IS 13452-5: Chemical Analysis of Ferrochromium, Part 5: Determination of Chromium in High Carbon Ferrochromium/Chargechrome by Dichromate Titration

8 Pages·2003·1 MB·English

by  Bureau of Indian Standards

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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]
“!ा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 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 BIS2003
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

.4prii2003 Price Group 1
.. ... ..,
Methods of Chemical Analysis ofFerrous 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 inthis series are:
(Part 1): 1992 Determination of silicon inhigh 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 ofphosphorus in ferrochromium/chargechrome by alkalimetric method
In this revision, major modifications are asfollows:
a) Scopeofthemethod hasbeen modified bylowering thelimit fordetermination ofchromium from 60to
50percent (Range from 50to 70percent).
b) Procedure hasbeen modified bytitrating theexcess ferrous ammonium sulphate bystandard potassium
bichromate solution instead of standard potassium permanganate solution.
Inreporting the result of atest or analysis made inaccordance with this standard, ifthe final value observed or
calculated, istoberounded off, itshallbedone inaccordance withIS2: 1960‘Rules forrounding 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 )
1SCOPE 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),
70percent (containing carbon above 1percent).
20 percent (v/v).
2REFERENCES 5.2.3Ammonium Persulphate, solid.
The standards listed below contain provisions which 5.2.4 Silver Nitrate Solution, 1percent (w/v).
through reference inthistext, constitute provisions of
5.2.5 Phosphoric Acid, rd = 1.75or 88 percent.
this standard. At the time of publication, the editions
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
ISNo. Title sulphate FeSOJNHJ2 SOd.6H20 in 500 ml of dilute
266:1993 Sulphuric acid (third revision) sulphuric acid (5percent) ina 1-litre volumetric flask
1070:1992 Reagentgradewater (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 Drypotassium bichromate inanovenat 105to
3 SAMPLING 110”Cfor one and a half hours, cool in a desiccator.

Weighexactly4.903 5g.Dissolve inwaterandtransfer
Thesampleshallbedrawn andprepar ed inaccordance

to 1-litre volumetric flask, dilute volume and mix.
with IS 1472.
5.2.10 Sodium Diphenylamine Sulphonate Indicator
4QUALITY 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 100ml hot distilled water.
for thetest.
5.2.11 Sodium Chloride Solution, 10 percent (w/v).
5DETERMINATION OF CHROMIUM
5.2.12 Concentrated Sulphuric Acid, rd = 1.84 ,
5.1Outline of the Method (conforming toIS 266).
The sample isfused with sodium peroxide, leached in 5.2.13Phosphoric and Su~huricAcidA4Mure— Take
water and acidified with sulphuric acid. Chromium is 1200 ml of distilled water in a 2-litre capacity flat
oxidized to bichromate by ammonium persulphate in bottomed flask and to it add 400 ml of concentrated
thepresenceofsilvernitrate.Thechromium insolution phosphoric acid followed by 400 ml of concentrated
isdetermined by adding excess offerrous ammonium sulphuric acidandcool itunder tap.
sulphatesolutionandbacktitratedtoapurpleendpoint
5.3 Procedure
with standard bichromate solution using sodium
diphenylamine sulphonate asindicator toapurple end 5.3.1 Weigh 0.5 g of finely ground and dried sample
point. inanickel crucible. Mixwellwith about 8gofsodium

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IS 13452 (Part 5) :2003
peroxide. Cover with an additional 1g 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 aflame till completely fused. to apurple 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 ablank 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 itisacidic. Add fitrther 30 ml
with standard bichromate solution using sodium
and boil for 5 to 10 min.
diphenylamine sulphonate as indicator to apurple 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
10min. Ifperrnanganate colour does not develop then
where
add further 4to 5gof 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) toroom 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 isgreen 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 toabout 400 mlwith distilled water. potassium bichromate solution.

2
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This Indian Standard has been developed from Doc :No. MTD2(4274).
Amendments Issued Since Publication
Amend No. Date of Issue Text Affected
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