gtcrustГеодинамика и тектонофизикаGeodynamics & Tectonophysics2078-502XInstitute of the Earth's crust of the Russian Academy of Sciences, Siberian Branch10.5800/GT-2022-13-2s-0601gtcrust-1437Research ArticleПАЛЕОГЕОДИНАМИКАPALEOGEODYNAMICSПРИМЕНЕНИЕ МЕТОДА РЕНТГЕНОФЛУОРЕСЦЕНТНОЙ СПЕКТРОМЕТРИИ С ПОЛНЫМ ВНЕШНИМ ОТРАЖЕНИЕМ (TXRF) К ГЕОЛОГИЧЕСКИМ ОБЪЕКТАМ: ОПЫТ ЛАБОРАТОРИИ TXRF (ЦКП «ГЕОДИНАМИКА И ГЕОХРОНОЛОГИЯ»)APPLICATION OF TOTAL-REFLECTION X-RAY FLUORESCENCE SPECTROMETRY (TXRF) TO GEOLOGICAL OBJECTS: EXPERIENCE OF THE TXRF LABORATORY, CENTER FOR GEODYNAMICS AND GEOCHRONOLOGYМальцевА. С.MaltsevA. S.

664033, Иркутск, ул. Лермонтова, 128

128 Lermontov St, Irkutsk 664033

ПашковаГ. В.PashkovaG. V.

664033, Иркутск, ул. Лермонтова, 128

128 Lermontov St, Irkutsk 664033

Институт земной коры СО РАНРоссияInstitute of the Earth’s Crust, Siberian Branch of the Russian Academy of SciencesRussian Federation202229032022132601601Copyright © Мальцев А.С., Пашкова Г.В., 20222022Мальцев А.С., Пашкова Г.В.Maltsev A.S., Pashkova G.V.Данная работа распространяется под лицензией Creative Commons Attribution 4.0.This work is licensed under a Creative Commons Attribution 4.0 License.https://www.gt-crust.ru/jour/article/view/1437

В отличие от традиционной рентгенофлуоресцентной спектрометрии, рентгенофлуоресцентная спектрометрия с полным внешним отражением не является распространенным и рутинным методом анализа твердых образцов с минеральной матрицей, но имеет большой потенциал для геохимических, геологических и археологических исследований. Быстрый многоэлементный анализ очень малого количества образца может быть выполнен с помощью способа внутреннего стандарта, который не требует стандартных образцов для калибровки. Это несомненное преимущество метода TXRF по сравнению с традиционным рентгенофлуоресцентным методом, особенно при ограниченном количестве доступного материала объекта и отсутствии подходящих эталонных образцов. В этой статье представлен наш опыт применения TXRF-спектрометрии для элементного анализа апатита, керамики, осадков, руд и конкреций. Особое внимание уделено процедуре пробоподготовки, поскольку она является одним из основных источников ошибок при анализе. Приготовить тонкий однородный образец из твердого образца со сложной минеральной матрицей непросто. Стратегию пробоподготовки следует выбирать с учетом особенностей аналитического объекта, содержания определяемых элементов и точности, необходимой для надежной интерпретации. Рассмотрены примеры приготовления суспензии для экспресс-анализа руд и осадков, оригинальные процедуры химического разложения апатита и керамики.

Unlike conventional X-ray fluorescence spectrometry, the total-reflection X-ray fluorescence spectrometry is not a widespread and routine method for analyzing solid samples with mineral matrix, but it has a great potential for geochemical, geological, and archaeological studies. Rapid multi-elemental analysis of very small sample amounts can be performed by the internal standard method which does not require the matrix-matched reference materials. This is an undoubted advantage of the TXRF method over the conventional X-ray fluorescence method, especially if there is a limited available sample amount and a lack of well-characterized reference materials. This paper presents our experience with the application of TXRF spectrometry in the elemental analysis of apatite, ceramics, sediments, ores, and nodules. Special attention has been paid to the sample preparation procedure because it is one of the main sources of errors in the analysis. Preparing thin homogeneous specimen from the solid sample with a complex mineral matrix is not easy. Sample preparation strategy should be chosen considering the features of an analytical object, the content of the elements to be determined, and the accuracy required for a reliable interpretation. Consideration is being given to the examples of the preparation of a suspension for rapid analysis of ores and sediments, and to the original techniques of chemical decomposition for apatite and ceramics.

рентгенофлуоресцентный анализ с полным внешним отражениеммногоэлементный анализпробоподготовкаоценка точностиапатитрудыконкрециикерамикаосадкиtotal-reflection X-ray fluorescencemulti-elemental analysissample preparationaccuracy assessmentapatiteoresnodulesceramicssedimentsИсследования выполнены на оборудовании Центра коллективного пользования «Геодинамика и геохронология» Института земной коры СО РАН (грант № 075-15-2021-682)The research was performed using the equipment of the Centre for Geodynamics and Geochronology of the Institute of the Earth’s Crust SB RAS (grant 075-15-2021-682)ReferencesAkhmetzhanov T.F., Pashkova G.V., Chubarov V.M., Labutin T.A., Popov A.M., 2021. Three Calibration Techniques Combined with Sample-Effective Design of Experiment Based on Latin Hypercube Sampling for Direct Detection of Lanthanides in REE-Rich Ores Using TXRF and WDXRF. 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The authors declare that there are no conflicts of interest present.