The effects of watershed-scale experimental acidification on the macronutrient content and decomposition of sugar maple ( Acer saccharum Marsh) leaves were investigated. Bear Brook Watershed in Maine (BBWM) is a paired forest watershed study where the West Bear (WB) watershed has been treated bi-monthly with 1800 eq ha −1 yr −1 of (NH 4) 2SO 4 since 1989, and the adjacent East Bear (EB) watershed has acted as a reference. Leaf samples collected from the treated WB watershed had significantly higher concentrations of N and P than leaves from the reference EB watershed. Leaves from both watersheds were decomposed for a 10-day laboratory incubation. Extractable total soluble carbon (C TS) content of the leaves decreased following decomposition to a greater extent in WB leaves than in EB leaves. Spectroscopic and chromatographic chemical analyses indicated similar chemical properties for the fresh WB and EB WEOM. However, after decomposition, the WB WEOM was more humified as compared to EB WEOM indicating that the watershed treatment resulted in leaves which were more biodegradable than those in the reference watershed. Multi-dimensional fluorescence spectroscopy with parallel factor analysis (PARAFAC) modeled five components: tyrosine-like, three humic substance-like, and terrestrial/anthropogenic associated-like fluorophores. Following decomposition, the relative concentrations of two of the humic-associated components increased to a significantly greater extent for WB than for EB WEOM. These observations were consistent with greater decomposition-related changes to the WEOM from WB samples relative to EB samples. Pearson correlation analysis showed that foliar N and P concentrations were positively correlated with indices of humification. Adsorption of WEOM to goethite and gibbsite was significantly greater for decomposed WB WEOM than EB WEOM. These results demonstrate that greater leaf N and P contents can increase short-term decomposition, accelerate production of more humic-like WEOM, and thereby potentially influence the distribution of organic matter within the soil carbon pool.