Pulsed glow discharge enables direct mass spectrometric measurement of fluorine in crystal materials – Fluorine quantification and depth profiling in fluorine doped potassium titanyl phosphate

Bodnar, Victoria; Ганеев, А. А.; Gubal, Anna; Solovyev, Nikolay; Glumov, O. V.; Yakobson, Viktor; Murin, I. V.

doi:10.1016/j.sab.2018.04.002

Cited by 24 publications

(15 citation statements)

References 69 publications

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“…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.…”

Section: Introductionmentioning

confidence: 99%

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

Gubal

Chuchina

Sorokina

et al. 2020

Mass Spectrometry Reviews

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The determination of nonmetals, first of all, the most electronegative ones—nitrogen, oxygen, fluorine, chlorine, and bromine, poses the highest challenge for element analysis. These elements are characterized by high reactivity, volatility, high ionization energy, and the absence of intensive spectral lines in the optical spectral range. Conventional techniques of their quantification include considerable “wet chemistry” stages so the application of these techniques for the solid sample is highly laborious and prone to uncontrollable uncertainties. Additionally, current development in material science and other areas requires the quantification of the elements at lower levels with good sensitivity. Owing to their robustness and flexibility, mass spectrometry techniques provide vast possibilities for the quantification, spatial and isotopic analysis, including the solutions for direct analysis of solids. The current review focuses on the application of major mass spectrometric techniques for the quantification of N, O, F, Cl, and Br in solid samples. The following techniques are mainly considered: thermal ionization mass spectrometry (TIMS), isotope‐ratio MS (IRMS), secondary ion MS (SIMS), inductively coupled plasma MS (ICP‐MS), and glow discharge MS (GDMS); as the most accessible and widely applied for the purpose. General ionization issues, advantages, limitations, and novel methodological solutions are discussed. © 2020 John Wiley & Sons Ltd.

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Section: Introductionmentioning

confidence: 99%

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

Gubal

Chuchina

Sorokina

et al. 2020

Mass Spectrometry Reviews

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“…In the current study, previously reported methods 23,24 employing high‐energy electron ionization or a high‐ionization‐energy discharge medium were adopted for the analysis of fluorine‐rich materials. It should be noted that the use of neon as the discharge medium is optimal for fluorine quantification, especially at low concentration levels, but it considerably reduces the sensitivities for heavy elements, such as rare earth metals.…”

Section: Resultsmentioning

confidence: 99%

“…determining most matrix components simultaneously, of fluorine‐rich materials would require accurate quantification of fluorine over a quite wide dynamic range, which is a nontrivial and challenging analytical task. As has been discussed in previous studies, 23,24 the majority of current analytical techniques available fail with that to a certain extent. For instance, the widely used ICP‐MS technique is virtually inapplicable for the quantification of fluorine due to its high ionization energy and interferences in high‐pressure argon plasma 25 .…”

Section: Introductionmentioning

confidence: 96%

“…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.…”

Section: Introductionmentioning

confidence: 99%

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

Chuchina

Gubal

Lyalkin

et al. 2020

Rapid Comm Mass Spectrometry

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Rationale: Dopants in ionic conductors play a crucial role in achieving the required electrochemical properties. A slight variation in their concentration considerably affects the conductivity of crystals and their applicability as ionic conductors and laser materials. To ensure the growth of high-quality fluoride crystals, adequate approaches for the quantification of matrix and admixture/dopant components are required. Methods: A panel of SrF 2 -and GdF 3 -doped LaF 3 single crystals was investigated.The electrical conductivity of the crystals was measured using impedance spectroscopy in the frequency range 100 Hz-1 MHz to control for crystal quality.Pulsed glow discharge mass spectrometry (GDMS) was used to simultaneously quantify fluorine, strontium, lanthanum, and gadolinium in the crystals. X-ray fluorescence, scanning electron microscopy-energy dispersive X-ray spectroscopy, and arc optical emission spectrometry were used for validation.Results: Quasiperiodic intensity drifts under sputtering of the ionic conductors were observed and attributed to F − redistribution on the sample surface, affecting surface conductivity and sputtering rate. Several sample preparation protocols were tested to address that effect. Full coating of the sample with a layer of silver several micrometers thick provided stable and effective sputtering. The parameters for the GDMS determination of F, Sr, La, and Gd were optimized. The elements' distribution was studied in different parts of the crystals. Conclusions:An analytical approach to the direct multi-element analysis of fluoridecontaining ionic conductors using pulsed GDMS with La 1−x−y Sr x Gd y F 3−x as an example was designed and tested. Instability effects of ionic conductivity were explained and coped with, providing effective and stable sputtering.

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“…Under such repelling pulse delay, the ions formed by the high-energy electron packet are detected. 11,17,18 The flow of the high-energy electron packet is formed at the front of the discharge pulse and is capable to ionise the components with the highest ionisation energies. 9,11 The obtained mass spectrum (Fig.…”

Section: No + + M → No + M +mentioning

confidence: 99%

New Possibilities for the Determination of Volatile Organic Compounds by Their Molecular Ions in Air Using µs-Pulsed GD TOFMS

Gubal¹

2021

At.Spectrosc.

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A recent trend in glow discharge analysis, previously considered as a 'purely inorganic' technique, is related to the effective ionisation of volatile organic compounds (VOCs). This approach was demonstrated to be capable of analysing VOCs in both model gas mixtures and ambient air. In the current study, the possibility of the direct determination of VOCs of different classes of organic compounds (including toluene, p-xylene, chlorobenzene and 1,2,4-trimethylbenzene) in ambient air using microsecond pulsed glow discharge time-of-flight mass spectrometry (µs-Pulsed GD TOFMS) with copper hollow cathode was demonstrated. The ionisation processes with the formation of molecular ions M + , which can be used for quantification, were discussed. The fragmentation of detected molecular ions of VOCs was found to be quite low, which benefits both qualitative and quantitative determination. The ease of identification and relative simplicity of the mass spectrum is promising for the analysis of VOC mixtures. One of the possible applications of the designed method is the direct determination of VOCs in human exhaled breath for the diagnosis of lung diseases, including lung cancer. However, revealing its potential applicability for this purpose requires further research.

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Pulsed glow discharge enables direct mass spectrometric measurement of fluorine in crystal materials – Fluorine quantification and depth profiling in fluorine doped potassium titanyl phosphate

Cited by 24 publications

References 69 publications

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

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

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

New Possibilities for the Determination of Volatile Organic Compounds by Their Molecular Ions in Air Using µs-Pulsed GD TOFMS

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