Gold nanoparticles (~30-60 nm in diameter
) weredeposited onto the surface of glassy carbon microspheres(10-20
m) through electroless plating to produce bulk(i.e., gram) quantities of nanoparticle surface-modifiedmicrospheres. The gold nanoparticle-modified powderwas then characterized by means of scanning electronmicroscopy and cyclic voltammetry. The voltammetricresponse of a macroelectrode consisting of a film of goldnanoparticle-modified glassy carbon microspheres, boundtogether and "wired-up" using multiwalled carbon nanotubes (MWCNTs), was investigated. We demonstrate thatby intelligently exploiting both nano- and microchemicalarchitectures and wiring up the electroactive centers usingMWCNTs in this way, we can obtain macroelectrodevoltammetric behavior while only using ~1% by mass ofthe expensive gold material that would be required toconstruct the equivalent gold film macrodisk electrode.The potential utility of electrodes constructed usingchemical architectures such as this was demonstrated byapplying them to the analytical determination of arsenic(III) concentration. An optimized limit of detection of 2.5ppb was obtained.