Home › Analytical Chem › NMR Sample Preparation
Steps
  1. 1 Select sample mass by NMR type 00:04
  2. 2 Prepare solvent and fill NMR tube 00:24
  3. 3 Dissolve sample in solvent method 00:40
  4. 4 Add solid sample direct method 01:29
  5. 5 Add reference standard to tube 02:06
  6. 6 Cap the sample tube 02:15
  7. 7 Label tube with sample information 02:23
  8. 8 Clean and store NMR tube 02:45
Analytical Chem YouTube (Curated Tutorials)

NMR Sample Preparation

Protocol
Difficulty
intermediate

Steps

1
Select sample mass by NMR type

Determine the appropriate sample mass based on your NMR experiment: use 10-15 milligrams for proton NMR or 50 milligrams for carbon NMR.

▶ 00:04
2
Prepare solvent and fill NMR tube

Add 0.6 milliliters of deuterated solvent to achieve a sample depth of 4-5 centimeters from the bottom of the tube.

▶ 00:24
3
Dissolve sample in solvent method

Place the compound in tin foil, add the deuterated solvent, and mix until completely dissolved. Then transfer the solution into the NMR tube.

▶ 00:40
4
Add solid sample direct method

Alternatively, scoop solid sample directly into the NMR tube using weighing paper, gently tap the tube, then add the deuterated solvent.

▶ 01:29
5
Add reference standard to tube

Add an internal reference compound to the prepared sample solution for NMR calibration.

▶ 02:06
6
Cap the sample tube

Securely place a cap on the NMR tube to prevent sample evaporation and contamination.

▶ 02:15
7
Label tube with sample information

Create a detailed label including the compound structure, nuclei to observe, solvent type, concentration, date, and your initials for sample identification and return.

▶ 02:23
8
Clean and store NMR tube

Empty the used sample solution and rinse the NMR tube thoroughly with acetone, then store for future use.

▶ 02:45
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