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We report equipment consisting of the coupling of an electrochemical system for measurement and regulation of oxygen partial pressure (PO2) to a symmetrical thermogravimetric analysis system built on the basis of a Cahn 1000 electrobalance. The electrochemical system allows the measurement and regulation of PO2 within a few percent, and has the additional advantage that it can be checked against systematic errors in an absolute way by means of the ’’Faraday’s law test.’’ The performance of the whole experimental setup is demonstrated by the resolution of a narrow hysteresis loop shown by PO2 as a function of composition in the U3O8 phase of the uranium–oxygen system.

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