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Bruker NMR User Manual

Bruker NMR User Manual

Variable temperature control using the 2h lock system of avance iii hd spectrometers
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NMR Thermometer
Variable Temperature Control Using the 2H Lock
●
System of AVANCE III HD Spectrometers
User Manual
Version 002
NMR
Innovation with Integrity

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  • Page 1 NMR Thermometer Variable Temperature Control Using the 2H Lock ● System of AVANCE III HD Spectrometers User Manual Version 002 Innovation with Integrity...
  • Page 2 Application & Electronics Departments © July 11, 2014 Bruker Corporation P/N: Z33085 DWG: Z4D12031 For further technical assistance for this product, please do not hesitate to contact your nearest BRUKER dealer or contact us directly at: Bruker Corporation Industriestrasse 26 8117 Fällanden Switzerland...

  • Page 3: Table Of Contents

    Contents Introduction............................5 Principle of NMR Thermometer ......................7 Requirements............................9 Getting Started..........................11 The edlock Menu....................... 11 Setting up the NMR System for the NMR Thermometer ........... 13 Examples........................... 15 4.3.1 Monitoring Mode........................ 16 4.3.2 Regulation Mode ....................... 17 Advanced Operation ........................
  • Page 4 Contents Z33085_2_002...

  • Page 5: Introduction

    This manual is planned as a user manual with limited technical detail. The main focus is on usability, whereas a few easy examples are provided showing how to get started with this new tool. Through use of this manual the user should get an idea for what the NMR Thermometer™ might be used for.
  • Page 6 Introduction Z33085_2_002...

  • Page 7: Principle Of Nmr Thermometer

    H signals using the lock channel (LTRX board) of the NMR system. The distance between the two signals is transferred into a temperature and directly used by the temperature control unit (BVT) for regulation. Thus, the NMR Thermometer acts as a temperature sensor (see figure below).
  • Page 8 Principle of NMR Thermometer Z33085_2_002...

  • Page 9: Requirements

    Requirements Requirements Hardware: Avance III HD. A hardware upgrade is required for Avance III, whereas an update to SmartVT™ and Digilock 2G is required. Software: TopSpin version 3.2 or higher. Firmware: Versions for Avance III HD. Z33085_2_002...
  • Page 10 Requirements Z33085_2_002...

  • Page 11: Getting Started

    Getting Started This chapter provides a short and straightforward introduction on how the NMR Thermometer works and guides you through the first steps using the NMR Thermometer. As an overview, the steps include: • Preparation of the edlock table if not yet done.

  • Page 12: Figure 4.2 Edit Solvent Parameters

    Getting Started Figure 4.2: Edit Solvent Parameters. In the submenu Lock window the solvents are listed, along with the probe for which the definition is valid (generic or specific probe), as well as other lock parameters (lock power, lock regulation triplet etc.). Figure 4.3: The Submenu Lock.

  • Page 13: Setting Up The Nmr System For The Nmr Thermometer

    It is possible to define all the signals for solvents with more than one H signal either as Signal, as Lock (signal used for field lock) or as Temperature (signal used for the NMR Thermometer). For any NMR Thermometer substance, temperature and shift values can be added or imported (see below).

  • Page 14: Figure 4.5 Edte Window: Nmr Thermometer Monitoring Mode (Disabled, Top), Regulation Mode

    Getting Started Figure 4.5: Edte Window: NMR Thermometer monitoring mode (disabled, top), regulation mode (enabled, middle) and the selection of both modes in the Configuration menu of the edte window (bottom). Another important parameter is the lockphase, which can be optimized automatically by starting autophase (BSMS display).

  • Page 15: Examples

    An easy example to begin with is to use the methanol sample (standard sample: 99.8% deuterated). Since this sample is the reference for the NMR Thermometer, the solvent entry in edlock containing the temperature and shift values is already predefined.

  • Page 16: Monitoring Mode

    As an exercise we will perform a temperature jump (e.g. 10K) and follow the different temperature and other BSMS values (flow/heater) in the monitoring window (edte - Monitoring, as well as, activate NMR Sensor Temperature, NMR Thermometer, Target Temperature, Current Power etc.).

  • Page 17: Regulation Mode

    Figure 4.11: TopSpin status bar with NMR Thermometer enabled. To test the performance of the NMR Thermometer start a TOCSY experiment and follow the temperature values (sensor, NMR Thermometer) in the monitoring window of the VTU display (edte).

  • Page 18: Figure 4.12 Monitoring Of The Sensor And The Sample Temperature In Edte During A Tocsy Experiment

    Figure 4.12: Monitoring of the sensor and the sample temperature in edte during a TOCSY experiment In the figure above, the upper part shows the temperature of the sensor and the NMR Thermometers; the lower part shows the heater power.

  • Page 19: Advanced Operation

    Advanced Operation Define a New Solvent To work with your own NMR Thermometer substances, you first have to define a new solvent in the edlock table. Select a solvent which is similar to your mixture (similar lock parameters) and click the right mouse button.

  • Page 20: Figure 5.2 Assign Signals To Type Of Signal (Signal, Lock, Temperature)

    Advanced Operation Figure 5.2: Assign Signals to Type of Signal (Signal, Lock, Temperature). In the next step you should import the shift-temperature values (.csv or .xml format) or fill in the values manually. You can also create your own .xml (see below). Figure 5.3: Dialog for importing temperature shift value files.

  • Page 21: Selection Of Nmr Thermometer Compounds

    The simplest compound for the NMR Thermometer is fully deuterated methanol used as a NMR solvent. While the deuterium signal of the methyl group is used for the field lock, the deuterium signal of the hydroxyl group is used for the NMR Thermometer. The deuterium...

  • Page 22: Predefined Solvents For The Nmr Thermometer

    • Price and availability. 5.2.1 Predefined Solvents for the NMR Thermometer The lock table contains solvents which are setup for usage with the NMR Thermometer. For these solvents a temperature calibration of the chemical shift difference of the two H signals has been performed and is included.

  • Page 23: Technical Considerations

    NMR Thermometer compound by the same factor. Examples: • The D of the NMR Thermometer signal to the field lock signals is about 3 ppm. The required signal to noise ratio of the NMR Thermometer compound has to be at least 200:1 (I-ratio <500:1).

  • Page 24: Considerations For Shimming With Topshim

    H sensitivity of a room temperature probe, such as an inverse or broad band observe probe, is about a factor 5-10 times lower compared to a cryogenically cooled probe. The concentration of the NMR Thermometer compound therefore needs to be higher, as listed in the following table: Figure 5.8: Typical concentrations required for the NMR Thermometer compound.
  • Page 25 Advanced Operation 2. Select the solvent of your choice and press the select file button. A new window will open, select the OK button to modify the shim parameters: 3. A new window will open and allow the selection of the shim nucleus. Enter 2 for H as the shim nucleus: 4.
  • Page 26 Advanced Operation 6. The definition of the selectivity for selective excitation is entered next. This depends on the difference of the chemical shift of the field lock solvent to the next closest signal of the thermometer compound. As an example, a selectivity of 0.5 ppm is sufficient for chemical shift difference of 1ppm.

  • Page 27: Applications

    Applications Identical Chemical Shifts at Different Spectrometers One of the most important applications of the NMR Thermometer is to use it as internal temperature reference and correct the temperature offset between sample and the temperature sensor of the probe. This is in general comparable to the conventional...

  • Page 28: Identical Chemical Shifts For Experiments With Different Heating Due To Experimental Conditions (Temperature Compensation)

    RF heating inside the sample is caused by, for instance, a spinlock sequence as used in TOCSY-type of pulse sequences, or decoupling as well as CPMG sequences. Such experiments are widely used in biomolecular NMR. As an example we show a 0.5 mM N-labeled ubiquitin in H...

  • Page 29: Heating Caused By Spinning Speed (Hr-Mas)

    Figure 6.3: Overlay of NOESY-HSQC (blue), TOCSY-HSQC (orange) and CPMG-HSQC (green) spectra of 0.5mM ubiquitin in 95:5% H2O/D2O measured at 800MHz TCI CP. In the figure above the left side shows the NMR Thermometer disabled (monitoring mode) and the right side the NMR Thermometer enabled (regulation mode).

  • Page 30: Figure 6.5 Comparison Of Tocsy Experiments Of A Liver Sample With Sodium Acetate Added Measured With Hr-Mas At 4 Khz Spinning Speed

    In the figure above is a comparison of TOCSY experiments of a liver sample with sodium acetate added measured with HR-MAS at 4 kHz spinning speed. The reference 1H spectrum is plotted as projection. Left part: NMR Thermometer disabled (monitoring mode); Right part: NMR Thermometer enabled (regulation mode).

  • Page 31: Frequently Asked Questions (Faq)

    4. The chemical shift of the compound used for the NMR Thermometer is too closed to the chemical shift of the solvent. Here it can happen that the lock procedure for both, the field and the frequency lock, is working fine on a 700 MHz spectrometer, while it fails on a lower field spectrometer due to the reduced shift difference (in Hz) at a lower field.
  • Page 32 Frequently Asked Questions (FAQ) Z33085_2_002...

  • Page 33: Contact

    Bruker BioSpin NMR provide dedicated hotlines and service centers, so that our specialists can respond as quickly as possible to all your service requests, applications questions, software or technical needs. Please select the NMR service center or hotline you wish to contact from our list available at: http://www.bruker.com/service/information-communication/helpdesk.html Z33085_2_002...
  • Page 34 Contact Z33085_2_002...

  • Page 35: List Of Figures

    Suggested compounds for the NMR Thermometer and samples in aqueous solution (D2O 5 – 100%), their properties and estimated concentration. Fully deuterated DSS and TSP are currently not available but will be synthesized on Bruker’s request at small amounts only for internal tests................
  • Page 36 List of Figures Z33085_2_002...

  • Page 37: Index

    ............... 11 exercise ............16 VT control ............11 import shift and temperature values ....20 xml files............. 20 Lock parameters..........12 lock phase ............14 LTRX ..............7 Monitoring............16 New solvent ............19 NMR Thermometer compounds ....... 21 Z33085_2_002...
  • Page 38 Index Z33085_2_002...
  • Page 39 Z33085_2_002...
  • Page 40 ● Bruker Corporation info@bruker.com www.bruker.com Order No: Z33085...

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