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Reaction products in electrochemical processes can be identified by coupling an electrochemical thin-layer flow cell to a thermospray mass spectrometer. The performance of this analytical method, electrochemical thermospray mass spectrometry, is demonstrated. This includes the characterization of the improved electrochemical thin-layer flow cell. This cell offers the possibility to combine cyclic voltammograms with mass spectrometry. This goal was achieved, too, by the construction of a new thermospray ion source and a special vacuum recipient.

Using differential electrochemical mass spectrometry, we determined the amount of H2‐evolution occuring during formaldehyde oxidation as a function in the potential region of the first oxidation wave. In the second wave, the oxidation product is CO2 in pH 8 solution, as opposed to more alcaline solutions where only formiate is formed. Formaldehyde is reduced to methanol at potentials negative of the RHE.—An electrochemical formaldehyde sensor was built with a sensitivity below 1 ppm. Cross sensitivities towards alcohols can be lowered by UPD of Ag or Hg.

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