Determination of fluoride and chloride in high-silicon silver concentrates by ion chromatography with sodium hydroxide fusion-ultrasound assisted-steam distillation
WANG Heng1, ZHUANG Mei1, LI Xiang-rong2, QIN Li-jun1 JIANG Yu1, FENG Ya-hui3
Abstract：During the direct determination of fluorine and chlorine in high-silicon silver concentrates by ion chromatography with steam distillation, the sulfur in sample will be spilled in the form of hydrogen sulfide gas, which is harmful for the operator′s health. Meanwhile, the determination results of fluorine and chlorine would be lower due to the incomplete digestion of high-silicon silver concentrate samples. In order to solve this problem, the determination of fluorine and chlorine in high-silicon silver concentrates by ion chromatography with sodium hydroxide fusion-ultrasound assisted-steam distillation was proposed. The sample was melted at high temperature with sodium hydroxide and then transferred into hot water. The fluorine and chlorine in melt and residue were leached by combining with ultrasonic technology. Then, the fluorine and chlorine were effectively evaporated by steam distillation, and finally determined by ion chromatography. The methods of sample fusion, ultrasonic time, fusion temperature, fusion time, volume of receptor fluid, and chromatographic elution time were optimized. The results showed that the linear correlation coefficients of fluoride and chlorine were 0.9998 and 0.9992 under the optimized experimental conditions, respectively. The limit of detection was 0.002% and 0.005%, respectively. The contents of fluoride and chlorine in high-silicon silver concentrate were determined according to the experimental method, and the relative standard deviations (RSD, n=6) of determination results were between 1.5% and 4.3%. The spiked recoveries were between 95% and 105%. The proposed method was compared with the pyrohydrolysis method. The results showed that the measured results of two methods were basically consistent.
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