The use of field portable X-ray fluorescence (XRF) spectrometry as a quantification tool for gypsum content in soils of West Texas and southern New Mexico, USA, was evaluated. Six sites were evaluated with gypsum contents ranging from less than 10% to greater than 90%. Samples collected from each site were scanned in the field using XRF and then transported to the laboratory for additional XRF scanning. Variables that might affect XRF scanning results, such as scanning time, particle size, moisture content, and so on, were evaluated. Both gypsum (CaSO4 • 2H2O) and calcite (CaCO 3) were quantified using standard laboratory techniques. Three data sets were compared: (1) soil characterization data, obtained from the National Soil Survey Laboratory Research Database in Lincoln, NE; (2) quantitative X-ray diffraction; and (3) portable XRF (PXRF). The best correlation of gypsum XRF data (via Ca quantification minus calcite content) and laboratory data was between PXRF and quantitative X-ray diffraction (R = 0.96). On average, PXRF provided results within 6% of soil characterization data, the current laboratory standard for gypsum quantification. Field PXRF shows considerable promise as a rapid, quantifiable measure of gypsum in soils.