Determination of vanadium and tungsten in waste vanadium-titanium-based denitration catalyst by inductively coupled plasma atomic emission spectrometry after extraction separation
CHEN Lin
School of Pharmaceutical and Environmental Engineering, Sichuan Vocational College of Chemical Technology, Luzhou 646300, China
Abstract：The accurate determination of vanadium and tungsten contents in waste vanadium-titanium-based denitration catalyst (V2O5-WO3/TiO2) has important significance for the recycle of related metal resources. In order to reduce the influence of matrix effect, the waste vanadium-titanium-based denitration catalyst was digested with sulfuric acid at high temperature. Then vanadium and tungsten were extracted with extractant (20% N1923+2% sec-octyl alcohol+78% sulfonated kerosene, V/V) for separation. Finally, the contents of vanadium and tungsten were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The pretreatment conditions of sample were obtained based on the single factor experiment results: the dosage ratio of catalyst to 80% sulfuric acid (m/m) was 1:40 (solid-liquid ratio, g/mL); the concentration of N1923 was 20% (volume fraction), and the volume ratio of organic phase to aqueous phase (O/A) was 2:1 in the extraction process; during back extraction, the concentration of sodium hydroxide solution was 1 mol/L, and the ratio of O/A was 1:2. The results showed that the mass concentration of vanadium and tungsten in range of 1.0-10.0 μg/mL and 2.0-20.0 μg/mL was linear to the corresponding emission intensity, respectively. The correlation coefficient was 0.999 5 and 0.999 6, and the limit of detection was 0.002% and 0.003% (mass fraction), respectively. The contents of vanadium and tungsten in three waste vanadium-titanium-based denitration catalyst samples were determined according to the experimental method, and the relative standard deviations (RSD, n=11) of measurement results were less than 4.0%. The found results were consistent with those obtained by X-ray fluorescence spectrometry in GB/T 31590-2015.
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