Services
Availability:
Measurements are performed on request of teachers and/or researchers/doctoral students.
Opening hours: M-F 9-17; the night schedule is established by mutual agreement between the operators, by recording into an internal register the person who will set the measurement during the night. These measurements will need to be completed by 8:00 the next morning at the latest
The operation of the spectrometers is allowed only to personnel specialized and trained in the operation of the spectrometers. The RMN infrastructure serves the entire academic community of the university and faculty as well as students at all levels of training (bachelor's, master's, doctorate) both in research activities and in specific teaching activities (trainings for determining the structures of synthetic and/or natural compounds).Infrastructura RMN se utilizează de asemenea și în proiectele de cercetare implementate în facultate dar și în relațiile de parteneriat sau contractuale cu alte instituții sau entități private.
The NMR spectroscopy system also responds to requests from outside the academic community, namely useful measurements for private entities, based on a service contract.
At the request of teaching staff, access to the NMR laboratory is ensured for students from the faculty, or for visitors/external collaborators, for a short demonstration of how it works and/or utility of the spectrometry system.
The conditions of access to NMR analyzes and the method of access to the recording of NMR spectra is described below.
Characteristics and information regarding samples submitted for NMR analyses:
Instructions and guidelines:
The set of instructions and guidelines presented below are subject to change without prior notice. These instructions are intended to make the equipment more efficient related to NMR laboratory resources
- Proton spectra can be requested by teachers/researchers/doctoral students and direct faculty collaborators by simply handing over the samples and completing an "NMR spectra request bulletin". The spectra are recorded at the normal working temperature of the spectrometer (20 0C). Spectra requested by students will be done through the teaching staff or the researcher with whom they carry out the activities.
- Spectra of unusual nuclei, 2D spectra, spectra at variable temperatures, other less common techniques, will be performed only after consultation and with the opinion of the persons appointed in this regard. Approval is given on the request form mentioned in point 1.
- Higher-than-normal temperature recordings can currently be made for proton spectra up to 80 C and for a maximum duration of 2 hours. It is mandatory that these records are continuously monitored, there is a danger of damage to the probe head if there is a deficiency in the gas flow that ensures the heating.
- Lower than normal temperature recordings can currently be made for proton spectra down to -50 0C and for a maximum duration of 2 hours. It is mandatory that these records are continuously monitored, there is a danger of damage to the sample head if there is a deficiency in the gas flow that ensures the cooling of the sample (the appearance of ice on the cooling stream).
- Recordings of spectra longer than 2 hours can only be done overnight and only for proton and carbon spectra, at room temperature. Bruker recommends monitoring the operation of the equipment. In the event that registrations will be made outside normal working hours, the applicant will usually provide a person to accompany the operator of the device.
- Obtaining accurate spectra is achieved following these recommendations:
- purification of the samples as much as possible and their delivery in appropriate packaging that does not contaminate the sample;
- notifying the NMR staff of any special rules for handling samples;
- determination of the appropriate solvent by trials with common, non-deuterated solvents, taking into account that:
- the dissolving power of deuterated solvents may be lower than their non-deuterated counterparts
- to obtain a good spectrum, concentrations close to 0.2 mmol/ml are required for 1H-NMR spectra and above 2 mmol/ml for 13C-NMR spectra;
- provide a suitable container if sample recovery is desired.
- evidence coding; each sample may be coded according to the applicant's own system. The sample code will be entered in this way, by the NMR operator, in the registration system;
- The registration of routine spectra is carried out according to the "first come, first served" principle, being equidistant from all applicants from the faculty, or direct collaborators, without favoritism and without discrimination. The recording of the spectra is carried out in the order of the requests received.
In completely exceptional and well-motivated situations, with the approval of the authorized persons, exceptions to the order of the request can be made, within reasonable limits.
We recommend careful selection of the types of spectra you request. Do not start from the principle "I want all types of 1D, 2D, VT spectra because it is possible"; if the results are unusable, time and especially resources (electricity, deuterated solvents, cryogenic fluids, etc.) are wasted. In addition, delays occur for other peers due to spectrometers being blocked for long periods of time.
In the case of beneficiaries from outside BBU, the procedure for purchasing NMR spectra recording services is done according to national legislation in the commercial field (request for offer, negotiation of service rates, conclusion of a commercial contract for the provision of services, provision of services, delivery of results, payment of services performed).
The instructions and recommendations above apply to all applicants, both within the faculty and outside it. Exceptions to point 7 are only requests based on contracts and paid orders.