In order to investigate the leaching process in more detail, a leaching study was carried out with timed intervals of 1, 2.5, 7.5 and 10 min. PXRD patterns showed a decrease in the amount of spinel present in the mixed cathode material with increasing time (Figure ). The chemical composition of the cathode materials before, during and after the leaching process was investigated using ICP-OES analysis and is shown in Table . In agreement with the results previously highlighted, the ICP-OES data for the ascorbic acid leachates shows the expected leaching of Mn and Li, and data also showed additional low amounts of Ni, Co and Al (Figure ). Calculated molar ratios of metals in LMO (leachate, 10min) from ICP-OES are given as 0.976:0.004:0.02 (Mn:Co:Al). After ascorbic acid leaching, the remaining cathode material was recovered and microwave digested in aqua regia. As expected, after ascorbic acid leaching there was a significant decrease in the percentage of Mn in the remaining cathode material such that levels are very low. In comparison only ≈ 80% of Li is leached suggesting this process does not result in excessive leaching in Li from the layered oxide phase. The metal ratios M in the LO (LiMO2) can be determined as Ni0.800Co0.145Mn0.007Al0.048 suggesting that the remaining layered oxide phase after the leaching process has a composition consistent with an NCA phase. SEM-EDX analysis was also conducted to probe the leaching process (Figure and Figure ). Prior to leaching, the cathode material showed clearly differentiated Mn-and Ni-rich domains attributed to LMO and LO phases, respectively. The Co that is present in the sample appears to reside within the layered oxide. The '0 minutes' timestamp refers to the material immediately after the NaOH bath, but prior to any exposure to the ascorbic acid. The two phases (Figure ) can be instantly recognised by their starkly differing Mn contents and as the ascorbic acid treatment proceeded the Mn-rich crystallites appeared to dissolve away. The size and number of Mn-rich crystallites diminished as the ascorbic acid leaching took place, with the observed crystallites mostly comprising the Ni-rich phase at 10 minutes, with a few residual amorphous Mn-rich deposits remaining around the LO-crystallites. Voids were now clearly visible in the cathode material and, rather than clearly distinct Mn and Ni domains, the remaining Ni, Mn and Co all appeared to be located in the same place suggesting that only the layered oxide remained within the carbon-polymer matrix. This agrees with the PXRD data shown in Figure , where at 10 minutes no spinel signal could be identified over the background, and no Mn-rich crystallites could be observed. This demonstrates the selective nature of the ascorbic acid as a separation method, which can be used to dissolve one type of cathode material (LMO, spinel-type) over another (Ni-rich, layered-oxide type) when both are physically mixed in the cathode material. initial aim for this route was to examine if Li could be reinserted into the layers and hence regenerate directly the layered oxide, as the host structure remains intact after the initial leaching treatment. This 'direct recycling' approach, where the active material is reconditioned and used directly in new cells, could potentially offer lower cost. Initial experiments (160°C/1M/12h) used LiOH, however, the PXRD results (Figure ) suggested the formation of M(OH)2 (where M= Ni, Co, Mn and Al) as the major phase rather than relithiation of the LO phase to form regenerated Li-LO. This M(OH)2 phase can still be used as a precursor for the regeneration of the LO phase via higher temperature synthesis. As direct relithiation was not successful it was decided to replace LiOH by NaOH to see whether the same results could be achieved using the lower cost reagent. The results (Figure ) show that the hydroxide can also be obtained using NaOH with no peak shifts that could be indicative of Na intercalation/contamination. A further reduction in the concentration from 1M to 0.5M resulted in the same hydroxide product.