Synthesis of molybdenite reference materials for in situ molybdenum and sulfur isotope measurement using laser ablation MC-ICP-MS

Analyzing sulfur (S) and molybdenum (Mo) isotope ratios in molybdenite, the most common sulfide mineral, is crucial for studying the genesis of ore deposits. However, it is necessary to prepare matrix-matched reference materials for molybdenite. In this study, we employed two different techniques, the high-temperature-high-pressure (HTHP) technique and the rapid hot-pressing technique, to synthesize molybdenites and assessed their suitability as reference materials for in situ Mo and S isotope analysis in molybdenite. The molybdenites synthesized through HTHP and rapid hot-pressing exhibit smooth surfaces and dense structures, making them suitable as reference materials for in situ Mo and S isotope analysis, respectively. These synthesized molybdenites exhibit homogeneous Mo and S isotope compositions based on a large number of LA-MC-ICP-MS measurements. The mean δ⁹⁸Mo_{NIST SRM 3134} values of 0.70 ± 0.06‰ (n = 4, 2SD) and 0.70 ± 0.05‰ (n = 4, 2SD) determined by solution nebulization MC-ICP-MS are suggested as recommended δ⁹⁸Mo/⁹⁵Mo values for Mo-H8 and Mo-P. The mean δ³⁴S_V-CDT value of −0.22 ± 0.10‰ (n = 9, 2SD) determined by elemental analyzer isotope ratio mass spectrometry (EA-IRMS) is suggested as a recommended δ³⁴S/³²S value for Mo-H8 and Mo-P. Therefore, we recommend combining ultrafine powders with a high-temperature–high-pressure technique and/or a rapid hot-pressing technique to synthesize reference materials for isotopic analysis of other minerals.