NATURE AND FATE OF NATURAL RESINS IN THE GEOSPHERE .1. EVALUATION OF PYROLYSIS-GAS CHROMATOGRAPHY MASS-SPECTROMETRY FOR THE ANALYSIS OF NATURAL RESINS AND RESINITES
NATURE AND FATE OF NATURAL RESINS IN THE GEOSPHERE .1. EVALUATION OF PYROLYSIS-GAS CHROMATOGRAPHY MASS-SPECTROMETRY FOR THE ANALYSIS OF NATURAL RESINS AND RESINITES
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DOI：
10.1021/ac00024a019
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发表时间：
1991-12-15
影响因子：
7.4
通讯作者：
WINANS, RE
中科院分区：
文献类型：
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作者：
ANDERSON, KB;WINANS, RE
应用热解-气相色谱/质谱（Py-GC/MS）分析天然树脂和树脂的基础上的二萜羧酸进行了研究，以确定这种技术用于分析这些材料的有用性。 已经发现，使用同时热解甲基化（SPM）的Py-GC/MS分析提供了这些材料的组成的准确指示，除了关于具有另外的羟基和/或羰基官能团的化合物。 树脂酸甲酯（RAMES）是有效地生产原位共热解与四甲基氢氧化铵。 热解不会导致本研究中表征的RAMES发生显著的热降解或异构化。 然而，观察到RAME醇的一些脱水，并且含羟基和羰基的RAME都与甲基化试剂发生不期望的副反应，这导致形成含氮产物。 在本研究所采用的条件下，低至中等等级树脂质岩的最佳热解温度为480 ℃。 没有原位甲基化的Py-GC/MS分析发现，提供的结构和组成分析的数据一般不太充分。
The application of pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) to the analysis of natural resins and resinites based on diterpenoid carboxylic acids has been investigated, in order to determine the usefulness of this technique for the analysis of these materials. It has been found that Py-GC/MS analyses using simultaneous pyrolytic methylation (SPM) provide an accurate indication of the composition of these materials, except with respect to compounds with an additional hydroxy and/or carbonyl functionality. Resin acid methyl esters (RAMES) are efficiently produced in situ by copyrolysis with tetramethylammonium hydroxide. Pyrolysis did not result in significant thermal degradation or isomerization of the RAMES characterized in this study. Some dehydration of RAME alcohols is observed however, and both hydroxy- and carbonyl-containing RAMES undergo undesirable side reactions with the methylating reagent, which results in the formation of nitrogen-containing products. The optimum pyrolysis temperature for low- to moderate-rank resinites using the conditions employed in this study was found to be 480-degrees-C. Py-GC/MS analyses without in situ methylation were found to provide generally less adequate data for structural and compositional analyses.