Determination of the Boron/Lead Ratio in Ceramic Materials Based on Electrochemical Quartz Crystal Microbalance

Abstract

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 À 0.25 to À 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 Li 2 B 4 O 7 mixtures are also presented. Results for boron-containing ceramic frits are in excellent agreement with those obtained by reference methods.