Report on the Production of Synthetic Organic Chemicals in the

Barium acetate, 0.26 per cent calcium, etc. Cobalt nitrate, 0.80 per cent chlorine. Hydroxylamine, hydrochloride, 21.0 per cent residue on ignition. M...
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Dec., 1919

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 CHEMISTRY

OTHER SOLUBLE SALTS-while seldom very bad, these are often contaminated with foreign metals, especially with alkali salts, reaching to tenths of one per cent. The mercury salts almost always leave an appreciable residue on ignition, mostly, if not entirely, iron. Zinc salts frequently contain 0.1 to 0.2 per cent of lead. Hydroxylamine and phenylhydrazine salts are grossly impure, bearing a large proportion of inorganic salts, reaching as high as 24 per cent. The following are a few instances of poor chemicals in the above class: Bari.um acetate, 0 . 2 6 per cent calcium, etc. Cob:rlt nitrate, 0 . 8 0 per cent chlorine Hydroxylamine, hydrochloride, 2 1 . 0 per cent residue on ignition Mercuric acetate, 9 . 0 per cent residue on ignition Nickel sulfate, 1 . 0 0 per cent alkali salts Zinc oxide, 0.22 per cent lead Zinc sulfate, 0 . 3 per cent alkali salts

INSOLUBLE PRODUCTS-This heading is meant to include all difficultly soluble products. It is in this class that we have made the largest proportion of rejections. Here an acceptable chemical is the exception; a poor chemical is the rule. A number of instances follow : Animal charcoal, 25.0 per cent residue on ignition Barium carbonate, 3 . 8 per cent soluble matter Calcium oxide, 22.8 per cent loss on ignition; iron sulfate present Calcium, 2.8 per cent foreign metals Copper carbonate, 4.4 per cent soluble matter Cupi.ic oxide, chlorine present Lead carbonate, 7.0 per cent soluble matter Lead chromate, 7.0 per cent soluble matter, largely acetate Lead chromate, 9.0 per cent soluble matter Lead peroxide, 3 0 . 0 per cent soluble matter “ANAI,YZED” CHEMICALS-At no time has it been our purpose to verify the label “analysis.” Our object was merely to pass on the suitability of the chemicals for our work. It is only incidentally that we have noted discrepancies numerous enough and large enough to warrant our distrust of all label analyses, except those of one firm, from which, however, we have received only a comparatively small number of samples.

SUMMARY

during the last four years about 1300 shipments of chemicals from a large number of dealers and manufacturers have been tested in the Bureau of Chemistry. The greater part of the reagents bore an analysis on the label. 2-Most of the chemicals examined are satisfactory. Occasionally impurities are found often enough in chemicals from practically all manufacturers to make it necessary to test all shipments. 3-The standard acids, ammonia, alkali salts and alkali, and most of the organic solvents are generally satisfactory. 4-The soluble salts other than alkali salts are generally acceptable but are seldom of a high degree of purity. 5-Certain organic solvents and solids are either unobtainable or unsatisfactory. 6-The insoluble products are generally unfit for use in analytical work. BUREAU OF CHEMISTRY

u. s. DEPARTMENT O F AGRICUkTURE WASHINGTON, D . C.

REPORT ON THE PRODUCTION OF SYNTHETIC ORGANIC CHEMICALS IN THE RESEARCH LABORATORY OF THE EASTMAN KODAK COMPANY FOR THE YEAR 1918-19191 By C.

E. K. MEES

The preparation of synthetic organic chemicals was commenced by the research laboratory of the Eastman Kodak Company in Presented before the Division of Industrial and Engineering Chemistry, American Chemical Society, Philadelphia, Pa., September 4, 1919.

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September 1918 in order to supply the demand for these chemicals by research workers in the United States. Proposals for the work were submitted a t the Cleveland Meeting of the AMERICAN CHEMICAL SOCIETY in September 1918, and there approved by the Divisions of Organic and Industrial Chemistry. A report was presented by Dr. Clarke a t the Buffalo Meeting of the AMERICAN CHEMICAL SOCIETY in April 1919; the present report represents experience in the working of the department for a period of eleven months. Much assistance in the undertaking has been received from the American chemical manufacturers, who have willingly supplied not only materials which they had on the market, but in many cases intermediates which they prepared for their own use. Much assistance has also been received from university laboratories. The University of Illinois has supplied a considerable number of the chemicals prepared under the direction of Dr. Adams. Professor Turner, of the University of Missouri, and Prof. H. I. Jones, of the University of Oklahoma, have also supplied a number of substances. Recently, Professor Acree, of the New York State College of Forestry, in Syracuse, has undertaken to prepare pure sugars and indicators. A wider extension of this collaboration is to be desired. If investigators who in the course of their researches make new or interesting organic compounds would prepare and sell small quantities in excess of their needs, samples for experimental or comparison purposes could then be supplied to other workers. Most substances sold have, however, been prepared in the laboratories of the Eastman Kodak Company and all materials listed under the name of Eastman Organic Chemicals have been tested there. The first list of chemicals was issued in January 1919, a second in March, and the most recent list in August 1919-this containing the names of 550 substances, of which 268 were prepared in the laboratory. Up to September I , 1919, a total of 348 preparations had been undertaken. Substances are listed in three degrees of purity: The “Eastman chemicals” are those of the highest purity which can be obtained. The “practical chemicals” are those which are of sufficient purity for ordinary synthetic work, and in most cases these can be substituted in preparations for the Eastman chemicals, especially as information can always be given as t o the impurities which these “practical chemicals” contain. The “technical chemicals” are those which are available on the market in bulk only but are retailed in small quantities for the convenience of both manufacturer and consumer. The financial situation of the work up to date is not very satisfactory. The total loss in the twelve months during which the department has been running is $14,822, this figure not containing any charges for rent or overhead of any kind, and representing only the apparatus, supplies and labor used in the department. This loss covers the whole of the working period and thus includes the first months, during which production was very low. It also includes depreciation in the value of materials bought, which is mainly due to the lowering of prices during the last twelve months. Many materials can now be purchased for much less than they cost during the war, and it has been necessary to write off the value of the stock to cover this depreciation. The investment in the stock is very considerable. The large number of chemicals held in stock and the considerable average value which they represent makes a very heavy investment necessary. At the present time the sales of materials are rising rapidly; but it is not anticipated that the department will meet its expenses during the next year, even with some increase in the prices, which will be necessary. The main cost is in the labor used for the preparations and is due primarily to the small scale on which the material can be prepared as well as to the new experimental work which is necessary in order to add new preparations. About twenty

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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

new preparations are added per month, and in most cases these cost from three to ten times the value of the material made. We believe that with the support of the American chemists we can finally make a success of this undertaking, and we are prepared to continue it in that belief. It is of no use to ignore the fact, however, that the next year will be a critical one for the undertaking, and if the American universities decide to purchase German chemicals, which may be sold a t a lower price than we can supply them, we shall be forced to discontinue this work. If chemists continue to purchase the chemicals from us we hope that finally we shall be able to prepare and supply them a t prices comparable with those a t which they can be purchased from abroad, and with that object we are prepared to continue our work. EASTMAN KODAKCOMPANY ROCHESTER, NEWYORH

THE EXAMINATION OF THE COLLEGE TRAINED CHEMIST FOR GOVERNMENT SERVICE By WILLIAM J. COTTON Received August 11, 1919

There are over one thousand institutions in the continental United States that style themselves as colleges or universities. Previous to the entrance of this country into the World War, the United States Civil Service Commission had recognized a large majority of these institutions as coming under the heading “college or university of recognized standing.” In the pre-war days the examinations of the Commission were for the most part “assembled;” that is, competitors were required to report a t designated places throughout the country and submit to a competitive written examination. With the advent of war this slow ‘method of maintaining registers of qualified eligibles was no longer practical. A more rapid method, requiring a minimum of work on the part of the Commission, had to be devised. The assembled type of examination had almost invariably been used to fill positions paying salaries up to $1800. To fill the relatively few positions paying more than this amount the “non-assembled” type of examination had frequently been used. This latter type of examination consisted of a rating on the sworn statement of education and experience of the applicant as set forth in the application he had filed with the Commission, subject to such corroborative evidence as the Commission desired to secure. To meet the war demand for qualified technical and scientific workers, the Commission decided to use the non-assembled type of examination to fill all such positions except where the government department concerned might request otherwise. Owing to the rather stiff qualifying requirements, the nonassembled types of examination had, previous to the war, produced usually but few applicants. The difficulty of arranging the applicants in the order of merit was not great. The applications could all be compared and rated at one sitting. The extension of the non-assembled types of examination to the lower grade technical positions, and a t a time, too, when for patriotic and other motives, thousands of technical men were answering the call of the Government, meant that on any one of many examinations hundreds of applications might be expected. Because of the lower salaries offered in the low-grade positions, a large amount of practical experience along technical lines could not be required as a prerequisite for consideration. The problem, therefore, essentially resolved itself into that of a just rating of the general and technical education of the applicant. From January 1917to January 1919,the writer served as chemical examiner for the Civil Service Commission. During the first year of this time he was privileged to be associated with Mr. Anton Prasil, now with the National Aniline and Chemical Company. Since the leaving of Mi. Prasil, the writer has

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handled the chemical end of the Civil Service work. Chemists and more especially the faculties of the chemistry departments of our colleges and universities, might be interested to know something of the “education” rating given on the chemistry examinations of the Commission, When the Commission made the decision above noted, three problems immediately presented themselves for solution : First, the vague. expression, “college or university of recognized standing,” which had theretofore been used in announcing examinations, must be replaced by an equivalent expression, the meaning of which would be definite and easily understood by the applicant. Second, for each examination announced, such prerequisites must be established as would insure that the previous training and experience of those passing the examination would qualify them to fill the position for which the examination was held. Third, it was necessary to determine, as accurately as possible, the relative value of the chemical training given a t each college or university from whose students and graduates applications might be received. These problems are stated in the order of increasing complexity. The first problem presented but little difficulty. Conferences with the Bureau of Education, together with the inspection of numerous college catalogues, resulted in recommending to the Commission that by “college or university of recognized standing” should be meant an institution requiring for entrance at least 14 units of high-school work, and for graduation an additional 118 semester credits of college work. It was further suggested that the substance of this recommendation be substituted in the printed announcements of examinations in lieu of the vague phrase theretofore used. The recommendation and suggestion were adopted by the Commission. For instance, the announcement of the junior chemist examination contained this statement: “Applicants must have graduated from a college or university which requires for entrance a t least 14 units of high-school work, and for graduation an additional 118 credit hours. By credit hour is meant * * * * ” It is of interest to note a t this point, t h a t of the institutions coming to the attention of the examiners, five hundred and thirty-one of them met this requirement. Whether or not there are more that could qualify, the writer is not in a position to state. Probably about five hundred and fifty could qualify. The practical operation of this clause soon suggested a further modification. It was found that certain institutions enjoyed an enviable reputation, and yet did not absolutely require more than 8 or I O units of high-school work for entrance. Many students entering these colleges, however, presented a full 14 units of work. In justice to these, the statement was reworded to read: “Applicants must have graduated from a full fouryear high-school course or have completed 14 units of highschool work accepted for college entrance. In addition applicants must have graduated with a degree from a college or university with the completion of a t least 118 credit hours of which * * * *, By credit hour is meant one lecture or recitation or two hours of laboratory work per week per semester.” This wording put the burden of qualifying on the individual applicant and not on the institution. Such a statement stood the test of almost two years of practical usage with uniformly pleasing results. It constituted the solution to the first of the problems above enumerated. Because this article is written primarily for those interested in the college training of chemists, the writer will describe how the second and third problems above noted were solved in the case of one particular type of position, that of junior chemist. The selection of the junior chemist is made because the particular type of chemist sought through examinations of this title is the college graduate, .who has majored in chemistry, and who need necessarily have had no practical experience. Chemists not meeting these requirements are provided for through other

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