Chemical Engineering Department

EXPERIMENT NO :

ANALYSIS OF AMMONIUM OXALATE / AMMONIUM SULPHATE OR AMMONIUM CHLORIDE

1 oxalate

Analysis of ammonium

Chemical Engineering Department Dat e: _____________ EXPERIMENT NO : ANALYSIS OF AMMONIUM OXALATE / AMMONIUM SULPHATE OR AMMONIUM CHLORIDE AIM : To determine the N2 content in Ammonium oxalate/Ammonium Sulphate or Ammonium Chloride by formalin method. PRINCIPLE : When formalin is added to an ammonium salt solution they react with each other by condensation. The condensation products are hexa-methylene tetramine (CH2)6N4 and an acid radical. CHEMICALS : sample of ammonium oxalate/ammonium sulphate or ammonium chloride, Standard N/10 NaOH solution, formalin solution (37% formaldehyde), distilled water etc. CHEMICAL REACTIONS : (1) 2(NH4)2SO4 +6HCHO (CH2)6N4 +2H2SO4 + 6H2O (2) 2NH4NO3 + 6HCHO (CH2)6N4 +2HNO3 + 6H2O (3) 2(NH4)2HPO4 + 6HCHO (CH2)6N4 + 2H3PO4 + 6H2O DAP (4) 4NH4Cl + 6HCHO (CH2)6N4 + 4HCl + 6H2O (5) 2(NH4COO)2 + 6HCHO (CH2)6N4 + 2(COOH)2 + 6H2O Ammonium oxalate Oxalic Acid (6) 2NH2CONH2 +6HCHO (CH2)6N4 + 2H2 CO3 + 2H2O Urea Carbonic Acid EQUIPMENTS : Balance, 50 ml burette, 250 ml volumetric flask, conical flask, 25 ml pipette, 25 ml measuring cylinder etc. PROCEDURE : (1) Weight accurately 1.5 gm of sample of Ammonium oxalate/Ammonium sulphate or Ammonium chloride. (2)Transfer it to 250 ml volumetric flask. (3) Add distilled water to it and dilute up to the mark, i.e. make it 250 ml. (4)Shake the solution; transfer 25 ml of this solution to 250 ml conical flask. (5) Now, to this solution add 10 ml of Formalin and 2 - 3 drops of thymal blue. 2 oxalate Analysis of ammonium

Chemical Engineering Department (6) Titrate this solution against ____N NaOH solutions until the color changes. (7)The end point will be yellow to violet color. (8) Also carryout blank test. For this take 25 ml of distilled water, add 10 ml of formalin and 2 - 3 drops of thymal blue indicator but dont add sample solution. (9) Titrate it against _____ N NaOH, the end point is yellow to violet color. (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 = = __________ N (B) OBSERVATION(With Sample Solution) : Weight of sample = 1.5 gm (i) Burette : Standard ___ N NaOH solutions. (ii) Conical flask : 25 ml of sample solution + 10 ml formalin + 2-3 drops of thymal blue (iii) Indicator : Thymal blue (iv) End point : Yellow to violet 3 oxalate Analysis of ammonium

Chemical Engineering Department OBSERVATION TABLE : Sr. no. Burette reading Initial Final

Difference ml

Average ml

(C) BLANK READING : (i) Burette : Standard _____ N NaOH solutions. (ii) Conical flask : 10 ml formalin + 25 ml water + 2-3 drops thymal blue (iii) Indicator : Thymal blue (iv) End point : Yellow to violet color. OBSERVATION TABLE : Sr. Burette reading no . Initial Final Difference ml Average ml

CALCULATION : Factor F = actual normality Theoretical normality F = ___________ % of N2 in ammonium oxalate/ ammonium sulphate or ammonium chloride sample = (burette reading blank reading) * 0.0014 * F * 250 *100 Weight of sample * 25 = = =

4 oxalate

Analysis of ammonium

Chemical Engineering Department

Also Calculate theoretical % of Nitrogen in given sample :

RESULT : (1) N2 content in ammonium oxalate/ ammonium sulphate or ammonium Chloride sample = ____________ % (2) Theoretical N2 content in the ammonium oxalate/ ammonium sulphate or Ammonium chloride = ___________ %

5 oxalate

Analysis of ammonium