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In-depth investigation on quantitative characterization of pyrolysis oil by P-31 NMR

机译：P-31 NMR对热解油定量表征的深入研究

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The characterization of different heteroatom functional groups by employing P-31 NMR has been developed for almost 30 years. In this study, an in-depth investigation of this commonly used method has been accomplished for the analysis of pyrolysis oil. Several commonly used internal standards for P-31 NMR have been examined by in situ monitoring. The results indicated that endo-N-hydroxy-5-norbornene2,3-dicarboximide (NHND) is not stable after a long period of storage or experiment (>12 hours), but both cyclohexanol and triphenylphosphine oxide (TPPO) can be used as internal standards if a long experiment or storage is required. The pyrolysis oil has also been investigated by both short time (16 hours) in situ monitoring and long time (14 days) ex situ monitoring. The results showed that aliphatic OH, carboxylic acids and water contents are not very stable after 2 hours, and thus a short time of preparation, storage, and experiment need to be considered to ensure a precise quantitative measurement. The decomposition products are still unclear, but some preliminary investigations for different acids, (e.g. formic acid) have been accomplished. The results indicated that the aromatic carboxylic acids (benzoic acid and vanillic acid) are more stable than formic acid and acetic acid. Interestingly, the formic acid will even decompose to some other compounds at the very beginning of the in situ monitoring test. Further characterization found that water is one of the major products for the decomposition of formic acid in the P-31 NMR solution. As far as we know, this is the first report on such time-dependent changes when using P-31 NMR to analyze the pyrolysis oil, and these results show that proper application of this method is essential to achieve reliable quantitative data.
机译：通过使用P-31 NMR的不同杂原子官能团的表征已经开发出近30年。在该研究中，已经实现了对这种常用方法的深入研究，以分析热解油。通过原位监测检查了几种常用的P-31 NMR内标准。结果表明，在长期的储存或实验（> 12小时）后，endo-N-羟基-5-降冰片烯2,3-二羧酰亚胺（NHND）在储存或实验（> 12小时）后不稳定，但环己醇和三苯基氧化膦（TPPO）可用作如果需要长实验或存储，则内部标准。在原位监测和长时间（14天）之前，也通过短时间（16小时）来研究热解油。结果表明，2小时后脂族哦，羧酸和水含量不是非常稳定的，因此需要考虑制备，储存和实验的短时间以确保精确的定量测量。分解产物尚不清楚，但已经完成了对不同酸的一些初步研究（例如甲酸）。结果表明，芳族羧酸（苯甲酸和香草）比甲酸和乙酸更稳定。有趣的是，在原位监测测试的开始，甲酸甚至会分解给一些其他化合物。进一步表征发现，水是P-31 NMR溶液中甲酸分解的主要产物之一。据我们所知，这是在使用P-31 NMR分析热解油的时间依赖性变化的第一个报告，这些结果表明，这种方法的适当应用对于实现可靠的定量数据至关重要。

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  • 来源
    《RSC Advances》 |2016年第21期|共7页
  • 作者

    Ben Haoxi; Ferrell Jack R. III;

  • 作者单位

    Natl Renewable Energy Lab Natl Bioenergy Ctr 15013 Denver West Pkwy Golden CO USA;

    Natl Renewable Energy Lab Natl Bioenergy Ctr 15013 Denver West Pkwy Golden CO USA;

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  • 正文语种 eng
  • 中图分类 化学;
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