Quantitative 14N NMR

Lawrence Byrnes (numare@cnj.digex.net)
Wed, 14 Feb 96 18:09:20 PST

14 February 1996, Wednesday, 1815 EST

Update:

Thanks to all who responded with suggestions and personal experiences
for observation of 35Cl with a system designed for 15N to 31P. Was able to
do quantitative 35Cl NMR determination of aqueous chloride with recovery
> 0.9964 Happy to share method with anyone interested.

Question:

Would now like to be able to perform quantitative 14N NMR analysis of
aq. soln., conc. ca. 11.4 mM, seven different nitrogens in cmpd.

Have observed what appear to be real NMR signals. However, when 90%
DMF in DMSO 15N sensitivity std. is observed, no sig. difference from signals
due to probe with no sample. Have considered possibility that observed
signals are electronic artifact rather than real or may be due to solid phase
nitrogen in adhesive that fastens rf coils to quartz coil supports. If the
latter is the case, perhaps the conc. of N in adhesive >> than conc. of N in
analytical sample.

'Signal' is two broad humps. Low field signal is about twice the
intensity of high field signal. Peak widths at half heights ca. 7000 Hz. Can
move in spectral window by adjusting transmitter offset. No phasing problem.

Any ideas/suggestions will be appreciated.

Thank you,

Best regards,

Lawrence
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Numare Spectralab, Inc.,
10 Summit Avenue, Unit 6, P.O. Box 96,
Berkeley Heights, NJ, 07922-0096,
Telephone 908-665-0066
Telefax 908-464-4192

Name: Lawrence Byrnes
E-mail: numare@cnj.digex.net (Lawrence Byrnes)
www: http://www.cnj.digex.net/~numare/index.html
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