A carbon fiber brush electrode (CFBE) was newly designed and used as a substrate for both controlled potential electrolysis and atmospheric solids analysis probe (ASAP) mass spectrometry. Electropolymerized and strongly adsorbed products of electrolysis were directly desorbed and ionized from the electrode surface. Electrochemical properties of the electrode investigated by cyclic voltammetry revealed large electroactive surface area (23 ± 3 cm2) at 1.3 cm long array of carbon fibers with diameter 6-9 μm. Some products of electrochemical oxidation of pentabromophenol and 2,4,6-tribromophenol formed a compact layer on the carbon fibers and were analyzed using ASAP. Eleven new oligomeric products were identified including quinones and biphenoquinones. These compounds were not observed previously in electrolyzed solutions by liquid or gas chromatography/mass spectrometry. The thickness around 58 nm and 45 nm of the oxidation products layers deposited on carbon fibers during electrolysis of pentabromophenol and 2,4,6-tribromophenol, respectively, was estimated from atomic force microscopy analysis and confirmed by scanning electron microscopy with energy-dispersive X-ray spectroscopy measurements.

中文翻译：

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碳纤维刷电极作为大气固体分析探针 (ASAP) 质谱的新型基材：溴化酚的电化学氧化

碳纤维刷电极 (CFBE) 是新设计的，并用作控制电位电解和大气固体分析探针 (ASAP) 质谱的基板。电解的电聚合和强吸附产物直接从电极表面解吸和电离。通过循环伏安法研究的电极的电化学性质显示，在直径为 6-9 μm 的 1.3 cm 长碳纤维阵列处具有大的电活性表面积 (23 ± 3 cm2)。五溴苯酚和 2,4,6-三溴苯酚的一些电化学氧化产物在碳纤维上形成致密层，并使用 ASAP 进行分析。确定了 11 种新的低聚物产品，包括醌类和双苯醌类。这些化合物以前没有通过液相或气相色谱/质谱法在电解溶液中观察到。在五溴苯酚和 2,4,6-三溴苯酚电解过程中沉积在碳纤维上的氧化产物层的厚度分别约为 58 nm 和 45 nm，通过原子力显微镜分析估计，并通过具有能量色散 X 的扫描电子显微镜证实射线光谱测量。