钛铁矿石中铁的化学物相分析  

Chemical phase analysis of iron in ilmenite ore

作　　者：夏传波 张文娟 姜云 田兴磊 王志明 赵伟 XIA Chuanbo;ZHANG Wenjuan;JIANG Yun;TIAN Xinglei;WANG Zhiming;ZHAO Wei(Shandong Institute of Geological Sciences,Jinan 250013,China;Shandong Provincial Key Laboratory of Metallogenic Geological Process and Resource Utilization,Jinan 250013,China)

机构地区：[1]山东省地质科学研究院,山东济南250013 [2]山东省金属矿产成矿地质过程与资源利用重点实验室,山东济南250013

出　　处：《冶金分析》2023年第7期60-68,共9页Metallurgical Analysis

基　　金：山东省地质勘察项目(鲁勘字[2020]8号);国家重点研发计划(2016YFF0201103,2021YFC2903004)。

摘　　要：钛铁矿石中铁的化学物相分析研究较少,不同文献对铁的化学相态划分不尽一致,各相态的提取方法也有所差异,且多数未报道单矿物浸取试验结果。在典型钛铁矿矿区采集试验样品,从中挑选出所需的单矿物,通过单矿物浸取试验和实际样品浸取试验,确定了各相态的较优浸取分离流程:用乙酸-过氧化氢-硼酸溶液浸取样品,滤液用于测定硫化物及碳酸铁中铁;残渣用氢溴酸-二氯化锡溶液浸取,滤液用于测定磁铁矿、赤铁矿与褐铁矿等氧化物中铁;残渣灰化后在800℃灼烧,用硝酸-氟化铵溶液浸取,滤液用于测定硅酸盐中铁;剩余残渣用于测定钛铁矿中铁。根据各相态提取液中铁含量的高低,采用电感耦合等离子体原子发射光谱法(ICP-AES)或重铬酸钾滴定法测定,建立了钛铁矿石中铁的化学物相分析方法。方法检出限为0.002%~0.045%。方法应用于铁矿石物相分析标准物质的测定,测定结果与认定值基本相符;应用于钛铁矿石实际样品的测定,各相态测定结果的相对标准偏差(RSD,n=12)小于4%;各相态铁量的加和与全量铁的相对偏差小于2%,满足DZ/T 0130—2006《地质矿产实验室测试质量管理规范》的要求,主要相态分析结果与自动矿物分析仪(MLA)结果基本吻合。实验方法可为相关标准的制定提供参考。There are few studies about the chemical phase analysis of iron in ilmenite ores.The chemical phase division of iron in different literatures is inconsistent,and the extraction methods are also different.The detailed results of single mineral leaching test are not reported in most literatures.Test samples were collected from one typical ilmenite mining area,and the required single mineral was selected.Through leaching tests of single mineral and actual sample,the optimal leaching and separation processes for each phase were obtained:the sample was leached with the mixed solution of acetic acid,hydrogen peroxide and boric acid,and the filtrate was used for the determination of iron in sulfide and iron carbonate;the residue was leached with the mixed solution of hydrobromic acid and tin dichloride,and the filtrate was used for the determination of iron in oxides such as magnetite,hematite and limonite;the residue was ashed and burned at 800℃followed by leaching with nitric acid and ammonium fluoride solution,and the filtrate was used for the determination of iron in silicate;the remaining residue was used for the determination of iron in ilmenite.According to the iron content in the leaching solution of each phase,the content of iron was determined by inductively coupled plasma atomic emission spectrometry(ICP-AES)or potassium dichromate titrimetric method.Consequently,the analysis method for chemical phases of iron in iron ores was established.The limit of detection was 0.002%-0.045%.The proposed method was applied to the determination of reference materials for phase analysis of iron ores,and the results were basically consistent with the certified values.The method was also used for the determination of samples of ilmenite ores,and the relative standard deviations(RSD,n=12)of determination results for phases were all below 4%.The relative deviation between the sum of each phase iron content and the total iron content was less than 2%,which could meet the requirements in DZ/T 0130-2006 The Specification of Test

关 键 词：钛铁矿石 铁 化学物相分析 电感耦合等离子体原子发射光谱法(ICP-AES) 重铬酸钾滴定法 

分 类 号：O657.31[理学—分析化学] TF521[理学—化学]