Microdosage du carbone dans les composés organiques par combustion quasi-instantanée et titrage coulometrique automatique du dioxyde de carbone

Abstract

A rapid simple method is described for the determination of carbon in organic compounds. The technique is based on a flash-combustion of the weighed sample (1-3 mg) in a hot empty combustion chamber at 950-1050 degrees and swept by a stream of oxygen at a rate of 80-100 ml min . Together with this flash and dynamic combustion in oxygen, a cupric oxide filling at 850 degrees is necessary. Halogens and sulphur oxidation products are retained by means of a silvered alumina filling at 750-800 degrees . Water and acidic oxides of nitrogen are absorbed at room temperature by means of magnesium perchlorate and manganese dioxide respectively. Carbon dioxide is absorbed in the cathodic compartment of an automatic coulometer and generates H(+) ions which are neutralized by OH(-) obtained by electrolysis. This method makes possible the determination of carbon in compounds containing halogens (including fluorine), phosphorus and metals. However, some metal compounds with polynuclear rings in their molecules give low results and require the addition of an oxidant to the sample in the boat for complete combustion. Vanadium pentoxide seems to be the best oxidant in the present working conditions. Solid samples are weighed and analysed in platinum or porcelain boats; liquid samples are weighed in Pyrex capillaries which are laid in platinum boats and covered with a small piece of platinum gauze. When normal liquid samples are analysed, one tip of the capillary is broken before its introduction into the combustion tube but in the case of volatile liquid samples the sealed capillary is introduced into the combustion chamber, where it explodes. The precision obtained is better than that of the classical methods.