1. Shenzhen Entry-exit Inspection and Quarantine Bureau, Shenzhen 518067, China; 2. Chinese Research Academy of Environmental Sciences, Beijing 100012,China; 3. Fangchenggang Entry-exit Inspection and Quarantine Bureau, Fangchenggang 538001, China
Abstract：During the determination of ZnO content in crude zinc oxide by semiquantitative X-ray fluorescence spectrometry (XRF) or chemical analysis method, the determination results were usually higher due to the presence of non-ZnO phases such as Zn and ZnFe2O4. As a result, some prohibited solid wastes were imported into China. Two types of crude zinc oxide samples were selected for analysis. The content of ZnO was firstly determined by semiquantitative XRF method, and then the quantitative phase analysis was conducted by X-ray diffraction (XRD) and Rietveld full spectrum fitting. Based on the scattering information of whole diffraction space, the Rietveld full spectrum fitting of experimental digital diffraction spectrum was conducted using several models with different physical meanings. In fitting process, the parameters in model were continuously adjusted using linear least square fitting algorithm to obtain the theoretical spectral lines which were consistent with the actual lines (the residual variance factor of weighted graph of Rwp＜10%). Finally the content of composition phases in sample could be obtained. Certain amount of ZnO was added into crude zinc oxide sample for the Rietveld full spectrum fitting analysis according to the proposed method, and the difference of results was less than 5.0%. The results showed that the obtained crystal structure parameters of common phases in crude zinc oxide by proposed method were very close to those reported in the literature. The accurate determination of ZnO content was realized. The proposed method could be used for the inspection supervision and property identification of imported crude zinc oxide.
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