Schmidt’s Test.—Add about 1 gram of sodium hydroxide to another part of the residue, and heat in an air-oven or oil bath, for half an hour at about 250° C., to convert the saccharin into salicylic acid. After it has cooled, acidify with sulfuric acid, extract and test for salicylic acid with 2 or 3 drops of ferric chlorid solution, letting the solutions come together slowly. A purple or violet coloration proves the presence of salicylic acid, which in turn indicates the presence of saccharin. This test cannot be used if salicylic acid was used as a preservative in the original product. A test for the acid should first be made.
Bornstein’s Test.—Heat the remainder of the above ether residue with resorcin and a very little sulfuric acid till it begins to swell. (It is best to do this heating in a test-tube.) Let cool till the action stops, heat again and repeat the operation several times. After cooling the last time, dilute with water and add sodium hydrate till neutral. If saccharin is present, there will be a red-green fluorescence.
Benzoic Acid
Acidify 50 cc. of the sample with sulfuric acid and shake vigorously with 50 cc. of a mixture of equal parts of ether and petroleum spirit. Let the liquids separate, then draw off as much as possible of the solvent and filter. (Use a centrifugal machine if an emulsion forms.) Separate the extract into 2 parts and evaporate each to dryness over a small flame and make the following tests:
Ferric Chlorid Test.—Dissolve one of these residues in ammonia, and evaporate to dryness on a water-bath. Take up the residue with warm water, filter, and collect the filtrate in a small test tube. Add a drop of ferric chlorid solution, and if benzoic acid is present a characteristic flesh or brownish colored precipitate of ferric benzoate forms. Sometimes in such products as sweet pickles, a basic ferric acetate precipitate comes down and the following test had better be applied.
Peter’s Method.—Take about 0.1 gram of the second part of the above ether residue, place in a large test tube (about 50 cc.) and dissolve in 5 to 8 cc. of concentrated sulfuric acid. Add from 0.5 to 0.8 gram of barium peroxide, a little at a time. Shake each time and cool in water if necessary. This should produce a permanent froth on the sulfuric acid. Let stand 25 or 30 minutes, then fill the tube three fourths full of water, shake and cool rapidly to the temperature of the room, and filter off the barium sulfate. Extract with chloroform or ether. Remove the extract and test it for salicylic acid with dilute ferric chlorid. (See first test under [salicylic acid].) In this method salicylic acid must first be proven absent.
Mohler’s Test.—Treat the remainder of the second part of the above ether residue with 2 or 3 cc. of concentrated sulfuric acid. Heat till white fumes appear. Add a few crystals of potassium nitrate and when cool dilute with water. Add an excess of ammonia, then a drop or two of ammonium sulfid. If a red color appears immediately on the surface, it shows the presence of benzoic acid.