Low Blank Isotope Ratio Measurements of Rhenium, Osmium, and Platinum Using Tantalum Filaments with Negative Thermal Ionization Mass Spectrometry

摘要

Platinum is most commonly used as a filament for Re and Os isotopic measurements, but it contains impurities of Re and Os. Tantalum is low in platinum group elements (PGE) and in Re, but it is not used for negative thermal ionization mass spectrometry because of high electron emission and high reactivity with O↓(2). High thermal electron emission from Ta distorts the preoptimized ion source optics. In addition, Ta consumes O↓(2), leaving little for samples, but O↓(2) is essential for isotopic ratio measurements of PGE and Re as they are measured as negatively charged oxides, such as OsO↓(3)↑(-) and PtO↓(2) ↑(-). These problems are solved by prebaking a filament to remove tantalum oxides before sample loading, keeping relatively high filament temperatures and high O↓(2) pressures (P↓[o↓(2))] during the sample run, and lowering the potential difference between the filament and the draw-out plate. At P↓[o↓(2)] of ~1× 10↑(-5) Torr in the source, strong (> 10 V) stable (>6 h) peaks of ReO↓(4) ↑(-), OsO↓(3)↑(-), and PtO↓(2)↑(-) are obtained at 750°C for Re, 850 °C for Pt, and over 900°C for Os. Accurate isotopic ratio measurements of Re, Os, and Pt at picogram levels are possible using Ta filaments.