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Electrode - electrolyte interface, where double electric layer is being formed and chemical reactions occur, is a heart of all electrochemical energy storage and conversion systems. The evolution of the chemical composition and structure at the interfaces affects overall functional parameters of the electrochemical systems including power and long-term stability of its performance. That’s why chemical processes at the interface should be thoroughly analyzed. Although it is of a great importance, the analytical techniques are still very limited, and in most cases electrochemists have no ability to accomplish the electrochemical data with direct experimental characterization of the interface, which is buried under electrolyte and thus is inaccessible to the most common surface science tools. Though ex situ studies help a lot, in many cases, nevertheless, they are not suitable for analysis of short-lived intermediates, which are often crucial for the understanding of the whole process. The approaches to probe chemical reactions at electrified interfaces by X-ray photoelectron spectroscopy are discussed in the talk. Recent operando XPS observations of electric double layer formation and redox processes at the electrochemical interfaces involving both solid and liquid electrolytes will serve as an examples for illustration of the new possibilities delivered by synchrotron radiation induced photoemission.