Quantitative mapping of metal ions freely diffusing in solution is important across ad iverse range of disciplines and is particularly significant for dissolution processes in batteries,m etal corrosion, and electroplating/polishing of manufactured components.H owever,m ost current techniques are invasive,r equiring sample extraction, insertion of an electrode,application of an electric potential or the inclusion of am olecular sensor.T hus,t here is an eed for techniques to visualize the distribution of metal ions non-invasively,i nsitu, quantitatively,inthree dimensions (3D) and in real time.Here we have used 1 Hm agnetic resonance imaging (MRI) to make quantitative 3D maps showing evolution of the distribution of Cu 2+ ions,n ot directly visible by MRI, during the electrodissolution of copper,w ith high sensitivity and spatial resolution. The images are sensitive to the speciation of copper,the depletion of dissolved O 2 in the electrolyte and showt he dissolution of Cu 2+ ions is not uniform across the anode.Inmany electrochemical experiments,i ti so ften assumed that the total measured current is distributed uniformly across the entire electrode surface.A ny evidence for an inhomogeneous distribution usually comes from post-mortem examination of electrode surfaces,w hich typically requires the system to be dismantled. This is adestructive process and can be,i nt he case of some batteries,p otentially dangerous. Hence,t here has long been considerable interest in the development of non-invasive,i nsitu measurements of local current distribution. One of the biggest challenges,i nt his respect, is the detection of the distribution of metal ions in solution, which is critical for the development of improved battery,anti-corrosion, and electroplating technologies.Thedetection of metal ions in solution can be performed either spectroscopically or electrochemically.I nsitu electrochemical detection typically uses ion-selective electrodes or scanning electrochemical microscopy [1] (SECM), which is often combined with anodic stripping voltammetry [2] (ASV) to detect metal-ion concentrations at the interface between the electrolyte and metal with as patial resolution on the order of tens of microns at concentrations in the parts per billion (ppb) to parts per trillion (ppt). However,a st he sample must be scanned relative to an electrode tip,t he technique is invasive,r esulting in the disturbance of mass transfer profiles,and images can be relatively slow to collect, cover arelatively small area (on the order 10 2 10 2 mm 2 )and are generally limited to atwo-dimensional (2D) region within the diffusion layer. In situ spectroscopic monitoring of electrochemical reactions [3] has employed av ariety of techniques,including UV/Vis,infrared (IR), and Raman spectroscopies.T he spectroscopic detection of metal ions is most commonly achieved through the use of molecular sensors, [4] which are typically probed using fluorescence spectroscopy or microscopy,enabling detection of the presence,concentration and envir...