We demonstrate the potential of designing magnetic resonance spectroscopy experiments for investigating electrochemically relevant setups. Up until now, such nuclear magnetic resonance measurements were heavily obstructed by the fact that conductive components interact with magnetic fields. In a new approach, we show that this interaction can be deliberately utilized to achieve a spatially selective measurement of electrochemical environments.

To measure very weak magnetic resonance signals without new hardware, we changed how data are collected. Rather than one long sweep, we recorded many short, overlapping pieces, cleaned each piece, and then merged them. On standard instruments and with equal measuring times, this increased usable signal compared with background by about 5 to 10 times across three test samples, helping reveal details that long averaging can hide.

Dual bilinear rotations are introduced, which lead to well-defined rotations for both heteronuclear spins I and S that depend on the presence or absence of a (large) coupling between them. These are therefore an extension of conventional bilinear rotations, which cause such a spin-system-dependent rotation only for the spin I. A general derivation of the approach is given, and a quadruple-J-resolved type experiment is introduced for demonstration.

It is shown that proton long-lived states can be observed on benchtop nuclear magnetic resonance spectrometers in molecules containing short aliphatic chains. The effects of strong coupling between methylene groups can be mitigated by optimizing the amplitude and duration of the excitation pulse.