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Name: Eghan Kojo

Index N o : 6138811
Experiment N 0 : I 2.2.3
Assistant: Appiah Johnson
Date: 12 t h February, 2013


1. To determine the carbonate content of garden lime, by performing an analysis involving a back titration.
2. To calculate for the percentage of carbonate in garden lime.

Garden lime is a soil additive made from pulverized limestone or chalk. The primary active component
is calcium carbonate. Additional chemicals vary depending on the mineral source and may include calcium
oxide, magnesium oxide and magnesium carbonate. Lime may occur naturally in some soils but may require
addition of sulfuric acid for its agricultural benefits to be realized. Gypsum is also used to supply calcium for
plant nutrition.
Calcium Carbonate is an exceptional mineral. The chemical formula CaCO3 covers a raw material,
which is widespread throughout nature, whether dissolved in rivers and oceans, in molten form as carbonatitelava, or solid as a mineral in the form of stalactites, stalagmites or as the major constituent of whole mountain
ranges. Plants and animals need calcium carbonate to form their skeletons and shells. In fact, when considering
our lives, modern mankind could hardly imagine existing without calcium carbonate. Almost every product in
our daily lives either contains calcium carbonate or has some association with the mineral during its production.
The Earths crust contains more than 4% calcium carbonate. As a result, the three calcium carbonate minerals calcite, aragonite and vaterite - are among the most important rock-forming minerals. Rocks are not the only
calcium carbonate deposits in nature, most stretches of water and countless plants and animals contain huge
amounts of calcium carbonate. Other industrially important source minerals which are predominantly calcium
carbonate include limestone, chalk, marble and travertine.
Calcium carbonate is a chemical compound with the formula CaCO3. It is a common substance found in
rocks in all parts of the world, and is the main component of shells of marine organisms, snails, coal balls,
pearls, and eggshells. Calcium carbonate is the active ingredient in agricultural lime, and is usually the principal
cause of hard water. It is commonly used medicinally as a calcium supplement or as an antacid, but excessive
consumption can be hazardous.
The vast majority of calcium carbonate used in industry is extracted by mining or quarrying. Pure
calcium carbonate can be produced from a pure quarried source.

Alternatively, calcium carbonate is prepared from calcium oxide. Water is added to give calcium hydroxide, and
carbon dioxide is passed through this solution to precipitate the desired calcium carbonate, referred to in the
industry as precipitated calcium carbonate
CaCO3 CaO + CO2
CaO + H2O Ca(OH)2
Ca(OH)2 + CO2 CaCO3 + H2O
Calcium carbonate is also used in the purification of iron from iron ore in a blast furnace. In the oil
industry, calcium carbonate is added to drilling fluids as a formation-bridging and filter cake-sealing agent; it is
also a weighting material which increases the density of drilling fluids to control the downhole pressure. In
ceramics/glazing applications, calcium carbonate is known as whiting, and is a common ingredient for many
glazes in its white powdered form.
Calcium carbonate shares the typical properties of other carbonates. Notably:
It reacts with strong acids, releasing carbon dioxide:
CaCO3(s) + 2HCl(aq) CaCl2(aq) + CO2(g) + H2O(l)
It releases carbon dioxide on heating, called a thermal decomposition reaction, (to above 840 C in the case of
CaCO3), to form calcium oxide, commonly called quicklime, with reaction enthalpy 178 kJ / mole:
CaCO3(s) CaO(s) + CO2(g)
Calcium carbonate will react with water that is saturated with carbon dioxide to form the soluble calcium
CaCO3 + CO2 + H2O Ca(HCO3)2
In this experiment, the garden lime was added to HNO3, this made it possible for the carbonate to react
with the nitric acid, releasing carbon dioxide and water.
CaCO3(s) + 2HNO3(aq) Ca(NO3)2(aq) + H2O(l) + CO2(g)
However the reaction requires heating to ensure it reaches completion and hence the amount of calcium
carbonate cannot be determined by titration the garden lime with the acid. Instead the technique of back titration
was used. The lime is first reacted with an excess of acid and heated to release all the carbon dioxide. The
resulting solution is titrated with sodium hydroxide to determine how much acid remains.
HNO3(aq) + NaOH(aq) NaNO3(l) + H2O(l)
The amount of acid reacting with the carbonate is calculated from the difference between the amount of acid
added to the lime and the amount of acid remaining when reaction is complete. In this way the amount of
carbonate in the garden lime can be determined.



Garden lime
0.1M NaOH
Bromothymol blue indicator
Distilled water


Electronic balance
3 conical flasks
10ml pipette
Electric plate

2.5g of garden lime was weighed into a conical
flask and then 20ml of 1M HNO3 added to it,
and stirred.
An extra 10ml of distilled water was added to
the solution.
The solution was heated to boil and then
allowed to cool for about 10mins.
The content of the conical flask after heating
was then transferred into a 100ml volumetric
flask and topped up to the mark.
10ml of the prepared solution in the volumetric
flask was measured and titrated against
standard sodium hydroxide using 2 drops
Bromothymol blue indicator.
The titration was repeated twice more using
further 10ml of the prepared in the volumetric

Volume of burette: 50 ml
Volume of pipette: 10 ml
Indicator Used: Bromothymol blue
Colour change: Yellow to blue

Some white precipitates in suspension were
The precipitates remained insoluble.
The insoluble sediments dissolved leaving
some dark sediments
More precipitates were forming.

There was a colour change from yellow to blue

indicating the endpoint.

Final volume/ml
Initial volume/ml
Titre value

Average titre =




18.60+18.60+ 18.50

= 18.56 ml

a) The average volume of sodium hydroxide used = 18.56 ml
b) From CiVi= CfVf
where Ci = initial concentration of HNO3= 1M
Vi= initial volume of HNO3 measured= 20ml
Vf= final volume of HNO3 = 100ml
Cf = final concentration of HNO3 in 100ml
Cf = (120)/100= 0.2M
hence n(HNO3) in the 100ml = 0.210010-3 = 0.02mol
c) n(HNO3) originally added to the lime= [HNO3]V(HNO3)
= 1M2010-3= 0.02mol
d) From the equation
HNO3(aq) + NaOH(aq) NaNO3(l) + H2O(l)
n(NaOH)= n(HNO3)
n(NaOH) that reacted with excess HNO3= 0.118.5610-3 = 1.85610-3mol
hence n(HNO3) that reacted with CaCO3= 0.02 - (1.85610-3) = 0.018144mol
e) From the equation
CaCO3 + 2HNO3 Ca(NO3)2 + H2O + CO2(g)
n(CaCO3)=n(HNO3)/2= 0.018144/2= 9.07210-3 mol
f) Mass of CaCO3 that reacted= n(CaCO3)M(CaCO3)
= 9.07210-3100
= 0.9072g
mass of calciumcarbonate
x 100
g) Given % carbonate in garden lime =
mass of gardenlime
x 100
= 362.88%

In the technique of back titration, garden lime is first reacted with an excess of acid and then heated to
release all carbon dioxide. The garden lime which was containing calcium carbonate could not be quantified
directly therefore it was first reacted with nitric acid. The acid reacted with the carbonate to produce the salt,
water and then a gas. The acid was added in excess in order to react with all calcium present. One important
reactions undertaken by nitric acid is it oxidation reaction as a result of the NO3- ion in the presence of the
hydrogen ions. This kind of oxidation depends greatly on the pH of the medium and also the nature of the
substances oxidized. Nitric acid reacts with almost all common metals on the periodic. So the introduction of
HNO3 to the sample not only reacted with the carbonate but all other metals as well as non-metals present in the
given sample, this either oxidized or formed a salt with it.
The amount of nitrate that react with the calcium is the same as the amount of carbonate liberated since
the reaction had a mole ratio of 1:1 and hence through a back titration with standard sodium hydroxide the
amount of carbonate in the garden lime was found to be 9.07210-3mol and this gave a mass of 0.9072g and the
percentage carbonate present in the garden lime was found to be 362.88%.


Care was taken with the addition of the distilled water so as to preventing overshooting the 100ml mark
The standard solution of 1M HNO3 was not measured with the pipette because HNO3 is corrosive.
A reagent blank was prepared prior to the titration.
The pipette was removed after filling the burette to prevent excess NaOH from dripping into the burette

Exact quantities of carbonate present in the garden lime sample could not be determined as the nitric
acid used reacted with other metals and non-metals present and also oxidizing other compounds.

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