Name: Florida, Danielle Grace N. Instructor: Engr. Noel Sabarillo, M.Sc.

Section: 1 CHE-C Date Performed: July 5, 2019

Group No.: 5 Date Submitted: July 11, 2019

Experiment 4: Volumetric Analysis of a Carbonate-Bicarbonate Mixture

ABSTRACT
The analysis of a Carbonate-Bicarbonate mixture that contains carbonate (CO32-), and bicarbonate
(HCO3-) is a sample of a mixture that uses double indicator method, which involves two indicators,
Phenolphthalein, an alkaline-range indicator, and Methyl Orange, an acid-range indicator. The experiment
aims to determine the percentage composition of carbonate and bicarbonate present in the unknown
sample. The unknown sample was diluted and three aliquots were titrated with HCl until a colorless (first
endpoint) and light peach (second endpoint) color appears. The volumes were recorded and computed,
reporting an average percentage of 3.74% Na2CO3 and an average percentage of 18.22% NaHCO3.

INTRODUCTION
An acid-base titration is an experimental procedure used to determine the unknown concentration
of an acid or base by precisely neutralizing it with an acid or base of known concentration. This allows us
to quantitatively analyze the concentration of an unknown solution (Ikoku et.al, 1984). This type of
titration makes use of indicators to know the equivalence point wherein an indicator changes its color if
an end point is reached.

Indicators are pigments or dyes that can be isolated from a variety of sources, including plants,
fungi, and algae that contains a class of organic pigments known as anthocyanin that can change color
with pH (Okoduwa et.al, 2015). Acid‐base titration requires indicators to show color change at each pH
interval. (Nuryanti et. al, 2013)

Most solution only requires one indicator, but a solution containing sodium carbonate,
sodiumhydrogen carbonate, and sodium hydroxide wherein no more than two of these three constituents
can exist in appreciable amount in any solution requires two titrations for its analysis. This method
involves two indicators, an alkaline-range indicator, and an acid-range indicator.

The experiment aims to determine the percentage composition of carbonate and bicarbonate
present in the unknown sample using two indicators, Phenolphthalein and Methyl orange. In the
experiment, an unknown solution sample containing sodium carbonate and sodium bicarbonate was
titrated using a strong acid, HCl. The resulting solution was then computed and the observers determined
the percent of Na2CO3 and NaHCO3.

MATERIALS AND METHODOLOGY

The following are the materials and equipment to be used in the experiment: Na2CO3, NaHCO3,
Phenolphthalein indicator, Methyl Orange indicator, Standard HCl, Pipette, Beakers, Titration setup, pH
meter and Tissues.

The preparation of the unknown solution and titration set-up were distributed to each member of
the group to be able to work simultaneously and efficiently. Member 1 was tasked to wash and dry all the
glassware to be used in the experiment. Member 2 was tasked to clean the burette by rinsing it with
distilled water and washing it with HCl, which was the titrant used in the experiment. The washing was
done to remove the remains of distilled water, to avoid any changes in the concentration of the titrant,
HCl. The burette was then filled with the titrant up to the 0mL mark. Member 2 also calibrated the pH
meter using pH 7 and pH 4.

Member 3 was tasked to prepare the unknown sample given by the instructor. A 1.8875g of
unknown sample was dissolved with 100mL of distilled water in a clean beaker. The dissolved solution
was transferred in to a 250mL volumetric flask, filled to mark with distilled water. Four 50mL aliquot
sample with each having 3 drops of Phenolphthalein indicator was prepared in three Erlenmeyer flask and
a clean beaker.

The aliquot sample in the beaker was first titrated. Using a magnetic stirrer and pH meter, the
solution was continually stirred and read every 0.5 mL of HCl was used. The pH and volumes obtained
were recorded until a colorless solution was formed. The colorless solution was then added 3 drops of
methyl orange and was again titrated, stirred and read every 0.5 mL of HCl was used. The pH and
volumes obtained were again recorded until a light peach solution was formed.

The three aliquot samples in an Erlenmeyer flask were also titrated with the same procedure but
without the pH meter and magnetic stirrer. The three pink aliquot samples were titrated until a colorless
solution was formed. The colorless solution was again added 3 drops of methyl orange turning the
colorless to yellow. The solution was again titrated until a light peach solution was formed. The volumes
obtained were recorded and procedure with the aliquot sample in the Erlenmeyer flask was repeated one-
by-one by each member of the group.
RESULTS AND DISCUSSION

Figure 1.1 shows the titration curved obtained from the experimental data by plotting each 0.5
mL used for titration versus the pH read by pH meter. The titration curve does not show the steepness of
the large pH fall during the titration of a weak base and a strong acid.

Figure 1.1 Titration curve of the Analysis of Carbonate-Bicarbonate Mixture

In Table 1.1 below, the volumes of the standard HCl used at first end point and second end point
for Trial 1 to Trial 3 were recorded. This data can prove that the mixture contains carbonate and
bicarbonate ions because the volume needed to neutralize the bicarbonate ion is greater than the volume
needed to neutralize the carbonate ion. The number of CO32- that reacted completely happened first due to
its more basic nature than HCO3-. It is signalled by the change in color from pink to colorless which is
exposed by the phenolphthalein indicator, an alkaline-range indicator with a pH range 8.2-10. The first
endpoint was reached at an average of 1.22 mL volume of HCl used. The number of HCO3- that reacted
completely happened second due to its less basic nature than CO32-. It is signalled by the change in color
from yellow to light peach which is exposed by the methyl orange indicator, an acid-range indicator with
a pH range 3.2-4.4. The second endpoint was reached at an average 8.68mL volume of HCl used. The
number of moles of CO32- was calculated using the formula from Equation 1.

(Equation 1)
Table 1.1 Determination of Percent Na2CO3 and NaHCO3

Weight Sample: 1.8875g

Trial 1 Trial 2 Trial 3
Aliquot portion 50mL 50mL 50mL
Grams sample in aliquot 0.3775g 0.3775g 0.3775g
M of Standard HCl 0.1099M
Part I
Vinitial of HCl burette 0mL 9.9mL 19.85mL
Vfinal of HCl burette 1.3mL 11.1mL 21.0mL
V of HCl used 1.3mL 1.2mL 1.15mL
Moles CO32- 1.4287x10-4 1.3188x10-4 1.2639x10-4
Mass Na2CO3 in aliquot 0.015g 0.01398g 0.01340g
% mass Na2CO3 in sample 3.97% 3.70% 3.55%
Average % mass Na2CO3 3.74%
Standard Deviation 0.2128
Relative Standard Deviation 5.69%
% Theoretical mass Na2CO3 3%
% Relative Error 23.67%
Part II
Vinitial of HCl burette 1.3mL 11.1mL 21.0mL
Vfinal of HCl burette 9.9mL 19.85mL 29.70mL
V of HCl used 8.6mL 8.75mL 8.70mL
Total moles HCO3- 9.4514x10-4 9.6163x10-4 9.5613x10-4
Moles HCO3- in the aliquot 9.0227x10-4 8.2975x10-4 8.2425x10-4
Mass NaHCO3 in the aliquot 0.06739g 0.06969g 0.06924g
% mass NaHCO3 in sample 17.85% 18.46% 18.34%
Average % mass NaHCO3 18.22%
Standard Deviation 0.32316
Relative Standard Deviation 1.77%
% Theoretical mass NaHCO3 15%
% Relative Error 21.47%
 The mass of Na2CO3 in aliquot was taken from the number of moles computed from Equation 1,
thus resulting for an average mass percent of 3.74% Na2CO3 with a relative error of 23.67%

(Equation 2)

The total moles of HCO3- were computed using the volume from the 1st end point up to the 2nd
end point with Equation 2, the moles of CO32- was subtracted from it, to get the number of moles of
HCO3- reacted at part II. Using the number of moles of HCO3-, the mass of NaHCO3 in the aliquot was
computed, resulting for an average mass percent of 18.22% NaHCO3 with a relative error of 21.47%.

CONCLUSION AND RECOMMENDATIONS

After the analysis of the results, it can be concluded that the objective of the experiment was
achieved, as we’ve calculated and determined the percentage composition of Na2CO3 and NaHCO3 in a
mixture containing carbonate and bicarbonate. The overall experiment resulted a large percent error from
both Part I and Part II, with 23.67% and 21.47%, respectively. The possible sources for this large percent
error may due to the over or under titration of the solution, inconsistent reading of burette and pipettes,
and overshooting the mark of the volumetric flask in the dilution of unknown solution. For a better result,
it is recommended that every procedure should be done with precaution.

REFERENCES

Ikoku C., Ahmed M., Joju E. Laboratory Exercise in Chemistry. Enugu, Nigeria: Fourth Dimension
Publishers; 1984.
Nuryanti, S., Matsjeh, S., Anwar, C., Raharjo, T. J., & Hamzah, B. (2013). Corolla of Roselle (Hibiscus
sabdariffa L.) as acid-base indicator. European Journal of Chemistry, 4(1), 20-24.
doi:10.5155/eurjchem.4.1.20-24.620
Okoduwa, S. I., Mbora, L. O., Adu, M. E., & Adeyi, A. A. (2015). Comparative Analysis of the
Properties of Acid-Base Indicator of Rose (Rosa setigera), Allamanda (Allamanda cathartica),
and Hibiscus (Hibiscus rosa-sinensis) Flowers. Biochemistry Research International, 2015, 1-6.
doi:10.1155/2015/381721
APPENDIX