c* If no - ACS Publications - American Chemical Society

c* If no. 5 per cent of bases in any coal-tar oil, the tar-acid separate at this temperature a very small funnel, type 2, should be used for this purp...
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T H E JOURNAL OF INDUSTRIAL A N D ENGINEERING T E S T HI6-TAR

BASES

This test shall be carried out exactly as described under H I I , using 2 0 per cent sulfuric acid instead of I O per cent caustic soda. As there are rarely more than 5 per cent of bases in any coal-tar oil, t h e tar-acid funnel, type 2 , should be used for this purpose. TEST HI7-DRY

SALTS AT

4.5'C.

(4O'F.)

APPARATUS-copper beaker, 500 cc., A. H. T. 21,812, E. & A. 7 50. Buchner funnel (a suitable type is A. H.T. 28,616, E. 8~ A. 3,254). Filter flask (a suitable type is A. H. T. 28,248, E. & A. 3,090). Letter press. Vacuum pump. METHOD-The whole sample of oil after the extraction of t a r acids as in H I I or H I Z shall be used. (Note t h a t this represents I O O cc. of the original oil.) It shall be placed in t h e copper beaker and cooled with stirring t o 4 . 5 ' C. (40' F.) in a suitable b a t h and held at t h a t temperature for 15 min. The contents of the beaker shall then be quickly filtered off on t h e Buchner funnel and t h e oil removed from t h e solids as quickly as possible. The solid cake shall then be removed from the filter and pressed re$eatedly in a letter press between strips of blotting paper or filter paper until only a trace of oil is given u p t o t h e paper. The solids shall then' be weighed. Their weight in grams divided b y t h e specific gravity o f t h e oil gives t h e per cent b y weight of dry solids. PRECAUTIONS-TO quicken the filtering, a spatula should be used t o press the solids down in the funnel and avoid channeling. ACCURACY* I per cent.

C H E M I S T R Y voi. Io,

NO.

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$or oils with limpid points below o o C. a special thermometer graduated from -30° to S O o c*may be wed. The lowest temperature Obtainable by the above freezing mixtures is about c* If no separate a t this temperature a very small amount of powdered naphthalene may be added t o seed out the solids. If no separation can be obtained in this manner, report should be made "no separation Obtainable." MIDDLE OIL TESTS

The usual tests made are water, specific gravity, distillation, t a r acids, dry salts, t a r bases, and limpid point, and these are made in t h e same manner as t h e corresponding tests given above under heavy oil. THEBARRETT COMPANY 17 BATTERY PLACE,NEW YORKCITY

THE POLARISCOPE SlTUATION AND THE NEED OF AN INTERNATIONAL SACCHARIMETRIC SCALE By C. A. BROWNE Received August 5, 1918

Among t h e many claims which are being made upon industry as a result of t h e present war there are probably none more pressing than t h e demand for certain kinds of scientific apparatus. I n the sugar industry alone there is a most serious shortage of polariscopes, refractometers, and colorimeters, and with the inability t o obtain certain repairs the number of such instruments available for technical control is constantly growing less. Seventy years ago practically all of the sugar testing apparatus used in t h e United States came from TEST HIS-LIMPID POINT France, and although most excellent saccharimetric APPARATUS-TeSt tube, 5 in. 10% by 1 in. inside instruments have always been obtainable from t h a t diameter. T'hermometer reading from O o t o 80' as country, nearly all of t h e polariscopes used in t h e used in D6. Distillation apparatus. sugar and food laboratories of t h e United States a t METHOD-Fifty CC. of dry oil shall be taken in a Clean the present time were manufactured in Germany or distilling apparatus such as used for naphthas and * Austro-Hungary. There are several explanations for light oils and distilled t o (Eyyfiess, no thermometer this preference for instruments of German manufacbeing used. The condenser water shall be kept hot ture: (I) Since t h e time of Liebig the technical t o avoid solidification of t h e distillate. schools and universities of Germany have been most The distillate shall be well mixed and 30 CC. trans- frequented by American students, t h e result being a ferred t o t h e test tube. This shall then be cooled, greater familiarity on t h e part of scientists in this using a freezing mixture (3 Parts of shaved i c e t o 1 Part country with instruments of German origin. ( 2 ) At of Salt) if necessary. During cooling t h e Oil shall be the time when many of our industries were established kept agitated b y stirring with t h e them10meter and German emigrants were t h e most available for certain Cooling continued Until a Strong Separation Of Crystals positions and German methods and apparatus were has taken Place. T h e tube Shall now be r m ~ o v e d thus naturally introduced. (3) German manufacfrom the cold bath and warmed a t the rate of 2 o c- turers have been much more active t h a n their French per minute, continually stirring, until all Crystals competitors in bringing their instruments t o t h e atdisappear. The temperature registered by t h e ther- tention of t h e ~~~~i~~~ public. mometer a t this moment shall be recorded as the jviti1 t h e entrance of the United States into t h e limpid point. present war the importation of scientific apparatus PRECAUTIONS-If free water should be present in from G~~~~~~ and Austria came t o an end. Those the Oil, this might be mistaken for crystals, hence who needed polariscopes were thus obliged, as 7 0 dry oil must be used. years ago, t o t u r n t o France, the birthplace and original ACCURACY=k 2 ' c. home of this instrument. The optical establishments of NOTES-The best method t o maintain t h e rise a t France were SO taxed, however, with t h e manufacz 0 C. per min. is t o place t h e tube in a beaker of water ture of periscopes, field glasses, gun sights, etc., t h a t or brine 3 't o 5 ' c. above the oil temperature and warm no time could be spared for manufacturing other the bath, a t about the 2' C. rate. apparatus, although t h e instrument-makers of France

Nov., 1918

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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 E N G I N E E R I N G C H E N I S T R Y

expressed their willingness t o supply the needs of foreign customers as soon as conditions permitted. I n a recent letter upon this subject, addressed t o t h e writer, t h e head of one of t h e oldest establishments in Paris stated t h a t he was most anxious t o bring his polariscopes and other apparatus t o t h e attention of t h e American public. He expressed himself as even willing t o modify t h e types of his apparatus t o satisfy individual preferences, b u t with one very important exception, zliz., t h a t he should not be asked t o copy or imitate German instruments. This exception happens, however, in t h e case of polariscopes, t o be a very important one, for nearly all instruments used at present in t h e United States are provided with t h e so-called Ventzke or German sugar scale, which requires a normal weight of 26 g. I n this connection t h e French manufacturer just mentioned writes as follows: I1 y a de plus la question de la charge type 26 gr. qui parait adoptee aux Etats-Unis. M. Pellet, qui s’est servi de 26.048 gr., puis de 26 gr., aussi bien que de 16.29 gr.. m’assure que 20 gr. est beaucoup plus commode et que c’est 20 gr. la charge type internationale. I1 n’y a pas plus de difficult6 pour moi a faire 26 gr. que 20 gr. ou 16.29 gr.-toutes baskes sur le mCme pouvoir rotatoire du sucre. Je suis nCanmoins oblig6 de dire que je n’aimerais pas faire 26 gr., car j’aurais l’air de copier les Allemands. Or ce sont les Allemands qui en realit6 n’ont fait que nous copier, car les instruments ii lumi&reblanche aussi bien que les instruments A lumihe jaune ont CtC 6tudi6s et construits pour la primiere fois dans ma maison. The feelings of national and local pride, which this manufacturer expresses so openly, are in every respect praiseworthy. The discoveries of Arago, Biot, Soleil, Laurent, and Duboscq have, without question, placed t h e contributions of France t o t h e science of polarimetry above those of other nations. Subtract from t h e s u m total of our knowledge in this field t h e p a r t which France has contributed and t h e remainder is pitifully small. I n certain particulars, however, English and German physicists have made important contributions and nothing is more certain t h a n t h a t t h e t r u e scientist in t h e choice of his instruments will always be guided by expediency a n d not b y prejudice or feeling. If t h e user of a polariscope desires his instrument t o be equipped with a Jellet, or a Laurent, or a Lippich polarizing system, manufacturers should meet this wish irrespective of their own feelings of national or personal preference. But apart from all this t h e question raised by t h e French manufacturer of substituting an international scale for t h e present German standard has a t t h e present time a new and more far-reaching importance in view of t h e increasing consolidation of interests among the different allied nations. Leaving aside t h e fact t h a t t h e Ventzke sugar scale is a German invention, there is much t o be said in favor of t h e United States and all t h e other allied nations adopting a standard which was proposed as long ago as 1896 and which is known as t h e international sugar scale. I n 1896, at the Second International Congress of Applied Chemistry, Sidersky a n d Pellet advocated t h e adoption of a new international sugar scale, t h e normal weight of which should be 20 g. Among t h e advantages suggested for its adoption are the follow-

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ing: (I) The 20 g. scale being a compromise between t h e French 16. z g g. scale and t h e German 26 g. scale is free from all national bias. ( 2 ) The results obtained with t h e 20 g. normal weight are easily converted into percentages by multiplying b y s, while t h e results obtained b y t h e French or German normal weights are not thus easily transformed. ( 3 ) Aliquot portions of jo, 25, 20, I O , and 5 cc. of t h e I O O cc. international scale normal solution represent even gram quantities (IO, 5, 4, 2 and I g . , respectively) which is not t h e case with t h e French or German standards. (4) The specific rotation of sucrose a t a concentration of 2 0 g. in I O O cc. (18.62 per cent) is about the maximum, while it is perceptibly lower a t concentrations above or below this amount. (5) A 20 g. normal weight is always available as a onepiece unit in t h e analytical set. The French and German normal weights are not always available as onepiece units and t o make u p t h e quantity from a n analytical set of weights is inconvenient as well as open t o error. No immediate action was taken b y t h e Second International Congress upon the proposition of Sidersky and Pellet, b u t t h e matter was again brought up a t t h e third, fourth, and fifth meetings of this Congress, more especially b y Dupont, who emphasized t h e statement made by Sidersky in 1896 “ t h a t without revolutionizing or disturbing t h e sugar industry t h e adoption of the proposed international scale would mark a decided step in advance. It would remove all the uncertainties which exist in saccharimetric standards as well as all the inconveniences and mistakes which result therefrom, since it would put in the hands of industrial and commercial sugar chemists analytical apparatus, whose graduation, being upon a n identical basis, would furnish results t h a t were everywhere alike.” While the various Congresses mentioned realized t h e numerous advantages of t h e proposed international sugar scale t h e influence of established usage was too strong t o permit its displacing t h e national standards then in vogue. The representatives of t h e Teutonic nations were particularly opposed t o t h e replacement of t h e German normal weight b y t h e new international standard. In 1912, a t the seventh meeting of t h e International Congress in Kew York, Bates reported t h a t investigations conducted a t t h e U. S. Bureau of Standards showed the present German standard t o be inaccurate inasmuch as 26 g. of pure sucrose would not polarize I O O upon saccharimeters provided with the Ventzke scale under t h e prescribed conditions of analysis. A committee was appointed t o investigate t h e question and make a report in 1915, b u t the outbreak of the war p u t an end t o all further proceedings. I n view of the uncertainty regarding t h e accuracy of the present German scale and in consideration of t h e numerous advantages of t h e proposed international scale, t h e present would seem t o be a fitting time for t h e adoption of a saccharimetric normal weight of 20 g. b y all t h e allied nations. The increasing shipment of sugar from t h e United States and

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T H E J O U R N A L O F I N D U S T R I A L A N D E N G I L V E E R I N G C H E M I S T R Y Vola I O , NO.

Cuba t o England, France, and Italy makes a concerted action of this kind especially necessary just at present, and i t is all t h e more desirable in view of t h e probability of an economic league in t h e near future between t h e various allied countries. If this could be done our sugar and food chemists would have a t their disposal a convenient, rational, accurate standard, while our confreres in France, relieved from t h e embarrassment of having t o copy a German scale, would be free t o supply t h e demand for polariscopes, t h e increasing shortage of which is becoming at present a serious detriment in many industries. An objection which has been urged against a change in t h e present sugar scale is t h a t all polariscopes now in use would be rendered valueless. This objection, however, as Dupont pFointed out at the Fifth International Congress of Applied Chemistry, is not a serious one. Polariscopes can be equipped with t h e new scales a t little cost and without changing t h e optical construction of t h e instruments. If t h e adjustment of t h e new scale could be performed b y our National Bureau of Standards t h e various polariscopes of t h e country would for the first time be placed upon a strictly uniform basis of comparison. Differences of as much as 0.3 have been noticed b y the author between the r o o o point of different German saccharimeters supplied t o t h e American trade. Preliminary t o t h e adoption of t h e proposed international sugar scale a committee of scientists from t h e different allied countries should agree upon a cons t a n t for the angular rotation of a normal quartz control plate wbich shall read roo’ upon a saccharimeter whose r o o o point has been established b y polarizing 2 0 g. of dry, chemically pure sucrose under t h e prescribed conditions of analysis. When this rotation value of t h e normal 100’ quartz plate has been established for sodium, mercury, or other monochromatic light, instrument-makers and users of polariscopes will have an infallible means of verifying the accuracy of their scales.

I

If instrument-makers will then show a disposition t o meet t h e wishes of their patrons in minor matters of construction there is no reason why t h e manufacturers of the allied nations cannot win for themselves a share of t h e market which heretofore has belonged almost exclusively t o the Central Powers. The manufacturers of t h e United States could find no better time t h a n t h e present in which t o make plans for the manufacture of polariscopes, saccharimeters, refractometers a n d other instruments t h a t were formerly imported from Germany a n d Austria. Before entering this field, however, t h e y should make it their aim t o adopt only those standards a n d types which are most convenient in t h e opinion of t h e chemists who use them. Heretofore chemists have been obliged t o take what t h e manufacturer was cont e n t t o offer. It is time t o reverse this illogical method of procedure. Let t h e chemists outline their specifications a n d give their orders t o t h e manufacturer who is most ready t o meet t h e m . The writer is already in consultation with sugar chemists upon specifications for saccharimeters. As i t will probably be many years before commercial and scientific relations are resumed with t h e Central Powers, it would be t h e height of folly t o wait for t h e resumption of such relations before restoring our depleted stocks of apparatus. I t is time t h a t we made ourselves independent of t h e Central Powers in this respect as in all others. Uniformity of standards will make it much easier for one allied nation t o supply t h e wants of another and will greatly help towards preserving t h a t spirit of united action which a common enemy has brought about. The same intimate cooperation which exists between t h e Allies a t the battle front will be necessary in t h e great work of reconstruction t h a t is t o follow. I n t h e recent words of Mr. Lloyd-George. “Let us not make t h e mistake of dissolving the partnership t h e moment t h e fighting is over.” NEW YORKSUGAR TRADE LABORATORY 80 SOUTH STREET, N E W Y O R K CITY

I

ADDRESSES THE POTASH SITUATION’ By A .

w.

STOCKETT

II

now being erected by the Government are in full working order, there should be a sufficiency oE nitrogen. The development of our pyrite supply and the establishment of sulfuric acid plants should insure a supply a t reasonable prices. The potash supply is the only weak link in the fertilizer chain, and the writer is of the opinion that it is possible to develop a domestic potash industry.

I n the last year or two potash has been very prominently before the public, and so much information and misinformatiori has been published that it is very difficult t o present any new facts on the subject. A s over ninety per cent of all the potash used before the war was in the manufacture of fertilizer, the readFOOD CHEM~CAL SOCIETY ing of this paper before the AMERICAN I I Fertilizer Labor may seem somewhat inappropriate. I I I Our dependence before the war on foreign sources for an imPiitrogen Phosphorus Potash portant element in our food supply may be shown by the accompanying diagram. Chilean Nitrates Acid Phosphate German The writer would be prepared t o go even further than the Potash Salts above and for the present have our labor also dependent on a Spanish Pyrites foreign source in the form of interned German prisoners of war. I t is well known to every one that before the war the entire The prospect of becoming independent of these foreign sources world was dependent on Germany for its potash supply, and after the war is promising. When the nitrogen fixation plants this country was importing annually about I,OOO,OOO tons of 1 Paper delivered in the Symposium on Potash held by the Division potash salts of various grades, containing approximately 240,000 of Industrial Chemists and Chemical Engineers a t the 56th Meeting of the tons of KzO. American Chemical Society, Cleveland, September 12, 19 I8

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