Biotic and abiotic factors both play critical roles in the cycling of organic matter and nutrients in aquatic ecosystems. Understanding the relative control of these factors on solute fate and transport in fluvial systems is important for understanding how climatic changes can affect water quality. Many processes that control solute cycling in streams occur at sub-daily scales, making high-frequency, in situ, sub-hourly measurements important for capturing the response of dissolved organic matter and nutrients to changes in the strength of controlling processes. The tightly coupled aquatic and terrestrial environments present in headwater streams make them particularly useful systems for studying high-frequency changes in water chemistry. In this study, we examined the patterns of dissolved organic carbon, nitrate, dissolved oxygen, temperature, dissolved organic matter fluorescence, and stream discharge using in-stream measurements at sub-hourly to monthly time scales to understand the daily and seasonal controls of aquatic organic matter and nutrient processing. We also conducted a laboratory incubation to measure the effects of dissolved organic carbon and nutrient treatments on consumption of carbon and nitrogen in our system. Our main objectives were to identify: 1) the relative controls of diel biotic and abiotic processes on stream dissolved organic carbon and nitrate-N; and 2) the mechanisms controlling rapid autumnal changes in dissolved organic carbon and nitrate-N in stream runoff. We found that hydrology plays a key role in transporting solutes to a forested headwater stream in the Piedmont Region, Maryland; however, once solutes reach the stream biotic controls dominate the stream solute patterns. Biology is an important regulator of diel patterns of streamwater dissolved organic carbon and nitrate concentrations during springtime and autumn leaf fall. Diel cycling is most apparent during the spring prior to leaf out when the water temperature is increasing. Where patterns were evident, nitrate (annual average in second order stream: 17:00) and discharge (17:28) reached their minimums during the afternoon within a few hours of the peaks in dissolved oxygen (13:16), temperature (15:17), dissolved organic carbon (16:06), and dissolved organic matter fluorescence (17:23). Larger amplitudes of dissolved oxygen, nitrate, dissolved organic carbon, and dissolved organic matter fluorescence correspond with larger daily temperature changes. Laboratory incubations showed increased consumption of nitrogen in the presence of labile carbon, but not in the presence of labile carbon plus nutrients, which indicates our system is carbon limited. Autumn dissolved organic carbon and nitrate dynamics also indicate our system is carbon limited. Increased rates of leaf litter fall corresponded with increased consumption of stream nitrate leading to a late October depression, or annual minimum, in nitrate concentration. Storm events accelerated the recovery of stream nitrate to early autumn concentrations as nitrate was mobilized and transported from soils to the stream. Hydrology is important for solute transport to and export from the stream. Autotrophic activity dominates on the daily scale, while heterotrophic activity controls seasonal responses in organic matter and nutrient cycling in this forested watershed. Carbon and nitrogen dynamics have been studied in other forested systems, as well, but the controlling processes vary among these watershed. Our results highlight the importance of understanding controlling processes within specific watersheds when making large scale predictions of the potential export of carbon and nitrogen from forested systems.