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熔融制样X射线荧光光谱法测定高铬赤泥中主次量组分
  • ISSN号:0254-5357
  • 期刊名称:《岩矿测试》
  • 时间:0
  • 分类:O614.611[理学—无机化学;理学—化学] O657.34[理学—分析化学;理学—化学]
  • 作者机构:[1]中南大学资源加工与生物工程学院,湖南长沙410083
  • 相关基金:国家自然科学基金重点项目(51234008);国家自然科学基金资助项目(51174230)
中文摘要:

高铬红土型铝铁复合矿经钠盐还原焙烧-磁选-浸出后,铬等有价金属在赤泥中富集(Cr2O3含量达到3%-30%),属难熔复合矿物,目前主要以化学分析方法为主,但操作复杂,且步骤繁琐,分析周期长。而应用X射线荧光光谱法分析测定,一般采用钠盐熔剂、较高稀释比等熔融制样,不利于钠及低含量元素的测定。本文采用四硼酸锂-偏硼酸锂(67∶33)作混合熔剂,硝酸铵作氧化剂,饱和溴化锂溶液作脱模剂制备玻璃熔片,建立了波长色散型XRF测定高铬赤泥中主次量组分(铬硅铝铁镁钙钠钾硫磷钛锰钒)的分析方法。研究表明,熔样稀释比低于24∶1时,稀释比越低,对铂金坩埚腐蚀越严重;稀释比在24∶1时,制样方法的相对标准偏差(RSD,n=10)最低;熔样时间越长,温度越高,RSD越低。由此确定熔样最优条件为稀释比24∶1,熔样时间15 min,熔样温度1100℃。分析中采用铬铁矿、铝土矿、黏土、铁矿石国家标准物质及人工标准样品校准,基本参数法进行基体校正,方法精密度(RSD,n=10)为0.3%-3.9%。与国内外其他含铬矿物的XRF分析方法相比,本方法采用不添加钠盐、一次熔片、常规熔样温度(1100℃)、低稀释比(24∶1)等进行制样,制样方法的精密度和分析精密度均低,解决了高铬赤泥的XRF分析方法问题,还可扩展到高铬、铝、硅、铁等复合矿原矿及其钠盐处理焙烧矿、精矿及尾矿的XRF分析。

英文摘要:

Cr and other valuable metals are enriched in red mud( Cr2O3: 3%- 30%) when high-Cr red clay type Al-Fe composite ores are comprehensively utilized by sodium reduction roasting-magnetic separation-leaching. HighCr red mud belongs to refractory ore whose analysis methods are dominated by chemical analysis,which is a wellestablished but complicated procedure. High-Cr red mud can also be analyzed by X-ray Fluorescence Spectrometry( XRF). However,a use of sodium flux and a high dilution ratio are not conducive to sodium and low content elements. In this paper,a method of XRF analysis is developed for the determination of the major and minor components( Cr,Si,Al,Fe,Mg,Ca,Na,K,S,P,Ti,Mn and V) in high-Cr red mud by fused bead preparation with Li2B4O7-Li BO2( 67 ∶ 33) flux,NH4NO3 oxidizer and saturated Li Br solution parting medium. When the dilution ratio of the melting sample is lower than 24 ∶ 1,the lower dilution ratio,the more serious is the corrosion on the PtAu crucible; the RSD( n = 10) of the sample preparation method is at a minimum when the dilution ratio is 24 ∶ 1;the longer the melting time and the higher the melting temperature,the RSD becomes lower. The optimization conditions of fused bead are obtained when the dilution ratio is 24 ∶ 1,the melting temperature is 1100℃ and the melting time is 15 min. The working curve was established by chromite,bauxite,clay,iron ore standards and manual preparation standard materials. The matrix effect and spectrum line overlap interference were corrected by a fundamental parameter method and standard regression. The results are consistent with certified values and the RSD( n = 10) is from 0. 3% to 3. 9%. Compared with domestic and foreign XRF methods for chromium-containing minerals,this method uses no sodium salt,a fuse piece,conventional sample melting temperature( 1100℃),low dilution ratio( 24 ∶ 1) for sample preparation,and the sampling precision and analysis precision are low. The problem with XRF analysis of high-Cr r

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期刊信息
  • 《岩矿测试》
  • 北大核心期刊(2011版)
  • 主管单位:中国科协
  • 主办单位:中国地质学会岩矿测试专业委员会 国家地质实验测试中心
  • 主编:罗立强
  • 地址:北京西城区百万庄大街26号
  • 邮编:100037
  • 邮箱:ykcs_zazhi@163.com
  • 电话:010-68999562 68999563
  • 国际标准刊号:ISSN:0254-5357
  • 国内统一刊号:ISSN:11-2131/TD
  • 邮发代号:2-313
  • 获奖情况:
  • 全国优秀科技期刊三等奖,地矿部科技期刊一等奖,优秀学术期刊三等奖,中国期刊方阵“双效”期刊
  • 国内外数据库收录:
  • 美国化学文摘(网络版),波兰哥白尼索引,美国地质文献预评数据库,美国乌利希期刊指南,美国剑桥科学文摘,中国中国科技核心期刊,中国北大核心期刊(2008版),中国北大核心期刊(2011版),中国北大核心期刊(2014版),英国英国皇家化学学会文摘,中国北大核心期刊(2000版)
  • 被引量:10625