The committee realizes that in the case of all methods for determining moisture by means of loss on heating there may be a loss due to volatile matter (especially fatty acids) other than water. The title of the determination moisture and volatile matter indicates this idea, but any considerable error from this source may occur only in the case of high acid fats and oils and particularly those containing lower fatty acids such as coconut and palm kernel oil. In the case of extracted greases which have not been properly purified, some of the solvent may also be included in the moisture and volatile matter determination, but inasmuch as the solvent, usually a petroleum product, can only be considered as foreign matter, for commercial purposes, it is entirely proper to include it with the moisture.
The committee has also considered the various distillation methods for the determination of moisture in fats and oils, but since according to the fundamental principles which it was endeavoring to follow it could only standardize one method, it was decided that the most desirable one on the whole was the vacuum-oven method as given. There are cases wherein a chemist may find it desirable to check a moisture determination or investigate the moisture content of a fat or oil further by means of one of the distillation methods.
However, in co-operative work the distillation method in various types of apparatus has not yielded satisfactory results. The difficulties appear to be connected with a proper choice of solvent and particularly with the tendency of drops of water to adhere to various parts of the glass apparatus instead of passing on to the measuring device. When working on coconut oil containing a high percentage of free fatty acids, concordant results could not be obtained by the various members of the committee when working with identical samples, solvents and apparatus.
On the other hand, the committee found by individual work, co-operative work and collaborative work by several members of the committee in one laboratory, that the old, well-known direct heating method (which the committee has designated the hot plate method) yielded very satisfactory results on all sorts of fats and oils including emulsions such as butter and oleomargarine and even on coconut oil samples containing 15 to 20 per cent free fatty acids and 5 to 6 per cent of moisture. Unfortunately, this method depends altogether on the operator's skill and while the method may be taught to any person whether a chemist or not so that he can obtain excellent results with it, it is difficult to give a sufficiently, complete description of it so that any chemist anywhere after reading the description could follow it successfully. The method is undoubtedly worthy of much confidence in careful hands. It is quick, accurate and reliable. It is probably the best single method for the determination of moisture in all sorts of samples for routine laboratory work. On account of this fact the committee desires to announce its willingness to instruct any person in the proper use of the method who desires to become acquainted with it and who will visit any committee member's laboratory.
INSOLUBLE IMPURITIES.
This determination, the title for which was adopted after careful consideration, determines the impurities which have generally been known as dirt, suspended matter, suspended solids, foreign solids, foreign matter, etc., in the past. The first solvent recommended by the committee is hot kerosene to be followed by petroleum ether kept at ordinary room temperature. Petroleum ether, cold or only slightly warm, is not a good fat and metallic soap solvent, whereas hot kerosene dissolves these substances readily, and for this reason the committee has recommended the double solvent method so as to exclude metallic soaps which are determined below as soluble mineral matter.
SOLUBLE MINERAL MATTER.
Soluble mineral matter represents mineral matter combined with fatty acids in the form of soaps in solution in the fat or oil. Formerly, this mineral matter was often determined in combination by weighing the separated metallic soap or by weighing it in conjunction with the insoluble impurities. Since the soaps present consist mostly of lime soap, it has been customary to calculate the lime present therein by taking 0.1 the weight of the total metallic soaps. The standard method as given above is direct and involves no calculation. The routine method given in the note has been placed among the methods for the reason that it is used in some laboratories, but has not been adopted as a standard method in view of the fact that the committee has made it a rule to adopt only one standard method. It should be pointed out, however, that the method cannot be considered accurate for the reason that insoluble impurities may vary from sample to sample to a considerable extent and the error due to the presence of large particles of insoluble impurities is thus transferred to the soluble mineral matter. The committee has found one type of grease (naphtha bone grease) which shows most unusual characteristics. The type sample contains 4.3 per cent soluble mineral matter by the committee method which would be equivalent to 43.0 per cent free fatty acid. The kerosene and gasoline filtrate was particularly clear, nevertheless the ash was found to contain 36.43 per cent P2O5 equivalent to 79.60 per cent of Ca3(PO4)2 and 9.63 per cent of Fe2O3. The method, therefore, determines the soluble mineral matter in this case satisfactorily but the factor 10 is not applicable for calculating the fatty acids combined therewith. It is necessary, therefore, in order to determine the fatty acids combined with soluble mineral matter in the original sample to determine the actual bases in the soluble mineral matter as obtained by ashing the kerosene and gasoline filtrate. To the bases so determined the factor 10 can then be applied.
FREE FATTY ACID.
The fatty acid method adopted is sufficiently accurate for commercial purposes. In many routine laboratories the fat or oil is measured and not weighed, but the committee recommends weighing the sample in all cases. For scientific purposes the result is often expressed as "acid number," meaning the number of milligrams of KOH required to neutralize the free acids in one gram of fat, but the commercial practice has been, and is, to express the fatty acids as oleic acid or in the case of palm oil, as palmitic acid, in some instances. The committee sees no objection to the continuation of this custom so long as the analytical report clearly indicates how the free acid is expressed. For a more exact expression of the free acid in a given fat, the committee recommends that the ratio of acid number to saponification number be used. This method of expressing results is subject to error when unsaponifiable fatty matter is present, since the result expresses the ratio of free fatty acid to total saponifiable fatty matter present.