粉末压片制样-X射线荧光光谱法测定炉渣中氟钾钠硫

炉渣中的氟、钾、钠、硫可以用于润滑,防止钢水与壁黏连,也可以用来调节熔点以及判定缺陷来源。实验利用转炉渣、高炉渣、电炉渣的标准样品和准确定值的炉渣生产试样绘制校准曲线,从而建立了粉末压片制样-X射线荧光光谱法(XRF)测定炉渣中氟、钾、钠、硫的分析方法。通过试验确定制样条件为:试样研磨过200目(74 μm)筛,压片机的压力为20 MPa,保压时间为30 s。按照实验方法,对1个炉渣试样压片11次测量,各元素测定结果的相对标准偏差(RSD)为0.17%～3.4%;正确度验证结果表明,实验方法的检测结果与其他分析方法(高频燃烧红外吸收法、电感耦合等离子体原子发射光谱法以及离子选择电位法)的检测结果一致,可以满足炉前分析量大、分析速度快的要求。

Determination of fluorine,potassium,sodium and sulfur in slag by X-ray fluorescence spectrometry with pressed powder pellet

Fluorine, potassium, sodium and sulfur in slag can be used for lubrication to prevent molten steel from adhering with the wall. Moreover, they can be also used to adjust the melting point and judge the source of defects. The certified reference materials of converter slag, blast furnace slag and electric furnace slag as well as the production sample of furnace slag after accurate determination were used to draw the calibration curve. The analysis method of fluorine, potassium, sodium and sulfur in slag by X-ray fluorescence spectrometry (XRF) with pressed powder pellet was established. The experimental conditions for sample preparation were obtained as follows: the ground sample passed through 200-mesh sieve (74 μm); the pressure of pressing machine was 20 MPa; the time of maintaining pressure was 30 s. One furnace slag sample was prepared and determined for 11 times according to the experimental method. The relative standard deviations (RSD, n=11) of determination results of testing elements were between 0.17% and 3.4%. The accuracy verification results showed that the determination results of proposed method were consistent with those obtained by other analysis method (high frequency combustion infrared absorption, inductively coupled plasma atomic emission spectrometry and ion selective potential method). The proposed method could meet the batch quantity and rapid analysis requirements of on-the-spot samples.