Abstract:The contents of silicon and organic matters in black shale are relatively high. After burning carbon in muffle furnace at 750℃, the samples were digested by hydrochloric acid-hydrofluoric acid-nitric acid at 200℃ to release silicon tetrafluoride. P 213.618nm, Mg 285.213nm, Fe 259.940nm, Al 396.152nm, Ca 317.933nm, Mn 257.610nm and Ti 334.941nm were selected as the analytical lines. The hydrofluoric acid resistant sample injection system was used for the direct determination of phosphorus pentoxide, magnesium oxide, iron oxide, aluminum oxide, calcium oxide, manganese oxide and titanium dioxide. Thus the analysis method of phosphorus pentoxide, magnesium oxide, iron oxide, aluminum oxide, calcium oxide, manganese oxide and titanium dioxide in black shale of Kunyang phosphate mine in Yunnan by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. Under the optimum working conditions of the instrument, the linear correlation coefficients of calibration curves were all greater than 0.9996. The detection limits of the method were between 0.0012μg/g and 0.028μg/g. The proposed method was applied for the determination of phosphorus pentoxide, magnesium oxide, iron oxide, aluminum oxide, calcium oxide, manganese oxide and titanium dioxide in black shale sample of Kunyang phosphate mine in Yunnan. The relative standard deviations (RSD, n=11) of the results were between 0.29% and 1.5%, and the spiked recoveries were between 97% and 105%. The contents of phosphorus pentoxide, magnesium oxide, iron oxide, aluminum oxide, calcium oxide, manganese oxide and titanium dioxide in certified reference materials of sediment in Tibet region (GBW 07320, GBW 07328 and GBW 07331) were determined according to the experimental method. The found results were basically consistent with the certified values.
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