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作 者:张昌鸣[1] 杨建丽[1] 薛永兵[1] 李允梅[1] 刘振宇[1]
机构地区:[1]中国科学院山西煤炭化学研究所煤转化国家重点实验室,山西太原030001
出 处:《分析测试技术与仪器》2006年第3期136-142,共7页Analysis and Testing Technology and Instruments
基 金:国家自然基金资助项目(No20076050;20076049)
摘 要:以柱液体色谱联合红外光谱(IR)、元素分析等手段,建立了一项测定渣油和沥青中烃族的族组成分析方法.通过色谱参数的评选和红外光谱的核实所建立的此方法具有溶剂和担体用量少、色谱分辨率高的特点,是一安全、经济、先进的族组成分析方法.所建方法中,选择的模型化合物为试剂纯碳24烷烃、二苯并[ah]蒽、乙酰苯胺.冲洗所获模型物制备段分,其红外光谱特征和元素分析结果和原试剂相一致,且具有好的回收率.所建方法对渣油和沥青实样的测定,不仅有很好的重复性,还具有很高的分离、分辩能力.IR和核磁共振氢谱(1H-NMR)的测定充分地证实了各制备段的不同特征.A modified method for group type analysis of asphalt was tested using column liquid chromatography and verified by infrared spectrum and NMR analysi. The method allows for the detection and quantitation of saturates, aromatics, resins and asphaltine. The technique is rapid and requires minimal quantities of sample and solvent. For about 0. 1 g sample, the solvent sequence is 20 mL nheptane for saturates, 35 mL n-heptane/dichloromethane (1/2.5, V/V) for aromatics and 30 mL dichloromethane/tetrahydrofuran (1/3, V/V) for resin. The model compounds are tetracosan for saturates, dibenz[ah] anthracen for aromatics and acetanilide for resin. The infrared spectrum and NMR analysis of the prepared fractions from the column liquid chromatography were in good agreement with that of pure reagents. The recovery of here model compounds were high. The proposed method was successfully applied to characterize heavy asphalt samples and showed high resolution, reliability and recovery. Some heavy asphalt were analyzed by this method, and the separated fractions were analyzed by IR and ^1HMR which showed satisfactory separation.
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