Determination of major nonmetallic impurities in magnesium by glow discharge mass spectrometry with a fast flow source using sintered and pressed powder samples

Abstract

Fast flow glow discharge mass spectrometry with a Grimm-type ion source providing a high sputter rate was used for the determination of major nonmetallic impurities in magnesium. The analytical signal was found to be strongly influenced by the electrical discharge parameters. For calibration by standard addition, synthetic standard samples were produced in two different ways-namely, by pressing and by sintering doped metal powders. The observed sensitivity of the calibration curves was shown to depend on the particle size of the powder. For the magnesium powders, the mass fractions of oxygen, nitrogen, boron, and silicon were determined to be about 0.01 kg·kg(-1) (relative standard deviation approximately 10-20 %), 2,700 mg·kg(-1), 150 mg·kg(-1), and 300 mg·kg(-1), respectively.

Mass Spectrometry‐based Techniques for Direct Quantification of High Ionization Energy Elements in Solid Materials—challenges and Perspectives

“…As was already mentioned, the Penning process is ineffective for N, O, Cl, and Br, so their ionization occurs only via electron impact and charge transfer mechanisms. The quantification of these elements is possible in conventional discharge (Shekhar et al, 2003; Kikuta, Asano, & Kikuchi, 2007; Gonzalez‐Gago et al, 2014; Plotnikov et al, 2014), but requires additional efforts compared to the elements effectively ionized in Penning process.…”

“…Halogens may be used as proxies for the evolution of hydrothermal fluids and ore deposits as well as for lithosphere and mantle circulations (Harlov & Aranovich, 2018). In material sciences, it is often required to control for the nonmetals as doping components or impurities; for instance, the determination of chlorine (Ganeev et al, 2012), oxygen (Itoh, Oguro, & Kobayashi, 2006), nitrogen (Tsuge, Tarutani, & Kudo, 1988; Itoh, Oguro, & Kobayashi, 2007; Ganeev et al, 2011; Hertzman & Charles, 2012) in steels and other alloys (Kikuta, Asano, & Kikuchi, 2007; Plotnikov et al, 2014); the quantification of oxygen (Gubal et al, 2018) and fluorine (Bodnar et al, 2018) in optical crystals and battery components.…”

“…Oxygen and nitrogen are the main constituents of the atmosphere and are widely distributed in the environment in general. Thus, it is often necessary to control for their presence in high purity materials, first of all, in metals and semiconductors (Tsuge, Tarutani, & Kudo, 1988; Tanaka et al, 1991; Itoh, Oguro, & Kobayashi, 2006, 2007; Kikuta, Asano, & Kikuchi, 2007; Ganeev et al, 2011; Hertzman & Charles 2012; Plotnikov et al, 2014; Davari et al, 2019). Oxygen impurities in fluoride‐based solid‐state batteries and working bodies of the laser setups (Chuchina et al, 2020) considerably reduces their properties.…”

A study of matrix and admixture elements in fluorine‐rich ionic conductors by pulsed glow discharge mass spectrometry

“…Glow discharge mass spectrometry (GDMS) is a promising technique for analyzing a variety of solids 33–35 . GDMS allows for the effective quantification of admixture elements in conducting materials and dielectrics 33,34,36,37 and it is also capable of elemental and isotopic analysis of minerals, 38–40 powders, 41 and microparticles, 42 and layer‐by‐layer analysis of thin films and coatings 43,44 . The main benefits of the GDMS‐based methods are accuracy, scanning speed, and narrow sensitivity drifts between different elements, significantly simplifying the calibration procedure 33 .…”

“…In recent years, there have been several studies devoted to the use of GDMS for the quantification of high‐ionization‐energy elements such as F, O, N, and Cl 23,41,45–48 . The complications in the determination of these elements are described in detail in previous publications 23,24,41,45 . In brief, these complications are related, first, to the low‐efficiency ionization of these elements in conventional argon glow discharge due to their high ionization energies.…”