Abstract Two catalytic fast pyrolysis (CFP) oils (bottom/heavy fraction) were analyzed in various solvents that are used in common analytical methods (nuclear magnetic resonance – NMR, gas chromatography – GC, gel permeation chromatography – GPC, thermogravimetric analysis – TGA) for oil characterization and speciation. A more accurate analysis of the CFP oils can be obtained by identification and exploitation of solvent miscibility characteristics. Acetone and tetrahydrofuran can be used to completely solubilize CFP oils for analysis by GC and tetrahydrofuran can be used for traditional organic GPC analysis of the oils. DMSO-d6 can be used to solubilize CFP oils for analysis by 13C NMR. The fractionation of oils into solvents that did not completely solubilize the whole oils showed that miscibility can be related to the oil properties. This allows for solvent selection based on physico-chemical properties of the oils. However, based on semi-quantitative comparisons of the GC chromatograms, the organic solvent fractionation schemes did not speciate the oils based on specific analyte type. On the other hand, chlorinated solvents did fractionate the oils based on analyte size to a certain degree. Unfortunately, like raw pyrolysis oil, the matrix of the CFP oils is complicated and is not amenable to simple liquid–liquid extraction (LLE) or solvent fractionation to separate the oils based on the chemical and/or physical properties of individual components. For reliable analyses, for each analytical method used, it is critical that the bio-oil sample is both completely soluble and also not likely to react with the chosen solvent. The adoption of the standardized solvent selection protocols presented here will allow for greater reproducibility of analysis across different users and facilities.

中文翻译：

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催化快速热解油的表征：溶剂选择对分析方法开发的重要性

摘要 在常用分析方法（核磁共振 – NMR、气相色谱 – GC、凝胶渗透色谱 – GPC、热重分析 – TGA）中使用的各种溶剂中分析了两种催化快速热解 (CFP) 油（底部/重馏分）用于石油表征和物种形成。通过识别和开发溶剂混溶特性，可以获得对 CFP 油的更准确分析。丙酮和四氢呋喃可用于完全溶解 CFP 油以进行 GC 分析，四氢呋喃可用于油的传统有机 GPC 分析。DMSO-d6 可用于溶解 CFP 油以通过 13C NMR 进行分析。将油分馏成不能完全溶解整个油的溶剂表明混溶性可能与油的性质有关。这允许根据油的物理化学性质选择溶剂。然而，基于 GC 色谱图的半定量比较，有机溶剂分馏方案并未根据特定分析物类型指定油类。另一方面，氯化溶剂确实在一定程度上根据分析物大小对油进行了分馏。不幸的是，与未加工的热解油一样，CFP 油的基质很复杂，不能通过简单的液液萃取 (LLE) 或溶剂分馏来根据各个组分的化学和/或物理特性来分离油。对于可靠的分析，对于所使用的每种分析方法，生物油样品必须完全可溶且不可能与所选溶剂发生反应，这一点至关重要。