December, 1923
INDUSTRIAL AND ENGINEERING CHEMISTRY
About twelve months ago I printed an account of Microscopical Observations made in the summer of 1827, on the Particles contained in the Pollen of Plants; and on the general Existence of active Molecules in Organic and Inorganic Bodies. I have remarked that certain substances, namely, sulfur, resin, and wax, did not yield active particles, which, however, proceeded merely from defective manipulation; for I have since readily obtained them from all these bodies; at the same time I ought to notice that their existence in sulfur was previously mentioned to me by my friend, Mr. Lister. He adds this information about his lenses: In proEecuting the inquiry subsequent to the publication of my Observations, I have chiefly employed the simple microscope mentioned in the Pamphlet, as having been made for me by Mr. Dollond, and of which the three lenses that I have generally used, are of a 40th, 60th, and 70th of an inch focus. Many of the observations have been repeated and confirmed with other simple microscopes having lenses of similar powers, and also with the best achromatic compound micrgscopes, either in my own possession or belonging to my friends. His sunimary is quoted in full: The results of the inquiry a t present essentially agree with that which may be collected from my printed account, and may here be briefly stated in the following terms, namely: That extremely minute particles of solid matter, whether obtained from organic or inorganic substances, when suspended
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in pure water, or in some other aqueous fluids, exhibit motions for which I am unable to account, and which from their irregularity and seeming independence resemble in a remarkable degree the less rapid motions of some of the simplest animalcules of infusions. That the smallest moving particles observed, and which I have termed Active Molecules, appear to be spherical, or nearly so, and to be between l/zo,oooth and l/ao,oooth of an inch in diameter; and that other particles of considerably greater and various size, and either of similar or of very different figure, also present analogous motions in like circumstances. I have formerly stated my belief that these motions of the particles neither arose from currents in the fluid containing them, nor depended on that [internal] motion which may be supposed to accompany its evaporation.
In Jean Perrin’s little book entitled “The Brownian Movement and Molecular Reality,” the famous French chemist says: They [the particles] go and come, stop, start again, mount, descend, remount again, without the least tending toward immobility. This is the Brownian movement, so named in memory of the naturalist Brown who discovered it in 1827 (very shortly after the discovery of the achromatic objective), then proved that the movement was not due to living animalculac, and recognized that the particles in suspension are agitated the more briskly the smaller they are. If we believe with Perrin and others in the reality of molecules and their continuous movements, then the name of Robert Brown will be immortal.
T h e Testing of Chemicals in t h e Bureau of Chemistry from 1920 to 1923’ By G. C. Spencer BUREAU OF
CAIMISTRY,
T
HE practice of testing all chemicals purchased a t the
Bureau of Chemistry has been systematically followed for over twenty years, with results that have demonstrated the sound economy of this policy. As an illustration of the necessity for watchfulness on the part of Government purchasing officers, instances have been noted where chemicals that had been rejected hy the Bureau of Chemistry were hauled away by the dealer and delivered directly to one of the neighboring bureaus, which accepted these supplies without examination. It is the purpose of this paper to discuss some of the cases that have arisen in the bureau during the past three years with a view to showing: 1-The nature of the objections that may be raised by the purchasers. 2-In vvhat respects the manufacturers may be to blame. 3-A few suggestions that might possibly lead to better uatderstandings between dealers and customers. The following examples of chemicals rejected by the bureau will help to illustrate in some measure the buyer’s point of view: Calcium oxide, discolored by iron and contained about 36 per cent of magnesium oxide Hydrochloric acid, 40 parts per million of arsenic. A replacement order contained 5 parts per million Fuming sulfuric acid, 50 per cent; not over 25 per cent free SO8 found, and was liquid a t room temperature Lead carbonate, 5.37 per cent water-soluble matter Absolute methanol, 5.5 mg. residue per 100 cc. Sodiunt hydroxide, high in sulfates and chlorides / Sulfuric acid, 10 parts per million of arsenic Ammonium thiocyanate, iron enough to give it a pink color Calcium chloride, 8.9 per cent alkalinity as CaO 1 Presented before the Division of Industrial and Engineering Cheniistry at the 66th Meeting of the American Chemical Society, Milwaukee, Wis., September 10 to 14, 1923.
WASRINGTON, D . C.
Potassium carbonate, 8 per cent foreign matter. The second and third replacement orders showed no improvement Absolute ether from two different dealers; both reacted strongly with sodium and contained aldehydes Benzene, put up in wet bottles Acetic acid 99.9 per cent; only 99.6 per cent was found. The manufacturer had depended upon the titration method of assay while the bureau used the cryoscopic method. As soon as the manufacturer adopted the latter method, he had no further trouble in supplying the desired acid strength Chlorinated lime; two samples contained not over 22 per cent available chlorine Ethyl acetate, 16 mg. residue from 100 cc.; brown color with sulfuric acid Carbon disulfide, 6 mg. residue from 100 cc. Amyl acetate, packed in dusty bottles as seen by suspended matter. Two replacement orders were rejected before a satisfactory lot was received. The last of these had a residue of 8 8 mg. from 100 cc. Magnesium oxide, iron and sulfates present Here also may be included the chemical samples that are just on the line of acceptability, not quite bad enough to send back but applicable only for certain kinds of work. Such samples cause more annoyance and take more time than any others. For example, the specifications of the General Supply Committee require a hydrochloric acid strength of 36 per cent and a sulfuric acid strength of 95 per cent. It has happened a number of times that the acid strengths found would run from 2 to 4 per cent below the required amounts. On a t least one occasion the dealer in question offered to adjust the price to conform to the lower strength found. Summarizing the objectionable features in the list just enumerated, it is found that the manufacturers are a t fault in permitting dirty or wet bottles t o be used for purified chemicals. This statement is justified by the number of cases, already cited in this paper, of distilled organic liquids which should be free from
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INDUSTRIAL A N D ENGINEERIhrG CHE,MISTRY
weighable residue, a t least, if they had been handled carefully in preparation. The mistakes of the manufacturers lie in their packing and shipping departments fully as much as in their preparation rooms. This point has been emphasized in letters t o chemical manufacturers, and usually their replies have indicated a good spirit of cooperation and a promise to see that carelessness would be eliminated as far as possible. On the other hand, the customer shares some of the blame. Instead of reporting grievances in a friendly spirit, he often complains to his associates of the poor quality of goods manufactured by the firm in question, does much to give the company a bad name, and buys from some one else. Wherever possible all chemicals purchased should be examined to ascertain their fitness for the purpose for which they are intended. This does not always mean an elaborate chemical analysis. A careful inspection is often sufficient to detect particles of dirt, foreign-colored bodies, and moisture, while in cases of volatile substances the lack of residue a t once proves the absence of heavy metals and of many minerals. Since May 1, 1920, the total number of chemicals passed upon in the Bureau of Chemistry is 465, from 40 different dealers. Of these chemicals 32 (6.9 per cent) have been returned as unfit for the bureau work. Reference may here be made to a previous article on this same subject.2 During the period from 1911 2
Buc, THISJOURNAI., 11, 1140 (1919).
Vol. 15, No. 12
to 1915, mentioned in Buc’s article, about 1300 samples were examined, of which 50 (3.8 per cent) were found to be unsatisfactory. During the war the percentage was three times as much. The conclusion to be drawn from these statements is that American manufacturers are, for the most part, making satisfactory chemicals. There is still a great deal to be done, however. The examples cited in this paper, as well as those given by Buc, show an unwarranted carelessness in preparing and shipping chemicals. Furthermore, all chemists who are experienced in examining those chemicals which bear analyses on their labels know very well how little dependence can be placed on such statements. I n 1921 the writer sent 119 copies of a circular letter to members of the Association of Qfficial Agricultural Chemists, asking for specific statements of unsatisfactory reagent chemicals. Only 17 replies were received, and of these only 5 had any complaints to make. From the lack of response to this letter i t may be assumed that the quality of reagents purchasable in this country is satisfactory; on the other hand, i t may be assumed that most of the recipients of this letter were satisfied to take the legend C. P., or the label analysis, on faith, and to trust to luck. If analytical chemistry is to be defined as the art of taking pains, the necessity for a tareful selection of reagents a t the time of purchase cannot be overstated.
Personals Irving E. Adams, chemical engineer and glass consultant, has terminated his contract with the J. E. Marsden Glass Works, Inc., Ambler, Pa., and is continuing his general glass consulting work a t 623 North Spring Garden St., Ambler, Pa. Fred W. Ashton, of the Structural Materials Research Laboratory of the Portland Cement Association, has been detailed to the Bureau of Standards. R. C. Atwater, formerly employed as chemical engineer with the Beech-Nut Packing Co., is now engaged as chemical engineer with the Atlantic Refining Co., Philadelphia, Pa. John J. Boyle has resigned his position with G. S. Alexander & Co., Inc., and has entered the brokerage field in chemicals and fertilizer materials, with offices a t 140 Liberty St., New York, N. Y. Ralph F. Brenner, formerly chief chemist of the H. C. Fry Glass Co., Rochester, Pa., is now connected with the Vitrolite Co., Parkersburg, W. Va. A. C. Bright has resigned his position as assistant physicist a t the Fixed Nitrogen Laboratory, Department of Agriculture, to accept an appointment as experimental engineer in the engineering department of E. I. du Pont de Nemours & Company. Edward Epstein, chemist a t the du Pont Fibre Silk Company’s plant a t Buffalo, N. Y., was seriously injured on November 2, while a t work in the laboratory, when a retort of chemicals flared up, badly burning his face. Carl Fellers, formerly associated with the Bureau of Chemistry and with the National Canners Association, has been appointed associate professor of the newly established department of food preservation, University of Washington. Arthur C. Gerlach, formerly of the Bureau of Yards and Docks, Navy Department, has been appointed as an assistant dust explosion prevention engineer and assigned to the office of Development Work of the Bureau of Chemistry, Washington, D. C. Bernhard G. Hartmann has been transferred from the Chicago Food and Drug Inspection Station of the Bureau of Chemistry to the Food Control Laboratory, Bureau of Chemistry, Washington, D. C. Lucille Johnson, who recently completed some research under the direction of A. W. Thomas a t Columbia University, has accepted a position as instructor in the Household Science Department of the University of California. Roland M. Kohr, formerly with the National Refining Co., Findlay, Ohio, is now metallurgist and special chemist for the Grasselli Chemical Co., Clarksburg, W. Va. Norman W. Krase has resigned his position in the Fixed Nitrogen Research Laboratory, to accept an instructorship in the Department of Chemical Engineering a t Yale University.
M. A. Lamme, formerly engaged in chemical and geological work in South America, has recently joined the research staff of the manufacturing organization of the Western Electric Co., Hawthorne Works, Chicago, Ill. Arthur D. Little, president of Arthur D. Little, Inc., was elected life member of the Corporation of the Massachusetts Institute of Technology at the fall meeting of the corporation held on October 24, 1923. Benno Lowy, of San Francisco, Calif., a chemist associated with the Pacific Chemical Laboratories, has been reappointed official chemist of the New York Produce Exchange for the Pacific Coast territory and the Orient. L. P. Miller has left the employ of the National Aniline & Chemical Co., Buffalo, N. Y., to accept an appointment in the control laboratory of the mill of the West Virginia Pulp & Paper Co., Piedmont, W. Va. B. H. Nissen, who received his B.S. from the University of Wisconsin in June, 1923, has accepted an appointment as research chemist for the Blue Valley Creamery Co., Chicago, Ill. B. Sandmann, who recently spent some time in Venezuela, has returned to New Orleans and will continue his former business as consulting engineer, specializing in animal and vegetable carbons. Earl A. Sewell, who received his degree of chemical engineer from the Tri-State College of Engineering, Angola, Ind., in August, 1923, has accepted a position as chemist in the laboratory of the Huron Portland Cement Co., Alpena, Mich. Philip P. Sharples, who for the past eighteen years has been in the employ of The Barrett Co., is now connected with the Palos Verdes Project, Redondo Beach, Calif. Harold Stose, who was connected with the Research Laboratory of Applied Chemistry a t the Massachusetts Institute of Technology, has accepted an appointment in the chemical department of the Hood Rubber Co., Watertown, Mass. Victor H. Transue resigned from his position in the laboratory of the Barber Asphalt Co., Maurer, N. J., to accept a position in the research laboratory of the Barrett Co., Frankford, Pa. J. E.:Underwood has resigned his position as research chemist with the Radium Emanation Corporation, to join the staff of the National Lime Association as assistant chemical director. A. T. Ward, who has been associated with the Union Carbide & Carbon Corp., New York, has gone in business for himself, operating under the name of Acme Coal Mining Sales Corp., 20 Broad St., New York, N. Y.
