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.
In all precipitations the reagent should be added slowly, with constant stirring, and should be hot when circumstances permit. The slow addition is less likely to occasion contamination of the precipitate by the inclosure of other substances which may be in the solution, or of the reagent itself.
FUNNELS AND FILTERS
Filtration in analytical processes is most commonly effected through paper filters. In special cases these may be advantageously replaced by an asbestos filter in a perforated porcelain or platinum crucible, commonly known, from its originator, as a "Gooch filter." The operation and use of a filter of this type is described on page 103. Porous crucibles of a material known as alundum may also be employed to advantage in special cases.
The glass funnels selected for use with paper filters should have an angle as near 60° as possible, and a narrow stem about six inches in length. The filters employed should be washed filters, i.e., those which have been treated with hydrochloric and hydrofluoric acids, and which on incineration leave a very small and definitely known weight of ash, generally about .00003 gram. Such filters are readily obtainable on the market.