The Bukit Botol and Bukit Ketaya deposits are two examples of volcanic-hosted massive sulphide (VHMS) deposits that occur in the Tasik Chini area, Central Belt of Peninsular Malaysia. The mineralisation is divided into subzones distinguished by spatial, mineralogical, and textural characteristics. The primary sulphide minerals include pyrite, chalcopyrite, sphalerite, and galena, with lesser amounts of Sn- and Ag-bearing minerals, with Au. However, pyrrhotite is absent from both deposits. This study presents the results of sphalerite chemistry analysed by using an electron microprobe. Two types of sphalerite are recognised: sphalerite from the Bukit Botol deposit reveals a range of <DL to 24.0 mole% FeS, whereas sphalerite from the Bukit Ketaya deposit shows a range of <DL to 3 mole% FeS. Significant variations are shown in Zn, Cu, Cd, and Ag levels. Although the sphalerite has a wide variation in composition, a discernible decreasing Fe trend is exhibited from the stringer zone towards massive sulphide. This compositional variation in sphalerites may in part reflect variable temperature and activity of sulphur in the hydrothermal fluids during ore formation. Alternatively, the bimodal composition variations suggest that mineral chemistry relates to contrasting depositional processes. The Zn/Cd ratios for sphalerite from both these deposits are similar to those exhibited by volcano−sedimentary deposits with a volcanic origin. Therefore, the consistently low Cd concentrations and moderate to high Zn/Cd ratios suggest mixing of seawater and minor magmatic fluids controlling the chemistry of sphalerite at both deposits during their formation.