The Astrum is designed to test high purity materials with the best detection limits. Three-dimensional mathematical models of the behaviour of the different species in a dcGD in argon were used to study the influence of the dimensions of flat-cathode/hollow-anode cylindrical cells on the calculated plasma quantities. Glow discharge analytical spectro-metric techniques are based on the detection and quan-tification of sample species within the plasma. For the handling of highly radioactive nuclear materials, GDMS systems are operated in sealed glove boxes (Betti et al., 1994). The analysis of nonconducting materials by dc GDMS is difficult due to charge-up effects on the sample surface. Atomic Spectroscopy. It appears that most peak intensities in this mass range are significantly decreased in the neon discharge. Search Copyright © 2021 Elsevier B.V. or its licensors or contributors. Analyte ions are extracted by electrostatic lenses and transferred through a mass analyser for eventual detection. Miroslav Ješkovský, ... Pavel P. Povinec, in Handbook of Radioactivity Analysis: Volume 2 (Fourth Edition), 2019. The rf-powered DIP must meet several design requirements including efficient coupling of the rf power to the sample, isolation of the sputtering to the sample surface and effective shielding of potential radiated power losses. When the spectrometer is operated in high resolution mode, this provides a powerful technique for the analysis of all trace and ultra-trace elemental constituents of inorganic materials. This allows cryogenic cooling of the discharge cell to remove trace impurities (which tend to decrease sputtering rates and result in the formation of molecular ions that increase spectral complexity) from the discharge gas. The glow discharge source is shown enlarged and worked out in more detail. Finally, advances in the use of GD ionization sources as detectors in gas and liquid chromatography separations will also be described. However, the application of GDMS in the determination of radionuclides is limited due to its low sensitivity and limited accessibility (Hou and Roos, 2008). Control of stoichiometry during growth, e.g., by providing a cadmium reservoir, can influence the uptake and activation of impurities through second phases and vacancies. Offrant une caractérisation complète des matériaux, principalement dans le domaine de la métallurgie, le système GD-MS Thermo Scientific Element GD Plus intègre une source d’ions à décharge luminescente rapide dans un spectromètre de masse à haute résolution. Direct investigations are carried out by means of GDMS (Barshick et al., 1998), whereas a comparison with TIMS once again showed that GDMS is competitive in terms of precision and accuracy for the relevant elements (Mayer et al., 2005). Glow Discharge Spectrometry utilizes a low-pressure, non-thermal process in which material is uniformly sputtered from the sample surface by a stream of argon ions. The sputtered atoms are ionized in this plasma and extracted into the mass spectrometer for separation and detection. This clearly demonstrates that these peaks are interfering peaks due to ArFe+ clusters, which can be avoided by using neon as the discharge gas. Glow Discharge Optical Spectroscopy and Mass Spectrometry. 1998a,b). Ecuyer, ... Z.F. In GDMS, an argon gas glow discharge (GD) at a pressure of 0.1–10 torr is used as an ion source. Spectrochimica Acta Part B: Atomic Spectroscopy 1995 , 50 (1) , 13-25. Depending on the specific sample material, either a direct current (dc) or radiofrequency (RF) power is used as the ion source. In this work, certified marine sediment doped with 237Np was used for the calibration strategy. The GD90 is a high resolution Glow Discharge Mass Spectrometer offering direct determination of elemental content (matrix to subtrace) in a variety of materials. Annemie Bogaerts, in Encyclopedia of Spectroscopy and Spectrometry, 1999. Samples ranging from 1 to 5 mm in diameter can be analysed directly without excessive machining. The Ar+ ions are accelerated by the source potential of a few hundred volts and sputter off sample constituents as atoms, ions, molecules, and clusters. Other impurities probably do so as well. Such a system provides high transmission (>75%) and a mass resolution of up to m/Δm ≈ 10,000. It is also frequently applied to the characterization of nuclear samples (Betti, 1996) as well as nuclear forensics (Betti et al., 1999). Indeed, it was found that the analyte ions are characterized by a peak at high energy, whereas argon ions and cluster ions possess a peak at low energy. Due to its getter capability for oxygen, tantalum is used specifically as a secondary cathode material as well. Glow Discharge Spectrometry (GDS) is an analytical method for direct determination of the elemental composition of solid samples. Pulsed RF Glow Discharge Spectrometers Ultra Fast Elemental Depth Profiling. Routinely, materials used for nuclear fuel production are tested by dc-GDMS on their isotopic composition of major elements and the concentration of trace elements, which might lead to severe radiocontaminations by neutron capture in the reactor. Glow discharge mass spectrometry (GD-MS) is one of the most comprehensive and sensitive techniques currently available for determining the composition of solid materials [1, 2].As a combined tandem source [], separation of the sputtering (sampling) and ionization processes in the GD provides a response that is, to a first approximation, independent of the sample matrix [4–6]. Although the electrical activity of impurities can be hampered by self-compensation from native defects or other residual impurities and by gettering of impurities into Te precipitates, p-type and n-type doping of CdTe is easy to achieve; here, the elements of the first and fifth columns of the periodic chart act as acceptors and those of the third and seventh columns as donors. The growth process is the primary area of concern. Similar results have been found for shallow acceptor levels associated with oxygen [39, 40]. Clemens Walther, Klaus Wendt, in Handbook of Radioactivity Analysis (Fourth Edition), 2020. The relative sensitivity factor (RSF) values were obtained from a comparison with other methods such as ICP-MS and ICP-AES in analyzing uranium metal specimens of different origin. Furthermore, it was found in the same study that both Zn and Se substitution enhances, and hydrogen purging reduces, the uptake of these contaminants. RF-GDMS permits the analysis of conducting as well as semiconducting or nonconducting materials without major restriction (Marcus, 1996). Thin and Thick films analysis. Elemental analysis by GD-MS provides substantial advantages over competing techniques in that it responds to metals and non-metals, exhibits a high sensitivity, suffers from minimal matrix effects and provides isotopic information. Due to charge-up effects on the sample, the analysis of nonconducting materials is difficult by GDMS. The primary complicating factor in GD-MS source design is the need to accommodate the ion source volume within the main vacuum chamber. A small population of atoms within the cell is initially ionized through random processes (collisions between atoms or with alpha particles, for example). The Finnigan ELEMENT GD, a combination of a glow discharge ion source with a high resolution mass spectrometer, is the ultimate tool for the direct analysis of conductive materials. GDMS supported the possibility of oxygen as all samples contain >90 ppb O. ScienceDirect ® is a registered trademark of Elsevier B.V. ScienceDirect ® is a registered trademark of Elsevier B.V. URL: https://www.sciencedirect.com/science/article/pii/B978012803224400056X, URL: https://www.sciencedirect.com/science/article/pii/B978012814397100008X, URL: https://www.sciencedirect.com/science/article/pii/B978012384873400013X, URL: https://www.sciencedirect.com/science/article/pii/B9780128143957000039, URL: https://www.sciencedirect.com/science/article/pii/S0167924402800105, URL: https://www.sciencedirect.com/science/article/pii/B0122266803001071, URL: https://www.sciencedirect.com/science/article/pii/B9780080965130000017, URL: https://www.sciencedirect.com/science/article/pii/B978012803581802395X, CdTe and Related Compounds; Physics, Defects, Hetero- and Nano-structures, Crystal Growth, Surfaces and Applications, 2010, Inductively Coupled Plasm Mass Spectrometry (ICPMS), Encyclopedia of Spectroscopy and Spectrometry (Third Edition), Handbook of Radioactivity Analysis (Fourth Edition), Harrison, 1988; Betti and de las Heras, 2004; Venzago and Pisonero, 2015, Duckworth et al., 1993; Barshick et al., 1993, 2000, Van Straaten et al., 1994; Venzago and Weigert, 1994, Inorganic Mass Spectrometry of Radionuclides, Handbook of Radioactivity Analysis (Third Edition), Miroslav Ješkovský, ... 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