碱熔—水蒸气蒸馏—离子色谱法测定铅精矿中的氟和氯

Detection of Fluoride and Chloride in Lead Concentrate by Alkali Melt-Water Vapor Distillation-Ion Chromatography Method

建立一种铅精矿氟和氯含量的测定方法。通过碱熔消除大量的硫对前处理的影响,采用水蒸气蒸馏的方法将氟和氯有效蒸出。用高容量Metrosep A Supp 5-250阴离子分析柱分离,以碳酸钠(3.2 mmol/L)和碳酸氢钠(1.0 mmol/L)混合溶液作为淋洗液,抑制电导检测器检测。结果显示,选定的方法在测定铅精矿中的氟和氯的线性相关性分别为0.9999和0.9998,加标回收率分别达96%和94%,方法的检出限分别为0.005%和0.006%,方法的相对标准偏差分别为4.53%~7.55%和2.91%~3.92%。

A method for detection of fluoride and chloride content in lead concentrate was established.By alkali fusion method,the influence of much sulfur on sample pretreatment process was eliminated.The fluoride and chloride were effective vaporized using water vapor distillation.Sodium carbonate(3.2 mmol/L)and sodium bicarbonate(1.0 mmol/L)mixture solution was used as eluent and the Metrosep A Supp 5-250 was used as anion analytical column for separation.A suppressed conductivity detector was for detection.Result indicated that,the correlation coefficient of fluoride and chloride 0.9999 and 0.9998 in lead concentrate via the selected method.The standard addition recoveries were 96%and 94%,the sample detection limit were 0.005%and 0.006%.Values of RSD's found were in the range of 4.53%~7.55%and 2.91%~3.92%.