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Here we evaluate measurement procedures currently used for the combined determination of highly siderophile element concentrations (HSEs: Re, Ir, Os, Ru, Pt and Pd) and Os isotope ratios in geological samples by isotope dilution mass spectrometry (ID-MS) applying high-temperature sample digestion using inverse aqua regia in closed glass vessels, such as Carius tubes or a high-pressure asher system (HPA). In particular, we address the question of whether an additional hydrofluoric acid dissolution step is required to release HSEs hosted in the silicate portions of rock samples. To do so, we conducted systematic experiments for basaltic (TDB-1 and BIR-1), ultramafic (UB-N and JP-1) and sedimentary (SCo-1, SDO-1 and JCh-1) reference materials with and without HF desilicification. Through the extensive tests on TDB-1—varying apparatus (microwave, Carius tube, high-pressure asher), conditions …