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Molecular mass estimation of derivatized compounds: a PFG NMR study
Author(s) -
Crutchfield Christopher A.,
Harris Douglas J.
Publication year - 2007
Publication title -
magnetic resonance in chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.483
H-Index - 72
eISSN - 1097-458X
pISSN - 0749-1581
DOI - 10.1002/mrc.1991
Subject(s) - chemistry , tetramethylsilane , carboxylic acid , alcohol , phenol , bisphenol a , organic chemistry , isocyanate , molecule , mass spectrometry , pulsed field gradient , amine gas treating , chromatography , epoxy , polyurethane
Pulsed‐field gradient (PFG) 1 H and 31 P 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 © 2007 John Wiley & Sons, Ltd.