Standard Vacuum Oven
The vacuum-oven method cannot be considered accurate in the case of fats of the coconut oil group containing free acid and the Committee recommends that it be used only for oils of this group when they contain less than 1 per cent free acid. In the case of oils of this group containing more than 1 per cent free acid, recourse should be had temporarily to the routine control method for moisture and volatile matter[27] until the Committee develops a more satisfactory method.
The air-oven method cannot be considered even approximately accurate in the case of the drying and semi-drying oils and those of the coconut oil group. Therefore, in the case of such oils as cottonseed oil, maize oil (corn oil), soy bean oil, linseed oil, coconut oil, palm kernel oil, etc., the vacuum-oven method should always be used, except in the case of fats of the coconut group containing more than 1 per cent free acid, as noted above.
INSOLUBLE IMPURITIES.
Dissolve the residue from the moisture and volatile matter determination by heating it on a steam bath with 50 cc. of kerosene. Filter the solution through a Gooch crucible properly prepared with asbestos,[28] wash the insoluble matter five times with 10-cc. portions of hot kerosene, and finally wash the residual kerosene out thoroughly with petroleum ether. Dry the crucible and contents to constant weight, as in the determination of moisture and volatile matter and report results as insoluble impurities.
SOLUBLE MINERAL MATTER.
Place the combined kerosene filtrate and kerosene washings from the insoluble impurities determination in a platinum dish. Place in this an ashless filter paper folded in the form of a cone, apex up. Light the apex of the cone, whereupon the bulk of the kerosene burns quietly. Ash the residue in a muffle, to constant weight, taking care that the decomposition of alkaline earth carbonates is complete, and report the result as soluble mineral matter.[29] When the percentage of soluble mineral matter amounts to more than 0.1 per cent, multiply the percentage by 10 and add this amount to the percentage of free fatty acids as determined.[30]
FREE FATTY ACIDS.
The alcohol[31] used shall be approximately 95 per cent ethyl alcohol, freshly distilled from sodium hydroxide, which with phenolphthalein gives a definite and distinct end-point.