MIXTURES OF HYDROCARBONS, Acidify the reservecf aqueous solu- tion with HC1, extract kith three 30-ml. portions of chloroform, and wash the combined chloroform ex- tracts with w:ater. Filter the washed chloroform extract through a cotton plug into a tared beaker, evaporate the chloroform on the steam bath, dry the residue in an oven at 100øC. for 15 minutes, cool and weigh as fatty acids. Repeat the heatting of the fatty acids until the weight is constant to 1-2 mg. Dissolve the unsaponifiable frac- tion in 50 ml. of boiling heptane and cool the solution to room tem- perature with stirring. Filter the resulting mixture through filter paper, wash the residue well with petroleum benzin, and reserve thee flitrate. Dissolve the residue on the filter paper by pouring hot chloroform through the filter, evap- orate the chloroform solution on the steam bath, dry the residt•e in an oven at 100øC. for 15 minutes, cool in a vacuum desic'cator, and weigh as unsaponifiable material insoluble in heptane and petroleum benzin. Re- peat the drying in the oven until the weight ik,constant to 1-2 mg. Evaporate the reserved petroleum benzin-heptane flitrate on the steam bath, take up the residue in 50 ml. of warm petroleum benzin (b.p. 30-75øC.), cool the solution to room temperature, transfer solution with the aid of 25 ml. petroleum benzin tO oa chromatograph tube contain- ing a 9 X a/4-in. activated A1203 column ("Alorco" grade F-20 mesh 80-200), and allow the solution to flow through the column at a rate BEESWAX, AND SPERMACETI 101 of 3.3 to 5 ml. per minute. Follow this solution with 175 ml. of petro- leum benzin, combine the flitrates, and label as first petroleum benzin fraction. Pass another 50 ml. of petroleum benzin through the •col- umn and label flitrate as second petroleum benzin fraction. Re- move the petroleum benzin by pass- ing 50 ml. of 95% alcohol, under air pressure, through the column. Follow this with 125 ml. of boiling alcohol which is also forced through the column at a rapid rate (4-7 minutes) with air pressure. Mark the combined two tiltrates as the first hot alcohol fraction. Pass an- other 50 ml. of boiling alcohol through the column and label as second hot alcohol fraction.* Evaporate the various fractions on the steam bath. Dry the tWO petroleum benzin fractions in an oven at 100øC. for 15 minutes, cool in a vacuum desiccator, and weigh. Repeat drying in oven until weight is constant to 1-2 rag. Redissolve each of the hot alcohol fractions in 10 ml. of chloroform, evaporate chloroform on steam bath, and dry and weigh residues in the manner described for the petroleum benzin fractions. Solubility Procedure. Weigh sam- ple into a 150-ml. beaker, add 80 ml. methyl alcohol, cover beaker with watch glass, and heat on hot plate until solution' is complete. Transfer beaker to ice bath and stir solution vigorously wi{h thermom- * The second fraction obtained in each case above should contain negligible amounts of non-/'olatile material.
102 JOURNAL OF THE SOCIETY OF COSMETIC CHEMISTS eter until the temperature is 5øC. Pour resulting mixture through a Bficllner funnel containing a 11-cm. No. 595 S&S filter paper turned up with a I/2-in. edge, and wetted with methanol. Filter by gravity or gentle suction. Do not allow the material on the filter to dry or cake. Wash residue with 20 ml. of ice- chilled methanol and draih dry with strong suction. Transfer the til- trate to a tared beaker with the aid of chloroform, evaporate to dryness on the steam bath, heat in an oven at 100øC. for 10 minutes, cool in'a vacuum desiccator, and weigh. Re- peat drying in oven until weight is constant to 1-2 mg. SUMMARY Studies have been made on a new analytical method for the analysis of mixtures of hydrocarbons , bees- wax, and spermaceti. Chroma- tography plays an important role in the procedure. It is believed that the outlined chromatographic pro- cedure can be used to detect adulter- ants particularly, hydrocarbons in beeswar and spermaceti. Work in this field is contemplated. BIBLIOGRAPHY 1. Williams, K. A., zlnalyst, 71, 259 (1946). 2. Fryer, P. J., and Weaton, F. E., "Tech- nical Handbook of Oils, Fats and Waxes," Vol. 1, page 1'86, Cambridge University Press (.1920).
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