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Sample Preparation

Users are expected to provide their own NMR tubes and deuterated solvents and to bring tubes to the facility prefilled. NMR “spinners” and NMR-tube depth gauges are provided at each instrument. Correct use of the depth gauge is critical for obtaining quality data and to avoid tube breakage. Its use will also be emphasized during the training checkout. 

NMR samples must be disolved homogeneously in a deuterated solvent with (ideally) enough solvent to achieve a full sample height in the tube. Full height is 5 cm for the Agilent instruments in SE2-20 amd 3 cm for the Bruker 600 MHz at Castle. For a full-length Agilent sample, set the bottom of the depth guage at 70 mm. Insert the tube through the spinner, place the spinner in the guage and push the tube to the bottom. If a shorter solvent length is desired, center the solvent column about the line at 43 mm. A short sample that is not centered may fail at the "autoshim" step of the study. Even if centered, very short samples may have poorer resolution and fail. For a full-length Bruker sample set the tube bottom and meniscus at the marks. 

Remember to use the depth guage!  A poorly adjusted sample tube may break in the instrument and possibly cause expensive damage.