zldmЗаводская лаборатория. Диагностика материаловIndustrial laboratory. Diagnostics of materials1028-68612588-0187ООО «Издательство «ТЕСТ-ЗЛ»10.26896/1028-6861-2023-89-5-14-18zldm-1928Research ArticleАНАЛИЗ ВЕЩЕСТВАSUBSTANCES ANALYSISОпределение кальция, фосфора и церия в новых биосовместимых материалах методом рентгенофлуоресцентного анализа с полным внешним отражениемQuantification of calcium, phosphorus, and cerium in novel biocompatible materials by total reflection X-ray fluorescence spectroscopyСамойловаА. А.SamoilovaA. A.

Алина Александровна Самойлова

119991, Москва, Ленинские горы, д. 1, стр. 3

Alina A. Samoilova

1-3, Leninskiye Gory, Moscow, 119991

gak1.analyt@gmail.comПетраковаН. В.PetrakovaN. V.

Наталия Валерьевна Петракова

119334, Москва, Ленинский пр-т, д. 49

Nataliya V. Petrakova

49, Leninsky prosp., Moscow, 119334

АндрееваН. А.AndreevaN. A.

Надежда Александровна Андреева

119334, Москва, Ленинский пр-т, д. 49

Nadezhda A. Andreeva

49, Leninsky prosp., Moscow, 119334

ПенкинаТ. Н.PenkinaT. N.

Татьяна Николаевна Пенкина

119334, Москва, Ленинский пр-т, д. 49

Tatiyana N. Penkina

49, Leninsky prosp., Moscow, 119334

ДорофеевС. Г.DorofeevS. G.

Сергей Геннадьевич Дорофеев

119991, Москва, Ленинские горы, д. 1, стр. 3

Sergey G. Dorofeev

1-3, Leninskiye Gory, Moscow, 119991

ФилатоваД. Г.FilatovaD. G.

Дарья Геннадьевна Филатова

119991, Москва, Ленинские горы, д. 1, стр. 3; 119334, Москва, Ленинский пр-т, д. 49

Dariya G. Filatova

1-3, Leninskiye Gory, Moscow, 119991; 49, Leninsky prosp., Moscow, 119334

Московский государственный университет имени М. В. Ломоносова, химический факультетРоссияLomonosov Moscow State UniversityRussian FederationИнститут 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. Ломоносова, химический факультет; Институт металлургии и материаловедения им. А. А. Байкова Российской академии наукРоссияLomonosov Moscow State University ; Baikov Institute of Metallurgy and Materials Science of the Russian Academy of SciencesRussian Federation2023260520238951418Copyright © Самойлова А.А., Петракова Н.В., Андреева Н.А., Пенкина Т.Н., Дорофеев С.Г., Филатова Д.Г., 20232023Самойлова А.А., Петракова Н.В., Андреева Н.А., Пенкина Т.Н., Дорофеев С.Г., Филатова Д.Г.Samoilova A.A., Petrakova N.V., Andreeva N.A., Penkina T.N., Dorofeev S.G., 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/1928

Предложен подход к определению состава новых биосовместимых материалов на основе церийсодержащих фосфатов кальция методом РФА ПВО. Определены диапазоны содержаний аналитов в растворах для правильного определения Ca, P, Ce методом внешнего стандарта. Отмечено систематическое занижение сигнала кальция при его содержании в анализируемой пробе композита выше 30 мг/л. Для оценки соответствия пробы критерию тонкого слоя проведен анализ спектров комптоновского рассеяния для раствора образца керамики, значение максимума составило 16,8 кэВ (96°). Согласно графику массового коэффициента ослабления для пленки заданного состава ослабление интенсивности линии кальция перпендикулярно подложке не связано с поглощением образца. Выбраны внутренние стандарты (Gd и Cu) и найдены условия для определения микро- и макрокомпонентов в растворах и суспензиях образцов. Показано, что при содержании кальция в пробе до 50 мг/л возможно правильное определение Ca, P и Ce методом РФА ПВО в растворах и суспензиях с Sr 0,05 и 0,09 соответственно. Отмечена сходимость результатов, полученных методами внешнего и внутреннего стандарта при соответствующих разбавлениях растворов и суспензий.

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