s40
T H E JOURNAL OF I N D U S T R I A L A N D ENGINEERING CHEMISTRY
'/a
in'
with
a
flange a t the t o p a n d a heavier one a t the bottom, 'both being on t h e outside; a plate in. thick, perforated with l / S 2 in. holes (l/8 in. center t o center) extending t o within l / g in. of the circumference:' a ring 9/16 in. wide -and l/g in. thick, threaded on the inside a n d milled on t h e outside, having a shoulder (or offset) on the upper inside which engages t h e lower upper surface of theshoulder of thecylinder, this latter preventing the ring from passing over the lower end of the cylinder; a coneshaped lower portion with stem having also a flange at t h e t o p '/4 in. thick a n d threaded on t h e outside so as t o mesh with the threads on t h e inside of the ring. T h e lower flange of the cylinder, t h e plate, a n d the t o p of t h e flange of t h e cone have approximately t h e same outside diameter as must also the gasket and filter paper to be used. T h e upper flange on t h e cylinder is n o t essential, except for strengthening the same; b u t the lower is essential as a shoulder of resistance for the ring when the cylinder, plate, cone, gasket, and paper are pressed together, b y meshing the ring FIG.2 with t h e cone. I n preparing the funnel for filtering i t is only necessary t o have the lower flange of the cylinder, the filter paper (placed on t o p of the plate), t h e perforated plate, t h e gasket (placed between the flange of the cone a n d plate), a n d the flange of the cone flush with one another, pass t h e ring with flange or shoulder uppermost over the t o p of the cone, screwing as tight as necessary t o secure a perfect joint. A key made of hard wood a n d carrying two slots which engage t w o offsets shown in t h e drawing a n d plate, opposite each other on the lower p a r t of the cone, facilitates t h e operation of tightening a n d loosening the parts. Another smaller funnel having approximately the dimensions 2 3 / 4 in. x I'/~ in. b u t in which t h e perforated plate is not separate b u t a p a r t of t h e cone h a s t h e advantage t h a t t h e rubber gasket is eliminated. I n this funnel the perforated plate is depressed '/IS in. below t h e upper edge of the cone flange a n d brazed in. Here i t is only necessary t o place t h e filter paper on the t o p of the perforated plate a n d screw t h e ring over the cone. RESEARCH LABORATORY PARKE,DAVISAND COXPANY DETROIT, MICHIGAN ~
11,
No.
2
A CONVENIENT AND EFFICIENT DIGESTION APPARATUS
DESCRIPTION
T h e funnel is of aluminum a n d consists essentially .of four parts having the following dimensions: a cast hollow cylinder approximately 4 in. high, 3 l / 2
in' in diameter,
Vol.
FOR THE DETERMINATION OF CRUDE FIBER By HOWELLD. SPEARS Received November 23, 1918
T h e official method of t h e Association of Agricul-
tural Chemists for t h e determination of crude fiber in feedingstuffs calls for the use of a reflux condenser connected t o the digestion container b y means of a rubber stopper. T h e waste of time in connecting a n d
FIG.
1-THIS PHOTOGRAPH SHOWS THE APPARATUS IN OPERATIONAND THE DRAWINGBELOWMAKESCLEAR THE CONSTRUCTION OR THE CONDENSER FLASKS
disconnecting such a n arrangement, where many determinations are t o be made, a n d certain difficulties in its manipulation led t o t h e construction of t h e simple a p p a r a t u s described herein, which is designed for use with tall beakers as the digestion containers. I t s convenience a n d efficiency have been proved b y several years' satisfactory use in t h e feedingstuffs laboratory of t h e Kentucky Agricultural Experiment Station. While there may be a slight loss of water from evaporation during t h e boiling, on account of t h e condensers not being attached t o t h e digestion containers by a tight joint, yet it is believed t h a t the concentration of t h e solvents t h u s brought about is not enough t o cause a n appreciable error in t h e results.
I
00
1
3
/I I\
FIG. 2
T h e condensers are a series of round flasks, with intake a n d outflow tubes, connected b y rubber tubing, through which flows t h e water for cooling. They are
Feb., 1019
T H E JOURNAL OF I N D U S T R I A L A N D ENGINEERING CHEMISTRY
suspended by loops of sheet zinc or tin, so that i t is easy t o lift a n y one of t h e m for t h e purpose of p u t t i n g a beaker in place or removing it or for washing down particles f r o m t h e sides. The flasks are a b o u t 2 ‘/8 in. in diameter, so as t o rest properly in t h e m o u t h of a n e x t r a tall beaker 2 in. diameter, 6 in. tall, and of a b o u t 3 7 5 cc. capacity. The addition of a few drops of a m y l alcohol t o prevent foaming also prevents material from creeping up the sides of t h e beakers. T h e following are some of the duplicate determinations made with this apparatus.
141
CRUDET
F CCIITBNT ~ ~
L
~
~
LL
FEEDSTUFF Per cent Per cent Cottonseed Meal.. .................. 15.28 15.23 Cottonseed Meal.. .................. 12 .OO 11.95 10.35 Cottonseed Meal.. 10.45 27.25 Cottonseed Feed.. 26.70 Brewer’s Dried Grains.. 14.43 14.73 Brewer’s Dried Grains.. ............. 14.13 13.68 Distiller’s Dried Grains. ............. 11.20 11.15 Distiller’s Dried Grains. 12.85 12.98 Alfalfa Meal.. ...................... 31.10 31.80 Wheat Bran and C o b . . 17.95 18.00 Wheat Bran.. 10.75 10.53 Wheat Shorts.. 9.28 9.20 Mixed Feed Wheat and Corn). ....... 11.98 11.76 Mixed Feed ICorn, Oats, and Alfalfa), 16.78 16.93 Rye Feed. 4.60 4.45 Hominy Meal.. 3.95 4.13 Chick Food.. : 2.88 2.93 KENTUCKY AGRICULTURAL EXPERIMENT STATION LEXINGTON, KENTUCKY
.................. .................. .............
............. .............. ...................... .....................
......................... ..................... .... ..................
ADDRESSES AND CONTRIBUTED ARTICLES A REVIEW OF THE AMERICAN PATENT LITERATURE ON ARSPHENAMINE (SALVARSAN) AND OTHER ARSENICALS By H. F. LEWIS Received November 22, 1918
At the present time there is much interest in the United States patents on the aromatic arsenic compounds due to the manufacture of these preparations in America. It has recently been necessary in connection with the work of the Color Laboratory to study the United States patent literature in this field and in order to prevent a duplication of work, the results of the investigation are herewith presented. For some time the value of inorganic arsenic salts had been known in the treatment of trypanosomiasis. Much of the early work was conducted by the Liverpool School of Tropical Medicine, but the inorganic salts they employed had the disadvantage of being toxic in dosage sufficient to have great effect on the trypanosomes. In the year 1902, the Vereinigten Chemischen Werken, A-G, Charlottenburg, introduced the sodium salt of p-aminophenylarsenic acid as an almost non-toxic arsenical, under the name atoxyl.1 This compound permits 40 to 50 times as much arsenic to be administered as in the case of sodium arsenite. In the same year, Ehrlich and Shiga2 started their researches on the subject of chemico-therapeutics, the treatment of parasitic diseases through the injection of chemicals. They studied the effect of atoxyl on trypanosomes, but the strain they used, which happened to be the only one a t hand, lately was found to be the only one nonreactive with arsenicals, and thus they observed no influence. A different result was obtained in 1905 in the Liverpool Tropical Institute by Thomas and They used a strain of trypanosome, which was extremely sensitive to arsenic compounds and so they were able to ascertain a favorable action on trypanosomiasis. When Ehrlich4returned to the study of atoxyl in 1905,he made the discovery that this compound is the sodium salt of p-aminophenylarsenic acid and not m-arsenic acid anilid, as had been stated.6 This discovery opened the way to many new syntheses of compounds possessing greater therapeutic value than the parent atoxyl. Atoxyl was first used as a cure for sleeping sickness and this led to its use in diseases caused bv the Sbidlaceae and esveciallv in the cure of syphilis. In this case, greater doses were necessary and disagreeable after-effects were obtained, blindness being Pharm. Ztg., 47 (1902), 170 and 211; Chem. Zenlr., 1 (1902), 775. B e d . klin. Wochschr., 4 1 (1904), 329 and 362. 3 Liverpool School of Tropical Research, “The Trypanosomes, Trypanosomiasis, and Sleeping Sickness,” Memoir, 16, 50. 4 Ehrlich and Bertheim, B e y . , 40 (1907), 3292. 5 Chem. Ztg., 1, 947; Pharm. Ztg., 47 (1902). 2104. 1
1
caused in many cases. The advent of many new remedies, in addition to the disagreeable after-effects, caused a great diminution in the use of atoxyl. Strange to relate, atoxyl has no action on the trypanosomes in vitro. The fact that this compound has such a marked action on trypanosomes in the human body points to a change taking place in the structure of atoxyl after it enters the body, This Ehrlich and others’ to be due to the reductionof
atoxY1 to P-aminoPhenYlarsenious oxide,
6
, a ComPoUd in
AS = 0 which arsenic is trivalent, that is, unsaturated. On the basis of the Ehrlich theory of immunity, the unsaturated arsenic will unite with the trypanosome, forming an arsenoceptor. Owing to the harmful after-effects of too great a dose of atoxyl, the efforts of investigators were directed toward obtaining compounds of arsenic that would be of value therapeutically and which would a t the same time be without the harmful aftereffects. Such known aryl arsenic compounds as atoxyl, arsenobenzene,2 oxyphenylarsenic acid, and phenylglycinarsenic acid* were used as starting materials in these syntheses. The first American patent on the general subject was applied for by Ehrlich and Bertheim,4 who stated that when p-aminophenylarsenic acid is boiled with acids, acyl derivatives may be obtained. These are of the type of C~H~(NHCOCH~)ASO~H~( I :4). This patent was assigned to Farbwerke vorm Meister Lucius and Bruening, as are all of Ehrlich’s patents. A. Michaelis and C. Schultesin 1881 and 1882 showed that by reducing either phenylarsenic acid or phenylarsenious oxide with the proper agents, such as phosphorous acid, the arsenobenzene, As = As,
A A
[v1 v) , could be produced.
Ehrlich and Bertheims formed
homologues of arsenobenzene by reducing p-arylglycinarsenic acid and obtained arsenoarylglycine, of the type (COOH-CHzNH(4)-Aryl(1)0As = )2. These compounds are used for the same purpose as atoxyl. They are insoluble in water but readily soluble in alkalies. In the Nobel lecture, delivered in Stockholm, December 11, Roehl, 1 Ehrlich, Ber., 4 1 (1909); Milnch. med. Wochschr, 1909, No. 5. B e d . Win. Wochschu., 46, No. 11; Z . Immunitdts, 11 A b t . Ref., 1909, 496. Michaelis, A n n . , 310 (1902), 275. 8 Ehrlich, Ber., 4 1 (1909), 29. 4 U. S. P. 907,016. Applied for, Oct. 3, 1907. Granted, Dec. 15, 1908. 5 6
1908.
Ber., 14 (1881), 912, and 16 (1882), 1952. U. S. P. 888,321. Applied for, Nov. 13, 1907.
Granted, May 19,
