,Infrared spectra of U.S. automobile original topcoats (1974-1989): V. Identification of organic pigments used in red nonmetallic and brown nonmetallic and metallic monocoats--DPP red BO and Thioindigo Bordeaux. J. Forensic Science, Volume 44, Issue 2 (March 1999)ISSN: 0022-1198
17.Parybyk AE, Kobus HJ, The Characterization of Plastic Automobile Bumper Bars Using Fourier Transform Infrared Spectroscopy (FTIR), Pyrolysis Gas Chromatography (PGC), and Energy Dispersive X-Ray Microanalysis Combined with a Scanning Electron Microscope (SEM-EDX), Volume 35, Issue 2 (March 1990), ISSN: 0022-1198
18.Abraham F.Jalbout,Tao Jiang ,Liu Fengqi,C.Ding,Abdalla M.Darwish,Spectrochimica Acta Part A ,Volume 58(2002)525-536
19.Suzuki EM,Forensic Science Applications of Diffuse Reflectance Infrared Fourier Transform, Spectroscopy (DRIFTS): IV. Direct Analysis of Metallic Paints—Sampling Considerations , J. Forensic Science ,Volume 34, Issue 1 (January 1989) ISSN: 0022-1198
20.Suzuki EM, Brown JA, Forensic Science Applications of Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS): V. Direct Analysis of Metallic Paints—Screening of Panels, J. Forensic Science ,Volume 34, Issue 1 (January 1989) ISSN: 0022-1198
20.Guineau B,Microanalysis of Painted Manuscripts and of Colored Archeological Materials by Raman, J. Forensic Science, Volume 29, Issue 2 (April 1984) ISSN: 0022-1198
21.Suzuki EM, Carrabba M,In situ identification and analysis of automotive paint pigments using line segment excitation raman spectroscopy:1. Inorganic topcoat pigments, J. Forensic Science ,Volume 46, Issue 5 (September 2001,ISSN: 0022-1198
22.Kuptsov AH ,Applications of Fourier Transform Raman Spectroscopy in Forensic Science, J. Forensic Science ,Volume 39, Issue 2 (March 1994) ISSN: 0022-1198
23.Beam TL, Willis WV,Analysis Protocol for Discrimination of Automotive Paints by SEM-EDXA Using Beam Alignment by Current Centering, J. Forensic Science ,Volume 35, Issue 5 (September 1990) ISSN: 0022-1198
24.Zeichner A, Levin N, Landau E,A Study of Paint Coat Characteristics Produced by Spray Paints from Shaken and Nonshaken Spray Cans, J. Forensic Science, Volume 37, Issue 2 (March 1992) ISSN: 0022-1198
25.Blackledge RD, Pyrolysis Gas Chromatography of Automobile Rubber Bumper Guard Samples, Volume 26, Issue 3 (July 1981), ISSN: 0022-1198
26.McMinn DG, Carlson TL, Munson TO, Pyrolysis Capillary Gas Chromatography/Mass Spectrometry for Analysis of Automotive Paints, J. Forensic Science, Volume 30, Issue 4 (October 1985) ISSN: 0022-1198
27.Cardosi PJ,Pyrolysis-Gas Chromatographic Examination of Paints, J. Forensic Science ,Volume 27, Issue 3 (July 1982) ISSN: 0022-1198
28.Armitage S, Saywell S, Roux C, Lennard C, Greenwood P,The analysis of forensic samples using laser micro-pyrolisis gas chromatography mass Spectrometry, J. Forensic Science ,Volume 46, Issue 5 (September 2001) ISSN: 0022-1198
29.M. C. Taylor , D. R. Cousins , R. H. Holding , J. Locke and J. M. Wilkinson ,A data collection of vehicle topcoat colours. 3. Practical considerations for using a national database, Forensic Science International ,Volume 40, Issue 2 , February 1989, Pages 131-141
30.J. Locke , J. M. Wilkinson and T. J. Hanford,A data collection of vehicle topcoat colours. 2. The measurement of colour samples used in the vehicle refinishing industry,Forensic Science International Volume 37, Issue 3 , May 1988, Pages 177-187
31.J. Locke , D. R. Cousins , L. W. Russell , C. M. Jenkins and J. M. Wilkinson,A data collection of vehicle topcoat colours. 1. Instrumentation for colourmeasurements, Forensic Science International Volume 34, Issues 1-2 , May-June 1987, Pages 131-142
32.David R. Cousins , Rosemary H. Holding , John Locke and Jacqueline M. Wilkinson, A data collection of vehicle topcoat colours. 4. A trial to assess the effectiveness of colour identification, Forensic Science International Volume 43, Issue 2 , October-November 1989, Pages 183-197
33.McDermott SD, Willis SM,A survey of the evidential value of paint transfer evidence, J. Forensic Science, Volume 42, Issue 6 (November 1997) ISSN: 0022-1198
34.Audette RJ, Percy RFE,A Rapid, Systematic, and Comprehensive Classification System for the Identification and Comparison of Motor Vehicle Paint Samples. II: Paint Data Collected from Chrysler Manufactured Cars, J. Forensic Science, Volume 27, Issue 3 (July 1982) ISSN: 0022-1198
35.Ryland SG, Kopec RJ, Somerville PN,The Evidential Value of Automobile Paint. Part II: Frequency of Occurrence of Topcoat Colors, J. Forensic Science, Volume 26, Issue 1 (January 1981) ISSN: 0022-1198
36.McDermott SD, Willis SM, McCullough JP ,The evidential value of paint. Part II: a Bayesian approach, J. Forensic Science, Volume 44, Issue 2 (March 1999) ISSN: 0022-1198
37.Thornton JI, Kraus S, Lerner B, Kahane D,Solubility Characterization of Automotive Paints, J. Forensic Science ,Volume 28, Issue 4 (October 1983) ISSN: 0022-1198
38.Giang YS, Wang SM, Cho LL, Yang CK, Lu CC,Identification of tiny and thin smears of automotive paint following a traffic accident, J. Forensic Science, Volume 47, Issue 3 (May 2002) ISSN: 0022-1198
39.Dabdoub G, Severin P,The Identification of Domestic and Foreign Automobile Manufacturers Through Body Primer Characterization, J. Forensic Science, Volume 34, Issue 6 (November 1989) ISSN: 0022-1198
40.Jacqueline M. Wilkinson , John Locke and David K. Laing, The examination of paints as thin sections using visible microspectrophotometry and Fourier transform infrared microscopy , Forensic Science International, Volume 38, Issues 1-2, July-August 1988, Pages 43-52
41.J. W. Bates , T. Allinson and T. S. Bal,The examination of paints as thin sections using visible microspectrophotometry and Fourier transform infrared microscopy, Forensic Science International, Volume 38, Issues 1-2 , July-August 1988, Pages 43-52
42.Filip Govaert and Magali Bernard ,Discriminating red spray paints by optical microscopy, Fourier transform infrared spectroscopy and X-ray fluorescence, Forensic Science International, Volume 40, Issue 1 , 10 February 2004, Pages 61-70
43.P. Burke , C. J. Curry , L. M. Davies and D. R. Cousins ,A comparison of pyrolysis mass spectrometry, pyrolysis gas chromatography and infra-red spectroscopy for the analysis of paint resins, Forensic Science International ,Volume 28, Issues 3-4 , August 1985, Pages 201-219
44.D.Thorburn Burns,K. P .Doolan, A comparison of pyrolysis-gas chromatography-mass spectrometry and Fourier transform infrared spectroscopy for the analysis of a series of modified alkyd paint resins ,Analytica Chimica Acta Volume 422(2000)217-230
45.Francesca Cappitelli,THM-GCMS and FTIR for the study of binding media in Yellow Islands by Jackson Pollock and
Break Point by Fiona Banner, J.Anal.Apply.Pyrolysis , Volume 71(2004)405-415
47.Yoshihiro Sugimura , Shin Tsuge , Fundamental Splitting Conditions for Pyrogram Measurements with Glass Capillary Gas Chromatography ,Analytical Chemistry, Volume 50(1978)1968-1972
48.Shin Tsuge, Tsuglo Takeuchi , Vertical Furnace-Type Sampling Device for Pyrolysis Gas Chromatography ,Analytical Chemistry, Volume 49(1977)348-350
49.Masahiko Takino, Shigeki Daishima, Sadao Nakamura, Analysis of waterborne paints by gas chromatography–mass spectrometry with a temperature-programmable pyrolyzer,Journal of Chromatography A, Volume 912 (2001) 329–334
50.N.Dadvand,R.S.Lehrle,I.W.Parsons,M.Rollinson, Use of pyrolysis-GC-MS. to assess the thermal degradation behaviour of polymers containing chlorine I. The limits of detection and measurement of HCl, deduced from astudy of PVC pyrolysis ,Polymer Degradation and Stability, Volume 66(1999)247-255
51.N.Regniger,B.Mortaigne,Analysis by pyrolysis/gas chromatography/mass spectrometry of glass fibre/vinylester thermal degradation produces,Polymer Degradation and Stability , Volume 49(1995)419-428
52.K.G.H.Raemaekers, J.C.J.Bart,Applications of simultaneous thermogravimetry-mass spectrometry in polymer analysis,Thermochimica Acta, Volume 295(1997)1-58
53.Janina Zi ba and Andrzej Pomianowski, A statistical criterion for the value of evidence: Application to the evaluation of the results of paint spectral analysis,Forensic Science International, Volume 17, Issue 2 , March-April 1981, Pages 101-108
54.Voskertchian GP, Quantitative Analysis of Organic Pigments in Forensic Paint Examination, Volume 40, Issue 5 (September 1995)
55.Abraham F.Jalbout , Tao Jiang , Liu Fengqi , C.Ding , Abdalla M. Darwish,Quantitative analysis of (styrene/acrylonitrile/mtehylmethacrylate)copolymer systems by infrared resonance spectroscope, Spectrochimica Acta Part A, Volume 58(2002)525-536
56.M. Herrera a, G. Matuschek a, A. Kettrup a,b, Fast identification of polymer additives by pyrolysis-gas chromatography/mass spectrometry, J. Anal. Appl. Pyrolysis , Volume 70 (2003) 35-42
57.Frank Cheng-Yu Wang , M.L. Dettloff , M.J. Null , J.E. White ,Qualitative and quantitative analysis of a thermoset polymer, poly(benzoxazine), by pyrolysis–gas chromatography ,Journal of Chromatography A, Volume 886 (2000) 217–224
58.Shin Tsuge , H.Ohtani, Structure characterization of polymeric materials by Pyrolysis GC/MS,Polymer Degradation and Stability , Volume 58(1997)109-130
59.E. Jakab, Md.A. Uddin, T. Bhaskar, Y. Sakata, Thermal decomposition of flame-retarded highimpact polystyrene
,J. Anal. Appl. Pyrolysis, Volume 68-69 (2003) 83-99
60.Taiehi Nonobe,Hajime Ohtani,Takao Usami,Teruo Mori,Hiroko Fukumori,Yukio Hirata,Shin Tsuge,Characterization of stereoregular polystyrenes by pyrolysis-gas chromatography,J.Anal.Apply.Pyrolysis ,Volume 33(1995)121-138