粉末压片-X射线荧光光谱法测定含碳化硅铝质耐火材料中8种组分

含碳化硅耐火材料已广泛地应用于冶金炉料中,目前对含碳化硅耐火材料测定常采用湿法分析,然而这些方法繁琐耗时,不适合大批量检测要求。实验采用聚酯(PET)薄膜包裹粉末压片法制样,以微晶纤维素为粘结剂,选取与待测试样粒度一致、基体相似、各成分含量有梯度的铝硅系耐火材料标准样品和碳化硅标准样品,按照不同的比例,配制成各组分含量从低到高具有一定梯度含碳化硅铝质耐火材料校准样品,对其拟合校准曲线,建立了X射线荧光光谱法(XRF)同时测定含碳化硅铝质耐火材料中TSi、Fe₂O₃、Al₂O₃、CaO、MgO、TiO₂、P₂O₅、K₂O含量的快速分析方法。采用PET薄膜包裹压片不仅减少粉尘污染,把对仪器损坏的几率降到了最低,而且可以防止压片暴露在空气中,增加压片保存时间。对含碳化硅铝质耐火材料试样进行了精密度考察,各组分测定结果的相对标准偏差(RSD,n=10)为0.08%～3.7%。采用实验方法对合成含碳化硅铝质耐火材料校准样品(未用于校准曲线绘制)和实际样品进行测定,结果与参考值或国标方法的分析值相吻合。

Determination of eight components in aluminum refractory containing silicon carbide by X-ray fluorescence spectrometry with pressed powder pellet

The refractories containing silicon carbide have been widely used in metallurgical furnace charge. At present, the determination of refractories containing silicon carbide often adopts wet analysis method. However, these methods are tedious and time-consuming, which is not suitable for the batch inspection. The sample was prepared by pressed powder pellet with thin polyester (PET) film for package. The microcrystalline cellulose was selected as the binder. The certified reference materials of aluminum-silicon refractory and silicon carbide with the same particle size, similar matrix and content gradient as the sample were selected to prepare a series of calibration samples of aluminum refractory containing silicon carbide with certain content gradient from low to high according to different proportion. Then the calibration curves were fitted with those calibration samples. Consequently, a method for the rapid analysis and simultaneous determination of TSi, Fe₂O₃, Al₂O₃, CaO, MgO, TiO₂, P₂O₅ and K₂O in aluminum refractory containing silicon carbide was established by X-ray fluorescence spectrometry (XRF). PET film was introduced into pack the pressed powder pellet, which not only reduced the dust contamination and the damage probability of the instrument to a minimum, but also prevented the sample from being exposed to the air, thus increasing the preservation time of the pellet. The precision tests for determination of eight components in aluminum refractory samples containing silicon carbide were conducted. The relative standard deviations (RSD, n=10) of determination results were between 0.08% and 3.7%. The proposed method was applied for determination of calibration sample (which was not used for the preparation of calibration curve) and actual sample of aluminum refractory containing silicon carbide. The results were consistent with the reference values or those obtained by the national standard method.