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A paper read before the Society of Chemical Industry, London, 1891. From the Journal
The "cryogen," a new apparatus constructed by Mr. E. Ducretet, from instructions given by Mr. Cailletet, is designed for effecting a fall of temperature of from 70° to 80° C. below zero, through the expansion of liquid carbonic acid.
The apparatus consists of two concentric vessels having an annular space between them of a few centimeters. A worm, S, is placed in the internal vessel R. All this is of nickel plated copper. The worm, S carries, at Ro', an expansion cock and ends, at O in the annular space, R'. A very strong tube is fixed to the cock, Ro', and to the ajutage, A'. It receives the tube, Tu, which, at the time of an experiment, is coupled with the cylinder of carbonic acid, CO². A tubulure, D, usually closed by a plug, Bo, communicates with the inner receptacle, R. This is capable of serving in certain experiments in condensation. The table, Ta, of the tripod receives the various vessels or bottles for the condensed products.
The entire apparatus is placed in a box, B, lined with silk waste and provided with a cover, C, of the same structure. Apertures, Th, Ro, and T", allow of the passage of a key for acting upon the cock, Ro', as well as of thermometers and stirrers if they are necessary.
When it is desired to operate, the internal vessel, R, is filled with alcohol (3 quarts for the ordinary model). This serves as a refrigerant bath for the experiments to be made. The worm, S, having been put in communication with the carbonic acid cylinder, CO², the cock, Ro, of the latter is turned full on. The cock of the worm, which is closed, is opened slightly. The vaporization and expansion of the liquid carbonic acid cause it to congeal in the form of snow, which distributes itself and circulates in the worm, S, and then in R. The flakes thus coming in contact with the metallic sides of S rapidly return to the gaseous state and produce an energetic refrigeration. At the lower part of the annular space, R', are placed fragments of sponge impregnated with alcohol. The snow that has traversed the worm without vaporizing reaches R'. and dissolves in this alcohol, and the refrigeration that results therefrom completes the lowering of the temperature. The gas finally escapes at O, and then through the bent tube, T'.
CAILLETET'S CRYOGEN.
The apparatus may be constructed with an inverse circulation, the carbonic acid then entering the annular vessel, R, directly, and afterward the worm, S, whence it escapes to the exterior of the apparatus. The expansion cock sometimes becomes obstructed by the solidification of the snow. It will then suffice to wait until the circulation becomes re-established of itself. It may be brought about by giving the cock, Ro', a few turns with the wooden handled key that serves to maneuver the latter. It is not necessary to have a large discharge of carbonic acid, and consequently the expansion cock needs to be opened but a little bit. A few minutes suffice to reduce the temperature of the alcohol bath to 70°, with an output of about from 4½ to 5½ lb. of liquid carbonic acid. When the circulation is arrested, the apparatus thus surrounded by its isolating protective jackets becomes heated again with extreme slowness. In one experiment, it was observed that at the end of nine hours the temperature of the alcohol had risen but from 70° to 22°. On injecting a very small quantity of liquid carbonic acid from time to time, a sensibly constant and extremely low temperature may be maintained indefinitely.--Le Genie Civil.
In carrying out my improved process in and with the apparatus employed in ordinary commercial distilleries, says Mr. Alfred Springer, of Cincinnati, O.. I preferably employ separate vats or tubs for the nitric acid solution and the material to be treated, and a convenient arrangement is to locate the nitric acid tub directly under the grain tub, so that one may discharge into the other. In the upper vat is placed the farinaceous material, preferably ground, thoroughly steeped in three times its weight of water, and, where whole grain is used, preferably "cooked" in the ordinary manner. The vat into which the dilute acid is placed is an ordinary cooking tub of suitable material to resist the acid, provided with closed steam coils and also nozzles for the discharge of steam into the contained mass. Into this vat is placed for each one hundred parts of the grain to be treated one part of commercial nitric acid diluted with fifty parts of water and brought to a state of ebullition and agitation by the steam coils and the discharge through the nozzles, the latter being regulated so that the gain by condensation of steam approximately equals the loss by evaporation. The farinaceous contents of the upper vat are allowed to flow slowly into the nitric acid solution while the ebullition and agitation of the mass is continued. This condition is then maintained for six to eight hours, after which the mass is allowed to stand for one day or until the saccharification becomes complete. The conversion can be followed by the "iodine test" for intermediary dextrins and the "alcohol test" for dextrin. After the saccharification is complete I may partially or wholly neutralize the nitric acid, preferably with potassium or Ammonium carbonate, preferably employing only one-half the amount necessary to neutralize the original quantity of nitric acid used, so that the mass now ready to undergo fermentation has an acid reaction. The purpose in view here is to keep the peptones in solution also, because an acid medium is best adapted to the propagation of the yeast cells. It is not absolutely necessary to even partially neutralize the nitric acid, but it is preferable. Yeast is now added, and the remaining processes are similar to those generally employed in distilleries, excepting that just prior to distillation potassium carbonate sufficient to neutralize the remaining nitric acid is added, in order to avoid corrosion of the still and correct the acid reaction of the slop.
As a variant of the process I sometimes add to the usual amount of nitric acid an additional one one-hundredth part of phosphoric acid on account of its beneficial nutritive powers--that is to say, to one hundred parts of grain one part of nitric acid and one one-hundredth part of phosphoric acid.
While my improved process is based on the well-known converting power of acids on starch, I am not aware that it has ever been applied in the manner and for the purposes I have described. For example, sulphuric and hydrochloric, also sulphuric and nitric, acids have been employed in the manufacture of glucose; but in every such case the resulting products were not capable of superseding those obtained by the existing methods of saccharification used in distilleries. In my process, on the other hand, the product is so capable. Not only may malted grain be entirely omitted, but more fermentable products are formed and the products of fermentation are purer. The saccharification being more complete, there are less intermediary and nonfermentable dextrins, and the yield of spirits is therefore increased. Malted grain being omitted or used in reduced quantity, there is less lactic acid and few or foreign ferments to contaminate the fermenting mass; also, the formation of higher alcohols than the ethyl alcohol is almost totally suppressed. Consequently the final yield of spirits is purer in quality and requires little or no further purification. Also, further, the nitrates themselves acting as nutrients to the yeast cells, these become more active and require less nutrition to be taken from the grain.
After describing other methods of determining the sensitiveness of plates, Mr. Gf. F. Williams, in theBr. Jour, of Photo., thus explains his plan. I will now explain the method I adopt to ascertain the relative sensitiveness of plates to daylight. Procure a small direct vision pocket spectroscope, having adjustable slit and sliding focus. To the front of any ordinary camera that will extend to sixteen or eighteen inches, fit a temporary front of soft pine half an inch thick, and in the center of this bore neatly with a center bit a hole of such diameter as will take the eye end of the spectroscope; unscrew the eyehole, and push the tube into the hole in wood, bushing the hole, if necessary, with a strip of black velvet glued in to make a tight fit. By fixing the smaller tube in the front of camera we can focus by sliding the outer tube thereon; if we fix the larger tube in the front, we should have to focus inside the camera, obviously most inconvenient in practice. Place the front carrying the spectroscopein situin the camera, and rack the latter out to its full extent; point the camera toward a bright sky, or the sun itself, if you can, while you endeavor to get a good focus. The spectrum will be seen on the ground glass, probably equal in dimensions to that of a quarter plate. Proceed to focus by sliding the outer tube to and fro until the colors are quite clear and distinct, and at same time screw down the slit until the Fraunhofer lines appear. By using the direct rays of the sun, and focusing carefully, and adjusting the slit to the correct width, the lines can be got fairly sharply. Slide your front so that the spectrum falls on the ground glass in just such a position as a quarter plate glass would occupy when in the dark slide, and arrange matters so that the red comes to your left, and the violet to the right, and invariably adopt that plan. It is advisable to include the double H lines in the violet on the right hand edge of your plate. They afford an unerring point from which you can calculate backward, finding Gr, F, E, etc., by their relative positions to the violet lines. Otherwise you may be mistaken as to what portion of the spectrum you are really photographing. The red should just be seen along the left edge of the quarter plate. When all is arranged thus, you utilize three-fourths of your plate with the spectrum, with just a little clear glass at each end. Before disturbing the arrangement of, the apparatus, it is desirable to scratch a mark on the sliding tube, and make a memorandum of the position of all the parts, so that they may be taken away and replaced exactly and thus save time in future.
To take a photograph of the spectrum, put a quarter plate in the dark slide and place in camera; point the camera toward a bright sky, or white cloud, near the sun--not at the sun, as there is considerable difficulty in keeping the direct rays exactly in the axis of the spectroscope--draw the shutter, and give, say, sixty seconds. On development, you will probably obtain a good spectrum at the first trial. The duration of exposure must, of course, depend upon the brightness of the day; but if the experiments are to have relative values, the period of exposure must be distinctly noted, and comparisons made for a normal exposure of sixty seconds, ninety seconds, two minutes or more, just according to whatever object one has in view in making the experiments. With a given exposure the results will vary with the light and the width of the slit, as well as being influenced by the character of the instrument itself. Further, all such experiments should be made with a normal developer, and development continued for a definite time. The only exception to this rule would be in the event of wishing to ascertain the utmost that could be got out of a plate, but, under ordinary circumstances, the developer ought never to vary, nor yet the duration of development. To try the effect of various developers, or varying time in development, a departure must be made of such a nature as would operate to bring out upon each plate, or piece of a plate, the utmost it would develop short of fog, against which caution must be adopted in all spectrum experiments.
On development, say for one, two, or three minutes, wash off and fix. You will recognize the H violet lines and the others to the left, and this experiment shows what is the sensitiveness of this particular plate to the various regions of the spectrum with this particular apparatus, and with a normal exposure and development. So far, this teaches very little; it merely indicates that this particular plate is sensitive or insensitive to certain rays of colored light. To make this teaching of any value, we must institute comparisons. Accordingly, instead of simply exposing one plate, suppose we cut a strip from two, three, four, or even half a dozen different plates, and arrange them side by side, horizontally, in the dark slide, so that the spectrum falls upon the whole when they are placed in the camera and exposed. There is really no difficulty in cutting strips a quarter of an inch wide, the lengthway of a quarter plate. Lay the gelatine plate film up, and hold a straight edge on it firmly, so that when we use a suitable diamond we can plow through the film and cut a strip which will break off easily between the thumb and finger. A quarter plate can thus be cut up into strips to yield about a dozen comparative experiments. When cut and snapped off, mark each with pencil with such a distinguishing mark as shall be clearly seen after fixing. The cut up strips can be kept in the maker's plate box.
The deep down underground electric railway in London has so far proved an unprofitable concern for its stockholders. It is 3½ miles long, touches some of the greatest points of traffic, but somehow or other people won't patronize it. The total receipts for the last six months were a little under $100,000, and they only carried seventeen persons per train mile. On this road the passengers are carried on elevators up and down from the street level to the cars. The poor results so far make the stockholders sick of the project of extending the road.
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