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The macro Kjeldahl method has been utilized for nitrogen analyses of a variety of petroleum samples because its technique is simple and the results obtained are accurate. But the use of such a catalyst as mercury for decomposition is undesirable from the viewpoint of subsequent waste liquor treatment.The most important factor in the effective use of the method is the proper choice of conditions for digestion with hot concentrated sulfuric acid.The chemical reactions involved in this type of digestion are so complicated they have eluded detailed studies.In the previous paper2), chemical reactions of various nitrogen compounds with hot concentrated sulfuric acid were discussed from the amounts of sulfuric acid consumed and the quantities of ammonia produced by digestion.In this paper, conditions of digestion for a number of petroleum samples without the use of a poisonous catalyst, such as mercury, were investigated.The final digestion temperature was controlled by the ratio of the amount of potassium sulfate to that of the residual sulfuric acid which was determined by titrimetry or direct weighing after completion of digestion. The extent of recovery of nitrogen was affected by this ratio.Catalytic activities of selenium, mercury and copper on digestion of a number of petroleum samples were similar to those found by Baker1) and Bradstreet3), and they are shown in Figs. 1 and 2, respectively.The amount of sulfuric acid required to digest a petroleum sample increased with increasing boiling point of the sample as shown in Figs. 3 and 4, and the amount of sulfuric acid consumed by the digestion reaction was generally less than 25 times that of the sample. The result is explained by the following equations:CnH2n+2+(3n+1)H2SO4→nCO2+(4n+2)H2O+(3n+1)SO2 (1)CnH2n-6m+3(n+m)H2SO4→nCO2+(4n-6m)H2O+3(n+m)SO2 (2)Where n and m are the number of carbon atom and condensed aromatic ring, respectively. The analytical value of nitrogen content in a petroleum sample was independent of the large excess of sulfuric acid used for digestion as shown in Fig. 5.On the other hand, both the time and the amount of sulfuric acid required for digestion of petroleum sample were decreased by the addition of hydrogen peroxide, and the nitrogen content in the sample was thoroughly recovered independently of the amount of hydrogen peroxide added as shown in Fig. 6.Hydrogen peroxide was found to be very useful as an oxidizing agent for digestion of petroleum samples.
- 公益社団法人 石油学会の論文
公益社団法人 石油学会 | 論文
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