Spectra of K X-rays emitted from pure 3d transition metals and their oxide and sulfate compounds were measured using a single crystal wavelength dispersive X-ray spectroscopy (WDXRF). The measurements were performed using a ZSX-100e sequential spectrometer equipped with an Rh X-ray tube operated. An accurate analytical representation of each line was obtained by a fit to a Lorentz function. The spectra were analyzed in order to examine the K X-ray peak parameters such as asymmetry index, peak energy and relative intensity ratios. The energy shifts and relative intensities weredetermined tobetter understand the chemical effect.