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Direct Multi-element Analysis of Liquids (Water) in Glow Discharge Mass Spectrometry

Received: 19 July 2022     Accepted: 11 August 2022     Published: 28 September 2022
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Abstract

Attempts to conduct direct mass spectral elemental analysis of liquids have been made many times. ICP mass spectrometry used for elemental analysis of liquids has a significant drawback — a large matrix effect, which limits its use for the analysis of liquids with a high content of impurities. The paper considers the possibility of direct multi-element analysis of water in glow discharge mass spectrometry. To carry out such an analysis, an ion source based on a hollow cathode was used. The method is based on the phenomenon of physical adsorption and desorption of water and its components on a metal surface. A capillary is inserted into the hollow cathode of the ion source, through which water with impurity elements is introduced into the source using a peristaltic pump. Water spreads and wets the metal surface; impurities are adsorbed on the metal surface around the capillary. Water evaporates in a vacuum. The glow discharge is excited in water vapor. Ions are pulled out of the negative glow, bombard the cathode-metal surface and desorb water molecules and impurities contained therein. Several designs of a source for supplying water to the spray area are given. In steady-state mode, the rate of water input into the source is less than 1 mm3/min, the adsorbed liquid layer is constantly updated. If the water flow rate is too high, an ice plug forms at the end of the capillary, which is sprayed in the discharge. To test the source, various elements were introduced into the analyzed water. At the same time, ICP mass spectrometry standards were used. Mass spectra of elements contained in water are obtained. Elemental sensitivity at the ppb level is achieved. The absolute sensitivity of the method is 3-4 orders of magnitude higher than the absolute sensitivity of the ICP mass spectrometry method. In the glow discharge, the matrix effect is absent, or is insignificant. Solutions of caustic sodium and caustic potassium with a concentration of components up to 20% were introduced into the ion source. Even with such a high concentration of components, the source continued to function. The proposed method is completely new, and obviously needs further research and improvement. In turn, the author is ready to provide consulting services to all interested persons and organizations.

Published in Modern Chemistry (Volume 10, Issue 3)
DOI 10.11648/j.mc.20221003.15
Page(s) 98-105
Creative Commons

This is an Open Access article, distributed under the terms of the Creative Commons Attribution 4.0 International License (http://creativecommons.org/licenses/by/4.0/), which permits unrestricted use, distribution and reproduction in any medium or format, provided the original work is properly cited.

Copyright

Copyright © The Author(s), 2022. Published by Science Publishing Group

Keywords

Ion Source, Glow Discharge, Adsorption, Desorption, Capillaries, Sputtering, Elemental Analysis

References
[1] Chupakhin M. S. Probe methods in spark mass spectrometry. Energoatomizdat, 1985, 109.
[2] Chupakhin M. S., G. Ramendik, I. Kryuchkova O. I., Analytical capabilities of spark mass spectrometry. M.: Atomizdat, 1972. 222 p.
[3] N. V. Garrilov, G. A. Hesyats, G. V. Radkovski, V. V. Bersenev. Development of Technological Sources of gas ions on the basis of Hollow Cathode Glow Discharge Surface and Coatings Technology, 96 (1997) 81, 88.
[4] D. Zhechev, V. I. Zhemenik, S. Tileva, G. V. Mishinsky, N. Pyrvanova, “A hollow cathode discharge modification as a source of sputtered atoms and their ions”, Nuclear Inst. and Methods in Physics Research, B 204, (2003) 387.
[5] Christopher M. Barshick, Douglas C. Duckworth, and David H. Smith Analysis of Solution Residues by Glow Discharge Mass Spectrometry. Am. Soc. Mass Spectrom 1993, 4, (47-53).
[6] Daughtrey, E. H., Jr,; D, L. Donohue, P. S. Slevin, and W, Harrison. Surface sputter effects in a hollow cathode discharge. Anal. Chem. 47, 683-8 (1975),
[7] Vacuum equipment and vacuum technology, edited by A. Guthrie and R. Walkerling, trans. from English, M., 1951.
[8] Sikharulidze G. G. Ion source with hollow cathode for elemental analysis of solids. Mass spectrometry №1, 1 - 8 (2004).
[9] Yavorsky B. M., Detlaf A. A. Handbook of Physics. Nauka, 1978. p. 944.
[10] Deriagin B.V., Zorin Z.M. JFH, vol. 29, No. 10, 1955, pp. 1755-1770.
[11] Sum B. D., Goryunov Yu. V. Physico-chemical bases of wetting and spreading. "Chemistry". (1976), p. 246.
[12] Greg S., Sing K. Adsorption, specific surface area, porosity. - M.: Mir, 1984. – 310 p.
[13] Adamson A. Physical chemistry of surfaces. – M.: Mir. 1979. – 568 p.
[14] Oura K., Lifshits V. G., Saranin A. A. and others. Introduction to Surface Physics / Edited by V. I. Sergienko. — M.: Nauka, 2006. — 490 p.
[15] Pleshivtsev N. V. Cathode sputtering. — M.: Atomizdat, 1968, p. 342.
[16] Lieberman M. A., Lichtenberg A. J. Principles of Plasma Discharges and Materials Processing. — John Wiley & Sons, 2005. — ISBN 0-471-72001-1.
[17] Ivanovskiy G. F., Petrov V. I. Ion-plasma processing of materials. — Moscow: Radio and Communications, 1986. — 232 p.
[18] Kolasinski N, Kurt W. (2012). Surface Science: Fundamentals of Catalysis and Nanoscience, Third edition. p. 203.
[19] Sikharulidze G. G. Patent "Plasma source with hollow cathode". Application 2002102255/28. Published 27. 08. 2003.
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  • APA Style

    Frohlich Georg. (2022). Direct Multi-element Analysis of Liquids (Water) in Glow Discharge Mass Spectrometry. Modern Chemistry, 10(3), 98-105. https://doi.org/10.11648/j.mc.20221003.15

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    ACS Style

    Frohlich Georg. Direct Multi-element Analysis of Liquids (Water) in Glow Discharge Mass Spectrometry. Mod. Chem. 2022, 10(3), 98-105. doi: 10.11648/j.mc.20221003.15

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    AMA Style

    Frohlich Georg. Direct Multi-element Analysis of Liquids (Water) in Glow Discharge Mass Spectrometry. Mod Chem. 2022;10(3):98-105. doi: 10.11648/j.mc.20221003.15

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  • @article{10.11648/j.mc.20221003.15,
      author = {Frohlich Georg},
      title = {Direct Multi-element Analysis of Liquids (Water) in Glow Discharge Mass Spectrometry},
      journal = {Modern Chemistry},
      volume = {10},
      number = {3},
      pages = {98-105},
      doi = {10.11648/j.mc.20221003.15},
      url = {https://doi.org/10.11648/j.mc.20221003.15},
      eprint = {https://article.sciencepublishinggroup.com/pdf/10.11648.j.mc.20221003.15},
      abstract = {Attempts to conduct direct mass spectral elemental analysis of liquids have been made many times. ICP mass spectrometry used for elemental analysis of liquids has a significant drawback — a large matrix effect, which limits its use for the analysis of liquids with a high content of impurities. The paper considers the possibility of direct multi-element analysis of water in glow discharge mass spectrometry. To carry out such an analysis, an ion source based on a hollow cathode was used. The method is based on the phenomenon of physical adsorption and desorption of water and its components on a metal surface. A capillary is inserted into the hollow cathode of the ion source, through which water with impurity elements is introduced into the source using a peristaltic pump. Water spreads and wets the metal surface; impurities are adsorbed on the metal surface around the capillary. Water evaporates in a vacuum. The glow discharge is excited in water vapor. Ions are pulled out of the negative glow, bombard the cathode-metal surface and desorb water molecules and impurities contained therein. Several designs of a source for supplying water to the spray area are given. In steady-state mode, the rate of water input into the source is less than 1 mm3/min, the adsorbed liquid layer is constantly updated. If the water flow rate is too high, an ice plug forms at the end of the capillary, which is sprayed in the discharge. To test the source, various elements were introduced into the analyzed water. At the same time, ICP mass spectrometry standards were used. Mass spectra of elements contained in water are obtained. Elemental sensitivity at the ppb level is achieved. The absolute sensitivity of the method is 3-4 orders of magnitude higher than the absolute sensitivity of the ICP mass spectrometry method. In the glow discharge, the matrix effect is absent, or is insignificant. Solutions of caustic sodium and caustic potassium with a concentration of components up to 20% were introduced into the ion source. Even with such a high concentration of components, the source continued to function. The proposed method is completely new, and obviously needs further research and improvement. In turn, the author is ready to provide consulting services to all interested persons and organizations.},
     year = {2022}
    }
    

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  • TY  - JOUR
    T1  - Direct Multi-element Analysis of Liquids (Water) in Glow Discharge Mass Spectrometry
    AU  - Frohlich Georg
    Y1  - 2022/09/28
    PY  - 2022
    N1  - https://doi.org/10.11648/j.mc.20221003.15
    DO  - 10.11648/j.mc.20221003.15
    T2  - Modern Chemistry
    JF  - Modern Chemistry
    JO  - Modern Chemistry
    SP  - 98
    EP  - 105
    PB  - Science Publishing Group
    SN  - 2329-180X
    UR  - https://doi.org/10.11648/j.mc.20221003.15
    AB  - Attempts to conduct direct mass spectral elemental analysis of liquids have been made many times. ICP mass spectrometry used for elemental analysis of liquids has a significant drawback — a large matrix effect, which limits its use for the analysis of liquids with a high content of impurities. The paper considers the possibility of direct multi-element analysis of water in glow discharge mass spectrometry. To carry out such an analysis, an ion source based on a hollow cathode was used. The method is based on the phenomenon of physical adsorption and desorption of water and its components on a metal surface. A capillary is inserted into the hollow cathode of the ion source, through which water with impurity elements is introduced into the source using a peristaltic pump. Water spreads and wets the metal surface; impurities are adsorbed on the metal surface around the capillary. Water evaporates in a vacuum. The glow discharge is excited in water vapor. Ions are pulled out of the negative glow, bombard the cathode-metal surface and desorb water molecules and impurities contained therein. Several designs of a source for supplying water to the spray area are given. In steady-state mode, the rate of water input into the source is less than 1 mm3/min, the adsorbed liquid layer is constantly updated. If the water flow rate is too high, an ice plug forms at the end of the capillary, which is sprayed in the discharge. To test the source, various elements were introduced into the analyzed water. At the same time, ICP mass spectrometry standards were used. Mass spectra of elements contained in water are obtained. Elemental sensitivity at the ppb level is achieved. The absolute sensitivity of the method is 3-4 orders of magnitude higher than the absolute sensitivity of the ICP mass spectrometry method. In the glow discharge, the matrix effect is absent, or is insignificant. Solutions of caustic sodium and caustic potassium with a concentration of components up to 20% were introduced into the ion source. Even with such a high concentration of components, the source continued to function. The proposed method is completely new, and obviously needs further research and improvement. In turn, the author is ready to provide consulting services to all interested persons and organizations.
    VL  - 10
    IS  - 3
    ER  - 

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Author Information
  • Institute of Problems of Microelectronics Technology and High-Purity Materials of the Russian Academy of Sciences, Chernogolovka, Russia

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