Dissolved samples were intermittently vortexed over a period of ~ 5 min, centrifuged (1500×g, 20 min), and supernatant transferred to 10 mm NMR tubes for P-NMR analysis.
All spectra were acquired in 3 mm NMR tubes using a Bruker 5 mm TCI cryogenically cooled NMR probe.
These results show that the preparative GC purification step, and later sample recovery and NMR sample preparation steps did not introduce significant contaminations into the NMR tubes.
We directly loaded 1-mm capillary NMR tubes with known amounts of the model compound geranyl acetate, and subjected them to 1H-NMR analysis.
Nuclear magnetic resonance (NMR) spectra were recorded at 293 K on 300 or 400 MHz Varian Mercury Vx spectrometers using 5 mm NMR tubes.
Fig. 1 shows the background spectrum due to deionized water and the glass NMR tubes.
The aliquots were dispensed into the magnetism-free NMR tubes (Shigemi, Tokyo, Japan).
With the solid, obtained NMR tubes were prepared in deuterated dimethyl sulfoxide (DMSO-d6).
Finally, 500 µL portions of reconstituted mixture were transferred to NMR tubes for further NMR analysis.
After filtration through a glass wool filter, the samples were placed in NMR tubes for analysis.
Moreover these results have been produced with large sample volumes (∼100 µL, i.e. 3 mm diameter NMR tubes).
