Feb., 1921
T H E J O U R N A L OF I N D U S T R I A L A N D ENGINEERING C H E M I S T R Y
DR. HENRY A. BUMSTEAD The following resolution on the death of Dr. Bumstead was adopted a t a special meeting of the Interim Committee of the National Research Council, January 3, 1921. RESOLVED, That the National Research Council learns of the death of Dr. Henry A. Bumstead, Chairman of the Council, with great sorrow and profound sense of loss. Dr. Bumstead in his association with the Council had revealed to its officers and members not only a high capacity for administration, and a most loyal fidelity to the aims and work of the Council, but also a sweetness of disposition and personal attractiveness which had won for him the devoted and affectionate regard of all of his colleagues in the Council. I n his death the Council and the scientific world lose a man of most eminent attainments, highest character, and lovable personality. The National Research Council extends to the bereaved wife and family its deepest sympathy and condolence and wishes t o express to them its full appreciation of the great value of the services which Dr. Bumstead rendered it in the period of his association with it and the great loss which it suffers by his untimely death. But may we all remember that “that life is long that answers life’s great ends.” NICHOLS MEDAL AWARD The William H. Nichols Medal for 1920 has been awarded to Dr. Gilbert N. Lewis, of the University of California, for his paper on the “Third Law of Thermodynamics and the Entropy of Solutions and of Liquids,” published in the Journal of the American Chemical Society, 42 (1920), 1529. The presentation of the medal will take place a t the meeting of the New York Section of the SOCIETY,in Rumford Hall, Chemists’ Club, New York City, May 6, 1921. JOHN SCOTT MEDAL AWARD Dr. C. E. Kenneth Mees has recently been awarded a John Scott Medal and Premium by the City of Philadelphia, on the
167
recommendation of the Franklin Institute. The award was made for special researches on the structure of photograph images, which form part of the systematic investigation of photographic theory undertaken by the research laboratory of the Eastman Kodak Co., of which Dr. Mees is director. RUMFORD MEDAL PRESENTATION , The Rumford Medal of the American Academy of Arts and Sciences was presented on Wednesday, January 12, 1921, to Dr. Irving Langmuir, of the General Electric Research Laboratory. PRESIDENT SMITH ADDRESSES JOINT MEETING President Edgar Fahs Smith, of the American Chemical Society, will deliver an address a t the joint meeting of the New York Section of the American Electrochemical Society with the New York Sections of the American Chemical Society and the Societe de Chimie Industrielle and the American Section of the Society of Chemical Industry, to be held in Rumford Hall, Chemists’ Club, New York City, on February 11, 1921. CALENDAR OF MEETINGS American Ceramic Society-Annual Meeting, Deschler Hotel, Columbus, Ohio, February 21 to 24, 1921. American Paper and Pulp Association-Annual Meeting, WaldorfAstoria and Hotel Astor, New York, N. Y . , April 11 to 15, 1921. American Electrochemical Society-Spring Meeting, Hotel Chalfonte, Atlantic City, N. J., April 21 to 23, 1921. American Chemical Society-Sixty-first Meeting, Rochester, N. Y., April 26 to 29, 1921.
NOTES AND CORRFPONDENCE HlSTORY OF THE PREPARATION AND PROPERTIES OF PURE PHTHALIC ANHYDRIDE Editor of the Journal of Industrial and Engineering Chemistry: An article on this subject was published in THISJOURNAL,12 (1920), 1017, by H. D. Gibbs of E. I. du Pont de Nemours & Company. As this article adds nothing to scientific knowledge and also varies somewhat from being an accurate statement of the facts, it was thought appropriate to present the following correction in order that a proper understanding might be reached. The matter under discussion is U. S. Patent 1,336,182, which claims as an article of manufacture, “phthalic anhydride being substantially chemically pure and having a melting point above 130” C. (corrected)” and “phthalic anhydride in the form of colorless needle-like crystals substantially chemically pure and having a melting point above 130” C. (corrected).” It is pointed out by Gibbs that Monroe’ prepared and described phthalic anhydride of a degree of purity which undoubtedly exceeds that of the product described in this patent in 1919 prior to the date of filing of this patent. Monroe2 states in this article that “the resublimed phthalic anhydride produced by the air oxidation process was of a high degree of purity but i t was determined to subject it to a more rigorous purification.” He found the equilibrium temperature of liquid and crystals when this especially purified material was used to be 130.84O. Quoting from his article, “A melting point identical within experimental error was obtained under similar conditions for the original anhydride which was the source of the care1
THISJOURNAL, 11 (1919), 1116 cit.
2 LOC.
fully purified material confirming the previous conclusion that no more than traces of impurities were contained in this.” It can be definitely proved that this original anhydride was a sample of the anhydride produced as described in the patent under discussion (U. S. Patent 1,336,182) and was sent to the Color Investigation Laboratory of the Bureau of Chemistry for investigational purposes. From this there would seem t o be no doubt about the priority of the product described in the patent. It seems quite probable that the anhydride described in this patent is a new commercial article of manufacture. Monroe1 investigated samples of Kahlbaum’s “Phthalsaure Anhydrid” and found the equilibrium point of solid and liquid t o be 129.6’. When this material was subjected t o purification, as in the case of the product obtained by air oxidation, he obtained a constant freezing point of 130.8’, which is the same as obtained from the latter material. He suggests that the original samples obtained contained a considerable admixture of phthalic acid. Certainly the material put on the market by Kahlbaum must have been as good as that sold in commercial quantities. Gibbs states that “a process of manufacture by air oxidation (using vanadium and molybdenum oxides as catalysts) which yields a product in the form of ‘long, colorless, glistening needles’ substantially chemically pure and having a melting point above 130’ C. (corrected) has been described and patented” by himself and C. Conover. The patents referred to are U. S. Patents 1,285,117 and 1,284,888. The essential claim of both of these patents is as follows: “A process for the manufacture of phthalic anhydride, phthalic acid, benzoic acid, and naphthaquinones, which process consists in subjecting naphthalene i n 1
LOG.cit.
168
T H E JOURNAL OF I N D U S T R I A L A N D ENGINEERING CHEMISTRY
the gaseous state and mixed with an oxygen-containing gas mixture, to the action of vanadium (molybdenum) oxides heated to temperatures ranging from 250” to 650” C. When the process is carried out according to the above claims either on a laboratory or commercial scale, phthalic anhydride is produced which may consist of long, glistening needles, but it is always far from colorless and anything but substantially chemically pure, and having a melting point above 130’ C. (corrected). The color ranges from a light yellow to black and the melting point never is as high as 130’ C. There is no mention made in either of the Gibbs-Conover patents as to the purity of the product, but Gibbs bases the disclosure of the remarkable purity of the product on Monroe’s work and an article published by him.’ It has been shown that Monroe carried out his work with material made according to U. s. Patent 1,336,182, which is the one under discussion. The article entitled “Phthalic Anhydride. I-Introduction,” just mentioned, was received for publication August 19, 1919, which was approximately two months earlier than the filing date of U. S. Patent 1,336,182. I t will be evident to those who have had charge of similar problems that two months is a very short time for the development of a manufacturing process for the product in question. In addition to this it can be definitely proved that this product was produced according to the claims of the patent in large quantities a t a much earlier date than either of these disclosures. It is evident also that Gibbs has neglected to consider the judgment reached by the examiners of the Patent Office after a very careful search of the Patent Office records as well as the literature on the subject. In view of the above facts i t does not seem impossible to conceive the grounds upon which such a patent was granted. C. E. ANDREWS TRBSELDENCOMPANY PITTSBURGH, PA.
November 15. 1920
THE IGNITION OF FIRE ENGINE HOSE WHEN IN USE Editor of the Journal of Industrial and Engineering Chemistry: Boston papers of November last had a most astonishing tale of the spontaneous ignition of fire hose when in service. The facts in the case are as follows: It was a new 50-ft. length of the usual 2.5-in. hose consisting of a simple rubber lining inside a heavy cotton jacket. Outside this was drawn a similar cotton jacket. The hose was used in a test made on the new pumping engines, and the stream was throttled down about 45 per cent, discharging about 250 gal. per min. Notwithstanding the fact that this quantity of cold water from the Charles River was used, the hose took fire between the cotton jackets. A spot 2 in. long by 1.12 in. wide was burned clear through each. Careful examination reveals the fact that on each side of the burned hole the inner casings or jackets are very severely chafed. This chafing coming from the vibration produced in the hose by the pump was in my opinion, sufficient to produce great heat and finally active combustion. I found also a similar state of things in another sample of hose used at a later test. The chemical composition of the rubber, in my opinion, had nothing to do with the case. I am of the opinion that the occurrence was due to excessive friction between the cotton casings produced by the vibration of the hose in service. It is interesting t o note that these results have been confirmed by ILlr. J. s. Caldwell, chief engineer oE the N. E. Insurance Exchange, with three different types of engines and three different makes of high-grade, standard hose. The experiments were made in Portland, New Bedford, and Boston, and in some cases the cotton was charred in about 15 min. MASSACHUSETTS INSTITUTE OF TECHNOLOGY A. H. GILL, CAMBRIDGE, MASSACHUSETTS January 13, 1921 1
THISJouarnl~.11 (1919). 1031.
Vol. 13, No. 2
REPAIRING IRON LEACHING VATS Editor of the Journal of Industrial and Engineering Chemistry: Herewith I should like to communicate an experience in repairing leaching vats which may be helpful to others. The bottom of a 5.5 f t . by 22 f t . circular cyanide leaching vat contained numerous holes, and some parts were so badly worn out that a needle could be passed through without effort. At first the leaks were calked with coal-tar soaked cotton waste. This method proved to be inefficient. Then a 2-in. cement bottom was laid on the inside af the tank, but pressure variations during charge and discharge, causing various bendings of the bottom, broke the cement layer in no time. This observation led to the construction of a more flexible bottom, built as follows: Over the whole defective bottom was laid a 0.25-in. asphalt layer, covered with a layer of canvas (in our case old filter leaves). Care was taken that the canvas was pressed on the asphalt while the latter was still hot, in order to secure a close contact. Finally the canvas was covered with asphalt 0.25 in. thick. After 24 hrs. the tank was filled with water, held under water pressure for 72 hrs., discharged, filled again, and held under pressure again for 72 hrs. During this experiment not the slightest leaking could be observed. The total repair cost amounted to approximately $92, whereas a new tank was quoted a t $750. To put a new iron bottom in was impossible, owing t o the fact that the bottom ends of the mantel-pieces would not stand a new riveting. As your Journal, which I receive as a member of the AMERICAN CHEMICAL SOCIET:TY, often gives me helpful suggestions, I should like to help someone who is in trouble. C. FLURY FRENCH MINES TAIYUDONG, KOREA, JAPAN October 13, 1920
VAPOR COMPOSITION OF ALCOHOL-WATER MIXTURES Editor of the Journal of Industrial and Engineering Chemistry: Under the above heading in THISJOURNAL, 12 (1920), 296 W. K. Lewis disposes of the writer’s earlier results on the same subject [THIS JOURNAL, 8 (1916), 2611 with the statement that “The work of Evans is obviously unreliable in view of the fact that he finds the composition of vapor and liquid identical a t 92 per cent by weight.” This statement of Lewis is incorrect, as the writer’s experiments did not extend beyond 91.1 per cent in the liquid, which corresponded to 91.8 per cent in the vapor. In correspondence Lewis says that he obtained the “92 per cent” by slightly extending the writer’s curves beyond the experimental regiongraphic extrapolation. In view of the admitted experimental error of possibly 1 per cent and the absence of evidence of the character of the curves beyond this region, this is manifestly unjustified, especially as the writer expressly accepted 96 per cent alcohol by weight, as found by others, 3s the constant boiling mixture. Lewis’ results are not experimentally obtained by him, but are graphically extrapolated (again) by him from experimental results of Wrewsky, the extrapolation being for as much as 25” beyond the actual observations! Surely experimental confirmation of results obtained in this way might be expected, and would be more convincing than Lewis’ belief that they are “by far the most accurate available.” A comparison of the curves obtained from Lewis’ extrapolated and the writer’s experimental results, pIotting alcohol per cent against boiling point, leaves the probability in favor of the writer, as judged from the form of the curves, especially for boiling points between 90’ and 97’, where they most diverge, Lewis’ curve showing an improbable bulge in this region.
,
