Analysis of copper, zinc, arsenic, lead, chromium, cobalt, nickel, mercury, thallium, selenium, silver, antimony, cadmium, tin, and barium was performed on soils and other particle matrices using two field-portable high-resolution X-ray fluorescence spectrometers (XRF). Quantitative determinations were based on fundamental parameter analysis and a second method that relies on analyte response factors and uses the Compton K a incoherent backscatter peak for matrix normalization. These two methods of instrumental analysis require only a few reference materials and are relatively insensitive to sample matrix composition. This study assessed the capability of these two rapid XRF analysis methods by determining metal concentrations in reference materials, field samples, and laboratory spiked soils. With the exception of nickel, cobalt, and chromium, concentrations within 50% of the expected values were consistently obtained at and below 1000 mg/g.