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Contact, Our Facility, NMR Service

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Contact Dr. Debbie Shalev Our Facility NMR Services / Sample Requirements

 

Queries and comments are welcome. Last updated November, 2003



 
 
 

 

Contact Dr. Debbie Shalev:
 

Phone:    02-6585460
Fax:        02-6585573
E-mail: debbie@macbeth.ls.huji.ac.il
Mail:
Wolfson Centre for Applied Structural Biology, Room 15
Hebrew University of Jerusalem
Edmond Safra Campus, Givat Ram
Jerusalem 91904, Israel
Directions to the Hebrew University and the Wolfson Centre
                                                                                                         Debbie's Page

Go to NMR Home

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Our Facility: 600 MHz Spectrometer
 

    • The NMR spectrometer is a Bruker Avance

    • DMX 600 MHz NMR spectrometer.

     
    • It has four channels and XYZ gradients.

     
    • It is equipped with selective, inverse and

    • multinuclear probes.

     
    • The spectrometer has a temperature

    • range of 0-60 degrees Celsius.

     
    • There is a preparation laboratory adjacent to

    • the spectrometer room for sample preparation.
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NMR Services:

We are happy to provide NMR services for academic institutions and for industry.

Please see sample requirements below.

For information regarding prices and scheduling, please contact Debbie Shalev.

 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 

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Sample requirements:
 

Amount
Purity
Solvent choice
Buffer and salt considerations
Stability
Recovery
Physical State of Compound
Additional Recommendations

It is strongly recommended to consult Debbie before preparing the sample.

Amount
A minimum of 1-3 mM of compound in 400-500 mL  is required forpreliminary assessment of NMR spectra for structural work.
This corresponds to 0.4-1.6 mmole of compound.
(Multiply by molecular weight for necessary sample weight in grams.)A minimum of 1-3 mM of compound in 400-500 mL  is required forpreliminary assessment of NMR spectra for structural work.
This corresponds to 0.4-1.6 mmole of compound.
(Multiply by molecular weight for necessary sample weight in grams.) The sample will be recoverable if degradation does not occur. One-dimensional spectra for compound identification by comparison
requires a minimum of approximately 0.6 mM in 400 mL (0.25 mmole).

     

     

Purity:

The sample must be >95% pure by HPLC for structural work.

 

Solvent:

The sample will need to be dissolved in deuterated solvent or deuteratedsolvent will need to be added to the sample. It is recommended to bring well lyophilized compound and prepare the sample in the NMR preparatory laboratory.

 

Buffers/salts:

All buffers and salts used in the process of sample preparation must either be removed or must conform to NMR requirements:

All buffers and salts must not be protonated (only inorganic buffers and salts -
no hydrogens). Usually this means using phosphate buffer and inorganic salts.

 

Stability:

The sample must be stable under the acquisition conditions for a timescale of weeks.

 

Recovery:

NMR does not harm samples in any way and samples should be completely recoverable unless they undergo degradation of any form or mechanical loss of compound occurs.

 

Physical state of the compound :

The compound must be completely soluble or miscible with the chosen solvent. It must be monomeric in solution.

 

Recommendations:

It is very highly recommended that the sample be well defined before arriving at the NMR:

NMR is a very expensive way to follow the kinetics of degradation.Make sure that the sample is stable, well-disolved and think about the temperature
parameters you want to use and the desired pH (acidic is better for NMR).

 

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