PRESERVATIVES
It is best to make a systematic examination for the different preservatives. The sample may be prepared by mixing 50 grams of the pulped material with sufficient water in a 250 cc. graduated flask. Add phosphoric acid till distinctly acid in reaction. Fill to the mark with water. Place in a distilling flask, and distil in a linseed oil or a paraffin bath till 30 cc. have been collected. Save this distillate for the following tests.
Formaldehyde
To 5 cc. of the above distillate in a test tube, add 2 or 3 drops of a 1 per cent aqueous solution of phenol and mix well. Incline the tube and carefully pour down the side 5 cc. of concentrated commercial sulfuric acid so that the two liquids do not mix. If formaldehyde is present there will be a crimson zone at the plane of union of the solutions. This coloration takes place when the formaldehyde is present in the proportion of 1 part in 100,000 parts. When there is a greater quantity of formaldehyde present a white turbidity or a light-colored precipitate forms above the coloring.
Phenylhydrazine Hydrochloric Test.—Dissolve 2 grams of phenylhydrazine hydrochlorid and 3 grams of sodium acetate in 20 cc. of water. Add 2 to 4 drops of this reagent and the same number of drops of sulfuric acid to 1 or 2 cc. of the above distillate, to be examined in a test tube. A green coloration is produced when formaldehyde is present.
Hydrochloric Acid Test.—Add 5 cc. of the distillate to be tested to about 5 cc. of milk known to be pure, and about 10 cc. of concentrated hydrochloric acid (sp. gr. 1.2) which contains 1 cc. of a 10 per cent ferric chlorid solution to each 500 cc. of the acid. Heat slowly to 80° or 90° C. over the free flame, agitating it at the same time to break up the curd. A violet coloration indicates formaldehyde.
Sulfurous Acid and the Sulfites
Free sulfurous acid is not largely used as a food preservative, though its salts are quite commonly employed.
Detection.—Mix 150 grams of the finely ground sample with enough water to make a thin paste. Acidify with phosphoric acid and distil till 25 cc. have been collected. (The delivery tube of the condenser should dip below the surface of a little water.) Treat the distillate with a few drops of bromine water and boil for a short time. If a precipitate forms on the addition of barium chlorid the presence of sulfurous acid is indicated.
Salicylic 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. When the liquids have separated, draw off as much as possible of the solvent and filter. If an emulsion forms use a centrifugal machine, and evaporate with a small flame. If needle-shaped crystals form, salicylic acid is present. Add a few drops of water and a drop of very dilute ferric chlorid solution in such a way that the solutions will come together slowly. The presence of salicylic acid gives a purple or violet color.
Saccharin
This is used quite extensively as a sweetening agent in canned sweet corn, and other similar products.
Macerate about 20 grams of the sample after mixing with 30 to 40 cc. of water and strain through muslin. Acidify with 1 or 2 cc. of sulfuric acid (1 to 3) and extract with ether. (If an emulsion forms, use a centrifugal machine.) Separate the ether layer and let the ether evaporate spontaneously and use the residue in the following tests:
Take up a part of the residue with water and taste. If it is very sweet saccharin is present. Confirm by the following:
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.