微波在离子色谱法测定难溶磷矿中氟和氯的应用  

Application of Microwave-Assisted Ion Chromatography for the Determination of Fluoride and Chloride in Difficult-to-Dissolve Phosphate Minerals

作　　者：彭桦 张江坤 朱桂华 王正南 张朝旺 田大明 李有华 杜雄雁 李永林 PENG Hua;ZHANG Jiangkun;ZHU Guihua;WANG Zhengnan;ZHANG Chaowang;TIAN Daming;LI Youhua;DU Xiongyan;LI Yonglin(Yunnan Phosphate Group Phosphorus Resources Development and Utilization Engineering Technology Research Center,Kunming 650600,China)

机构地区：[1]云南磷化集团磷资源开发利用工程技术研究中心,云南昆明650600

出　　处：《云南化工》2025年第2期74-77,共4页Yunnan Chemical Technology

基　　金：磷矿选冶过程标准样品研制(十四五项目子课题2.6)130000001688。

摘　　要：磷矿石有一些种类难以被酸溶解完全(伴生矿的不同),例如:磷钇矿、硫磷铝锶矿等,标准SN/T2993—2011《磷矿石中氟和氯的测定》规定,用一定体积的稀硫酸溶液在蒸馏装置中消解同时蒸馏用离子色谱仪测定,但难溶的磷矿石基体中的氟氯消解不完全。尝试用微波作用少量硫酸溶液短时间消解完全,放入蒸馏装置加入剩余体积的硫酸溶液蒸馏分离出氟氯离子,此法不使用高温设备,操作简易,与(1)碱熔后用离子选择电极测定结果(GB/T 1872—1995磷矿石和磷精矿中氟含量的测定-离子选择性电极法);(2)碱熔后硫酸酸化蒸馏后再用离子色谱仪测定(SN/T 2993—2011磷矿石中氟和氯的测定)比较,结果和2种方法测定结果无显著性差异,微波消解法加标回收率在92.28%~110.00%之间,氟离子相对标准偏差0.87%,氯离子相对标准偏差1.66%,取得了良好的检测结果,方法简单可靠。Phosphate rock has some types that are not fully soluble in acid(due to the presence of impurity minerals),such as apatite,strontiumite,etc.The standard SN/T2993—2011“Determination of Fluorine and Chlorine in Phosphate Rock”specifies that the phosphate rock matrix and im-purity minerals are dissolved in a certain volume of dilute sulfuric acid solution in a distillation apparatus and then separated by distillation using ion chromatography to determine the fluorine and chlorine content.However,the impurity minerals in the difficult-to-dissolve phosphate rock matrix do not dissolve completely.An attempt was made to completely dissolve the phosphate rock matrix and impurity minerals by using microwave action on a small amount of sulfuric acid solution for a short time,and then adding the remaining volume of sulfuric acid solution to the distillation appara-tus to separate out the chloride ions.This method does not use high-temperature equipment and is easy to operate.The results obtained with this method are comparable to those obtained with methods①ion selective electrode determination after alkali fusion(GB/T 1872—1995 Determina-tion of Fluorine Content in Phosphate Rock and Phosphate Concentrate-Ion Selective Electrode Method);and②alkali fusion followed by acidifica-tion with sulfuric acid and determination by ion chromatography(SN/T 2993—2011 Determination of Fluorine and Chlorine in Phosphate Rock),and the recovery rates for spiked samples were between 92.28%and 110.00%.The relative standard deviations of fluoride ions were 0.87%,and those of chloride ions were 1.66%.Good detection results were obtained,and the method is simple and reliable.

关 键 词：微波消解 难溶磷矿石 同时测定氟和氯 

分 类 号：TQ440.72[化学工程—化学肥料工业]