The basic principles and procedures for performing accurate X-ray microanalyses on semiconductor materials as well as the differences and advantages of EDS (energy-dispersive spectroscopy) and WDS (wavelengthdispersive spectroscopy) are presented. Many of the techniques discussed are the result of extensive experience with some photovoltaic materials such as CuInSe2, GaAs, CdTe, CdS, CdSnP, Id?, ZnP, and amorphous Si-based alloys.Results of an experiment designed to compare the performance of an energydispersive X-ray spectrometer (EDS) and a wavelength-dispersive X-ray spectrometer (WDS) on some semiconductor materials are presented. CdTe, CdSe, CuInSez, ZnSe, and InSb standards were used to measure the k-ratios with pure element standards employing both types of X-ray spectrometers to demonstrate the ability of each to measure elemental compositions under various operating conditions. Both types of spectrometers were utilized on a Cameca MBX electron microprobe at identical X-ray take-off angles.The EDS spectrometer was found t o perform equal to the WDS spectrometer when integral peak-to-background ratios were greater than seven, when the X-ray line being measured was greater than about 1,000 eV, and when adjacent peaks were separated by more than three times the detector energy resolution.