In cold humid temperate regions, peak nitrous oxide (N2O) fluxes from agricultural soils occur during spring freeze-thaw periods. Fall-applied manure that adds water-soluble nutrients to the soil prior to freeze-up could contribute to spring N2O emissions. The objective of our field experiment was to evaluate the relationship between water-soluble nutrients and N2O emissions during the spring freeze-thaw period in a sandy-loam soil with fall-applied manure and fall-sown cover crops in Québec, Canada. Dairy cattle manure (solid or liquid form) was applied in September, then 100% ryegrass (Lolium multiflorum Lam.) and 50% ryegrass and 50% hairy vetch (Vicia villosa Roth) were sown. In the following spring (March–April), soil N2O fluxes were measured in non-steady-state closed chambers, and soil samples were analyzed for soil reactive nitrogen (ammonium, NH4+ and nitrate NO3−), dissolved organic carbon and nitrogen, soil moisture (water-filled pore space), and denitrification activity. Spring N2O fluxes were not related to the fall-applied manure and cover crop treatments, possibly due to nitrogen transformations or loss from soil after manure application. The NH4+ concentration, water-filled pore space, and denitrification activity were significant predictors of soil N2O emissions during the spring freeze-thaw period, but only explained about 24% of the variation in these N2O emissions. This suggests that N2O was produced by biological processes such as nitrifier denitrification. N2O emission may be the result of stochastic diffusion processes through pores with ice-water mixtures, as well as through cracks that form during freezing-thawing processes. Therefore, water-soluble soil nutrients may be poor predictors of spring N2O emissions from manure-amended soils in our region.