QUANTITATIVE

ANALYSIS OF SODA ASH OR ALKALI MIXTURE BY

DOUBLE-INDICATOR TITRATION


B.R.D. LAO
DEPARTMENT OF CHEMICAL ENGINEERING, COLLEGE OF ENGINEERING
DATE PERFORMED: FEBRUARY 27, 2020
INSTRUCTOR’S NAME: REINA TERESA VALDERRAMA

1. Discuss the properties of an ideal Table 1. Constituents of Soda Ash Sample

primary standard. based on Volume Relationship at the
Phenolphthalein and Methyl Orange
Primary Standards should be a) 100% Endpoints
pure, with a 0.01-0.02% impurity Constituents Volume
allowance if it is accurately known, b) Relationship
stable to drying, and room temperatures, Na2CO3 Vph > 0; Vmo = 0
c) readily, and relatively inexpensively Na2CO3 & NaOH Vph < Vmo
available, and d) with high formula weight. NaHCO3 & Na2CO3 Vph > Vmo
Furthermore, if it is to be used in titration, NaOH Vph = 0; Vmo > 0
the equilibrium of the reaction should be
far to the right to obtain a sharp endpoint. Net volume from the titration at the
(Christian & Dasgupta, p168) phenolphthalein and methyl orange
endpoints are approximately 4.4 mL and
2. Is it possible to use NaOH as the 11.57 mL, respectively. Larger net volume
primary standard for HCl? at the methyl orange endpoint than the at
phenolphthalein endpoint implies that the
NaOH cannot be used as a primary standard due unknown soda ash sample contains
to its hygroscopic property, and because it Na2CO3 & NaOH.
contains significant amounts of water and sodium
carbonate; however, if a standardized NaOH 4. Why is the mixture of NaOH and
solution is available, HCl can be standardized
NaHCO3 incompatible?
thus, NaOH solution is considered a secondary
standard (Christian & Dasgupta, p42).
Titration is not feasible for NaOH and
3. Discuss the basic components of the NaHCO3 due to the ability of NaHCO3 to act
unknown soda ash sample based on the as both an acid and base. The mixture of
volume relationship at the the two cannot exist together as they
phenolphthalein and methyl orange combine to form carbonates (METU).
endpoints.
5. Explain the rationale behind not
The double-indicator method allows the storing basic solutions in volumetric
determination of the constituents of soda glassware.
ash based on the volume relationship of
the titrations at the phenolphthalein and Strong basic solutions attack the
methyl orange indicator endpoints. As volumetric glassware, which can lead to
such, table 1 summarizes the relationship etching and change in volume, thus, why
between the constituent of the soda ash alkaline solutions are not stored in
and the net volume of the titrations. volumetric glassware (Harris, p36)

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6. Why is there a need to boil the distilled composition of the unknown soda ash
water in the preparation of base sample (Christian & Dasgupta, p288).
solutions?
9. Discuss the cause of carbonate error
Water dissolves carbonate, which may and its effect on the calculated values
result in an error in analysis. Thus, CO2 is on the calculated values obtained in
removed from water used to prepare standardization and sample analysis.
alkaline solutions by boiling the water and
then cooling it (Christian & Dasgupta, Hydration reaction is rapid as carbon
p42). dioxide reacts directly with hydroxide to
form bicarbonate. The extra H+ ions from
7. Why is there a need to boil the solution the reaction may react with the analyte,
before reaching the methyl orange which then would cause a decrease in
endpoint? amount of titrant to be used, and therefore,
cause an increase in the calculated
Boiling the solution before reaching the molarity (UCDavis).
methyl orange endpoint brings the
advantage of sharpening the endpoint at
the given indicator (Christian & Dasgupta, REFERENCES
p42-43).
[1] Christian, G.D.; Dasgupta, P.K.; Schug, K.A.
8. Discuss the possible sources of errors Analytical Chemistry, 7th ed.; John Wiley &
and their effect on calculated Sons, Inc: USA, 2014; pp 168, 42-43, 288
parameters.
[2] Harris, D.C. Quantitative Chemical Analysis,
8th ed.; W.H. Freeman and Company: USA
Errors could arise from the presence of
2010; pp 36
carbonate impurities that were not fully

removed from the boiled water, which
[3] Middle East Technical University.
may result in pH variation, and therefore,
Retrieved from
a difference in percent composition of the
http://users.metu.edu.tr/chem223/Analysis
unknown soda ash sample. Titration error,
%20of%20carbonate%20mixtures.pdf
where the difference between the
equivalence point and the end point is [4] University of California, Davis. Carbonate
inaccurately measured, may also lead to Equilibria. Soil Chemistry. Retrieved from
miscalculations in the percent http://lawr.ucdavis.edu/classes/ssc102/secti
on5.pdf

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