MAY 15. 1938
ANALYTICAL EDITION
rotating, yet allow it to tip 1x1 every direction as the drive shaft rotates (Figures 1 and 2 ) . The contents of containers or bottles mounted on the platform are shaken very effectively by this eccentric action. Details of construction are shonn in the illustrations. The motor used by the author is a Motorola phonograph attachment equipped with a built-in reducing gear and a vertical shaft. Other types of phonograph motors should be as satisfactory, and can generally be obtained on the second-hand market. The speed of the drive shaft should be about 100 to 200 r. p. m. for good results. The ball bearing by which the platform is joined to the drive shaft is made from a steel chest caster with ball-bearing swivel joint. This type has a flat steel plate for fastening to furniture by mood screws. The wheel is removed and the frame cut down and drilled so that it can be bolted securely to a wooden block. The block is attached to the drive shaft as shown in Figure 2. The flat plate of the caster is fastened to the platform with screws. The platform is 22.5 cm. (9 inches) in diameter and 1.25 em. (0.5 inch) thick. A circular disk of mood, 7.5 cm. ( 3 inches) in diameter and 1.9 cm. (0.75 inch) thick, is mounted in the center of the platform. Six screw eyes in this block are used for fastening the flasks to the platform. The metal cups in Khich the flasks are set are Kerr Mason jar rims. A ring made of KO. 16 B. & S. wire, with two hooks soldered at diametrically opposite points, is slipped over the neck of a flask and anchored to screw hooks in the platform by means of several rubber bands. The three springs which anchor the platform t o the base may consist of several long rubber bands each, or of long coil springs. These springs must not be so &owerful as t o prevent motion of the shaker platform, and must e of equal strength.
283
K E R R MASOH JAR R I M SCREW H W K S
RUBBER BANDS (OR COIL SPRINGS)
1FIGURE2. DETAILSOF
DRIVE S H A F T
SHAKING
EXTENDED ro HOOK IN BASE
API’ARATUB
The base on which the whole apparatus is mounted is of heavy lumber. Careful selection of the motor is of vital importance t o the success of this machine. A motor with good bearings, easily lubricated, and capable of running a long time without overheating is the ideal type. A rheostat may be used for a speed control. RECEIVED March 7 , 1938.
An Improved Mercury U-Gage A. ZIMMERLI, New Jersey .4gricultural Experiment Station and Rutgers University, New Brunswick, N. J.
T
HE most widely used manometer for the measurement
of moderately low pressures-for example, in vacuum distillations-is a U-shaped glass tube with one end sealed and filled with mercury. I t s usefulness is based mainly on its simple direct indication of the absolute pressure which can easily be read a t any moment. It has, however, some objectionable features-for example, the necessity of boiling the mercury in the glass tube to remove the air from the closed reference limb when filling the gage and the ease with which air gets into the reference limb after short service, rendering i t useless for accurate work. The customary constructionhas the added drawback of inaccuracy due to capillary action on the meniscus of the mercury. The modified gage described here has been designed to overcome these difficulties while preserving the desirable features of the U-gage, and is essentially a modification of the manomet e r r e c o m m e n d e d b y yon Rechenberg (4). Referring to Figure 1, A and B are the limbs of a U-tube, each having a diameter of 16 mm. Tube A , the indicating limb, is connected to the vacuum line in the customary manner. Tube B, the reference limb, however, instead of being sealed at the top, is connected to a capillary tube, FIGURE1
C, which in turn is joined to a wide tube, D, a t the bottom. D is also connected to the vacuum line. This connection of both the indicating and the reference limbs to the same vacuum line forms the fundamental difference from the ordinary U-tube manometer which has a closed reference limb. It greatly facilitates filling the gage and maintaining i t in perfect working condition. To get the gage ready for operation, mercury is poured through the side tube until A and B are about two-thirds full. It is then connected to a good vacuum pump and exhausted. By inclining it backward almost to a horizontal position and by tapping the glass sharply, the air adhering t o the glass walls is brought to the surface of the reference as well as of the indicating column, and removed by the pump. When no more air bubbles are visible under the reduced pressure at which the gage is t o be used, it is tilted to the left until mercury flows over the top of B through C into D , thus removing the last traces of air from B and forming a seal which prevents air from getting into it again. When the mercury level in A approaches the bottom, the gage is put back into its vertical position and the vacuum is released. The mercury will rise in C and €3 until the two columns flow together at the top of the bend, filling B and C completely. The levels in A and D should be about 20 mm. above the bottom, so as to form an effective seal. The gage is now ready for use and may be connected t o the apparatus in which the pressure is t o be measured. As soon as the pressure is reduced to a value corresponding to the difference in heights of the mercury columns in A and B (or C and D ) , the mercury will separate at the top of the bend, between B and C, and as the pressure diminishes each part will recede in B and C until the levels become constant. The difference in height of the mercury levels in A and B indicates the absolute pressure.
For accurate and convenient reading of the pressure the gage may be provided with blackened metal sleeves which can be moved u p and down over limbs A and B. When
IKDUSTRIAL AND ENGIKEERIKG CHEMISTRY
284
viewed against diffused light the lower edges of the sleeves and the meniscus of the mercury show up against a white background as sharply defined straight and curved lines. T h e n the sleeves are adjusted so that they seem to touch the tops of the mercury columns the absolute pressure is represented by the difference in height between the edges of the sleeves. (A gage with arrangements for reading to 0.1 mm. is manufactured by the Scientific Glass Apparatus Company, Bloomfield, Pi. J., U.S.Patent 2,075,326, March 30, 1937.) The reasons for choosing a comparatively wide diameter for the limbs of the manometer are threefold: 1. The mercury meniscus is independent of forces of capillary
attraction. 2 . The visibility is greatly improved, even if the inside of the glass becomes dirty after long use. The production of a film on the glass can be minimized by avoiding contact of the mercury with rubber, by using clean mcrcury free from other metals (b), and by t’rapping dust and mist by an appropriate filter. 3. Air, which after long use or by too sudden release of vacuum may get into the reference limb, will collect a t the t,op of the bend in C. If the air bubble has a diameter of 0.2 mm., a size clearly visible t o the naked eye, its volume would be 0.42 cu. mm. at 7.6 mm. of mercury (0.01 atmosphere) and 4.2 cu. mm. at 0.76 mm. of mercury (0.001 atmosphere). -445the cross section of B
VOL. 10, KO. 5
is 200 sq. mm., the height of the air layer would be 0.0021 mm. at 7.6 mm. of mercury, and 0.0210 mm. at 0.76 mm. The error caused in the reading would be 0.03 and 2.8 per cent, respectively. Even such small errors can be avoided by driving the air out of C in the following manner: The gage is tilted to the right until the mercury level in D approaches the bot’tom, and is connected with the vacuum line while in thie position. When the gage is evacuated, it is tilted to the left until the mercury flows over the top bend of C, pushing the air out into D. When the level in -4 approaches the bottom, the gage is put back in its vert,ical position. For correct reading it is necessary to have the gage in a perfectly vertical position. Other precautions to be observed, especially for pressures of 2 mm. and less, have been discussed repeatedly in the literature (1, 3).
Literature Cited (1) (2) (3) (4)
Burton, M.. IXD.EYG.CHEM.,Anal. Ed., 9 , 335 (1937). Easly, H. F., Ibid., 9, 82 (1937). Hickman, K. C. D., Reo. Sci. Instruments, 5, 161-4 (1934). Kechenberg, C. van, “Einfache und fraktionierte Destillation,” Miltitz hei Leipzig, Schimniel 8: Co., 1923.
RECEIVED February 12, 1938. Journal Series paper of t h e New Jeraey Agricultural Experiment Station. D e p a r t m e n t of Agricultural Biochemistry.
High-Vacuum Fractional Distillation without Gravitational Reflux G. VOh ELBE
*%DB.
R. SCOTT. Coal Research Laborator?. Carnegie Inqtitute of Technolog?, Pittsburgh, Pa.
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\ I I I SCHEhLlTIC REPRESESTATIOS O F A N .%PP.IR.ITUS FOR HIGH-VACUCM FRACTIOS l L DISTILLATIOX AS U 6 E D FOR S E P l R A T I o X OF
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HE usual method of fractional distillation involving
gravitational reflux cannot be applied to the separation of mixtures of substances of low rapor pressure, since, to maintain a reasonably fast reflux rate, the vapor pressure of the components must, in general, exceed 1 mm. Furthermore, this method is not applicable to liquid volumes smaller than a few milliliters, since the holdup losses then become a significant fraction of the total input. K i t h the following apparcntly not previously described method, which is free from
gravitational reflux, the mixture to be fractionated is placed in a rather long, evacuated glass tube, along which for a certain distance a temperature gradient is maintained by a thermostat system. The mixture tends to accumulate a t the low-temperature end of the gradient, which is the coldest part of the tube; by pulling the latter slowly and uniformly through the gradient in the direction toward the warm end. the mixture can be made to distill continuously within the gradient and to separate more or less completely into its com-
