The performance of four graphites and glassy carbon as sensor anode materials in chronoamperometry experiments for possible determination of Al2O3 were comparatively examined in alumina-cryolite melts at 1010-degrees-C. With graphite anode materials, the anode process(es) is (are) not fully diffusion controlled nor are the results adequately reproducible. Only at glassy carbon is (are) the anodic process(es) diffusion controlled. Consequently, at glassy-carbon sensor anodes, the dependence of the response current function on Al2O3 concentration is found to be approximately linear. The presence or absence of Al metal, dissolved in the melt, as arises in the practical technology of electrolytic aluminum smelting, has a significant effect on the results due mainly to background current contributions from oxidation of dissolved Al.