Rock magnetic studies of tuffs are essential to the interpretation of paleomagnetic data derived from such rocks, provide a basis for interpretation of aeromagnetic data over volcanic terranes, and yield insights into the depositional and cooling histories of ash flow sheets. A rhyolitic ash flow sheet, the Miocene-aged Tiva Canyon Member of the Paintbrush Tuff, contains both titanomagnetite phenocrysts, present in the magma prior to eruption, and cubic Fe-oxide microcrystals that grew after emplacement. Systematic variations in the quantity and magnetic grain size of the microcrystals produce large variations in magnetic properties through a section of the ash flow sheet penetrated in a borehole on the Nevada Test Site. Natural remanent magnetization varies from less than 1 × 10⁻⁴ to more than 8 × 10⁻⁴ A m³ kg⁻¹, and in-phase magnetic susceptibility varies from less than 1 × 10⁻⁶ to more than 10 × 10⁻⁶ m³ kg⁻¹. The microcrystals, which include both magnetite and maghemite, have Curie points and maximum unblocking temperatures between 580°C and 640°C. Rock magnetic data, including in-phase and quadrature magnetic susceptibilities as well as hysteresis parameters, demonstrate that these microcrystals are of superparamagnetic and single-domain sizes. Titanomagnetite phenocrysts are the dominant remanence carriers in the central 50 m of the section, whereas microcrystals are important contributors to remanent magnetization and magnetic susceptibility in two 15-m-thick zones at the top and bottom. Within these zones the size of microcrystals decreases both toward the quenched margins and toward the interior of the sheet. The decrease in microcrystal size toward the interior of the sheet is interpreted to indicate the presence of a cooling break; possibly represented by a concentration of pumice. Laboratory heating produces changes in magnetic properties which vary complexly from sample to sample. Such changes include (1) decrease in saturation magnetization, (2) both increase and decrease in in-phase and quadrature magnetic susceptibilities, and (3) shifts in coercivity spectra. The complex sample-to-sample variation in response to heating is attributed to differences in initial grain-size distributions.