Chemical Engineering Department

EXPERIMENT NO :

N2-ESTIMATION BY INDIRECT METHOD

N2 Estimation by indirect method

Chemical Engineering Department Date: _______________ EXPERIMENT NO: N2 ESTIMATION BY INDIRECT METHOD AIM : To estimate N2 content in given (NH4)2 SO4 by back titration method. APPARATUS : Burette, pipette, 500ml Beaker, 250ml fask, burner, wight box CHEMICALS : (NH4)2 SO4, NaOH, Succinic Acid, HCl, etc. INDICATOR : Methyl orange, Phenolphthalein REACTION : (NH4)2 SO4 + 2NaOH NH4CL + NaOH Na2SO4 + 2H2O + 2NH3 NaCl +H2O + NH3

THEORY : In the indirect method of N2 estimation of Ammonium salt (other than the carbonate) the salt is boiled with known excess of standard NaOH solution. The boiling is continued until all ammonia escape with the steam. The excess of NaOH is titrated with standard acid solution using Phenolphthalein as an indicator. PROCEDURE : Weight accurately about 1 gm of (NH4)2 SO4 sample. Transfer it in 500 ml Beaker and add 50 ml water to dissolve (NH4)2 SO4 by stirring thoroughly. Prepare 250 ml, 0.1 N standard Succinic or Oxalic acid solution by taking proper weight of it. Prepare 500 ml of 0.1N NaOH solution by dissolving approximately 2.2 gm of NaOH in 500 ml of distilled water. Find out the exact normality of this NaOH solution by titrating the solution with 0.1 N standard Succinic or Oxalic acid solution. Take the NaOH solution in burette. Add 300ml of above NaOH solution in beaker containing 50 ml (NH4)2SO4 Solution. Heat the content till all the NH3 produced due to reaction is drawn off.
TEST FOR THE PRESENCE OF AMMONIA :

Take a drop of concentrated HCl on a glass rod and keep it above the mouth of conical flask.

N2 Estimation by indirect method

Chemical Engineering Department If while fumes are evolved the presence of NH3 is suggested. The care must be taken that no drop of concentrated HCL should fall in conical flask during the performance. After ammonia is completely drawn off, cool the content and measure the volume of the remaining solution by standard measuring cylinder and Note down it. Take out 10 cc of standard 0.1N Succinic acid or Oxalic acid solution in conical flask and titrate it with above reacted NaOH solution kept in Burette.

OBSERVATIONS : Weight of (NH4)2SO4 = ________gm. Volume of reaction mixture in Beaker at the start of Reaction = 350 ml Volume of reaction mixture in Beaker at the end of Reaction (v) = _______ml (A) Standardization of NaOH (Titration -1) : First of all prepare 500 ml dilute solution of NaOH of approximate normality 0.1N by dissolving 2.2 gm NaOH pellets in 500ml distilled water. The exact normality of this solution can be found by titrating the solution with standard 0.1N Succinic Acid or 0.1N Oxalic Acid Solution. So first prepare 250 ml of 0.1N Succinic Acid or 0.1N Oxalic Acid solution. Burette : x N NaOH solution Pipette : 0.1N succinic acid Indicator : Phenolphthelein End point : Colorless to Pink
OBSERVATION TABLE :

Sr. no

burette reading Initial Final

difference (ml)

average (ml)

Actual Normality of NaOH : NaOH Succinic acid N1V1=N2V2 N1 = N2V2 V1 = (n1) = __________ N

N2 Estimation by indirect method

Chemical Engineering Department (B) Back titration of NaOH(Reaction Mixture) after completion of reaction : Burette : x N NaOH solution(Reaction Mixture after cooling) Pipette : 0.1N succinic acid Indicator : Phenolphthelein End point : Colorless to Pink
OBSERVATION TABLE :

Sr. no

burette reading Initial Final

difference (ml)

average (ml)

Actual Normality of NaOH(Reaction Mixture after cooling) : NaOH Succinic acid N1V1= N2V2 N1 = N2V2 V1 = (n2) = __________ N CALCULATION : (NH4)2 SO4 + 2NaOH (A) Na2SO4 + 2H2O + 2NH3

NaOH Consumed in the reaction : (i) NaOH in solution before reaction : Gm/lit of NaOH in solution before reaction = Normality * Equivalent Weight = (n1) * (40) = G1 = ___________ gm/lit 1000ml solution contains G1 = ___________ gm of NaOH 300ml of NaOH solution contains = 300*G1/1000 = G2 =___________ gm of NaOH (ii) NaOH in solution after reaction : 4 N2 Estimation by indirect method

Chemical Engineering Department

Gm/lit of NaOH in solution after reaction = Normality * Equivalent Weight = (n2) * (40) = G2 = ___________ gm/lit 1000ml solution contains G2 = ___________ gm of NaOH (v)=________ml of NaOH solution(After reaction) contains = (v) * G2/1000 = G2 =___________ gm of NaOH Hence NaOH Consumed in the reaction : = NaOH taken at the start of reaction -NaOH remained after reaction = G1 - G2 (G) =__________ gm reacted Gm moles of NaOH reacted = (G) /40 = (z) = _________gm moles NaOH Gm moles of NH3 generated = Gm moles NaOH reacted = (z) =___________ gm mole Gms of NH3 generated = (Z) = (z) * 17 Hence 1 gm of (NH4)2SO4 contains (Z) = ________ gm of NH3 100 gm of (NH4)2SO4 contains = (p) = 100 * (Z) = _________gm of NH3 practically Hence percentage of Ammonia in (NH4)2SO4 = (p) = _________

N2 Estimation by indirect method

Chemical Engineering Department 17 gm NH3 has 14 gm N2 (p)= _______ gm NH3 has (p)*14/17 = ____________ (q) =____________ gm N2 Percentage of N2 in (NH4)2SO4= (q) =__________ Also Calculate theoretical percentage of NH3 and N2 in the NH4Cl

RESULT : (1) Percentage of Ammonia in (NH4)2SO4 =___________ (2) Percentage of N2 in (NH4)2SO4 =_______________

N2 Estimation by indirect method