WANG Jingfeng, ZHOU Huarong, KONG Junjie, XIE Wanwen WANG Dexin, REN Mande, SONG Fuxi, ZHANG Haiming
Vanadium shale is a dominant vanadium resource in China, and vanadium extraction from shale represents an important approach for the development and utilization of domestic vanadium resources. Therefore, it is urgent to establish a method for the rapid and accurate determination of various elements in vanadium shale. In this tudy, sodium peroxide was used as the flux, and the sample was fused in an alumina crucible at 720 ℃ for 15 min. The addition of 15 mL nitric acid during leaching could effectively extract the target elements in the sample. The analytical lines of V 290.882 nm, P 177.495 nm, Cu 324.754 nm, Cd 226.502 nm, Ni 231.604 nm and Mo 204.598 nm were selected for vanadium, phosphorus, copper, cadmium, nickel and molybdenum, respectively. Accordingly, a method for the determination of vanadium, phosphorus, copper, cadmium, nickel and molybdenum in vanadium shale by alkali fusion-inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The linear correlation coefficients (r) of calibration curves for all elements were greater than 0.999. The limits of detection for the elements in this method ranged from 0.000 2% to 0.001 1% (mass fraction). The contents of vanadium, phosphorus, copper, cadmium, nickel and molybdenum in certified reference material GBW07876 of stone coal vanadium ore was determined according to the experimental method, and the results were consistent with the certified values. The proposed method was applied to the determination of vanadium, phosphorus, copper, cadmium, nickel and molybdenum in actual vanadium shale samples. The relative standard deviations (RSD,n=11) of determination results were between 0.01% and 5.2%. The measured values were compared with those obtained by X-ray fluorescence spectrometry and ammonium ferrous sulfate titration, and the results were satisfactory.
