FIELD: chemistry.
SUBSTANCE: method for determining proton concentration in proton-conducting oxides consists in the following: oxide sample is placed into reactor, connected with gas circuit, dried with heating to temperature 900÷1000°C. After that, gas phase is replaced by hydrogen-containing atmosphere, change in time of oxide parameter value, directly connected with change of quantity of protons in oxide, is registered, with achievement of state of oxide equilibrium with gas phase, and calculation of proton concentration in proton-conducting oxide as quantity of substance in oxide, related to one oxide mole, is carried out. As oxide parameter, directly connected with change of quantity of protons in proton-conducting oxide, value of hydrogen pressure above oxide in closed gas circuit of constant volume is used, for which purpose sample is placed into reactor, which is vacuum tightly connected with gas circuit, isolated from atmosphere. After that, gas circuit with reactor is pumped to high vacuum and sample is dried, exposing it at drying temperature until residual pressure not higher than 10-7 Pa is set. After that, vacuum tight connection of reactor with gas circuit is closed, highly pure hydrogen is supplied into circuit to specified pressure, vacuum tight connection of reactor with gas circuit is opened, and after immediate setting of common hydrogen pressure in "reactor-gas circuit" system change of value of hydrogen pressure above sample in time is registered, with achievement of state of equilibrium of oxide with gas phase, calculation of proton concentration in proton-conducting oxide is carried out on the basis of difference of hydrogen pressure, set immediately after opening of vacuum tight connection, and obtained equilibrium value of hydrogen pressure above sample.
EFFECT: increased degree of examined sample drying, increased accuracy of measurement of proton concentration in dry hydrogen atmosphere, as well as reduction of hydrogen consumption.
2 dwg
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Authors
Dates
2015-11-20—Published
2014-05-05—Filed