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粉末压片制样-X射线荧光光谱法测定锂云母中的高含量氟

Determination of High Concentration of Fluorine in Lithium Mica by X-ray Fluorescence Spectrometry with Pressed-Powder Pellets

  • 摘要: 锂云母中的氟含量很高(1.36%~8.71%),在焙烧锂云母矿物时锂的浸出率随着含氟量的增加而逐步下降,随着锂云母脱氟率的提高,锂的浸出率也相应提高,准确测定锂云母中的氟、控制氟含量可为确定焙烧过程的工艺条件、设备参数及成本提供依据。目前氟的测定主要采用离子选择电极法,但过程复杂、分析时间长且空白值高。本文采用粉末直接压片制样X射线荧光光谱法测定锂云母中的氟,氟的检出限为46±4μg/g。将锂矿石标准物质和人工配制校准物质制成工作曲线,经验系数校正基体效应和谱线干扰,方法精密度(RSD,n=10)为1.03%。采用本法分析由标准样品合成的样品,测定值与理论值吻合良好;用实际样品验证,测定结果与离子选择电极法的测定值相符。本法适用于分析锂云母中0.68%~9.14%的氟。

     

    Abstract:
    BACKGROUNDThe fluorine content in lithium mica is very high (1.36% to 8.71%), and the leaching rate of lithium during roasting lithium mica minerals decreases gradually with the increase of fluorine content. With increased defluorination of lithium mica, the leaching rate of lithium is also increased accordingly. Therefore, accurate determination of fluorine in lithium mica and control of fluorine content can provide a basis for determining the process conditions, equipment parameters and cost of roasting process. At present, the most common used method for determination of fluorine is the ion selective electrode method. However, the process is complex, the analysis time is long and the blank value is high. X-ray Fluorescence Spectrometry (XRF) is a green and pollution-free method, which is simple, fast and accurate.
    OBJECTIVESTo determine the fluorine content in lithium mica.
    METHODSThe fluorine content in lithium mica was determined by XRF with pressed-powder pellets. The working curve was made from standard material lithium ore and manually prepared calibration material, and the experience coefficient was used to correct the matrix effect and spectral interference.
    RESULTSThe method precision(RSD, n=10) is 1.03% and the detection limit of fluorine is 46±4μg/g. Analytical results of samples synthesized from standard samples acquired by this method are in good agreement with theoretical values. It is demonstrated by actual samples that the determination results are consistent with those of the ion selective electrode method.
    CONCLUSIONSThis method is suitable for determining fluorine in lithium mica with contents ranging from 0.68% to 9.14%.

     

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