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NMR Thermometer

Variable Temperature Control Using the 2H Lock
System of AVANCE III HD Spectrometers

User Manual

Version 002

Innovation with Integrity

●

NMR

Summary of Contents for NMR

Page 1: ...NMR Thermometer Variable Temperature Control Using the 2H Lock System of AVANCE III HD Spectrometers User Manual Version 002 Innovation with Integrity NMR...

Page 2: ...ed 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 th...

Page 3: ...ction 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 6 Applications 27 6 1 Ide...

Page 4: ...Contents 4 Z33085_2_002...

Page 5: ...al 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 reaso...

Page 6: ...Introduction 6 Z33085_2_002...

Page 7: ...X 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...

Page 8: ...Principle of NMR Thermometer 8 Z33085_2_002...

Page 9: ...002 9 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 Version...

Page 10: ...Requirements 10 Z33085_2_002...

Page 11: ...VT control with the sensor and the NMR Thermometer Calibration of the spectrometer for measurements of real samples after the setup of the NMR Thermometer is finished The edlock Menu First we will pr...

Page 12: ...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 By executing...

Page 13: ...e shift value has already been defined Setting up the NMR System for the NMR Thermometer Since the NMR Thermometer is observing a 2 H signal the system has to be properly set up lock shimming optimal...

Page 14: ...ase is selected in the edlock window Lock Level Default Spectrum and Enhanced Lock Level in the figure below Figure 4 6 Selection of the Auto Phase Algorithm To prevent saturation the Lockpower and lo...

Page 15: ...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 val...

Page 16: ...tune in Progess Edte disable NMR Thermometer if not already done Change target temperature edte for instance a 10K temperature jump As an exercise we will perform a temperature jump e g 10K and follow...

Page 17: ...h internal RF heating e g TOCSY After setting up the system lock shim and enabling the NMR Thermometer edte the sample temperature is used for temperature regulation which is visible on the status bar...

Page 18: ...figure below lower part and hence the sensor temperature figure below upper part white line Figure 4 12 Monitoring of the sensor and the sample temperature in edte during a TOCSY experiment In the fig...

Page 19: ...new solvent in the edlock table Select a solvent which is similar to your mixture similar lock parameters and click the right mouse button In the resulting pull down menu you can add the new solvent F...

Page 20: ...value files The xml file figure below contains the name of the solvent identical with the solvent name and two shift values one for the field shift and one for the temperature shift The values have t...

Page 21: ...ock the deuterium signal of the hydroxyl group is used for the NMR Thermometer The deuterium chemical shifts of commonly used organic NMR solvents like CDCl3 acetone d6 and DMSO d6 are virtually indep...

Page 22: ...structural properties of the sample Acceptance Difference compounds are commonly added to protein solutions These can be buffers like TRIS or stabilizers like EDTA These compounds can be used if deute...

Page 23: ...her the concentration of the compound used for the NMR Thermometer should be As a rule of thumb reducing the distance of the two lock signals by a factor of 2 increases the necessary concentration dec...

Page 24: ...im nucleus For aqueous solutions e g 5 D2O in H2O 1 H is the shim nucleus therefore the shim routine for Topshim does not need to be changed For deuterated organic solvents 2 H is used as the shim nuc...

Page 25: ...on to modify the shim parameters 3 A new window will open and allow the selection of the shim nucleus Enter 2 for 2 H as the shim nucleus 4 Now the frequency of the signal has to be defined As default...

Page 26: ...nucleus is used to define the repetition time for the shim procedure Typical values for the T1 relaxation time are about 1 sec for D2O 3 sec for C6D6 and 5 sec for acetone d6 8 In a final step the op...

Page 27: ...p the system tuning matching shimming the sample temperature is displayed immediately After enabling the NMR Thermometer the sample temperature can be used as target temperature edte If the temperatur...

Page 28: ...F 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 biomolecu...

Page 29: ...Right part NMR Thermometer enabled regulation mode An interesting application of the NMR Thermometer is high resolution MAS on biological material Depending on the spinning speed used in HR MAS 1 to...

Page 30: ...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 spectr...

Page 31: ...nce in Hz at a lower field In that case a different thermometer compound has to be used The lock procedure worked well for field and frequency lock but the temperature regulation of the NMR Thermomete...

Page 32: ...Frequently Asked Questions FAQ 32 Z33085_2_002...

Page 33: ...NMR service centers 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 so...

Page 34: ...Contact 34 Z33085_2_002...

Page 35: ...re shift values filled in 21 Figure 5 6 Suggested compounds for the NMR Thermometer and samples in aqueous solution D2O 5 100 their properties and estimated concentration Fully deuterated DSS and TSP...

Page 36: ...List of Figures 36 Z33085_2_002...

Page 37: ...0 edsolv 11 exercise 16 I import shift and temperature values 20 L Lock parameters 12 lock phase 14 LTRX 7 M Monitoring 16 N New solvent 19 NMR Thermometer compounds 21 O Overview 11 P PID values 14 P...

Page 38: ...Index 38 Z33085_2_002...

Page 39: ...Z33085_2_002 39...

Page 40: ...Bruker Corporation info bruker com www bruker com Order No Z33085...

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