QUALITATIVE DETERMINATION OF SODA ASH

COMPOSITION BY DOUBLE INDICATOR

TITRATION
W. YBAEZ1
NATIONAL INSTITUTE OF MOLECULAR BIOLOGY AND BIOTECHNOLOGY, COLLEGE OF SCIENCE
UNIVERSITY OF THE PHILIPPINES, DILIMAN, QUEZON CITY 1101, PHILIPPINES
DATE SUBMITTED: 29 FEBRUARY 2016
DATE PERFORMED: 23 FEBRUARY 2016
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ANSWERS TO QUESTIONS
1. Why is there a need for the distilled water to be used in this experiment to be boiled?
The distilled water should be boiled in order to remove dissolved CO2. Since CO2 is a gas
dissolved in water, increasing the temperature would in turn increase the kinetic energy
of the gas molecules, enabling them to escape from the solution more easily.
The removal of dissolved CO2 in the solution is necessary for accurate titrimetry. CO2 in
the solution can affect the accuracy of the procedure since it forms into carbonic acid[1],
as shown in (1).
2() + 2 () 2 3( ) (1)
Since carbonic acid donates H+ into the solution, the H+ might react with the basic
components in the standard/analyte and might cause a lower calculated molarity of HCl
and in turn, lower percentages of the components.
2. Why is the mixture NaOH and NaHCO3 incompatible?
Sodium hydroxide donates OH- while sodium bicarbonate donates HCO3- into the
solution. This two react as in (2).
3 + 2 + 32 (2)
The bicarbonate and hydroxide ions react to form carbonate ions which introduces errors
in the calculations for percent composition.
In a sense, it is like starting off with a sample containing only carbonate ions (as in a
Na2CO3 only sample), giving data reflective of that sample (Vmo = Vph). This data does not
give any insight to the experimenter onto how to calculate for the percentage of both
NaOH and NaHCO3 in the sample, and will lead to a misidentification of the
composition of the soda ash sample (as Na2CO3).
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3. Why is there a need for the solution to be boiled before reaching the methyl orange
endpoint?
In the methyl orange endpoint, all HCO3- ions must be neutralized. However, in the
neutralization of the bicarbonate ions with H+ (3), H2CO3 is generated.
3 + + 2 3 (3)
The formation of carbonic acid can alter the color of the methyl orange indicator, making
it seem as if the analyte has already reached the endpoint even though it havent (since
carbonic acid makes the solution more acidic). As seen in (1), carbonic acid exists in
equilibrium with carbon dioxide and by the Le Chateliers principle, decreasing [CO2] by
boiling will shift the equilibrium to the right (1). This will thereby rid the solution of
carbonic acid and minimize errors.
4. What are the basic components of the unknown soda ash sample based on the volume
relationship at the phenolphthalein and methyl orange endpoints? Report the
percentage of each components and the percent error.
The titration of the CO32- with H+ is according to the successive acid-base reactions:
32 + + 3 (4)
3 + + 2 3 (3)
This is a complex acid-base titration system wherein there are two endpoints to be
established. The first endpoint in reaction (4) is wherein the phenolphthalein indicator
changes color; while the second endpoint in reaction (3) is wherein the methyl orange
indicator changes color[2].
In theory, in the titration of CO32- (Na2CO3 only sample), the volume of HCl used to
reach the phenolphthalein endpoint is equal to the volume used to reach the methyl
orange endpoint (Vph = Vmo), following the stoichiometry[2]. However, in the titration of
the soda ash sample in the experiment, Vph < Vmo. More H+ ions was expended to reach
the methyl orange endpoint than was used to reach the phenolphthalein endpoint. This
translates that there was more HCO3- than CO32-in the solution. This only implies that
NaHCO3, which supplies the added bicarbonate ions, is also present in the soda ash
sample.
That being said, to calculate for the amount of NaHCO3 present in the sample, the
molarity of HCl is multiplied by the difference of Vmo and Vph. This is because the volume
of H+ used to reached the methyl orange endpoint is used to neutralize both HCO3coming from CO32- and the sample[3].

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From table 2 (see Appendix A), the sample was 15.2% 0.4% NaHCO3 and 53.8% 0.7%
Na2CO3. Percent error was found to be 23.8% for the percent NAHCO3 while 7.7% from
the percent Na2CO3.
5. What are the possible sources of errors and their effect on the calculated parameters?
Rationalize.
One major source of error in the experiment is the wastage of reagents and the apparent
lethargy of the experimenters. A trial for the analysis of soda ash wasnt performed due
to this and this insufficiency of data greatly affects the statistical analysis. Three data
points wouldve made a more accurate estimation of the populations true behavior and
would hypothetically lower the large values of the standard deviation and confidence
limit in the calculation for %NaHCO3.
Another possible source of error in the experiment is the calibration of glassware and
equipment. Faulty calibration of equipment, such as the analytical balance, and
glassware, such as measuring pipettes and volumetric flasks, may cause errors in
solution preparation. Instrumental uncertainties greatly affect the value of calculated
molarities and moles of substance (subsequently %composition) present since their
values are largely dependent on the accuracy of the concentrations made in the solution
preparation.
Another possible source of error is personal uncertainties such as personal judgments,
bias and shortcomings. The indicator method is based on colors and color judgment is
subjective. This may cause variation in the data obtained from experimenter to
experimenter. Another error may be due to wrong titration technique (over-titration)
and interpreting the interpretation of meniscus. This may affect the accuracy of the
calculated % compositions of each substance since they are also dependent on the
accuracy of the titrimetric procedure.

REFERENCES
[1] Brown, T., LeMay, H., Bursten, B., Murphy, C., Woodward, P. (2012) Chemistry: The
Central Science. (12th Edition). (p. 267-268). Illinois: Pearson Education, Inc.
[2] Analytical Chemistry Group. (2013). Analytical Chemistry Lab Manual. Quezon City:
University of the Philippines Institute of Chemistry
[3] microL AB. (2013). ANALYSIS OF SODA ASH (#11.2). The Computers in Chemistry
Laboratory Instruction Initiative. Retrieved on February 28, 2016, from http://mi
crolabinfo.com/wp-content/uploads/2013/09/11.2.Anal_.Soda_.Ash_.Summ_.pdf

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