Abstract

Modern express methods of analytical control are widely used for monitoring the quality of oxide materials. However, the possibilities of these methods are currently limited by the lack of versatile homogeneous reference materials (RMs). Such RMs can be produced most effectively by vitrification methods. In this connection, glassy RMs based on bismuthborate systems are of great interest. In the earlier research, bismuth-borate RMs were used for comparison purposes in determining the composition of complex oxide systems using the X-ray fluorescence method. This work considers issues associated with the synthesis and application of bismuth-borate glassy RMs for determining the content of transition elements in oxide compounds and mixtures using luminescence analysis. Luminescence analysis was used as a research method due to its high selectivity and low detection limits with respect to elemental impurities in controlled objects (usually constituting 1 · 10–6–1 · 10–4 wt %). Bismuth-borate glassy RMs are shown to be capable of luminescence under UV radiation in the visible range at the temperature of 77 K. It is established that the introduction of the oxides of transition and rare earth elements (REE) into the RM composition leads to the quenching of the exciton emission band in the glasses studied at 77 K, as well as to the appearance of bands typical of REE ion radiation both at 77 K and at 298 K. Glassy RMs doped with transitionelement oxides are found to quench the luminescence of both bismuth and REE ions at the temperature of 77 K. On the basis of the results obtained, procedures for determining the content of quenching elements in oxide materials have been developed. The metrological characteristics of these procedures have been evaluated.

Highlights

  • Поступила в редакцию 13 декабря 2018 г., после доработки – 2​ 0 января 2019 г

  • The possibilities of these methods are currently limited by the lack of versatile homogeneous reference materials (RMs)

  • This work considers issues associated with the synthesis and application of bismuth-borate glassy RMs for determining the content of transition elements in oxide compounds and mixtures using luminescence analysis

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Summary

USE OF REFERENCE MATERIALS

Рассмотрены проблемы синтеза и применения висмутатно-боратных стеклообразных образцов сравнения для определения содержания переходных элементов в составе оксидных соединений и смесей методом люминесцентного анализа. В качестве альтернативных методов для определения содержания переходных элементов в составе образцов (в частности, меди) использовали методы рентгенофлуоресцентного (РФлА) и атомно-абсорбционного анализа (ААА). Результаты исследования и их обсуждение До настоящего времени не проводились люминесцентные исследования возможности применения висмутатно-боратных стеклообразных образцов для определения переходных элементов и редкоземельных ионов (РЗИ) в составе сложных оксидных систем с использованием эффекта тушения собственной полосы люминесценции РЗИ и экситонной полосы излучения ионов Bi3+ при температуре 77К. Анализ экспериментальных результатов позволил предположить, что уменьшение интенсивности излучения ионов Bi3+ происходит по гиперболическому закону и предложить для описания зависимости величины относительной люминесценции от содержания иона переходного элемента уравнение Штерна-Фольмера: Fig. 2 Dependency of the luminescence intensity of bismuth-borate glassy RMs doped with Fe (III), Co

Объект анализа CuO
Метод анализа
Анализируемый компонент
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