A laboratory X-ray emission spectrometer for phosphorus Kα and Kβ study of air-sensitive samples
A laboratory X-ray emission spectrometer for phosphorus Kα and Kβ study of air-sensitive samples
复制标题
实验室 X 射线发射光谱仪，用于空气敏感样品的磷 Kα 和 Kβ 研究
DOI：
10.1039/d3ja00053b
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发表时间：
2023
影响因子：
3.4
通讯作者：
Seidler, Gerald T.
中科院分区：
文献类型：
--
作者：
Abramson, Jared E.;Holden, William M.;Rivera-Maldonado, Ricardo A.;Velian, Alexandra;Cossairt, Brandi M.;Seidler, Gerald T.
含磷材料的分析化学通常受到以下因素的阻碍：31P NMR光谱法所需的长测量时间和相对大的样品质量，在PK边缘的能量范围内操作的同步加速器光束线的稀缺性和访问限制，液体萃取期间物种相互转化带来的挑战，以及许多含磷材料和纳米相典型的相当大的空气敏感性。为此，我们报告了一种新的实验室光谱仪的设计和操作，该光谱仪可以同时进行PK α和Kβ X射线发射光谱（XES），同时安装在研究级可控气氛手套箱中。对磷化镍纳米相的示范研究说明了无空气XES的重要性以及同时Kα和Kβ光谱在识别P氧化态和研究纳米尺度对价态电子结构的影响方面的价值。
The analytical chemistry of phosphorus-containing materials is often impeded by the long measurement times and relatively large sample masses needed for 31P NMR spectroscopy, by the scarcity and access limitations of synchrotron beamlines operating in the energy range of the P K-edge, by the challenges posed by species interconversion during liquid extraction, and by the considerable air-sensitivity typical of many phosphorus-containing materials and nanophases. To this end, we report the design and operation of a new laboratory-based spectrometer to simultaneously perform P Kα and Kβ X-ray emission spectroscopy (XES) while being housed in a research-grade controlled-atmosphere glovebox. Demonstration studies on nickel phosphide nanophases illustrate the importance of air-free XES and the value of simultaneous Kα and Kβ spectroscopy for identifying the P oxidation state and for investigating nanoscale influences on valence level electronic structures.