Abstract：The accurate determination of fluorine and chlorine has an important guidance to evaluate the utilization value of phosphate ores. The sample was treated by microwave digestion at 160 ℃ for 15 min using nitric acid (1+1) and hydrogen peroxide as the digestion solution. The digestion solution was filtrated with 0.22 μm on-line ultrafiltration system. The contents of fluorine and chlorine were determined by electrical conductivity detector using Metrosep A Supp 5-250/4.0 anion chromatography column. 3.2 mmol/L sodium carbonate and 1.0 mmol/L sodium bicarbonate buffer solution were selected as the eluent. The determination method of fluorine and chlorine in phosphate ore by ion chromatography with microwave digestion was established. The results showed that the occurrence time of characteristic peak of fluorine and chlorine was 6.29 min and 9.17 min, respectively. The mass concentration of fluorine and chlorine in range of 10.00-50.00 mg/L had good linear relationship with the corresponding peak area. The linear correlation coefficients were not less 0.999 6. The limits of detection for fluorine were 0.102 μg/L and 0.162 μg/L, and the limits of quantification were 0.343 μg/L and 0.540 μg/L, respectively. The certified reference materials of phosphate ore were determined according to the experimental method. Moreover, the standard stock solution of single fluorine was added for the recovery tests of standard addition. The relative standard deviations (RSD, n=7) of determination results of fluorine were less than 1%. The results showed that the found results of fluorine were in good agreement with the certified values, and the recoveries were between 98% and 105%. The proposed method was applied for the determination of fluorine and chlorine in six phosphate ore samples. The RSDs (n=7) of determination results were less than 1%. The results showed that the measured values were basically consistent with those obtained by ion selective electrode method in GB/T 1872-1995 or silver chloride turbidimetry in GB/T 9729-2007.
贾海峰, 王峰, 罗琦林, 倪海燕, 刘恒杰, 兰绿灯. 微波消解-离子色谱法测定磷矿石中氟和氯[J]. 冶金分析, 2022, 42(8): 62-67.
JIA Haifeng, WANG Feng, LUO Qilin, NI Haiyan, LIU Hengjie, LAN Lüdeng. Determination of fluorine and chlorine in phosphate ore by ion chromatography with microwave digestion. , 2022, 42(8): 62-67.
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