ANALYTICAL EDITION
August, 1945
Speedway motor No. 953 W, shaft speed 40 r.p.m., 110-volt, 60-cycle, with shaft in vertical position is suitable (manufactured by the Speedway Mfg. Co., 1834 South 52nd Ave., Cicero, Ill.). The rotor of the Ford timer may be directly attached to one end of a g/16 inch shaft 2 inches long, drilled a t the other end to slip over the shaft of the motor and fitted with a setscrew. The center part of the 9/16 inch brass extension shaft acts as the commutator surface. The motor is fastened in a wooden housing with a hole drilled in the top for the vertical shaft. The commutator brush is mounted on the housing top and the timer's rotor above it. The timer is slipped over this and is kept from rotating by two brass straps bent in the form of an L and fastened to the opposite sides of the timer's housing. Through holes in the base of the brass
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supports, screws hold the housing in place a t the corrcct distance above the top of the wooden housing. Wires from the commutator's brush and from the contact3 on the timer's hou5ing lead to binding posts on the side of the woo,den housing. Speedway motors with different shaft speeds may be obtained, so that practically any number of interruptions per minute desired may be obtained. LITERATURE CITED
(1) Baume, G.,
J. chim. pkys., 9, 245-89 (1911). (2) Booth, H. S.,and Martin, D. R., Chem. Rea., 33, 57-88 (1943).
Apparatus for Rapid Removal of Solvents W. F. BARTHEL AND H. L. HALLER United States Department of Agriculture, Agricultural Research Administration, Bureau of Entomology and Plant Quarantine, Beltsville, M d .
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NE of the problems encountered in the preparation of puri-
fied pyrethrum concentrates ( I ) , using nitromethane as a solvent, was how to prevent .the decomposition of the pyrethrum concentrates while distilling the nitromethane. Conventional vacuum-distillation apparatus for large volumes is likely to be very bulky and unwieldy. When the residue in the still is the desired product, and this is present in the starting solution a t a low concentration, even greater trouble may be encountered. Then, too, removal of the last traces of solvent from the concentrates is often desirable. It has been found that the apparatus described by Smith(@ could be modified for use under reduced pressure and that this modification was excellent for re-
moving medium-boiling solvents from not only pyrethrum concentrates but other plant extracts and organic compounds. The apparatus is pictured in Figure 1. The solution to bc evaporated is placed in the holder, 1. The stopcock, 2, regulates the flow into the boiler, 3. The boiler and the stripper, 6, are heated by means of steam passing in 14 and out 19. A bead, 4, prevents a rush of liquid through constriction 5 into 6. A trap, 8, prevents entrained liquid from passing into the condenser with the vapors. Most of the solvent is evaporated in the boiler, but the remainder is evaporated in t>hestripper so that the combined vapors pass into the condenser, 9, and are recovered. .4 double condenser is used because an extremely long condenser would be awkward. The solute from the stripper is collected in receiver 7, and the condensed solvent collects in receiver 10. Obviously the size of the receivers depends upon the quantity and proportions of solvent and solute. A glass rod, 18, connects the two arms of the condenser to prevent undue strain on the lower point of attachment. With liquids of high vapor pressure it is well to use an ice trap in the vacuum line from 17. A useful part of the apparatus is the steam generator. This is attached to the still a t 14 and is heated by means of coil, 12, connected to a variable-voltage transformer by means of leads, 13. The water level is kept constant a t 11 by recovering the steam through condenser 15. The connecting tube, 14, is large enough to permit any water from condensed steam in the still to pass back into the steam generator. The vent, 16, is necessary to prevent having a closed system; it may also be used for filling the steam generator. The coil, 12, is 240 cm. (8 feet) of KO.22 Chrome1 A wire. I t is important to connect the coil to the power source by means of copper leads from below the water level; otherwisc, the life of the coil will be short. I n actual use thc apparatus has more than met expectations. I n the preparation of pyrethrum concentrates the nitromethane solution seldom contained more than 10% of pyrethrins, yet it was possible to remove the nitromethane almost quantitatively at, the rate of 1500 ml. per hour. When solvent was removed at this rate, it was necessary to run the concentrate through a second time to remove the last traces of solvent. Little extra time is needed to make this second run. At no time has any evidence been found that the pyrethrins have been decomposed in this apparatus. When tested against houseflies, the pyrethrins prepared had the same potency as commercial samples of pyrethrum containing the same concentration of the active ingredients. For liquids boiling below 70" to 80" C. the apparatus can be used without vacuum. I n this manner it can be employed for recovering alcohol and other solvents. By adjusting the pressure, steam flow, and rate of intake, it can be used for the rapid concentration of solutions when it is desired to retain a certain amount of solvent, ais in concentrations prior to crystallization. LITERATURE CITED
W Figure 1.
Diagram of Apparatus
Barthel, W. F., Haller, H. L., aiid LaForge. F. B., S o a p and Sanit. Chemicals. 20, No. 7 , 121, 135 (1944). (2) Smith, F. H., IND. ENG.CHEM.,ANAL.ED., 14, 255 (1942).
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