NATURAL AND SYXTHETIC WAXES 12,5 Table II Instrument Parameters and Smnple Concentrations used for GLC Analysis Instrument Recorder Colmnn Carrier gas Air Hydrogen Detector temperature Injector temperature Sensitivity Temperature program Sample size Solution concentrations in chloroform Hydrocarbons Alcohols Methyl ester derivatives of the acids Perkin-Elmer CG Model 800 Leeds and Northrup (one mv) 18 in. X •/• in. O.D. copper, Apiezon I, 1.5% on 60/80 mesh Chromosorb C-•AW/DMCS Nitrogen at 105 ml/min 50 psig 26 psig 220-320øC 320øC lOO X Hydrocarbons, 180ø-290øC at 10øC/min Alcohols, 210ø-290øC at 7.5øC/min Acid-derivatives, 160ø-290øC at 10øC/min 1.0 •1 9.0 t•g/t•l 22.0 t•g/t•l 15.0 t•g/t•l Table III Per Cent of Fractions A-E (Table I) Found using Column Chromatography Waxes A B C D E Recovery, % _ Beeswax, natural 14.5 Candelilla wax 42.7 Wool wax (lanolin) 1.0 Adulterated beeswax +20% Paraffin wax 30.8 +20% Carnauba wax 11.1 +20% Wool wax 13.1 Synthetic wax Sample//la 21.5 Sample//2a 19.7 25 4 6 1 26 3 2O 7 29 3 26 4 21.2 15.5 22.0 13.4 5.3 22.4 16.5 12.7 44.9 14.4 11.0 20.3 10.4 14.1 21.8 15.3 18.1 24.2 11.6 90 8 93 0 99 3 93 2 91 6 93 4 13.2 47.6 82.3 22.0 22.0 85.8 Commercial sa•nples of "unknown" composition. Carnauba wax could not be eluted from the column at room tempera- ture. It would require heat to keep it in solution throughout the pro. cedure. However, it was found that carnauba wax when mixed with beeswax vent through the procedure at room temperature without dif- ficulty.
126 JOURNAL OF THE SOCIETY OF COSMETIC CHEMISTS Figlite •. ( as-liquid chromatogram of natural hydrocarbons from beeswax, Temperature [)togram: 180ø--290øC at 10øC/min on 1.5% Apiezon L, 60/80 mesh Chromosorb G AW I•MC . Sample injection of 1.0 /zl •_ 9.0 /xg Though several waxes were examined via GLC, essentially the frac- tions of beeswax and candelilla wax will be discussed to demonstrate the effective separation of the classes of constituents. The identification o1• the separated constituents was made by known retention time of pure standards and by the "spiking" of the samples with pure standards. The hydrocarbons of beeswax (Fig. 4) consist mainly of the odd carbon- ('hain n-hydrocarbons C2a-aa, with C•7 being predominant. Those of candelilla wax consist mainly of n-hydrocarbons C,2•-aa, with Caa being predominant. The beeswax alcohols (Fig. 5) are mainly of the even carbon-chain n-alcohols C24-a2 and the candelilla wax alcohols consist mainly of Ca0. The beeswax n-acids (Fig. 6) are of even carbon- chain consisting of C• a•, with C•o and C24 being predominant. The ('andelilla wax n-acids are also of even carbon chain, with Ca0 and Ca2 being predominant. The results of the above GLC analysis compare favorably with the work of other investigators (8). Though the combination of the three methods described above was used for a detailed study of waxes, it is preferable in certain instances to
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