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[Display omitted] • Automatic setting of rf-power parameters through reference rf-fields for concerted setting of all MAS dependent rf-amplitudes. • CPMAS setup with concerted rf-field parameters in one step for MAS frequencies up to 20 kHz using interdependence of rf-fields given by HH matching condition. • Fast signal optimization for all CPMAS experiments above 20 kHz MAS using interdependence of the participating rf-fields through HH matching conditions relative to the sample's mechanical rotation frequency. • Fast concerted field optimization for all CPMAS experiments with half integer quadrupole nuclei. • Accelerated setups for all advanced recoupling experiments using reference fields and the known MAS frequency dependence of the rf-field amplitudes. • Concerted setup for HFC and HNC double CP experiments using the various HH matching conditions eases access to these more demanding experiments to finding the optimal signal amplitude in few simple steps. Automation in solid state NMR (ssNMR) requires appropriate hardware, from rotor loading mechanisms over highly stable rf-transmitters and probe circuitry to automatic tuning and matching capabilities including automatic magic angle adjustment for ssNMR probes. While these hardware capabilities are highly desirable and are, to various degrees, provided by manufacturers, we focus herein on automating experiment setup using radio frequency (rf) fields, which are key parameters in solid state NMR experiments. Specifically, these include spinlock fields during cross polarization (CP), or rf-fields for homo- or heteronuclear spin recoupling or decoupling. Often, these fields have specific relationships to the magic angle spinning (MAS) frequency. Relying on a well-maintained spectrometer, the experiment setup shifts from traditionally required optimization of rf-power values for each element of an experiment sequence to automatically setting all parameters correctly without any need for optimization. The proposed approach allows executing an experiment by reading its rf-amplitude requirements based on the actual MAS rotation frequency just before starting data acquisition, while all other hardware-related parameters are automatically provided through global tables and scripts. Under modest MAS frequencies, no further rf-power optimization is required while providing optimal sensitivity of better than 90% of the optimal signal to noise. Any optional parameter optimization relates only to adjusting rf-nutation frequencies to the requirements of the sample and the sample rotation frequency rather than the spectrometer hardware. Fast MAS CP experiments with MAS frequencies above 40 kHz require a semi-automated setup by optimizing Hartmann-Hahn (HH) matched rf-fields that are synchronously varied relative to the MAS-frequency. This allows for a significant reduction of setup steps by up to one order of magnitude for such experiments, avoiding the traditional grid search for optimal CPMAS conditions. The approach presented here can also be applied to decoupling or recoupling sequences, requiring rotor synchronized rf-fields, reducing the setup to a few steps addressing the spin system's properties rather than the spectrometer hardware. Our approach permits automating all basic solid state NMR experiments for high throughput analytical tasks. [ABSTRACT FROM AUTHOR]

Abstract: In this contribution we present a constant time version of the well known REDOR pulse sequence which enables us to determine the second moments in multiple spin systems with strong dipolar couplings. From the resulting dipolar evolution curves, accurate values for the second moments can be obtained without the need to incorporate the full information about the detailed spin geometry of the multiple spin systems into the simulation protocol. [Copyright &y& Elsevier]

Abstract: In this work a combination of complementary advanced solid-state nuclear magnetic resonance (NMR) strategies is employed to analyse the network organization in aluminophosphate glasses to an unprecedented level of detailed insight. The combined results from MAS, MQMAS and 31P-{27Al}-CP-heteronuclear correlation spectroscopy (HETCOR) NMR experiments allow for a detailed speciation of the different phosphate and aluminate species present in the glass. The interconnection of these local building units to an extended three-dimensional network is explored employing heteronuclear dipolar and scalar NMR approaches to quantify P–O–Al connectivity by 31P{27Al}-heteronuclear multiple quantum coherence (HMQC), -rotational echo adiabatic passage double resonance (REAPDOR) and -HETCOR NMR as well as 27Al{31P}-rotational echo double resonance (REDOR) NMR experiments, complemented by 31P-2D-J-RESolved MAS NMR experiments to probe P–O–P connectivity utilizing the through bond scalar J-coupling. The combination of the results from the various NMR approaches enables us to not only quantify the phosphate units present in the glass but also to identify their respective structural environments within the three-dimensional network on a medium length scale employing a modified Q notation, Q n m ,AlO x , where n denotes the number of connected tetrahedral phosphate, m gives the number of aluminate species connected to a central phosphate unit and x specifies the nature of the bonded aluminate species (i.e. 4, 5 or 6 coordinate aluminium). [Copyright &y& Elsevier]

• WASPs provide sensitivity-enhanced versions of frequently used 3QMAS sequences. • Extensive comparison between simulated and experimental MQMAS data. • WASPs are shown to be free of amplitude and phase transients. • Compared to conventional pulses, WASPs enable a safer application of high rf-fields. • Easy implementation of WASPs without any additional optimization required. Two-dimensional multiple-quantum MAS (MQMAS) NMR spectroscopy is one of the most widely used solid-state NMR techniques for resolving multiple overlapping central-transition lineshapes for half-integer spin quadrupolar nuclei. In particular when relying on nutation-driven MQ coherence transfers, this technique suffers from low sensitivity that can only be improved by increasing the rf-amplitude of the involved radio-frequency (rf) pulses, which are therefore typically operated at the rf-limit. In such situations, frequently encountered for the three-pulse z-filtered and split-t 1 shifted-echo MQMAS NMR sequences, we introduce the advantages of rf-pulses with smoothly truncated amplitude profiles, which we have termed WURST-Amplitude Shaped Pulses (WASPs). When considering the NMR spectrometer hardware, we demonstrate that WASPs feature more suitable properties in comparison to conventional rectangular pulses, enabling a substantial reduction of voltage reflections and transient effects under identical rf-conditions. By employing extensive numerical simulations and experimental validation, we further show that WASPs intrinsically possess a higher potential for nutation-based 3Q excitation involving spin-3/2 and 3Q and 5Q excitation for spin-5/2 quadrupolar nuclei, specifically when large nutation frequencies are available. The concept of smoothly truncating rf-amplitudes is also extended to Fast Amplitude Modulation (FAM) pulses, normally incorporated for rotor-driven 1Q conversion. We additionally evaluate the potential of employing WASPs with peak rf-amplitudes beyond the rf-limit for conventional rectangular rf-pulses. [ABSTRACT FROM AUTHOR]

We present a detailed analysis of the radiofrequency (RF) field over full volume of a rotor that is generated in a solenoid coil. On top of the usually considered static distribution of amplitudes along the coil axis we describe dynamic radial RF inhomogeneities induced by sample rotation. During magic angle spinning (MAS), the mechanical rotation of the sample about the magic angle, a spin packet travels through areas of different RF fields and experiences periodical modulations of both the RF amplitude and the phase. These modulations become particularly severe at the end regions of the coil where the relative RF amplitude varies up to ±25% and the RF phase changes within ±30°. Using extensive numerical simulations we demonstrate effects of RF inhomogeneity on pulse calibration and for the ramped CP experiment performed at a wide range of MAS rates. In addition, we review various methods to map RF fields using a B 0 gradient along the sample (rotor axis) for imaging purposes. Under such a gradient, a nutation experiment provides directly the RF amplitude distribution, a cross polarization experiment images the correlation of the RF fields on the two channels according to the Hartmann-Hahn matching condition, while a spin-lock experiment allows to calibrate the RF amplitude employing the rotary resonance recoupling condition. Knowledge of the RF field distribution in a coil provides key to understand its effects on performance of a pulse sequence at the spectrometer and enables to set robustness requirements in the experimental design. [ABSTRACT FROM AUTHOR]