NMR Service

© Dr. Klaus Bergander

The NMR laboratory of the Organic Chemistry provides with this  equipment a comprehensive NMR service for all the scientists at WWU Münster. All necessary information for preparing and submitting your sample is detailed below. All NMR data will be saved on the NMR server mora and software is available for processing and analyzing NMR spectra.

  • Sample Preparation and Forms

    NMR tube

    NMR tube Info consumable material NMR.pdf
    Diameter 5 mm
    Length 18-20,5 cm  (7 bis 8 inch), no tubes longer than 21,5 cm!
    Filling height 5 cm
    Solvent deuterated, e.g. CDCl3
    Amount for 1H 30-50 mg (at least 10 mg)
    Amount for 13C ~ 100 mg (at least 50 mg)
    Consistency clear homogeneous solution, without precipitate
    The sample tube has to be absolutely clean on the outer surface!
    Don't use broken NMR tubes or old and leaky caps!

    Sample labelling

    The sample label is composed by 3 parts: Acronym (3 letters, for members of Organic Chemistry this is assigned by Dr. Christian Sarter upon commencing work in the institute), the number of your reaction (max. 4 digits) and an additional number to differentiate, for example, several fractions of chromatography. This labelling should be used in all analytic groups in the Institute of Organic Chemistry. External coworkers will receive an acronym on request (klaube@wwu.de).

    example: mue591-1

    • mue: acronym for Mr. Mueller
    • 591  : reaction number (only digits, no letters!)
    • -1: increasing number, starting with 1:  -1, -2, -3, -4, ...      (e.g. for screening, chromatography, titration, ...)

    Preparation of sealed NMR tubes: "Freeze, Pump and Thaw method":

    For preparing sealed NMR tubes the following instruction is obligatory:

  • Sample Submission and Choice of Spectrometer

    1D NMR am AV300 und AV400 :

    Location Samples are submitted at the entrance to the NMR laboratory.
    Measurements 1H, 13C, DEPT
    19F, 7Li, 11B, 29Si, 31P, ...
    Amount 30-100 mg
    Contact Karin Voß, Tel.: 83 39773, bussek@wwu.de
    Ingo Gutowski, Tel.: 83 36509, gutowski@wwu.de

    1D- and 2D NMR at the highfield NMR spectrometer at 400 to 600 MHz

    Location Samples are submitted inside NMR laboratory, to the right as you enter.
    Measurements 1H, 13C, X-Kerne (direct and indirect detection)
    gCOSY, gHSQC, gHMBC, NOESY
    Selective NOE, ROE and TOCSY experiments
    19F-NMR: 1H{19F}, 13C{1H,19F}, 19{1H}, 1H,19F-HOESY
    NMR measurements at low sample concentration
    Multi- and bandselective decoupling
    Homo and heteronuclear decoupling
    DOSY
    X nuclei measurements
    Measurements at variable temperature
    Further special measurements on request
    Contact 500-600 MHz: Dr. Klaus Bergander, Tel.: 83 39776, klaube@wwu.de 
    400 MHz: Karin Voß, Tel.: 83 39773, bussek@wwu.de

  • Downlowd of NMR Data

    You can download your nmr data from the mora server. The server is protected by a firewall and can only be accessed from within the WWU network, or with an established VPN connection. 

    Connection to mora inside of the WWU network:

    Windows

    a) Command line:  \\mora\nmr     or

    b) File explorer ⇒ Computer ⇒ map 

    • drive:  Z
    • folder:  \\mora\nmr
    • connect as:  NWZ \ < your account >

    MAC

    c) open finder ⇒ cmd-key K ⇒ smb://nwz; < your account >@mora.uni-muenster.de/nmr

    Connection to mora outside of the WWU network:

    First, you have to establish a VPN to the WWU network, then connect as described above. The ZIV provides a manual, how you can connect to vpn.uni-muenster.de with the anyconnect client.

    What can you do, if you don't get an access?

    Please write an Email with the following information to Dr. Klaus Bergander: (klaube@wwu.de)

    • Benutzergruppe of your Arbeitskreisleiters (Please, check your membership in this group!) and
    • The IP adress range of your WWU computer, from which you want to access the server mora.

  • Automatic Data Download with the Program NMR-Check

    Patrik Unsleber (AG Neugebauer) has provided us with software, which downloads your Bruker NMR data directly onto your own computer, immediately after the measurement has been completed. To use it, you need only to enter your acronym and a destination folder. 

    Please, bear in mind:

    • Don't change the usertag (your acronym), when you've started the program once.
    • Each user can install his "own" version of the program (with your acronym and your destination folder) into a local folder and launch it from there.
    • Thus several users can save simultaneously their data on one computer into a local folder with write access.
    • Precondition for the simultaneously appliance: You need one folder (either local or on a server) with write access for all users (e.g. the group disk).

    Download und Installation des Programms:

    You'll find the program on  \\mora\nmr\mnova

    Instruction for installation of NMR-Check

    Acknowlegment:

    Patrik, thanks a lot for this very nice and helpful tool!

  • Requirements for Supporting Information

    List of spectrometers:

    1. Agilent DD2 600
    2. Agilent DD2 500
    3. Bruker Avance II 400
    4. Bruker Avance II 300
    5. Bruker DPX 300 (group of Prof. Dr. A. Studer)

     Determination of the spectrometer frequency (e.g. 19F):

    • Load the corresponding NMR file (e.g. 19F) in MNova
    • Upper menu bar: View ⇒ Tables ⇒ Parameters 
    • You'll find the parameter spectrometer frequency  in the table

    IUPAC referencing

    • All in the NMR department measured spectra are referenced according to the IUPAC recommendation of 2001:
    1. Firstly, the spectrometer tries to reference the TMS signal in 1H NMR to 0 ppm. If no TMS was added, the spectrometer uses the residual solvent signal for indirect referencing.
    2. The referencing of all other spectra of the same sample, which were measured on the same day and spectrometer (same lock frequency), will then be calculated by the unified scale, according to the proton resonance of TMS as primary reference.
    • Normally, you have to redo the referencing, due to an inacurate spectrometer referencing of the proton NMR spectrum (step 1).
      (see IUPAC-Referenzierung in MNova - Quick Access).
    • Basically, you can use this note in supporting information:
      1H NMR chemical shifts are given relative to TMS and are referenced to the solvent signal. Spectra of other nuclides like 13C, 19F, 11B, 31P, ... are referenced according to the proton resonance of TMS as the primary reference for the unified chemical shift scale (IUPAC recommendation 2001).
      [R. K. Harris, E. D. Becker, S. M. Cabral De Menezes, R. Goodfellow, P. Granger, Pure Appl. Chem. 2001, 73, 1795-1818]
    • If you use another referencing method, you've to mention it accordingly (e.g. CFCl3 as internal standard in 19F NMR spectra)