The invention provides a method and apparatus for preparing samples of carbon dioxide with a .sup.14C content for analysis in liquid scintillation counting equipment, the sample being of a known mass and being introduced into and substantially wholly absorbed into an absorption "cocktail", absorption being completed at a stage before saturation of the absorbent occurs. The absorbent is contained in a vial which, when absorption has been completed, is transferred into the scintillation counting equipment without intermediate transfer of the contents.