Determination of fluoride and chloride in nonferrous metal oreby pyrohydrolysis-ion chromatography
LI Xiang-rong1,HUANG Yuan2,LAI Tian-cheng1
1. Polytechnic Service Center of Fangchenggang Entry-Exit Inspection and Quarantine Bureau, Fangchenggang538001, China 2. Guangxi-ASEAN Technology Transfer Center, Nanning 530001, China
Abstract：The sample was treated in automatic pyrohydrolysis device. The determination method of fluoride and chloride contents in nonferrous metal ore by pyrohydrolysis-ion chromatography was established. The pretreatment effect of sample by steam distillation and pyrohydrolysis was compared. The sample pretreatment method of pyrohydrolysis was selected in this study. The use condition of catalyst in pyrohydrolysis process was investigated. The fluoride and chloride in catalyst was removed by pyrohydrolysis to eliminate their influence on determination results. The content of fluoride and chloride in determination range had good linear relationship to the peak area. The correlation coefficients were both 0.9999. The detection limit of fluoride and chloride in this method was 0.11ng/mL and 0.24ng/mL, respectively. The copper concentrate with certified value of fluoride as well as certified reference materials of polymetallic ore without certified values of fluoride and chloride were determined according to the experimental method. The relative standard deviations (RSD, n=11) were all less than 5%. The found result of fluoride in copper concentrate was consistent with the certified value. The spiked recoveries of fluoride and chloride in polymetallic ore were between 97.0% and 100.0%. The lead concentrate, copper concentrate and zinc concentrate samples from different countries were determined, and the found results of fluoride and chloride were basically consistent with those obtained by ion selective electrode method and potentiometric titration method, respectively. The experimental method was compared with the ion selective electrode method, and the detection limit was reduced from g/mLto ng/mL. Compared to the existing steam distillation method, the pyrohydrolysis process improved the extraction rate of testing components. It solved the problem that the fluoride and chloride in copper concentrate, lead concentrate and zinc concentrate samples with high sulfur content could not be extracted by steam distillation method.
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LI Xiang-rong,HUANG Yuan,LAI Tian-cheng. Determination of fluoride and chloride in nonferrous metal oreby pyrohydrolysis-ion chromatography. , 2018, 38(2): 53-58.
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