Alkali
Shake a portion of the sample with twice its volume of water. If no precipitate forms, an alkali is present. A flocculent reddish-brown precipitate shows no alkali is present. If the solution is milky it indicates the presence of a foreign resin.
Add hydrochloric acid drop by drop to the diluted extract. Nothing more than a mere turbidity should result. Should it be quite turbid and the color fading after a time, it shows that an alkali has been used.
Foreign Resins
Mix a portion of the extract slowly with twice its volume of water, frequently shaking the mixture. When this solution is milky, it indicates a foreign resin.
Hess’ Test.—Dealcoholize 25 cc. of the sample by concentrating on the water-bath, adding water from time to time to retain the original volume. When no alkali is present in the extract, pure vanilla resin will be thrown down as a reddish-brown flocculent precipitate. Collect the resin, whatever its color, on a filter, and wash. Save the filtrate to test for caramel. Place a piece of the paper and resin in a dilute solution of potassium hydroxid. If the resin is that of pure vanilla it will dissolve, giving a deep-red color, and is reprecipitated when the alkali is neutralized with hydrochloric acid. Dissolve another part of the precipitate in alcohol, and to a part of this solution add a few drops of ferric chlorid; and to the other part, hydrochloric acid. There should be no marked coloration in either case if the resin is that of pure vanilla. Foreign resins nearly always produce a coloration.
CARAMEL
Shake the bottle of vanilla, and if the bubbles, which form, are a bright caramel color, keeping the color till all are gone, the presence of caramel is indicated.
Concentrate a portion of the filtrate, which was saved in making the test for foreign resins, at a rather low temperature until it has about the same color as the original extract. Add a few drops of strong hydrochloric acid and heat very gently. If caramel is present, a yellowish-red flocculent precipitate will form. After the liquid cools, filter and wash with water. Should this precipitate contain caramel, it will not dissolve in water, ether, and alcohol, but will dissolve in sodium hydroxid, dilute alcohol, and glacial acetic acid.