Mineralogical information forms a vital basis for designing, diagnosing and optimizing mineral processing circuits. Often modal mineralogical mass balance (i.e. mass balance on mineral grades) is adequate; i.e. liberation data is not required. In analysing mineral grades in process samples automated mineralogy (SEM based image analysis) is mostly used. As this method is tedious, slow, and costly, and has some limitation, an alternative technique was developed by combining quantitative X-ray diffraction (XRD) and chemical assays by X-ray fluorescence (XRF). A case study on magnetic separation test is presented. Method has potential for an automatized off-line technique for providing mineralogical mass balance in majority of mineral processing plants.