A prepared flat sample is mounted on the glow discharge source, the source is evacuated and backfilled with argon. Authors: Pahl, M; Weimer, U Publication Date: Mon Sep 01 00:00:00 EDT 1958 Research Org. Spectrochimica Acta Part B: Atomic Spectroscopy 1995 , 50 (1) , 13-25. Since the sample preparation for GDMS analysis is very simple and samples can be directly analyzed, the risk of contamination is low. The analysis of nonconducting materials by dc GDMS is difficult due to charge-up effects on the sample surface. The GD ion source gained popularity in the past two decades on account of its stability, sensitivity and operational simplicity. The Astrum is designed to test high purity materials with the best detection limits. RF-GDMS permits the analysis of conducting as well as semiconducting or nonconducting materials without major restriction (Marcus, 1996). An example is the sorption or desorption of actinides in various host rocks or technical barrier materials. By continuing you agree to the use of cookies. Both, initial raw materials and fuel pellets were studied (De la Heras et al., 2000). 1 mbar. Other versions of this article Annemie Bogaerts ... and the photons or ions created in this way can be detected with optical emission spectroscopy or mass spectrometry. A prepared flat sample is mounted on the glow discharge source, the source is evacuated and backfilled with argon. GDMS is used for the determination of trace elements in bulk solid samples, but it was also successfully applied for the fast analysis (without chemical separation, like for ICP-MS and TIMS) of uranium (Ganeev et al., 2017) and plutonium isotopes (Betti and Aldave de las Heras, 2004). These types of studies, which imply depth information, are important for the conception and planning of nuclear waste repositories, and GDMS is a highly versatile tool for that purpose (Betti and de las Heras, 2004). There is a newer version of this article Robert E. Steiner. Almost all GDMS, which can sample many elements in one analysis and generally has sensitivity of ppba, appears to be the most useful analytical method (Bollong et al., 1995). mass spectrometry, is the so-called Grimm source(8) and derivations of it. Moreover, another method has recently been proposed in the literature, which tries to suppress the cluster interferences by sampling from a reversed hollow cathode ion source. 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. GDMS involves the sputtering of usually a solid sample (liquid as a dried solution) by Ar+ ions produced in gas glow discharge. Due to charge-up effects on the sample, the analysis of nonconducting materials is difficult by GDMS. The schematic of a glow discharge ion source is illustrated in Fig. Major work was done by Betti’s working group using the VG 9000 to characterize radioactive waste materials in electrically conducting and nonconducting materials, e.g., for different types of nuclear fuels, alloys containing Pu and U, cladding materials, and nuclear waste glasses. To illustrate this, Figure 7 presents a part of the mass spectrum (m/z 90–100) of a pure iron sample, both in argon and in neon. neon instead of argon. This serves as the cathode for a low-pressure argon plasma, burning at a pressure of ca. If attention is focused on only one, or a few impurities, more sensitive techniques such as sputter initiated resonant ion spectroscopy may be appropriate (Tower et al., 1996; Sen et al., 1996). At least three commercial instruments were already available in the early 1990s. Introduced into the plasma, it influences the signal by quenching metastable atoms and by forming oxide complexes with the analyte. Furthermore, it was found in the same study that both Zn and Se substitution enhances, and hydrogen purging reduces, the uptake of these contaminants. Atomic Spectroscopy. It is capable of analyzing, conducting, semi … The titanium specimen to be analyzed may be in the form of a disk, casting, foil, sheet, plate, extrusion or some other wrought form or shape. Finally, the clusters can also be used for quantification. The surface oxides on the high-purity elements, the residual gases, and the hydrocarbon vapors from the evacuation system were identified as well as sources of contamination from infrared absorption experiments [121]. 8.15. Typically, from 10 to 100 Pa of Ar is used to produce sufficient ions, which are accelerated toward the sample on the cathode surface, with energies from hundreds to thousands eV. 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The typical discharge operation conditions for GD–MS are 1–5 mA, 800–1500 V and 0.2–2.0 torr. The optimal working conditions for the detection of Ga and In by proposed method are 660 V discharge voltage, 3.0 mL min −1 solution flow rate and pH = 1.0 HNO 3 as supporting electrolyte. 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 precise and accurate measurement of isotope ratios is a further application of GDMS, which is of high relevance, for example, in nuclear forensics. In another study, such acceptors as Li, Na, K, As, Cu, Ag, Sb, and Bi, donors as Al, Cl, Ga, In, and Tl, and neutral elements as Si, Ca, Cr, Co, Sn, and Pb, were identified as classical residual impurities in as-grown p-type VB CdTe crystals [274]. The DIP is placed through the clamp assembly and the rf feedthrough is placed directly behind the sample (cathode), which locks it in place. A common problem in GDMS, as in most mass spectrometric methods, is the occurrence of spectral interferences in the mass spectrum, e.g. Positive ions from the glow discharge are emitted via an exit aperture through the anode and are analyzed usually by a double-focusing mass spectrometer, for example, in reverse Nier–Johnson geometry like the commercial VG-9000 instrument (Winsford, UK), as sketched in Fig. Unsurprisingly, it has developed into the most prominent GD coupling. Tomashik, in, CdTe and Related Compounds; Physics, Defects, Hetero- and Nano-structures, Crystal Growth, Surfaces and Applications, Binary and Multinary II–VI Compounds (CdTe, CdZnTe, CdMnTe) Grown from the Melt, Reference Module in Materials Science and Materials Engineering, . From: CdTe and Related Compounds; Physics, Defects, Hetero- and Nano-structures, Crystal Growth, Surfaces and Applications, 2010, C. Derrick QuarlesJr, ... R. Kenneth Marcus, in Encyclopedia of Spectroscopy and Spectrometry (Third Edition), 2017. Betti and coworkers detected trace and ultratraces of radioisotopes in soils, sediments, and vegetation by GDMS (Betti et al., 1996). GDMS :: GLOW DISCHARGE MASS SPECTROMETRY. For the color version of the figure, the reader is referred to the online version of the book. In general, the investigation of the diffusion mechanism of trace elements is an important aspect in the characterization of environmental processes. Thanks to the use of a pulsed RF source, coupled with a high resolution optical spectrometer, the GD Profiler 2 provides an excellent depth resolution, allowing the fast evaluation of the coating quality. Vous n'avez pas de compte? 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. Using a pulsed glow discharge, U contents and 235U/238U isotope ratios were studied in Chernobyl microparticles (Ganeev et al., 2017). Figure 7. Clemens Walther, Klaus Wendt, in Handbook of Radioactivity Analysis (Fourth Edition), 2020. The maximum doping levels achievable in bulk CdTe are of some 1017 cm−3 for holes (As, P, Li) and about 1018 cm−3 for electrons (Al, I, In), very close to the deviations from stoichiometry on both Cd and Te sides. 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. One key difference between MS and optical detection techniques is that the sample material must be physically transferred out of the source. Providing complete material characterization mainly for metallurgy, the Thermo Scientific Element GD Plus GD-MS system features a fast glow discharge ion source in a high-resolution mass spectrometer. If this end is discarded, the remaining crystal has purity adequate for most applications. The sputtering produces atoms for excitation that takes place away from the sample surface. The application of glow discharge mass spectrometry (GDMS) in the Geosciences has been limited largely to the elemental analysis of soils, meteorites, and ceramics. The simplest type of glow discharge is a direct-current glow discharge. 13.5 (lower part in the middle). 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