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Applications of pyrolysis gas chromatography/mass spectrometry for the analysis ofpolymeric samples.

机译:热解气相色谱/质谱在聚合物样品分析中的应用。

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摘要

This dissertation focuses on the applications of pyrolysis gas chromatography/mass spectrometry (py-GC/MS) for the analysis of polymer samples. Pyrolysis applies heat to reduce the polymer to smaller fragments more amenable to analysis by GC/MS. Analysis of these fragments is useful for characterization of polymer structure.; Breath analysis is a non-invasive method for the investigation of the volatile compounds present in human breath. We have developed a methodology using solid phase microextraction (SPME) and capillary gas chromatography for the analysis of various compounds in human breath. Results show that SPME-GC analysis of breath is a simple and accurate method.; Application of principal component analysis (PCA) and canonical variates analysis (CVA) to the chromatograms from the pyrolysis of poly(styrene:acrylate) based toners produced characteristic peaks relevant to differentiation. Our results demonstrate that py-GC/MS is a useful tool for characterization of copied or laser printed documents.; Pyrolysis gas chromatography (Py-GC) has been the standard method for the analysis of automotive paint samples for a number of decades. Pattern recognition techniques such as PCA and CVA were used to assess the statistical validity of differences observed between different samples. Results show that multivariate data analysis techniques can be used to effectively categorize various automotive paint samples.; A quantitative py-GC/MS method using principal component regression (PCR) was developed. Synthetic copolymers are often analyzed using only the ratios of monomer peaks. By using all of the information present in the chromatogram, a more accurate measurement of the composition of the synthetic copolymer can be performed.; Two different fast GC techniques were investigated for the purposes of obtaining faster run times: fast temperature programming and using small internal diameter (ID) columns. These fast GC techniques were applied for pyrolysis of polymeric samples. Both fast temperature programming and small ID columns proved useful for reducing run times while providing the same amount of information as the longer run times obtained using standard capillary columns.
机译:本文主要研究热解气相色谱/质谱(py-GC / MS)在聚合物样品分析中的应用。热解通过加热将聚合物还原为更适合于通过GC / MS分析的较小碎片。这些片段的分析对于表征聚合物结构是有用的。呼吸分析是一种非侵入性方法,用于研究人呼吸中存在的挥发性化合物。我们已经开发出一种使用固相微萃取(SPME)和毛细管气相色谱法分析人类呼吸中各种化合物的方法。结果表明,SPME-GC分析呼吸是一种简单而准确的方法。将主成分分析(PCA)和规范变量分析(CVA)应用于基于聚(苯乙烯:丙烯酸酯)的碳粉热解的色谱图,得出与鉴别有关的特征峰。我们的结果表明py-GC / MS是表征复印或激光打印文档的有用工具。数十年来,热解气相色谱法(Py-GC)一直是分析汽车涂料样品的标准方法。模式识别技术(例如PCA和CVA)用于评估不同样品之间观察到的差异的统计有效性。结果表明,多元数据分析技术可用于有效地对各种汽车油漆样品进行分类。建立了使用主成分回归(PCR)的定量py-GC / MS方法。通常仅使用单体峰的比率来分析合成共聚物。通过使用色谱图中存在的所有信息,可以对合成共聚物的组成进行更准确的测量。为了获得更快的运行时间,研究了两种不同的快速气相色谱技术:快速温度编程和使用小内径(ID)色谱柱。这些快速的气相色谱技术被用于聚合物样品的热解。事实证明,快速温度编程和小型ID色谱柱均有助于减少运行时间,同时提供与使用标准毛细管色谱柱获得的较长运行时间相同的信息量。

著录项

  • 作者

    Kochanowski, Brian Keith.;

  • 作者单位

    University of South Carolina.;

  • 授予单位 University of South Carolina.;
  • 学科 Chemistry Analytical.; Chemistry Polymer.
  • 学位 Ph.D.
  • 年度 1999
  • 页码 133 p.
  • 总页数 133
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类 化学;高分子化学(高聚物);
  • 关键词

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