Comparison of Three Aqua Regia Digestion Methods for Twenty Florida Soils

It is important to evaluate different digestion methods to accurately determine elemental concentrations in soils. Three commonly used digestion procedures, hotplate aqua regia, microwave aqua regia, and microwave aqua regia + HF, were compared for digestion of three standard reference materials (SRMs 2704, 2709, and 2711) and 20 Florida soils (three groups of Quartzipsammemts, one group of Alaquods, and one group of Paleudults). Sixteen elements (Al, Ba, Ca, Fe, K, Mg, Mn, P, Zn, As, Cd, Cr, Cu, Ni, Pb, and Se) were analyzed using either an inductively coupled plasma optical emission spectrometer (ICP‐OES) or a graphite furnace atomic absorption spectrophotometer (GFAAS). Precise analysis was achieved for all elements except As (1.0–25%), Cd (1.8–22%), and Se (4.1–22%) in the SRMs using all three procedures, with the microwave aqua regia + HF procedure having slightly better precision (3.7%) averaged across all elements. Compared with the elemental recoveries in SRMs by the microwave aqua regia digestion (80%), microwave aqua regia + HF digestion achieved greater accuracy (94%), whereas the hotplate aqua regia digestion achieved less accuracy (74%). In general, the microwave aqua regia + HF digestion was overall the best procedure for determining concentrations of most metals in SRMs and Florida soils, followed by the microwave aqua regia and the hotplate aqua regia digestion. However, this so‐called total–total digestion procedure (microwave aqua regia + HF) may underestimate total Pb concentration in Florida soils and total Al, Ca, Fe, Mg, and Ba concentrations in the Florida Paleudults.