The dataset documents results from portable X-ray fluorescence (pXRF) analysis conducted on a suite of sediment samples from U.S. Army Base Fort Drum, Jefferson County, New York. Most of the pXRF samples were collected from representative cells in a series of five portable optically stimulated luminescence (OSL) grids, here denoted G1 through G5, to constrain variations in grain size within the grids. These samples were also collected in conjunction with OSL for absolute chronology. In the lab, pXRF analysis was conducted using a Bruker S1 Titan instrument housed in the Bascom Laser Diffraction Sedimentology Laboratory at the U.S. Geological Survey in Reston, Virginia. Most of these samples were previously analyzed for particle size, and subsamples from G3 and G4 were also analyzed for elemental concentrations via inductively coupled plasma - mass spectrometry (ICP-MS). This work is a collaboration with the Fort Drum Environmental Division and the Fort Drum Cultural Resources Division and was funded by the National Cooperative Geologic Mapping Program.