1. China Nonferrous Metal(Guilin) Geology and Mining Co.,Ltd.,Guilin 541004,China; 2. Ecological Environmental Protection Monitoring Station of Pingle County,Guilin 542499,China
Abstract：The accurate determination of water-soluble fluorine, chlorine and sulfate in tungsten tailing is of great significance to the monitoring of water quality in the surrounding environment of tailing piling area. The water-soluble fluorine, chlorine and sulfate were extracted from the samples by ultrasonic extraction with temperature controlled using circulating water. Thus, the determination of these three water-soluble anions in tungsten tailing was realized by ion chromatography. The ultrasonic extraction conditions were optimized as follows:the volume of extraction solution was 80 mL, the ultrasonic power was 350 W, and the ultrasonic time was 12 min. Compared with the standard of GB 5085.3-2007 Identification standard for hazardous wastes-Identification for extraction procedure toxicity, the ultrasonic time was shortened by properly increasing the ultrasonic power. The use of circulating water to control the ultrasonic temperature effectively solved the problem of the temperature rise of extraction solution due to ultrasonic vibration as well as the poor stability of determination results. The experimental results showed that the correlation coefficients of the calibration curves for fluorine, chlorine and sulfate were all higher than 0.999. The method detection limits were 0.19, 0.32 and 0.41 mg/kg, respectively. The minimum quantitative detection limits were 0.76, 1.28 and 1.64 mg/kg, respectively. The proposed method was applied to the determination of water-soluble fluorine, chlorine and sulfate in tungsten tailing samples. The relative standard deviations (RSD, n=6) of determination results were between 0.4% and 3.6%, and the recoveries were between 95% and 103%. The determination results were basically consistent with those obtained by other methods, i.e., determination of water-soluble fluorine by ion selective electrode method, determination of water-soluble chlorine by potentiometric titration method, and determination of water-soluble sulfate by gravimetric method.
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