A New Laboratory Mill'

mil by its soluhility. The hiiiling point of tltr mixed alrohols separaied after sapotiifieatioil was 190" C. by the capillriry totie method. S o anis...
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Aromatic Constituents of Bourbon Beans

Fur the work on Bourbon beans, prime 20-cni. lieuriiuii Iwans were used. Fifl,y-nine kilograms of the finely chopped material were extracted hy ma,ceration and percolation with chloroform during a period of one month. The chlorofi,rm extract was treated in much the same manner as the extract obtained from the Tahiti beans. Three grams of light yellow volatile oil were obtained. Tlx reSrai,tire index a t 24' C . vas 1.4850; specific gravity at C., 1.079; taste,slightly pungent; odor, agrceirblc sit(! rstremely uersistent; and it was insoluble in boiling watrr or in 40 per ~ e n alcohol t hut soluble in alcohol. On chilling to - 20° C a few small crystals formed, hut the bulk remainrri liqiiic!. .4eids, phenols, and aldehydes had been previously riwioI:id. Appropriate qualitatiT-e tests indicated the prrsenre of ahwhois and enters. A port,ion of the oil was sapiinihed with aqneous pot:assiitni liydmaide solution. From tbe saponification products :I smd1 amount of ciniirimio arid was isolated. This was identified tiv its melting point,, 131 c.,b.v the formation of b e n d drhyde on treating with cold dilute permanganate solotiim, mil by its soluhility. The hiiiling point of tltr mixed alrohols separaied after sapotiifieatioil was 190" C. by the capillriry totie method. S o anisyl alcohol or anisic acid was present, eitber befirre or after the saponification, Ciriiiamir acid mat formd i u small amorint in the alkalinr washing.; wt~ercitnisic Rcid I i u d hrm Sonnrl i n the Tahiti beans. A n i a ~ Alcuhol l i n Vanilla ExtractsTealfor Age of

d r : i r t s were of statrdard stretigt.1, (IO gralirs of beaus per 100 vr.1 and r:oiitained 40 per cent aleohol and 12 grains of sogm per 100 ce. The results are given in the table. Forty per cent alcohol extracts of shavings from oak arid fir harrels gave negative tests. By comparison with known mixtures under identical conditions thc test can be made roughly qiiantitative. Summary

'l'lir whitilc! uil of Tahiti vanilla beans consists cliieHy miisyl iilrohol a,%Wnhlharirn has pointed out. The tieails m i t n i n about O.O(i per rent of volatile oil. Anisic :acid is :also present in these beans. The vidat.ile oil of Bourbon vmiliir kieaia does not coiitaiii i m i s y l alcohol brit consists of a small amount of cinnanrie :wid esters and an unidentified alcohol haviirg a pleasatit persistent odor. Cinnamic acid is present in minute quantities in Bourbon heans. The percentage of volatile oil is Jbiiiit me-tenth of the amount present in Tahiti beans. ;knisyl alcohol is also present in vanillons. .i method for detecting anisyl alcohol in vanilla extracts is dc?scriheil. By this test the presence of 5 to 10 per ceut of Tahiti extract or extract of vanillotis in t,he more costly llourbon or Mexican extract cat1 be dct.ected. Mexican, South American. and J n r a ranilla extracts, iis wcll as 13oiirh01i extracts, *vi: negatiI:r tevts for a i k y l akottol by tliia metho& iif

A New Laboratory Mill'

extract

KIND0s BEAN Mericso Mexican Mexican MeXica*-

South American Java Bourbon tComoieri Bourbon (Reunion) Bourbon Reunion) Bourbon {Rexxt%ion>

Months 23 18 6 4 I 1 27 I8

10

1

Tonka Surinam

5

T o o k Angosturn Tahiti Tahiti Tahiti Tahiti Tahiti (contained 105%BIYE-

5

27 24 14

6 I

Detection of Anisyl Alcohol i n Vanilla Extract

It. was clearly shown that Tahiti berrns contain anisyl d c i i l i d and Bourbon beans do not,. This suggested a posribk method for distinguishing betweeti the extracts of the two kinds of beans, sincc the color react.iirn produrrd on itrisiitg a minute quantity of anisyl alcohol Tvith 2 to 3 cc. of i:onceiitrated sulfuric acid is VPI ' semitiye. The following test was foimd to give satisfaet,o rrsults when :ipi)Iiril to differeitt vanilla extracts: 1

Measure 50 cc. of the extract into an t.uapoiating dish anti evaporate spontaneously before a iarr to 8 volume pf about 15 C E . Transfer to a separatory funnel r\&h water, dilutmg to 50 cc. Extract once with 50 cc. of ether. Wash the ether extract thrce times with 15-cc. portions of 2 per mnt sotlimn hydroxide .solution and once with 15 cc. of water. Evaporate the ether cxtract before a fan,and as soon as the ethpr is driven offdissolve the residue in 0.5 ec. of alcohol. Add two to three drops of the alcohol solution to 2 to 3 cc. of concentrated sulfuric acid in a test tnbe and mix. In the case o i Tahiti vanilla extract a deep, prrmanent red color develops immediately.

This method was applied to a number of different extracts i u the lalioratorr from hmtrs of knovn oripin. These

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By S . W. Wiley \\:~LxY

& C o i i r ~ ~Iuu .r , . B I I . T I M O ~ L Sin .

W I L recently there has not beeu any mill on the mnrkct bith so wide a range of adaptation as the laborat,ory inill hiarewith illustrated. Four knives on a revolving ahaft work with a shearing action against six knives which are set in the frame of the mill. Since the screen is dovetailed into this frame, none of the material comes out of the grinding chamber itntil it is fine enough to pass through the mesh. The door tieing hinged, the mill is quickly and easily i.lraned. With-