The routine determiniation of lead and zinc in soil by atomic absorption spectrometry (AAS) of a hotaqua regiaextract and by X‐ray fluorescence (XRFS) spectrometry of the powdered soil is described and the results obtained by the two techniques compared. A strong positive correlation was found between the concentration for both elements obtained by the two methods. Generally, assaying by XRFS gave higher soil lead and zinc concentrations than that determined by AAS assay of an acid extract. However, extraction byaqua regiafollowed by AAS provides a satisfactory method for determining the lead and zinc concentrations in soil as a routine procedure.