The promising micromethod of Unterzaucher for the direct determination of oxygen in organic compounds has been investigated. The procedure involves pyrolysis of the compound in a stream of nitrogen and conversion of all the oxygen in the pyrolysis products to carbon monoxide over carbon at 1120°C.The carbon monoxide is oxidized to carbon dioxide by iodine pentoxide, and the equivalent amount of iodine liberated is determined titrimetrically. A furnace meeting the high-temperature requirements is described. Criteria are presented for the selection of carbon which gives quantitative conversion of the oxygen to carbon monoxide, and iodine pentoxide for quantitative oxidation of the carbon monoxide.The results obtained to date in this laboratory show over-all precision and accuracy somewhat less than those now obtained in carbon and hydrogen analyses. The method, however, possesses several outstanding advantages over other methods for oxygen determination, in that the apparatus is somewhat less elaborate, the presence of other compounds, such as sulfur, nitrogen, and halogens, has no effect on its applicability, and catalyst poisoning does not present a problem.ALTHOUGH oxygen is one of the most commonly occurring il constituents in organic compounds, there is, at present, no entirely satisfactory method for its direct determination. The lack of such a method is clearly emphasized in the recent excellent review by Elving and Ligett ($), who present a critical examina-
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