Here, 256 μL of aqueous solution of MHA (5 mM) was introduced into 5 mL of aqueous solution of purified Au25(MHA)18 NCs (0.2 mM Au atom basis). The pH was kept at 9.10 ± 0.20. Glass containers were used in the experiments. The container was saturated with air after adding the thiol ligands to initiate the etching process, and it was kept airtight. The solution for testing was drawn out by a syringe to avoid possible loss of solvent. The temperature was kept at 25 °C. The container was also kept in dark to avoid possible influence of light. Three batches of experiments were conducted to ensure the reproducibility of the etching process. The reaction solution was directly purged into ESI-MS instrument without further purification, enabling a real-time ESI-MS monitoring of the etching process.
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