In recent years, many problems of elemental sulfur deposits in natural gas transmission line systems have been noted. These problems occur very often immediately downstream of a pressure reduction facility. To prevent the apparition of solid sulfur deposits causing security and maintenance problems it is imperative to determine sulfur solubility in natural gas at pressures and temperatures corresponding to transport conditions. In a previous work (Serin et al. J. Supercrit. Fluids 2010, 53, 12-16), an original experimental apparatus was designed, and experimental saturation values of carbon dioxide in sulfur were obtained. The protocol principle is schematically divided into three steps: saturation, trapping, and quantification. In this work, experimental sulfur solubility in methane was measured and compared to available studies at 363.15 K in the pressure range from (4 to 25) MPa. This paper presents these measurements and the improvements of the trapping and quantification steps that have been made to get these solubility data.