Iron and aluminium are the two most abundant metals on the Earth's crust, but they display quite different biogeochemical properties. While iron is essential to many biological processes, aluminium has not been found to have any biological function at all. In environmental studies, iron has been studied in detail for its limiting role in the bioproductivity of high nutrient, low carbon oceanic zones, while aluminium is routinely used as a reference of crustal contributions to atmospheric deposition archives including peat bogs, lacustrine and marine sediments and ice sheets and glaciers. We report here the development of a flow injection analysis technique, which has been optimised for the simultaneous determination of soluble iron and aluminium in polar ice cores. Iron was determined by its catalytic role in the reduction of N,N-dimethyl-p-phenylenediamene (DPD) to a semiquinonic form (DPDQ) and subsequent absorption spectroscopy at 514 nm. Aluminium was determined by spectroscopic analysis of an aluminium-lumogallion complex that exhibits fluorescence at 560 nm. These techniques have been applied to a section of Greenland ice dated to 1729-1733 AD and indicate that volcanism is a source of highly soluble aluminium and iron.