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锂精矿中二氧化硅、三氧化二铝和氟量同时快速检测分析

  • 作者:
  • 刘芳美|李文英|甘聪|钟坚海

  • 作者单位:
  • (1. 紫金铜业有限公司;2. 福建省铜绿色生产及伴生资源综合利用重点实验室;3. 厦门海关技术中心)
  • 详细信息:

  • 作者简介:
  • 刘芳美(1992—),女,工程师,研究方向为实验室管理,矿石与矿物、贵金属与合金、水质分析方法应用开发等;E-mail:liufangmei2014@ 163. com
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Simultaneous and rapid analysis of SiO₂, Al₂O₃, and F contents in lithium concentrate

  • English Author:
  • Liu Fangmei1,2, Li Wenying1,2, Gan Cong1,2, Zhong Jianhai3

  • Unit:
  • (1. Zijin Copper Co., Ltd.; 2. Fujian Key Laboratory for Green Production of Copper and Comprehensive Utilization of Associated Resources; 3. Technology Center, Xiamen Customs)
  • 摘要
  • 在线预览
  • 参考文献

摘要:

锂精矿中的硅、铝、氟等杂质对下一步的精制过程有很大影响,可能降低锂回收率并影响产品质量。研究采用氢氧化钠-过氧化钠对锂精矿样品进行熔融前处理,分别采用硅钼蓝分光光度法、络合滴定法、离子选择性电极法同时快速测定样品中的二氧化硅、三氧化二铝和氟含量。探讨了熔剂的选择、熔融温度和时间、酸度等实验条件对各元素测定结果的影响。实验表明,采用氢氧化钠-过氧化钠作为混合熔剂,熔融温度为700C,熔融时间为15 min,盐酸加入量为20 mL时,试样溶解完全。本方法二氧化硅、三氧化二铝和氟测定结果的相对标准偏差(RSD,n=7)分别为0.53%~0.57%、0.37%~0.64%、0.31%~1.18%,符合GB/T 32465-2015《化学分析方法验证确认和内部资料控制要求》对相对标准偏差的要求,且与3种行业标准方法测定结果吻合良好。该方法可应用于锂精矿中二氧化硅、三氧化二铝和氟的同时快速检测分析。

关键词:

锂精矿;硅钼蓝分光光度法;络合滴定法;离子选择性电极法;同时测定;快速测定

Abstract:

Impurities such as silicon, aluminum, and fluorine in lithium concentrate significantly affect the sub-sequent refining process, potentially reducing lithium recovery rates and impacting product quality. This study proposes a rapid method for the simultaneous determination of SiO2, Al203, and F contents in lithium concentrate. Lithium con-centrate samples were pretreated before fusion with sodium hydroxide-sodium peroxide mixture, followed by analysis using the silicomolybdenum blue spectrophotometric method, complexometric titration, and ion-selective electrode method. The effects of flux selection. fusion temperature and duration, and acidity on the determination results were investigated. The test shows that when using the sodium hydroxide-sodium peroxide mixed flux, with a fusion temperature of 700 °C, fusion time of 15 min, and adding 20 mL of hydrochloric acid, the sample is completely dissolved. The relative standard deviations (RSD, n=7) of SiO2, AL03, and F using the method were 0.53 %-0.57 %,0.37 %-0.64 %, and 0.31 %-1.18 %,respectively, meeting the requirements of the GB/T 32465-2015 Requirement for Verification & Validation of Detection Methods and Internal Quality Control on Chemical Analysis for RSD, and the results are consistent with 3 industrial standard methods. The method can be applied to the simultaneous and rapid analysis of SiOz, Al203, and Fcontents in lithium concentrate.


Keywords:

lithium concentrate; silicomolybdenum blue spectrophotometric method; complexometric titration; ion⁃ selective electrode method; simultaneous determination; rapid determination