Energy and Environmental Science

Subject Code:
 Experiment No. 1

Aim
To determine the strength of calcium (Ca) as calcium
oxide (CaO) in a given cement extract solution
provided N/20 KMnO4 solution

Chemical requirement
• Ammonium oxalate solution
• anmonia solution
• methyl red
• N/20 KMNO4 solution.
Apparatus requirement
Pipette, beaker, Funnel, 100 ml. measuring Flask and Conical Flask.
Indicator used:

1. KMnO4 (Self indicator)

2. Methyl red to check the
alkalinity of solution.

End Point:
Persistence of Pink Color
Theory

Calcium Present in solution of cement extract can be precipitated as

oxalate [Ca(COO)2] by adding ammonium oxalate in slightly
alkaline medium using ammonia. The white ppt of calcium oxalate is
Filtered and washed with distilled water to remove excess of oxalate
and then dissolved in dil. H2SO4 as shown in Following reaction.
Theory

The oxalic acid so liberated in the reaction is equivalent to amount

of Calcium present in the original solution which is determined by
titration with N/20 KMNO4 solution. The following chemical
equations are involved in this titration.
Procedure
• Pipette out 20 ml of cement extract solution and transfer it to 500 ml
beaker.
• Add 80 ml of distilled water and 4-5 drops of methyl red indictor and
heat the resulting solution up to 60-80 °C.
• Now add 20 ml of ammonium oxalate solution drop wise and add
ammonium hydroxide until the color of the solution turn to yellow.
• Mix the solution well and keep them undisturbed for about 20-25
minutes and allow to settled down precipitate of calcium oxalate.
• Filter the precipitate of calcium oxalate with the help of filter paper
and wash with cold distilled water.
• Take this precipitate along with filter paper in funnel and keep them
over the mouth of the 100 ml measuring flask.
Principle
• Puncher the filter paper by using glass rod and add 20 ml of dilute
H2SO4 to dissolve and collect the white ppt. in measuring flask and
shake the solution to dissolve the ppt. completely. Using distilled water
wash and transfer the precipitate from filter paper. Make up the volume
with distilled water up to the mark i.e. 100 ml. Stopper the flask and
mix the solution well to make sure that the solution is homogeneous.
• Pipette out 20 ml of this prepared clear solution and transfer to 250 ml
conical flask and add around 5 mL i.e. small test tube of dilute
sulphuric acid.
• Warm the solution up to 50-60 °C and titrate against N/20 KMnO4
solution until a pink color persisted.
• Note the volume of KMnO4 solution consumed and repeat the titration
to get concordant readings.
Procedure
Procedure
Observations

Titration of prepared solution Vs N/20 KMnO4 solution

Volume of the prepared solution to take for each titration = 20 ml

100 ml of the prepared solution = 20 ml of cement extract solution.

20 ml of the prepared solution = 20/100 x 20 = 4 ml of cement
extract solution.
Calculation:

Normality of the prepared solution from cement extract can be

calculated by the following equation: N1V1 (oxalic acid solution) =
N2V2 (KMnO4)

N1x 4 = 1/20 x A or N1 = A/80

Therefore, the strength of calcium oxide is = N1x Equivalent

weight of CaO
=A/80 x 28 (gm/L)
= A/80 X 28 x 1000 (mg/L)
Result:
Strength of Ca as CaO =……………….mg/L or ppm
Precaution
• As KMnO4 solution is colored, so the upper meniscus
should be taken as the correct reading.
• Parallax errors should be avoided.
• The measuring flask and other glass should be
washed properly.
Thank You