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IS 13840-2 (1993): Chemical analysis of ferro titanium,Part 2: Determination of silicon by gravimetric method [MTD5: Ferro Alloys]

IS 13840( Part2):1993

Indian Standard

CHEMICAL ANALYSIS OF FERROTITANIUM PART 2 DETERMINATION OF SILlCON BY GRAVIMETRIC METHOD

UDC 669’15’782-198 : 543’21 [ 546’28 ]

c

@ BIS 1993

BUREAU 0% INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MA,RO;

NEW DELI-II 110002

October 1993 Price Group 1

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

FOREWORD

This Indian Standard ( Part 2 ) was adopted by the Bureau of Indian Standards, after the draft finalized by the Methods of Chemical Analysis of Ferrous Metals Sectional Committee had been approved by the Metallurgical Engineering Division Council.

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

The methods of chemical analysis of various constituents of ferromolybdenum and ferrochromium are covered in a series of parts of IS 12614 and IS 13452 respectively. ferrotitanium is covered in a series of parts of this standard.

The chemical analysis of With the publication of these parts

the analysis of relevant constituent prescribed for ferrotitanium in IS 1559 : 1967 will be superseded. This part covers the method for determination of silicon by the gravimetric method. The other parts of this series are:

Part 1 Determination of carbon by the direct combustion gravimetric m,ethod

Part 3 Determination of titanium by the cupferron ( gravimetric ) method

Part 4 Determination of aluminium

Part 5 Determination of sulphur

During this revision the method for determination of silicon by the gravimetric 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 13840 ( Part 2 ) : 1993.

Indian Standard

CHEMICAL ANALYSIS OF FERROTITANIUM

PART 2 DETERMINATION OF SILICON BY GRAVIMETRIC METHOD

1 SCOPE

This standard ( Part 2 ) describes the method for determination of silicon up to 25 percent in ferrotitanium by gravimetric method.

2 REFERENCES

The following Indian Standards are necessary adjuncts to this standard:

IS No. Title

1070 : 1992 Laboratory ~grade water ( third revision )

1472 : 1977 Methods of sampling of ferro- alloys for chemical composition (first revision )

3 SAMPLING

Samples shall be drawn and prepared in accor- dance with IS 1472 : 1977.

4 QUALITY OF REAGENTS

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

5 DETERMINATION OF SILICON

5.1 Outline of the Method

The sample is decomposed by fusion with sodium peroxide. Silica is separated by dehydra- tion from the acidified extract after addition of oxalic acid and finally determined gravimetri- tally.

5.2 Reagents

5.2.1 Sodium Peroxide, solid.

5.2.2 Oxalic Acid Solution ( 100 g/l )

Dissolve 100 g of oxalic acid in water and dilute to one litre.

5.2.3 Hydrojuoric Acid, 40 percent.

52.4 Dilute Sulphuric Acid, 1 : 1, 1 : 200 ( V/V ).

5.3 Procedure

5.3.1 Weigh 0’500 g of finely ground dried sample for silicon content up to 15 percent and 0’25 g of sample for silicon above 25 percent

range, into a nickel crucible containing 4 to 8 g of sodium peroxide. Mix well. Fuse the content carefully over the dull flame of Meeker burner or in a muffle furnace at a temperature of 700°C to 800°C. Care should be taken not to raise the temperature rapidly, as to cause spattering. When the mass is molten, a slight rotary motion is imparted to the crucible, to stir up any unattacked particles of alloy, on the bottom or sides.

The temperature is to be increased to a bright redness for a minute just before completion of fusion. If followed carefully a very quite fusion without any spattering will result. When the crucible has cooled and the fusion has solidified, slowly drop the crucible’In 50 ml of cold water in a 500 ml polytetrafluoroethylene ( PTFE ) beaker and cover. When the reaction has subsided, take out the crucible and wash with dilute sulphuric acid ( 1 : 1 ) and then with water, collecting all the washings in the same PTFE beaker.

5.3.2 Neutralize the extract ( 5.3.1 ) with dilute sulphuric acid ( 1 : 1 ) and add 50 ml of dilute sulphuric acid ( 1 : 1 ) and then transfer the solution to 500 ml glass beaker. Add 50 ml of oxalic acid solution and evaporate slowly to” fumes. Heat to dense white fumes and continue the fuming for 3 to 5 minutes. Cool, add 200 ml of warm water and heatto dissolve sulphates. Filter through medium textured filter paper and wash at least 20 times with hot dilute sulphuric acid ( 1 : 200 ) and finally with hot water.

5.3.3 Transfer the residues along with the filter paper to a platinum crucible. Heat to dryness. Carefully char the filter paper and finally ignite at 1 100°C to constant mass. Allow to cool in a desiccator and weigh the crucible containing impure silica ( A ).

5.3.4 Moisten the impure silica with few drops of water and add about 2 or 3 drops of sulphuric acid. Add about 5 ml of hydrofluoric acid and evaporate to dryness until fumes cease to evolve. Ignite in a muffle furnace at 1 100°C to a constant mass. Allow to cool in a desiccator and weigh the crucible ( B ).

5.3.5 Blank

Carry out a blank determination following the procedure specified in 5.3.1 to 5.3.4 and using same amount of all reagents. Correct the finat results for the blank value, if any ( C ).

I

BS 13840 ( Part 2 ) : 1993

5.4 Calculation

;;i;a;‘spercent = [ ( A - B ) - C] x 46’74 D

where A = mass in g, of crucible before

hydrofluorization;

B = mass in g, of crucible after hydrofluorization;

C = mass in g, of silica from the blank; and

D = mass in g, of sample taken.

c

2

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c

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Dot : No. MTD 2 ( 3793 )

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