1980 年 59 巻 6 号 p. 377-381
Combination of the pyrolysis method, previously invented by the authors, and the semi-micro gasification method, presented in the current JIS method for the nitrogen in coke, was investigated in order to establish a new method for the determination of nitrogen in coal.
Hongay and Yubari coal were selected as typical coals of anthracite and bituminous coal, respectively, to investigate the optimum conditions of the method.The optimum analytical procedure is demonstrated as follows.
A coal sample of 0.1g, pulverized up to under 149pm in diameter, was accurately weighed out, and mixed with powdered soda lime of 1.5g.The mixture was distributed in a sample boat, and uniformly covered with FeCl3-Al2O3 catalyst of 2.0g, prepared by mixing FeCl3 aq.soln and active Al2O3 for column chromatography and drying.The boat was inserted into the hot zone of a pyrolysis tube heated at 900-1, 000°C.The nitrogen in the sample was pyrolyzed in the presence of steam (3.0g/min of flow rate) and converted to ammonia quantitatively within 10 min.The ammonia was determined by the conventional titration method.
The method was applied to various coals, and the results agreed with those obtained by the current JIS method (semi-micro Kjeldahl method).