University Of Karachi

CHEMICAL PROCESS TECHNOLOGY

(Practical file)

Syed Saad Ahmed B-0933040 B.E 3rd Year Chemical Engineering

Submitted To: Maam Khehkashan

CHEMICAL PROCESS TECHNOLOGY 2012

Experiment no. 9
OBJECT:
To determine the nitrogen content of urea using the Kjeldahls Method

APPARATUS AND REAGENTS:

Kjeldahl flask. Glass bulb. Bunsen burner. Round-bottomed flask. Kjeldahl trap. Reflux condenser. Nitrogen-containing sample. Concentrated H2SO4, 0.1N H2SO4. Potassium sulfate. Copper sulfate. 40% NaOH solution, 0.1N NaOH solution.

THEORY:
Kjeldahls method is based on the fact that when an organic compound containing nitrogen is heated with concentrated sulfuric acid, the nitrogen in it is quantitatively converted into ammonium sulfate. The resultant liquid is then treated with excess of alkali and the liberated ammonia gas absorbed in excess of standard acid. The amount of ammonia (and hence of nitrogen) is determined by finding the amount of acid neutralized by back titration with some standard alkali.

PROCEDURE:
A weighed quantity of the sample substance (0.3 to 0.5 grams) is placed in a special long-necked Kjeldahl flask made of pyrex glass. About 25 ml of concentrated sulfuric acid together with a little potassium sulfate and copper sulfate is added to it. The flask is loosely stoppered by a glass bulb and heated gently in an inclined position. The heating is continued till the brown color of the liquid first produced, disappears leaving the contents clear as before. At this point all the nitrogen in the substance is converted to ammonium sulfate. The Kjeldahl flask is then cooled and its contents diluted with some distilled water, and then carefully transferred into a one-liter round-bottomed flask. An excess of sodium hydroxide solution is poured down the side of the flask and it is fitted with a Kjeldahl trap and a water condenser. The lower end of the condenser dips in a measured volume of the excess of the 0.1N H2SO4 solution. The liquid in the round-bottomed flask is then heated and the liberated ammonia distilled into sulfuric acid. When no more ammonia passes over (test the distillate with red litmus), the receiver is 2

Prepared By: Syed Saad Ahmed | B.E Chemical Engineering

CHEMICAL PROCESS TECHNOLOGY 2012

removed. The excess of acid is then determined by titration with 0.1N NaOH solution using phenolphthalein as the indicator.

CALCULATION:
Let the weight of the organic substance be w grams. V ml of H2SO4is required for completeneutralization of ammonia evolved. V ml of 1NH2SO4 = V ml of 1N NH3 1000 ml of 1N HCl consumed by 17 grams of ammonia 1000 ml of 0.1N HCl consumed by 17 grams of ammonia

Titration of HCl by NaOH: Serial no.

1 2 3 4 5

Initial reading
2.8 17.5 23.8 30.1 36.5

Final reading
8.8 23.8 30.1 36.5 42.8

Average rading

6.3

For 10 ml HCl 6.3 ml of NaOH is used HCl consumed is 10-6.3 = 3.7 For 100 ml HCl = 3.7 100 = 37 Then, 37 ml of 0.1N HCl consumed by grams of ammonia 37 ml of 0.1N HCl consumed by 0.0629 grams of ammonia 1 gm of urea contains 0.3 gm of ammonia

RESULTS:
The amount of nitrogen present in the given compound is found to be 21% 3

Prepared By: Syed Saad Ahmed | B.E Chemical Engineering

CHEMICAL PROCESS TECHNOLOGY 2012

DISCUSSION:
Urea:
Urea, white crystalline solid containing 46% nitrogen, is widely used in the agricultural industry as an animal feed additive and fertilizer. Urea or carbamide is an organic compound with the chemical formula CO (NH2)2. The molecule has two NH2 groups joined by a carbonyl (C=O) functional group.

Urea as a Fertilizer:
Urea breakdown begins as soon as it is applied to the soil. If the soil is totally dry, no reaction happens. But with the enzyme urease, plus any small amount of soil moisture, urea normally hydrolizes and converts to ammonium and carbon dioxide the chemical reaction is as follows: CO (NH2)2 + H2O + urease 2NH3 +CO2

Urea can be produced as prills, granules, flakes, pellets, crystals, and solutions. Urea has the highest nitrogen content of all solid nitrogenous fertilizers. It is highly soluble in water.

REFERENCE:
Improving Efficiency of Urea Fertilizers by Inhibition of Soil Urease Activity By S. Kiss, M. Simihaian The Fertilizer Encyclopedia By Vasant Gowariker, V. N. Krishnamurthy, Sudha Gowariker, Manik Dhanorkar, Kalyani Paranjape http://www.scribd.com/doc/96226761/Improving-Urea-Fertilizer-Efficiency

Prepared By: Syed Saad Ahmed | B.E Chemical Engineering