Abstract: A directly quantitative method for the determination of asbestos contents in talcum samples by X-ray powder diffraction (XRD) method and polarizing microscopy was developed. A set of talcum samples with asbestos contents ranged from 0.1% to 1.5% was prepared as reference standards for XRD measurements. The method has been applied to the quantitative determination of trace asbestos in talcum samples with satisfactory results. The method also provides the advantages of low detection limit, good reproducibility, high efficiency and less consuming.