TopSolids Where Expertise meets Convenience

Transcription

1 TopSolids Where Expertise meets Convenience Dr. Sebastian Wegner Bruker BioSpin, France 30 ème Réunion Utilisateurs Novembre 2016 Innovation with Integrity

2 12/9/ With TopSolids the delicate setup of solid state NMR experiments is made easy by reliable automated procedures whatever your background and experience may be 2 nd generation finally available with TopSpin free of charge compatible with 4 mm and 3.2 mm double and triple channel SB/ WB probes (more to come)

3 12/9/ TopSolids 2.0 News & Updates different modules in flow bar design: New Preparation (incl. advanced user interface to fetch general information in one step, import of former data possible) Probe Setup (not only for general setup, but for e.g. testing a probe after repair, etc.) Bio (incl. setup and optimization, up to 4D 13 C-detected experiments) New Materials (1D/ 2D X, HX CP and MQMAS experiments) modules use an optimum of automation minimized user interactions

4 12/9/ Launching TopSolids execute expinstall for Solid State Systems once open any data set open the Acquire tab in TopSpin (1) pull down the menu item More (2) select TopSolids (3)

5 12/9/ Preparation Module leads back to the Acquire tab the Preparation module opens automatically all flow bars comprise the navigation buttons and an information field to identify the currently used TopSolids module

6 12/9/ Preparation Module New start new user interface if unknown: select the currently installed probe open the new user interface and create your project

7 12/9/ New User Interface for Project Handling simplified creation of a new project TopSolids organizes the data set handling automatically

8 12/9/ New User Interface for Project Handling General Information 1 2 mandatory: fill in directory and sample names select the TopSolids module you want to launch 3

9 12/9/ New User Interface for Project Handling General Information recommended, but not mandatory: load a shim file 4

10 12/9/ New User Interface for Project Handling General Information this might take some seconds 4 5 creates the new directory within the active data path creates a parameter data bank for the new project within this directory loads the respective first data set (dependent on the chosen module) opens the next tab automatically, once finished

11 12/9/ New User Interface for Project Handling Import Previous Data possibility to import a previous TopSolids parameter data bank requirement: New part and serial Nos. of the probe need to match

12 12/9/ New User Interface for Project Handling Import Previous Data click on Import browse to the former TopSolids data set select the file topsolidspars.xml

13 12/9/ New Parameter Handling TopSolids parameter handling is based on: 1. parameter sets 2. PROSOL entries New 3. parameter data bank ensures reasonable values for parameters at any time whether optimized or not yet at the end of any optimization, the determined parameters are stored in the parameter data bank ready for further usage parameters can be reviewed in form of a PDF report at any time, e.g. to assist fast publication

14 12/9/ Probe Setup Module from time to time probe performance needs to be tested though routine work, it can be time consuming even for an NMR expert Probe Setup module offers a high level of convenience to: adjust the magic angle optimize 1 H and 13 C hard pulses on standard samples shim the probe and calibrate spectra with least user interaction to overcome the necessity for extensive prior knowledge only two samples needed: KBr, adamantane

15 12/9/ Probe Setup Module Magic Angle Setting New Magic Angle setting is done on KBr ( 79 Br) at 5 khz MAS TopSolids: checks for fixed frequency H/C/N probes to adjust respective parameter sets automatically New New can detect a Cover Module 2, which can be used for MA adjustment at the spectrometer directly if wanted records a reference spectrum and evaluates the quality of the MA setting

16 12/9/ Probe Setup Module Magic Angle Setting center peak line width = 139 Hz 5 th left SBB line width = 132 Hz

17 12/9/ Probe Setup Module New New probe shimming is done on adamantane at 10 khz MAS automated Z shimming possible (2-5 minutes dependent on starting values) automated B 0 field referencing (towards TMS) in the background shim quality is determined automatically

18 12/9/ Probe Setup Module line width = 4.5 Hz calibrated to ppm (referenced to neat TMS)

19 12/9/ Protein Applications News & Updates whole setup to run multidimensional (nd) experiments on biological sample is divided into three modules: 1. Standard Sample Setup standard sample: [ 13 C, 15 N]-labeled glycine for NCO transfer: any [ 13 C, 15 N]-labeled peptide (e.g. fmlf) or standard protein (SH3, GB1, ubiquitin) 2. Biological Sample Setup (re-) optimize parameters on your sample of interest New optional optimizations: spectral widths, carrier frequencies, 1 H decoupling during acquisition 3. nd Experiments New reverse optimization possible does no longer rely on prior optimization

20 Protein Applications Standard Sample Setup Module cross polarization transfers: optimized hard pulses & the current MAS rate* are used to suggest a suitable Hartmann-Hahn condition * when MAS III unit is used, the rate is detected automatically in the background 12/9/

21 12/9/ Protein Applications Standard Sample Setup Module New

22 12/9/ Protein Applications Biological Sample Setup Module comprises optimizations of all parameters needed for multidimensional experiments available in TopSolids + some optional ones if the Standard Sample Setup module has not been executed before, starting values are taken from PROSOL (+ parameter data bank, if parameters are available)

23 12/9/ Protein Applications Biological Sample Setup Module standard 13 C spectral width complete 13 C region 13 CO region 13 Cα region New the smaller a spectral width in an indirect dimension, the shorter the experimental measurement time of an nd experiment TopSolids can optimize spectral widths & carrier frequencies fully automated - based on CP experiments completely optional!

24 12/9/ Protein Applications nd Experiments Module the flow bar itself did not change from the first generation of TopSolids 2D to 4D experiments for protein backbone assignment and distance measurements

25 12/9/ Protein Applications Reverse Optimization Do I need to go through all these optimizations if I only want to record one specific nd experiment? Which parameters do I need for recording a 3D NCOCx experiment? New Start from scratch & use reverse optimization: select an nd experiment of interest in the nd Experiments module TopSolids automatically detects missing parameters & initiates the respective optimization directly using least user interaction once all parameters have been optimized, it will go back to the nd experiment to support its set up a simplification dedicated especially to unexperienced users

26 12/9/ Protein Applications Reverse Optimization Backbone Assignment 3D NCOCx correlation experiment (CC transfer via PDSD) on biological sample of interest CO-Cx mixing time: 30 ms MAS rate: 10.0 khz number of scans: 48 relaxation rate: 2.0 s acquisition time F3(Cx): ms acquisition time F2 (CO): 5.70 ms acquisition time F1 (N): 5.60 ms number of time domain points F3 (Cx): 2048 number of time domain points F2 (CO): 38 number of time domain points F1 (N): 28 total experimental time: 1 d 5 h 46 min 42 sec experiment in queue experiment finished 3D NCOCx recorded with reverse optimized parameters processing was done fully automated by TopSolids after acquisition was finished New titles include information about acquisition parameters

27 12/9/ TopSolids Material Samples New high demand to implement automation and setup support for applications on material samples TopSolids now provides guided routines to: any X nucleus of choice the mounted probe can handle as for protein applications: optimizations on standard samples and/ or sample of interest for: X hard pulse HX CP 1D/ 2D MQMAS

28 12/9/ Material Applications Standard Sample Setup guides through basic setup routines of 90 degree pulse calibration and CP setup X 90 degree pulse optimization either as a high or a low power pulse, depending on the X nucleus of choice for MQMAS experiments switch to the nd Experiment module, once the 90 degree pulse is known

29 12/9/ Material Applications nd Experiments guides step by step through the setup process to run a 2D MQMAS experiment by optimizing: 1. the minimum spectral width needed as indirect dimension to reduce 2D measurement time

30 12/9/ Material Applications nd Experiments guides step by step through the setup process to run a 2D MQMAS experiment by optimizing: 2. specific MQMAS excitation and reconversion pulse lengths for optimum sensitivity using automated parameter optimization and B 1 excitation field calculations reconversion excitation

31 12/9/ Material Applications nd Experiments TopSolids: guides through the 2D setup step by step takes care that a multiple of the phase cycle is used as number of scans automatically synchronizes the optimized spectral width with the MAS rate applies basic processing and shearing user interaction only needed for entering number of scans and relaxation delay

32 12/9/ TopSolids Summary Simplified user interface Suited for protein and material samples, including quadrupolar nuclei New automation features and minimized user interactions, including basic processing up to 3D s Materials modules include HX CP and MQMAS setup Forward & reverse parameter optimization for protein samples Supports 3.2 and 4 mm double and triple channel probes Extended parameter reporting, including information about nd experiments All multidimensional experiments can be queued basic processing is done as soon as an experiment will have been finished

33 Contact core application people solid-state NMR: Gerhard Althoff (DE) Venita Decker (DE) Sebastian Wegner (DE) Barbara Perrone (CH) Jochem Struppe (US) Fabien Aussenac for solids DNP + all the other application people world wide! important s: solids@bruker.com

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35 Revisiting a former TopSolids Project open a previous TopSolids data set and start TopSolids 12/9/