.4886
----- × 100 = 96.73% KOH in sample.
.505
Caustic potash often contains some caustic soda, and while it is possible to express the results in terms of KOH, regardless of any trouble that may be caused by this mixture in soap making, an error is introduced in the results, not all the alkali being caustic potash. In such cases it is advisable to consult a book on analysis as the analysis is far more complicated than those given we will not consider it. The presence of carbonates, as already stated, also causes an error. To overcome this the alkali is titrated in absolute alcohol, filtering off the insoluble carbonate. The soluble portion is caustic hydrate and may be titrated as such. The carbonate remaining on the filter paper is dissolved in water and titrated as carbonate.
SOAP ANALYSIS.
To obtain a sample of a cake of soap for analysis is a rather difficult matter as the moisture content of the outer and inner layer varies considerably. To overcome this difficulty a borer or sampler may be run right through the cake of soap, or slices may be cut from various parts of the cake, or the cake may be cut and run through a meat chopper several times and mixed. A sufficient amount of a homogeneous sample obtained by any of these methods is preserved for the entire analysis by keeping the soap in a securely stoppered bottle.
The more important determinations of soap are moisture, free alkali, or fatty acid, combined alkali and total fatty matter. Besides these it is often necessary to determine insoluble matter, glycerine, unsaponifiable matter, rosin and sugar.
MOISTURE.
The analysis of soap for moisture, at its best, is most unsatisfactory, for by heating it is impossible to drive off all the water, and on the other hand volatile oils driven off by heat are a part of the loss represented as moisture.
The usual method of determining moisture is to weigh 2 to 3 grams of finely shaved soap on a watch glass and heat in an oven at 105 degrees C. for 2 to 3 hours. The loss in weight is represented as water, although it is really impossible to drive off all the water in this way.
To overcome the difficulties just mentioned either the Smith or Fahrion method may be used. Allen recommends Smith's method which is said to be truthful to within 0.25 per cent. Fahrion's method, according to the author, gives reliable results to within 0.5 per cent. Both are more rapid than the above manipulation. To carry out the method of Smith, 5 to 10 grams of finely ground soap are heated over a sand bath with a small Bunsen flame beneath it, in a large porcelain crucible. The heating takes 20 to 30 minutes, or until no further evidence is present of water being driven off. This may be tested by the fogging of a cold piece of glass held over the crucible immediately upon removing the burner. When no fog appears the soap is considered dry. Any lumps of soap may be broken up by a small glass rod, weighed with the crucible, and with a roughened end to more easily separate the lumps. Should the soap burn, this can readily be detected by the odor, which, of course, renders the analysis useless. The loss in weight is moisture.
By Fahrion's method[13], 2 to 4 grams of soap are weighed in a platinum crucible and about three times its weight of oleic acid, which has been heated at 120 degrees C. until all the water is driven off and preserved from moisture, is added and reweighed. The dish is then cautiously heated with a small flame until all the water is driven off and all the soap is dissolved. Care must be exercised not to heat too highly or the oleic acid will decompose. The moment the water is all driven off a clear solution is formed, provided no fillers are present in the soap. The dish is then cooled in a dessicator and reweighed. The loss in weight of acid plus soap is moisture and is calculated on the weight of soap taken. This determination takes about fifteen minutes.