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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
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  • 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.

    目錄 中文摘要 英文摘要 目錄 表目錄 圖目錄 第一章緒論 前言 1-1一般交通事故案件常見跡證 1-2車漆內常見之成分及用途 1-3現行各國交通事故案件責任之認定 1-3-1用路權之有無 1-3-2刑事偵查方向 1-3-3科學鑑定 1-4車漆成分鑑定 1-4-1實體顯微鏡檢視 1-4-2顯微分光光譜法 1-4-3紅外線光譜分析法 1-4-4拉曼光譜分析法 1-4-5掃瞄式電子顯微鏡/X射線能譜分析法 1-4-6熱裂解氣相層析質譜分析法 1-4-7資料庫建比對法 1-4-8顯微溶解試驗法 1-4-9綜合分析方法 1-5熱裂解器介紹 第二章實驗儀器設備 2-1車漆樣品取樣工具 2-2取樣作法 2-3實驗分析儀器 2-4其他設備 2-5藥品、試劑、氣體、容器 2-6其他 第三章實驗內容 3-1熱效應質譜儀分析車漆樣品條件建立 3-2質譜調機狀態及操作參數 3-3熱效應質譜分析法圖譜型態之分類 3-4熱重分析儀之應用並與熱效應質譜分析法結合分析真實樣品 3-5聚苯乙烯之熱解性質、溶劑的選擇及標準溶液的製備 3-6熱裂解氣相層析質譜儀分析聚苯乙烯條件之建立 3-7可能產生苯乙烯裂解產物的高分子討論 3-8聚苯乙烯標準溶劑之單體檢量線的建立 3-9檢量線確認及標準添加分析 3-10熱裂解氣相層析質譜儀分析真實樣品 3-11熱裂解氣相層析質譜儀分析能力試驗樣品及實際案 例樣品 3-12訊號變動之原因及影響定量的因素 3-13以熱解方式分析其他常見樹脂成分之可行性 3-14 二種定量方法優、缺點之比較 第四章結果與討論 4-1熱效應質譜分析法分析車漆樣品條件建立 4-2熱重分析儀之應用 4-3真實案件分析比對結果 4-4熱裂解氣相層譜分析法針對車漆中特定成分之定量 4-5車漆內其他成分定量之可行性評估 4-6熱重分析儀及熱裂解氣相質譜分析法定量結果之比較 4-7本法運用於實務上之結合 第五章結論 第六章參考文獻 附件一 附件二 附件三 附件四 2003 US ASCLD/LAB Collaborative Testing Services~ Forensic Testing Program Testing No.03-546:Paint Analysis

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