This article describes a methodology for analyzing zinc in zinc concentrates materials by wavelength-dispersive X-ray fluorescence (WD-XRF) spectrometry with gel for sample preparation. The sample was decomposed with aqua regia. The sample solution mixed with agaron gel was heated to boiling. The mixture became quasi-solid gel under normal temperature. The elements dispersed in gel medium were detected by WD-XRF spectrometry. The method has both advantages of the solution preparation method and the solid preparation method. In addition, this method was adapted in detecting high content ores, because it avoided the risking of using platinum crucible. The method has been applied to the determination of lead, zinc and iron in zinc concentrates successfully. (C) 2008 Elsevier Ltd. All rights reserved.