QUANTITATIVE DETERMINATION OF SODA ASH COMPOSITION
BY DOUBLE INDICATOR TITRATION
YZZA CAMILLE A. DIAZ
DEPARTMENT OF FOOD SCIENCE AND NUTRITION, COLLEGE OF HOME ECONOMICS
UNIVERSITY OF THE PHILIPPINES DILIMAN, DILIMAN, QUEZON CITY 1101, PHILIPPINES
DATE SUBMITTED: 25 JULY 2013
DATE PERFORMED: 18 JULY 2013
ABSTRACT
In this experiment, the composition of soda ash is quantitatively determined by the use of double-indicator titration
method. The indicators used were phenolphthalein 8.3 <pH< 10.0 which accounts for basicity and methyl orange 3.1
<pH< 4.5 which accounts for acidity[3], has close equivalence point to our desired endpoint. This titration involves a
weak base- strong acid titration. The standardization of HCl was done using Na2CO3 as primary standard. Latterly,
since Vph < Vmo― Na2CO3 and NaHCO3 were determined as the components of soda-ash. For the first trial 32.9%
Na2CO3 and 72. 1 %NaHCO3; for the second trial 24.1 % N a2CO3 and 76. 1% NaHCO3; and lastly the third trial 23.8
% N a2CO3 and 94.6% NaHCO3.It is rational therefore that the soda ash sample consists NaHCO3 since it is a
product of the thermal decomposition of sodium carbonate. This experiment is significant to know the total acid
neutralizing capacity of soda ash which can be used in the industry for the production of soap, glasses, paper etc.
INTRODUCTION Before starting the experiment, solutions of a 250 mL
1.0 M stock HCl and 250 mL 0.050 M standard HCl
Soda ash is an unrefined product acquired from the solution from 1.0 M HCl were prepared. After this, we
thermal decomposition of Sodium carbonate proceeded to the standardization of the 0.050 M HCl
(NaHCO3)[1]. In this experiment, the goal is to solution. First, we weighed 0.1 g of the primary
determine quantitatively, its composition by double standard Na2CO3. This was then dissolved by 75 mL
indicator titration method. Moreover, it aims to relate boiled distilled water, then we added 3 drops of the
the concept of strong acid-strong base and weak methyl orange indicator and titrated it with 0.050 M
acid-weak base titrations and carbonate system HCl. When the solutions turn to yellow or near
titration. Titration of substances basically is used to orange, we temporarily stopped the titration to boil the
determine the amount of acid or base in a solution[2]. solution for two to three minutes. When it again turns
In a double indicator titration method, we use two to yellow, we continue its titration to end point. After
indicators namely phenolphthalein and methyl orange this, the analysis of soda ash sample is started by
instead of the common titration wherein there is only weighing 0.5 0.2 g of soda ash sample in an
one indicator used. It is used only if there are two analytical balance and dissolved it using 75 mL of
bases present in the solution. These indicators are boiled distilled water. We divided the solution into
qualified to be used in the experiment because the three and added 50 ml of boiled distilled water to
endpoints which are at 8.3 <pH< 10.0 and 3.1 <pH< each solution. Subsequently, we added 3 drops of the
4.5 respectively, are close to the desired titration phenolphthalein indicator and titrated it with 0.050 M
equivalence point. The solution is said to have HCl. When the phenolphthalein endpoint is reached,
reached the endpoint if it changed color, in this case three drops of methyl orange indicator is then added
solutions turn to yellow or near orange or in some, red and titration was continued. When the color changes
because of over titration. from yellow to near orange titration is temporarily
stopped and then the solution was boiled for two to
three minutes. Similar to the standardization process, NaHCO3 (Vmo– Vph)
when the solution turns back to yellow, the titration is Na2CO3: M Vph
continued until the methyl orange endpoint.
Since, Vph< Vmo the expected compositions of the
Determining the percent composition of compounds soda ash sample are Na2CO3 and NaHCO3. A greater
present in a soda ash sample helps in terms of
Vmo implies that the HCl used to neutralize HCO3 is
knowing its alkalinity value. The alkalinity value is the
total acid neutralizing capacity of soda ash, by greater than the amount needed to neutralize CO3.
knowing how much NaHCO3, Na2CO3 and NaOH (if Therefore indicating the presence of NaHCO3[3]. We
there is any) is present in the sample, we may also can determine the percent composition of these
know its acid neutralizing capacity. This implies the compounds by using the Table 1 and equating it as
behavior of these groups of compounds and can later seen in the calculations part of the appendix. The
be convenient for chemical purposes (e.g. results for the first trial for the % Na2CO3 is 32. 9 %
manufacture of soap, glass, paper, etc.). [1]
while NaHCO3 is 72. 1 %; for trial 2 24.1 % N a2CO3
RESULTS AND DISCUSSIONS and 76. 1% NaHCO3; and lastly for trial 3 23.8 % N
a2CO3 and 94.6% NaHCO3. This results are rational
For us to be able to determine the components of the because sometimes it is not possible for a 100%
unknown sample, we need to obtain the volume of composition because the solutions may have
HCl required to reach two distinct endpoints which are impurities.
the volume of phenolphthalein endpoint and the
volume of methyl orange endpoint. These two The color change which is from yellow to near
indicators are used because the endpoints which are orange in the first titration is its fake endpoint. For us
at 8.3 <pH< 10.0 for phenolphthalein and 3.1 <pH< to be able to determine the true endpoint, we need to
4.5 for methyl orange, are close to the desired boil the solution for two to three minutes to remove
titration equivalence point [2], and at these respective the CO2 formed. After this we can resume titration
endpoints, the solutions changes their color to signal and get the true endpoint as the solution again turns
neutralization of different protons of the complex from yellow to near orange. If the solution turned red,
system. it is over titrated.
The values of Vph and Vmo are obtained using the The absence of NaOH in the composition of the soda
average net volume phenolphthalein endpoint and ash makes the composition of Na2CO3 and NaHCO3
methyl orange endpoint respectively. The solutions compatible. The incompatibility of NaOH in the
shown in the appendix gave the values of Vph = sample is because the presence of OH- will react with
9.489666667 and Vmo = 45. Using Table 1, we can the HCO3-. This will cause a decrease in
relate Vph and Vmo and determine the substance concentration and production of carbonate ions. [3]
present in the soda ash sample.
For this experiment, there are possible sources of
Table 1. The volume relationships for different error. Firstly, in weighing the soda ash and the
compositions of soda ash. primary standard using the analytical balance.
Relationship of Composition of Moles of Analytical balances, requires weighing by difference,
Vph and Vmo sample substance one might have used the opposite of it which is
present weighing by addition. Secondly, wrong burette
Vph=0; Vmo>0 NaHCO3 M Vmo reading which can lead to a smaller or larger amount
Vmo=0 NaOH M Vph of HCl recorded which will affect on the concentration
Vph= Vmo Na2CO3 M Vph or M Vmo of phenolphthalein and methyl orange endpoint. And
Vph > Vmo Na2CO3 and NaOH: M(Vph lastly, over titration of the solution. If it is over titrated,
NaOH –Vmo) we can no longer determine the true endpoint of
Na2CO3: M Vmo phenolphthalein and methyl orange in this case.
Vph< Vmo Na2CO3 and NaHCO3: M
SUMMARY AND CONCLUSIONS
REFERENCES
The experiment have shown that Vph< Vmo which [2] Zumdahl, Steve. Chemistry 4th edition. Houghton
implies that the components of the soda ash sample Mifflin Company. 1997.
are Na2CO3 and NaHCO3. It is a titration of a weak [4] Brady, Humiston. General Chemistry Principles
base with a strong acid, in this particular experiment and Structure 3rd edition. John Wiley and Sons Inc.
the weak bases are Na2CO3 and NaHCO3 and their USA.
percent composition in the soda ash sample are
determined using two indicators, phenolphthalein and Internet References:
methyl orange; and the HCl is the strong acid titrant. [1]www.microlabinfo.com/.../CD...2...Soda.Ash.../11.2.
In the course of the addition of HCl the solution still Anal.Soda.Ash.pdf (Accessed July 23, 2013)
contains some unreacted weak base and salt [3] http://www.scribd.com/doc/92576976/Formal-
therefore acting as a buffer. The solution will contain Report-1-Expt-7-Chem-26-1#download (Accessed
salt of the weak base at the endpoint and by July 24, 2013)
hydrolysis of the cation pH can be determined. The
pH of the solution is dependent to the excess
hydrogen ion from the titrant. [4]
APPENDIX
DATA GATHERED:
Standardization of Hydrochloric Acid Solution
Primary Standard used: Na2CO3
Percent Purity of Primary Standard: 99.7 %
Formula mass of Primary Standard: 105.99 g Na2CO3
Table 1. Obtained values from the Standardization of Hydrochloric Acid Solution.
Trial 1 2 3
Primary Standard weight, g 0.1006 0.0002 0.0954 0.0002 0.0951 0.0002
Final volume of HCl, ml 40.5 0.08 35.7 0.08 35.6 0.08
Initial volume of HCl, ml 1.9 0.08 0.6 0.08 1.4 0.08
Net volume of HCl, ml 38.6 0.08 35.1 0.08 34.2 0.08
M HCl 38.6 0.0001 35.1 0.0002 34.2 0.0002
Average M HCl 0.0508
Sample Analysis
Sample Stock Solution
Mass Sample: 0.5633 0.0002
Total Volume of Sample Stock: 75.00 0.05
Working Sample Solution
Volume of Sample Stock: 25.00 0.05
Total volume of Working Sample: 75.00 0.05
Table 2. Obtained values from the analysis of the sample.
Trial 1 Trial 2 Trial 3
Phenolphthalein endpoint
Final Volume of HCl, mL 11.5 0.05 17.9 0.08 18.1 0.08
Initial Volume of HCl, mL 0.03 0.05 9.5 0.08 9.801 0.08
Net Volume of HCl, mL 11.47 0.05 8.4 0.08 8.299 0.08
Methyl Orange endpoint
Final Volume of HCl, mL 54.7 0.05 59.8 0.08 68 0.08
Initial Volume of HCl, mL 11.5 0.05 17.9 0.08 18.1 0.08
Net Volume of HCl, mL 43.2 0.05 41.9 0.08 49.9 0.08
Relationship of Vph and Vmo: Vph ˂ Vmo
Composition of Soda Ash: Na2CO3 and NaHCO3
CALCULATIONS:
Determination of the M HCl for the three trials in the Standardization of Hydrochloric Acid solution
Trial 1
M HCl= = 0.04903102111 M HCl 0.0001
Trial 2
M HCl= = 0.051133029 M HCl 0.0002
Trial 3
M HCl= =0.05231360787 M HCl 0.0002
∑
Average M HCl= = = 0.05082588599 M HCl
Error Propagation
Trial 1
R= 0.04903102111
r= R √
r= √ = 0.0001
Trial 2
R= 0.05231360787
r= √ = 0.0002
Trial 3
R= 0.05082588599
r= 0.05082588599√ = 0.0002
Determination of Vph and Vmo and their relationship using the data gathered in Table 2.
∑
Vph= = = 9.489666667
∑
Vmo= = = 45
Since the calculated value of Vph is 9.489666667 and Vmo is 45 it implies that Vph ˂ Vmo, hence the components of the
soda ash sample are Na2CO3 and NaHCO3.
Determination of the percent composition of Na2CO3 and NaHCO3 in the soda ash sample.
Trial 1
% NaOH = 0 %
% Na2CO3=
= (100%) = 32. 9 % N a2CO3
( )
% NaHCO3=
= = 72. 1 % NaHCO3
Trial 2
% NaOH = 0 %
% Na2CO3=
= (100%) = 24.1 % N a2CO3
( )
% NaHCO3=
= =76. 1% NaHCO3
Trial 3
% NaOH = 0 %
% Na2CO3=
= (100%) = 23.8 % N a2CO3
( )
% NaHCO3=
= =94.6% NaHCO3