PART III

GRAVIMETRIC ANALYSIS

GENERAL DIRECTIONS

Gravimetric analyses involve the following principal steps:  first, the weighing of the sample; second, the solution of the sample; third, the separation of some substance from solution containing, or bearing a definite relation to, the constituent to be measured, under conditions which render this separation as complete as possible; and finally, the segregation of that substance, commonly by filtration, and the determination of its weight, or that of some stable product formed from it on ignition.  For example, the gravimetric determination of aluminium is accomplished by solution of the sample, by precipitation in the form of hydroxide, collection of the hydroxide upon a filter, complete removal by washing of all foreign soluble matter, and the burning of the filter and ignition of the precipitate to aluminium oxide, in which condition it is weighed.

Among the operations which are common to nearly all gravimetric analyses are precipitation, washing of precipitates, ignition of precipitates, and the use of desiccators.  In order to avoid burdensome repetitions in the descriptions of the various gravimetric procedures which follow, certain general instructions are introduced at this point.  These instructions must, therefore, be considered to be as much a part of all subsequent procedures as the description of apparatus, reagents, or manipulations.

The analytical balance, the fundamentally important instrument in gravimetric analysis, has already been described on pages 11 to 15.

PRECIPITATION

For successful quantitative precipitations those substances are selected which are least soluble under conditions which can be easily established, and which separate from solution in such a state that they can be filtered readily and washed free from admixed material.  In general, the substances selected are the same as those already familiar to the student of Qualitative Analysis.

When possible, substances are selected which separate in crystalline form, since such substances are less likely to clog the pores of filter paper and can be most quickly washed.  In order to increase the size of the crystals, which further promotes filtration and washing, it is often desirable to allow a precipitate to remain for some time in contact with the solution from which it has separated.  The solution is often kept warm during this period of “digestion.”  The small crystals gradually disappear and the larger crystals increase in size, probably as the result of the force known as surface tension, which tends to reduce the surface of a given mass of material to a minimum, combined with a very slightly greater solubility of small crystals as compared with the larger ones.

Amorphous substances, such as ferric hydroxide, aluminium hydroxide, or silicic acid, separate in a gelatinous form and are relatively difficult to filter and wash.  Substances of this class also exhibit a tendency to form, with pure water, what are known as colloidal solutions.  To prevent this as far as possible, they are washed with solutions of volatile salts, as will be described in some of the following procedures.