A novel method of nonintrusive measurement of surface profile, packing density, and surface charge distributions of a powder layer deposited on a substrate is reported. The method employs the deposition of electrostatically charged monodispersed fluorescent latex spheres (FLS), approximately 2 mum in diameter, on the surface of: (1) the substrate before deposition, (2) the powder layer after deposition, and (3) the film formed by curing the powder layer. The surface topography in all cases was mapped using an epi-fluoreseent microscope with a vertical resolution of 2 mum in the z axis and +/-10 mum in the x and y axes. An area of 1 cm x 1 cm is scanned in 1 mm segments, providing approximately 100 data points per cm(2) for the surface topography. For each measurement of surface topography, the substrate was positioned on the microscope stage in a manner such that the reference points (x, y, and z) remained the same for all measurements of the substrate. The surface profiles, with respect to the same reference points, were plotted using Origin 6.0 software for 3D presentation of the topography. The method was also applied to map the surface charge density distribution of electrostatically charged surfaces. The FLS imaging method provides a new tool for examination of surface profiles, packing density, and charge distribution of powder layers on a microscopic scale not provided by optical or atomic force/electrostatic force microscopy (AFM/EFM). While AFM and EFM are very effective in providing similar information with nanometer resolution, they cannot be directly applied on a larger macroscopic scale to study powder layers and for a larger surface area (up to 1 cm(2) or greater) involving deposited particles in the range of 1-50 mum in diameter. For AFM, the range in the z-axis is limited to +/-3 mum and the x-y scan area is limited to 100 mum x 100 mum. The FLS method has a much wider range but it is operated manually; an automated scanning process is required for rapid measurement. A comparison of the FLS and EFM techniques as they apply to analyzing charge distribution on coal surfaces is presented.