98 JOURNAL OF THE SOCIETY OF COSMETIC CHEMISTS TABLE 5--CHROMATOGRAPHY OF BEESWAX UNSAPONIFIABLE MATTER Sample "a," Sample "b," Sample "c," Sample "d," Gm. Gm. Gm. Gm• Unsaponifiable matter 1. 696 1.688 1. 687 1. 705 Unsaponifiable matter insoluble in heptane and petroleum benzin (insoluble beeswax alcohols) 0. 987 1.014 0. 983 0. 928 Unsaponifiable matter soluble in heptane and petroleum benzin (by difference) 0. 709 O. 674 O. 704 O. 777 First petroleum benzln fraction* 0.427(13.6%) 0.423 (13.5%) 0.422(13.4%) 0.423 (13.3%) Second petroleum benzin fraction 0.001 0.000 0.000 0.000 First hot alcohol fraction 0. 276 0. 246 0. 275 0. 325 Second hot alcohol frac- tion 0.003 0.003 0. 003 0.021 * Av. 13.5%. Sample "a"--rate 5 ml. p.b./minute. Sample ?' --rate 4 ml. p.b./minute. Sample c' --rate 4 ml. p.b./minute. Sample "d"-:-rate 31/a mi. p.b./minute. TABI, V. 6---SOLUBILITY or BEv. swAx ALCOHOLS IN COLD MV. THYL ALCOHOL Beeswax Alcohols, Gm. Soluble Material, Expt. 1 Expt. 2 Av. Insoluble Material (by Difference) Av., Gm. 0.100 0.200 O. 300 0.400 0.500 0.026 0.028 0.027 0.073 0.040 0.039 0.040 0.160 0.046 ,0.044 0.045 0.255 0.054 0.054 0.054 0. 346 0.061 0.062 0.062 0.438 (12-14%) (2). The unsaponifiable material insoluble in heptane and petroleum benzin is also beeswax alcohols which are removed to de- crease the amount of material neces- sary to chromatograph. ' - T•. ANAL¾S•S or B•.•.SWAX- SPERMACET! ALCOHOL MIXTURES An empirical methoc• based on the solubility differences in cold methyl alcohol can be used to analyze mix- tures of the two alcohols. The pro- cedure is to treat a weighed sample with methyl alcohol, chill the solu- tion, and filter off the insoluble ma- terial. Evaporate the methyl alco- hol from the tiltrate and weigh the residue. Calculate the insoluble material, mostly beeswax alcohols, by difference. By use of Fig. 1, compute the weight'of soluble bees- wax alcohols associated with the insoluble beeswax alcohols. The sum Of the insoluble material and the soluble beeswax alcohols is ap- proximately equivalent to the total beeswax alcohols in the sample.

MIXTURES OF HYDROCARBONS, BEESWAX, AND SPERMACETI 99 Subtract the weight of the beeswax alcohols from the weight of sample taken the remainder is spermaceti alcohols. The results of a series of experiments employing this method are given in Table 7. All the results were in the range 100 •- 14%. It will be observed that the determinations of the major component of the mixture were ac- curate to •-5%. The minor com- ponent was determined with less accuracy. It will also be noted that with but one exception the re- coveries of spermaceti alcohol were somewhat low while those of the beeswax alcohols were high. In analyzing mixtdres of this type, it might be well to remember this and weigh the results accordingly. ANALYSI'S OF A MIXTURE OF HYDRO- CARBONS, BEESWAX, AND SPERM- ACETI Saponify and chromatograph the mixture of hydrocarbons, beeswax, and spermaceti according to the described experimental procedure. Combine the u.nsaponifiable alco- hols and treat a 0.5-gm. aliquot by the given solubility procedure. The data presented in Table 8 show the results obtained in a typical experi- ment by following procedure de- scribed. Estimation of Beeswax and Spermaceti The soluble alcohols (Table 8.) from a 0.5-gm. sample were foun'd to be 0.261 gm. The insoluble alcohols (by differ- ence) = 0.500 gm. - 0.261 gm. =. 0.239 gm.