The principles of energy dispersive x-ray fluorescence (EDXRF) technique and its elemental analysis applications were described in some books and reviews [1-4]. PCBs are an important application for nickel-phosphorus (NiP) coatings, on top of which, additional gold and/or palladium coatings are applied. Phosphorous concentration of chemically (or electroless) deposited nickel-phosphorus (NiP) coating can be analyzed in nondestructive manner in atmosphere without stripping Au and Pd coatings. The FP-based WinFTM software allows a reliable determination of both the mass per unit area of the NiP layer and its P concentration . The reproducibility and accuracy of the analysis is verified by means of certified standard reference material. Their quantification is traceable to accurate mass per unit area primary standards analyzed by several suitable techniques . The typical measurement spot size is about 1mm, but in case of micro-spot instruments even smaller spot sizes (less than 100 µm) are achievable.