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NMR Services

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Service procedure and preparation

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LMA-Laboratory of Molecular Analysis

Nuclear Magnetic Resonance (NMR) Services

Laboratory of Molecular Analysis infrastructure includes three Varian NMR spectrometers. A 600 and a 300 MHz for high resolution NMR experiments, and a 400 MHz for solid state samples. The 300 MHz spectrometer is equipped with a 9 sample carousel for fast and automated routine NMR experiments.

Services Provided

Material Characterization
Molecular Structure Determination
Polymorphism of drugs
Study of bio-inorganic complexes (i.e Sn or Ti complexes with citrate)
Study of Zeolites (27Al, 29Si)
Study of drug:membrane interactions
Study of the structure of cellulose (13C CP/MAS)
Analysis of archaeological samples
Structure elucidation of natural products
Analytical Problem Solving

We offer :

High Spectral Quality and Information Content at a Reasonable Cost
Spectral Interpretation and Analysis Services
Spectra can be sent to customer by Email attachment in a variety of formats (Postscript, Microsoft Word File, PDF, JPEG etc).
In addition to the NMR service we can provide molecular modelling services.

Contact Details

Tel. +30210.72.73.870
Fax. +30210.72.73.872
e-mail. lmaservices@eie.gr

Infrastructure

HR-NMR Technical Characteristics

Varian V600 MHz

This spectrometer was installed in July 2007 and has the following features:

2 RF Channels
Z-axis Pulse Field Gradient module
Ultrastable temperature control
Variable Temperature capabilities (from -80 to 130 ^oC)

¹ H( ¹⁵N- ³¹P) PFG AutoX Indirect 600 probe
4mm Nanoprobe (gHX 8 ¹⁵W- ³¹P[ ¹H] )
¹ H- ¹⁹F/ ¹⁵N- ³¹P AutoX Dual BB600 probe

Two dimensional spectra such as COSY, TOCSY, NOESY, HSQC amd HMBC to fully characterize small molecules

Varian V300 MHz

2 RF Channels
Z-axis Pulse Field Gradient module
Auto sampler unit with 9 sample positions
Ultrastable temperature control
Variable Temperature capabilities (from 25 to 150 ^oC)

5mm BB( ³¹P- ¹⁰⁹Ag) observe ¹H/ ³¹P decouple
Gradient enabled acquisition of ¹H- ¹⁹F/ ¹³C- ³¹P

Solid-State NMR Technical Characteristics

Solid-state NMR analysis covers a wide range of applications that cannot be addressed by liquid-state experiments. In solid-state NMR samples are place in 3,2 mm diameter spinning rotors and spun at high speeds (3-15 kHz) in order to allow acquisition of NMR spectra with sufficient resolution to allow chemical determinations to be made.

Varian V400 MHz Solid-State NMR

2 RF Channels
Magic-angle spinning (MAS)
Cross-Polarization Magic angle spinning (CP-MAS)
Fast MAS rates - up to 15 kHz.
Ultrastable temperature control
Variable Temperature capabilities (from 50 to 100 ^oC)
3,2mm Double Resonance HX-MAS probe

Other than routine nuclei (¹³C, ³¹P) are done upon request and discussion.

Service Procedure and Preparation

Samples must be accompanied by a fully completed form which can be downloaded as PDF and can either be brought personally or sent by mail service.
Samples should be submitted with the appropriate documentation
Please include as much information as possible on the sample - possible structures (X-ray or MS data if available), expected results, solvent solubility.
NMR experiment requirements
Complete and attach the NMR Service Request Form with the samples. Customers should indicate if the samples are to be returned after analysis (charges apply).

Sample requirements

¹³C Experiments require 10-20 milligrams for quantitative data to be obtained in a timely manner.
¹H and 2D experiments require less sample (minimum 1mg).
Sub-milligram quantity samples must be arranged beforehand as special NMR tubes and solvents/standards must be prepared.
As a general rule, experimental time decreases as sample quantity increases.

Prices

Pricelist [pdf]

Samples should be submitted to :

NMR services, Laboratory of Molecular Analysis, Division of Organic and Division Chemistry, National Hellenic Research Foundation, Vas. Constantinou 48, 11635, Athens, Greece

Tel. +30210.72.73.870
Fax. +30210.72.73.872
e-mail: lmaservices

Confidentiality agreement

Laboratory personnel is very experienced in dealing with samples of a confidential nature. Confidentiality can be ensured either on an informal basis or by contracting a customized "non disclosure" agreement.

Last Update: 02.07.2012