Tips & Tricks around temperature

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1 Tips & Tricks around temperature 40. NMR Benutzertagung 2016 Karlsruhe Frank Schumann Bruker BioSpin AG, Schweiz Innovation with Integrity

2 Temperature in NMR NMR experiments are sensitive to small changes (of less than 10mK) even small deviations of the sample temperature have an impact on the quality of the NMR spectra (line broadening and shifting of the NMR lines) Precise, stable and reliable regulation required Stability of the experiment temperature subject of different influences Change of the ambient temperature Sample heating cause by RF pulses (heating of the coils) Convection flow inside the sample (10mm samples) Evaporation and condensation of the sample liquid

3 Temperature Regulation Temperatur sensor not inside the sample offset of the sample temperature (CryoProbe around 2K for RT range) CryoProbes: Direct flow Higher VT gas flow required compared to RT Excellent thermal insulation

4 CryoProbes: Temperature range 2 different temperature ranges for CryoProbes: Probe Type Target Temperature Standard -40 C + 80 C Elevated Temperature (ET) Probe Type 0 C C Target Temperature Requested Flow [l/h] 1.7mm 0 C + 80 C 400 5mm -40 C + 80 C 0 C C mm 0 C C

5 Spinners Standard (-40 C +80 C) Elevated (0 C +135 C) POM: 0-80 C KEL-F: C Ceramic: down to -80 C up to 135 C

6 SmartVT: Immunity to external VT gas and temperature variations Sensor/pneumatics and heater units Gas flow, pressure, etc. measured and regulated Probe interfaces Excellent digital temperature sensor electronics Plug & Play intelligent probe interfacing Dual sensor probes support (MAS)

7 SmartVT: Intelligent VT gas flow management Ultra stable VT electronics Temperature sensor within +/-15mK 5 4 bar 4 3 bar 3 2 bar 2 1 bar

8 SmartVT: Bruker self tune Features Small overshoot (~1-2K, Bio samples) Automatic heater power evaluation

9 SmartCooler: 2nd Generation NMR cooler (BCU I/II) Cooler technology Better probe interface Different cooling power modes TopSpin 3.0 integrated operation Benefits Best cooling with new Probes Lower NMR sample temperatures Good to know Compatible with all VTU and probes Maintenance free

10 SmartCooler (BCU): New cooler technology Johnston type plug No icing No leakage Adapters available for other probes Operational Modes Remote BCU controlled by the TopSpin 3.0 Flush/0 Purge BCU and probe No cooling power 1 Min. cooling power (RT temperatures) 2 Max. cooling power (Low temperatures)

11 SmartCooler and SmartVT: Improved sample temperature stability x64 SmartVT SmartCooler More than 2x better 100mM Sucrose / 5mm TCI700 spin-echo difference (HMQC without gradients, non-decoupled, refocused)

12 Different operation modes Operation at room temperature (common operation mode in NMR) BCU I (1, 2) Operation at temperatures below room temperature (max. -40 C) BCU II mode (1, 2, 3) Operation at elevated temperatures BCU I («Flush») Working at low and elevated temperatures: Temperature offset higher compared to room temperature Regulation Mode: slope limited; max. 5 K per min Watch shim coil temperature during operation (less critical)

13 Sample temperature stabilization

14 Offset of the sample temperature: Temperature correction Compounds with exchangeable protons (methanol, glycol) Distance of two signals in 1Hspectrum is temperature dependent TOPSPIN: calctemp D : measure distance and calculate real temperature automatically CryoProbes: 99.8%D methanol Methanol OH D CH ppm Findeisen & Berger, Magn. Reson. Chem., 2007, 45,

15 VTU display (edte)

16 Save and enable temperature correction

17 Temperature Artefakt in NMR TOCSY (sucrose sample) Not enough dummy scans

18 Problem TOCSY and NOESY (sucrose sample)

19 Solution NMR Thermometer TOCSY (sucrose sample) TOCSY and NOESY

20 NMR Thermometer Maintaining the sample temperature Standard NMR Thermometer time experiment start ppm ppm Spectra of 10 mm raffinose in D 2 O with ~50 mm NaAc-d3 H 2 O: ~ 0.01ppm / = 6Hz / K

21 NMR Thermometer - Introduced in 2012 Hardware and software DigiLock TM SmartVT TopSpin3.2 AVANCE III HD

22 NMR Thermometer Temperature measurement inside Probe sensor (outside) Inside the sample Add thermometer substance (temperature sensitive) Temperature sensor T T

23 How does the NMR Thermometer work?

24 How to choose the right substance? Compounds (typical concentrations mm) C 4 D 9 OD 1.2 ppm edlock: T_* - solvents

25 NMR Thermometer TM for bio-nmr deuterated micelles

26 NMR Thermometer TM for bio-nmr deuterated micelles Sample heating due to CC-spinlock monitored temperatures: target = green sample internal = yellow HCCH-TOCSY experiment 50ms spinlock duration recycle delay = 1 sec sample: protein in DHPC, acqueous solution

27 Limits of the NMR thermometer - substance (concentration) requirements Shift difference D between field and frequency lock Signal ratio field and frequency lock signal Intensity ratio D

28 Limits S/N (2H): about 200:1 to obtain reliably lock-in performance compare S/N(2H) 1% D 2 O on TCI-CP600 > 1000:1 (0.2% considered to be the lower limit) Depending on the shift difference and the signal intensity ratio of the lock signals Rule of thumb: Shift difference 3ppm -> ~1.5ppm -> approx. 2x concentration of the NMR thermometer substance necessary

29 NMR Thermometer - features

30 Application fields Main applications: NMR experiments with heating (RF, rotation) Keep temperature, small temperature range, absolute temperature not that important Other applications: Same temperature between different systems Bigger temperature range, absolute (exact relative) temperature Measurements of temperature dependent parameters (kinetics, thermodynamics) exact (absolute) temperature

31 NOESY-HSQC, TOCSY-HSQC, CPMG-HSQC TCI CryoProbe 800MHz OFF NMR thermometer ON 0.5mM 13 C/ 15 N labeled ubiquitin/ 50mM Naac-d3 in H 2 O/D 2 O 95/5%

32 HR-MAS on biological samples

33 Same temperature at different systems Easy temperature referencing

34 Temperature Correction Flow change 550 to 500l/h MeOD (99.8%), pseudo 2D time NMR Thermometer off NMR Thermometer on

35 Long time temperature stability NMR thermometer temperature [K] OFF ON mK 0.9mK 50mM Naac in H2O/D2O 95/5% at 600MHz AVIIIHD TCI-CP time [h] time [h] T-stab.: 4 Probe Sensor NMR Therm.

36 Automation

37 Flowbar available in TS3.5 (since pl4) The flowbar uses the AU- program nmr_therm

38 Flowbar: Show regulation parameters

39 Flowbar: Operation modes

40 Flowbar: Tools Automatic temperature correction

41 NMR Thermometer manual included

42 New function Keep temperature Create T_ solvent (2 signals) Lock on that solvent

43 New function Keep temperature Execute AU-program keep_temp -> Creation of temperature-shift table (.xml) in background lock - NMR-T. in regulation mode (automatically)

44 Intermediate.xml in dataset

45 New workflow Keep temperature function Start experiment

46 Conclusion - Outlook CryoProbes (5mm) come in two temperature ranges (-40 to 80 C and 0 to 135 C) Well proven chillers (SmartCooler: BCU I/ II) and temperature regulation (SmartVT) available for highest temperature performance Since TopSpin 3.5pl4 the NMR-T. flowbar is part of the TS release (including the nmr_therm AU program) Easier access to the NMR-T. via the Keep temperature function (TS3.5pl6) for the majority of applications (heating experiments) More to come

47 Thanks to Wolfgang Bermel, Daniel Mathieu, Clemens Anklin, Helena Kovacs Rolf Hensel Marina Maurer, Werner Mausshardt, Eberhard Schweizer, Christof Johann, Peter-René Steiner

48 Copyright 2011 Bruker Corporation. All rights reserved. Innovation with Integrity

49 NMR thermometer using Naac (S/N-performance) Monitoring Experiment (SL, CPD) 400MHz BBFO 600MHz BBFO 600MHz TXI 600MHz QCI 850MHz TCI <1mK 1-3mK >200mM mM 50mM 1-2mK 3-6mK mM 2-4mK 6-12mK mM <200mM 100mM 20mM <20mM <100mM 50mM 10mM <10mM 4-8mK 12-30mK mM <50mM 20mM >8mK >30mK <50mM

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