We examined different concentrations of HCI, such as 0.4, 0.6, 0.8, 1.0 and 1.2 M, for decalcification of fossil bones and different times of 0.1 M NaOH treatment on collagens to determine the best conditions for purifying collagen through extraction of humic contaminants, and compared the alkali treatment method with the XAD-2 treatment method for several types of fossils. The yield of acid-insoluble bone fractions did not change over the range from 0.4 to 1.0 M HCI and decreased suddenly with 1.2 M HCl on decalcification, and the 14 C ages of the extracted gelatins from the five decalcified fractions were unchanged, suggesting that <1.0 M, and probably about 0.4 M, is recommended to the best concentration of HCI to decalcify fossil bones efficiently. The alkali treatment was done with 0.1 M NaOH at room temperature. The NaOH-treated collagens, with a considerable loss of organic bone protein especially for long treatment time, gave almost the same C-14 ages as those of the XAD-purified hydrolysates. The NaOH-treatment time should be less than several hours to avoid a loss of collagen. The fossil bones used are relatively well-preserved, but the alkali treatment could bring about a lot of loss of organic bone proteins for poorly-preserved bones. The XAD-2 treatment method is effective for accurate radiocarbon dating of fossil bones, if the XAD-2 resin is completely precleaned. (C) 2004 Elsevier B.V. All rights reserved.