QUANTITATIVE ANALYSIS

TITRATION

OF

SODA ASH

BY

DOUBLE-INDICATOR

S.A.P. SAAVEDRA1, J. C. VILLASIS2, J.T. LIM2 AND M.C.Z. PORTEZA3

1NATIONAL INSTITUTE OF PHYSICS, COLLEGE OF SCIENCE
2DEPARTMENT OF FOOD SCIENCE AND NUTRITION, COLLEGE OF HOME ECONOMICS
3
DEPARTMENT OF MINING, METALLURGICAL AND MATERIALS ENGINEERING, COLLEGE OF ENGINEERING
UNIVERSITY OF THE PHILIPPINES, DILIMAN, QUEZON CITY, PHILIPPINES
DATE PERFORMED: JUNE 22, 2016
INSTRUCTORS NAME: GARRERO, M.J.

1. Why is there a need to boil the distilled

water in the preparation of base
solutions?

3. Why is there a need to boil the solution

before reaching the methyl orange
endpoint?

Boiling distilled water is essential to

remove dissolved carbon dioxide (CO2)
present in the solution. Presence of CO2 in
water makes the solution slightly acidic. CO2
solubility increases with pH, thus addition of
base solution will cause a redox reaction to
occur, forming a buffer solution. This will
affect the concentration of base solution and
then the accuracy of the determination of
endpoint.

As with boiling distilled water, the

solution is boiled before reaching methyl
orange endpoint to remove dissolved CO2.
Non removal of CO2 can cause buffer solution,
affecting reading of methyl orange endpoint.

2. Why is the mixture NaOH and NaHCO3

incompatible?

NaOH is a strong base in nature while

NaHCO3, which acts as base in a reaction with
HCl, can also act as a weak acid. A mixture of
the two compounds give:
(1)

This will then react in a neutralization

reaction. In general, NaOH and NaHCO3 is
incompatible.

4. Discuss the basic components of the

unknown soda ash sample based on
the volume relationship at the
phenolphthalein and methyl orange
endpoints

Titration is first done using the

phenolphthalein indicator, noting that initial
solution is basic. Net Volume 1 (V1) indicates
the volume needed to reach solution endpoint
(change from fuchsia pink to colorless). Once
reached, a second indicator, methyl orange,
was used to determine second solution
endpoint. Net Volume 2 (V2) indicates volume
needed to reach solution endpoint from V1.

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TABLE 1. Volume Relationship of the

Possible Components of the Soda Ash
Sample
Component
Na 2CO2
NaHCO3
NaOH
Na 2CO2 + NaHCO3
Na 2CO2 + NaOH

Volume Relationship
V1 = V2
V1 = 0, V2 > 0
V2 = 0, V1 > 0
V1 > V2
V2 > V1

From experiment, soda ash components

are Na2CO2 and NaOH
5. Is it possible to use NaOH as the
primary standard for HCl?

NaOH is not a possible standard for HCl

since it is highly hygroscopic. It readily
absorbs moisture from the air, forming
Na 2CO3, thus reducing the amount of NaOH
that must react with HCl 1 . Therefore,
preparation of NaOH solution as primary
standard is not possible without resorting to
air-and-water free environment to retain
known molarity.

These properties are rare to come from

any compound, thus it is usually normal to
makes use of less ultrapure compounds as a
substitute. A secondary standardization must
be made, however, to determine purity of
new standard.
7. Explain the rationale behind not
storing basic solutions in volumetric
glassware.

Volumetric glassware (or glassware in

general) are composed silicic materials which
are acidic. These will then react with basic
solutions, the latter attacking and dissolving
the glass 3 . Long term storage of basic
solutions in volumetric glassware will cause
etchings in glass and neutralization of the
base.
8. Discuss the possible sources of errors
and their effect on calculated
parameters.
Some possible sources of errors that are:

6. Discuss the properties of an ideal

primary standard.

The following are some of the important

requirements for a primary standard,
according to Skoog 2:

Highly purified
Atmospheric stability
Absence of hydrate water so that
composition of solid does not
change with respect to humidity
Relatively large MM, such that
relative error in weighing the
standard is minimized

reaction of base with CO2 forming

carbonates;
contamination of reagent solutions;
impurities in primary standard
Na 2CO2; and,
end point determination errors
(addition of too much or too less HCl
titrant)

These errors will affect calculations of

molar concentration of the soda ash
components and the HCl solution. Other
sources of errors are parallax error,
equipment failure and human error(s).

9. Discuss the cause of carbonate error

and its effect on the calculated values

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on the calculated values obtained in

standardization and sample analysis.
Carbonate error is an error in endpoint
determination due to the presence of carbonic
acid in the solution4. Since our solution, initially
alkaline in nature, reacts with the carbonic
acid, it forms a more neutralized solution,
changing the desired pH value.
Therefore, values of volume obtained
during titration for both standardization and
sample analysis will not be accurate. It will
affect determination of soda ash sample
components since it is highly titrant-volume
based.
REFERENCES
[1] Stoichiometry in Solution Standardization
of
Sodium
Hydroxide.
http://www.macalester.edu/~kuwata/Cl
asses/200405/chem%20111/111l%20experiment%
208%20-%20naoh.pdf (accessed June 23,
2016)

[2] Skoog D.A., West D.M., Holler J.F. In

Introduction to Analytical Chemistry, 8th
ed.; Cengage Learning: Pasig, 2012; p 264.
[3] Molecular Biology Problem Solver: A
Laboratory Guide. Edited by Alan S.
Gerstein. A.S., G., Ed.; Wiley-Liss, Inc.: New
York, 2001; p 38.
[4] Chemistry 3600 Exam Key, 1999. Stephen
E.
Bialkowski
Teaching.
http://ion.chem.usu.edu/~sbialkow/Clas
ses/3600/Exam2-1999/Exam2-key.html
(accessed June 24, 2016).

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