If this is your first time handing in a sample, use the Quick Guide here.
The recording of the individual routine NMR spectra takes place without the direct involvement of the NM spectroscopists in the department and is a service that the NMR laboratory provides for the individual permanent scientific staff at the Department of Physics, Chemistry and Pharmacy.
As a result, the rights to results obtained from such routine spectra belong to the permanent scientific staff in question. Unless there is a special agreement, routine NMR spectra can only be obtained in connection with research activities that take place at the Department of Physics, Chemistry and Pharmacy.
Involvement of the NMR spectroscopists at the laboratory in recording or interpretation of NMR spectra can be obtained by special agreement. In such cases, it will be a project collaboration. Results obtained in such a collaboration cannot be published without the consent or co-authorship of the NMR spectroscopist involved.
A project collaboration could be NMR recorded at a lower temperature or at a higher field, for example 500 MHz.
Recording of spectra
Routine NMR spectra are obtained by submitting a sample to the NMR laboratory, in the cabinet marked NMR-Service. Alongside submitting the sample, a requisition form must be filled out and sent electronically to the NMR laboratory.
The substance from which an NMR spectrum is to be recorded must be dissolved in 600 µl of a suitable NMR solvent and placed in a 5 mm NMR tube. It is important for the acquisition of spectra that the sample volume is 600 µl /~ 4.4 cm, neither more nor less.
It is crucial for obtaining satisfactory NMR spectra that the sample preparation has been carried out carefully. In particular, you have to think about having a sufficiently high concentration of your substance and make sure there is no sediment in the sample. You cannot obtain good NMR spectra from bad samples!
At least twice a day, all submitted NMR samples will be placed in the auto-sampler of the 400 MHz NMR spectrometer. Routine spectra are recorded within 24 hours after the samples have been submitted. Urgent samples can be taken more quickly by special agreement with the NMR laboratory technicians. The auto-sampler can only take NMR tubes which have the original length of 17.6 cm. If your tube is broken at the top, throw it away. A pipe that is too short blocks the entire queue.
All samples submitted without special instructions will be recorded with standard parameters, see the table further down. For temporal reasons, an upper limit on how long accumulation takes place during the recording of the 13-C NMR spectrum has been placed. A too "thin" sample therefore typically provides a poor 13-C NMR spectrum. A separate assessment of whether the spectrum is good enough will not be made before recording is interrupted and the sample is "shot".
When the sample has been recorded, they are automatically sent to our server S:\DATA\NMR\Spectre\mmm_ÅÅ\data\service\nmr, for further processing. mmm and åå marks the month and the year in which the spectrum was recorded, respectively.
Please note that files are saved on the server before the recording is completely finished. Use the web interface to see if your sample has been recorded.
Naming of the spectra
The folder containing the spectra is named as follows:
[NMR-initials][mmddaa][E][substance name] where:
NMR initials are the user's SDU username, (text before @ in e-mail)
mm is the month,
dd is the day
åå is the year
E is the experiment,
substance name is the name of the sample. (max 5 characters and no special characters *-()# etc.)
|
Eksperiment |
E |
Standardscan |
File i Mestre |
Frequency (MHz) |
|
Proton |
h |
8 |
fid |
400,12 |
|
Carbon |
c |
256 |
fid |
100,62 |
|
Phosphor |
p |
64 |
fid |
161,97 |
|
Flour |
f |
16 |
fid |
376,49 |
|
DEPT |
d |
256 |
fid |
100,62 |
|
COSY |
cosy |
1 |
ser |
|
|
HMBC |
hmbc |
8 |
ser |
|
|
HSQC |
hsqc |
2 |
ser |
Example: If the Requester is pku and the name of the substance is 001, then a proton spectrum is called: pku112108h001
Everyone who needs to be enrolled in NMR must use the SDU username they have been assigned.
It is the individual user's own task to post-process and print the spectrum using the program Mestre Nova. You can get access to - and instructions for - the program by contacting the NMR laboratory.
Remember to pick up your sample when your spectrum has been uploaded to the department server.
Deuterated solvents and NMR tubes are available on request.