Optimized sample preparation procedures for the analysis of solid materials by total-reflection XRF

Determination of the elemental composition of tissues of the cardiovascular system by atomic spectrometry, mass spectrometry and X-ray spectrometry methods

“…In order to obtain the layers of human biotissues [171], wet digestion was used for complete decomposition of the organic constituents. Other authors [172] used the method of microwave digestion in order to remove the matrix using HNO 3 and H 2 O 2 mixture. One can directly analyze by TXRF the thin cuts (0.5-60 µm) of the biotissues obtained using cryomicrotome and then freeze dried [173,174].…”

“…The sample treatment was optimized for different solid samples including their decomposition both in micro wave oven and Teflon autoclaves. The digestion proce dure was tested and optimized for several types of stan dard samples, including IAEA H 4 standard sample (animal muscle) [172]. The first method is as follows: after freeze drying concentrated HNO 3 and H 2 O 2 (5 : 1) were added to a 0.5-0.7 g sample (and the stan dard sample).…”

“…In study [172], TXRF was used for the analysis of different types of solid samples of biological and geo logical origin as well as environmental samples. The sample treatment was optimized for different solid samples including their decomposition both in micro wave oven and Teflon autoclaves.…”

Activities in the IAEA X‐ray fluorescence laboratory at Seibersdorf

“…Optimised sample preparation procedures (from the point of view of speed, precision, accuracy and completeness of digestion by applying a microwave oven and a PTFE bomb) were developed for total reflection XRF analysis of solid materials of biological, geological and environmental origin. 3 In order to follow the trends in the XRF field, the laboratory at Seibersdorf contributed to the development of portable XRF spectrometers and relevant methodologies for in situ applications 4 as well as a capillary-based x-ray microfluorescence system for microanalysis and microtomography. 5,6 To increase the direct benefits for laboratories in member states, the XRF laboratory at Seibersdorf provided analytical services (mostly for cross-check analysis) and organised worldwide proficiency tests (PTs) for biological materials and air particulates collected on filters-the PTs are now organised systematically, often in support of the laboratories involved in regional TC projects in the Asia and Pacific Region, Europe and Latin America.…”

Application de la fluorescence X à réflexion totale à l’étude des matières particulaires et des métaux lourds de la pollution de l’air dans la ville d’Antananarivo, Madagascar

“…Les échant illons à analyser par la technique de la fluorescence X à réflexion totale doive nt être solubilisés à haute pression dans une bombe d'attaque avec 600 III de CHCI 3 , 3 ml de HN0 3 (63 %) et 1 ml de H 2 0 2 (30 %) (suprapure) à une température de 165 "C pendant quatre heures [9] ; 200 III de cette solution préparée sont dilués dans 800 III d'eau bi-distillée ; 5 119 de coba lt (1 000 ppm) sont utilisés comme standard interne. Ensuite , 10 III de cette solution préparée sont déposés sur le réflecteur porte-échantillon (Quartz Synsil) , puis séchés dans le dessiccateur et enfin analysés.…”