T H E JOURNAL OF I N D U S T R I A L A N D ENGINEERING CHEMISTRY
Vol. 13, No. 12
vious analytical results show is further given by fusion experiments made upon the purified sodium salts by Mr. Max Phillips of this laboratory. The methods of fusion and resorcinol determinations have already been described.' The optimum fusion conditions were followed. From the amount of resorcinol found in the fusion mixture the amount of disulfonate necessary for such a yield was calculated. This calculated amount was slightly greater than that found by determining the barium in a weighed sample of the dried salts.
SUMMARY The sulfonation of benzenemonosulfonic acid was carried out a t temperatures approximating 220 ', 250", and 280 ", using acid of 95 and 98 per cent concentration and varying in quantity from 50 to 700 per cent excess. The time variation was from 1 to 10 hrs. The results obtained show that: 1-Of the temperatures tested, 250" is the most efficient, considering time and quantity of acid used. 2-Ninety-five per cent acid gives better results than 98 per cent. 3-A large excess of acid, such as 300 to 700 per cent, is unnecessary. 4-Sodium (introduced as the carbonate) and vanadium pentoxide act as catalyzers separately, but no particular advantage is gained by using both. 5-With sodium as a catalyst, heating for 1hr. is sufficient.
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American Field Service Fellowships for French Universities 2
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FIG.I11 1-Temperature %Temperature 8-Temperature 4-Temperature
220' 220' 250' 250'
C., catalyst none C.,catalyst N a and VzO6 C., catalyst N a C.. catalyst none
that obtained with sodium. The results obtained by using both sodium and vanadium pentoxide at an average temperature of 221" are shown by Curve 4, Fig. 11. Of the former 0.1 per cent was used, and of the latter 0.05 per cent was added. One hour's heating yielded 57.9 per cent of the diacid. Further heating gave a very consistent gain. Curves 2 and 6, Fig. I, and 1 and 4, Fig. 11, are brought together for a further comparison in Fig. 111. These particular curves are chosen in order to represent clearly the best results with and without catalysts at both temperatures, 220" and 250". There is quite a noticeable drop in the amount of disulfonic acid found toward the end of some of the experiments. This is particularly true in those cases where the amount of excess acid is small, or a relatively high temperature is maintained, as shown by Curves 3, 4, and 9, Fig. I. This drop is probably due to the formation of sulfone compounds, such as benzenesulfonesulfonic acid, C&&%C6H4sO3H, and benzenesulfonedisulfonic acid, HS03C6H4S0&6H4S03H. The analytical results obtained where such compounds are present are, of course, in error in proportion to the amount of the sulfonesulfonic acid present. However, the actual ampunt of the disulfonic acid present is greater than the figures in such cases indicate. Evidence tending to prove the presence of such compounds was obtained by making sulfur determinations with the Parr calorimeter. More sulfur was found by this method than the barium method of analysis indicated was present. Indication that a slightly greater amount of disulfonic acid is present at such stage in the sulfonation than the pre-
Attention is again called to the fellowships offered by the Society for American Field Service Fellowships for French Universities. Applications for the 1922-23 awards must be made not later than January 1, 1922. These fellowships, not to exceed twenty-five in number, are of the value of $200 and 10,000 francs. They are awarded for one year, and may be renewed for a second year. They are offered in various fields of science, art, and literature. Applicants must be citizens of the United States, between twenty and thirty years of age, and must be graduates of a college requiring four years of study for a degree or of a professional school requiring three years of study for a degree, or, if not qualified in either of these ways, must be twenty-four years of age and have spent five years in an industrial establishment in work requiring technical skill. A practical knowledge of French is also essential. Application blanks and complete information regarding the fellowships may be obtained from the Secretary, Dr. I. L. Kandel, 522 Fifth Ave., New York City.
Perkin Medal Award The Perk'in medalist for 1921 is Mr. William M. Burton, to whom the award is made in recognition of his work on the distillation of petroleum under pressure, resulting in the production of enormously large supplies of gasoline for fuel in internal combustion engines and of artificial asphalt which is largely used in the place of the natural product. The medal will be presented a t the meeting of the American Section, Society of Chemical Industry. a t Rumford Hall, Chemists' Club, New York City, on January 13 1922. Standard specifications for the testing and use of permissible explosives for use in mines, Bureau of Mines Schedule 17, are now before the American Engineering Standards Committee for consideration and approval as tentative American standard. These standards are the result of thirteen years' experience by the Bureau of Mines in testing and assisting manufacturers to develop explosives that offer the minimum hazard, when properly used, in gaseous and dusty mines. The final revision of these rules was made and approved as Schedule 17 on April 8, 1921. 1
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