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溶出伏安法中玻碳镀汞电极表面的汞膜状态 被引量:3

THE APPEARANCE OF THE MERCURY FILM PLATING ON GLASSY CARBON ELECTRODE EMPLOYED IN STRIPPING VOLTAMMETRY
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摘要 本文对不同条件下形成的汞膜进行了显微观察,并与电化学方法结合,研究了玻碳电极上汞膜的形成过程、汞膜形态与其形成条件的关系以及对溶出峰的影响.结果表明:玻碳表面的汞膜是由视直径小于10μm的微汞滴构成,其分布密度随镀汞电位的负值增加而增加;微汞滴在电析过程中不断长大并相聚成更大一些的微汞滴,在旋转玻碳电极上,汞膜的最大平均厚度不会超过5μm,而适用于溶出分析的范围为0.05~1μm,比文献记载的范围(0.001~10μm)要窄得多;镀汞用的Hg浓度的适用范围为1×10~2×10M;Hg浓度为2×10M时虽经长时间镀汞亦不易产生较大的微汞滴.实验还表明峰高的重现性与电极表面的载汞量有关.还观察到较大的微汞滴在电极表面滑动以致被甩离电极表面的现象,严重时会引起峰高的下降. The processes of the formation of mercury film on the surface of glassy carbon electrode,the relation between the appearance of the film and the deposition condition,and the effect of the result of stripping analysis are experimentally investigated by means of a microscope equipped with a camera,as well as by electrochemical methods.Both the preparation of mercury film and stripping analysis are carried out in 0.1M KCl base solution(pH4).The film deposited on glassy carbon electrode consists of microdrops of mercury with maximum diameter less than 10μm.The applicable average thickness of mercury film plated on rotating glassy carbon electrode is from 0.05 to 1μm.The suitable concentration of Hgfor plating the film is from 1×10to 2×10M,and 2×10M is recommended.
出处 《化学学报》 SCIE CAS 1985年第2期134-139,共6页 Acta Chimica Sinica
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