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IS 13452-5 (2003): Chemical Analysis of Ferrochromium, Part

5: Determination of Chromium in High Carbon
Ferrochromium/Chargechrome by Dichromate Titration [MTD 5:
Ferro Alloys]

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 - .- . . .. . . .
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IS 13452 (Part 5) :2003

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Indian Standard
CHEMICAL ANALYSIS OF FERROCHROMIUM
PART 5 DETERMINATION OF CHROMIUM IN HIGH CARBON
FERROCHROMIUM/CHARGECHROME BY DICHROMATETITRATION

(First Revision )

Ics 77.100

0 BIS 2003

BUREAU OF INDIAN STANDARDS

MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

.4prii 2003 Price Group 1

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

FOREWORD
This Indian Standard (Part 5) (First 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.
This Standard (Part 5) covers the method for determination of chromium in high carbon ferrochromium/
chargechrome by Bichromate titration, the other parts in this series are:
(Part 1): 1992 Determination of silicon in high carbon ferrochromium by gravimetric method
(Part 2): 1992 Determination of silicon in low carbon ferrochromium by gravimetric method
(Part 3): 1992 Determination of phosphorus in low carbon ferrochromium by gravimetric method
(Part 4): 1992 Determination of total sulphur in low carbon and high carbon ferrochromium by direct
combusion method
(Part 6) :1997 Determination of chromium in low carbon ferrochromium
(Part 7): 2003 Determination of phosphorus in ferrochromium/chargechrome by alkalimetric method
In this revision, major modifications are as follows:
a) Scope of the method has been modified by lowering the limit for determination of chromium from 60 to
50 percent (Range from 50 to 70 percent).
b) Procedure has been modified by titrating the excess ferrous ammonium sulphate by standard potassium
bichromate solution instead of standard potassium permanganate solution.
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 13452 (Part 5): 2003

Indian Standard
CHEMICAL ANALYSIS OF FERROCHROMIUM
PART 5 DETERMINATION OF CHROMIUM IN HIGH CARBON
FERROCHROMIUWCHARGECHROME BY DICHROMATETITRATION

(First Revision )

1 SCOPE 5.2 Reagents

This standard (Part 5) describes the method for 5.2.1 Sodium Peroxide, solid.
determination of chromium in the range from 50 to
5.2.2 Dilute Sulphuric Acid, 5 percent (v/v),
70 percent (containing carbon above 1 percent).
20 percent (v/v).
2 REFERENCES 5.2.3 Ammonium Persulphate, solid.
The standards listed below contain provisions which 5.2.4 Silver Nitrate Solution, 1 percent (w/v).
through reference in this text, constitute provisions of
this standard. At the time of publication, the editions 5.2.5 Phosphoric Acid, rd = 1.75 or 88 percent.
indicated were valid. All standards are subject to 5.2.6 Potassium Permanganate Solution, 25 gll.
revision and parties to agreements based on this
5.2.7 Dilute Hydrochloric Acid, 1:1.
standard are encouraged to investigate the possibility
of applying the most recent editions of the standards 5.2.8 Ferrous Ammonium Sulphate Solution, 0.1 N.
indicated below:
5.2.8.1 Dissolve 39.2 g of pure ferrous ammonium
IS No. Title sulphate FeSOJNHJ2 SOd.6H20 in 500 ml of dilute
266:1993 Sulphuric acid (third revision) sulphuric acid (5 percent) in a 1-litre volumetric flask
1070:1992 Reagent grade water (third revision) and make up to the mark with dilute sulphuric acid
1472:1977 Methods of sampling of ferroalloys (5: 95).
for determination of chemical
5.2.9 Standard Potassium Bichromate Solution, 0.1 N.
composition (first revision)
5.2.9.1 Dry potassium bichromate in an oven at 105 to
3 SAMPLING 110”C for one and a half hours, cool in a desiccator.
The sample shall be drawn and prepared in accordance Weigh exactly 4.903 5g. Dissolve in water and transfer
with IS 1472. to 1-litre volumetric flask, dilute volume and mix.
5.2.10 Sodium Diphenylamine Sulphonate Indicator
4 QUALITY OF REAGENTS Solution, 0.2 percent (m/v).
Unless specified otherwise analytical grade reagents 5.2.10.1 Dissolve 0.2 g of sodium diphenylamine
and distilled water (see IS 1070) shall be employed sulphonate in 100 ml hot distilled water.
for the test.
5.2.11 Sodium Chloride Solution, 10 percent (w/v).
5 DETERMINATION OF CHROMIUM
5.2.12 Concentrated Sulphuric Acid, rd = 1.84 ,
5.1 Outline of the Method (conforming to IS 266).

The sample is fused with sodium peroxide, leached in
water and acidified with sulphuric acid. Chromium is
oxidized to bichromate by ammonium persulphate in
the presence of silver nitrate. The chromium in solution
is determined by adding excess of ferrous ammonium
sulphate solution and back titrated to a purple end point
with standard bichromate solution using sodium
diphenylamine sulphonate as indicator to a purple end
point.
5.2.13 Phosphoric and Su~huricAcidA4Mure— Take
1200 ml of distilled water in a 2-litre capacity flat
bottomed flask and to it add 400 ml of concentrated
phosphoric acid followed by 400 ml of concentrated
sulphuric acid and cool it under tap.
5.3 Procedure
5.3.1 Weigh 0.5 g of finely ground and dried sample
in a nickel crucible. Mix well with about 8 g of sodium

I
 -q

IS 13452 (Part 5) :2003

peroxide. Cover with an additional 1 g of sodium 5.3.5 Titrate (see 5.3.4) the excess ferrous ammonium
peroxide, Heat carefully over a low temperature and sulphate with standard potassium bichromate solution
finally fuse the mass over a flame till completely fused. to a purple end point.

5.3.2 Cool the melt. Place the crucible in a 500 ml 5.3.6 Blank
beaker and dissolve . Remove the crucible and wash
Run a blank determination following the procedure and
with water any particles adhering to the crucible. Add
using the same amount of all the reagents and titrate
dilute sulphuric acid until it is acidic. Add fitrther 30 ml
with standard bichromate solution using sodium
and boil for 5 to 10 min.
diphenylamine sulphonate as indicator to a purple end
5.3.3 Add 4 to 5 drops of KMnOA solution (25 g/1) if point.
manganese is not present. Then add 10 ml of silver
5.3.7 Calculation
nitrate solution, warm to about 70 to 80°C and add
about 4 to 5 g of ammonium persulphate. Keep on Chromium, percent (~-v2)Nxo.01734 xloo
warm condition about 5 min and boil the solution for .
by mass M
10 min. If perrnanganate colour does not develop then
where
add further 4 to 5 g of ammonium persulphate and boil.
Continue boiling for about 30 min to destroy excess VI = volume, in ml, of potassium bichromate
ammonium persulphate. Add 20 ml of NaCl solution solution required for ferrous ammonium
(10 percent w/v) and again boil for 5 to 10 min till sulphate used;
oxides of manganese or any permanganate disappears.
Vz = volume, in ml of potassium bichromate
5.3.4 Cool the solution (see 5.3.3) to room temperature. solution required for the back titration;
Dilute to 350 ml. Add known quantity of ferrous N = normality of potassium bichromate; and
ammonium sulphate till the colour is green and add an M = mass, in g, of the sample taken.
excess of 5 ml. Add 10 ml acid mixture followed by NOTE — If vanadium content in the material is more than
5 to 10 drops of sodium diphenylamine sulphonate 0.3 percent, use potassium permanganate, solution in place of
indicator and dilute to about 400 ml with distilled water. potassium bichromate solution.

2
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Review of Indian Standards

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This Indian Standard has been developed from Doc : No. MTD 2 (4274).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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