FILTRATION AND WASHING OF PRECIPITATES
Solutions should be filtered while hot, as far as possible, since the passage of a liquid through the pores of a filter is retarded by friction, and this, for water at 100°C., is less than one sixth of the resistance at 0°C.
When the filtrate is received in a beaker, the stem of the funnel should touch the side of the receiving vessel to avoid loss by spattering. Neglect of this precaution is a frequent source of error.
The vessels which contain the initial filtrate should !always! be replaced by clean ones, properly labeled, before the washing of a precipitate begins. In many instances a finely divided precipitate which shows no tendency to pass through the filter at first, while the solution is relatively dense, appears at once in the washings. Under such conditions the advantages accruing from the removal of the first filtrate are obvious, both as regards the diminished volume requiring refiltration, and also the smaller number of washings subsequently required.
Much time may often be saved by washing precipitates by decantation, i.e., by pouring over them, while still in the original vessel, considerable volumes of wash-water and allowing them to settle. The supernatant, clear wash-water is then decanted through the filter, so far as practicable without disturbing the precipitate, and a new portion of wash-water is added. This procedure can be employed to special advantage with gelatinous precipitates, which fill up the pores of the filter paper. As the medium from which the precipitate is to settle becomes less dense it subsides less readily, and it ultimately becomes necessary to transfer it to the filter and complete the washing there.
A precipitate should never completely fill a filter. The wash-water should be applied at the top of the filter, above the precipitate. It may be shown mathematically that the washing is most !rapidly! accomplished by filling the filter well to the top with wash-water each time, and allowing it to drain completely after each addition; but that when a precipitate is to be washed with the !least possible volume! of liquid the latter should be applied in repeated !small! quantities.
Gelatinous precipitates should not be allowed to dry before complete removal of foreign matter is effected. They are likely to shrink and crack, and subsequent additions of wash-water pass through these channels only.
All filtrates and wash-waters without exception must be properly tested. !This lies at the foundation of accurate work!, and the student should clearly understand that it is only by the invariable application of this rule that assurance of ultimate reliability can be secured. Every original filtrate must be tested to prove complete precipitation of the compound to be separated, and the wash-waters must also be tested to assure complete removal of foreign material. In testing the latter, the amount first taken should be but a few drops if the filtrate contains material which is to be subsequently determined. When, however, the washing of the filter and precipitate is nearly completed the amount should be increased, and for the final test not less than 3 cc. should be used.
It is impossible to trust to one's judgment with regard to the washing of precipitates; the washings from !each precipitate! of a series simultaneously treated must be tested, since the rate of washing will often differ materially under apparently similar conditions, !No exception can ever be made to this rule!.
The habit of placing a clean common filter paper under the receiving beaker during filtration is one to be commended. On this paper a record of the number of washings can very well be made as the portions of wash-water are added.
It is an excellent practice, when possible, to retain filtrates and precipitates until the completion of an analysis, in order that, in case of question, they may be examined to discover sources of error.
For the complete removal of precipitates from containing vessels, it is often necessary to rub the sides of these vessels to loosen the adhering particles. This can best be done by slipping over the end of a stirring rod a soft rubber device sometimes called a "policeman."