zldmЗаводская лаборатория. Диагностика материаловIndustrial laboratory. Diagnostics of materials1028-68612588-0187ООО «Издательство «ТЕСТ-ЗЛ»10.26896/1028-6861-2026-92-5-16-19zldm-2825Research ArticleАНАЛИЗ ВЕЩЕСТВАSUBSTANCES ANALYSISСпектрофотометрическое определение кремния в образцах различного составаSpectrophotometric quantification of silicon in the samples of various compositionОвчинниковаО. А.OvchinnikovaO. A.

Ольга Александровна Овчинникова

119991, Москва, Ленинский просп., д. 49

Olga A. Ovchinnikova

49, Leninsky prosp., Moscow, 119334

ФоминаА. А.FominaA. A.

Алла Алексеевна Фомина

119991, Москва, Ленинский просп., д. 49

Alla A. Fomina

49, Leninsky prosp., Moscow, 119334

АндрееваН. А.AndreevaN. A.

Надежда Александровна Андреева

119991, Москва, Ленинский просп., д. 49

Nadezhda A. Andreeva

49, Leninsky prosp., Moscow, 119334

ПенкинаТ. Н.PenkinaT. N.

Татьяна Николаевна Пенкина

119991, Москва, Ленинский просп., д. 49

Tatiana N. Penkina

49, Leninsky prosp., Moscow, 119334

ФилатоваД. Г.FilatovaD. G.

Дарья Геннадьевна Филатова

119991, Москва, Ленинские горы, д. 1

Daria G. Filatova

1, bld. 3, Leninskie gory, Moscow, 119991

gak1.analyt@gmail.comИнститут металлургии и материаловедения им. А. А. Байкова Российской академии наукРоссияBaikov Institute of Metallurgy and Materials Science of the Russian Academy of SciencesRussian FederationМосковский государственный университет имени М. В. ЛомоносоваРоссияLomonosov Moscow State University, Department of ChemistryRussian Federation2026270520269251619Copyright © Овчинникова О.А., Фомина А.А., Андреева Н.А., Пенкина Т.Н., Филатова Д.Г., 20262026Овчинникова О.А., Фомина А.А., Андреева Н.А., Пенкина Т.Н., Филатова Д.Г.Ovchinnikova O.A., Fomina A.A., Andreeva N.A., Penkina T.N., Filatova D.G.Данная работа распространяется под лицензией Creative Commons Attribution 4.0.This work is licensed under a Creative Commons Attribution 4.0 License.https://www.zldm.ru/jour/article/view/2825

Фотометрический метод — рентабельный и простой в применении, результаты определения кремния данным методом характеризуются высокой воспроизводимостью. При этом учесть влияние матрицы на результаты фотометрического определения кремния с реагентом молибденовым синим сложнее, чем для определения методом атомно-эмиссионной спектрометрии с индуктивно-связанной плазмой (ИСП-АЭС). Для фотометрического определения кремния в образцах сложного переменного состава были опробованы методики ГОСТ 12346–78 для сталей и ГОСТ 2642.3–2014 для огнеупорных материалов. Предложена универсальная комбинированная процедура пробоподготовки для разложения образцов различного состава — катализаторов на основе оксида алюминия, руды, функциональных композитных материалов, которая подходит для всех анализируемых материалов с различным содержанием кремния. Добавление ЭДТА в процессе растворения плава позволяет маскировать примеси, влияющие на фотометрическое определение кремния, за счет образования прочных комплексонатов. Результаты определения кремния в данных образцах, полученные фотометрическим методом, совпали с результатами ИСП-АЭС в пределах погрешности 5 %. Отмечено, что результаты фотометрического определения кремния в рудных материалах характеризуются более низкой воспроизводимостью (sr ≥ 0,09), что связано со сложным переменным составом этих образцов. При этом воспроизводимость результатов фотометрического определения кремния в других материалах выше, чем полученных методом ИСП-АЭС.

The photometric method is cost-effective and easy to use, and the results of silicon determination using this method are highly reproducible. At the same time, it is more difficult to take into account the effect of the matrix on the results of photometric determination of silicon with the molybdenum blue reagent than for the determination by the ICP AES method. The procedures of GOST 12346–78 for steels and GOST 2642.3–2014 for refractory materials were tested for photometric determination of silicon in samples of complex variable composition. A universal method of sample preparation is proposed for the decomposition of samples of various compositions — catalysts based on aluminum oxide, ore, and functional composite materials. It is shown that the developed combined technique is suitable for all analyzed materials with different silicon content. The addition of EDTA during the dissolution of the melt makes it possible to mask impurities affecting the photometric determination of silicon due to the formation of strong EDTA complexes. The results of the determination of silicon in these samples obtained by the photometric method agree with the results of the ICP AES method within an error of 5%. It is noted that the results of photometric determination of silicon in ore materials are characterized by lower precision (sr ≥ 0.09), which is associated with the complex variable composition of these samples. At the same time, the precision of the results of silicon determination in other materials by this method is higher than those obtained by the ICP AES method.

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The authors declare that there are no conflicts of interest present.