X-ray fluorescence spectrometry is widely accepted as a highly versatile and potentially accurate method of instrumental analysis. The occurrence of sulphur deficiencies in many areas has led to increased research on the role of sulphur as a plant nutrient. To carry out such research effectively, convenient and accurate analytical methods for determining amounts of sulphur are necessary. This study involves the setting into operation of the newly installed, X-ray fluorescence plant at Lincoln College, and the formulation of an analytical procedure for the rapid determination of total sulphur in soil material. The resultant procedure is applied to analysis for total sulphur in the Reefton chronosequence of soils currently under study in the Soil Science Department.