U-Pb laser ablation–multicollector–inductively coupled plasma–mass spectrometry (LA-MC-ICP-MS) ages have been determined from large zircon crystals separated from pegmatites of the Adirondack Mountains, New York. Emplacement and metamorphic ages ranging from 949 \textpm 10 to 1222 \textpm 12 Ma help constrain the timing of igneous, metamorphic, and deformational history of the region, and are associated with Shawinigan, Ottawan, and Rigolet orogenesis. Geologically reasonable ages were obtained from most zircon separates despite large size, a limited number of grains, high uranium and thorium contents, dark and opaque interiors, high density of fractures, and widespread areas of metamictization and Pb loss. However, few grains show zoning or differences in composition when viewed with the backscattered mode on the scanning electron microscope. Large, clear, internally featureless, U-poor grains yield the best constrained ages. U-Th-Pb monazite ages, determined by electron probe, vary from 874 \textpm 27 Ma to 297 \textpm 62; the younger age may reflect the timing of hydrothermal fluid infiltration related to late Acadian events. This study suggests that, with appropriate care, zircons from pegmatites are a reasonable target for LA-MC-ICP-MS geochronology, widening the current arsenal of sampling targets.