PNNL

Abstract

Mixed-acid digestion is a method often used for the determination of elemental analysis of sediment samples. It is crucial that efficiency details associated with the digestion method be well understood on an element by element basis. Battelle’s Marine Sciences Laboratory Standard Operating Procedure for Sediment Mixed-Acid Digestions was modified to identify conditions which produce optimal recovery of elements. The parameters that were adjusted for testing were mass of sediment, mixed-acid volume, mixed-acid composition and digestion time. Digestion involves treatment of the sediment sample with mixed-acid mixtures at 135º C ± 10º in a Teflon® digestion bomb. Typical analytical methods include Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) and Inductively Coupled Plasma – Mass Spectrometry (ICP-MS). Initial experiments involved determining the optimal ratio of acid volume to mass of sediment. Experiments were designed to identify the point at which insufficient acid was used to effectively digest a given mass of sediment. When the mass of sediment was varied between 0.2 and 1.0 gram using a 4 mL aqua regia acid mixture (3 mL hydrochloric acid and 1 mL nitric acid), there was no effect on the recovery of the elements Al, Ba, Ca, Co, Cr, Cu, Fe, Mg, Mn, Ni, Pb, Sr, Ti, V, and Zn. The next experiments focused on a time study to resolve the shortest digestive time for optimal elemental recovery. Two masses of sediment were investigated, 0.25 and 0.7 g, again utilizing aqua regia digestion (4 mL). Maximum recovery was reached after 4 hours of digestion; additional digestion time released no or only minimal amounts of elements from the sediments. The final set of experiments was designed to identify optimal conditions for the total digestion of sediment using a mixture of hydrochloric acid, nitric acid, hydrofluoric acid, hydrogen peroxide, and boric acid. These experiments were designed to determine the optimal volume of hydrofluoric acid needed to achieve a total digestion. Utilizing two masses of sediment 0.25 and 0.5 g and varying the volume of hydrofluoric acid and boric acid. Total digestion was achieved with a minimum volume of 0.5 mL hydrofluoric acid and a .25 g of sediment. Future experiments incorporating the findings in these experiments will be executed using a heated carbon block as the source for thermal energy.