- Dissolved organic matter (DOM) is a critical component of the carbon cycle linking terrestrial and aquatic ecosystems. Although many factors influence DOM fluxes and quality in rivers, controls on DOM compositions in catchments of the western U.S. are poorly understood. UV and fluorescent spectroscopy is a simpler, faster, and less expensive DOM fingerprinting technique compared to techniques, such as nuclear magnetic resonance (NMR) spectroscopy or wet chemical fractionation, and could be useful for characterizing complex DOM chemistry. However, only 1 % of DOM is estimated to be fluorescent, and the utility of UV and fluorescent spectroscopy for DOM characterization needs to be further investigated. This dissertation applied UV and fluorescent spectroscopy to examine hydrologic and land cover controls on DOM chemistry in streams of 45 catchments in the forested headwaters and a mixed landscape of the Willamette River Basin, Oregon, based on two years of monitoring. This dissertation contributes three major findings. First, freezing of water alters DOM chemistry by preferentially precipitating aromatic DOM. Second, UV and fluorescent spectroscopy was able to discriminate DOM delivered from highly processed, protein-rich deep subsurface sources during dry seasons especially in forested headwater streams of the H. J. Andrews Experimental Forest (HJA), where nitrogen inputs are very low. In addition, fluorescent DOM chemistry differed among watersheds with varying forest management history. Third, although fluorescent DOM in a headwater forested system differed among land use history, fluorescent DOM composition did not vary among streams draining a well-mixed landscape of urban, pasture/hay, forest, and agricultural land cover types in the central Willamette River Basin, where nitrogen inputs to streams are relatively high. Dissolved organic carbon (DOC) concentration decreased and the fluorescent index indicated an increase in terrestrial sources of DOM from small (1st and 2nd order) to large (4th to 6th order) streams. A protein-like DOM component that was detected in the headwater forested study site (HJA) was not detected in stream samples from the middle basin study site. These findings indicate that in-stream respiration, fueled by nutrient additions from agriculture runoff, consumes bioavailable, labile DOM (proteins) preferentially relative to more recalcitrant, terrestrial sources of DOM along water flow paths from headwater streams to major rivers. This study shows the clear applicability of the fluorescent characterization of DOM in identifying hydrologic and landscape controls as well as varying DOM chemistry and functions throughout watershed ecosystems.