IS 14529: Chemical Analysis of Ferrosilicon-Magnesium Alloy

2004·1.1 MB·English

by  Bureau of Indian Standards

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IS 14529 (2004): Chemical Analysis of
Ferrosilicon-Magnesium Alloy [MTD 5: Ferro Alloys]
“!ान $ एक न’ भारत का +नम-ण”
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IS 14529:2004
[Superseding IS 14529 (Part 2)]

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Indian Standard
CHEMICAL ANALYSIS OF
FERROSILICON-MAGNESIUM ALLOY
(First Revision)
lCS 77.100

G BIS 2004
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELH1 110002

Oc!ober 2004 Price Group 2
Ferro Alloys Sectional Committee, MTD 5
FORE WORD
This Indian Standard (First Revision) was adopted by the Bureau of Indian Standards, after the draft finalized by
the Ferro Alloys SectionaI Committee had been approved by the Metallurgical Engineering Division Council.
The Committee felt to formulate a standard on the chemical analysis of ferrosilicon-magnesium alloy in two
parts that is, Part 1covering determination of silicon by gravimetric method and Part 2covering determination of
calcium and magnesium by EDTA method.
While finalizing Part 1of IS 14529 ‘Chemical analysis of ferrosilicon-magnesium alloy: Part 1Determination of
silicon by gravimetric method’, the Committee decided to have a single standard by merging Part 1into Part 2
of 1S14529 ‘Chemical analysis offerrosilicon-magnesium alloy: Part 2Determination ofcalcium and magnesium’,
which was first published in 1998.
This standard supersedes 1S 14529 (Part 2) :1998,
For the purpose of deciding whether a particular requirement of this standard is complied with, the final
value, observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance
with IS 2 : 1960 ‘Rules for rounding off numerical values (revised)’. The number of significant places retained
in the rounded off value should be the same as that of the specified value in this standard.
IS 14529:2004
Indian Standard
CHEMICAL ANALYSIS OF
FERROSILICON-MAGNESIUM ALLOY
(First Revision)
YSCOPE and potassium cyanide to mask residual traces of iron,
copper, nickel, manganese and aluminum that may be
This standard describes the method for determination
present. Calcium is titrated with disodium (ethylene
of calcium inthe range 0.25 to 3.0 percent, magnesium
dinitrilo) tetra acetate (EDTA) atpH 12. Magnesium
in the range from 2 to 25 percent by EDTA method
plus calcium is titrated with EDTA at pH 10.0
and silicon inthe range 45 to 75 percent by gravimetric
and magnesium concentration is calculated by
method in ferrosilicon magnesium alloy.
correcting for the volume of EDTA required to titrate
2 REFERENCES the calcium.
The standards listed below contain provisions, which 5.2 Reagents
through reference in this text, constitute provisions of
5.2.1 Ammonium Chloride BuferSolution (pH 10.0) —
this standard. At the time of publication, the editions
Dissolve 60 g of amonium chloride in 200 ml water,
indicated were valid. All standards are subject to
add 570 ml of ammonium hydroxide and dilute
revision and parties to agreement based onthis standard
to 1Iitre.
are encouraged to investigate the possibility ofapplying
the most recent editions of the standards indicated 5.2.2 Standard Calcium Solution (1 ml= 0.2002 mg
below: Ca) — Dissolve 0.500 g of dried calcium carbonate
(purity 99.9 percent, &fin) in 100 ml of dilute
[S No. Title
hydrochloric acid (5 percent). Boil for 1rein, cool and
264:1976 Nitric acid (second revision)
transfer to a 1litre volumetric flask and mix.
265:1993 Hydrochloric acid ~ourth revision)
1070:1992 Reagent grade water (third revision) 5.2.3 Disodium Ethytenedinitrilo — Tetra Acetate
1472:1977 Methods of sampling of ferroalloys Dihydrate (EDTA] Standard Solution (0.005 W —
for chemical composition (first Dissolve 1.8613 gofdisodium (ethylenedinitri lo)tetra
revision) acetate dehydrate inwater, transfer to 11itre volumetric
flask, dilute to volume and mix well.
3 SAMPLING
5.2.3.1 Transfer 25 ml of calcium solution (see 5.2.2)
The sample shall be drawn and prepared as per the to a 250 ml beaker, add 1ml of magnesium chloride
method given in IS 1472.
solution and 100 ml water and proceed as per the
procedure specified in 5.2.3.2.
4 QUALITY OF REAGENTS
5.2.3.2 Calculate the calcium equivalent of EDTA
Unless specified otherwise analytical grade reagents
solution as follows:
and reagent grade water (see IS 1070) shall be
employed for the test.
Calcium equivalent (mg/ml) C = ~
5 DETERMINATION OF CALCIUM AND
MAGNESIUM BY EDTA (TITRIMETRIC where
METHOD)
A = milligrams, of calcium;
5,1 outline of the Method
B = volume, inml, of EDTA solution required to
After dissolution ofthe sample innitric and hydrofluoric titrate calcium solution; and
acids, an ammonium hydroxide precipitation is made
C = calcium equivalent.
toseparate other elements from calcium andmagnesium.
Caiciunl and magnesium,plus calcium are titrated in 5.2.3.3 Calculate the magnesium equivalent of the
separate aiiquot portions after adding triethanolamine solution as follows:
IS 14529:2004
Magnesium equivalent (mg/ml) = C x 0.6068 5.3.3 Filter about 200 ml of above solution (see 5.3.2)
through a medium textured filter paper into a dry
where
beaker. Transfer 50 ml of this solution to another
C = calcium equivalent (see 5.2.3.2). 2.S0ml beaker.
5.2.4 Erichrome Black TIndicator Solution (6 g/1 oj 5.3.4 Titration of Calcium
methanol) -– Dissolve 0.3 g of Erichrome Black T
Add 5 ml of triethanolamine solution stir and
and 1 g of sodium borate decahydrate in 50 ml of
immediately add 5 ml of KOH buffer solution. Add
methanol.
100 mg of hydroxyl napthol blue indicator mixture.
NOTE–– (Jsethe solution within 8hofpreparation. Titrate with EDTA solution (().005 M) to the
disappearance of last trace of the red colour.
5.2.5 Hydroxy Napthol Blue Mixture — Mix 1.0 g of
indicator with 100 g sodium chloride and mix 5.3.5 Titration of Calcium and Magnesium
thoroughly.
Using a pipette, transfer a second aliquot portion of
5.2.6 Magnesium Chloride Solution (2.5 g/m[) — the filtered solution from 5.3.3 to a 250 ml beaker in
Dissolve 0.25 g of magnesium chloride hexahydrate accordance with the following:
in 50 ml water and dilute to 100 ml.
Magnesium, Sample Aliquotfor Magnesium
5.2.7 Potassium Cyanide Solution (50 g/1) — Dissolve Percent Weight Determination
2 g of potassium hydroxide in water and add 5 g of g ml
potassium cyanide to it, dilute to 100 ml and transfer
2.0 to 5.0 1.0 50
to a plastic bottle.
5.0 to 12.0 1.0 25
NOTE — Caution — The preparation, storage and use of
potassium cyaniderequirecareandattention.Avoidinhalation
5.3.6 Add 5 ml of triethanolamine solution stir and
of fomes aod exposure of the skin to the chemical and its
immediately add 10ml of ammonium chloride buffer
solutions. Works inawellventilated hood.
solution. Add 5ml of potassium cyanide solution (see
5.2.8 Potassium Hydroxide Bufler Solution (pH 12.5)
Note) and 3to 5 drops of erichrome black T solution.
— Dissolve 531 g of potassium hydroxide in water,
Titrate with EDTA solution (0.005 M) to the
add 50 g of potassium cyanide and dilute to 1 Iitre.
disappearance of last trace of the red colour.
Store the solution in a plastic bottle.
NOTE—Ingoingthroughtheendpoint, thecolour changes
5.2.9 Triethanolomine Solution (200 mill) — Dilute fromredtobluetobluegreen.
20 ml of triethanolamine to 100 ml of water.
5.4 Calculations
5.3 Procedure
5.4.1 Calculate the percentage of calcium as follows:
5.3.1 Weigh accurately 1.0gof samp l e and transfer to
AxB
adry TFE — fluorocarbon beaker. Add 10ml of nitric
Calcium, percent by mass = ~ x100
acid. Cautiously add 10 ml of hydrofluoric acid and
heat gently till the sample isdissolved. Wash the sides
where
of the beaker with a fine stream of water. Add 20 ml
of perch loric acid, place on ahot plate at atemperature A= volume in ml, of EDTA solution required to
not exceeding 3000C and evaporate to dense fumes of titrate the calcium (see 5.3.4);
perch loric acid. Cool, add 10ml of dilute hydrochloric
B = calcium equivalent, in mg/ml, of the EDTA
acid (1:1) and heat to dissolve the salts. Transfer to a
solution (see 5.2.3.2); and
600 ml beaker and evaporate to moderate dryness on a
hot plate. Place on aburner and evaporate to complete C = mass, inmg, ofthe sample represented by the
dryness. Add 20 ml of dilute hydrochloric acid (1:1), final aliquot.
wash the sides of the beaker with atine stream of water
5.4.2 Calculate the percentage of magnesium as
and heat to dissolve the salts.
follows:
5.3.2 Add 200 ml of water and 5 g of ammonium
D-+ xF’x1OO
chloride. Boil and cool. Add ammonium hydroxide Magnesium, percent by mass= ()
until the iron begins to precipitate and continue addition G
where
dropwise till the precipitation is completed. Cool to
room temperature, transfer to a 500 ml volumetric D =volume, in ml, of EDTA solution required to
flask, dilute to volume, and mix. Let itstand for 1h to titrate magnesium and calcium (see 5.3.6);
allow the precipitate to settle.

2
IS 14529:2004
A= volume, in ml, of EDTA solution required to tothecrucibletostirupanyunattached particles ofalloyon
thebottomorsides.Thecrucibleandcontentsbeingmaintained
titrate the calcium (see 5.3.4);
at a low red heat. Just before completion of fusion, the
E= 50 divided by ml of aliquot taken for titration temperature isincreasedtobrightrednessforaminute.
of magnesium and calcium (see 5.3.5);
6.3.2 When the crucible has cooled for the molten mass
F = magnesium equivalent, in mg/ml, of EDTA
to solidifi, slowly drop the crucible with its solidified
solution (see 5.2.3.3); and
melt in 50 ml of cold water in a 500 ml PTFE beaker
G = mass, inmg, of sample represented inthe final
and cover the beaker immediately by PTFE cover glass.
aliquot.
When the reaction has subsided, take out the crucible
and the lid and wash them thoroughly, first with warm
6 DETERMINATION OF SILICON BY
dilute hydrochloric acid (10 percent,v/v) and then
GRAVIMETRIC METHOD
with water, collecting the washings in the same
6.1 Outline of the Method PTFE beaker. Acidify the extract by concentrated
hydrochloric acid and transfer the solution to a500 ml
Sample isdecomposed by fusion with sodium peroxide
beaker.
and sodium carbonate and silica is separated by
dehydration, from the acidified extract. Any silica 6.3.3 Insert glass rod into the solution, add 40 ml (or
remaining inthe filtrate isprecipitated alongwith ferric even more if necessary) sulphuric acid (1:1) and
hydroxide by precipitation with ammonium hydroxide evaporate to fumes. Allow to cool and add 200 ml of
and then dehydrated by fuming with perchloric acid. dilute hydrochloric acid (1:9). Heat until salts are in
After ignition, the combined silica residues are treated solution and filter through apaper pulp pad. Wash with
with hydrofluoric acid and silicon determined by dilute hydrochloric acid (5:95) and finally with hot
volatilization as silicon tetrafluoride. water till itisfree from chlorides. Transfer the residue
to a platinum crucible and preserve.
6.2 Reagents
6.3,4 Add tothe filtrate and washings reserved in6.3.3,
6.2.1 Sodium Peroxide, solid. 5g of ammonium chloride, heat nearly to boiling and
precipitate with ammonia solution (1: 1). Heat to
6.2.2 Sodium Carbonate, anhydrous.
boiling, filter through a medium textured filter paper
6.2.3 Dilute Hydrochloric Acid, 2:98, 1:10,5:95 (v/v). and wash with hot water. Transfer the precipitate and
paper to the original beaker, add 30 ml of concentrated
6.2.4 Concentrated Hydrochloric Acid, r.d = 1.16
nitric acid and 10ml of dilute sulphuric acid (1:1) and
(see 1S265).
evaporate to fumes. Cool and add 20 ml of concentrated
6.2.5 Ammonium Chloride, solid. hydrochloric acid, 100 ml of water and heat until the
6.2.6 Ammonia Solution, 50 perce nt (v/v). salts are in solution. Filter through medium textured
filter paper, wash as before and transfer the pad to the

6.2.7 ConcentratedNitric Acid, r.d = 1.42 (see 1S264). platinum crucible containing the first silica residue.
6.2.8 Perch[oric Acid, 60 percent (v/v). Ignite at low temperature and finally at 1 100”C to
1 150”C to constant mass (A) in a muffle furnace.
6.2.9 Dilu~c Sulphuric Acid, 1:1 (v/ v).
6.3.5 Moisten the residue with 1ml of dilute sr.dphuric
6.2.10 Hydrojluoric Acid, 40 percent (v/v). acid (1:4) and add 10ml ofhydrofluoric acid, evaporate
to dryness, ignite at 1 100°C to 1 150°C, cool and
6.3 Procedure
weigh (B).
6.3.1 Weigh accurately 0.25 g of finely ground dried
6.3.6 Carry out a blank determination following the
sample into a 25/30 ml nickel crucible containing 5 g
same procedure as specified in6.3.1 to 6.3.5 and using
of sodium peroxide and 2g of anhydrous sodium
same amount of all the reagents and correct the final
carbonate. Mix well and cover with 2 g of sodium
result for the blank value, if any.
peroxide. Cover the crucible and fuse the contents
carefully on the flame of a bunsen burner. Cover the 6.4 Calculations
crucible and allow itto cool.
(A- B)x 46.72
N()I’m Silicon, percent by mass=
c
1 Ihe fusionisbestaccompaniedbyholdingthecruciblewith
where
apairoftongs andslowly revolving itaroundtheouteredge
otfhe tlalmeuntilthecontentshavemelteddownquietly.Care A = mass, in g, of silica before hydroflurization;
hcing taken not to raise the temperature so rapidly so asto
B = mass, ing,of silica after hydroflurization; and
causespattering.
2 Whenthemassismolten, aslightrotarymotionisimparted C = mass, in g, of sample taken.

3
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This Indian Standard has been developed from Dot: No. MTD 5 (4568).
Amendments Issued Since Publication
Amend No. Date of Issue Text Affected
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