The qualitative and quantitative analyses of crystalluria have clinical significance in the diagnosis and prognosis of urolithiasis. The aim of this paper is to provide a new accurate methodology to get qualitative and quantitative data on urine particulate in patients with renal stone disease.The procedure involves a urine collection, the separation of the solid residual by centrifugation, and its analysis by X-ray diffraction, utilizing a micro-diffractometer in order to analyze very low amounts of residual. The spectrum obtained was converted into 2 θ -I profiles and quantitatively refined by Rietveld method. The proposed methodology has the advantage to accurately quantify all crystalline phases and the amorphous component of the urine; anyway urine samples have to be centrifuged and analysed as soon as possible, because the quantitative results obtained by the X-ray microdiffraction showed that after some days and at room temperature urine increased significantly both amorphous and crystalline phases.