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采用波长色散X射线荧光(X-ray fluorescence,XRF)光谱法对铂铑合金中Pt和Rh的含量进行测定,建立了一种Pt和Rh的分析测量方法。实验设定波长色散XRF光谱仪激发电压为60 k V、电流为50 m A,采用100mm的黄铜滤光片、间距300mm的准直器、PX10分光晶体和闪烁探测器对Pt的La线和Rh的Ka线进行分析测量;为消除样品杯罩产生的干扰使用直径27 mm的准直器面罩。应用经验系数法对基体效应进行了校正,建立了Pt和Rh的校正曲线,其K值和RMS值(均方根偏差)较小,线性相关性较好。分析结果表明,Pt和Rh的相对误差分别小于0.09%和0.54%,相对标准偏差分别为0.11%和0.17%(n=10),检出限分别为208mg·g~(-1)和37mg·g~(-1),该方法能准确可靠地测定铂铑合金中Pt和Rh的含量,单样分析时间仅需74 s。将该方法应用到铂铑合金配制生产过程中,Pt和Rh的测定结果与配方值的相对误差分别小于0.06%和0.20%。在铂铑合金稀释熔炼中,对稀释后样品的Rh含量进行测量,其测量结果与计算值的相对误差低于0.29%。该方法能够满足大批量铂铑合金样品的分析需求,为生产实践提供准确可靠的科学数据。
The content of Pt and Rh in platinum-rhodium alloy was determined by X-ray fluorescence (XRF) spectroscopy, and a method for the analysis and measurement of Pt and Rh was established. The experimental setup wavelength dispersion XRF spectrometer excitation voltage of 60 k V, a current of 50 m A, with 100mm brass filter, a pitch of 300mm collimator, PX10 spectrometer and scintillation detector on the Pt La line and Rh Ka line for analysis and measurement; To eliminate the interference caused by the sample cup cover the use of a 27 mm diameter collimator mask. The matrix effect was corrected by using the empirical coefficient method. The calibration curve of Pt and Rh was established, and the K and RMS values (root mean square deviation) were small and the linear correlation was good. The results showed that the relative errors of Pt and Rh were less than 0.09% and 0.54%, respectively. The relative standard deviations were 0.11% and 0.17%, respectively. The detection limits were 208 mg · g ~ (-1) and 37 mg · g ~ (-1). The method can accurately and reliably determine the content of Pt and Rh in the platinum-rhodium alloy. The analysis time is only 74s. When applying this method to the preparation of platinum rhodium alloy, the relative errors between the results of determination of Pt and Rh and the formulation values are less than 0.06% and 0.20% respectively. In the rhodium alloy dilution smelting, the Rh content of the diluted sample was measured, and the relative error between the measured value and the calculated value was less than 0.29%. This method can meet the analytical needs of high-volume platinum-rhodium alloy samples and provide accurate and reliable scientific data for production practice.