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Anal Chem. 2018 Jun 19;90(12):7154-7157. doi: 10.1021/acs.analchem.8b02498. Epub 2018 Jun 7.

In Situ Mass Spectrometric Screening and Studying of the Fleeting Chain Propagation of Aniline.

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State Key Laboratory of Urban Water Resource and Environment , Harbin Institute of Technology , Harbin , Heilongjiang 150040 , P.R. China.
Department of Chemistry , Stanford University , Stanford , California 94305 , United States.
Biological & Chemical Engineering Department , Weihai Vocational College , Weihai , Shandong 264210 , P.R. China.


A simple and effective approach to studying the mechanism of electrooxidation of aniline (ANI) is reported in this paper. It was accomplished by an innovative electrochemistry (EC)-mass spectrometry (MS) coupling, which can sample directly from a droplet-scale reacting electrolyte for mass spectrometric analysis. With this setup, the polymer chain growth of ANI could be monitored in situ and in real-time. The short-lived radical cations (ANI•+, m/ z 93.06) as well as the soluble dimer ( m/ z 183.09) and oligomers ( m/ z 274.13, 365.18, ...) were successfully captured. Using the EC-MS and tandem mass spectrometry, the dimers produced by head-to-tail (4-aminodiphenylamine), head-to-head (hydrazobenzene), and tail-to-tail (benzidine) coupling of radical cations were found in the same polymerization process. Moreover, the EC-MS method was also applicable for determining the propagation speed of ANI when applying different electrolyte salts and oxidizing potentials.

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