Studies have shown that the addition of P amendments to Pb and Zn contaminated soils reduces the bioavailability of these metals. At this time we are unsure if the source of P influences the efficiency and rate of reaction product formation. These limitations can be overcome by molecular scale studies that allow us to investigate redistribution/speciation of Pb and Zn upon addition of different P sources to contaminated soils. This research investigates the distribution and speciation of metal phosphates that are formed when different P amendments are added to a Pb and Zn contaminated soil. The P amendments included several granular forms: diammonium phosphate, triple superphosphate, and phosphate rock, along with 2 fluid forms: phosphoric acid and ammonium polyphosphate. A small amount of contaminated soil (approximately 25% gravimetric water content) was placed in plastic containers. The P materials were added and then covered with additional contaminated soil. Samples were allowed to incubate for 1 month in a moist condition after which the entire volume of soil was air-dried for 24 h and then impregnated with an epoxy resin. A second set was incubated for 1 year. Thin sections (maximum 30 μm thick) were prepared by cutting through the resin block perpendicular to the lines of P. Cuts were then mounted on polystyrene. XRF maps were collected to assess the redistribution of Pb and Zn in the samples due to P application and to select points of interest on which μ-EXAFS and μ-XRD analyses were conducted.