In this study, arsenic sulphide As4S4 nanoparticles have been prepared, by high-energy wet milling, in the presence of sodium dodecylsulphate, which acts a surfactant. Solid state properties of the nanoparticles were characterised by XRD, Raman scattering, specific surface area and particle size distribution. Changes in surface areas of the particles, in the 0.2 - 5.4 m2 g-1 range, and nanosize distributions, in the 100 - 250 nm range, characterise the surface and morphological properties of nanorealgar. Raman scattering revealed various species in the milled sample that indicate a disproportionate reaction (3As4S4 → 4As2S3 + 4As) occurring as a consequence of milling. Anticancer effects, of the milled species, were confirmed for the human multiple myeloma U266 and OPM1 cell lines. Dissolution experiments in simulated gastric fluid show a possibility for the application of the realgar nanoparticles as an oral dose in future arsenic drug cancer treatments.