Optical diagnostics have become indispensable tools for the study of turbulent flows and flames. However, optical diagnostics developed in the past have been primarily limited to measurements at a point, along a line, or across a two-dimensional (2D) plane; while turbulent flows and flames are inherently four-dimensional (three-dimensional in space and transient in time). As a result, diagnostic techniques which can provide 4D measurement have been long desired. The purpose of this dissertation is to investigate two of such 4D diagnostics both for the fundamental study of turbulent flow and combustion processes and also for the applied research of practical devices. These two diagnostics are respectively code named tomographic chemiluminescence (TC) and volumetric laser induced fluorescence (VLIF). For the TC technique, the emission of light as the result of combustion (i.e. chemiluminescence) is firstly recorded by multiple cameras placed at different orientations. A numerical algorithm is then applied on the data recorded to reconstruct the 4D flame structure. For the VLIF technique, a laser is used to excite a specific species in the flow or flame. The excited species then de-excite to emit light at a wavelength longer than the laser wavelength. The emitted light is then captured by optical sensors and again, the numerical algorithm is applied to reconstruct the flow or flame structure. This dissertation describes the numerical and experimental validation of these two techniques, and explores their capabilities and limitations. It is expected that the results obtained in this dissertation lay the groundwork for further development and expanded application of 4D diagnostics for the study of turbulent flows and combustion processes.Ph. D.