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  • J-modulation effects in DOSY experiments and their suppression: the Oneshot45 experiment.

J-modulation effects in DOSY experiments and their suppression: the Oneshot45 experiment.

Journal of magnetic resonance (San Diego, Calif. : 1997) (2010-12-28)
Adolfo Botana, Juan A Aguilar, Mathias Nilsson, Gareth A Morris
ABSTRACT

Diffusion-ordered spectroscopy (DOSY) is a powerful NMR method for identifying compounds in mixtures. DOSY experiments are very demanding of spectral quality; even small deviations from expected behaviour in NMR signals can cause significant distortions in the diffusion domain. This is a particular problem when signals overlap, so it is very important to be able to acquire clean data with as little overlap as possible. DOSY experiments all suffer to a greater or lesser extent from multiplet phase distortions caused by J-modulation, requiring a trade-off between such distortions and gradient pulse width. Multiplet distortions increase spectral overlap and may cause unexpected and misleading apparent diffusion coefficients in DOSY spectra. These effects are described here and a simple and effective remedy, the addition of a 45° purging pulse immediately before the onset of acquisition to remove the unwanted anti-phase terms, is demonstrated. As well as affording significantly cleaner results, the new method allows much longer diffusion-encoding pulses to be used without problems from J-modulation, and hence greatly increases the range of molecular sizes that can be studied for coupled spin systems. The sensitivity loss is negligible and the added phase cycling is modest. The new method is illustrated for a widely-used general purpose DOSY pulse sequence, Oneshot.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Tetramethylsilane, electronic grade, ≥99.99% trace metals basis
Supelco
Tetramethylsilane, analytical standard, for NMR spectroscopy, ACS reagent
Sigma-Aldrich
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Sigma-Aldrich
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Supelco
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Sigma-Aldrich
Camphene, 95%