Experiment: Soil Chemical Analysis – Calcium Carbonate

OBJECTIVE:

1. To determine the calcium carbonate in soil by using Acid Neutralization Method.

2. To study about the carbonate analysis titration method.

INTRODUCTION:

Calcium carbonate, which is also known as limestone, is a major component of calcareous soils, ranges
from a few percent in slightly calcareous soils to more than 80 percent in some extremely calcareous
soils. It is the chief component of limestone, which is a widely used amendment to neutralize soil acidity
and to supply calcium (Ca) for plant nutrition.

Limestone is a common sedimentary rock found in widespread geologic deposits. It has been used
throughout much of recorded history as a building material, a cementing agent, and in agriculture to
improve acid soils. An agricultural liming material (ag lime) is broadly defined as any substance
containing Ca or magnesium (Mg) and capable of neutralizing acidity. Limestone of a smaller particle size
reacts quickly since there is more exposed surface area for chemical reaction. Larger particles are slower
to react, but provide a sustained, longer term source of acid neutralization.

When a given weight of soil is reacted with an excess of acid, carbon dioxide gas is released and the acid
not used in the dissolution of carbonates is back titrated with sodium hydroxide solution. Soil carbonate
is usually quantified by acid dissolution as summarized in the reactions below (Allison & Moodie, 1965;
Nelson, 1982):

CaCO3 + 2H+ à Ca2+ + CO2 + H20 ----(1)

CaMg(CO3)2 + 4H+ à Ca2+ + Mg2+ + 2CO2 + 2H20 ----(2)

To determine the content of calcium carbonate in the soil, soil is treated with an excess of standard
hydrochloric acid, which will destroy the carbonates. The amount of excess acid is determined by
titration with standard sodium hydroxide, after separation from the soil by filtration. The amount of acid
destroyed in dissolving the metals is equivalent to the amount of alkali used to precipitate the
hydroxides. However, acid is lost by reaction with primary minerals. Alkaline soils of high pH also destroy
some acid through neutralization by sodium carbonate.

PROCEDURES:

1g of air-dry soil was weighed and put into a 250mL Erlenmeyer flask.

10mL of 1N hydrochloric acid solution was added to the flask with volumetric pipette.

The flask was heated for 10 minutes in oven.

50mL of DI water was added by using graduated cylinder, 2 to 3 drops of phenolphthalein

indicator was added.
 1N of sodium hydroxide solution was titrated while the flask was swirled. The titration was
continue until a faint pink colour developed. The reading, R was taken.

RESULT:

Mass of soil with beaker: 34.825g

Mass of empty beaker: 32.82g

Mass of soil: 34.825-33.82= 1.005g

Initial burette reading: 14mL

Final burette reading: 23.4mL

Volume of NaOH used, R :

Final burette reading- Initial burette reading

= 23.4-14

=9.4mL

CALCULATIONS:

Percentage of CaCO3 in soil:

NHCl = normality of HCl solution=1

NNaOH = normality of NaOH solution

R = volume of NaOH solution used (mL)

Wt= weight of air-dry soil (g)

DISCUSSION
Soil by definition is a natural body of mineral and organic constituents differentiated into horizons which
differ among themselves as well as from the underlying material in morphology, physical making,
chemical composition and biological characteristics. The soil body is made up of four components,
mineral, organic matter, water and gas. Under natural conditions the mineral and organic components
remain fairly constant in any individual soil type. The water and gas components vary from day to day
even from hour to hour. Most of the agricultural soils have pH values lying between 4 and 8. pH controls
the sorption of and distribution of the various cations by soil colloids. The solubility of many soil
constituents is sensitive to pH since the various minerals of the soil dissolve at different pH levels.

From this experiment, the 1g of air- dry soil was weighed and put into a 250mL Erlenmeyer flask.
Then, 10mL of 1N hydrochloric acid solution was added to the flask with volumetric pipette. The flask
was heated for 10 minutes in the oven. 50 mL of distilled water was added by using the graduated
cylinder and 3 drops of phenolphthalein indicators was added. 1N of sodium hydroxide solution was
titrated while the flask was swirled slowly. The titration was ended until a faint pink color was observed.

This experiment was followed the carbonate analysis titration method to be conducted. First the
soil was mixed with HCL causing the dissolution of the carbonate (CaCO3) and creating Calcium chloride
(CaCl2).

CaCO3 + 2HCl ⇒ CaCl2 + H2O + CO2

Second is The amount of acid left over is measured by titrating it with sodium hydroxide (NaOH) to
produce sodium chloride (NaCl) and water. Adding phenolphthalein indicator to the solution causes it to
turn pink when all the acid has reacted.

HCl + NaOH ⇒ NaCl + H2O

From the result recorded, the volume of NaOH used was 9.4mL which means that 9.4mL of
NaOH solution was used to neutralize the acidic soil. Soil is treated with an excess of standard
hydrochloric acid, destroying carbonates. The amount of excess acid is determined by titration with
standard sodium hydroxide after the separation from the soil by filtration. After that, the percentage of
CaCO3 in soil was calculated by the formula of:

Whereby the NHCl = normality of HCl solution=1,

NNaOH = normality of NaOH solution,

R = volume of NaOH solution used (mL),

Wt= weight of air-dry soil (g).

The percentage of CaCO3 determined was 2.985% which means that the hardness in soil has 2.985% of
Ca2+ ions. By determining the carbonate content, the amount of total neutralization potential
attributable to carbonate minerals can be determined. The remaining neutralization potential is
attributable to non-carbonate minerals for example silicate minerals, natural oxides, hydroxides, and
phosphates. In addition, carbonate, in various forms, is often added to soils, tailings, and waste rock to
increase the neutralization potential of these potentially acid producing materials.

There has some limitations that will cause the inaccurate of the results and affect the precision
of the results during the experiment. For example, the soil was not dried completely or accidentally
contact with the water in the flask before mixing with the hydrochloric acid. In addition, the mixture in
the flask was not swirled constantly when the titration process was carrying out.

LIMITATIONS:

There were some limitations that need to discuss and noticed.

1. There are parallel error occurred when taking the reading of the pipette due to the eye level was not
perpendicular to the reading.

2. The soil may not totally dried due to only short time drying by using the oven.

3. The sodium hydroxide solution that added to the soil by using the pipette was not accurate due to the
over added of sodium hydroxide solutions.

PRECAUTIONS STEPS:

1. The eyes level must perpendicular to the reading of the of pipette to get the most accurate reading of
the volume of sodium hydroxide solutions added.

2. The soil must be completely dry by using the oven.

3. The soil must be swirled when doing titration to have the most accurate titration.

CONCLUSION:

In overall, the amount of sodium hydroxide solutions that added into the solutions was 9.4mL and the
percentage of calcium carbonate was determined by using the formula above The percentage of
calcium carbonate in the soil was 2.985%. The percentage showed that how many calcium ions
presented in the soil. The chemical content in the soil was determined and the soil organic matter that
affect the soil structure was discussed.

The titration method was used in the experiment for determining the amount of sodium hydroxide
solutions added into the solutions. Titration was the most suitable and accurate method that used to
determine the small amount of sodium hydroxide solutions added. By using the titration method, an
accurate result was determined for the experiment.

LIMITATIONS:

There were some limitations that need to discuss and noticed.

1. There are parallel error occurred when taking the reading of the pipette due to the eye level was not
perpendicular to the reading.

2. The soil may not totally dried due to only short time drying by using the oven.

3. The sodium hydroxide solution that added to the soil by using the pipette was not accurate due to the
over added of sodium hydroxide solutions.

PRECAUTIONS STEPS:

1. The eyes level must perpendicular to the reading of the of pipette to get the most accurate reading of
the volume of sodium hydroxide solutions added.

2. The soil must be completely dry by using the oven.

3. The soil must be swirled when doing titration to have the most accurate titration.

CONCLUSION:

In overall, the amount of sodium hydroxide solutions that added into the solutions was 9.4mL and the
percentage of calcium carbonate was determined by using the formula above The percentage of
calcium carbonate in the soil was 2.985%. The percentage showed that how many calcium ions
presented in the soil. The chemical content in the soil was determined and the soil organic matter that
affect the soil structure was discussed.

The titration method was used in the experiment for determining the amount of sodium hydroxide
solutions added into the solutions. Titration was the most suitable and accurate method that used to
determine the small amount of sodium hydroxide solutions added. By using the titration method, an
accurate result was determined for the experiment.