Application of microwave digestion for complete dissolution of igneous silicate rock samples: A simple and quick...

In the area of geochemical analyses of rock solutions, achieving a complete sample dissolution is a fundamental prerequisite for obtaining accurate, precise and reliable analytical results. The challenge posed by the presence of resistant minerals such as zircon, rutile, corundum, spinel, tourmaline, beryl, chromite, and cassiterite in different silicate rocks is a well-recognized challenge in geological studies. These minerals, due to their resilient nature, demand additional efforts to ensure complete dissolution during sample preparation. The prevailing conventional sample digestion methods require several days of laboratory work and the handling of large amounts of multiple types of acids, which also increase sample blanks. Until recently, there was a widely held belief that microwave-assisted digestion, where microwave radiation is transformed to heat, faced limitations in achieving complete dissolution of refractory minerals. This prevailing opinion led to skepticism about the applicability of microwave-assisted digestion for sample preparation of e.g. igneous rock samples containing these minerals. This study introduces a novel, universal and quick closed-vessel (pressurized) high-temperature microwave-assisted digestion method appropriate for dissolution of all major types of igneous silicate rock samples, including rocks containing refractory minerals. This streamlined and expeditious procedure, comprising three steps, requires only a total time of ∼9 h. The method proves its versatility by successfully dissolving both, mafic igneous samples (e.g., basalt) with low-content of resistant minerals, and felsic igneous samples (e.g., granite) with relatively high-content of resistant minerals. To validate the reliability of this procedure, 36 trace elements were analyzed: Li, Be, Sc, V, Cr, Co, Ni, Cu, Zn, Ga, Rb, Sr, Y, Zr, Nb, Cs, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Hf, Ta, Pb, Th and U in several geological Certified Reference Materials (CRMs). The CRMs including basalts JB-3, BCR-2, BHVO-2; andesites JA-2, AGV-2; granodiorite GSP-2; granite JG-2 and alkaline granite MGL-OShBO, were digested and analyzed using triple quadrupole Inductively Coupled-Plasma-Mass Spectrometer (ICP-QQQ). The results of the analysis demonstrate remarkable consistency, closely aligning with both certified and literature values.