Preparation of an NMR Sample

Use a specialized thin spatula with a trough to transfer the solid compound into the NMR tube. Fill the bowl portion at the bottom of the tube with approximately two scoops of solid material for a concentrated sample suitable for carbon or proton NMR analysis.

Using a pipette, add approximately one inch or two finger-widths of NMR solvent to the tube containing the solid compound. Pour slowly and carefully to reach the proper volume.

Place a cap on the NMR tube and invert it repeatedly to dissolve the solid compound into the solvent. Ensure complete dissolution before proceeding, as solid particles will prevent proper locking of the NMR instrument.

If the compound does not dissolve easily through inversion, use a sonicator to aid dissolution. It is recommended to test solubility of the compound in the NMR solvent in advance to avoid this issue.

For liquid samples, dip the tip of a pipette into the liquid to fill approximately the lower half inch to one centimeter of the pipette tip. Carefully insert the pipette into the NMR tube without losing the sample.

Carefully add NMR solvent to the tube containing the liquid sample. Add solvent gradually to avoid exceeding the proper fill level, which is easy to overshoot.