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Determination of the boron/lead ratio in ceramic materials based on electrochemical quartz crystal microbalance

机译:基于电化学石英晶体微量天平的陶瓷材料中硼铅比的测定

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摘要

A method for quantitatively determining the relationship boron/lead in ceramic materials is presented. It is based on the attachment of microsamples of ceramic frits to an electrochemical quartz crystal microbalance (EQCM). After a reductive deposition step in the - 0.25 to - 0.85 V (vs. AgCl/Ag) potential range, well-defined stripping peaks are recorded in 0.10 M NaCl plus 0.10 M mannitol. The deposition of boron and lead from suspensions of solid materials, and its subsequent oxidative dissolution can be monitorized at the EQCM. The quotient between the maximum mass gain and the corresponding charge passed enables for a direct quantitation of the boron/lead molar ratio in ceramic materials. Addition methods based on the EQCM examination of i) sample plus lead white (2PbCO(3).Pb(OH)(2)) and ii) sample plus Li2B4O7 mixtures are also presented. Results for boron-containing ceramic frits are in excellent agreement with those obtained by reference methods.
机译:提出了一种定量确定陶瓷材料中硼/铅关系的方法。它基于陶瓷熔块的微量样品与电化学石英晶体微量天平(EQCM)的附着。在-0.25至-0.85 V(vs. AgCl / Ag)电位范围内进行还原性沉积步骤后,在0.10 M NaCl和0.10 M甘露糖醇中记录了明确定义的溶出峰。可以从EQCM监控固体材料悬浮液中硼和铅的沉积及其随后的氧化溶解。最大质量增益与所通过的相应电荷之间的商可直接定量陶瓷材料中的硼/铅摩尔比。还提出了基于EQCM检验的添加方法,该方法包括:i)样品加铅白(2PbCO(3).Pb(OH)(2))和ii)样品加Li2B4O7混合物。含硼陶瓷熔块的结果与通过参考方法获得的结果非常吻合。

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