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The determination of trace nitrogen in various fractions of petroleum has so far been made by the ter Meulen method or Kjeldahl method and Duma's method combined with adsorption3) or extraction technique. However some of the details of the methods have not been elucidated.In the previous paper2), some details on the conditions for preconcentration of nitrogen compounds in various fractions of petroleum by silica gel adsorption and sulfuric acid extraction were given.In this paper, a method for the determination of nitrogen in ppm levels was investigated by using the automatic Duma's method combined with the silica gel adsorption technique mentioned in the previous paper in order to extend the applicability of the JIS method.The reagents and apparatus used conformed to the JIS K 2609, and the nitrogen compounds in the petroleum samples were preconcentrated by the method of the previous paper2).The effect on the blank test value of the mean pore diameter of silica gel used as an adsorbent for preconcentration is shown in Fig. 1.On the other hand, the mean pore diameter of silica gel for practical applications is 40-100Å, that is, not more than 50μl/g as blank test value. The blank test value of silica gel decreased by purging it with carbon dioxide at higher temperatures (Fig. 2), requiring a tedious technique.The comparison of the results obtained by the present method with those by the direct combustion method (JIS K 2609) is shown in Fig. 3 which indicated that the content obtained by the JIS K 2609 was higher than that of the present method combined with the silica gel adsorption technique.In the case of direct combustion of a petroleum sample, large errors are attributable to incomplete combustion of the gases developed.The blank test values obtained by direct (JIS method) and indirect (present method) combustion of a nitrogenfree liquid paraffin sample are shown in Fig. 4.The blank test value obtained by the direct combustion method increased proportionally with the amount of liquid paraffin used; however that of the indirect combustion method was almost independent of the amount used (liquid paraffin was not adsorbed by the silica gel adsorption technique).The distribution of nitrogen compounds concentrated in the adsorption column is shown in Fig. 5, that is, the plot of the fraction of the adsorbent in the column against the relative nitrogen content. The nitrogen compounds in a petroleum sample were completely adsorbed on the silica gel under the optimum condition as described previously2).The comparison of the analytical results obtained by the present method and the macro Kjeldahl method combined with preconcentration by sulfuric acid extraction is shown in Table 1.The automatic Duma's method combined with preconcentration by the silica gel adsorption technique seemed applicable to the determination of small amounts of nitrogen in various fractions of petroleum.
- 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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