Hostname: page-component-586b7cd67f-g8jcs Total loading time: 0 Render date: 2024-11-23T23:24:36.907Z Has data issue: false hasContentIssue false
  • English
  • Français

Optimization of the Graphitization Process at Age-1

Published online by Cambridge University Press:  18 July 2016

Mojmír Němec ,
Lukas Wacker  and
Heinz Gäggeler
Mojmír Němec*
Affiliation:
Department for Chemistry and Biochemistry, Universität Bern, Freiestrasse 3, CH-3012 Bern, Switzerland Laboratory of Ion Beam Physics, HPK, Schafmattstrasse 20, CH-8093 Zürich, Switzerland Department of Nuclear Chemistry, Czech Technical University, in Prague, Brehova 7, 115 19 Prague 1, Czech Republic
Lukas Wacker
Affiliation:
Laboratory of Ion Beam Physics, HPK, Schafmattstrasse 20, CH-8093 Zürich, Switzerland
Heinz Gäggeler
Affiliation:
Department for Chemistry and Biochemistry, Universität Bern, Freiestrasse 3, CH-3012 Bern, Switzerland
*
Corresponding author. Email: [email protected]
Rights & Permissions [Opens in a new window]

Abstract

Core share and HTML view are not available for this content. However, as you have access to this content, a full PDF is available via the ‘Save PDF’ action button.

The reaction conditions for the graphitization of CO2 with hydrogen were optimized for a fast production of high-quality carbon samples for accelerator mass spectrometry (AMS) measurement. The iron catalyst in use is first oxidized by heating with air to remove possible carbon and other impurities and then after evacuation reduced back to iron with hydrogen in several flushing steps to remove any iron oxide. The optimum conditions for a fast graphitization reaction were experimentally determined by changing the reaction temperatures and the H2/CO2 ratio. The resulting graphite samples were measured by AMS to find the smallest isotopic changes (δ13C) at a minimum of molecular fragment formation (13CH current). The improvements are based on thermodynamic data and are explained with Baur-Glaessner diagrams.

Type
Sample Preparation
Information
Radiocarbon , Volume 52 , Issue 3: 20th Int. Radiocarbon Conference Proceedings , 2010 , pp. 1380 - 1393
Copyright
Copyright © 2010 by the Arizona Board of Regents on behalf of the University of Arizona 

References

Dee, M, Bronk Ramsey, C. 2000. Refinement of graphite target production at ORAU. Nuclear Instruments and Methods in Physics Research B 172(1–4):449–53.CrossRefGoogle Scholar
Gudenau, HW, Senk, D, Wang, SW, Martins, KD, Stephany, C. 2005. Research in the reduction of iron ore agglomerates including coal and C-containing dust. ISIJ International 45(4):603–8.Google Scholar
Jull, AJT, Donahue, DJ, Hatheway, AL, Linick, TW, Toolin, LJ. 1986. Production of graphite targets by deposition from CO/H2 for precision accelerator 14C measurements. Radiocarbon 28(2A):191–7.Google Scholar
Liaw, S-J, Davis, BH. 2000. Fischer-Tropsch synthesis. Compositional changes in an iron catalyst during activation and use. Topics in Catalysis 10(1–2):133–9.Google Scholar
Manning, MP, Reid, RC. 1977. C-H-O systems in presence of an iron catalyst. Industrial & Engineering Chemistry Process Design and Development 16:358–61.CrossRefGoogle Scholar
McNichol, AP, Gagnon, AR, Jones, GA, Osborne, EA. 1992. Illumination of a black box: analysis of gas composition during graphite target preparation. Radiocarbon 34(3):321–9.Google Scholar
Oeters, F, Ottow, M, Senk, D, Beyzavi, A, Güntner, J, Lüngen, HB, Koltermann, M, Buhr, A, Yagi, J, Formanek, L. 2009. Iron. In: Ullmann's Encyclopedia of Industrial Chemistry. Weinheim: Wiley-VCH. 178 p.Google Scholar
Pichler, H, Merkel, H. 1949. Chemical and thermomagnetic studies on iron catalysts for synthesis of hydrocarbons. Washington, DC: US Bureau of Mines. p 16–27.Google Scholar
Sacco, A, Reid, RC. 1979. Water limitation in the C-H-O system over iron. AIChE Journal 25(5):839–43.Google Scholar
Sacco, A, Thacker, P, Chang, TN, Chiang, ATS. 1984. The initiation and growth of filamentous carbon from alpha-iron in H2, CH4, H2O, CO2, and CO gas mixtures. Journal of Catalysis 85:224–36.CrossRefGoogle Scholar
Santos, GM, Southon, JR, Griffin, S, Beaupre, SR, Druffel, ERM. 2007. Ultra small-mass AMS 14C sample preparation and analyses at KCCAMS/UCI Facility. Nuclear Instruments and Methods in Physics Research B 259(1):293–302.Google Scholar
Slota, PJ Jr, Jull, AJT, Linick, TW, Toolin, LJ. 1987. Preparation of small samples for 14C accelerator targets by catalytic reduction of CO. Radiocarbon 29(2):303–6.Google Scholar
Synal, H-A, Stocker, M, Suter, M. 2007. MICADAS: a new compact radiocarbon AMS system. Nuclear Instruments and Methods in Physics Research B 259(1):7–13.Google Scholar
van der Laan, GP, Beenackers, AACM. 2000. Intrinsic kinetics of the gas-solid Fischer-Tropsch and water gas shift reactions over a precipitated iron catalyst. Applied Catalysis A 193(1–2):39–53.Google Scholar
Verkouteren, RM, Klinedinst, DB, Currie, LA. 1997. Ironmanganese system for preparation of radiocarbon AMS targets: characterization of procedural chemical-isotopic blanks and fractionation. Radiocarbon 39(3):269–83.CrossRefGoogle Scholar
Vogel, JS. 1992. Rapid production of graphite without contamination for biomedical AMS. Radiocarbon 34(3):344–50.Google Scholar
Vogel, JS, Southon, JR, Nelson, DE, Brown, TA. 1984. Performance of catalytically condensed carbon for use in accelerator mass spectrometry. Nuclear Instruments and Methods in Physics Research B 5(2):289–93.Google Scholar
Vogel, JS, Nelson, DE, Southon, JR. 1987a. 14C background levels in an accelerator mass-spectrometry system. Radiocarbon 29(3):323–33.CrossRefGoogle Scholar
Vogel, JS, Southon, JR, Nelson, DE. 1987b. Catalyst and binder effects in the use of filamentous graphite for AMS. Nuclear Instruments and Methods in Physics Research B 29(1–2):50–6.Google Scholar
Wacker, L, Němec, M, Bourquin, J. 2010. A revolutionary graphitisation system: fully automated, compact and simple. Nuclear Instruments and Methods in Physics Research B 268(7–8):931–4.Google Scholar
Walker, PL Jr, Rakszawski, JF, Imperial, GR. 1959a. Carbon formation from carbon monoxide-hydrogen mixtures over iron catalysts. 1. Properties of carbon formed. Journal of Physical Chemistry 63(2):133–40.Google Scholar
Walker, PL Jr, Rakszawski, JF, Imperial, GR. 1959b. Carbon formation from carbon monoxide-hydrogen mixtures over iron catalysts. 2. Rates of carbon formation. Journal of Physical Chemistry 63(2):140–9.Google Scholar
Xu, XM, Trumbore, SE, Zheng, SH, Southon, JR, McDuffee, KE, Luttgen, M, Liu, JC. 2007. Modifying a sealed tube zinc reduction method for preparation of AMS graphite targets: reducing background and attaining high precision. Nuclear Instruments and Methods in Physics Research B 259(1):320–9.CrossRefGoogle Scholar
Yoneda, M, Shibata, Y, Tanaka, A, Uehiro, T, Morita, M, Uchida, M, Kobayashi, T, Kobayashi, C, Suzuki, R, Miyamoto, K, Hancock, B, Dibden, C, Edmonds, JS. 2004. AMS 14C measurement and preparative techniques at NIES-TERRA. Nuclear Instruments and Methods in Physics Research B 223–224:116–23.Google Scholar