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Magnetite surface area titration using nitric oxide, II. Pretreatment effects and silica-supported samples

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Abstract

The use of NO adsorption for determination of Fe3O4 surface areas has been examined and extended, from earlier work on unsupported samples, to silica-supported Fe3O4. Gravimetric studies confirm earlier suggestions that the irreversible NO adsorption uptake on unsupported Fe3O4 is dependent upon sample pretreatment. Long (ca. 24 h) vacuum treatment at 650 K leads to increased apparent NO adsorption uptakes due to reduction of the surface. Magnetite particle size estimates were made using irreversible NO adsorption uptakes on silica-supported Fe3O4 samples that had received a “standard” 1 h vacuum pretreatment at 650 K. These estimates agreed well with average particle sizes calculated using x-ray line-broadening and magnetization measurements, indicating that NO adsorption can, in fact, be used to measure magnetite surface areas on silica-supported samples.

Abstract

Использование адсорбции NO для определения поверхности Fe3O4 было проверено и далее разработано, исходя из более ранних работ для образцов без носителя, для Fe3O4 нанесенного на окись кремния. Гравиметрические исследования подтверждают более ранние предположения о том, что необратимая адсорбция NO на Fe3O4 без носителя зависит от предварительной обработки образца. Продолжительная (октоло 24 часов) вакуумная обработка при 650 К приводит к увелицению кажущейся адсорбции NO вследствие восстановления поверхности. Определение размера частиц магнетита было проведено, используя необратимую адсорбцию NO на образцы Fe3O4, нпнесенные на окись кремния, получившие „стандартную” 1-часовую предварительную вакуумную обработку при 650 К. Эти определеления хорошо согласуются со средними размерами частиц, рассчитанными из уширения рентгеновской линии и измерения намагничиваемости, указывая, что адсорбция NO может, фактически, быть использована для измерения поверхности магнетита на образцах с носителем окиси кремния.

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References

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Author notes

  1. Yi Chen (Visiting Scholar)

    Present address: Department of Chemistry, Nanking University, People's Republic of China

Authors and Affiliations

  1. Department of Chemical Engineering, University of Wisconsin, 53706, Madison, Wisconsin, USA

    J. E. Kubsh, C. R. F. Lund, Yi Chen (Visiting Scholar) & J. A. Dumesic

Authors
  1. J. E. Kubsh
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  2. C. R. F. Lund
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  3. Yi Chen
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  4. J. A. Dumesic
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Additional information

Camille and Henry Dreyfus Foundation Teacher-Scholar; to whom all correspondence should be addressed.

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Kubsh, J.E., Lund, C.R.F., Chen, Y. et al. Magnetite surface area titration using nitric oxide, II. Pretreatment effects and silica-supported samples. React Kinet Catal Lett 17, 115–119 (1981). https://doi.org/10.1007/BF02069526

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  • DOI: https://doi.org/10.1007/BF02069526

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