ABSTRACT. We present results that validate a new wet oxidation, stepped-combustion procedure for dating "old" charcoal samples. An acid-base-wet oxidation (ABOX) pretreatment procedure has been developed that is used in place of the conventional acid-base-acid (ABA) pretreatment. Combustions and graphitizations are performed in a vacuum line that is insulated from the atmosphere by a second backing vacuum to eliminate the risk of atmospheric leakage into the line at any stage of the procedure. Combustions are performed at 3 temperatures (330 °C, 630 °C and 850 °C) with a graphite target produced from the CO2 evolved during each combustion step. In this way, the removal of any contamination can be monitored, and a high degree of confidence can be placed on the final age. The pretreatment, combustion, graphitization, and measurement blank for the procedure, based on the analysis of a "radiocarbon-dead" graphite, is 0.5 ± 0.5 tg C (16, n=14), equivalent to 0.04 ± 0.02 pMC or an "age" of approximately 60 ka for a 1 mg graphite target. Analyses of a "radiocarbon-dead" natural charcoal after ABOX pretreatment and stepped combustion suggest that the total blank (including contamination not removed by pretreatment) may be higher than for graphite, ranging up to 0.10 ± 0.02 pMC. Additional experiments confirm good agreement with accepted values for the international low-14C "New Kauri" standard (0.16-0.25 pMC). They also confirm excellent reproducibility, with 3 separate dates on different aliquots of a charcoal sample from Ngarrabullgan Cave (Queensland, Australia) ranging from 35.2 to 35.5 ka 14C BP. It is also demonstrated that the ABOX pretreatment, in conjunction with the new vacuum line described here, is able to remove contamination not removed by the conventional ABA pretreatment, suggesting that the technique can be used to produce reliable 14C dates on charcoal up to at least 50 ka.
Late Pleistocene glaciation of the Australian mainland was restricted to a small area of the southeastern highlands. Geomorphic mapping of the area and exposure dating using thein situproduced cosmogenic isotope10Be provides evidence for at least two distinct glaciations. The Early Kosciuszko glaciation consisted of a single glacier advance before 59,300 ± 5400 years ago (Snowy River Advance). The Late Kosciuszko glaciation comprised three glacier advances 32,000 ± 2500 (Headley Tarn Advance), 19,100 ± 1600 (Blue Lake Advance), and 16,800 ± 1400 years ago (Mt. Twynam Advance). The Early Kosciuszko glaciation was the most extensive and the Late Kosciuszko advances were progressively less extensive. These periods of glaciation in the highlands correspond to episodes of periglacial activity and peaks in lake levels and river discharge at lower elevations in southeastern Australia. Glacier advances on the Kosciuszko Massif correlate with advances in Tasmania, South America, and New Zealand and are broadly representative of hemispheric climate changes during the last glacial cycle.
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