We assessed factory-calibrated field-portable X-ray fluorescence (pXRF) data quality for use with minimally-prepared aquatic sediments, including the precision of replicate pXRF measurements, accuracy of factory-calibrated pXRF values as compared to total digestion/ICP-OES concentrations, and comparability of calibrated pXRF values to extractable concentrations. Data quality levels for precision, accuracy, and comparability were not equivalent for element/analyzer combinations. All analyses of elements that were assessed for precision and accuracy on a single analyzer were both precise (<10% relative standard deviation) and accurate (r2>0.85) for K, Ca, Ti, Mn, Fe, and Zn. Calibrated pXRF values for Al, K, Ca, Ti, Mn, Fe, Cu, Zn, and Pb were within ∼10% relative difference of total digestion/ICP-OES concentrations. Calibrated pXRF values for Fe, Cu, Zn, As, and Pb were within ∼20% relative difference of extractable concentrations. Some elements had a higher level of data quality using specific analyzers, but in general, no pXRF analyzer had the highest level of data quality in all categories. Collectively, our data indicate that a wide range of factory-calibrated pXRF units are capable of providing high-quality total concentrations for the analysis of aquatic sediments.
Separating the timing and effects of multiple watershed disturbances is critical to a comprehensive understanding of lakes, which is required to effectively manage lacustrine systems that may be experiencing adverse water quality changes. Advances in X-ray fluorescence (XRF) technology has led to the availability of high-resolution, high-quality bulk geochemical data for aquatic sediments, which in combination with carbon, nitrogen, δ13C, and δ15N have the potential to identify watershed-scale disturbance in lake sediment cores. We integrated documented anthropogenic disturbances and changes in bulk geochemical parameters at 8 lakes within the Halifax Regional Municipality (HRM), Nova Scotia, Canada, 6 of which serve as drinking water sources. These data reflect more than 2 centuries of anthropogenic disturbance in the HRM that included deforestation, urbanization and related development, and water-level change. Deforestation activity was documented at Lake Major and Pockwock Lake by large increases in Ti, Zr, K, and Rb (50–300%), and moderate increases in C/N (>10%). Urbanization was resolved at Lake Fletcher, Lake Lemont, and First Lake by increases in Ti, Zr, K, and Rb (10–300%), decreases in C/N (>10%), and increases in δ15N (>2.0‰). These data broadly agree with previous paleolimnological bioproxy data, in some cases identifying disturbances that were not previously identified. Collectively these data suggest that bulk geochemical parameters and lake sediment archives are a useful method for lake managers to identify causal mechanisms for possible water quality changes resulting from watershed-scale disturbance.