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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

Simultaneous and rapid analysis of SiO₂, Al₂O₃, and F contents in lithium concentrate

  • 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700 ℃,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。

     

    Abstract: Impurities such as silicon, aluminum, and fluorine in lithium concentrate significantly affect the subsequent refining process, potentially reducing lithium recovery rates and impacting product quality. This study proposes a rapid method for the simultaneous determination of SiO₂, Al₂O₃, and F contents in lithium concentrate. Lithium concentrate samples were pretreated before fusion with sodium hydroxide-sodium peroxide mixture, followed by analysis using the silicon molybdenum 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, Al₂O₃, 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 SiO₂, Al₂O₃, and F contents in lithium concentrate.

     

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