X-ray L. beta. emission spectrum of Ru in Ru(NH)Cl

One of the broader applications of synchrotron radiation has been to EXAFS studies for material structure determination, i.e., for an analysis of x-ray absorption over an extended energy region beyond a core ionization limit. Studies of the near edge structure (XANES) give a different type of information, characteristic of the local symmetry and electronic configuration of the absorbing atom. This type of information is reflected also in the x-ray emission spectra, in particular for transitions involving the valence levels. Examination of the near edge absorption or the emission spectrum does not require an instrument capable of scanning a wide energy range with high counting statistics, as does EXAFS; the needs are rather for good resolution and a reliable calibration of the energy scale. Some of the problems of near edge spectra were particularly evident in our investigation of Ru-L..beta../sub 2/ /sub 15/ emission from Ru(NH/sub 3/)/sub 6/Cl/sub 3/. The Ru-L..beta../sub 2/ /sub 15/ emission was measured with a laboratory Rowland circle x-ray spectrometer with a curved quartz (1010) crystal (radius = 22 inches) in a fixed position appropriate to the energy range, and a position sensitive detector which can be positioned along the Rowland circle. The Ru spectrum was excitedmore » mainly by Sn-L/sub ..cap alpha../ primary radiation from a Sn anode in a demountable x-ray tube operating at 13 kV and 120 mA. The resolution of the instrument in this region is 1.5 eV. An accurate calibration of the energy scale was conveniently obtained by measuring a reference x-ray emission line in the same instrumental configuration. In the present case the Pd-L/sub ..cap alpha../ emission line at 2838 eV was used to establish the energy scale. The energy dispersion of the instrument was determined from the Cl-K/sub ..beta../ emission spectrum of CH/sub 3/Cl between 2810 eV and 2830 eV and Pd-L..cap alpha../sub 1/ /sub 2/ and extrapolated to the energy region of the recorded emission spectrum. 6 references, 1 figure.« less