By T. T. Gorsuch (Auth.)
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Sample text
Some part of the element may occur in, or be converted to, a volatile form which may escape from the vessel used to contain the organic sample. Some part of the element may combine with the vessel used to contain the sample, with some component of the inorganic residue remaining after oxidation, or with some other solid material present, in such a way as to be irrecoverable by the normal procedures used for solution of the ash. The probability that the types of behaviour listed above will occur will vary markedly with the element to be determined and the method of oxidation selected, but whereas, with one technique, care might be taken to prevent a particular type of behaviour, with another the same type of behaviour could be an advantage.
For this element there would seem to be a good case for using perchloric acid mixtures, where oxidizing conditions can be maintained throughout. The last, and probably the greatest, source of trouble is the presence of chlorine in the sample, and difficulties can arise whether it is present in inorganic or covalent form. In general ionic chlorine will give the least difficulty if its presence is recognized and suitable precautions taken. Digestion of the sample with nitric acid will generally remove chloride ion, as nitrosyl chloride, at temperatures below the volatilization temperatures of most other chlorides.
Included in this general term are the methods in which the sample is heated to a relatively high temperature in a stream of air or oxygen; the related low-temperature technique where excited oxygen is used; bomb methods using oxygen under pressure; and the oxygen flask technique in which the sample is ignited in a closed system at approximately atmospheric pressure. Oxidative fusion methods are considered separately. All the methods involve the following series of processes, although the relative significance of each of them varies from one method to the other.