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含磷试剂衍生-核磁共振技术分析醇类化合物 被引量:1
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作者 李腾 黄桂兰 +1 位作者 袁铃 周世坤 《分析科学学报》 CAS CSCD 北大核心 2018年第2期205-208,共4页
本研究以含磷试剂二苯基次膦酰氯、三氯氧磷、2-氯-4,4,5,5-四甲基-1,3,2-二噁磷杂戊环(CTMP)为衍生试剂,对5种醇类化合物奎宁醇、硫二甘醇、甲基二乙醇胺、三乙醇胺、二异丙胺基乙醇进行衍生化,然后进行^(31)P{~1H}-NMR谱测定。实验考... 本研究以含磷试剂二苯基次膦酰氯、三氯氧磷、2-氯-4,4,5,5-四甲基-1,3,2-二噁磷杂戊环(CTMP)为衍生试剂,对5种醇类化合物奎宁醇、硫二甘醇、甲基二乙醇胺、三乙醇胺、二异丙胺基乙醇进行衍生化,然后进行^(31)P{~1H}-NMR谱测定。实验考察了衍生试剂、衍生溶剂、缚酸剂作用,以及衍生时间和温度对衍生效率的影响。结果表明,以二苯基次膦酰氯为衍生试剂,二甲基甲酰胺(DMF)为衍生溶剂,吡啶作为缚酸剂,50℃衍生1h衍生条件下,5种目标化合物奎宁醇、硫二甘醇、甲基二乙醇胺、三乙醇胺、二异丙胺基乙醇的检出限(S/N=3)依次为8.90、7.33、5.95、5.96、10.16μg/mL。该方法具有良好的专一性和稳定性。同时考察了水样基质中该衍生方法的回收率。 展开更多
关键词 31p{1H}-nmr 磷酰化衍生 非磷前体 化学毒剂
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STUDIES ON THE CHEMICAL STRUCTURES OFACTIVATED CARBON FIBERS BY SOLID STATE NMR
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作者 FU Ruowen LIU Ling +2 位作者 ZENG Hanmin HUANG Wenqiang SUN Pingchuan 《Chinese Journal of Reactive Polymers》 1999年第1期12-19,共8页
The solid stale C13-NMR spectra of different ACFs from various precursor fiberswere recorded in this paper. The effects of activation conditions on chemical structuresOf ACFs, as well as the changes of chemical struct... The solid stale C13-NMR spectra of different ACFs from various precursor fiberswere recorded in this paper. The effects of activation conditions on chemical structuresOf ACFs, as well as the changes of chemical structures during carbonization and redoxreaction were investigated by NMR technique. At same time, the solid state P31-NMRspectra of ACFs are studied The C13-NMR spectra of ACFs can be divided into sixbands that are assigned to methyl and methylene groups, hydroxyl and ether groups,acetal (or methylenedioxy carbon, graphite-like aromatic carbon structure, phenol,and quinone groups, respectively. Only phosphorous pentoxide exists on ACFs andCFs. Moreover, most of them are stuck over the crystal face but not at the edge ofgraphite-like micro-crystaL The carbonization and activation conditions affect theC13-NMR spectra of ACFs. The experimental results indicate that the redox reactionof ACFs with oxidants greatly consumes C-H group. 展开更多
关键词 Activated carbon fiber Solid state C13-nmr Solid state p31-nmr Oxidation-reduction
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