Home Analytical Chem NMR Sample Preparation
Steps
  1. 1 Gather all required materials --:--
  2. 2 Measure and transfer sample material 00:41
  3. 3 Dissolve sample in deuterochloroform 01:27
  4. 4 Transfer solution to NMR tube 02:14
  5. 5 Check sample depth with gauge 02:46
  6. 6 Label sample with student identifier 03:12
Analytical Chem YouTube (Curated Tutorials)

NMR Sample Preparation

Protocol
Difficulty
intermediate

Steps

1
Gather all required materials

Collect the NMR tube, micro test tube, sample of organic molecules, deuterochloroform solvent, weigh paper, microspatula, transfer pipette, and kimwipes needed for sample preparation.

▶ --:--
2
Measure and transfer sample material

Using a microspatula, measure out a few dozen milligrams of crystalline sample by visual estimation and transfer it to the small test tube, then return any unused sample to storage.

▶ 00:41
3
Dissolve sample in deuterochloroform

In the fume hood, add one pipette volume of deuterochloroform to the test tube containing the solid sample and aspirate gently with the pipette to agitate and ensure complete dissolution without undissolved solids remaining.

▶ 01:27
4
Transfer solution to NMR tube

Remove the cap from the NMR tube and carefully use the transfer pipette to transfer the dissolved solution into the NMR tube, being cautious not to break the pipette tip inside the tube.

▶ 02:14
5
Check sample depth with gauge

Replace the cap on the NMR tube and hold it up to the depth gauge on the lab bench to verify that the solvent level is above the minimum sample height line for proper analysis.

▶ 02:46
6
Label sample with student identifier

Using a fine-point Sharpie, write your Georgetown net ID directly on the top of the NMR tube so the TA can identify and track your sample during analysis.

▶ 03:12
💬 Comments coming soon