Abstract: A method of X-ray diffraction (XRD) for quantitative analysis of kyanite was proposed. The sample was powdered to size between 10 and 15 μm, and pressed in a mould to form a sample wafer with its thickness of 0.2 mm. Eleven calibration samples were prepared by mixing purified kyanite and pure quartz in various proportions and were used for preparation of working curve; same amounts of corundum were added separately to each sample as internal standard for correction of matrix interference. The proposed method was used in the analysis of geological sample of kyanite, and the results obtained were checked quite well with the theoratical values.