Bezbaruah Achintya N, Zhang Tian C
Civil Engineering Department, University of Nebraska-Lincoln at Omaha, Omaha, Nebraska 68182-0178, USA.
Anal Chem. 2002 Nov 15;74(22):5726-33. doi: 10.1021/ac020326l.
A new method for fabrication of anodically electrodeposited iridium oxide film pH microelectrodes has been developed in this study. Novel for its tip size (3-10-microm tip diameter), the microelectrode is fabricated in a tapered glass micropipet filled with a low melting point alloy. The tapered end is recessed and platinized. Thereafter, iridium oxide is electrodeposited over the platinized end in the recessed part. The microelectrode has a very short response time (t80 < 5 s) in the pH range of 0-12 with an accuracy of 0.05 pH unit. The pH microelectrode is not affected by most ions and complexing agents of relevance in environmental and biological studies; it can be used in fluids over wide ranges of stirring speeds (0-55 rpm) and temperatures (approximately 5-40 degrees C). Redox agents such as dissolved oxygen and hydrogen peroxide have no effect on the pH response while quinhydrone, ferro- and ferricyanide, and sodium sulfide have marked effects. However, the microelectrode can still be used in any sample when calibration is done in standards having similar redox characteristics.
本研究开发了一种制备阳极电沉积氧化铱薄膜pH微电极的新方法。这种微电极的新颖之处在于其尖端尺寸(尖端直径为3 - 10微米),它是在填充有低熔点合金的锥形玻璃微吸管中制造的。锥形末端凹陷并镀铂。此后,在凹陷部分的镀铂端上电沉积氧化铱。该微电极在0 - 12的pH范围内响应时间非常短(t80 < 5秒),精度为0.05个pH单位。该pH微电极不受环境和生物学研究中大多数相关离子和络合剂的影响;它可用于不同搅拌速度(0 - 55转/分钟)和温度(约5 - 40摄氏度)范围内的流体。溶解氧和过氧化氢等氧化还原试剂对pH响应没有影响,而醌氢醌、亚铁氰化物和铁氰化物以及硫化钠有显著影响。然而,当在具有相似氧化还原特性的标准溶液中进行校准时,该微电极仍可用于任何样品。