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In natural water and waste water, the forms of nitrogen of greatest interest are nitrate, nitrite, aOrganic Chemistry Chemistry Question

Nitrogen in Wastewater

In natural water and waste water, the forms of nitrogen of greatest interest are nitrate, nitrite, ammonia, and organic nitrogen. All these forms of nitrogen, as well as nitrogen gas, are biochemically interconvertible and are components of the nitrogen cycle. The macro Kjeldahl method, in combination with a titration method, is often used in the determination of organic nitrogen in wastewater. In the first step, H2SO4, K2SO4, and HgSO4 are added to the sample solution. After digestion, the solution is neutralized by the addition of concentrated NaOH. The gas liberated by the treatment is then distilled into a solution of excess boric acid and the latter subsequently titrated with 0.01 M-H2SO4.

Nitrite is known to cause the illness methemoglobinemia in infants. In the laboratory, nitrite can be determined by a colorimetric method. The method requires the preparation of a series of standard nitrite solutions. However, nitrite is readily oxidized in the presence of moisture and hence standardization of the stock nitrite solution is required in order to achieve high accuracy in the subsequent analysis. The standardization is carried out by adding a known excess of standard KMnO4 solution and H2SO4 solution are added into the nitrite stock solution. The purple color of the solution due to the presence of excess permanganate was subsequently discharged by the addition of a known quantity of Na2C2O4 and the mixture back titrated with standard permanganate solution.

5.1.

Identify the product formed in the digestion step.

Model Answer

NH4+

5.2.

Identify the gas liberated upon the addition of NaOH.

Model Answer

NH3

5.3.

Write a balanced equation for the reaction between the liberated gas and boric acid.

Model Answer

H3BO3 + NH3  NH4+ + H2BO3

5.4.

Write a balanced equation for the final titration step.

Model Answer

H2BO3– + H3O+  H3BO3 + H2O

5.5.

Which of the following indicators is most suitable to be used in the final titration step:
Methyl orange (transition range pH 3.1 – 4.4), phenolphthalein (transition range pH 8.0 – 9.6) is chosen as the indicator. Explain your choice.

Model Answer

Methyl orange. At the equivalence point, the solution contains boric acid and ammonium ion, therefore, an indicator with an acidic transition interval is required.

5.6.

Write a balanced equation for the reaction of the nitrite solution with KMnO4.

Model Answer

2 MnO4– + 5 HNO2 + H+  2 Mn2+ + 5 NO3– + 3 H2O

5.7.

Write a balanced equation for the back titration.

Model Answer

2 MnO4– + 5 H2C2O4 + 6 H+  2 Mn2+ + 10 CO2 + 8 H2O

5.8.

Write a mathematical equation for calculation of nitrogen concentration if:
A: mg of N in cm 3 of NaNO2 stock solution
B: total volume (cm 3 ) of standard KMnO4 solution used
C: concentration of KMnO4 in the standard solution in mol dm –3
D: total volume (cm 3 ) of standard Na2C2O4 solution
E: concentration of Na2C2O4 in the standard solution in mol dm –3
F: volume of the stock NaNO2 solution taken for titration

Model Answer

A = [ 5 ( B × C) – 2 ( D × E ) ] × 7 / F

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