采用熔融法制样,建立了X射线荧光光谱法(XRF )测定铁矿石中14种组分(T Fe、CaO、SiO2、MgO、Al2O3、MnO、TiO2、K2O、Na2O、Ni、Cu、Co、P、S)含量的方法。通过试验确定熔解铁矿石最佳的熔剂为混合熔剂[m(Li2 B4 O7)∶ m(LiBO2)=67∶33],稀释比为1∶20,预氧化条件为700℃下预氧化10 min。此措施很好地解决了低含量元素和轻元素因熔剂影响而测量强度下降的问题。使用理论α系数和经验系数法相结合进行校正,有效地消除了基体效应和重叠谱线干扰的影响,校正后校准曲线的离散度(RM S )较小。各组分的检出限在0.61~335.09μg/g之间。对铁矿石试样进行精密度考察,各组分含量的相对标准偏差在0~8.7%范围内;对铁矿石标准样品进行分析,各组分的测定值与认定值相符。相对于其他铁矿石分析的XRF方法,实验方法可用于Co、Ni、Cu及难于准确测量的Na和S的测定,且满足进出口商品检验工作对效率和准确度的要求。
T he determination method of 14 components (including T Fe ,CaO ,SiO2 ,M gO ,Al2 O3 ,M nO , TiO2 ,K2 O ,Na2 O ,Ni ,Cu ,Co ,P and S) in iron ore by X‐ray fluorescence spectrometry (XRF) with fusion sample preparation was established .The optimal flux for the decomposition of iron ore was mixed flux [m(Li2B4O7)∶ m(LiBO2)=67∶33] with dilution ratio of 1∶20 .The sample was pre‐oxidized at 700 ℃for 10 min .The problem of measurement strength decrease of low content elements and light elements caused by flux could be w ell solved .T he matrix effect and spectral overlapping interference could be effec‐tively eliminated after the use of theoretical α coefficient method and empirical coefficient method correc‐tion .The root mean square (RMS) of calibration curve after correction was small .The detection limits of testing components were between 0.61 μg/g and 335.09 μg/g .The precision test of iron ore sample was also conducted .The relative standard deviations (RSD) were between 0 and 8.7% .The certified reference material of iron ore was analyzed according to the experimental method ,and the found results of each com‐ponent were consistent with the certified values .Compared to other XRF methods for the analysis of iron ore ,the proposed method was applicable for the determination of Co ,Ni and Cu ,and also Na and S which were difficult to be accurately determined .Moreover ,it could meet the requirements of inspection efficien‐cy and accuracy for import and export commodities .
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