Practical considerations on the use of low RF-fields and cosine modulation in high-resolution NMR of I = 3/2 spin...

Despite its ease in experimental set up, the low sensitivity of MQMAS experiments is often a limiting factor in many practical applications. This is mainly due to the large radiofrequency (RF) field requirement of the two short hard-pulses often used for the optimum MQ excitation and conversion steps. Very recently, two novel MQMAS experiments have been proposed for I = 3/2 nuclei, namely lp-MQMAS and coslp-MQMAS, enabling an efficient MQ excitation/conversion with a reduced RF requirement, by utilizing two long pulses lasting one rotor period each, with or without cosine modulation. In this study, we focus on the practical considerations of these new methods and discuss their pros and cons to elucidate their appropriate use under both moderate and fast spinning conditions. Using four I = 3/2 (⁸⁷Rb, ⁷¹Ga, ³⁵Cl and ²³Na) nuclei at a moderate magnetic field (B₀ = 14.1 T), we show the superior use of these experiments, especially for samples with large C_Q values and/or low-gamma nuclei. Compared to all other existing sequences, the coslp-MQMAS method with initial WURST signal enhancement is the most robust, efficient and resolved high-resolution 2D method for spin 3/2 nuclei. Furthermore, using {²³Na}-¹H spin systems, we demonstrate the sensitivity advantage of the WURST coslp-MQ-HETCOR acquisition upon ¹H detection and fast MAS conditions.