As a consequence of the surplus of glycerol generated from the development of the biodiesel industry, making valuable products from it has been an ongoing subject for the past few years. In previous work, several products have been synthesized from glycerol, such as solketal, with a proven value as an additive to different types of fuels. On the other hand, n-hexadecane is frequently used as a reference compound to model diesel properties. This work presents a thorough experimental study on the determination of different volumetric properties of binary mixtures containing n-hexadecane and solketal, namely, density, viscosity, surface tension, refractive index, and the excess properties and deviations thereof derived. These properties were measured over the entire range of compositions in increments of the molar fraction of the components of 0.1 in the range from 293.15 or 298.15 to 323.15 K. Finally, correlation of the Redlich Kister equation to the experimental excess properties and deviations was made, allowing for the retrieval of the corresponding fitting parameters.