High-performance liquid chromatography with nuclear magnetic resonance detection applied to organosilicon polymers. Part 2. Comparison with other methods.
LC-NMR utilizing (1)H and (29)Si NMR spectroscopy is ideally suited for the analysis of silicones. It is shown that reversed phase gradient LC-NMR surpasses standard gel permeation chromatography (GPC) and diffusion ordered spectroscopy (DOSY) in the analysis of model hydride terminated polydimethylsiloxane. (1)H and (29)Si NMR in the stopped-flow arrangement leads to full identification of the components. Concentration gradient introduces a dependence of the (29)Si shifts on solvent composition, this dependence can be substantially reduced by a proposed method of referencing. It is shown that the ADEQUATE version of powerful but insensitive 2D INADEQUATE experiment can be used for complete line assignment.
Blechta
Vratislav
V
Institute of Chemical Process Fundamentals, Academy of Sciences, Rozvojová 135, 16502 Prague, Czech Republic.
Kurfürst
Milan
M
Sýkora
Jan
J
Schraml
Jan
J
D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D011108:Polymers / Q000737:chemistry*; D015203:Reproducibility of Results; D012825:Silicon / Q000737:chemistry*; D012997:Solvents / Q000737:chemistry
D011108:Polymers; D012997:Solvents; D012825:Silicon