Manometric real-time studies of the mechanochemical synthesis of zeolitic imidazolate frameworks.

We demonstrate a simple method for real-time monitoring of mechanochemical synthesis of metal-organic frameworks, by measuring changes in pressure of gas produced in the reaction. Using this manometric method to monitor the mechanosynthesis of the zeolitic imidazolate framework ZIF-8 from basic zinc carbonate reveals an intriguing feedback mechanism in which the initially formed ZIF-8 reacts with the CO byproduct to produce a complex metal carbonate phase, the structure of which is determined directly from powder X-ray diffraction data. We also show that the formation of the carbonate phase may be prevented by addition of excess ligand.