Home Analytical Chem How to Prepare and Run a NMR Sample
Steps
  1. 1 Gather materials and determine sample amounts 00:02
  2. 2 Dissolve sample in deuterated solvent 00:41
  3. 3 Filter sample into NMR tube 01:26
  4. 4 Adjust solvent level and label sample 02:19
  5. 5 Insert sample into NMR spectrometer 03:15
  6. 6 Configure spectrometer parameters and run experiment 05:14
  7. 7 Process data into final spectrum 05:36
Analytical Chem YouTube (Curated Tutorials)

How to Prepare and Run a NMR Sample

Protocol
Difficulty
intermediate

Steps

1
Gather materials and determine sample amounts

Collect your compound of interest, deuterated NMR solvent, NMR tube, lid, pipettes, and cotton for filtering. Determine the required sample amount: approximately 2-5 weeks for proton NMR or about 20 mg for carbon NMR.

▶ 00:02
2
Dissolve sample in deuterated solvent

Dissolve your compound in deuterated chloroform using approximately 0.7 mL of solvent to achieve about 4 centimeters of depth in the NMR tube. Mix thoroughly to ensure complete dissolution.

▶ 00:41
3
Filter sample into NMR tube

Use a cotton-wool filter in a pipette to filter your dissolved sample into an NMR tube, removing any particulate matter that could contaminate the instrument.

▶ 01:26
4
Adjust solvent level and label sample

Add fresh solvent to achieve the appropriate 4-centimeter fill depth in the NMR tube, cap the tube with a lid, and carefully label your sample to distinguish it from others in the lab queue.

▶ 02:19
5
Insert sample into NMR spectrometer

Place your labeled sample into a sample holder and use a depth gauge to ensure proper positioning. Wipe the outside of the tube to remove contaminants before carefully lowering it into the NMR machine using compressed air suspension or an automation robot arm.

▶ 03:15
6
Configure spectrometer parameters and run experiment

Input the sample information into the spectrometer, specifying that you are using deuterated chloroform as the solvent and select the desired NMR experiment (such as proton or hydrogen NMR). Start data acquisition.

▶ 05:14
7
Process data into final spectrum

Once data acquisition is complete, process the raw NMR data using the spectrometer software to generate and visualize the final NMR spectrum.

▶ 05:36
💬 Comments coming soon