BASIC ANALYTICAL

CHEMISTRY
LABORATORY REPORT
EXPERIMENT NUMBER & EXPERIMENT 3 - DTERMINATION OF CALCIUM
TITLE CARBONATE CONTENT IN EGGSHELL BACK
TITRATION

GROUP : AS1204D

NAME : CASSY LUGAK

STUDENT NO : 2018433928

LECTURER’S NAME : Nur Maria Ulfa Binti Seruji

DATE OF EXPERIMENT : 17 March 2020

DATE OF SUBMISSION : 22 Mei 2020

 DETERMINATION OF CALCIUM CARBONATE IN EGGSHELL BY
BACK TITRATION
PURPOSE
To determine the calcium carbonate content in eggshell.

INTRODUCTION
The major component of eggshells is calcium carbonate,CaCO3.This analysis is
done volumetrically by using a characteristics reaction of carbonate
compounds,namely their reaction with acids.Calcium carbonate(limestone) is very
insoluble in pure water but readily reacts in acid according to the reaction below.

CaCO3 + 2HCl → CaCl2 + CO2 + H2O

This reaction cannot be used directly to titrate the CaCO3,because it is really slow
when the reaction is close to the endpoint.Instead the determination is achieved by
adding an excess of hydrochloric acid to react with all the CaCO3 and then remaining
unreacted HCl with NaOH solution to determine the amount of acid which did not
react with the calcium carbonate.Furthermore,the reaction used to determine the
amount of unreacted acid by titration which is back-titration.

APPRATUS
Burette
Pipette
Erlenmeyer Flask
Electronic balance
Mortar
Bunsen Burner

CHEMICALS AND MATERIALS

0.2 M Potassium Hydrogen phthalate (KHC8H4O4)
Sodium hydroxide solution
Hydrochloric acid solution
Phenolphthalein indicator
Methyl orange indicator
Eggshell
PROCEDURE
(A) Standardization of the NaOH solution
1. A burette was filled with the NaOH solution
2. 20 mL of the standard potassium hydrogen phthalate,KHC8H4O4 solution was
pipette into an Erlenmeyer flask(we ask the instructor for the exact concentration of
this solution.) 2 drops of phenolphthalein indicator was added.
3. The KHC8H4O4 with the NaOH solution was titrated.
4. The titration was repeated two times.
5. The concentration of the NaOH solution have been calculated.
Use 0.5 gram.

(B) Standardization of the HCl solution

1. 10 mL of the HCl solution was pipette into an Erlenmeyer flask.2 drops of
phenolphthalein indicator was added.
2. The HCl with NaOH solution have been titrate from the burette.
3. The titration has been repeated.If the result is not closed to first one,carry out
another titration and calculated the mean volume.
4. The concentration of HCl solution has been calculated.

(C) Analysis of eggshells

1. Some dried eggshell were obtained with the inner membrane being removed.Grind
the eggshell in a mortar into small particles.(About the sine of fine sand)
2. 1.0 g of the eggshell have been weighted in an Erlenmeyer flask.
3. 20ml of the standard HCl solution was pipette into the Erlenmeyer flask that
contains eggshell.After waited for 3 minutes the reaction has been completed.
4. The reaction mixture was heated until boiled.2 drops of methyl orange indicator
has been added and cooled it down.
5. The mixture has been titrated with NAOH until the colour changes to yellow.
6. Step2 to 5 was repeated.
7. The percentage of CaCO3 in the eggshell has been calculated in each replicate.
8. The mean percentage of CaCO3 n the eggshell was calculated.
RESULTS

A) Standardization of the NaOH solution.

Test 1 2 3
Initial burette 7.45 12.70 18.00
reading (ml)
Final burette 12.70 18.00 23.25
reading (ml)
Volume of NaOH 5.25 5.30 5.25
solution used (ml)

(B) Standardization of HCl solution.

Test 1 2 3
Initial burette 4.60 4.15 14.70
reading (ml)
Final burette 38.30 36.85 48.95
reading (ml)
Volume of NaOH 33.70 32.70 34.25
solution used (ml)

( C ) Analysis of the eggshell

Test 1 2 3
Mass of the 0.50 0.53 0.51
eggshell (g)
Initial burette 0.55 15.05 18.35
reading (ml)
Final burette 15.05 34.75 34.30
reading (ml)
Volume of NaOH 14.50 19.70 15.95
solution used (ml)
CALCULATIONS
1. Calculate the concentration of NaOH solution.
1L
20 ml x = 0.02 L
1000 ml

Moles of KH8H4O4=Molarity of KH8H4O4 (M) x L of solution

= 0.1 M x 0.02 L
= 0.002 mol

NaOH + KH8H4O4 → KNaC8H4O4 + H2O

1 mol of KH8H4O4 = 1 mol of NaOH

0.002mol of KH8H4O = 0.002 mol of NaOH
Gap 5.30  5.25
QTEST = = =1
Range 5.30  5.25
Refer to Q-Test table,QCal > QTab so the data was rejected.

5.25 ml  5.25 ml
Volume of NaOH used =
2
1L
= 5.25 ml x
1000 ml
= 0.00525 L

Molar mass of NaOH = 22 + 16 + 1

= 39 g/mol

Mass of NaOH,g = Moles of NaOH x Molar mass of NaOH

= 0.002 mol x 39g/mol
=0.078 g

moles of NaOH(mol)
Molarity of NaOH (M) =
L of solution
 0.002mol
= = 0.3809 M
0.00525 L

Mass of NaOH, g
Concentration of NaOH,C =
Volume of NaOH used, L
0.078 g
=
0.00525 g/L
= 14.857 g/L

2. Calculate The concentration of HCl solution.

NaOH + HCl → NaCl + H2O

Gap 32.70  33.70

QTEST = = = 0.6452
Range 34.25  32.70
Refer to the QTEST table, QCal > Qtab in 95% confident limit,the data was retained.

33.70  32.70  34.25

Volume of NaOH used =
3
1L
= 33.55 ml x
1000 ml
= 0.03355 L
1 ml
10 ml x = 0.01 L
1000 ml

M1V1 = M2V2
(0.3809 M)(0.03355 L) = (M2)(0.01 L)
0.01278
M2 =
0.01
= 1.278 M

Moles of HCl = Molarity of HCl x Volume of HCl used

= 1.278 M x 0.01 L
= 0.01278 mol

Molar mass of HCl = 1+ 35

 = 36 g/mol

Mass of HCl,g = Moles of HCl x Molar mass of HCl

= 0.01278 mol x 36 g/mol
= 0.46008 g

Mass of HCl, g
Concentration of HCl ,C =
Volume of HCl, L
0.46008 g
=
0.01 L
= 46.008 g/L

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

Gap 19.70 - 15.95

QTEST = = = 0.7212
Range 19.70 - 14.50
Refer to QTEST >QTAB in 95% of confident limit,so the data was retained.

14.50 ml  19.70 ml  15.95 ml

Volume of NaOH used =
3
1L
= 16.7167 ml x
1000 ml
= 0.01672 L
1L
25 ml x = 0.025 L
1000 ml

M1V1 = M2V2
(0.3809)(0.01672) = (M2)(0.025)
0.006368
M2 =
0.025
= 0.25472 M

Moles of HCl (initial) = Molarity od HCl x Volume of HCl used

= (1.278) (0.01)
 = 0.01278 mol

Moles of HCl (excess) = Molarity of HCl x Volume of HCl used

= 0.25472 x 0.025
= 0.006368 mol

Moles of HCl reacted = Moles of HCl(initial) - moles HCl (excess)

= 0.01278- 0.006368
= 0.006412 mol

Formula weight,CaCO3 = 40+ 12 + 3(16)

= 100 g/mol

HCl : CaCO3
2:1
0.006412 mol : 0.003206 mol

Mass of CaCO3, g = Moles of CaCO3 x Molar mass of CaCO3

= (0.003206 mol) (100 g/mol)
= 0.3206 g

Test 1
0.3206 g
x 100% = 64.1%
0.50 g

Test 2
0.3206 g
x 100% = 60.5 %
0.53 g

Test 3
0.3206 g
x 100% = 60 %
0.51 g
4. Calculate the mean percentage of CaCO3 in the eggshell.

64.1%  60.5%  60%

=
3
= 61.5 %

Percent error(%) =
actual value - experimental value x 100%
actual value
95%  61.5%
=
95%
= 0.3526 x 100%
= 35.26 %
DISCUSSION
Firstly,back titration is a method that used to determine the concentration of
analyte by reacting it with a known number of moles of excess reagent.The excess
reagent then titrated with a second reagent.In this experiment we wanted to determine
the percent of calcium carbonate in eggshell by back titration.Therefore,the amount of
calcium carbonate in eggshell can be determined by measuring the amount of standard
hydrochloric acid required to react completely with it.

For the first part,which is standardization of NaOH solution,in this part NaOH
was titrated with potassium hydrogen phthalate .From the reaction below,

NaOH + KH8H4O4 → KNaC8H4O4 + H2O

We can determined the concentration and the molarity of NaOH .For the molarity we
can used the formula moles of NaOH divided with the volume of solution and the
value of molarity NaOH is 0.3809 M.From the molarity value,we can find out the
concentration by using the formula molarity x molar mass.Then,the concentration
value for NaOH are 14.857 g/L.

Next,for the second part hydrochloric acis was titrated with NaOH to
standardized the HCl solution.The formula for the reaction between this two reaction
is,
NaOH + HCl → NaCl + H2O
From this equation we can find the molariy of HCl by used the formula M1V1=M2V2
and the molarity of NaOH (0.3809) can used in the formula therefore the molarity of
HCl we calculated is 1.278 M.From the molarity of HCl,we can find the concentration
the same formula in part one which is molarity x mass.Then,the concentration of HCl
is 46.008 g/L.

The third experiment,we carried out the analysis of the eggshell.This analysis will
be done volumetrically.Actually this reaction cannot be used directly to titrate the
calcium carbonate because it is very slow when the reaction close to the
endpoint.So,we adding an excess of acid dissolve all the calcium carbonate and titrate
it with sodium hydroxide to calculate the percentage of calcium carbonate.
 The eggshell was analysed to determine the percentage of calcium carbonate
slowly by adding a base which is NaOH to eggshell which was mixed with 20 ml
hydrochloric acid.From all the information that we get,we can determine the moles
HCl from initial,excess and reacted.All this value can we used to find out what are the
mass of calcium carbonate.From the mass of calcium carbonate the mean percentage
in the eggshell can be calculated.The mean percentage of calcium carbonate in the
eggshell we got through the experiment is 61.5%.

The source of errors in this experiment that may effect the results of the
experiment.Firstly,how we handle the apparatus while using its.For example,pipette
that we used to transfer HCl solution into conical flask.This cause the systematic error
in the amount of moles of hydrochloric acid present in conical flask.Other than
that,the Erlenmeyer flask that was not swirling correctly and make the solution do not
mixed well and the result will not correct as well.Not only that,it may effect the mean
value for NaOH in the experiment because the value is not consistent.

Some precautions have been taking care to to improve the results in this
experiment.Firstly,the pipett that we used to transfer the HCl must be sprayed with
distilled water.The distilled water actually do not affected the amount of moles of
NaOH in the conical flask,but will ensure all the NaOH solution is transferred into the
flask.To overcome errors when swirling,we should swirled vigorously throughout the
experiment, and the colour change should be checked closed.Last but not least,this is
the important while we do the experiment,which is keep our eyes in the level with the
liquid surface while taking the burette reading during titration to avoid systematic
error.So,we must avoid all this errors to get a good result for the experiment.
CONCLUSIONS
In the conclusions,from the experiment we actually can determined calcium
carbonate content in the eggshell.In this experiment,I have been calculated the
percentage errors which is 35.26%.The amount of calcium carbonate in eggshell was
61.5%.

REFERENCES
 https://www.academia.edu/30947897/OBJECTIVE_To_determine_the_calci
um_carbonate_content_in_eggshell
 https://www.scribd.com/doc/114262995/Determination-of-Calcium-carbonat
e-from-Egg-shells
 http://www.markedbyteachers.com/as-and-a-level/science/determination-of-c
alcium-carbonate-in-eggshells-by-acid-base-titration.html