Particulate samples were collected using McLane in situ pumps (P. Lam, UCSC) at various depths (Bishop et al., 2012), with splits (ca. 1/16 section) from a 0.8 µm Supor filter processed and immediately frozen for storage and return to the ODU Lab. The volume of water that passed through each filter was recorded by the pumps.
Water column particulate filters were solubilized using the nitric-perchloric acid reflux digestion procedure described by Cutter (1985) but using a microwave digestion unit. The digestion solutions were analyzed using selective hydride generation, liquid nitrogen-cooled trapping, and then revolatilization and determination with gas chromatography/photoionization detection (Cutter et al., 1991). Calibration performed daily via the standard additions method, with a minimum of 4 additions of AsV. The slope from the linear fit to these data was then applied to all samples for that day. The detection limit for total particulate As, assuming an average filtration volume of 24 liters, was 0.0001 nmol/L (3s, n=24), with an accuracy of 87±14 % recovery of the BCR 277R estuarine sediment standard reference material and a precision of 10.5% (RSD) at 0.0001 nmol/L.