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By L. M. Jackman, S. Sternhell, D. H. R. Barton and W. Doering (Auth.)

ISBN-10: 0080229530

ISBN-13: 9780080229539

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Extra resources for Application of Nuclear Magnetic Resonance Spectroscopy in Organic Chemistry

Example text

Even when this method is employed it is wise to calibrate a second spectrum, in which the field is swept in the opposite direction, and check the consistency of the results. Another method of determining line separations, known as the "wiggle beat" technique, is ideal for measuring small separations ( < 15 Hz) such as observed for many spin multiplets. We have seen that rapid sweeping through sharp signals produces a distortion known as ringing (p. 35). The ringing pattern from a single absorption peak decays exponentially.

In practice, it is possible to modulate simultaneously at more than one frequency. As we are only interested in the relative positions of resonance absorptions in a spectrum (p. 12) we wish to measure the position of a given absorption relative to a reference or control absorption which is observed at a constant field-to-frequency ratio. The control absorption can be derived from a separate sample {external lock system) or from a reference compound added to the sample under investigation {internal lock system).

2403 for references). φ spectrum which is frequently of interest and it appears to be sensitive to the 1 1 03 presence of aromatic solutes. Acetonitrile, dioxan and t-butanol have also 1 3 04 been recommended, the first two being preferred, since t-butanol appears to be more affected by aromatic solutes. Tetramethylammonium chloride has been used as an internal reference for concentrated sulphuric acid solu6 3 1 7 94 t i o n s ' and is probably satisfactory for aqueous solutions. The absorp- An Introduction to NMR Spectroscopy 48 tion signal of water itself is an unsatisfactory reference as its position is sensitive to both pH and temperature.

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Application of Nuclear Magnetic Resonance Spectroscopy in Organic Chemistry by L. M. Jackman, S. Sternhell, D. H. R. Barton and W. Doering (Auth.)


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