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Chromatographic separations enabling the structural characterisation of heavy petroleum residues

机译：色谱分离可实现重油残渣的结构表征

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Two petroleum residues from European crudes have been fractionated using solvent (heptane) separation and column chromatography. The residues and the separated fractions have been characterised by size exclusion chromatography (SEC) and by UV-fluorescence spectroscopy (UV-F). Matrix assisted laser desorption/ionisation-mass spectrometry of the whole residues and the heptane insoluble fractions indicated that the bulk of the residues covered the mass range m/z 300―2000, while the heptane insolubles (1―2% of the whole) contained material in the mass range from about m/z 300 to 10 000. The upper mass ranges indicated by SEC using polystyrene standards were higher; the earliest eluting material from both distillation residues eluted at times corresponding to polystyrene standards of MMs above 1.85 million u. Possible reasons for the different observations are given. Data from UV-F suggests that the heptane solubility separation method was the most successful for the separation of the largest molecular mass and also probably the most polar materials in these residues. However, all three fractionation methods produced similar trends, showing greater polarity of the fractions to correlate with increasing molecular mass. The shift of maximum intensity of fluorescence towards longer wavelengths (in UV-fluorescence) with increasing molecular size, as indicated by SEC, strongly suggests that the fluorescing molecules are large rather than aggregates of small molecules. Differences in comparison with American petroleum residues can be observed.
机译：使用溶剂（庚烷）分离和柱色谱法分离了欧洲原油中的两种石油残留物。残留物和分离出的馏分已通过尺寸排阻色谱法（SEC）和紫外荧光光谱法（UV-F）进行了表征。整个残渣和庚烷不溶级分的基质辅助激光解吸/电离质谱分析表明，大部分残渣的质量范围为m / z 300-2000，而庚烷不溶物（占总量的1-2％）材料的质量范围在m / z 300到10000之间。SEC使用聚苯乙烯标准物表示的质量上限较高；从两种蒸馏残留物中最早洗脱的物质，其洗脱时间对应于大于185万微米的MM的聚苯乙烯标准。给出了不同观察结果的可能原因。 UV-F的数据表明，庚烷溶解度分离方法最成功地分离了这些残基中的最大分子量，也可能是极性最大的物质。但是，所有三种分馏方法均产生相似的趋势，显示出馏分的极性更大，与分子量增加相关。如SEC所示，随着分子大小的增加，最大荧光强度向更长波长（在UV荧光中）的转移强烈表明，发荧光的分子是大分子，而不是小分子的聚集体。可以观察到与美国石油残留物相比的差异。

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