The Nuclear Magnetic Resonance Laboratory is equipped with a Bruker Avance III HD 400 MHz spectrometer with a BBFO 31P-15N probe and a TXI 1H / 13C / 31P three-channel probe.
Type of analyzes performed
Routine measurements:
- 1H
- 31P{1H}, 31P
- 13C{1H}, 13C
Special measurements after agreeing with the operators.
Operation time
The spectrometer is available for continuous measurements (24 hours a day, 7 days a week), except during maintenance and service.
Terms of use
Only trained users have independent access to the spectrometer. Otherwise, staying in the laboratory is only possible in the presence of the operator. People who perform and order NMR measurements participate in the costs of using the spectrometer.
Persons authorized to operate the spectrometer:
- Rafał Grubba, Ph.D., D.Sc., Eng.
maintenance and measurements - Aleksandra Wiśniewska, Ph.D., Eng.
maintenance and measurements - Kinga Kaniewska-Laskowska, Ph.D., Eng.
measurements - Katarzyna Kowalewska, M.Sc.
measurements
Method of sample preparation and delivery
The samples should be prepared in high-precision (HP) NMR tubes with a diameter of 5 mm. Pay special attention to whether the tube is not damaged (e.g. small cracks), as this may damage the spectrometer. The sample should contain at least 0.7 ml of deuterated solvent (corresponding to a minimum of 5 cm of a column of liquid in the tube) and should not contain sediment. Samples should be tightly closed with a stopper. The minimum amounts of the solute depending on the spectrum are presented in the table below:
| Spectrum | Organic compound | Complex compound |
|---|---|---|
| 1H | 5 mg | 10 mg |
| 31P | 20 mg | 40 mg |
| 13C | 20 mg | 40 mg |
The sample should be labelled:
In addition, the sample data should be entered in the notebook with measurement records:
- Sample name
- Name of the ordering person
- Date
- Department
- Deuterated solvent
- Type of spectrum
- Desired measuring range for each type of spectrum
Samples for measurements to be performed on the changer should be left in the cabinet next to the entrance to the NMR laboratory in a container marked "Do pomiaru". The samples to be collected are in the same place in the container marked "Do odbioru". The notebook with the measurement records is located in the cabinet.
Method of carrying out measurements
Measurements are carried out in two modes, depending on the type of experiments performed and user rights:
- Automated measurements with sample changer (Z) – Samples collected during the day and measurements performed overnight. Samples are queued by operators or trained users.
- Self-measurements performed by trained users (S) – measurements performed during the day (S).
Receiving the results
Access to data, in electronic form, is possible via a network drive from anywhere in the Faculty and outside it.
