EXPT.

4: Quantitative Analysis of Soda Ash by

Double-Indicator Titration
I. Soda Ash
common name for sodium carbonate (Na2CO3)
primarily used in glass-making
II. Volumetric Titration
reaction between a standard solution and an
unknown solution (analyte) to determine
stoichiometric or equivalence point
can be used to calculate for the amount of the
analyte based on the volume of standard solution
used
A. Standard solution
strong acids or bases
due to pH changes of weak acids or bases near
the equivalence pt
commonly used HCl or NaOH
standardized using a primary standard
- high purity, stability towards air, absence
of hydrate water, ready availability,
reasonable solubility, reasonably large
molar mass
B. Acid-Base Titration
based on neutralization reactions
also called acidimetric or alkalimetric
titration
H3O+ + OH- 2H2O (1)

unknown sample may contain sodium

carbonate, sodium bicarbonate, sodium
hydroxide or a mixture of the 3

METHODOLOGY
I. Standardization of the HCl
Solution
Titration of dissolved Na2CO3 in boiled distilled
water with methyl orange indicator
Stop titration: yellow to near orange
Solution was boiled and allowed to cool to room
temperature (yellow solution)
Titration was continued until end point (orange
solution)
II. Analysis of Soda Ash Sample
Titration of dissolved soda ash sample in boiled
distilled water with phenolphthalein indicator
--end point: pink to clear solution
Methyl orange indicator was added and titration
was continued
Stop titration: yellow to near orange
Solution was boiled and allowed to cool to room
temperature (yellow solution)
Titration was continued until end point (orange
solution)
RESULTS AND DISCUSSION
Table 1: Volume of Acid Relationships in the
Analysis of Mixtures Containing Na2CO3,
NaHCO3 and NaOH
Constituent(s)
Volume Relationship
NaOH
V2 = 0
Na2CO3
V1 = V2
NaHCO3
V1 = 0
Na2CO3and NaOH
V1 > V2
Na2CO3 and NaHCO3 V1 < V2

III. For the Experiment :)

acid-base double indicator titration
-Phenolphthalein and methyl orange
-phenolphthalein changes color after
reactions 1 and 2
-methyl orange after reaction 3
two component complex system
-CO32- and HCO3 primary standard Na2CO3 of known
reaction with the standard acid titrant is
shown below

NaHCO3 and NaOH , incompatible:(

mixture results in the formation of Na 2CO3 until
one of them, or even both, will be used up

CO32- + H3O+ HCO3- + H2O (2)

Kb = 2.1x104

Unknown Soda Ash Sample: V1 < V2

basic components: Na2CO3 and NaHCO3

HCO3- + H3O+ H2CO3 + H2O CO2 + H2O (3)

Kb = 2.4x10-8

boiled distilled water was used to prevent

Carbonate Error

Boiling of solution before methyl orange

end point (near orange):
- to remove the buffer created at
that point due to the large amount of
dissolved CO2and small amounts of H2CO3 and
unreacted HCO3-to achieve a sharper end point
Carbonate Error
CO2 + 2OH- CO32- + H2O
NaOH as primary standard?
contains carbonate from reaction with
atmospheric CO2
contains adsorbed water; making it difficult to
weigh exactly

4. What would be the effect on the calculated

amount of sodium carbonate if Abi forgot to use
boiled distilled water when she prepared the
samples?
5. If someone unknowingly exhaled on the sample
being titrated after the phenolphthalein endpoint,
what would be its effect on the calculated
parameters?
Answers?
1. V , M , % Na2CO3
2. V --- % Na2CO3
3. Vphth, % Na2CO3, % NaHCO3
4.

V , %Na CO
MO
2
3

5. color will revert back, Vphth, %NaHCO3

basic solutions: stored in polyethylene

bottles rather than volumetric glassware
silicon - used in glass wares
because of the reaction forming sodium silicates
concentration of base will decrease slowly
Possible Sources of Errors:
difficulty of determining the exact end point of
the methyl orange indicator
>color change was gradual
>rate of change of pH at equivalence point was not
as rapid as with an HCl-NaOH titration
>over titration
failure to cool solution to room temperature
before completing titration
>changes in temperature during titration affect the
rate at which the reaction will take place
Increase, Decrease, or No Effect?
1. In the standardization of HCl solution, Marionne
failed to observe the actual Methyl Orange end
point and over titrated the solution. What will
happen to the calculated % Na2CO3?
2. If Abi forgot to boil the solution right after she
observed the phenolphthalein endpoint, what would
be the effect on the calculated %Na2CO3?
3. Marionne titrated the soda ash sample without
removing the bubbles under the buret. What was the
effect on the calculated % Na 2CO3?on % NaHCO3 ?
:D

Prepared by: Mar & Abi