An Introductory Course of Quantitative Chemical Analysis | Page 9

cubic centimeter.
[Note 1: The ends of the colored paper used as an aid to accurate readings may be fastened together by means of a gummed label. The paper may then remain on the burette and be ready for immediate use by sliding it up or down, as required.]
[Note 2: To obtain an accurate reading the eye must be very nearly on a level with the meniscus. This is secured by the use of the paper as described. The student should observe by trial how a reading is affected when the meniscus is viewed from above or below.
The eye soon becomes accustomed to estimating the tenths of the divisions. If the paper is held as directed, two divisions below the meniscus, one whole division is visible to correct the judgment. It is not well to attempt to bring the meniscus exactly to a division mark on the burette. Such readings are usually less accurate than those in which the tenths of a division are estimated.]
CALIBRATION OF GLASS MEASURING DEVICES
If accuracy of results is to be attained, the correctness of all measuring instruments must be tested. None of the apparatus offered for sale can be implicitly relied upon except those more expensive instruments which are accompanied by a certificate from the !National Bureau of Standards! at Washington, or other equally authentic source.
The bore of burettes is subject to accidental variations, and since the graduations are applied by machine without regard to such variations of bore, local errors result.
The process of testing these instruments is called !calibration!. It is usually accomplished by comparing the actual weight of water contained in the instrument with its apparent volume.
There is, unfortunately, no uniform standard of volume which has been adopted for general use in all laboratories. It has been variously proposed to consider the volume of 1000 grams of water at 4��, 15.5��, 16��, 17.5��, and even 20��C., as a liter for practical purposes, and to consider the cubic centimeter to be one one-thousandth of that volume. The true liter is the volume of 1000 grams of water at 4��C.; but this is obviously a lower temperature than that commonly found in laboratories, and involves the constant use of corrections if taken as a laboratory standard. Many laboratories use 15.5��C. (60�� F.) as the working standard. It is plain that any temperature which is deemed most convenient might be chosen for a particular laboratory, but it cannot be too strongly emphasized that all measuring instruments, including burettes, pipettes, and flasks, should be calibrated at that temperature in order that the contents of each burette, pipette, etc., shall be comparable with that of every other instrument, thus permitting general interchange and substitution. For example, it is obvious that if it is desired to remove exactly 50 cc. from a solution which has been diluted to 500 cc. in a graduated flask, the 50 cc. flask or pipette used to remove the fractional portion must give a correct reading at the same temperature as the 500 cc. flask. Similarly, a burette used for the titration of the 50 cc. of solution removed should be calibrated under the same conditions as the measuring flasks or pipettes employed with it.
The student should also keep constantly in mind the fact that all volumetric operations, to be exact, should be carried out as nearly at a constant temperature as is practicable. The spot selected for such work should therefore be subject to a minimum of temperature variations, and should have as nearly the average temperature of the laboratory as is possible. In all work, whether of calibration, standardization, or analysis, the temperature of the liquids employed must be taken into account, and if the temperature of these liquids varies more than 3�� or 4�� from the standard temperature chosen for the laboratory, corrections must be applied for errors due to expansion or contraction, since volumes of a liquid measured at different times are comparable only under like conditions as to temperature. Data to be used for this purpose are given in the Appendix. Neglect of this correction is frequently an avoidable source of error and annoyance in otherwise excellent work. The temperature of all solutions at the time of standardization should be recorded to facilitate the application of temperature corrections, if such are necessary at any later time.
CALIBRATION OF THE BURETTES
Two burettes, one at least of which should have a glass stopper, are required throughout the volumetric work. Both burettes should be calibrated by the student to whom they are assigned.
PROCEDURE.--Weigh a 50 cc., flat-bottomed flask (preferably a light-weight flask), which must be dry on the outside, to the nearest centigram. Record the weight in the notebook. (See Appendix for suggestions as to records.) Place the flask under the burette and draw out into it about 10 cc. of water, removing any