Yang Yi-Qing, Chen Hui, Wang Ya-Hong, Pan Zhi-Shuang
Institute of Chemistry and Chemical Engineering, Northwest Normal University, Lanzhou 730070, China.
Guang Pu Xue Yu Guang Pu Fen Xi. 2009 Jul;29(7):2001-4.
The aim of the authors' research work was to develop a new technique for quantitative analysis of phosphorus and iron contents in cocatalyst by X-ray fluorescence spectrometry (XRFS). A set of standard samples synthesized were prepared for the experiments with this purpose when the interferences of inter-elements had been corrected by empirical coefficient method. The standard samples were manually synthesized, and the powder pellets were used for sample preparation and the matrix effects were corrected by the experience coefficients. The characteristic X-rays of phosphorus and iron elements could selectively be determined with the enhanced accuracy and reduced time consumption within a range without signal interference from main-component elements. Manufacturing sample and measurement conditions of the new method was brought up; the matrix effects of cocatalyst samples were verified by empirical coefficient method. The results of experiment show that the accuracy and precision of this method satisfactorily had the high repeatability. The measuring ranges of elements were omega 0.01%-2.5% for phosphorus and omega 0.01%-2.5% for iron with the relative deviations of 0.34% for phosphorus and 0.59% for iron, respectively. This method showed satisfied accordant results compared with the chemical method and inductively coupled plasma (ICP). It has provided the analytical values for phosphorus and iron in cocatalyst for maximum propylene production. This new method has the advantages of satisfactory accuracy, high precision, less interference, easy sample handling and efficiency. In addition, the samples are not decomposed during the analysis process when each sample only requires 5 minutes for measurement This new method will be able to meet the growing demands of quantitative analysis of phosphorus and iron content in cocatalysts. This method had the satisfactory accuracy and precision, the analytical range was large, and had been successfully applied to the determination of phosphorus and iron in cocatalyst.
作者研究工作的目的是开发一种通过X射线荧光光谱法(XRFS)对助催化剂中磷和铁含量进行定量分析的新技术。为此,制备了一组合成的标准样品用于实验,同时采用经验系数法校正了元素间的干扰。标准样品是人工合成的,使用粉末压片进行样品制备,并通过经验系数校正基体效应。在无主成分元素信号干扰的范围内,能够选择性地测定磷和铁元素的特征X射线,提高了准确性并减少了时间消耗。提出了新方法的制样和测量条件;采用经验系数法验证了助催化剂样品的基体效应。实验结果表明,该方法的准确性和精密度令人满意,具有高重复性。元素的测量范围为磷0.01%-2.5%(质量分数,下同)、铁0.01%-2.5%,磷和铁的相对偏差分别为0.34%和0.59%。与化学法和电感耦合等离子体法(ICP)相比,该方法的结果一致性良好。它为最大丙烯产量的助催化剂中的磷和铁提供了分析值。这种新方法具有准确性好、精密度高、干扰少、样品处理简便和效率高的优点。此外,分析过程中样品不分解,每个样品仅需5分钟即可完成测量。这种新方法能够满足助催化剂中磷和铁含量定量分析不断增长的需求。该方法具有令人满意的准确性和精密度,分析范围广,已成功应用于助催化剂中磷和铁的测定。