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IS 13938-3 (1993): Chemical analysis of ferromanganese,Part 3: Determination of phosphorous by volumetric(alkalimetric) method [MTD 5: Ferro Alloys]

IS 13938 ( Part 3 ) : 1993

Indian Standard

CHEMICAL ANALYSIS OF FERROMANGANESE ,

PART 3 DETERMINATION OF PHOSPHORUS BY (ALKALIMETRIC ) METHOD

VOLUMETRIC

UDC 669’15’ 74 - 198 : 543’847

6 BIS 1993

BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG l

NEW DELHI 110002

December 1993 Price Group 1

Methods of Chemical Analysis of Ferrous Metals Sectional Committee, MTD 2

FOREWORD

This Indian Standard ( Part 7 ) was adopted by the Bureau of Indian Standards, after the draft finalized by the Method5 of Chemical Analysis of Ferrous Metals Sectional Committee had been approved by the Metallurgical Engineering Division Council.

IS 15.59 : 1961 ‘Methods of Chemical Analysis of Ferroalloys’ covers the chemical analysis of different ferro alloys, namely, ferrosilicon, ferrochromium, ferromanganese and speigeleisen, silicomclnganese, ferromolybdenum, ferrophosphorus, ferrotitanium, ferrovanadium andferrotungsten. While reviewing this standard the Sectional Committee decided that a separate series for each ferro- alloy be prepared. Accordingly, IS 1559 in its various parts was published for the methods of chemical analysis of ferrosilicon.

The methods for chemical analysis of various constituents of forromolybdenum, ferrochromium and ferrotungsten are covered in a series of parts of IS 126 14, IS 13452 and IS 13840 respectively. The chemical analysis of ferrotitanium is covered in a series of parts of this standard. With the publication of these parts, the analysis of relevant constituent prescribed for ferromanganese in IS 1559 : 1967 will be superseded. This standard ( Part 3 ) covers the method for determination of phosphorus by volumetric ( alkalimetric) method. The other parts of this series are:

Part I Determination of silicon by gravimetric method

Part 2 Determination of manganese by the Vo!hard’s method

Part 4 Determination of total sulphur by direct combustion method

Part 5 Determination of total carbon

During this revision the method for determination of phosphorus by volumetric ( alkalimetric ) method has been updated.

In reporting the result of a test or analysis made in accordance with this standard, if the final value, observed or calculated, is to be rounded off, it shall be done in accordance with IS 2 : 1960 ‘Rules for rounding off numerical values ( revised)‘.

IS 13938 ( Part 3 ) : 1993

Indian

CHEMICAL ANALYSIS PART 3 DETERMINATION OF

Standard

OF FERROMANGANESE PHOSPHORUS BY VOLUMETRIC

( ALKALIMETRIC ) METHOD

1 SCOPE 5.2.5 Ammonium Molybdate Solution

This standard ( Part 3 ) describes the method for determination of phosphorus in the range UPto 0’50 percent in ferromanganese by_ volumetric ( alkahmetric ) method.

5.2.5.1 Weigh 50 g of ammonium molybdate in a beaker, add 200 ml of ammonium hydroxide, dissolve and keep it separately ( Solution A ).

2 REFERENCES

5.2.5.2 Mix 400 ml of nitric acid and 400 ml of wattr in 2-litre conical flask, cool and keep it sep Irately ( Solution B ).

The following Indian Standards are necessary adjuncts to this standard:

IS No.

264 : 1976

265 : 1993

1070 : 1992

Title

Nitric acid ( second revision )

Hydrochloric acid (fourth revision)

Reagent grade water ( third revision )

5.2.5.3 Add slowly Solution A to Solution B with contin(lous shaking and cooling. Now to the ammonium molybdate solution add about 0’1 g of ammonium phosphate and allow for settle- ment. Filter and use the solution for precipitation of phosphorus.

5.2.6 Standard Nitric Acid ( 0 07.5 N )

1472 : 1977 Methods of sampling ferroalloys Add 4 7 ml of nitric acid to one iitre of water for chemical composition (jirst and standardize against standard sodium revision ) carbonate solution.

3 SAMPLING 52.7 Standard Sodium Carbonate Solution ( 0’075 N !

The sample shall be drawn and prepared as per the method given in IS 1472 : 1977.

4 QUALITY OF REAGENTS

Weigh exactly 0’397 g of sodium carbonate pre- heated to 260” to 270°C for one hour and cool. Dissolve in distilled water and make up to the mark in 100 ml volumetric flask.

Unless specified otherwise, analytical grade reagents and distilled water ( see 1070 : 1992 ) shall be employed for the test.

5.2.8 Potassium Nitrate Wash Solution, 1 percent ( mlv )

5 DETERMINATION OF PHOSPHORUS Dissolve 1 g of potassium nitrate in 100 ml of water.

5.1 Outline of the Method 5.2.9 Nitric Acid Wash Solution ( 1 : 99 ) ( v/v)

After removal of silica by treatment with nitric acid and hydrochloric acid, phosphorus is pre- cipitated as phosphomolybdate by ammonium molybdate and estimated by the usual Alkali- metric Method.

5.2.10 Phenolphthalein

Dissolve 0’5 g of the reagent in 50 m! of alcohol and dilute with 50 ml of distilled water with constant stirring.

5.2 Reagents 5.3 Procedure

5.2.1 Nitric Acid, rd = 1’42 (Conforming to IS 264 : 1976 )

5.2.2 Hydrochloric Acid, rd = I‘ 16 ( Conforming to IS 265 : 1993

5.2.3 Ammonium Hydroxide, rd = 0’90

5.2.4 Sodium Hydroxide ( Approximately 0’075 N )

Dissolve 3 g of sodium hydroxide in one litre of carbonate free water.

5.3.1 Weigh accurately I g of the sample in a 500 ml beaker. Add to it about 30 ml of nitric acid. Cover the beaker with a watch glass and heat the contents on a hot plate till dissolution is complete. Add 200 ml of perchloric acid. Evaporate to dense white fumes or until manganese dioxide begins to precipitate. Redis- solve the mass with 40 ml of hydrochloric acid by warming and dilute with about 150 ml of hot water. Boil and allow to settle. Filter through a medium textured filter paper. Wash the ‘residue several times with hot water. Preserve the filtrate.

1

IS 13938 ( Part 3 ) : 1993

5.3.2 Ignite the residue in a platinum crucible and add 5 ml of hydrofluoric acid and 2 ml of perchloric acid. EVdpOrate to dense white fumes and add to the filtrate preserved under 5.3.1.

5.3.3 Evaporate the filtrate to 200 ml. Cool and transfer to a stoppered conical flask.

5.3.4 Add 2 ml of nitric acid and about 25 to 30 ml of ammonium molybdate solution at room temperature. Stopper the flask and shake vigorously for about 5 minutes to precipitate phosphorus as ammonium phosphomolybdate. Allow the precipitate to settle for I hour. Filter through a close textured filter paper containing small quantity of filter paper pulp. Wash the precipitate with potassium nitrate wash solution till 10 ml of the filtrate collected in a test tube gives pink colour with phenolphthalein by a drop of sodium hydroxide.

NOTE - Normally five washings are sufficient for the precipitate to be free from acid.

5.3.5 Transfer the precipitate to the original flask where the phosphorus was first precipitated. Add

known excess of sodium hydroxide ( 0’075 N ). Titrate the excess of sodium hydroxide with standard nitric acid ( 0’075 N ) by using phenol- phthalein as indicator.

5.3.6 Take a blank of sodium hydroxide used in the experiment and from the difference, calculate the percentage of phosphorus as given in 5.4.

5.4 Calculation

Phosphorus, percent by

where

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

k’s = volume in ml, of standard acid required in the experiment;

N = strength of acid used; and

m = mass in g, of the sample taken.

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