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The ultimate goal of the present study is to enhance high heat flux removal and thermal management using spray cooling techniques. As a result, a two-phase heat transfer spray cooling loop was developed capable of removing high heat fluxes from a 0.0001 m2 (1 cm2) heated surface using water. The specific objectives were based on providing the necessary measuring tools and instrumentation for designing an efficient heat transfer loop diagnostics and measuring system. The instruments used consisted of the following measurement device types: flow rate, pressure, temperature, and void fraction. The selection of these devices involved preliminary analyses which were done in order to insure the measuring tool’s suitability for measuring quantities and parameters of interest. Two designs of capacitive void fraction sensors were considered. Over the course of the present study, some of the problems associated with the first void fraction sensor electrode design were identified and a new sensor electrode configuration was developed which provided a more sensitive and repeatable response. Data was collected covering a wide range of void fraction measurements ranging from 0 to 1 for two candidate fluids. The calibration data obtained was nonlinear for the full range of void fraction measurements. The present study also consisted of designing a thick film resistive high heat flux heater. The design and calibration procedures developed and used for each measuring tool is discussed further in detail.