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利用粉末压片法制备样品,通过在Omnian无标定量分析软件中添加与待测组分相似样品来建立标签,可校正粉末样品可能存在的矿物效应、颗粒效应及制样引进的误差,从而实现X射线荧光光谱法(XRF )对稀土矿物中P2 O5的准确测定。通过试验确定了压片制样的最佳制样条件为:样品粒度小于0.074 m m、压力为40 t、称样量为6.00 g 和保压时间为30 s。对含不同梯度含量P2 O5的稀土矿石进行正确度考察,发现以Omnian软件未添加标签而直接测定的P2 O5结果差值较大,而Omnian添加标签的分析结果与国家标准方法的分析结果基本吻合;精密度试验表明,P2 O5测定结果的相对标准偏差(RSD ,n=8)小于3%。无需大量的标样建立校准曲线,能满足稀土矿石含磷量的精确分析要求。

The sample was prepared by pressed powder pellet method .The tag was established by adding the standard sample with similar components into Omnian standard-less quantitative analysis software . T hus ,the errors caused by possible mineral effect ,particle effect and sample preparation could be correc-ted for powdered samples .The accurate determination of P2 O5 content in rare earth ores by X-ray fluores-cence spectrometry (XRF) was achieved .The optimal sample preparation conditions were obtained by ex-periments :the particle size was less than 0 .074 mm ;the pressing pressure was 40 t ;the sample mass was 6 .00 g and the holding time was 30 s .The accuracy test was investigated using rare earth ore containing different content gradients of P2 O5 .It was found that the direct determination results of P2 O5 by Omnian software without addition of tag showed large errors .After adding tag ,the analytical results by Omnian were basically consistent with those obtained by national standard method .The precision test indicated that the relative standard deviation (RSD ,n=8) of determination results for P2 O5 was less than 3% .The proposed method could meet the accurate analysis requirements of P2O5 in rare earth ores without the es-tablishment of standard curve using large amounts of standard samples .

参考文献

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