地质样品正构烷烃组分分离纯化的部分问题探究
Exploration of Some Problems in the Separation and Purification of n-alkanes in Geological Samples
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摘要: 用实验室自配的标准正构烷烃样品分别经硅胶或氧化铝柱层析后发现,等量溶剂洗脱的情况下硅胶对长链正构烷烃无吸附而氧化铝具有一定吸附性。进一步通过用植物样品测试4种层析柱填充方法,发现不论是只用氧化铝填充还是上部硅胶下部氧化铝和上部氧化铝下部硅胶,都会对长链正构烷烃产生一定的吸附,且这种吸附效果随着碳链的增长而增强。在实验条件下,当碳链加长到C36时,用硅胶加氧化铝填充层析柱的吸附量已达到20%左右,而只用氧化铝填充层析柱的吸附量则高达50%。故建议对研究高碳数正构烷烃的地质样品组分提取时用单一的硅胶柱层析方法。同时,实验显示对于一些杂质多的正构烷烃样品经过尿素络合后比络合前"干净"得多。18个黄土-古土壤和植物样品平均回收率为50%左右,经过尿素络合后的样品正构烷烃各组分相对含量基本不会发生改变,也不会产生明显的同位素分馏效应。因此在进行非正构组分干扰较大的正构烷烃各组分相对含量或同位素分析时,可以选择尿素络合的方法来将其纯化。Abstract: Adsorption characteristics of silica gel and alumina for n-alkanes were tested by column chromatography under equivalent solvent elution. The results showed that alumina could adsorb long chain n-alkanes in certain extent, while silica gel exhibited the opposite characteristic. The further experiments using plant samples and chromatographic columns filled with different materials were carried out. The experiment results indicated whether the columns filled with alumina and silica gel or with alumina alone, it exhibited adsorption characteristics for long chain n-alkanes and the adsorption effect became explicit with increasing of length of carbon chain. Under the proposed experiment condition, when the chain length reached C36, adsorbed amounts by the columns filled with silica gel-alumina and with alumina alone reached up to 20% and 50%, respectively. Therefore, silica gel chromatographic column could be the better choice when long chain n-alkanes in geological samples were analyzed. Moreover, the experiment results also indicated that urea was an effective purification agent in pretreatment of some very "dirty" samples. The average recovery for n-alkanes in 18 loess, paleosoil and plant samples was about 50% and relative abundance for each component of n-alkanes in samples kept unchanged and without distinct isotopic fractionation after sample purification with urea. Therefore, urea could be used in purification of complex geological samples to avoid the serious interference from non-n-alkanes species in determination of relative abundance and isotope composition of n-alkanes.
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Keywords:
- n-alkanes /
- geological /
- sample /
- column /
- chromatography
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