The melting point of genuine vanillin is a characteristic indication. Admixtures of vanillic acid and antifebrin cause depression of the melting point (4-8 ° C. according to the amount and character of the two substances [Welmans])[155]. For the quantitative determination of vanillin in mixtures, Welmans takes advantage of its behaviour towards caustic alkalis, with which, like phenol, it forms compounds that are easily soluble in water, but sparingly so in alcohol. The process is as follows: 1 gramme of the substance is placed in a cylinder of 200 ccm capacity with 25 ccm of alcohol, 25 ccm of approximately semi-normal alcoholic potash and 2 or 3 drops of phenolphthalein solution and agitated until completely dissolved. The excess of alkali is then titrated with semi-normal hydrochloric acid, and, at the same time, the strength of the alcoholic potash after adding 25 ccm of alcohol is ascertained. The number of cubic centimetres consumed is multiplied by 0·076, the semifactor for vanillin. In the case of vanilla sugar, 10 grammes are treated with 50 ccm of water to dissolve the sugar, then the alcoholic potash is added and the operation carried out as before described.
1 gramme of vanillin requires 6: 58 ccm of normal potash (= 0·36842 g KOH).
| C6H3(OH) | ∕ OCH3 | : KOH |
| ∖CHO | ||
| 152 | : 56 = 1 : x |
If cumarin is suspected to have been added to the vanillin it can be detected and separated, according to Zipperer’s experiments, by the method of W. H. Hess and A. B. Prescott.[156]
The substance is dissolved in ether and the solution shaken up with a weak solution of ammonia. The vanillin will be found in the aqueous layer in the form of an ammonium compound, whilst the cumarin will be dissolved by the ether. The vanillin can be identified by the sandal-wood oil reaction as described by Bonnema,[157] and the cumarin can be determined by direct weighing.
The financial advantage in using vanillin in place of vanilla is apparent. The average price of vanilla is now 45 to 50 shillings per kilo. But as 25 grammes of vanillin are equal in perfume to 1 kilo of vanilla and, at the rate of 35 shillings per kilo, that quantity costs only 10½ vanilla is nearly sixty times dearer than vanillin. The consumption of vanillin has increased to an enormous extent, and in the United States Henning has estimated the consumption during 1897-1898 at over 100000 ounces. The same author points out the remarkable fact that this enormous consumption of vanillin has scarcely any effect on the demand for vanilla pods, the market value of which is not only maintained but has a tendency to increase.
In order to have it in a finely divided condition, as required for the factory, it is recommended to rub the vanillin down with sugar, in the proportion of 100 grammes of vanillin to 2 kilos of sugar, in the following manner; 100 grammes of vanillin are dissolved in 500 grammes of hot alcohol and this solution added to 2 kilos of finely powdered sugar; then the whole is placed in a rotatory comfit boiler and dried by a blast of warm air at 40 ° C. Whilst vanilla must be very carefully packed that it may not become mildewed and deteriorate, vanillin on the other hand keeps very well in such mixtures so long as they are kept from damp, which might cause the sugar to ferment and thus gradually decompose the vanillin.
d) Cinnamon.
There are three commercial kinds of cinnamon in Europe.
1. Ceylon cinnamon, which represents the finest kind, is the bark of Cinnamomum ceylanicum, a native of the island of Ceylon. The bark is very light and brittle, seldom more than 0·5 mm thick, externally yellowish brown with long stripes, whilst it is somewhat darker on the inside. Its fracture is short and fibrous, and a traverse section shows externally a sharply defined light colour with a darker inside zone.