IS 1559-5: Chemical Analysis of Ferrosilicon, Part 5: Determination of Aluminium in Ferrosilicon (Aluminium 0.05 to 1.75 Percent)

8 Pages·2003·1 MB·English

by  Bureau of Indian Standards

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IS 1559-5 (2003): Chemical Analysis of Ferrosilicon, Part
5: Determination of Aluminium in Ferrosilicon (Aluminium
0.05 to 1.75 Percent) [MTD 5: Ferro Alloys]
“!ान $ एक न’ भारत का +नम-ण”
Satyanarayan Gangaram Pitroda
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“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता हहहहै””ै”
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IS 1559 (Part 5) :2003
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Indian Standard
CHEMICAL ANALYSIS OF FERROSILICON
PART 5 DETERMINATION OF ALUMINIUM IN FERROSILICON
(ALUMINNJM 0.05 TO 1.75 PERCENT)
(Second Revision )
ICS 77.100

0 BIS 2003
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

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Methods of Chemical Analysis of Ferrous Metals Sectional Committee, MTD 2
FOREWORD
This Indian Standard (Part 5) (Second Revision) 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, which was published in 1961, covered the chemical analysis of ferro alloys, namely ferrosilicon
ferrochromium, ferromanganese and speigeleisen silicomanganese, ferrovanadium ferromolybednum,
ferrophosphorous, ferrotitanium, and ferrotungsten. It was revised again in 1982 covering only ferrosilicon.
Method of analysis for other ferro alloys covered in separate standards. This part covers the determination of
aluminium. The other parts coveJ as follows.
Part 1 Determination of silicon
Part 2 Determination of carbon
Part 3 Determination of sulphur
Part 4 Determination of thosthorus
Part 6 Determination of calcium
Part 7 Determination of manganese
The revision of this standard has been undertaken on the basis of experience gained during the implementation
of thestandard by the manufacturers and testing laboratories. In this revised standard, major modifications areas
follows.
a) Scope of the method has been modified by lowering the limit for determination of aluminium from 0.40
to 0.05 percent (Range from 0.05 to 1.75 percent), and
b) Blank titration has been included in the procedure and formula for calculating aluminium percentage
has been changed.
In reporting the result of a test or analysis made in accordance with this standard, if the final value observed or
calculated, isto be rounded off, itshall be done in accordance with IS 2: 1960 ‘Rules for rounding off numerical

values (revised)’.
. ..
7
IS 1559 (Part 5) :2003
Indian Standard
CHEMICAL ANALYSIS OF FERROSILICON
PART 5 DETERMINATION OF ALUMINIUM IN FERROSILICON
(ALUMINIUM 0.05 to 1.75 PERCENT)
(Second Revision)
1SCOPE 5.2 Reagents
This standard (Part 5) covers the determination of 5.2.1 Hydrofluoric Acid — 40percent (v/v).
aluminium (0.05 to 1.75 percent) in ferrosilicon.
5.2.2 Cottcentrated Nitric Acid — rd = 1.42
(conforming to IS 264).
2 REFERENCES
5.2.3 Dilute Hydrochloric Acid — 1:1 (v/v).
The following standards are subject to revision and
parties to agreements based on this standard are 5.2.4 Concentrated Hydrochloric Acid — rd = 1.18
encouraged to investigate the possibility of applying (conforming to IS 265).
the most recent editions of the standards indicated
5.2.5 Sodium Hydroxide Solution — 25percent (m/v).
below.
5.2.6 Ammonium ChlorideSolution— 50percent (nv$).
IS No. Title
264:1976 Nitric acid (second revision) 5.2.7 Ammonium ChlorideSolution — 2percent (m/v).
265:1993 Hydrochloric acid (third revision) 5.2.8 Phenolphthalein Solution — 1 percent in
1070:1992 Reagent grade water (thirdrevision) alcohol (m/v).
1472:1977 Methods of sampling of ferroalloys
5.2.9 EDTA Solution (0.01M)—Dissolve3.7222 g
for determination of chemical
of EDTA disodium salt in 500 ml water and transfer
composition (jlrst revision)
into a 1litre volumetric flask, dilute upto the mark.
3 SAMPLING 5.2.10 Congo RedIndicator Paper — Take apinch of
congo red indicator and dissolve it in 50 ml rectified
It shall be drawn and prepared in accordance with
spirit. Cut the filter paper clippings into small pieces
IS 1472.

and dip them inside the solution. Take out the papers,

4 QUALITY OF REAGENTS dry them and use the paper as indicator.
Unless otherwise specified, pure chemicals and 5.2.11 Ammonium Hydroxide Solution —
50 percent (v/v).
distilled water (see IS 1070) shall be employed in the
tests. 5.2.12 Bufler Solution (pH = 5.3) — Dissolve 21.5 g
of sodium acetate in 300 ml water containing 2 ml of
NOTE — ‘Pure chemicals’ shall mean chemicals that do not
contain impurities which affect the results ofanalysis. glacial acetic acid and dilute to 1litre.
5 OUTLINE OF THE METHOD 5.2.13 Xylenol Orange Solution — 0.5 percent (w/v)
in water acidified with 2 drops of dilute hydrochloric
5.1 The sample is decomposed in hydrofluoric acid acid (1 : 1).
and nitric acid in aplatinum beaker. The excess acids
5.2.14 Zinc Acetate — Solid.
are removed by evaporation to a low bulk and fumed
with perchloric acid and extracted in water. Iron and 5.2.15 Zinc Acetate Solution (O.01 M) — Dissolve
aluminium are separated as Rutile Oxide (RZOJ. 2.1938 gzinc acetate (see 5.2.14) inwater containing
Aluminium forms soluble sodium aluminate with 0.5 ml of glacial acetic acid and 20 ml of buffer
sodium hydroxide and is separated from ferric (see 5.2.12). Transfer to 1 litre volumetric flask and
hydroxide by filtration through adry filter paper. From dilute up to the mark. Standardize the solution against
the filtrate alutninium is determined by 25 ml standard aluminium solution (see 5.2.17)
complex ometric titration with EDTA using following the procedure (see 5.3.6) and establish
orangexyienol as indicator. aluminium in g/ml of zinc acetate solution.

1
6 ,-
IS 1559 (Part 5) :2003
5.2.16 Standard Alwniniurn Stock Solution (0.05 M) and make up the volume to the mark with distilled
— Wash a portion of aluminium foil purity 99.99 water. Shake thoroughly and keep for sometime to
percent in absolute alcohol and dry in a desiccator. settle the precipitate. Filter through dry filter paper and
Weigh 0.6745 g and place in a 500 ml beaker collect the filtrate in a dry beaker.
containing 150 ml water and 50 ml of concentrated
5.3.6 Pipette out an aliquot (100 ml) of the solution
hydrochloric acid. Heat the solution to dissolve the
prepared under 5.3.5 into a 250 ml conical flask. Add
metal. Cool, transfer in a500 ml volumetric flask and
about 25 ml of EDTA solution (0.01 M) for high
dilute to the mark.
aluminium ferrosilicon or 10 ml EDTA solution
5.2.17 StandardAlunliniutn WorkingSolution (0.01M) (0.01 M) for low aluminium ferrosilicon and 1 to 2
— Pipette out 50 ml of 0.05 M aluminium solution and pieces of congo red indicator paper. Neutralize the
transfer to a 250 ml volumetric flask and dilute to the solution with dilute hydrochloric acid (1: I v/v), till the
mark (1ml of this solution= 0.0002698 g Al). paper turns to blue. Then add 20 ml of buffer solution
OH= 5.3), boil the solution for 10 min. Cool to room
5.2.18 Ammonium Fluoride Solution —
temperature, add 5 to 6 drops of xylenol orange
10 percent (w/v).
solution and back titrate the excess EDTA with zinc
acetate solution to ajust pink end point. Add 10ml of
5.3 Procedure
ammonium fluoride solution and boil the solution again.
5.3.1 Weigh accurately 1gofwell agated and predried for 10 rein, cool, add 10 ml of buffer and back titrate
sample (at 11O“C) into a 250 ml platinum dish. Add the released EDTA with zinc acetate solution tojust a
about 10ml ofhydrofluoric acid and concentrated nitric pink end point. Let the titrate volume of 2nd titrate be
acid dropwise till the vigorous reaction subsides. Aml of zinc acetate.
Evaporate the solution to a low bulk. Add 10 ml of
5.3.7 Blank
perchloric acid and fume itinhot plate till the copious
white fumes come out for about 5 min.
Conduct blank experiment following the procedure and
using the same amount of reagent and titrate the
5.3.2 Cool, dilute with distilled water and dissolve the
released EDTA with zinc acetate solution to ajust pink
salt by heating the solution on a hot plate.
end point. Let this volume be B ml.
5.3.3 Neutralize the hot solution obtained from 5.3.2
with ammonium hydroxide. Filter through medium size 5.3.8 Calculation
paper filter No. 40. Wash the precipitate 2 or 3 times
(A-B) XCX5X,00
with ammonium chloride solution. Dissolve itindilute
Aluminium, percent=
hydrochloric acid (1 :1 v/v) in a separate beaker and M
heat to boiling.
where

5.3.4 Take 75 to 80 ml of sodium hydroxide solution
A = zinc acetate required for 2nd titration in
into a 500 ml polythene beaker and heat on a water
experiment
bath.
B = zinc acetate required, in ml, for 2nd
5.3.5 Add the hot solution obtained in 5.3.3 into the titration in the blank experiment;
polythene beaker containing hot sodium hydroxide
C = equivalent aluminium, in g/ml of zinc
solution (see 5.3.4) with constant shaking. Heat the
acetate solution; and
mixture for 20 min on the steam bath and then cool to
M = mass, in g, of sample taken.
room tenlperature.Transfer toa500 mlvolumetric flask

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needed; if the review indicates that changes are needed, it is taken up for revision. Users of Indian Standards
should ascertain that they are in possession of the latest amendments or edition by referring to the latest issue of
‘BIS Catalogue’ and ‘Standards: Monthly Additions’.
This Indian Standard has been developed from Doc :No. MTD 2 (4273).
Amendments Issued Since Publication
Amend No. Date of Issue Text Affected
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