粉末压片制样-X射线荧光光谱法测定硅锰合金中硅锰磷

基于对试样检测周期的要求,实验采用可溶性淀粉为稀释剂兼粘结剂进行压片制样,选取与待测试样组成、结构及粒度相似的具有一定梯度含量的硅锰合金试样系列,经国家标准方法确定硅、锰和磷值后作为校准样品,采用能量色散X射线荧光光谱法测定硅锰合金中硅、锰、磷。通过正交实验,确定优化的制样条件为:称取4.000 0g样品及0.400 0g可溶性淀粉,混合均匀后,于30t的压力压制样片,所得样片强度适中、均匀光滑,重现性好。精密度试验结果表明,硅锰合金中硅、锰、磷测定结果的相对标准偏差(RSD,n=10)分别为0.59%、0.19%和5.7%;正确度试验结果表明,实验方法的测定值与国标方法相一致,满足冶炼现场快速检验的需要。

Determination of silicon,manganese and phosphorus in silicon-manganese alloy by X-ray fluorescence spectrometry with pressed powder pellet

Based on the requirements of sample detection period, the soluble starch was used as diluent and binder for sample preparation of pressed powder pellet. A series of silicon-manganese alloy samples with certain content gradient, which were similar to the samples in composition, structure and particle size, were selected as the calibration samples after determining the contents of silicon, manganese and phosphorus using the national standard methods. The contents of silicon, manganese and phosphorus in silicomanganese alloy were determined by energy dispersive X-ray fluorescence spectrometry. The optimized sample preparation conditions were obtained through orthogonal tests: 4.0000g of sample and 0.4000g of soluble starch were mixed uniformly for sample preparation under pressure of 30t. The prepared pellets were uniform and smooth with moderate strength, and the reproducibility was good. The results of precision test showed that the relative standard deviation (RSD, n=10) for silicon, manganese and phosphorus in silicon-manganese alloy was 0.59%, 0.19% and 5.7%, respectively. The accuracy results indicated that the determination values of experimental method were consistent with those obtained by national standard methods, which could meet the requirements of rapid detection at the site of smelting.