Highly sensitive analysis of trace germanium derived from the efficient electrosynthesis and spectral introduction of GeH4 on foam electrode

Anal Chim Acta. 2024 Jan 25:1287:342130. doi: 10.1016/j.aca.2023.342130. Epub 2023 Dec 13.

Abstract

Background: The electrochemical hydride generation technology, which uses electrolysis instead of chemical reagents to generate reducing species to achieve gaseous transformation and sample introduction of the tested elements, has received widespread attention in the field of atomic spectroscopy due to its simple, economical, and green characteristics. However, limited by the effective area of the electrode, the introduction efficiency and spectral signal of most elements (e.g., germanium) in practical applications are lower than traditional chemical hydride generation.

Results: In this paper, an efficient electrochemical hydride generation (EHG) method based on metal foam electrode for μg L-1 level germanium was constructed. Systematic electrochemical and spectral tests showed that the low charge transfer resistance and the high electrochemical activity of nickel-based foam electrodes jointly promoted the efficient electroreduction of Ge(IV). Besides, the porous network structure of the metal foam material improves the contact probability of reactants while reducing the gas-evolution effect caused by bubble accumulation. Interestingly, adequate reaction sites are crucial for the conversion of germanium, but large foam electrodes are not always compatible with analytical performance. After coupling atomic fluorescence spectroscopy, this new electrolysis method has been proven to be suitable for efficient conversion and quantitative detection of Ge over a wide concentration range (5-150 μg L-1).

Significance: Our proposal to improve the electrosynthesis efficiency of germanane (GeH4) by using metal foam electrode is extremely effective for the detection of trace or ultra-trace germanium. The exploration of electrode material, structure, and especially effective area will also provide ideas for the establishment of highly sensitive analysis methods in the future.

Keywords: Cathode material; Electrochemical active area; Electrochemical hydride generation; Ge(IV); Metal foam electrode.