Phosphorus in Ferro Chrome

DETERMINATION OF PHOSPHORUS IN FERRO CHROME/CHARGECHROME BY
ALKALIMETRIC METHOD
BRIEF DESCRIPTION OF ITS PRINCIPLE
Sample is digested with HCl and HNO3 acid and fumed with perchloric acid. During fuming P & Cr
are oxidized. Subsequently oxidized chromium is removed as chromylchloride on addition of
hydrochloric acid. Phosphorus present as orthophosphate is precipitated as ammonium
phosphomolybdate and determined by alkalimetric titration.
REFERENCE TO THE STANDARD ON WHICH THE PROCEDURE IS BASED
IS 13452 (Part7): 2003
CHEMICAL REAGENT REQUIRED
1. Concentrated Nitric Acid rd = 1.42

2. Hydrofluoric Acid -48 percent rd = 1.16
3. Perchloric Acid 60 percent
4. Concentrated Hydrochloric Acid - sp. Gr. 1.16
5. Ammonium Nitrate Solution 50 percent (w/v)
6. Ammoniummolybdate Solution -
a) Weigh 50 g of ammoniummolybdate in a 500 ml beaker, add 100 ml of
ammonium hydroxide, dissolve and make up to 200 ml. Keep it separately.
b) Add 400 ml of nitric acid to 400 ml of distilled water in a 1 litre conical flask, cool and
keep it separately.
Slowly add solution a) into solution b) with continuous stirring and cooling. Allow to settle and filter
before use.
7. Potassium Nitrate Wash Solution – 2 percent (w/v)
8. Standard Nitric Acid (0.075N) -

Take 4.7 ml of concentrated nitric acid (rd = 1.42) to a 1 litre volumetric flask and make to the
mark. Standardize the solution against standard sodium carbonate solution using methylorange as
indicator.
9. Standard Sodium Carbonate Solutiion (0.075N) –

Weigh 0.3975 g preheat sodium carbonate from 250 to 2700 C for half-an-hour. Cool in a
desiccator, and transfer into a 100 ml volumetric flask. Dissolve in distilled water and make up to
the mark.
10. Methylorange –
Dissolve 0.05 g in 100 ml distilled water.
11. Phenolphthalein –
Dissolve 0.5 g in 50 ml alcohol and dilute with 50 ml distilled water with constant stirring .
12. Hydrochloric Acid – 1 : 3 (v/v)

13. Sodium Hydroxide Solution (approximately 0.075N) -
dissolve 3 g of sodium hydroxide in 1 litre of distilled water.
AN UNAMBIGUOUS STEP BY STEP INSTRUCTION
1. Weigh 2 g dried and agated sample (for P 0.01 to 0.03 percent ) or 1 g (for P 0.03 percent above)
agated sample and transfer to 500 ml conical flask. Add 10 ml hydrochloric acid followed by 5
ml nitric acid and few drops of hydrochloric acid. Heat the solution a hot plate. After about 30
min, add 10 ml of perchloric acid and reflux for 30 min, after fuming starts. Again add 10 ml of
perchloric acid and continue fuming on a hot plate till the mass almost dissolves. Cool the
beaker and dissolve the salts with minimum quantity of water and transfer the contents into a
conical flask of 500 ml capacity. Clean the bottom of the flask with a little concentrated
hydrochloric acid and boil. Evaporate the solution on a hot plate till dense white fumes come
out.
2. Add concentrated hydrochloric acid (4) drop wise till brown fumes come out. Keep on hot plate
and again efflux for some time to reoxidize chromium. Again add hydrochloric acid to remove
chromium.
3. Continue the operation (2) till all chromium is expelled, that is, no more brown fumes on
addition of hydrochloric acid.
4. Evaporate the bulk to syrupy condition. Dissolve the salts with about 50 ml of water. Add 25
ml of ammonium nitrate solution and 50 ml ammonium molybdate solution. Warm the content
to 650 C with constant shaking. Remove from the heat and shake further for about 5 min.
Phosphorus is precipitated as fine yellow crystal. Allow the precipitate to settle for 2 h atleast.
5. Filter the precipitate on a paper pulp pad, wash the flask and precipitate several times with cold
neutral potassium nitrate wash solution until the washings tested no longer acidic to
phenolphthalein. Transfer the precipitate with pad to the original flask where phosphorus was
precipitated. Add 10 to 15 ml of distilled water and shake the flask to discipate the pad.. Add 10
ml of sodium hydroxide solution to the flask and shake well. Titrate the excess sodium
hydroxide solution with standard acid using phenolphthalein as indicator.
6. Carry out a reagent blank with same quantity of all the reagents and chemicals used except the
sample.
CALCULATION:
Phosphorus , percent = (V1 – V2) X N X 0.00135 X 100

M
Where,
V1 = volume in ml, of standard nitric acid required by the blank;
V2 = volume in ml, of standard nitric acid required in the test sample ;
N = normality factor of standard nitric acid used ; and
M = mass in g, of the sample taken

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DETERMINATION OF PHOSPHORUS IN FERRO CHROME/CHARGECHROME BY

BRIEF DESCRIPTION OF ITS PRINCIPLE

REFERENCE TO THE STANDARD ON WHICH THE PROCEDURE IS BASED

IS 13452 (Part7): 2003

CHEMICAL REAGENT REQUIRED

1. Concentrated Nitric Acid rd = 1.42

8. Standard Nitric Acid (0.075N) -

9. Standard Sodium Carbonate Solutiion (0.075N) –

12. Hydrochloric Acid – 1 : 3 (v/v)

AN UNAMBIGUOUS STEP BY STEP INSTRUCTION

Phosphorus , percent = (V1 – V2) X N X 0.00135 X 100

V1 = volume in ml, of standard nitric acid required by the blank;

V2 = volume in ml, of standard nitric acid required in the test sample ;

N = normality factor of standard nitric acid used ; and

M = mass in g, of the sample taken

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