IS 13452-1: Chemical Analysis of Ferrochromium, Part 1: Determination of silicon in high carbon ferrochromium by gravimetiric method

9 Pages·1992·1.1 MB·English

by  Bureau of Indian Standards

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IS 13452-1 (1992): Chemical Analysis of Ferrochromium, Part
1: Determination of silicon in high carbon ferrochromium by
gravimetiric method [MTD 5: Ferro Alloys]
“!ान $ एक न’ भारत का +नम-ण”
Satyanarayan Gangaram Pitroda
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Indian Standard
CHEMICALANALYSISOFFERROCHROMIUM
PART 1 DETERMINATION OF SILICON IN HIGH CARBON FERROCHROMIUM
BY GRAWMETRIC METHOD
UDC 891-62*51*966 : 12*345 [ 546.28 ]

@ SIB 1992
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
WEN IH>TED 110002
’)ruf 1992 ecirP puorG 1
Methods of Chemical Analysis of Ferrous Metals Sectional Committee, MTD 2
FOREWORD
This Indian Standard ( Part 1 ) 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 ferro-
alloys, namely, ferrosilicon, ferrochromium, ferromanganese and speigeleisen, silicomanganese, ferro-
molybdenum, ferrophosphorus, ferrotitanium, ferrovanadium and ferrotungesten. While reviewing this
standard, the Sectional Committee had decided that a separate ‘series for each ferroalloy be prepared.
Accordingly, IS 1559 in its various parts was published for the chemical analysis of ferrosilicon.
The chemical analysis of ferromolybdenum is covered in a series of parts of IS1 2614. The chemical analy-
sis of ferrochromium is covered in a series of parts of this standard. With the publication of these parts the
analysis of relevant constitueut prescribed for ferrochromium in IS 1559 : 1961 will be superseded, This
part covers the method for determination of silicon in high carbon ferrochromium. The other parts are:
Part 2 Determination of silicon in low carbon ferrochromium
Part 3 Determination of phosphorus in low carbon ferrochromium
Part 4 Determination of t o tal sulphur in low and high carbon ferrochromium
Part 5 Determination of chro m ium in high carbon ferrochromium
Part 6 Determination of chromium in low carbon ferrochromium
Part 7 Determination of nitrogen in high and low carbon ferrochromium
Part 8 Determination of carbon ( total ) in low and high carbon ferrochromium
In this revision the determination of silicon in high carbon ferrochromium 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 cloue in accordance with IS 2 : 0691 selnR‘ rof
rounding off numerical values ( rsziwd ) ‘.
IS 13452 ( Part 1 ) : 1992
Indian Standard
CHEMICAL ANALYSIS OF FERROCHROMIUM
PART 1 DETERMlNATlON OF SILICON IN HIGH CARBON FERROCHROMlUM
BY GRAVIMETRIC METHOD
1 SCOPE sodium peroxide and 2 g of anhydrous sodirun
carbonate. Mix well and cover with 2 g of sodium
This standard ( Part 1 ) describes the method for peroxide. Fuse the content carefully over the dull
determination of silicon in high carbon ferro- flame of Meeker burner or in a muffle furnace
chromium ( containing carbon above one at a temperature 5509 to 600%. Care should be
percent ). taken not to raise the temperature rapidly as to
cause spattering. When the mass is molten, a
2 REFERENCES
slight rotary motion is imparted to the crucible
The following Indian Standards are necessary to stir up any unattacked particles of alloy on t.hc
adjuncts to this standard: bottom or sides. The temperature is to be
increased to a bright redness for a minute just
IJ'JfO. ‘Title before completion of fusion. If followed carefully,
265 : 1%: Hydrochloric acid ( third revision ) a very quite fusion without any spattering will
result. After the crucible has cooled, slowly drop
1070 : 1977 Water for general laborator)l use
the crucible with its solidified melt in 50 ml ob’
( second revision )
cold water in a 500 ml polytetrafluroethylene
1472 : 19i7 Methods of sampling of ferroalloys ( PTFE ) beaker and cover with PTFE cove-~-
for determination of chemical glass. When the reaction has subsided take out
composition ( jr9 revision ) crucible and wash with warm hydrochloric acid
( 10 percent ) and then with water collecting all
3 SAMPLING
the washings in the same PTFE beaker.
‘The sample shall be drawn and prepared in
accordance with IS 1472 : 1977. 5.3.2 Acidify the extract ( 5.3.1 ) by addir.g
50 ml of hydrochloric acid and then transfer
4 QUALITY OF REAGENTS the solution to a 500 ml glass beaker, evaporate
to almost syrupy stage and add 30 ml of
Unless specified otherwise, analytical grade
perchloric acid and keep the beaker on hot
reagents and distilled water ( .rec IS 1070 : 7791 )
plate until white perchloric acid fumes are
shall 1~ employed for the test.
refluxed for 15 minutes.
5 DETERMINATION OF SIL ICON NOTE - The dehydration of the silica in high carbon

ferrochromium can be carried out even by sulphuric
5.1 Outline of the Method acid, but the difficulties are frequently encountered drw
to the insolubility of basic chromic salts due to thl:
The sample is decomposed by fusion wit11 sodium presence of high chromium content of the alloy. By
peroxide and silicic acid dehydrated from the fuming with perchloric acid for dehydration, siht tros
acidified txtract by fuming with perchloric acid uf difficulty will not occur as perchloratcs are easily
and finally estimated gravimetrically. soluble even in cold water.
5.3.3 Cool solution ( 5.3.2 ) and add 20 ml ot’
5.2 Reagents
hydrochloric acid ( 50 percent ) and dilute with
5.2.1 Sodium Peroxide, solid ( yellow granular ). distilled water. Boil, cool and filter the silica on
an ashless medium textured filter paper placecl on
5.2.2 Sodirrm ,elnnobrnC solid, the fluted glass funnel. Rinse the beaker with
warm water using bobby and transfer the content
5.2.3 H~d~~cl~Loric Acid, rd - I. 16 ( conr‘orming
to the filter paper. Wash with warm hydrochloric
to IS 26.5 : 1987 ).
acid. Then finally wash several times with hot.
5.2.4 Pcrridoric Acid, 60 .tlrecrcp water till it is free from chloride.
5.2.5 I@rlr@oric Acid, 40 prrc:ent. NOTE - Check the solution I;r precipitation ,rk
chloride by silver nitrate solution ( 10 percent ).
5.2.6 Dilute Hydrochloric Acid, 2 percent ( U/V) .
5.3.4 Transfer the residue on ( 5.3.3 ) along with
5.2.7 Dilufe Suljhric~ Acid, 50 percent ( U/V ). the filter paper to a platinum crucible. Evaporate
to dryness and ignite at temperature of 1 ,o()“c
3.3 Procedure
ot a constant mass. Allow to cool in a desiccator,
and weigh the cruciblf* containin< ilrlpl”~‘-
silrca (A).
1
3.51 3452( Part 1 ) t 1992
5.3.5 Moisten the impure silica with few drops of 5.4 Calculation
water and add about 2 or 3 drops of dilute sul-
phuric acid ( 50 percent ). Add about 5 ml of Silicon, percent
[(A-B))--,1 x46.74
hydrofluoric acid -and evaporate to dryness until by mass = --_____-
D
fumes cease to evolve. Ignite in a muffle furnace
at 1 100°C to a constant mass. Allow to cool in a where
desiccator and weigh the crucible (U) . A = mass in g, of crucible before hydrofluori-
zation,
5.3.6 Blank
B - mass in g, of crucible after hydrofluori-
Carry out a blank determination following the zation
procedure specified in 5.3.1 to 5.3.5 and using
C = mass in g, of silica from the blank, and
same amount of ail reagents. Correct the final
results for the blank value, if any (C). D = mass in g, of sample taken.

2
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