A cell for combined UV-visible and x-ray absorption spectroscopy studies under low-temperature and air exclusion conditions

摘要

A measuring system that integrates a low-temperature optical cell UV-visible (UV-Vis) for air exclusion experiments with a liquid x-ray absorption spectroscopy (XAS) cell (x-ray absorption near-edge spectroscopy and extended x-ray absorption fine structure) is reported here together with its application in studies of organometallic complexes. UV-Vis measurements are performed in a three-compartment glass vessel, fitted with an external fiber optics probe. This UV-Vis cell is suitable for the measurement of oxygen- and air-sensitive compounds at variable temperatures (RT to -78℃). The liquid XAS cell is filled with the UV-Vis solution at low temperature and can be used in both fluorescence- or transmission-mode measurements with (frozen) solutions. The complete measuring system is reusable and easy to clean and handle. To test the performance of these cells the oxygenation behavior of a dinuclear organometallic copper(I) complex was studied in acetone by UV-Vis and XAS. It is shown that direct correlation of low-temperature UV-Vis and XAS data is possible in organic solvents.