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熔融制样-X射线荧光光谱法测定高铬铁矿石中11种组分

Determination of 11 components in high-chromium iron ore by X-ray fluorescence spectrometry with fusion sample preparation

  • 摘要: 针对高铬铁矿石中铬元素难熔融及钠、磷等元素难以同时准确测定等问题,实验通过组合高铬镍铁矿石、铁矿石、铬铁矿、红土镍矿、镍矿石等多种标准物质/标准样品,并采用混合配制方式建立校准系列,实现了熔融制样-X射线荧光光谱法(XRF)对高铬铁矿石中氧化钠、氧化镁、三氧化二铝、二氧化硅、五氧化二磷、氧化钾、氧化钙、二氧化钛、三氧化二铬、氧化锰、氧化镍共11种组分的同时测定。采用四硼酸锂-偏硼酸锂混合熔剂(质量比12∶22),控制样品与熔剂稀释比为1∶15,以碘化铵和溴化锂溶液为脱模剂,在1 100 ℃熔融15 min,可制备得到均匀透明的玻璃熔片。使用仪器自带SPECTRAPLUS软件进行理论α系数基体校正,有效克服基体效应影响。按照实验方法测定高铬铁矿石中11种组分,测定结果的相对标准偏差(RSD,n=12)为0.10%~4.8%;t检验显示该方法与经典化学法的测定结果无显著性差异;对3个高铬镍铁矿标准物质和2个由标准样品合成的样品的测定值均与认定值或参考值相一致,方法适用于高铬铁矿石的综合分析。

     

    Abstract: To address the difficulties in fusing chromium and the simultaneous accurate determination of sodium,phosphorus and other elements in high-chromium iron ore,a calibration series was established by combining various certified reference materials(CRM/RM) including high-chromium nickel iron ore,iron ore,chromite,lateritic nickel ore and nickel ore through mixed preparation.On this basis,the simultaneous determination of 11 components(sodium oxide,magnesium oxide,aluminum oxide,silicon dioxide,phosphorus pentoxide,potassium oxide,calcium oxide,titanium dioxide,chromium sesquioxide,manganese oxide and nickel oxide) in high-chromium iron ore by X-ray fluorescence spectrometry(XRF) with fusion sample preparation was realized.A mixed flux of lithium tetraborate-lithium metaborate(m∶m=12∶22) was adopted with a sample-to-flux dilution ratio of 1∶15.Ammonium iodide and lithium bromide solution was used as releasing agent.Uniform and transparent glass fused beads were obtained after fusion at 1 100 ℃ for 15 min.The built-in SPECTRAPLUS software was applied for matrix correction using theoretical α coefficient,which effectively eliminated the influence of matrix effect.The contents of 11 components in high-chromium iron ore were determined according to the experimental method,and the relative standard deviations(RSD,n=12) of determination results ranged from 0.10% to 4.8%.The t-test indicated that there was no significant difference between the results obtained by this method and those by traditional chemical methods.The measured values of three CRMs of high-chromium nickel iron ore and two synthetic samples prepared from CRM/RM were consistent with the certified or reference values.The proposed method was suitable for the comprehensive composition analysis of high-chromium iron ore.

     

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