DALMIA CEMENT RESEARCH CENTER CHENNAI

P2O5 Determination – Without Ammonium Nitrate

Introduction:
Keeping in view to the restrictions imposed on Ammonium Nitrate usage, determination of P2O5 in gypsum and
cement is affected badly. The method described below eliminates the usage of Ammonium Nitrate. This Method
is applicable to ores and other materials where Phosphorous content is less than 5 %.

Reagents:
A) Ammonium nitro – molybdate solution:
Dissolve 100g ammonium molybdate in 200ml boiling water. Cool the solution and add 200ml ammonia
(0.88 sp. gr.). Separately mix 750ml of water and 500ml of HNO3 and cool. Add ammonium molybdate
solution to the nitric acid solution slowly with constant stirring and cooling. Filter the solution with
double 41 filter paper and keep in stoppered flask.

B) 0.1N Standard Sodium Hydroxide Solution:

Prepare 0.1N sodium hydroxide solution. Allow it to stand for 24 hours and standardize against primary
standard.

C) 0.1N Standard Nitric Acid Solution:

Prepare 0.1N Nitric Acid solution by 1.42 sp. gr. HNO3 standardize against standard NaOH solution using
Phenolphtalein indicator.

D) Potassium Permanganate Solution: Prepare 3% KMnO4 solution.

E) Na2SO3 or KNO2 or FeSO4 Solution: Prepare 5% Na2SO3 or KNO2 or FeSO4 solution.

F) 1% KNO3 solution: For washing

G) 3% HNO3 solution: For washing

DALMIA CEMENT RESEARCH CENTER CHENNAI

P2O5 Determination – Without Ammonium Nitrate

Procedure:
Weigh 2.0g sample, digest with 30 ml 1.42 sp. gr. HNO3, filter the solution by Whatman 40 filter paper to separate
any insoluble residue. Heat the filtrate to boiling to boil off all excess nitrogen. Add 5 ml of 3% KMnO4 solution, and
digest for 5 minutes. Destroy the precipitated MnO2 by adding dropwise 5% of Na2SO3 or KNO2 or FeSO4 solution till
solution becomes clear. Continue boiling for a minute or two after all MnO2 has been dissolved. Add 15 ml of conc.
o
HNO3. Cool to 70 C. Add 50 ml Ammonium nitro – molybdate solution. Shake vigorously and let for 5 – 10 minutes.
o
As the precipitation of phosphomolybdate is rapid when the solution is at 70 C.

Filter the precipitate with Whatman 40 filter paper after letting it stand for some time. Wash the flask and filter
paper containing precipitate a few times with a 3% solution of HNO3 and then with a 1% KNO3 solution until free
from acid.

Transfer the precipitate along with the filter paper to the original flask. Add 50 ml of distilled water. Add
measured quantity of standard NaOH solution in excess and dissolve the precipitate along with filter paper till
no yellow tint remains. Add few drops of Phenolphtalein indicator and then titrate excess of NaOH solution with
the standard HNO3 till pink color is completely disappears.

Calculation:
Phosphate:
[0.3088 X (V1−V2) X N]
a) As P2O5:
[0.1349 X (V1−V2) X N]
b) As P:

Here:

V1 = Volume of 0.1 N NaOH consumed

V2 = Volume of 0.1 N HNO3 consumed by excess of NaOH

N = Normality of NaOH

W= Weight of sample taken.

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