Development of Reference Materials for Calibration of the Hydrogen Analyzer at High Concentration
https://doi.org/10.20915/2077-1177-2022-18-3-29-40
Abstract
The study discusses the issues of improving the accuracy of measuring high hydrogen concentrations in the development of storage materials in the hydrogen energy industry. The purpose of the study was to develop reference materials for calibration of the hydrogen analyzers at high concentrations. The main methods for determining the hydrogen content in materials were analyzed. It was established that the extraction method in an inert gas medium has found the widest application. The main methods for determining the hydrogen content in materials are analyzed, it is established that the extraction method in an inert gas medium has found the widest application. The need for calibration of analyzers on reference materials with a high hydrogen concentration was noted. Reference materials of titanium alloy VT-1-0 with hydrogen concentration up to (4.0±0.1) wt.% have been developed. The optimal parameters for the analysis were selected. On the example of the hydrogen analyzer RHEN602 (LECO, USA), calibration was carried out on the developed reference materials to obtain a calibration dependence. The reliability of the obtained calibration curve with the application of stoichiometric zirconium hydride was estimated. The confidence interval of the resulting calibration curve was ±10 %. It has been established that the calibration on the developed materials makes it possible to analyze materials with a hydrogen content of 0.5 to 4.0 wt.%. The practical significance of the study lies in the development of reference materials that can be applied to calibrate hydrogen analyzers operating on the principle of melting in an inert gas medium at a high hydrogen concentration.
Keywords
hydrogen analyzer,
hydrogen,
reference material,
titanium alloy,
calibration,
extraction method,
concentration,
hydrogenation
Supporting agencies: The work was sponsored by the State Assignment «Science», research project No. FSWW-2020–0017.
About the Authors
A. A. Spiridonova
State Regional Center for Standardization, Metrology and Testing in the Tomsk Region; National Research Tomsk Polytechnic University
Russian Federation
Russian Federation
Alena A. Spiridonova – Metrology Engineer; postgraduate student of the School of Nuclear Technology
30 Lenina ave., Tomsk, 634050
V. N. Kudiiarov
National Research Tomsk Polytechnic University
Russian Federation
Russian Federation
Viktor N. Kudiiarov – Cand. Sci. (Eng.), Associate Professor of the Department of Experimental Physics
30 Lenina ave., Tomsk, 634050
A. M. Lider
National Research Tomsk Polytechnic University
Russian Federation
Russian Federation
Andrey M. Lider – Dr. Sci. (Eng.), Professor, Head of the
Department of Experimental Physics
30 Lenina ave., Tomsk, 634050
References
1. Borzenko V., Eronin A. The use of air as heating agent in hydrogen metal hydride storage coupled with PEM fuel cell. International Journal of Hydrogen Energy. 2016;41(48):23120–23124. https://doi.org/10.1016/j.ijhydene.2016.10.067
2. García-Triviño P., Fernández-Ramírez L. M., Gil-Mena A. J, Llorens-Iborra F., García-Vázquez C. A., Jurado Fr. Optimized operation combining costs, efficiency and lifetime of a hybrid renewable energy system with energy storage by battery and hydrogen in grid-connected applications. International Journal of Hydrogen Energy. 2016;41(48):23132–23144 p. https://doi.org/10.1016/j.ijhydene.2016.09.140
3. Ortiz A. L., Zaragoza M. J. M., Collins-Martínez V. Hydrogen production research in Mexico: A review. International Journal of Hydrogen Energy. 2016;41(48):23363–23379. https://doi.org./10.1016/j.ijhydene.2016.07.004
4. Ramírez-Dámaso G., Ramírez-Platón I. E., López-Chávez E., Castillo-Alvarado F. L., Cruz-Torres A., Caballero F. et al. A DFT study of hydrogen storage on surface (110) of Mg 1– x Al x (0d xd 0.1). International Journal of Hydrogen Energy. 2016;41(48):23388– 23393. https://doi.org/10.1016/j.ijhydene.2016.08.202
5. Liu W., Aguey-Zinsou K. F. Hydrogen storage properties of in-situ stabilised magnesium nanoparticles generated by electroless reduction with alkali metals. International Journal of Hydrogen Energy. 2015;40(47):16948–16960. https://doi.org/10.1016/j.ijhydene.2015.07.020
6. Bouazizi N., Boudharaa T., Bargougui R., Vieillard J., Ammar S., Le Derf F. et al. Synthesis and properties of ZnO-HMD@ ZnO-Fe/ Cu core-shell as advanced material for hydrogen storage. Journal of Colloid and Interface Science. 2017;491:89–97. https://doi.org/10.1016/j.jcis.2016.12.024
7. Köse D. A., Yurdakul Ö., ùahin O., Öztürk Z. The new metal complex templated polyoxoborate (s)(POB (s)) structures. Synthesis, structural characterization, and hydrogen storage capacities. Journal of Molecular Structure. 2017;1134:806–813. https://doi.org/10.1016/j.molstruc.2017.01.010
8. Kolachev B. A., Shalin R. E., Ilyin A. A. Hydrogen storage alloys: A Handbook. Moscow: Metallurgy; 1995. 384 p.
9. Zhang Y., Li J., Zhang T., Wu T., Kou H., Xue X. Hydrogenation thermokinetics and activation behavior of non-stoichiometric Zr-based Laves alloys with enhanced hydrogen storage capacity. Journal of Alloys and Compounds. 2017;694:300–308. https://doi.org/10.1016/j.jallcom.2016.10.021
10. Suárez-Alcántara K., Palacios-Lazcano A. F., Funatsu T., Cabañas-Moreno J. G. Hydriding and dehydriding in air-exposed Mg Fe powder mixtures. International Journal of Hydrogen Energy. 2016;41(48):23380–23387. https://doi.org/10.1016/j.ijhydene.2016.06.242
11. Chen X., Zou J., Zenga X., Ding W. Hydrogen storage properties of a Mg-La-Fe-H nano-composite prepared through reactive ball milling. Journal of Alloys and Compounds. 2017;701:208–214. https://doi.org/10.1016/j.jallcom.2017.01.056
12. Ma M., Duan R., Ouyang L., Zhu X., Chen Zh., Peng Ch. Hydrogen storage and hydrogen generation properties of CaMg 2-based alloys. Journal of Alloys and Compounds. 2017;691:929–935. https://doi.org/10.1016/j.jallcom.2016.08.307
13. Suárez-Alcántara K., Palacios-Lazcano A. F., Funatsu T., Cabañas-Moreno J. G. Mg–M–LiH alloys prepared by mechanical milling and their hydrogen storage characteristics. International Journal of Hydrogen Energy. 2015;40(48):17344–17353. https://doi.org/10.1016/j.ijhydene.2015.04.083
14. Hino S., Grove H., Ichikawa T., Kojima Yo., Sørby M. H., Hauback B. C. Metal aluminum amides for hydrogen storage–Crystal structure studies. International Journal of Hydrogen Energy. 2015;40(47):16938–16947. https://doi.org/10.1016/j.ijhydene.2015.05.012
15. Tarasov B. P., Lototsky M. V., Yartys V. A. Problem of hydrogen storage and prospective uses of hydrides for hydrogen accumulation. Russian Chemical Journal. 2006;50(6):34–48. https://doi.org/10.1134/S1070363207040329
16. Kulik O. P., Chernyshev L. I. Hydrogen energy: storage and transportation of hydrogen (review). Preprint of NAS of Ukraine, Institute of Problems of Materials Science. I. N. Frantsevich. P. 67.
17. Pundt A., Kirchheim R. Hydrogen in metals: microstructural aspects. Annual Review of Materials Research. 2006;36(1):555–608. https://doi.org/10.1146/annurev.matsci.36.090804.094451
18. A critical review of mg-based hydrogen storage materials processed by equal channel angular pressing. Metals. 2017;7(9):324. https://doi.org/10.3390/met7090324
19. da Silva Dupim I., Ferreira Santos S., Huot J. Effect of cold rolling on the hydrogen desorption behavior of binary metal hydride powders under microwave irradiation. Metals. 2015;5(4):2021–2033. https://doi.org/10.3390/met5042021
20. Perevezentsev A. N., Andreev B. M., Kapyshev V. K., Rivkis L. A., Malek M. P., Bystritskii V. M. Hydrides of intermetallic compounds and alloys, their properties and applications in nuclear technology. Fizika elementarnykh chastits i atomnogo iadra = Physics of elementary particles and the atomic nucleus. 1988;19(6):1386–1439.(In Russ.).
21. 21. Azhazh V. M. Materials for hydrogen storage: analysis of development trends based on data on information flows. Voprosy atomnoi nauki i tekhniki. Seriia: Vakuum, chistye materialy, sverkhprovodniki. 2006;1:145–152.(in Russ.).
22. Milanoviü I., Miloševiü S., Raškoviü -Lovre ä., Novakoviü N., Vujasin R., Matoviü L. et al. Microstructure and hydrogen storage properties of MgH 2–TiB2–SiC composites. Ceramics International. 2013;39(4):4399–4405. https://doi.org/10.1016/j.ceramint.2012.11.029
23. Fernandez A., Deprez E., Friedrichs O. A comparative study of the role of additive in the MgH 2 vs. the LiBH 4–MgH 2 hydrogen storage system. International journal of hydrogen energy. 2011;36(6):3932–3940. https://doi.org/10.1016/j.ijhydene.2010.12.112
24. Friedrichs O., Kolodziejczyk L., Sánchez-López J. C., Fernández A., Lyubenova L., Zander D. et al. Influence of particle size on electrochemical and gas-phase hydrogen storage in nanocrystalline Mg. Journal of Alloys and Compounds. 2008;463(1):539–545. https://doi.org/10.1016/j.jallcom.2007.09.085
25. Leardini F., Bodega J. L., Ares J. R., Fernández J. F. Realistic simulation in a single stage hydrogen compressor based on AB2 alloys. International Journal of Hydrogen Energy. 2016;41(23):9780–9788. https://doi.org/10.1016/J.IJHYDENE.2016.01.125
26. Kumar S., Jain A., Ichikawa T., Kojima Y., Dey G. K. Development of vanadium based hydrogen storage material: a review. Renewable and Sustainable Energy Reviews. 2017;72:791–800. https://doi.org/10.1016/j.rser.2017.01.063
27. Shao H., Xin G., Zheng J., Li X., Akiba E. Nanotechnology in Mg-based materials for hydrogen storage. Nano Energy. 2012;1(4):590– 601. https://doi.org/10.1016/J.NANOEN.2012.05.005
28. Zhang T., Zhang Y., Zhang Mi., Hu R., Kou H., Li J. et al. Hydrogen absorption behavior of Zr-based getter materials with Pd Ag coating against gaseous impurities. International Journal of Hydrogen Energy. 2016;41(33):14778–14787. https://doi.org/10.1016/j.ijhydene.2016.06.073
29. Tarnawski Z., Kim-Ngan N. T. H. Hydrogen storage characteristics of Ti–and V–based thin films. Journal of Science: Advanced Materials and Devices. 2016;1(2):141–146. https://doi.org/10.1016/j.jsamd.2016.05.003
30. Protsenko O. M., Karachevtsev F. N., Mekhanik E. A. Experience on development of measurement procedure for determination of hydrogen content in titanium alloys. Proceedings of VIAM. 2014;12:1–5. https://doi.org/10.18577/2307-6046-2014-0-12-8-8
31. Grigorovich K. V. New possibilities of modern methods for determination of gas-forming impurities in metals. Inorganic Materials. 2007;73(1):23–34. https://doi.org/10.1134/S0020168508140094
32. Furuya Y., Takasaki A., Mizuno K., Yoshiie T. Hydrogen desorption from pure titanium with different concentration levels of hydrogen. Journal of Alloys and Compounds. 2007; 446:447–450. https://doi.org/10.1016/j.jallcom.2007.04.304
33. Eliezer D., Tal-Gutelmacher E., Cross C. E., Boellinghaus Th. Hydrogen absorption and desorption in a duplex-annealed Ti-6Al-4V alloy during exposure to different hydrogen-containing environments. Materials Science and Engineering: A. 2006;433(1):298–304. https://doi.org/10/1016/j.msea.2006.06.088
34. Tal-Gutelmacher E., Eliezer D., Abramov E. Thermal desorption spectroscopy (TDS)—Application in quantitative study of hydrogen evolution and trapping in crystalline and non-crystalline materials. Materials Science and Engineering A-structural Materials Properties Microstructure and Processing. 2007; 445:625–631. http://doi.org/10.1016/j.msea.2006.09.089
35. Von Zeppelin F., Haluška M., Hirscher M. Thermal desorption spectroscopy as a quantitative tool to determine the hydrogen content in solids. Thermochimica Acta. 2003;404(1):251–258. https://doi.org/10.1016/S0040–6031(03)00183-7
36. Takasaki A., Furuya Y., Ojima K., Taneda Y. Hydride dissociation and hydrogen evolution behavior of electrochemically charged pure titanium. Journal of Alloys and Compounds. 1995;224(2):269–273. https://doi.org/10.1016/0925–8388(95)01565-5
37. Mikhaylov A. A., Laptev R. S., Kudiiarov V. N., Volokitinad T. L. Titanium defect structure change after gas-phase hydrogenation at different temperatures and cooling rates. AIP Conference Proceedings. 2016;1783:020152. https://doi.org/10.1063/1.4966445
38. Hadjixenophontos E., Michalek L., Roussel M.,. Hirscher M, Schmitz G. The role of surface oxides on hydrogen sorption kinetics in titanium thin films. Applied Surface Science. 2018; l(441):324–330. https://doi.org/10/1016/j.apsusc.2018.02.044
39. Laptev R., Lider A., Bordulev Yu., Kudiiarov V., Garanin G. Hydrogenation-induced microstructure changes in titanium. Journal of Alloys and Compounds. 2015;645:193–195. https://doi.org/10.1016/j.jallcom.2014.12.257
40. Stepanova E., Bordulev Y., Kudiiarov V., Laptev R., Lidere A., Xinming J. Effect of hydrogen on the structural and phase state and defect structure of titanium alloy. AIP Conference Proceedings. 2016;1772:030016. https://doi.org/10.1063/1.4964554
41. Sakintuna B., Lamari-Darkrim F., Hirscher M. Metal hydride materials for solid hydrogen storage: a review. International Journal of Hydrogen Energy. 2007;32:1121–1140. https://doi.org/10.1016/j.ijhydene.2006.11.022
42. Larionov V. V., Lider A. M., Laptev R. S. Control of changes in the defect structure of titanium saturated with hydrogen. IOP Conference Series: Materials Science and Engineering. 2016;135(1):012025. https://doi.org/10.1088/1757–899X/135/1/012025
43. Ulmer U., Dieterich M., Pohl A., Dittmeyer R., Linder M., Fichtner M. Study of the structural, thermodynamic and cyclic effects of vanadium and titanium substitution in laves-phase AB2 hydrogen storage alloys. International Journal of Hydrogen Energy. 2017;42(31):20103–20110. https://doi.org/10.1016/j.ijhydene.2017.06.137
44. Macin V., Christ H. J. Influence of hydride-induced microstructure modification on mechanical properties of metastable beta titanium alloy Ti 10V-2Fe-3Al. International Journal of Hydrogen Energy. 2015;40(47):16878–16891. https://doi.org/10.1016/j.ijhydene.2006.11.022
45. Vizcaíno P., Lopez Vergara I. A., Banchik A. D., Abriata J. P. Terminal solid solubility determinations in the H–Ti system. International Journal of Hydrogen Energy. 2015;40(47):16928–16937. https://doi.org/10.1016/j.ijhydene.2015.06.167
46. Kudiiarov V. N., Lider A. M. Investigation of hydrogen sorption and desorption processes with the help of automated complex GAS REACTION CONTROLLER LP. Fundamental Research. 2013;10–15:3466–3471. (In Russ.).
Review
For citations:
Spiridonova A.A., Kudiiarov V.N., Lider A.M. Development of Reference Materials for Calibration of the Hydrogen Analyzer at High Concentration. Measurement Standards. Reference Materials. 2022;18(3):29-40. (In Russ.) https://doi.org/10.20915/2077-1177-2022-18-3-29-40
Views:
504
This work is licensed under a Creative Commons Attribution-NonCommercial 4.0 International (CC BY-NC 4.0).
Email this article 
