Quantification of calcium, phosphorus, and cerium in novel biocompatible materials by total reflection X-ray fluorescence spectroscopy

A. A. Samoilova, N. V. Petrakova, N. A. Andreeva, T. N. Penkina, S. G. Dorofeev, D. G. Filatova
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引用次数: 0

Abstract

An approach to the determination of the composition of novel biocompatible materials based on cerium-containing calcium phosphates by TXRF is proposed. The ranges of analyte contents in solutions for the correct determination of Ca, P, Ce by the external standard method were determined. A systematic underestimation of the calcium signal at a Ca content in the analyzed composite sample above 30 mg/liter is noted. The Compton scattering spectra for the ceramic sample solution were analyzed to assess the compliance of the sample with the thin layer criterion, the maximum value was 16. 8 keV (96°). According to the graph of the mass attenuation coefficient for a film of a given composition, the attenuation of the calcium line is not related with the absorption effect of the sample. The internal standards (Gd and Cu) were selected and conditions for the determination of micro- and macro-components in solutions and suspensions of samples were determined. It is shown that with a calcium content up to 50 mg/liter in the sample, it is possible to determine correctly Ca, P, and Ce by TXRF method in solutions and suspensions with Sr 0.05 and 0.09, respectively. The convergence of the results obtained is noted by the methods of external and internal standards with appropriate dilutions of solutions and suspensions.
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用全反射x射线荧光光谱法定量测定新型生物相容性材料中的钙、磷和铈
提出了一种用TXRF法测定新型含铈磷酸钙生物相容性材料组成的方法。确定了外标法正确测定Ca、P、Ce的溶液中分析物的含量范围。注意到在所分析的复合样品中的钙含量高于30毫克/升时,钙信号的系统性低估。对陶瓷样品溶液的康普顿散射光谱进行分析,以评估样品是否符合薄层准则,其最大值为16。8 keV(96°)。由给定成分的薄膜的质量衰减系数曲线图可知,钙谱线的衰减与样品的吸收效应无关。选择内标Gd和Cu,确定样品溶液和悬浮液中微量和宏观组分的测定条件。结果表明,当样品中钙含量高达50 mg/l时,TXRF法可以正确测定溶液和悬浮液中Ca、P和Ce的Sr分别为0.05和0.09。采用适当稀释溶液和悬浮液的外标法和内标法,得到的结果具有收敛性。
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