A new apparatus suitable for the combustion of the organic component in bones as well as the extraction of carbon dioxide at different temperature levels consists of the following essential parts: 1) a 15 liter reaction vessel made of heat and corrosion resistant molybdenum steel; 2) a thermostatically controlled electric oven; and 3) the gas and vacuum lines to enable operation in the combustion mode when the vessel containing sample is filled with oxygen or extraction of carbon dioxide when the vessel is pumped out at elevated temperatures. Carbon dioxide obtained either by combustion of organic matter or thermal decomposition of mineral fraction is purified and converted into CH₄ for measurement in a proportional counter. A systematic study is in progress to determine the difference in the activity of carbon dioxide of fractions obtained under different conditions, namely the combustion of organic fraction and the thermal decomposition of bone apatite. Collagen is also extracted from the same bone for comparison with the data obtained by the new method. Whenever possible, the results are compared with those of the associated wood or charcoal samples. The new technique makes possible a relatively simple and straightforward processing of fossil bone samples. The bone sample is thoroughly cleaned, crushed, and subjected to combustion and carbon dioxide extraction. Both fractions are routinely measured. Results of dating fossil bones of various ages and provenance are presented, as well as a comparison of data obtained by using the collagen extraction method and the new technique. Depending on the ambient conditions and the age of fossil bones, the new technique revealed various degrees of sample contamination ranging from well-preserved clean samples to heavily contaminated with organic and mineral compounds.