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There are many reports on polymorphs of pharmaceutical and/ or biological compounds due to humidity–dependent hydration/ dehydration processes [1]. For precise analysis of these phase transitons, some important results have been reported using laboratory X-ray systems with humidity controller RIGAKU HUM-1 [2]. For synchrotron experiments, we have introduced a noble humidity control system with HUM-1 on the large Debye-Scherrer camera at the BL19B2 Engineering Science Research I beamline of SPring-8 [3], [4]. Small amount of powdery sample is mounted on a special UV-polyimide device and a humidity controlled mini-chamber adapted with HUM-1 is loaded for in-situ X-ray powder diffraction experiment. For evaluation, we precisely determined phase transitions of nucleosides and nucleotides in wide range of relative humidity (rh) from 0% to 90% at 25°C. Guanosine dihydrate changed to the anhydrous form at 0% rh and it recovered the dihydrate state at 30% rh within 1 hour. Disodium adenosine 5’-monophosphate heptahydrate (Form A) at 50% rh changed to Form B at 80% rh in 1 hour. Form A changed to Form C at 2% rh, and then to Form D at 40% rh. We expect many polymorph mechanisms of hydrate/dehydrate processes will be cleared using this humidity controlled system near future. These experiments were performed with the approval of the Japan Synchrotron Radiation Research Institute (JASRI) (Proposal No. 2009B2068, 2010A1849 and 2010B1803).

Noble humidity control system forin situX-ray powder diffraction at SPring-8