QUANTITATIVE DETERMINATION OF SODA ASH COMPOSITION BY

DOUBLE INDICATOR TITRATION

ANSWERS TO QUESTIONS

1. What are the possible components of a soda ash sample. Why is it that some of the
components never co-exist together? What is the practical importance of analysis of
soda ash samples?
Soda ash is the trade name or common name for crude sodium bicarbonate (NaHCO3). Soda
ash is an impure solution that may also contain trace amounts of sodium carbonate (Na2CO3),
sodium hydroxide (NaOH). It is frequently used as a commercial neutralizing agent, and can
also be used as processing aids and additives (PubChem, 2019).
Sodium bicarbonate, NaHCO3, is a monoprotic acid and has amphoprotic properties meaning
it can act as both an acid and base, but not at the same time. The neutralization of carbonate
ion proceeds in two separate steps:
𝐶𝑂32− + 𝐻3 𝑂+ ↔ 𝐻𝐶𝑂3− + 𝐻2 𝑂 𝐾𝑏1 = 2.1𝑥104
𝐻𝐶𝑂3− + 𝐻3 𝑂+ ↔ 𝐻2 𝐶𝑂3− + 𝐻2 𝑂 𝐾𝑏2 = 2.4𝑥10−8
It is a two component system wherein the second component is a product of the first reaction.
The first component is the carbonate ion, 𝐶𝑂32− and the second is the bicarbonate ion, 𝐻𝐶𝑂3− .

2. What are the advantages of the double indicator method? When is it applicable?
Volumetric or titrimetric analysis involve the reaction of a standard solution of known
amounts with an unknown solution or analyte to determine the stoichiometric or equivalence
point. Since there are several kinds of acids and bases, there are also corresponding methods of
titration for each system. Simple system, usually involving monoprotic acids or base, make use
of the simple titration method. On the other hand, for complex system involving solutions of
amphiprotic and/or polyprotic acids or bases, the double titration method is used. Since
complex system involve two or more acidic or basic species, the ionization of polyprotic acids
occur stepwise, with each step having a different ionization constant expression. For such
systems, double indicator method is more advantageous since it could assess the different
endpoints for each ionization/neutralization step with different indicators.

3. What species are being neutralized under phenolphthalein and methyl orange
indicator.
The neutralization of soda ash occurs in two-steps:
𝐶𝑂32− + 𝐻3 𝑂+ ↔ 𝐻𝐶𝑂3− + 𝐻2 𝑂 (1)
𝐻𝐶𝑂3− + 𝐻3 𝑂+ ↔ 𝐻2 𝐶𝑂3− + 𝐻2 𝑂 (2)
The pH for the first step equivalence point (1) occurs at a pH of ~8.0, hence a suitable and
commonly used indicator is phenolphthalein. While the second equivalence point (2) occurs at
a pH ~ 4.0, where methyl orange is most commonly used. This is because the neutralized
species for each indicator: the carbonate ion, 𝐶𝑂32− and the bicarbonate ion, 𝐻𝐶𝑂3− under
phenolphthalein and methyl orange respectively, corresponds to the pH ranges of the
corresponding indicator.
The complete equation for this reaction is as follows:
𝑁𝑎2 𝐶𝑂3 + 2 𝐻𝐶𝑙 ↔ 𝐶𝑂2 + 𝐻2 𝑂 + 2 𝑁𝑎𝐶𝑙

4. Why is it necessary that boiled distilled water be used in the preparation of standard
and sample solutions?
Distilled water is the purest form and most inert type of water in the sense that all of the
dissolved substances mixed in water have been removed by evaporation. Boiling distilled water
 further purifies the water by removing the dissolved gases such as carbon dioxide, CO2. This is
done because the CO2 in water may react with the base components of the soda ash forming
products such as carbonic acid, H2CO3 which could lead to erroneous or faulty data.

5. What are the basic components of the unknown soda ash sample based on the volume
relationship at the phenolphthalein and methyl orange endpoints?
The soda ash sample is assumed to contain compounds of sodium bicarbonate (NAHCO3) and
sodium carbonate (NA2CO3) and other impurities.
Assuming a stoichiometric ratio of 1 : 1, from the equation (2), the number of mole of HCl
determined from the methyl orange titration is equal to the number of mole of NaHCO3(aq).
Likewise, total number of moles of NaOH(aq) and Na2CO3(aq) in the solution mixture can be
calculated according to the volumes of HCl(aq) added at the end point indicated by the colour
change of the phenolphthalein indicator. Or using the complete equation, the components of
the soda ash could be based on the number of moles of Na2CO3 equals ½ the number of moles
of HCl required to reach the second equivalence point.

6. What are the possible sources of errors and their effect on the calculated parameters?
Rationalize.
Possible sources of error in the titration include random and systematic errors. Errors could be
from pipetting errors, solution preparation errors, subjective titration. One possible error
could also come from the purity of the solutions used. For the boiled distilled water, it is
possible that not all carbon dioxide gas was removed and may have affected the neutralization
process. Possible errors could come from determining the equivalence point by determining the
color of the indicator since it could be hard to distinguish the color change, especially with the
methyl orange indicator; overshooting the titration.

REFERENCES

[1] Harris, D. C. (2010). Chemical Equilibrium. In D. C. Harris, Quantitative Chemical Analysis (pp. 171-
177). New York: W. H. Freeman and Company.

[2] Harvey, D. (2000). Equilibrium Constants for Chemical Reactions. In D Harvey, Modern Analystical
Chemistry (pp.155-156). New York: McGraw-Hill Companies.

[3] Petrucci, R., F.G, H., Madura, J., & Bissonette, C. (2010). Buffer Solutions. In R. Petrucci, H. F.G, J.
Madura, & C. Bissonette, General Chemistry: Principles and Modern Applications (pp. 750-754).
Toronto: Pearson Canada Inc.

[4] Institute of Chemistry. (2017). Chemistry 26.1: Introduction to Quantitative Chemical Analysis
Laboratory Manual. Laboratory Manual. Quezon City, Manila, Philippines: University of the
Philippines Diliman.