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QUANTITATIVE ANALYSIS OF SODA ASH BY DOUBLE-INDICATOR

TITRATION

D. J. Q. YTAC
DEPARTMENT OF CHEMICAL ENGINEERING, COLLEGE OF ENGINEERING
UNIVERSITY OF THE PHILIPPINES, DILIMAN, QUEZON CITY, PHILIPPINES
DATE PERFORMED: 27 SEP 2014
INSTRUCTOR’S NAME: ERICKA ITANG

ANSWERS TO QUESTIONS

1. Discuss why there is a need to boil distilled water in the preparation of base solutions.

Distilled water was boiled to remove the CO2 dissolved in the solution. NaHCO3 and Na2CO3
can be formed when CO2 reacts with NaOH and these products can affect the results of titration [1]
as described by the equation: CO2 + 2OH − → CO3 2− + H2 O.
Furthermore, CO2 gas dissolved in water forms H2CO3. This makes the solution slightly
acidic and could also affect titration. Water was boiled to release as much of this CO2 gas and make
the pH close to 7.

2. Discuss why a mixture of NaOH and NaHCO3 is incompatible.

HCO3- is an amphiprotic species; it can act both as an acid or a base. If an acid is present in
the solution, it acts as a base. If a base is present, it acts as an acid. Therefore, a mixture of the two is
incompatible because of their reaction: NaHCO3 + NaOH → Na2 CO3 + H2 O [1]. From this, NaHCO3
can act as the limiting reactant and be consumed completely in the reaction. Na 2CO3 is produced
and is the only component that will be identified from the analysis. The other case where NaOH is
the limiting reactant produces both Na2CO3 and excess NaHCO3. Another case is when OH- and
HCO3- anions react to form H2CO3, giving products composed of NaOH and H2CO3 only. All of these
could affect titration and produce erroneous results and data.

3. Discuss why there is a need to boil the solution before reaching the methyl orange endpoint.

This was done to remove CO2 and the carbonic acid formed from CO2 produced from the
reaction between the carbonate and acid, which makes the solution acidic [1]. This could then affect
the results of titration. Since the substances are less soluble in high temperatures, they are removed
from the solution by heating. This helps in obtaining a sharp endpoint indicated by the correct color
of methyl orange.

4. Discuss the basic components of the unknown soda ash sample based on the volume relationship
at the phenolphthalein and methyl orange endpoints.

The amount of titrant used to reach the methyl orange endpoint is greater than that of
phenolphthalein. This means that the sample contains carbonate and bicarbonate bases. The
sources of bicarbonate base are neutralization of carbonate and the sample. Thus, larger amount of
acid is required to neutralize the bicarbonate bases [1].
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5. Discuss the possibility of using NaOH as primary standard for HCl and the properties of an ideal
primary standard.

The properties of an ideal primary standard are: highly pure, stable in the atmosphere, with
high molecular weight, soluble in titration medium, and of modest cost. NaOH fails to be a good
primary standard because it is unstable, hygroscopic, and has low molecular weight [1].

6. Discuss the rationale behind not storing basic solutions in volumetric glassware.

Basic solutions react with glass to form sodium silicates which interfere with titrimetric
analyses.

7. Discuss the possible sources of errors and their effect on calculated parameters.

One source of error is the failure to read the burette measurements at eye level. This
increases the molarity of HCl obtained and also affects the composition of Na 2CO3 and NaHCO3
obtained. Another error is approximating the endpoint to be the equivalence point. This does not
necessarily coincide with the stoichiometric equivalence point in the reaction [1].

8. Discuss the cause of carbonate error and its effect on the calculated values obtained in
standardization and sample analysis.

Carbonate error comes from the failure to boil the water used for the preparation of NaOH
solutions. This therefore causes the percentage of Na2CO3 to increase and at the same time, NaHCO3.

REFERENCES

[1] Skoog, D. A., West, D. M., Holler, F. J., Crouch, S. R. Fundamentals of Analytical Chemistry 9th ed.
Cengage Learning. 2013.

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SAMPLE CALCULATIONS

99.8 1
% 𝑝𝑢𝑟𝑖𝑡𝑦 1 2(0.100𝑔 𝑁𝑎2 𝐶𝑂3 ) ( 100 ) ( 𝑔 )
2(m𝑁𝑎2 𝐶𝑂3 ) ( 100 ) (𝐹𝑊 ) 105.99
𝑁𝑎2 𝐶𝑂3 𝑚𝑜𝑙
𝐌𝐇𝐂𝐥 = =
𝑉𝐻𝐶𝑙 36.7𝑚𝐿
1000
= 0.0513

m = mass in grams
𝑎 2 𝑏 2 0.0002 2 0. 2
r = R√( ) + ( ) = 0.0513√( 0.1
) + (0.0367) = 0.1
𝐴 𝐵

3.70 𝑚𝐿 𝑔
(𝑀𝐻𝐶𝑙 𝑉1 )(𝐹𝑊𝑁𝑎2𝐶𝑂3 ) (0.0513 M) ( ) (105.99 )
%𝐍𝐚𝟐 𝐂𝐎𝟑 = × 100 = 1000 𝑚𝑜𝑙 × 100
𝑚𝑠𝑎𝑚𝑝𝑙𝑒 0.1000 𝑔
= 20.1 % Na2 CO3
0.1 2 0.1 2 0.0002 2
r = 0.201√(0.0513) + (0.0037) + ( 0.1
) = 5.4 = 5 %

𝑀𝐻𝐶𝑙 (𝑉2 − 𝑉1 )(𝐹𝑊𝑁𝑎𝐻𝐶𝑂3 )


%𝐍𝐚𝐇𝐂𝐎𝟑 = × 100
𝑚𝑠𝑎𝑚𝑝𝑙𝑒
7.50 − 3.70 𝑚𝐿 𝑔
(0.0513 M) ( ) (84.008 )
= 1000 𝑚𝑜𝑙 × 100 = 16.4 % 𝑁𝑎𝐻𝐶𝑂3
0.1000 𝑔

0.1 2 0.1 2 0.0002 2


r = 0.164√( ) + ( ) + ( ) =4%
0.0513 0.0038 0.1

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Statistical Analysis

𝑥 0.051 + 0.052 + 0.051


𝐌𝐞𝐚𝐧 = = = 0.051
𝑛 3

Range = Highest Value-Lowest Value = 0.052-0.051 = 0.0013


r = √𝑎2 + 𝑏 2 = √0.0522 + 0.0512 = 0.0016 =0.002

(𝑥𝑖 − 𝑥)𝟐 (0.051−0.051)𝟐 +(0.052−0.051)𝟐 + (0.051−0.051)2


Standard Deviation (s) = √ =√ =0.00066
𝑛−1 3−1

𝑠 0.00066
Relative Standard Deviation (RSD) = 𝑥 × 1000 = 0.051
× 1000 = 12.773 ppt

ts (4.30)(0.00066)
Confidence Limits (at 95% confidence level) = 𝑥 ± = 0.051 ± = 0.051 ± 0.002
√𝑛 √3

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