Molecular mass estimation of derivatized compounds: a PFG NMR study

Molecular mass estimation of derivatized compounds: a PFG NMR study
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DOI:
10.1002/mrc.1991
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发表时间:
2007-06-01
影响因子:
2
通讯作者:
Harris, Douglas J.
Harris, Douglas J.
中科院分区:
化学3区
文献类型:
--
作者:
Crutchfield, Christopher A.;Harris, Douglas J.

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开发了脉冲场梯度(PFG)H-1和P-31 NMR方法来定量估计用三氯乙酰基异氰酸酯(TAI)或2-氯-4,4,5,5-四甲基-1,3,2-二氧磷杂环戊烷(氯磷杂环戊烷)衍生的化合物的分子量。这些试剂对含有醇、胺、羧酸或硫醇官能团的分子提供高灵敏度的选择性分析。使用四甲基硅烷(TMS)或双酚A作为内扩散参考。相对扩散系数和分子质量之间的经验关系,建立了一组单和双官能的化合物的分子量在32-330克/摩尔。通过对润滑油中醇、酚、羧酸组分的分析,证明了该方法的实用性。版权所有(C)2007约翰威利父子有限公司
Pulsed-field gradient (PFG) H-1 and P-31 NMR methods were developed to quantitatively estimate the molecular mass of compounds, derivatized with either trichloroacetyl isocyanate (TAI) or 2-chloro-4,4,5,5-tetramethyl-1,3,2-dioxaphospholane (chlorophospholane). These agents provide selective analysis with high sensitivity for molecules containing alcohol, amine, carboxylic acid, or thiol functional groups. Tetramethylsilane (TMS) or bisphenol A was used as internal diffusion reference. The empirical relationship between relative diffusivity and molecular mass was established for a set of mono- and difunctional compounds with molecular masses in the range 32-330 g/mol. The utility of the method was demonstrated by analyzing alcohol, phenol, and carboxylic acid components in lubricating oil. Copyright (C) 2007 John Wiley & Sons, Ltd.