Caffeine determination in beverages by voltammetry with the carbon-containing electrodes modified with aryldiazonium salts

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The method of carbon containing electrode (CCE) modification with tosylated arendiazonium salts (ADT) was proposed for the voltammetric (VA) determination of caffeine in beverages. The comparison of chemical spontaneous and electrochemical modification approaches was carried out for ADT modified CCE for VA caffeine determination for the first time. A new class of ADT is characterized by high solubility and stability for one month that plays significant role in the process of electrode surface modification. Salts with nitro and carboxy substituents were tested. The optimal conditions for the spontaneous chemical modification of the CCE were selected: ADT modifier with N02 substituent, electrode immersion time in the modifier solution for 10 seconds, modifier concentration of 5 mg/dm3. ADT deposition on the electrode surface was confirmed by the IR spectroscopy and scanning electron microscopy with the formation of covalent bonds between the carbon atoms of electrode surface and the benzene rings of the modifier. It was shown that the electroactive surface area increases by two times after the modification. Consequently, the technique sensitivity increasing the detection limit of 51 mg/dm3 and linear range extension from 154 up to 500 mg/dm3 was observed. While applying the modified electrode, the analysis time was reduced to 15 minutes. Furthermore, the suitability of CCE modified with N02 substituent was tested for the analytical purposes. As a result, the caffeine was determined in some tonic and carbonated drinks. The comparison of the results obtained by the proposed method with ADT modified CCE and the level declared by the manufacturer was carried out. The high compliance was established. In addition, the obtained data was consistent with the results by the independent spectrophotometric method.

Original languageEnglish
Pages (from-to)56-65
Number of pages10
JournalAnalitika i Kontrol
Issue number1
Publication statusPublished - 1 Jan 2020


  • Caffeine
  • Carbon-containing electrode
  • Cyclic voltammetry
  • Diazonium aromatic salts
  • Ir spectroscopy
  • Modifier
  • Sem
  • Spontaneous modification
  • Voltammetry

ASJC Scopus subject areas

  • Analytical Chemistry

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