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COURSE NAME:
BASIC ANALYTIC CHEMISTRY (CHM256)

EXPERIMENT: 3
DETERMINATION OF CALCIUM CARBONATE CONTENT IN EGGSHELL BY BACK
TITRATION

LECTURER’S NAME:
-

DATE OF EXPERIMENT:
- 2020

STUDENT’S NAME:

GROUP MEMBERS/LAB PARTNER:

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Objective
To determine the calcium carbonate content in eggshell.

Procedure

a) Standardization of NaOH solution


1. A burette was filled with the NaOH solution.
2. 20mL of the standard potassium hydrogen phthalate, KHC8H4O4 solution were
pipette into an Erlenmeyer Flask and 2 drops of phenolphthalein indicator were
added.
3. KHC8H4O4 were titrate with the NaOH solution.
4. The titration was repeated two times.
5. The concentration of the NaOH solution were calculated.

b) Standardization of the HCl solution


1. 10mL of the HCl solution were pipette into an Erlenmeyer Flask and 2 drops of
phenolphthalein indicator were added.
2. The HCl were titrate with the NaOH solution from the burette.
3. The titration was repeated once.
4. The concentration of the HCl solution were calculated.

c) Analysis of the eggshell


1. Dried eggshell with the inner membrane being removed were obtained. And the
eggshell was grinded in a mortar into small particles about the size of fine sand.
2. The eggshell was weight about 1.0g and were put into Erlenmeyer Flask.
3. 25mL of the HCl standard solution were pipette into the Erlenmeyer Flask that
contained eggshell. 2 - 3 minutes were needed for the reaction to complete.
4. The reaction mixture was heated to boil. The mixture was cooled down and 2 drops
of methyl orange indicator were added.
5. The mixture was titrated with the NaOH and the colour changed to yellow.
6. Steps 2 - 5 were repeated.
7. The percentage of CaCO3 in the eggshell in each replicate were calculated.
8. The mean percentage of CaCO3 in the eggshell were calculated.
Results

a) Standardization of the NaOH solution

1 2 3 Average

Initial burette reading of NaOH solution (mL) 0 0 0 0

Final burette reading of NaOH solution (mL) 15.6 15.1 15.8 15.5

Used NaOH solution (mL) 15.6 15.1 15.8 15.5

b) Standardization of the HCl solution

1 2 Average

Initial burette reading of NaOH solution (mL) 0 0 0

Final burette reading of NaOH solution (mL) 27.0 26.2 26.6

Used NaOH solution (mL) 27.0 26.2 26.6

c) Analysis of the eggshell

1 2 Average

Initial burette reading of NaOH solution (mL) 0 0 0

Final burette reading of NaOH solution (mL) 16.7 16.7 16.7

Used NaOH solution (mL) 16.7 16.7 16.7


Data Analysis

1. Calculate the concentration of the NaOH solution

Molarity of NaOH = 0.35M

Molar Mass of NaOH = 39.997g/mol

Concentration = Molarity * Molar Mass

= 0.35M * 39.997g/mol

= 13.999gdm-3

2. Calculate the concentration of the HCl solution

Molarity of HCl = 1M

Molar Mass of HCl = 36.46g/mol

Concentration = Molarity * Molar Mass

= 1M *36.46g/mol

= 36.46gdm-3

3. Calculate the percentage of CaCO3 in the eggshell of each replicate.

2HCl + CaCO3 → Ca2+ + CO2 + H2O + 2Cl

HCl + NaOH → H2O + Na+ + Cl-

No. of mole of NaOH used to react with HCl

= Molarity * Volume

= 0.35M * 0.0155L

=5.425*10-3 mol

No. of mole of HCl = No. of mole of NaOH

= 5.425*10-3 mol

Initial no. of mole of HCl = Molarity * Volume


= 1M * 0.010L

=1*10-2 mol

No. of mole of HCl used to react with CaCO3 = (10*10-3 - 5.425*10-3) mol

= 4.575*10-3mol

According to the equation two moles of HCl required to react with one mole of CaCO 3

No. of mole of CaCO3 reacted

= Moles of HCl reacted * (1 mol of CaCO3 / 2 mol of HCl)

= 4.575*10-3mol / 2

= 2.2875*10-3mol

Molar Mass = 100.1g/mol

Weight of CaCO3 = 2.2875*10-3mol * 100.1g/mol

=0.2287g

The percentage of CaCO3 in eggshell = (0.2287g/1.0g) *100%

=22.87%

4. Calculate the mean percentage of CaCO3 in the eggshell.

The percentage of CaCO3 in eggshell for the first and second data are the same

= 22.87%

Mean percentage of CaCO3 in eggshell

= (22.87% + 22.87%) / 2

= 22.87%
Discussion

In this experiment, the calcium carbonate content in eggshell was determined by back
titration. Back titration was done when an excess amount of HCl standard solution is required for a
complete reaction with the analyte. First, the NaOH solution were standardize potassium hydrogen
phthalate and phenolphthalein as the indicator. In this experiment, the concentration of NaOH solution
had not yet to be known.
Then, HCl were standardize with NaOH. The steps were repeated few times to find the closest
reading to the first titration and mean volume were calculated. In this experiment, the concentration of
HCl solution had not yet to be known.
After that, the analysis of amount of CaCO3 were made by titrating NaOH into a mixture of
HCl and grinded eggshell in an Erlenmeyer Flask. Then, the percentage of CaCO 3 in eggshell were
calculated.
Throughout running this experiment, precaution steps needed to be taken such as handling
concentrated solution with immense care, hands should be washed thoroughly after performing each
experiment and if possible, one should be wearing hand gloves to prevent from any possible damage.
The results might also meet the expectation as there might be errors during conducting this
experiment such as the eggshell powder was not fully dried or there is some part of the shell where the
inner membrane was not removed, the eggshell powder did not dissolve completely with HCl solution
when waiting for the reaction to complete and some droplets of solution may still adhere on the
beaker and the glass rod which lead to the reduction in number of moles excess of HCl.

Conclusion
The back-titration method in this experiment were meant to determine the calcium carbonate content
in eggshell. The percentage of CaCO3 in eggshell calculated for the first and second data are the same
which is 22.87%. Therefore, the mean percentage of CaCO 3 in eggshell is 22.87%.

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