University of the Basque Country UPV / EHU General Service Nuclear Magnetic Resonance Unit (Guipúzcoa) Chemical Sciences faculty Pº Manuel Lardizabal, 3, 20018 Donostia-San Sebastián (Guipúzcoa) Edificio Joxe Mari Korta Avda Tolosa, 72 20018 Donostia-San Sebastian (Guipúzcoa) General Service Nuclear Magnetic Resonance Unit (Vizcaya) Faculty of Science and Technology Barrio Sarriena CD3, s / n 48940 Leioa (Vizcaya) General Service Nuclear Magnetic Resonance Unit (Álava) Faculty of Pharmacy Basement Paseo de la Universidad, 7 01006 Vitoria-Gasteiz (Alava) Lucio building Lascaray (CIEA) Miguel de Unamuno, 01006 Vitoria-Gasteiz 3 (Álava)
Access to the unit of Nuclear Magnetic Resonance (NMR) involves meeting the requirements set forth in the Protocol for access to SGIker and the services it provides. Similarly, the Specific standards for access to NMR Bizkaia must be meet .
The germ that grew into the current NMR Service of the UPV/EHU sprouted in 1996, combining high-field NMR equipment (frequencies from 1H to 200 MHz) from the Departments of Organic Chemistry (Chemistry Faculty of San Sebastián, the Pharmacy Faculty of Vitoria and the Faculty of Science and Technology of Leioa), in addition to the Material Physics Department at the Chemistry Faculty of San Sebastián. Since 2002, the NMR Service has adapted to the new Regulations governing the Advanced Research Facilities (SGIker) of the University, in accordance with the directives set out in the First University Plan. It was set up to lend supra-departmental support to basic and applied research that may be accessed by all researchers from the UPV/EHU, from the Basque Network of Science, Technology and Innovation (RVCTI), and also other external researchers, under similar conditions to those from the UPV/EHU. The NMR Service is arranged into three Units. The administrative headquarters and address for the Service is at the Chemistry Faculty (San Sebastián), which is associated with the Units of the Pharmacy Faculty (Vitoria) and the Faculty of Science and Technology (Leioa). The aim of this distribution of equipment is to bring the facilities offered by the Service closer to direct users and to facilitate their use. The main facilities consist of the structural study of organic and organometallic molecules, biomolecules, materials, additives and traces, etc. via the qualitative and quantitative determination of their components. It is also possible to approach the study of dynamics processes and structural changes with temperature, etc., in the aforementioned materials. The current equipment enables work to be carried out under simultaneous observation of different nuclei, including: 1H, 13C, 19F, 31P, 29 Si, etc. All the installations and equipment are inter-connected via the UPV/EHU data network and the spectra acquired in the different equipment may be accessed from any installation existing at the UPV/EHU or the Basque Technology Network, just by having a minimal infrastructure at one's disposal (personal computer). The NMR Service is willing to adapt at any time to the needs of its users, whereby the equipment available has a sufficiently open configuration to enable complements to be incorporated (particularly probes and additional software programmes) that are able to meet new needs. The NMR Service equipment comprises nine instruments in total, three of which can be considered routine (300 MHz, samples in solution) and operate exclusively on a self-service basis for basic research at the UPV/EHU. The two 500 MHz pieces of equipment (located in San Sebastián and Leioa), two 400 MHz equipment (three channels/CPMAS) in Vitoria (19F-broadband San Sebastian), and two spectrometer for solid state sample 400Mhz and 300 MHz equipment located in San Sebastián, are those set aside for the provision of external services. There are three types of rate for accessing the NMR Service facilities: a) on a self-service basis, only for authorised personnel, b) via ordinary service, which includes carrying out experiments without interpretation by Service personnel, and c) service under contract. Access on a self-service basis (recommended for research scholarship holders who work with routine samples) only depends on user needs and the authorisation of the Service coordinator. The self-service system guarantees the simultaneous use of equipment, favouring the dissemination of the NMR technique among users. Access as an ordinary service (for internal and external users of the UPV/EHU who are interested in information about spectra but not in their registration details), constitutes an attempt to lend effective support to basic and applied research to the maximum possible number of university departments and technology centres that decide to make use of NMR in their projects and contracts, etc. Lastly, the service under contract is aimed at any user who wishes to carry out an analysis or structural study of unknown substances or materials, etc. via the integral management of the problem. It includes the preparation of samples, carrying out of personalized experiments, interpretation of results and drafting of reports, etc. This is done according to estimate and is aimed at users who, being unfamiliar with NMR, wish to obtain analytical results using this technique. The protocol of access to the Advanced Research Facilities enables all NMR users to access their services via personnel from the Units, both in order to carry out routine experiments and others of greater complexity. To acquire spectra via the ordinary service by NMR Service personnel, all that is required is a request sent to the contact persons at the different Units and to adhere to the rules for use.
Performing NMR spectra of different nuclei, including 1H, 19F, 13C, 31P, 15N, 29Si 27Al, 113Cd… of liquid,solution, gels or solid sample, with simultaneous observation of two or three channels and with Z axis gradients, applicable in, for example: - Structural identification of unknown compounds by means of 1D and 2D experiments. - Confirmation of structures and determining compositions in mixtures. - Direct characterisation of fruit juices by means of the statistical analysis of 1H and 13C signals.- Determining residual monomer in aqueous polymerizations. - Determining polymers and additives in plastic formulas by means of 1H and 13C combined analysis and heteronuclear correlation 2D experiments. - Non-chromatographic characterisation and determination of surfactants in aqueous formulations. - Analysis of narcotic substances and adulterating agents in drugs. - Determining enantiomeric excess. - Determining the dissolved structure. - Conformational analysis of peptides or small proteins in water, DMSO etc… by means of NOESY/ROESY experiments combined with molecular modelling (XPLOR). - Monitoring reaction, kinetic, molecular association constant processes. - Determining diffusion coefficients (DOSY). - Determining T1 relaxation times. - Polymorphism studies. Distinguishing polymorphs in pharmaceutical formulations by means of CPMAS (13C).
The NMR Service provides users with a wide variety of NMR experiments carried out in different magnetic fields, ranging from 300 to 500 MHz, with the collaboration of its technical personnel. All requests and enquiries are treated with the utmost confidentiality. The results obtained using NMR techniques may be complemented by other analytical techniques available at the Advanced Research Facilities (SGIker) of the UPV/EHU, university departments and technology centres, etc. The results obtained from the experiments carried out by users on a self-service basis or via ordinary service are uploaded on the NMR server and may be collected via ftp by those interested parties. Users of the service under contract may, in addition to in electronic format, request printed spectra via fax or ordinary post. The corresponding reports can also be drafted by prior request in which the results obtained are interpreted. In the case of standard experiments (1H, 13 C) and except in cases of force majeure, results can be made available within a period of 48 hours from the time of receipt of the samples and instructions. The possibility also exists of replying faster, according to certain needs. Facilities: By way of a prior step to the provision of the services indicated, enquiries may be made without any commitment as regards the most suitable experiments or possibilities available for dealing with the problems raised. Acquiring NMR spectra from different nuclei, including 1H, 19F, 13C, 31P, 15N , 29Si , 27Al, 113Cd, etc. of liquid samples, solutions and gels, with simultaneous observation of two or three channels and with gradients on Z axis. Solid spectra are acquired using the CPMAS spectra (Cross Polarization Magical Angle Spinning ) a variable temperature with a sample rotation speed of approximately 10,000 Hz. The nuclei that can be observed with the probe available are, among others, 13C, 27Al, 29Si and 31P. Reports on the results obtained (on a request basis). Allocation of spectra (on a request basis). Advice in the field of application involving the NMR technique. Implementation, development of NMR methods and experiments for researchers from the UPV/EHU and technology centres. The technical features of the spectrometers, probes and software available may be consulted in the equipment section. The person in charge of the NMR Service should be consulted if more detailed information is required regarding facilities and the possibilities offered by the equipment. Applications: NMR can be used in a wide variety of industrial applications, ranging from the identification of unknown products to the monitoring of quality control processes, the study of catalysis, and allocation / confirmation of end products. It is possible to study a large number of organic and inorganic (non-ferrous) products via NMR in solution, its only being necessary for the material to be soluble in some deutered solvent. Some of the applications are listed below: Structural identification . Confirmation of structures. Identification of composites. Composition of samples. Molecular mobility: determination of conformations in solution. Monitoring of process , kinetics. Polymorphism studies . Determination of association processes. High and low temperature studies . Determination of enantiomeric excess. One of the advantages of the technique is its non-destructive nature, which means that the sample can be recovered if required.
Two-channel console with gradients (50G/cm) on Z axis.
Two-channel inverse detection probe BBI 1H / 31P- 109 Ag gradients on the Z axis. Temperature interval: -100 °C +180 °C.
Two-channel direct detection probe BBO 1H / 31P- 15 N gradients on the Z axis. Temperature interval: -100 °C +180 °C.
Two-channel direct detection probe BBO 1H-19F / 31P- 15 N gradients on the Z axis. Temperature interval: -100 °C +180 °C.
Two-channel console with gradients (50G/cm) on Z axis.
Two-channel inverse detection probe BBI 1H / 31P- 109Ag gradients on the Z axis. Temperature interval: -100 °C +180 °C.
High-precision temperature control from -150 to +400 °C. Gas conditioning system with a work interval from -10 °C to +90 °C. Additional gas conditioning system with a work interval from +20 °C to -150 °C.
PC control computer with Windows
Location: Faculty of Science and Technology Leioa
Three-channel console with gradients (50G/cm) on Z axis.
5mm QNP probe pre-tuned for (1H/13C/19F/31P) with gradients on the Z axis. Temperature interval: -150 °C +180 °C.
High-precision temperature control unit from -150 to +400 °C. Gas conditioning system with a work interval from -10 °C to +90 °C. Additional gas conditioning system with a work interval from +20 °C to -150 °C.
PC control computer
Location: Pharmacy Faculty Vitoria-Gasteiz
Two-channel console with gradient (50G/cm) in axis Z two channel, direct detection BBO ^1 H-^19 F / ^31 P- ^15 N (Z axis gradient). Temperature interval : -100°C +180 °C.
Unidad de control de temperatura de alta precisión -150 hasta +400 °C. Sistema de acondicionamiento de gases con una intervalo de trabajo de -10 °C hasta +90 °C. Sistema de acondicionamiento de gases adicional con un intervalo de trabajo de +20 °C a -150 °C
PC control computer with Linux
Location: Joxe Mari Korta R&D Centre
Broadband two-channel probe BBO 31P- 109Ag/1H . Temperature interval: -100 °C +180 °C. Suitable for studying heteronuclei.
High-precision temperature control unit from -150 to +400°C. Gas conditioning system with a work interval from -10°C to +90°C. Additional gas conditioning system with a work interval from +20°C to -150°C
PC computer control with Linux
Location: Chemistry Faculty Donostia
Three channel console.
1.3 mm probe high speed (60 KHz) ^1 H-^19 F / X. Temperature interval: -30 °C +70 °C.
4 mm probe for solid sample (CP-MAS) ^1 H-^19 F / X / Y ( ^13 C, ^15 N,^31 P, ^27 Al,^29 Si ) Temperature interval : -150 °C +180 °C.
7 mm probe for solid samples (CP-MAS) ^1 H / X( ^31 P- ^15 N). Temperature interval : -150 °C 180 °C.
High-precision temperature control unit from -270 °C to +400 °C. Gas conditioning system with a work interval from -10 °C to +90 °C. Gas conditioning system with a work interval from -150 °C to 20 °C.