Energy and Environmental Science
Subject Code: CHLR11
Experiment No. 4
Aim
To determine the strength of sodium nitrite (NaNO 2) in
the given water sample provided N/10 KMnO4 solution
and N/10 Mohr’s salt solution.
Chemical requirement
N/10 KMnO4 solution, N/10 Mohr’s salt solution and
0.75 N H2SO4
Apparatus requirement
1. Burette
2. Pipette
3. Funnel
4. 250mL flask
5. Burette holder
6. Measuring Cylinder
Indicator used:
KMnO4 acts as a self-indicator.
End Point:
Disappearance of pink colour
Theory
Nitrites can be naturally or artificially occurring in groundwater.
Nitrites come from fertilizers through run-off water, sewage and
mineral deposits. High levels of nitrites are toxic to humans and
animals, especially infants. It can enter the body as nitrate, a nutrient
which is essential to plant growth and be converted into nitrite,
which disrupts the oxygen delivering ability of hemoglobin in the
bloodstream. Infants can develop a life-threatening blood disorder
known as blue baby syndrome if exposed to the nitrite contaminated
water. Therefore it is important to determine the strength of nitrite
ion in the water sample.
The strength of NaNO2 in a given water sample can be measured by
titrating the given nitrite solution against standard KMnO 4 solution
in acidic medium. Acidified KMnO4 oxidizes nitrite ion to nitrate ion
and it reduces to manganese ions as per the following reactions:
Theory
The following problems were observed :
1. Nitrite ion is unstable in acidic medium and readily gets
converted into nitrous acid which is volatile.
Theory
2. Environmental oxidation of NO2¯ may take place and produce an
error in the result.
3. The reaction between KMmO4 and NO2¯ is not instantaneous; hence
accurate reading cannot be obtained.
In order to avoid these problems, we may change our approach from
direct to indirect titration in which a known excess volume of KMnO 4
is taken in a conical flask in acidic medium and temperature is raised
up to approximately 400 C following by addition of a known volume of
nitrite solution. At this temperature, the reaction between KMnO 4 and
NO2- is fast and instantaneous as soon as we add the NO2¯ in the conical
flask.
The volume of KMnO4 is taken in slight excess and un-reacted KMnO4
is determined by titrating the reaction mixture against N/10 Mohr’s salt
solution.
Acidified KMnO4 solution being oxidizing agent
oxidizes Fe2+ to Fe3+ and itself reduces to Mn2+ ions.
The redox reaction between Mohr’s salt and KMnO4
is as follows:
Theory
In order to overcome the problem for the formation of volatile
nitrous acid and environmental oxidation of NaNO2 precaution
should be taken that the tip of the pipette should be dipped in the
solution while slowly adding nitrite solution, so that no atmospheric
oxidation of NaNO2 takes place and NO2¯ ions do not get any time or
any chance to change to nitrous acid. In this way, we can determine
the amount of KMnO4 left un-reacted and hence the amount of
KMnO4 used by NO2¯ ions.
Procedure
• Pipette out 10 mL of N/10 KMnO4 and transfer it to 250 mL conical
flask
• Add 100 mL of 0.75 N H2SO4 with the help of measuring cylinder.
• Warm the resulting solution up to 400C (approx).
• Now slowly add 10 mL of nitrite solution to the solution in the conical
flask by keeping the tip of the pipette below the surface of the liquid.
• Titrate the resultant solution against N/10 Mohr’s salt solution till the
disappearance of pink colour.
• Note the volume of Mohr’s salt solution consumed
• Repeat the experiment to get concordant reading.
Procedure
Procedure
Observations
Concordant reading = A
Calculation:
Volume of N/10 KMnO4 solution taken each time = 10 mL
Volume of nitrite solution taken each time = 10 mL
Volume of Mohr’s salt solution consumed for the unreacted N/10 KMnO4
solution = A mL
Therefore, Volume of N/10 KMnO4 used for oxidising nitrite solution = (10
– A) mL
Now, by applying normality equation
N1V1 (NaNO2) = N2V2 (KMnO4)
N1 x 10 = 1/10 x V2
N1 x 10 = 1/10 x (10 – A) N
Strength = N x Eq. Wt. of NaNO2 x 1000 mg/L
Result:
The strength of NaNO2 solution = mg/L or ppm.
Thank You