Large-Size Extractor for Liquids FREDERICK W. SCHREIBER 934 Brill St., Philadelphia, Penna.
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URING the isolation of certain alkaloids from aqueous
concentrates, i t became necessary t o employ some method whereby sizable quantities of solution could be extracted continuously with ether until alkaloid-free. Although many authors ( I , 2, 4, 6, 7 ) have described largescale apparatus for the extraction of solid material, the writer has been unable to find in the literature any description of a plant-size extractor for liquids. Employing the principles embodied in the liquid extractor described by Palkin (6), a n apparatus has been built for the extraction of 40-liter batches of liquid by lighter-than-water solvents.
used when the material being extracted is unstable at room temperature. C and C’ represent six hollow cylinders sealed at one end and constructed of Aloxite brand porous corundum (medium grade), These cylinders are attached by corks to the six legs of a radial glass manifold, which, in turn, is connected by means of 15-mm. glass tubing to the 500-cc. aspirator bottle, E . The remaining parts of the extractor consist of three Allihn condensers, F , F’, F”, a spherical condenser, G, a 12-liter Pyrex balloon flask, I , and miscellaneous glass fittings such as are found in every laboratory. K is made of 40-mm. glass tubing, the short leg of which has been tapered to meet the T-tube at L. M is a cork “umbrella” to prevent condensed moisture from running into E.
Operation of Extractor
Description of Extractor As shown in Figure 1, A is a glazed earthenware 60-liter crock equipped with lid. A hole 25 mm. in diameter has been drilled in the center of the lid, and a similar hole drilled in the side of the crock about 15 mm. above the 40-liter level. B is an ice bath
The aqueous concentrate to be extracted is placed in A and, if necessary, is diluted to 40 liters. The solvent (ether in this case) is placed in I along with the necessary acid solution, if the alkaloid is t o be converted immediately into a salt. The solvent is brought to a boil by means of water bath J , the vapor passes up through K , is condensed by F , F’, and G, and drops into E . The purpose of E is to enable the operator to follow the rate of flow. The solvent passes from E down into the porous cylinders, from which it emerges as a fine spray. As this spray rises through the aqueous liquid, it extracts the alkaloid and spills through the side outlet back into I. F” revents hot vapors from I from passing into l a n d heating the liquid. Portions of solvent are drawn off at N from time to time and tested chemically to determine completion of extraction. This extractor has been in use in the writer’s laboratory for over a year for the extraction of the recently discovered ergot alkaloid, ergonovine. A t an approximate concentration of 0.025 per cent this particular alkaloid is completely extracted by ether in 10 to 12 hours’ operation of the extractor, as evidenced b y a negative test with Glycart’s modification of Smith’s reagent (3). Less than 500 cc. of ether is lost during an 8-hour extraction. T h e size of the setup can be varied t o accommodate t8hevolume of liquid to be extracted.
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Literature Cited (1) Cameron, A. E., IND. ENQ.CHEM., Anal. Ed., 4, 394 (1932). (2) Drake, N. L., and Spies, J. R., Ibid., 5,284 (1933). (3) Glyoart, C. K., J. Assoc. Oficial Agr. Chem., 20, 566 (1937). (4) Grant, L. S., and Pilling, W. M., IND.ENO. CHEM.,Anal. Ed., 6,285 (1934). (5) McCay, C. M., Ibid., 5, 213 (1933). (6) Palkin, S., Murray, A. G., and Watkins, H. R., IND. ENQ.CHEM., 17, 612 (1925). (7) Quick,A. J., Ibid., Anal. Ed., 5, 76 (1933).
FIGURE 1. DIAGRAM OF EXTRACTOR
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