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.

  • First steps and NMR guidelines for new coworkers

    New coworker of Organisch-Chemisches Institut

    1. At the beginning of your master thesis you'll get a three-digit acronym as a user-identifier from Dr. Christian Sarter.  Please, use this three-letter abbreviation when submitting samples to the analytic departments (NMR, MS and XRay).
    2. Please, read the NMR guidelines for OC coworkers carefully, before submitting your first samples.

     

    External coworkers

    1. At first you need a three-digit acronym as user-identifier. Please, send together with your groupname and with your phone number a request to  Dr. Klaus Bergander.
    2. Please, read the NMR guidelines for external coworkers carefully, before submitting your first sample!

     

    Important Hint: If you don't respect these guidelines to 100%, the sample will be returned unmeasured!

  • 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 at 400 MHz NMR spectrometer:

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

     

     

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

    Sample Submission Samples are submitted right to the entrance to the NMR laboratory.
    Sample Return Samples are returned left to the entrance to the NMR laboratory.
    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 

     

  • NMR server mora - map the network drive

    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.

     

  • Data Download with the Program "mora the explorer"

    Matt Milner (Research Group Studer) has provided us with software, which downloads your Bruker (up to 400 MHz) and your Agilent (500 & 600 MHz) NMR data directly onto your own computer. Versions are available for Windows, macOS (11.7.9 or higher) and Linux. To use it, you need only to enter your acronym, your group and a destination folder. Various options to customize the search parameters and saved filenames are available. These options can be saved as defaults. To search, the spectrometer and date are selected.

    Features:

    • Acronym (initials), group and target folder will be saved as defaults.
    • You need one folder (either local or on a server) with write access for the user account.
    • Download of data from all spectrometers including Bruker (up to 400 MHz) and Agilent (500 & 600 MHz) is possible.
    • The initials can optionally be included in the filename. For Bruker NMR data up to 400 MHz, there is also the option to include the solvent in the filename.
    • For the current day, the NMR measurements can be retrieved at regular intervals (e.g. every 5 minutes).

    Download and Installation of the Program:

    Versions of the program for different operating systems can be found at 
    \\mora\nmr\mnova\mora_the_explorer

    Instruction for installing: mora the explorer

    Acknowledgment:

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

  • Automatic Bruker 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!

  • Introduction open access NMR spectrometer

    The usage of the open access NMR spectrometer is reserved to coworkers of the Organisch-Chemisches Institut.

    Requirements for the usage:

    1. You are coworker of the Organisch-Chemischen Institut
    2. The routine NMR service was used for at least 2 weeks
    3. You have carefully read and understood the first two pages of the document  NMR-Guidelines_open-access.pdf
      (The third page will be explained during the introduction)

    Arrange an appointment for the introduction: Timon Reckmann, Tel.: 83 39773, timon.reckmann@wwu.de

     

     

  • Requirements for Supporting Information

    List of spectrometers:

    1. Agilent DD2 600
    2. Agilent DD2 500
    3. Bruker NEO 400 (all measurements at 400 MHz since June 2021)
    4. Bruker Avance II 400 (all measurements at 400 MHz before June 2021)
    5. Bruker Avance II 300 (AG Prof. Dr. A. Studer since June 2021)
    6. Bruker DPX 300 (AG Prof. Dr. A. Studer before June 2021)

     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)