AbstractThe mass absorption coefficient is a useful parameter for quantitative characterization of materials. If the chemical composition of a sample is known, the mass absorption coefficient can be calculated directly. However, the mass absorption coefficient must be determined empirically if the chemical composition is unknown. Traditional methods for determining the mass absorption coefficient involve measuring the transmission of monochromatic X-rays through a sample of known thickness and density. Reynolds (1963,1967), however, proposed a method for determining the mass absorption coefficient by measuring the Compton or inelastic X-ray scattering from a sample using Mo radiation on an X-ray fluorescence spectrometer (XRF). With the recent advances in solid-state detectors/electronics for use with conventional powder diffractometers, it is now possible to readily determine mass absorption coefficients during routine X-ray diffraction (XRD) analyses.Using Cu Kα radiation and Reynolds’ method on a Siemens D-500 diffractometer fitted with a Kevex Si(Li) solid-state detector, we have measured the mass absorption coefficients of a suite of minerals and pure chemical compounds ranging in μ/ρ from graphite to Fe-metal (μ/ρ = 4.6-308 using Cu Kα radiation) to ±4.0% (lσ). The relationship between the known mass absorption coefficient and the inverse count rate is linear with a correlation coefficient of 0.997. Using mass absorption coefficients, phase abundances can be determined during quantitative XRD analysis without requiring the use of an internal standard, even when an amorphous component is present.