An Introductory Course of Quantitative Chemical Analysis: With Explanatory NotesTalbot, Henry Paul
Science
An Introductory Course of Quantitative Chemical Analysis: With Explanatory Notes
Talbot, Henry Paul
Chemistry, Analytic -- Quantitative
PROCEDURE.--In order to secure a sample which shall represent the
average value of the ash, it is well to take at least 5 grams. As this
is too large a quantity for convenient titration, an aliquot portion
of the solution is measured off, representing one fifth of the entire
quantity. This is accomplished as follows: Weigh out on an analytical
balance two samples of soda ash of about 5 grams each into beakers
of about 500 cc. capacity. (The weighings need be made to centigrams
only.) Dissolve the ash in 75 cc. of water, warming gently, and filter
off the insoluble residue; wash the filter by filling it at least
three times with distilled water, and allowing it to drain, adding the
washings to the main filtrate. Cool the filtrate to approximately the
standard temperature of the laboratory, and transfer it to a 250 cc.
measuring flask, washing out the beaker thoroughly. Add distilled
water of laboratory temperature until the lowest point of the meniscus
is level with the graduation on the neck of the flask and remove any
drops of water that may be on the neck above the graduation by means
of a strip of filter paper; make the solution thoroughly uniform by
pouring it out into a dry beaker and back into the flask several
times. Measure off 50 cc. of the solution in a measuring flask, or
pipette, either of which before use should, unless they are dry on the
inside, be rinsed out with at least two small portions of the soda ash
solution to displace any water.
If a flask is used, fill it to the graduation with the soda ash
solution and remove any liquid from the neck above the graduation with
filter paper. Empty it into a beaker, and wash out the small flask,
unless it is graduated for !delivery!, using small quantities of
water, which are added to the liquid in the beaker. A second 50 cc.
portion from the main solution should be measured off into a second
beaker. Dilute the solutions in each beaker to 100 cc., add two drops
of a solution of methyl orange (Note 1) and titrate for the alkali
with the standard hydrochloric acid solution, using the alkali
solution to complete the titration as already prescribed.
From the volumes of acid and alkali employed, corrected for burette
errors and temperature changes, and the data derived from the
standardization, calculate the percentage of alkali present, assuming
it all to be present as sodium carbonate (Note 2).
[Note 1: The hydrochloric acid sets free carbonic acid which is
unstable and breaks down into water and carbon dioxide, most of which
escapes from the solution. Carbonic acid is a weak acid and, as such,
does not yield a sufficient concentration of H^{+} ions to cause the
indicator to change to a pink (see page 32).
The chemical changes involved may be summarized as follows:
2H^{+}, 2Cl^{-} + 2Na^{+}, CO_{3}^{--} --> 2Na^{+}, 2Cl^{-} +
[H_{2}CO_{3}] --> H_{2}O + CO_{2}]
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