Bruker NMR Manuale utente
NMR Thermometer
Variable Temperature Control Using the 2H Lock
System of AVANCE III HD Spectrometers
User Manual
Version 002
Innovation with Integrity
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NMR
Copyright © by Bruker Corporation
All rights reserved. No part of this publication may be reproduced, stored in a retrieval
system, or transmitted, in any form, or by any means without the prior consent of the
publisher. Product names used are trademarks or registered trademarks of their
respective holders.
This manual was written by
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
Phone: + 41 44 825 91 11
FAX:+ 41 44 825 9696
E-mail: [email protected]
Internet: www.bruker.com
Contents
Z33085_2_002 3
Contents
1Introduction......................................................................................................................................... 5
2Principle of NMR Thermometer......................................................................................................... 7
3Requirements...................................................................................................................................... 9
4Getting Started.................................................................................................................................. 11
4.1 The edlock Menu............................................................................................................... 11
4.2 Setting up the NMR System for the NMR Thermometer ................................................... 13
4.3 Examples........................................................................................................................... 15
4.3.1 Monitoring Mode................................................................................................................ 16
4.3.2 Regulation Mode ............................................................................................................... 17
5Advanced Operation ........................................................................................................................ 19
5.1 Define a New Solvent........................................................................................................ 19
5.2 Selection of NMR Thermometer Compounds ................................................................... 21
5.2.1 Predefined Solvents for the NMR Thermometer ............................................................... 22
5.2.2 Technical Considerations .................................................................................................. 23
5.2.3 Considerations for Shimming with Topshim ...................................................................... 24
6Applications ...................................................................................................................................... 27
6.1 Identical Chemical Shifts at Different Spectrometers ........................................................ 27
6.2 Identical Chemical Shifts for Experiments with Different Heating due to Experimental
Conditions (Temperature Compensation) ......................................................................... 28
6.2.1 RF Heating ........................................................................................................................ 28
6.2.2 Heating caused by Spinning Speed (HR-MAS)................................................................. 29
7Frequently Asked Questions (FAQ)................................................................................................ 31
8Contact .............................................................................................................................................. 33
List of Figures................................................................................................................................... 35
Index .................................................................................................................................................. 37
Contents
4Z33085_2_002
Introduction
Z33085_2_002 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.
The comparability of data (chemical shifts) and results derived from NMR data (diffusion data,
relaxation measurements), as well as the quality of the NMR spectra, depend on an accurate
and precise temperature measurement. That is the reason why the temperature
measurement should ideally take place inside the NMR tube and not outside of it. In general
the temperature sensor of the probe is not reflecting the real situation inside the NMR tube.
The NMR Thermometer not only monitors the temperature, but also compensates for
different heating effects (e.g. RF heating) that occur during an NMR experiment.
1
Introduction
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Principle of NMR Thermometer
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Principle of NMR Thermometer
The NMR Thermometer measures the temperature inside the sample by observing the
chemical shifts of two 2H 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).
To obtain the second lock signal, a thermometer substance needs to be added. One of the
signals should also be temperature dependent.
Figure 2.1: Principle of the NMR Thermometer.
2
Principle of NMR Thermometer
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Requirements
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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.
3
Requirements
10 Z33085_2_002
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