Determination of fluorine in ore by mixed alkali fusion-ion selective electrode method
XIAO Fang1,2, NI Wen-shan1,2, MAO Xiang-ju*1,2 LI Xian-zhen1,2, ZHANG Hong-li1,2, LIU Lu1,2
1. Zhengzhou Institute of Multipurpose Utilization of Mineral Resources,Zhengzhou 450006,China; 2. Engineering Technology Research Center of the National Comprehensive Utilization of Nonmetallic Mineral Resources,Zhengzhou 450006,China
Abstract：The sample was fused with mixed flux, i.e., 1 g of sodium peroxide and 2 g of sodium hydroxide. The melt was leached with hot water. At this time, the elements including iron, calcium, titanium, lead, copper, zircon and rare earths were removed in the forms of hydroxide precipitates. The color interference of manganese was eliminated by adding little ethanol followed by boiling. With the pH of solution adjusted to 5.5-6.5 and in presence of total ionic strength adjustment buffer solution of trisodium citrate dihydrate-potassium nitrate, a method was established for determination of fluorine in ore by ion selective electrode method using bromocresol green as indicator. The experimental results showed that the negative logarithm of mass concentration of fluorine ion was linear to the corresponding potential (E). The correlation coefficient was r=0.999. The linear range was 0.2-20.0 μg/mL. The detection limit of method was 0.019 μg/mL. The further interference tests indicated that the elements in sample including silicon, aluminum, magnesium, calcium, zinc, phosphorus and chlorine did not interfere with the determination. The proposed method was applied to the determination of fluorine in ten types of ore certified reference materials(lithium ore, tantalum ore, molybdenum ore, tungsten ore, tin ore, phosphorus ore, zinc ore, tantalum ore, antimony ore, lead ore and copper ore). The results were consistent with the certified values. The relative standard deviations (RSD, n=6 or n=12) were between 0.30% and 5.0%.
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