The water content of electrochemically deposited polyvinylferrocene films was studied using the electrochemical quartz crystal microbalance. Unhydrated films were introduced into aqueous sodium perchlorate solution. Using cyclic voltammetry, the mass and charge change accompanying electrochemical cycling between oxidized and reduced states was determined. During the first oxidation cycle, water uptake into the unhydrated film is triggered after ca. 40% conversion. Of the water taken up during the first cycle, about 50% is retained upon reduction. The water expelled during reduction is reversibly taken up during the next oxidation cycle. Loss and gain of water during subsequent cycling is chemically reversible. After the first oxidation half-cycle, water uptake/loss is linearly correlated with charge transfer in either direction.) unless CC License in place (see abstract). ecsdl.org/site/terms_use address. Redistribution subject to ECS terms of use (see 132.239.1.231 Downloaded on 2014-11-18 to IP
A cold stage for Bragg–Brentano geometry X‐ray powder diffraction is described for use in the temperature range from about 250 to 300 K. The stage is constructed in such a way that it may be removed from the diffractometer and pre‐cooled to its base temperature before the sample is loaded. After loading, thermoelectric cooling maintains the specimen at low temperature (ice free) whilst the body of the stage is allowed to return to room temperature prior to remounting on the diffractometer.
An apparatus for the compression of materials to ∼2 GPa and subsequent rapid chilling to 80 K with extraction to ambient pressure is described. The partial resolution of a long-standing problem concerning the high-pressure phase behaviour of a water-rich salt hydrate is demonstrated using the equipment.
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