Abstract

The development of efficient methods for preconcentration and purification of petroleum metal porphyrins is the necessary condition for further progress of basic and especially applied research concerning the properties of these compounds and their role in oil genesis and maturation. This study deals with chromatographic preparation of high-purity vanadyl porphyrins using a sulfuric acid cation exchanger that can be readily prepared from silica gel and sulfuric acid and is simple in use. At the silica gel : sulfuric acid : water weight ratio of 60 : 15 : 25, the suggested sulfuric acid cation exchanger retains most efficiently nonporphyrin impurities of the asphaltene polar extract, whereas a significant fraction of vanadyl porphyrins (up to ~50%) passes through the chromatographic column virtually without retention with the stationary phase. In contrast to traditional adsorbents, the suggested sulfuric acid cation exchanger allows preparation of spectrally pure vanadyl porphyrins in one chromatographic purification step, thus ensuring the minimal consumption of the eluent and adsorbent. High purity of the vanadyl porphyrins obtained was confirmed by mass-spectrometric and spectroscopic methods of analysis.

中文翻译：

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硫酸阳离子交换剂的组成对石油氧钒卟啉色谱纯化效率的影响

摘要

石油金属卟啉的预浓缩和提纯的有效方法的发展，是进一步发展有关这些化合物的性质及其在油的生成和成熟中作用的基础研究，特别是应用研究的必要条件。这项研究涉及使用硫酸阳离子交换剂色谱制备高纯度钒基卟啉的方法，该阳离子交换剂可以容易地由硅胶和硫酸制备，并且使用简单。在硅胶：硫酸：水的重量比为60：15：25时，建议的硫酸阳离子交换剂可最有效地保留沥青质极性萃取物中的非卟啉杂质，而大部分的钒基卟啉（高达〜50％）通过通过色谱柱几乎没有保留在固定相中。与传统的吸附剂相比，建议的硫酸阳离子交换剂可在一个色谱纯化步骤中制备光谱纯的钒基卟啉，从而确保洗脱液和吸附剂的消耗最少。通过质谱和光谱分析法证实了所获得的钒基卟啉具有高纯度。