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Preparation of Small Samples for 14C Accelerator Targets by Catalytic Reduction of CO

  • P J Slota (a1), A J T Jull (a1), T W Linick (a1) and L J Toolin (a1)

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Graphite in various forms has become the standard target for accelerator 14C dating. Graphite has been made by catalytic graphitization of charcoals (Lowe, 1984). Thin films of graphite have also been produced by thermal cracking (Beukens & Lee, 1981), electric discharge (Andrée et al, 1984; Wand, Gillespie & Hedges, 1984). Vogel et al (1984) pointed out the ease of graphite formation on iron from CO2 and H2 mixtures at ca 600°C. The deposition reactions of carbon from the CO, H2, and CO2 equilibria are well known (Wagman et al, 1945) and well studied. Formation of graphite from CO2 was discussed extensively by Boudouard (1902) and Schenck and Zimmerman (1903), and was known to chemists in France in 1851. We have used a related method, where graphite forms away from the iron, by using a higher temperature, and reduction of CO2 to CO over Zn in the presence of H2 (Jull et al, 1986) as an alternative to the use of Fe alone. The object of this paper is to point out an even simpler graphite preparation system, which eliminates hydrogen. The decomposition reaction of CO (Boudouard, 1902) takes place according to reaction (1).

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References

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Andrée, M, Beer, J, Oeschger, H, Bonani, G, Hofmann, H J, Morenzoni, E, Nessi, M, Suter, M and Wölfli, W, 1984, Target preparation for milligram-sized 14C samples and data evaluation for AMS measurements: Nuclear Instruments & Methods, v 223, no. B5, p 274279.
Beukens, R P and Lee, H W, 1981, The production of small carbon samples by R F dissociation of acetylene, in Kutschera, W, ed, Symposium on Accelerator Mass Spectrometry, 2nd, Proc: Argonne Natl Lab, p 416425.
Boudouard, O, 1902, Recherches sur les équilibres chimiques: Ann Chim Phys, v 24, ser 7, p 585.
Jull, A J T, Donahue, D J, Hatheway, A L, Linick, T W and Toolin, L J, 1986, Production of graphite targets by deposition from CO/H2 for precision accelerator 14C measurements, in Stuiver, M and Kra, R S, eds, Internatl 14C conf, 12th, Proc: Radiocarbon, v 28, no 2A, p 191197.
Lowe, D C, 1984, Preparation of graphite targets for radiocarbon dating by tandem accelerator mass spectrometry: Internatl Jour Applied Radiation Isotopes, v 35, p 349352.
Schenck, R and Zimmerman, F, 1903, Ueber die Spaltung des Kohlenoxyds und das Hochofengleichgewicht: Berichte deutschen chem Gesellschaft, v 36, p 12311235.
Slota, P J Jr and Taylor, R E, 1986, AMS 14G analysis of samples from archaeological contexts: pretreatment and target preparation, in University of California AMS conf Proc: Livermore, Inst Geophysics Planetary Physics.
Vogel, J S, Southen, J R, Nelson, D E and Brown, T A, 1984, Performance of catalytically condensed carbon for use in accelerator mass spectrometry: Nuclear Instruments & Methods, v 223, no. B5, p 289293.
Wagman, D D, Kilpatrick, J E, Taylor, W J, Pitzer, K S and Rossini, F D, 1945, Heats, free energies and equilibrium constants of some reactions involving D2, H2, H2O, C, CO, CO2 and CH4 : Jour Research Natl Bur Standards, v 34, p 143161.
Wand, J O, Gillespie, R and Hedges, R E M, 1984, Sample preparation for accelerator-based radiocarbon dating: Jour Archaeol Sci, v 11, p 159163.

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Preparation of Small Samples for 14C Accelerator Targets by Catalytic Reduction of CO

  • P J Slota (a1), A J T Jull (a1), T W Linick (a1) and L J Toolin (a1)

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