The Planar Laser Induced Exciplex Fluorescence (PLIEF) technique is widely used to visualize and measure the fuel concentration fields in both liquid and vapor phases of DI Diesel sprays. However, the real limitations of the PLIEF technique in Diesel sprays and the accuracy of the results obtained are still a source of controversy. In this work, a complete methodology for maximum penetration and fuel concentration measurements in evaporating conditions in Diesel sprays has been developed and the reliability of the results obtained has been investigated. The methodology includes new procedures for measuring both liquid and vapor phases, adapting, when necessary, correlations available in the literature for calibration. An experimental matrix of nine test points with different injection pressures and combustion chamber densities has been performed. A critical analysis of the different error sources for proper quantification is made. Results have shown that macroscopic features can be accurately determined using the PLIEF technique, but for fuel concentration measurements special considerations have to be taken into account, particularly in the regions where liquid and vapor coexist. (c) 2005 Elsevier Ltd. All rights reserved.