Preparation of Sintered Glass Filters - Analytical Chemistry (ACS

Ind. Eng. Chem. Anal. Ed. , 1935, 7 (2), pp 135–136. DOI: 10.1021/ac50094a028. Publication Date: March 1935. ACS Legacy Archive. Cite this:Ind. Eng...
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A Six-Atmosphere Mercury Manometer WALTERSCHOLLAND R. 0. E. DAVIS Bureau of Chemistry and Soils, U. S. Department of Agriculture, Washington, D. C.

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N MEASURING vapor pressures over solutions of urea and liquid ammonia, a simple mercury manometer capable of measuring pressures u p to six atmospheres was constructed. A method for reading the manometer was provided by the use of a periscopic arrangement consisting of a sliding unit, with a light, a mirror, and a reading glass, mounted to reflect the image of the mercury meniscus downward to another mirror conveniently placed for o b s e r v a t i o n s . The assembled manometer is shown in perspective in Figure 1. The wooden post 13 em. square, as shown at the end section, was made up of five 2-cm. white pine boards. A beam of this c o n s t r u c t i o n was found to be free from warping and had very little bending movement. The Pyrex U was made of tubing 6 mm. outside diameter and 4 mm. inside diameter and the two parallel arms were so spaced as to be close to the scale, mounted b e t w e e n them. The scale was made up from selected wooden meter sticks carefully jointed so as to eliminate, as far as possible, any large corrections. The scale was compared with a Bureau of StandFIGURE 1 ards c a l i b r a t e d steel tape, For convenience in reading, a paper scale was prepared from millimeter coordinate paper, by printing the total millimeters in a horizontal position a t each centimeter of length. The paper scale was shellacked to 2.5-cm. wooden strips and mounted to the right of the mercury U. The strips should be boiled in paraffin to prevent warping.

A track in the form of a T channel, for the accommodation of the slide units Band C, was mounted to the right of the manometer. The track was made by assembling several brass strips: first the base plate (50 X 3 mm.), attached to the beam with screws, and then the spacers (14 X 7 mm.) and face plates (19 x 3 mm.) attached to this by machine screws at frequent intervals to prevent bending the slides. The unit C, a steel piece 17 cm. long, carried a slotted arm to which was attached the lower mirror, and was provided with a thumb screw for locking it in position. The unit B was a slotted steel piece 38 cm. long and provided for mounting the second mirror at 180" to the first and 45" to the plane of the supporting beam. On this unit also was attached a 25-watt bulb blackened so as to illuminate the manometer and scale only and placed just above the mirror. Below the mirror was a 12.5-cm. reading glass adjusted to the focal length, about 15 cm. from the mirror. To the upper and lower ends of unit B were attached the ends of a length of picture wire used in moving the unit. The picture wire passed over four brass pulleys a t the top and bottom, and opposite each other, on the front and back faces of the beam. The wire made several turns on a brass drum, shown at D, which when turned supplied sufficient friction for moving the unit B in any desired direction. To the drum was attached a ratchet and a wooden hand-hold mounted on the end of the axis. The ratchet held B at any desired position. The manometer and attachments were mounted on the wooden beam before raising to the vertical position and adding the mercury. To the top of the U a t A was attached, by means of a metal joint ( 1 ) supported by a clamp, a copper tube through which the gas pressure to be measured was applied. The other side of the U connected to a trap, not shown in the figure, for mercury inadvertently forced out of this arm. Three thermometers, placed at equal intervals along the side of the mercury U, were used for making the necessary temperature corrections. The manometer as constructed had an accuracy of 1 2 mm. a t 5 atmospheres pressure.

LITERATURE CITED (1) McKelvey and Taylor, J.Am. Chem. SOC.,42, 1364 (1920). RECEIVED December 19, 1934.

Preparation of Sintered Glass Filters PAUL L. KIRK,Division of Biochemistry, University of California Medical School, Berkeley, Calif.

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S MANY cases in which sintered glass filters' are highly useful, very fine grades and carefully standardized porosities are not necessary. If, in addition to this, the diameter of disk need not exceed about 15 mm., i t has been found very easy to make such filters directly in the flame of an air-gas blast lamp. Various investigators are making such filters for their own use as aerators and for other simple requirements, b u t it seems desirable t h a t the method be recorded in the literature. The chief field of use of such filters in this laboratory has been in the form of filter sticks similar to those described by Kirk (1). This apparatus is made by blowing on one end of a t hick-walled capillary tube a small thin-walled bulb which is filled with ground glass, mounting the tube in a stirring motor in a vertical position with the bulb down, and rotating the tube in a moderate air-gas blast burner flame for about 10 minutes. If the flame is properly adjusted, the ground glass will sinter through without fusing the bulb walls. The 1 Manufacture of sintered glass filters is covered by patents held by Schott & Gem, in the United States by Patent No. 1,620,815.

glass should scarcely be red during the heating. After cooling, the end of the bulb is ground away, preferably on a slowspeed silicon carbide wheel, until the sintered disk is of proper thickness. For making larger diameters of filter, the process is essentially the same, except that the tuhe is of the correct size for the filter desired. Instead of having a bulb on the end it is simply pulled off in a flame until it is roughly squared across the end, leaving the walls thin, after which the powdered glass is poured in and sintered as described, followed by grinding off the end. For larger filters the heat must be a little more intense. Either Pyrex brand chemical or soda glass may be used, though the former yields the better results. The glass powder may be of any size desired, but not finer than about 200-mesh. For aeratow, coarse filters, and the like, 100mesh is satisfactory, though finer may be used. The filter sticks are most satisfactorily used with asbestos as described by Miller and Kirk (S), and are of the greatest utility when so employed. Another valuable application is in the filtration

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of mercury, as, for example, spraying it into a washing tower. I n this case about a 40-mesh glass should be used. An extremely rapid filtration is obtained with the delivery of a mercury cloud, the particles of which are individually barely visible. While not so universally applicable as the method described by Kirk, Craig, and Rosenfels (d), this method should be of considerable value in solving many special problems arising in the research and analytical laboratory.

CHEMISTRY

Vol. 7, No. 2

A Simple Inexpensive Galvanometer Suspension H. ROSWELLJONES~ Chemical Laboratory, Johns Hopkins University, Baltimore, Md.

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N T H E course of recent work it was found necessary to insulate thoroughly a high-sensitivity galvanometer (Leeds (1) Kirk, P. L., Mikrochemie, 14,1 (1933). & Northrup Co., Type HS) from all mechanical shock. (2) Kirk, P.L., Craig, R., and Rosenfels, R. S.,IXD. EN^. CHEM., This was accomplished with the modified Julius suspension Anal. Ed., 6, 154 (1934). shown. The heavy soapstone slabs, A , are separated by the (3) Miller, R.P.,and Kirk, P. L., Mikrochemie,14,15 (1933). threaded rods, B. The slabs are free to move vertically and can be held in any position by means of the lock nuts, C. RECEIVED February 4, 1935. Aided by a grant from the Research Board of the university of California. The galvanometer, G, rests on a sheet of tin plate, L, which is set on t h e base block. T h e t i n Use Sintered Glass Disks in plate is g r o u n d e d t h r o u g h a flexible Distillations lead and acts as an electrostatic shield M. MATTIKOW, Columbia University, New York, N. Y. for the galvanometer. The legs of the HE writer has had occasion to extract material with galvanometer r e s t large volumes of volatile organic solvents. When the u p o n small blocks extract, containing a high percentage of oily and other matters, of paraffin. was concentrated by distilling the volatile organic solvents, The whole is supconsiderable difficulty was ported by the three experienced in preventing eyebolts, E, spaced bumping. The common ex- a t the corners of an pedients, such as putting in isosceles t r i a n g 1e. glass beads, pieces of por- These are connected celain, pumice, and capillary through the springs, tubing, were found to be of F , to the supportlittle aid. ing dog chain, D. The incidence of bump- All electrical connecing was completely elimi- tions are made by wires dipping into 30-cc. beakers containn a t e d b y i n h o d u c i n g a ing mercury, mounted on small paraffin blocks placed on the sintered filter disk as shown base block. Mercury is used because it allows the use of large i n t h e d i a g r a m . ( S u c h lead wires and a t the same time prevents the transmission of glass tubes are sold com- any mechanical disturbances through the leads to the galmercially under the name of vanometer. It was found that when the galvanometer was “gas distribution tubes with enclosed in a large metal compartment with a glass door, the fused-in fritted-glass filter absolute lack of air currents made the customary damping FIGURE 1 d i s k s . ” ) A i r , F a s s e d vanes of the Julius suspension unnecessary. The metal of the through the tube, is broken box made an efficient electrostatic shield when grounded. In operation the upper soapstone slab is raised or lowered up into many tiny bubbles which keep stirring the solution, thus preventing local superheating. When the solvent has until the center of gravity of the system is a t the mirror, M , been almost all distilled and a fresh charge of extract put in, the of the galvanometer. Under these conditions the system whole is effectively mixed by allowing air to be blown more will rotate about this point and the mirror will be a t the point rapidly through the solution, thereby obviating the necessity of least motion of the system. Then, with the springs abof disengaging the flask from its clamped position and rotating sorbing all vertical impulses and the chain the horizontal or shaking to effect mixing. Several fresh charges have been ones, with the system once in equilibrium, the mirror will not added to the original one by this method without disturbing be disturbed by outside mechanical forces. This condition the distilling flask. Despite the increasing concentration of has been realized in actual operation. This suspension has proved satisfactory in measuring deoily matters, there was no bumping a t any stage. I n certain cases where air is not desirable because it may flections of 0.1 mm. on a scale placed a t l m. with several oxidize the extracted matter, or induce chemical change, an large electric motors operating very close to the galvanometer. inert gas like nitrogen or carbon dioxide may be used. RECEIVED February 25, 1935. It is suggested that heated gases be used to distill the sol1 Present address: The Atlantic Refining Go., Franklin, Pa. vents instead of an outside source of heat. Steam distillation also has been carried out smoothly and effectively by leading the steam through the sintered glass disk.

LITERATURE CITED

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RECEIVED January 12, 19351