All samples were washed to remove any contaminant debris, broken into fragments (1 to 2cm), and placed in hydrochloric acid (0.5M HCl) for between 3 and 4 days. The HCl was replenished until the pH of the solution remained at approximately 2.0. The samples were then drained and given two water washes to remove calcium ions that could form humates. The decalcified samples were placed in a HCl solution (pH 2.0) at 90oC for approximately 18 hours. The extracted collagen was filtered and the supernatant reduced in a moisture extraction oven, it was then redissolved in cold distilled water, filtered, and once more dried in the moisture extraction oven.
Collagen extracted from the bone and antler was combusted in a stream of zero grade oxygen and nitrogen (McCormac et al 1993). The burnt gases were passed through a copper oxide furnace (600oC) which converted carbon monoxide to carbon dioxide and through a silver furnace (400oC) which removed halogens. The gas was then passed through a saturated solution of a strong oxidising agent (KMnO4) and though a drikold trap to remove moisture. The resultant carbon dioxide was sub-sampled after equilibration in a 40 litre volume for 13C determination. The carbon dioxide was converted to benzene (C6H6) following the procedure described by Noakes et al (1965). Benzene was taken off the chromium catalyst at 120oC with drikold, while actively pumping off radon contamination. Samples were allowed to rest in a freezer for a minimum of 14 days so that any remaining radon frozen into the benzene could decay.
Results from the Y and Z Holes