The internal combustion engine continues to be the main source of power in various modes of transport and industrial machines. This is due to its numerous advantages, such as easy adaptability, high efficiency, reliability and low fuel consumption. Despite these beneficial qualities of internal combustion engines, growing concerns are related to their negative environmental impacts. As a result, environmental protection has become a major factor determining advancements in the automotive industry in recent years, with the search for alternative fuels being one of the priorities in research and development activities. Among these, fuels of plant origin, mainly alcohols, are attracting a lot of attention due to their high oxygen content (around 35%). These fuels differ from diesel oil, for instance, in kinematic viscosity and density, which can affect the formation of the fuel spray and, consequently, the proper functioning of the compression–ignition engine, as well as the performance and purity of the exhaust gases emitted into the environment. The process of spray formation in direct injection compression–ignition engines is extremely complicated and requires detailed analysis of the fast-changing variables. This explains the need for using complicated research equipment enabling visualisation tests and making it possible to gain a more accurate understanding of the processes that take place. The present article aims to present the methodology for alternative fuel visualisation tests. To achieve this purpose, sprays formed by diesel–ethanol blends were recorded. A visualisation chamber and a high-speed camera were used for this purpose. The acquired video provided the material for the analysis of the changes in the vertex angle of the spray formed by the fuel blends. The test was carried out under reproducible conditions in line with the test methodology. The shape of the fuel spray is impacted by an increase in the proportional content of ethanol in the diesel and dodecanol blend. Based on the present findings, it is possible to note that the values of the vertex angle in the spray produced by the diesel–ethanol blend with the addition of dodecanol are most similar to those produced by diesel oil at an injection pressure of 100 MPa. The proposed methodology enables an analysis of the injection process based on the spray macrostructure parameters, and it can be applied in the testing of alternative fuels.