A novel, high yield (91 ± 5%) photochemical vapor generation (PVG) method is reported for Os, achieved via photo-reduction reactions in a 1% CH₃COOH medium containing 50 mg L⁻¹ Fe^3/2+. A sample flow rate of 2 mL min⁻¹ delivered to a flow-through photoreactor provided a 21 s irradiation time prior to passage of the volatile product to an inductively coupled plasma mass spectrometer for detection at m/z 192. A method detection limit of 0.16 pg mL⁻¹ was achieved, a 10-fold enhancement over that obtained using parallel photo-oxidation synthesis of OsO₄ from a 5% HNO₃ medium. Precision of replicate measurement was 4% (RSD) at 10 ng mL⁻¹. Although the identity of the product has not yet been ascertained by GC-MS, based on the chemistry of Os and the reaction conditions, as well as its difference in volatility from OsO₄, a carbonyl or alkyl-substituted carbonyl is suspected e.g., Os_w(CO)_x(CH₃)_yH_z.

中文翻译：

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锇的高效光还原蒸汽发生

报道了一种用于 Os 的新型高产率 (91 ± 5%) 光化学蒸汽发生 (PVG) 方法，该方法通过在含有 50 mg L ^-1 Fe ^3/2+的 1% CH ₃ COOH 介质中的光还原反应实现。输送到流通式光反应器的样品流速为 2 mL min ^-1，在挥发性产物通过电感耦合等离子体质谱仪以在m / z 192处检测之前提供了 21 秒的辐照时间。实现了0.16 pg mL ^-1，比使用5% HNO ₃的 OsO ₄平行光氧化合成获得的性能提高了 10 倍中等的。在 10 ng mL ^{-1 时}，重复测量的精度为 4% (RSD) 。尽管尚未通过 GC-MS 确定产物的身份，但基于 Os 的化学性质和反应条件，以及其与 OsO _{4 的}挥发性差异，怀疑是羰基或烷基取代的羰基，例如Os _w (CO) _x (CH ₃ ) _y H _z。