Impurities in industrial synthetic diamond powder samples were analyzed by X-ray diffraction (XRD) and Flame Atomic Absorption Spectrometry (FAAS). Specimen for FAAS is required in solution form. Diamonds are chemically inert to most acids and alkalies. Carbon was removed as CO2 on heating and estimated gravimetrically. The remaining residue was fused with di-lithium tetraborate and dissolved in nitric acid. Impurities such as Si, Al, Fe, Ca, Mg, W, Na, Co and Ni were then determined by FAAS. Crystalline phases of major impurities were identified by XRD. (C) 2004 Kluwer Academic Publishers.