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The results of the elemental and chemical composition analysis of human medical samples (blood, serum, hair, urine, tooth, kidney stones, gallstones) and environmental samples (slag, cereal, vegetables, our, pork bones, pork meat, sh) are presented. The analysis were performed by application of the total re ection X-ray uorescence, wavelength dispersive X-ray uorescence and X-ray powder di raction methods. With X-ray uorescence methods the following elements were identi ed: O, Na, Mg, Al, Si, P, S, Cl, K, Ca, Ti, Mn, Fe, Ni, Cu, Zn, Se, Br, Rb, Sr, Zr, I, Ba, and Pb, whose concentrations were from a few ng/g to tens of percent. For some samples the elemental analysis was extended by X-ray powder di raction measurements. With this method the chemical composition was determined. In the paper the experimental setups, methodology of samples preparation and methods of carrying out the measurements are described. As an example the X-ray spectra registered for gallstone sample are discussed in detail. Finally, the results of X-ray di raction and elemental analysis for selected medical and environmental samples are summarized.