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An interlaboratory comparison has been undertaken of X-ray and photoluminescence measurements of InGaAsP on InP. Six 1 cm2 specimens were measured, with nominal photoluminescence wavelengths of 1.1, 1.3 and 1.5 μm (2 of each). Preliminary maps of the specimens by X-ray and photo luminescence showed relatively large degrees of nonuniformity. This specimen nonuniformity appears to have dominated the variation in the X-ray measurements, making the results more sensitive to beam positioning and peak identification than to other instrument and/or measurement differences. The photoluminescence uniformity was sufficient to allow the variation between measurements by different instruments to be assessed. Offsets between measurements from different instruments were observed, and potential causes, such as pump wavelength, wavelength calibration, sample temperature, pump power density, and peak identification were identified.