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Sample Chemistry for the Oxford High Energy Mass Spectrometer

  • Richard Gillespie (a1) and Robert E M Hedges (a1)

Abstract

Chemical pretreatment procedures for the decontamination, extraction, and isolation of organic materials for 14C dating using the Oxford accelerator system are described. Specific details are given for the isolation and chromatographic purification of amino acids from bone and tooth collagen, of lipids from sediments, and of cellulose and glucose from wood, paper, and textiles. A description is also given of the apparatus used for the routine preparation of 1 to 5mg graphite samples on tantalum wire, for use in the accelerator ion source.

The high energy mass spectrometer (HEMS) approach to 14C dating allows the use of very small samples in the low milligram range. Sample pretreatment and decontamination procedures can be both more vigorous and more selective than those used by conventional dating laboratories. Specific chemical compounds can be isolated from archaeologic or geologic samples; such compounds may be characteristic of particular source materials and, hence, provide more detailed information than is generally possible using bulk organic samples. The Oxford Radiocarbon Unit has concentrated on three sample types that represent the kind of material we expect to work on initially: bone, lake sediment, and wood.

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References

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Birks, HH, 1980, Plant macrofossils in lake sediments: Archiv Hydrobiol Beih, v 15, p 160.
Brooks, PW, Eglinton, G, Gaskell, SJ, McHugh, DJ, Manwell, JR, and Philip, RP, 1976, Lipids of recent sediments Part I. Straight chain hydrocarbons and carboxylic acids of some temperate lacustrine and sub-tropical lagoonal/tidal flat sediments: Chem Geol v 18, p 2138.
Cranwell, PA, 1973, Chain length distribution of n-alkanes from lake sediments in relation to post-glacial environmental change: Freshwater Biol, v 5, p 259265.
Hedges, REM, Wand, JO, and White, NR, 1980, The production of C- beams for radiocarbon dating with accelerators: Nuclear Instruments and Methods, v 173, p 409421.
Hoopes, EA, Peltzer, ET, and Bada, JL, 1978, Determination of amino acid enantiomeric ratios by gas chromatography of the N-trifluoroacetyl-L-prolylpeptide methyl esters: Jour Chromatographic Sci, v 16, p 556560.
Taylor, RE and Slota, PS, 1979, Fraction studies on marine shell and bone samples for radiocarbon dating, in Berger, R and Suess, HE, eds, Radiocarbon dating, Internatl 14C conf, 9th, Proc: Berkeley, Univ California Press, p 442–432.
Wand, JO (ms) 1981, Microsample preparation for radiocarbon dating: Unpub DPhil thesis, Univ Oxford.
White, NR, in press, The inverted spherical ionizer sputter ion source (IS3): Nuclear Instruments and Methods, in press.

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