Scribd Logo
Upload

Welcome to Scribd!

  • 31 views

    Χρήση Επιτραπέζιου Nmr

    Uploaded by

    parouti
    This document discusses experiences with a benchtop FT-NMR spectrometer. It describes how NMR can provide additional analytical capabilities compared to GC-MS and FT-IR for identifying unknown substances. Two examples are provided where NMR helped identify compounds where GC-MS and FT-IR results were ambiguous. The advantages of benchtop NMR are its compact size, ease of use, fast measurements, and ability to provide 1H, 13C and 19F spectra. Based on these positive experiences, the laboratory decided to purchase a 60 MHz benchtop NMR spectrometer to add to its analytical capabilities.

    Copyright:

    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd
    Flag for inappropriate content

    You might also like

    Χρήση Επιτραπέζιου Nmr

    Uploaded by

    parouti
    31 views11 pages
    This document discusses experiences with a benchtop FT-NMR spectrometer. It describes how NMR can provide additional analytical capabilities compared to GC-MS and FT-IR for identifying unknown substances. Two examples are provided where NMR helped identify compounds where GC-MS and FT-IR results were ambiguous. The advantages of benchtop NMR are its compact size, ease of use, fast measurements, and ability to provide 1H, 13C and 19F spectra. Based on these positive experiences, the laboratory decided to purchase a 60 MHz benchtop NMR spectrometer to add to its analytical capabilities.

    Original Description:

    bench-top NMR

    Copyright

    © © All Rights Reserved

    Available Formats

    PDF, TXT or read online from Scribd

    Did you find this document useful?

    Is this content inappropriate?

    Report this Document
    This document discusses experiences with a benchtop FT-NMR spectrometer. It describes how NMR can provide additional analytical capabilities compared to GC-MS and FT-IR for identifying unknown substances. Two examples are provided where NMR helped identify compounds where GC-MS and FT-IR results were ambiguous. The advantages of benchtop NMR are its compact size, ease of use, fast measurements, and ability to provide 1H, 13C and 19F spectra. Based on these positive experiences, the laboratory decided to purchase a 60 MHz benchtop NMR spectrometer to add to its analytical capabilities.

    Copyright:

    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd
    Flag for inappropriate content
    Download as pdf or txt
    31 views11 pages

    Χρήση Επιτραπέζιου Nmr

    Uploaded by

    parouti
    This document discusses experiences with a benchtop FT-NMR spectrometer. It describes how NMR can provide additional analytical capabilities compared to GC-MS and FT-IR for identifying unknown substances. Two examples are provided where NMR helped identify compounds where GC-MS and FT-IR results were ambiguous. The advantages of benchtop NMR are its compact size, ease of use, fast measurements, and ability to provide 1H, 13C and 19F spectra. Based on these positive experiences, the laboratory decided to purchase a 60 MHz benchtop NMR spectrometer to add to its analytical capabilities.

    Copyright:

    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd
    Flag for inappropriate content
    Download as pdf or txt
    of 11

    First Experiences with a

    Benchtop FT-NMR Spectrometer

    Dr. Andrea Schwarz Brüssel, 11.-12.01.2017


    Typical analytical problems
    identifying
    unknown substances

    • GC-MS or FT-IR show small variations to known substances -> Isomeres?

    • GC-MS result but no FT-IR spektrum to compare


    • FT-IR result but no mass spektrum to compare
    • GC-MS result contradictious to FT-IR result

    • time-consuming datasearch => often unsuccessful


    •
    => •
    Derivatisation
    LC-DAD
    • External analysis

    Dr. Andrea Schwarz Brüssel, 11.-12.01.2017


    NMR

    High Field NMR Benchtop NMR


    Advantages:
    - Compact, benchtop size and weight
    - No cryogens
    Additional analytical method to - No spinning or compressed gas
    GC-MS and FT-IR ? - Simple handling
    - 1H, 13C, 19F spectra
    - 1D and 2D NMR experiments

    Dr. Andrea Schwarz Brüssel, 11.-12.01.2017


    Example 1:
    N-Methylphenethylamine (NMPEA)
    GC-MS: NMPEA (Isomer amphetamine => slight differences in retention time and mass spectrum)
    FT-IR: NMPEA => not in complete accordence to libary spectrum

    60 MHz spectrum

    -NH Aromatic-H -CH2 -CH3

    Dr. Andrea Schwarz Brüssel, 11.-12.01.2017


    13C-NMR

    Dr. Andrea Schwarz Brüssel, 11.-12.01.2017


    DEPT (Distortionless Enhancement by Polarization Transfer)
    Determination of the multiplicity of carbon atom substitution with hydrogens

    Aromatic C-H

    CHx

    13C-NMR

    CH

    CH2 negativ

    Dr. Andrea Schwarz Brüssel, 11.-12.01.2017


    Two-dimensional NMR
    1H,13C-HSQC (Heteronuclear Single Quantum Coherence)

    x-Axis => 1H-chemical shift


    y-Axis => 13C-chemical shift

    Dr. Andrea Schwarz Brüssel, 11.-12.01.2017


    Example 2:
    Testosterone acetate

    Ac

    ? ?
    Testosterone acetate
    m/e: 330

    Our estimation:
    Ac Our solution: Ac

    1-Testosterone acetate Boldenone acetate


    Dihydroboldenone m/e: 328

    Dr. Andrea Schwarz Brüssel, 11.-12.01.2017


    Dr. Andrea Schwarz Brüssel, 11.-12.01.2017
    Ac

    1-Testosterone acetate
    Dihydroboldenone

    Dr. Andrea Schwarz Brüssel, 11.-12.01.2017


    Summary
    Advantages:
    - Additional method to GC-MS und FT-IR
    - Not expensive in purchasing and operating costs
    - Easy for anyone to use Our decision:
    - User-friendly software Additional analytical method
    - Fast measurements to GC-MS and FT-IR
    - 1H, 13C und 19F spectra in our Laboratory
    (only by choosing nucleous and experiment) (60 MHz spectrometer from Magritek
    - Good quality of 13C-spectra Shipment in January 2017)
    - Automate experiments with scripts
    - Two-dimensional experiments (COSY, HSQC …)
    - Samples in 5 mm-NMR-tubes

    Disadvantages:
    - Max. 60 MHz spectrometer
    - No autosampler
    - Not suitable for structure determination

    Perspective:
    - Quantification measurements are possible

    Dr. Andrea Schwarz Brüssel, 11.-12.01.2017

    You might also like