Analytica Chimica Acta ( IF 5.7 ) Pub Date : 2023-12-13 , DOI: 10.1016/j.aca.2023.342130 Xiao-Na Liu 1 , Xin-An Yang 1 , Xiang-Feng Chu 1 , Wang-Bing Zhang 1
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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.
中文翻译：
泡沫电极上 GeH4 的高效电合成和光谱引入，对痕量锗进行高灵敏度分析
背景
电化学氢化物发生技术利用电解代替化学试剂产生还原性物质来实现被测元素的气态转化和进样，以其简单、经济、绿色的特点在原子光谱领域受到了广泛关注。然而，受电极有效面积的限制，实际应用中大多数元素（例如锗）的引入效率和光谱信号都低于传统的化学氢化物发生。
结果
本文构建了一种基于泡沫金属电极的高效μg L -1级锗电化学氢化物发生（EHG）方法。系统的电化学和光谱测试表明，镍基泡沫电极的低电荷转移电阻和高电化学活性共同促进了Ge(IV)的高效电还原。此外，泡沫金属材料的多孔网络结构提高了反应物的接触概率，同时减少了气泡堆积引起的析气效应。有趣的是，足够的反应位点对于锗的转化至关重要，但大型泡沫电极并不总是与分析性能兼容。耦合原子荧光光谱后，这种新的电解方法已被证明适用于宽浓度范围（5–150 μg L -1 ）内Ge的高效转化和定量检测。
意义
我们提出的利用金属泡沫电极提高锗烷（GeH 4 ）电合成效率的建议对于痕量或超痕量锗的检测非常有效。对电极材料、结构、特别是有效面积的探索也将为未来高灵敏分析方法的建立提供思路。
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