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Over the past 20 years, many designer drugs derived from controlled substances have been widely distributed as easily available psychoactive substances and have become a serious problem in Japan. In order to determine the absolute structures of four new designer drugs derived from medicines (methylphenidate and phenmetrazine) X-ray single-crystal structure analyses were performed using the BL26B1 beamline of synchrotron radiation facility SPring-8. The results show that the molecular configuration of these designer drugs (having two asymmetric carbons), which were distributed in the illegal drug market had threo-forms as found for methylphenidate and phenmetrazine.
In order to exploit X-ray powder spectro-diffractometry, the program RIETAN-97ß for refining crystal structure and lattice parameters by the Rietveld method was modified extensively. The resulting software can be used to refine anomalous scattering factors, fr and fi, for specified crystallographic sites near the X-ray absorption edge of a particular element. The effectiveness of the modified software was tested by using powder diffraction patterns simulated by the original RIETAN-97ß software and a series of measured powder diffraction patterns of Fe3O4 with incident X-ray energies near the absorption edge of iron.
Oxygen K-V (Kα) X-ray fluorescence spectra of MgO, Cu2O, CuO, La2CuO4, La2-xSrxCuO4, YBa2Cu3O7-x , and GdBa2Cu3O7-x are measured. The local (oxygen) and partial (2p) electron density of states (DOS) of these compounds are calculated by the cluster approximation with the discrete variational (DV) Hartree-Fock-Slater (Xα) method. The calculated O 2p DOS are compared with the measured X-ray fluorescence spectra. It is found that the measured 0 K-V X-ray fluorescence line shapes are well reproduced by the O 2p DOS calculated by a cluster including the second nearest neighbor atoms (oxygen atoms) in the solids. This indicates that the oxygen K-V X-ray emission spectra reflect the oxygen-oxygen orbital hybridization in the solid as well as the oxygen-metal orbital hybridization.
Near-surface-layer analysis by x-ray fluorescence critical takeoff-angle detection was examined theoretically and experimentally. The takeoff-angle dependence of Cr K-L x-ray fluorescence from Cr thin films was measured with practical analyzed depth varying from several thousand to less than one hundred angstroms. Comparison of Cr K-L and K-M takeoff-angle dependence shows the analyzed depth depends on the observed x-ray energy even with identical takeoff angles. The potential of nondestructive depth profiling is also discussed.
A synchrotron radiation X-ray micro analyzer(SRXMA) was developed at Photon Factory in Japan. The present SRXMA combines a double crystal monochromator and mirror optics and either a white or a monochromatic microbeam can be used. Micro X-ray fluorescence analysis was carried out, and a minimum detection limit of 1 ppm for Mn was obtained for 100 sec measurement with the white beam. With monochromatic beam excitation, micro X-ray spectroscopies are now feasible.
The obtained beam size was 1.6 μ;m - 34 μm* The beam was blurred in one direction by the scattered X-rays caused by the surface irregularities of the focusing mirror. Improvements in the mirror quality will ensure a beam spot of just a few microns with sufficient intensity.
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