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}]
[Note 2: A determination of the alkali present as hydroxide in soda ash may be determined by precipitating the carbonate by the addition of barium chloride, removing the barium carbonate by filtration, and titrating the alkali in the filtrate.