Two methods of calibrating the parameters K and Alpha for use in Gy's formula for the fundamental sampling error were investigated. Approximately 480 kg of broken ore from Harmony's Target gold mine in South Africa was used to compile the replicate samples for two experiments. The duplicate series analysis (DSA) and segregation free analysis (SFA) methods differ in terms of their approach to recovering the sized materials required for the calibration procedure. In this experiment the DSA method split off six more-or-less equal masses of material from a 75 kg lot that was successively crushed to finer and finer fragment sizes. The sublots so formed were split into 32 samples and fire assayed for gold. The SFA method used approximately 250 kg of broken ore crushed to 95 per cent passing 2.50 cm, which was then passed through successively finer screens until a sublot of less than 0.0075 cm was obtained. Each of the 15 sublots obtained in this way were split using a riffle splitter into 32 samples that were fire assayed. A total of 672 fire assays were used in these experiments. The sampling parameters K and Alpha were used for the compilation of a nomogram and to calculate the gold liberation size of the ores. While there are no definitive results in terms of the actual gold grain sizes against which the calculated sizes can be compared, it appears that the DSA method produces more acceptable results.CITATION:Minnitt, R, 2014. A comparison of two methods for calculating the constants K and alpha in a broken ore, in Proceedings Sampling 2014 , pp 165-178 (The Australasian Institute of Mining and Metallurgy: Melbourne).