GRADUATION OF FLASKS

It is a general custom to purchase the flasks ungraduated and to graduate them for use under standard conditions selected for the laboratory in question.  They may be graduated for “contents” or “delivery.”  When graduated for “contents” they contain a specified volume when filled to the graduation at a specified temperature, and require to be washed out in order to remove all of the solution from the flask.  Flasks graduated for “delivery” will deliver the specified volume of a liquid without rinsing.  A flask may, of course, be graduated for both contents and delivery by placing two graduation marks upon it.

Procedure.—­To calibrate a flask for !contents!, proceed as follows:  Clean the flask, using a chromic acid solution, and dry it carefully outside and inside.  Tare it accurately; pour water into the flask until the weight of the latter counterbalances weights on the opposite pan which equal in grams the number of cubic centimeters of water which the flask is to contain.  Remove any excess of water with the aid of filter paper (Note 1).  Take the flask from the balance, stopper it, place it in a bath at the desired temperature, usually 15.5 deg. or 17.5 deg.C., and after an hour mark on the neck with a diamond the location of the lowest point of the meniscus (Note 2).  The mark may be etched upon the flask by hydrofluoric acid, or by the use of an etching ink now commonly sold on the market.

To graduate a flask which is designed to !deliver! a specified volume, proceed as follows:  Clean the flask as usual and wipe all moisture from the outside.  Fill it with distilled water.  Pour out the water and allow the water to drain from the flask for three minutes.  Counterbalance the flask with weights to the nearest centigram.  Add weights corresponding in grams to the volume desired, and add distilled water to counterbalance these weights.  An excess of water, or water adhering to the neck of the flask, may be removed by means of a strip of clean filter paper.  Stopper the flask, place it in a bath at 15.5 deg.C. or 17.5 deg.C. and, after an hour, mark the location of the lowest point of the meniscus, as described above.

[Note 1:  The allowable error in counterbalancing the water and weights varies with the volume of the flask.  It should not exceed one ten-thousandth of the weight of water.]

[Note 2:  Other methods are employed which involve the use of calibrated apparatus from which the desired volume of water may be run into the dry flask and the position of the meniscus marked directly upon it.  For a description of a procedure which is most convenient when many flasks are to be calibrated, the student is referred to the !Am.  Chem J.!, 16, 479.]

GENERAL DIRECTIONS FOR VOLUMETRIC ANALYSES

It cannot be too strongly emphasized that for the success of analyses uniformity of practice must prevail throughout all volumetric work with respect to those factors which can influence the accuracy of the measurement of liquids.  For example, whatever conditions are imposed during the calibration of a burette, pipette, or flask (notably the time allowed for draining), must also prevail whenever the flask or burette is used.