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目前,国内没有关于半钢发热剂的国家标准检测方法,只能根据组分范围分别检测各个组分,不仅耗时而且使用的大量化学试剂对环境造成污染。故研究了X-射线荧光光谱法快速测定半钢发热剂中Si,P,S的方法。采用粉末压片制样,研究其制样条件,包括磨样时间、压样时间和压力对测定结果的影响。采用其它方法定值提供的检测样品,作为X-射线荧光光谱法内控标准样品,采用经验系数法进行基体校正,通过解谱拟合建立校准曲线,校准曲线建立后仪器建立漂移校正程序。实验结果精密度好,各元素的相对标准偏差在0.15%~1.3%。准确度满足生产需求,实验方法可用于快速检测半钢发热剂化学组分。
At present, there is no national standard test method for semi-steel heating agent in China, and each component can only be tested separately according to the range of components, which not only takes time but also uses a large amount of chemical reagents to pollute the environment. Therefore, the rapid determination of Si, P, S in semi-steel heating agent by X-ray fluorescence spectrometry was studied. Powder tabletting was used to study the sample preparation conditions, including the effect of grinding time, pressure time and pressure on the determination results. The test sample provided by other methods is used as a standard sample for internal control of X-ray fluorescence spectrometry, the matrix is corrected by the empirical coefficient method, and the calibration curve is established by solving the spectrum fitting. After the calibration curve is established, the instrument establishes a drift correction program. The experimental results show good precision with relative standard deviations of 0.15% -1.3%. Accuracy to meet production needs, experimental methods can be used for rapid detection of semi-steel heating agent chemical composition.