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Whereas the Parliament of India has set out to provide a practical regime of right to
information for citizens to secure access to information under the control of public authorities,
in order to promote transparency and accountability in the working of every public authority,
and whereas the attached publication of the Bureau of Indian Standards is of particular interest
to the public, particularly disadvantaged communities and those engaged in the pursuit of
education and knowledge, the attached public safety standard is made available to promote the
timely dissemination of this information in an accurate manner to the public.

“जान1 का अ+धकार, जी1 का अ+धकार” “प0रा1 को छोड न' 5 तरफ”

Mazdoor Kisan Shakti Sangathan Jawaharlal Nehru
“The Right to Information, The Right to Live” “Step Out From the Old to the New”

IS 4737 (1982): Chromite for chemical industries [CHD 1:

Inorganic Chemicals]

“!ान $ एक न' भारत का +नम-ण”

Satyanarayan Gangaram Pitroda
“Invent a New India Using Knowledge”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता ह”

है”
ह
Bhartṛhari—Nītiśatakam
“Knowledge is such a treasure which cannot be stolen”
( Reaffirmed 1999 )
 IS : 4737 - 1982

Indian Standard
SPECIFICATION FOR
CHROMITE FOR CHEMICAL INDUSTRIES
(First Revision)

Inorganic Chemicals ( Mist ) Sectional Committee, CDC 3

Chairman Representing
DR M. S. VAIDYA The Dharamsi Morarji Chemical Co Ltd, Bombay

Members
SHRI P. V. S. RAO ( Alternate to
Dr M. S. Vaidya )
SHRI S, K. BASU Directorate General of Supplies and Disposals,
New Delhi
SHRI D. S. CHOWDHURY( Alternate )
DR R. M. BHATNAGA~ The Fertilizer ( P & D ) India Ltd, Sindri
SHRI B. N. BHA=ACHARYYA Geological Survey of India, Calcutta
SHRI S. N. BHATTACHARYA Tata Chemicals Ltd, Bombay
SHRI S. GANAPATHY( Alternate )
SHRI S. S. HONAVAR Italab Pvt Ltd, Bombay
SHRIJ. C. DEY ( Alternate I )
SHRI M. V. DABHOLKAR( Alternate II )
SHRIJ. S. MATHARU Directorate General of Technical Development, New
Delhi
SHRI R. C. BHATTACHARYYA( Alternate )
SHRI S. V. NAYAK J. K. Chemicals Ltd, Thane
SHRI P. A. MENON ( Alternate )
SHRIJ. K. PATWX Sarabhai M. Chemicals, Vadodara
SHRI H. H. KAVARANA ( Alternate )
SHRI A. K. RAO D. C. M. Chemical Works, New Delhi
SHRI B. K. VAHI ( Alternate )
SHRI B. K. SACHAR Ministry of Defence ( R & D )
SHRI A. D. GUPTA ( Alternate )
SHRI C. R. SANTHANAKRISHNAN Travancore Chemical & Mfg Co Ltd, Mettur Dam
SHRI K. V. MANI ( Alternate )
DR H. S. SAR~AR The Durgapur Projects Ltd, Durgapur
SHRI P. SATYANARAYAN Development Commissioner, Small Scale Industries,
New Delhi
DR E. R. SAXENA Regional Research Laboratory ( CSIR ), Hyderabad
DR MOD ZAFAR JAMIL ( Alternate )

( Continued on page 2 )

0 Copyright 1982
INDIAN STANDARDS INSTITUTION
This publication is protected under the Indian Copyight Act ( XIV of 1957 ) and
reproduction in whole or in part by any means except with written permission of the
publisher shall be deemed to be an infringement of copyright under the said Act.
IS : 4737 - 1982

( Continwd from page 1 )

Members R@rw&ng
SHRI H. C. SHAH Golden Chemicals Pvt ‘Ltd, Bombay
SHRI S. GANAPATHY( Alternafa )
SHRI Y. v. SHETTY Indian Oil Corporation Ltd (Refineries and Pipe-
lines Division ), New Delhi
DR V. SRINIVAUN Glaxo Laboratories ( India ) Ltd, Bombay
SHRI P. MANWKHANI ( Alternate )
DR SURJITSINQH Ministry of Defence ( DGI )
DR A. K. SEN ( Alternate )
Smu N. C. THAKKAR Indian Chemical Manufacturers’ Association,
Calcutta
DR HAIU BHAOWAN, Director General, IS1 ( Ex-o@cio Member )
Director ( Chem )

Secretay
Smu M. BAK.W GIJPTA
Assistant Director ( Chem ), IS1

Minerals for Chemical and Allied Industries Subcommittee, CDC 3 : 17

Convener
SHRI B. N. BHA~ACHARWA Geological Survey of India, Calcutta

MnnbcrS
SHRI J. A. ASTHAPUTRE Ministry of Defence ( DGI )
SI.IRIK. P. MAJUMDAR ( Ahnate )
CONTROLLER Indian Bureau of Mines, Nagpur
SHRI A. S. GOPALACHARI( Alternate )
SHRIJ. V. JOSHI The Associated Cement Companies Ltd, Bombay
DR V. C. ~~ALASHE ( Alternate )
SHRI V. M. KARVE Indian Chemical Manufacturers’ Association,
Calcutta
SHRI B. K. VAHI ( Alternate )
DR A. K. LAH~RY Raiasthan State Mineral Development Corporation
Ltd, Jaipur
SHRI V. R. V. RAGHAVAN Tata Chemicals Ltd. Bombay
SHRI K. K. RAY The U.P. State Mineral Development Corporation
Ltd, Lucknow
DR P. K. RAO Regional Research Laboratory ( CSIR ), Bhubanesh-
war
_ ^DR^ P. K. SAHOO ( Alkrnute )
DR S. SARAVANAN Tamil Nadu Minerals Ltd, Madras
SHRI S. THONTHIAPPAN( Alternate )
SHRI V. SHIVKUMAR Grindwell Norton Ltd, Bangalore
SHRI &MESH SINHA Oil & Natural Gas Commission, Dehra Dun
SHRI D. K. VERMA Bihar State Mineral Development Corporation Ltd,
Ranchi

2
 IS :4737- 1982

Indian Standard
SPECIFICATION FOR
CHROMITE FOR CHEMICAL INDUSTRIES
(First Revision)

0. FOREWORD
0.1This Indian Standard ( First Revision ) was adopted by the Indian
Standards Institution on 24 February 1982, after the draft finalized by
the Inorganic Chemicals ( Mist ) Sectional Committee had been approved
by the Chemical Division Council.

0.2 Chromite is the main chromium bearing mineral of commercial im-

portance. The mineral chromite has the composition Fe0 . Cr,O,, with a
theoretical content of 68 percent Cr,O, and 32 percent Fe0 by mass.
It is a group of cubic minerals known as spinels which is represented by
the general formula X0 .Y,O, where ‘ X ’ is a divalent metal ion usually,
iron, calcium, magnesium or manganese and Y is the trivalent metallic
ion usually, iron, chromium or aluminium. In natural chromite deposits,
replacement of chromium and iron by other elements usually occurs to
some extent, chromium being replaced by aluminium and trivalent iron,
and iron by magnesium. Consequently, commercial chrome ore rarely
contains more than 50 to 55 percent chromium and some containing up to
20 percent of both Al,O, and M,O.

0.3 Chromite finds extensive use in the metallurgical refractories and

chemical industries, the respective use depending on the chemical compo-
sition. The chemical use of chromite is almost entirely in the primary
production of sodium dichromate, and other chromium salts are subse-
quently produced.

0.4 As vanadium is present in chromite in small amount, it is counted as

chromium in this standard, and no separate method has been given for the
estimation of vanadium.

0.5 This standard was first published in 1968. It is being revised in the
light of the experience gathered during testing. In this revision major
changes have been effected in:
a) The methods of determination of silica, alumina, chromium, iron,
lime and magnesium; and
b) The method for the preparation of sample.

3
IS : 4737 - 1982

1. SCOPE

1.1 This standard prescribes the requirements and the methods of sampling
and test for chromite for chemical industries.

2. REQUIREMENTS

2.1 Description - The material shall be either in the form of lumps or

concentrates free from dirt and other foreign matter.

2.2 The material, when tested according to the methods prescribed in

Appendix A shall comply with the requirements specified in Table 1.
Reference to the relevant clauses of Appendix A is given in co1 (4) of the
table.

TABLE 1 REQUIREMENTS FOR CHROMITE FOR CHEMICAL INDUSTRIES

SL No. CHARACTERISTIC ( ON RRYBASIS) REQUIREMENT METHODOF TEST.

REP TO CL No.’
IN APPENDIX A

(1) (2) (3) (4)

9 Chromic oxide ( as C&O, ), percent by mass, 44’0 A-3

Min
ii) Total iron ( as Fe0 ), percent by mass, Max 20’0 A-3

iii) Alumina ( as Al,03 ), percent by mass, MUX 14’0 A-4

iv) Silica ( as SiOz ), percent by mass, Max 7’0 A-5

v) Lime ( as CaO ), percent by mass, Max 3’0 A-5

vi) Magnesia ( as MgO ), percent by mass, Max 14’0 A-5

3. PACKING AND MARKING

3.1 Packing-Unless otherwise agreed to between the purchaser and

the supplier, the material shall be supplied in open wagons.

3.2 Marking-A good sized metallic or cardboard label bearing the

following information with suitable paint or ink shall be conspicuously
displayed on the carrier and also placed inside:

Name of the material;

Mass of the material;
Lot number; and
Manufacturer’s name and recognized trade-mark, if any.

4
 IS : 4737 - 1982

3.2.1 The material may also be marked with the IS1 Certification Mark.

Nom-The use of the IS1 Certification Mark is governed by the provisions

of the Indian Standards Institution ( Certification Marks) Act, and the Rules
and Regulations made thereunder. The IS1 Mark on products covered by an
Indian Standard conveys the assurance that they have been produced to comply
with the requirements of that standard under a well-defined system of inspection,
testing and quality control which is devised and supervised by IS1 and operated
by the producer. IS1 Marked products are also continuously checked by IS1 for
conformity to that standard as a further safeguard. Details of conditions under
which a licence for the use of the IS1 Certification Marks may be granted to
manufacturers or processors, may be obtained from the Indian Standards Insti-
tution.

4. SAMPLING

4.1 The method of drawing representative samples of the material shall be

as prescribed in IS : 2109-1962*. However, the number of tests and criteria
for conformity shall be as prescribed in 4.2 and 4.3 respectively.

4.2 Number of Tests - Tests for determining chromic oxide (as Cr,O,),
shall be made on each of the individual samples separately. Tests for all
other requirements shall be made on the composite sample only.

4.3 Criteria for Conformity

4.3.1 For Individual Samples - For chromic oxide tested on the individual
samples, the mean and the range of test results shall be computed as follows :

Sum of individual test results

Mean (X) =
Number of test results

Range ( R ) = difference between the minimum and the maximum

test results.

The lot shall be declared to be in conformity with chromic oxide require-

ment if the value of expression ( X - 0.6 R ) is not less than the specified
minimum value.

4.3.2 For Composite Sample -- For declaring the conformity of the lot to
the requirements tested on the composite sample, the test results in respect
of each characteristic shall satisfy the corresponding specified requirements.

*Methods of sampling dolomite, limestone and other allied materials.

5
IS : 4737 - 1982

APPENDIX A
(Clause 2.2 )
ANALYSIS OF CHROMITE FOR CHEMICAL INDUSTRIES

A-l. QUALITY OF REAGENTS

A-1.1 Unless specified otherwise, pure chemicals and distilled water ( see
IS : 1070-1977*) shall be employed in tests.

NOTE- ‘ Pure chemicals ’ shall mean chemicals that do not contain impurities
which affect the resuIts of analysis.

A-2. PREPARATION OF THE SAMPLE

A-2.1 Procedure - Crush the representative sample so as to pass through

150-micron IS Sieve. Powder about lo-15 g of the sample so prepared in
an agate mortar with agate pestle till 100 percent of the sample pass through
63-micron IS Sieve. This sampIe shouId be taken for chemical analysis.

A-2.1.1 Free moisture in the sample may be determined separately

on 1 g sample drying at 1 IO + 5°C for 2 hours.

A-3. DETERMINATION OF CHROMIUM AND IRON

A-3.0 Outline of the Method - The sample is fused with sodium peroxide
in nickel crucible. Chromium is converted to dichromate and estimated
with the addition of excess ferrous ammonium sulphate in acidified solution
which is back titrated with standard potassium permanganate solution.

A-3.1 Reagents

A-3.1.1 Sodium Peroxide - Powder.

A-3.1.2 Dilute Sulphuric Acid - 1 : 1 ( v/v ).

A-3.1.3 Ferrous Ammonium &&hate Solution - 0.1 N.

A-3.1.4 Standard Potassium Permanganate Solution - 0.1 N.

A-3.1.5 Dilute Hydrochloric Acid - 1 : 1 ( v/v).

A-3.1.6 Orthophosphoric acid

*Specification for water for general laboratory use ( second~&ion ).

6
 IS i 4737 - 1982”

A-3.2 Procedure - Weigh accurately 0.5 g of the prepared sampIe in a

nickel crucible of about 30 ml capacity. Add and mix thoroughly with
about 4 g of sodium peroxide with a dry glass rod. Heat the crucible over a
flame till the mixture inside melts. Rotate the crucible gently with a pair
of tongs to mix the contents well. Then keep the crucible over the flame
at cherry red heat for about 5 minutes. Remove and allow the crucible to
cool down. Introduce the crucible into a 400 ml beaker containing about
loo-150 ml of water and covered with a watch glass. The crucible should
submerge under water. Slowly boil till evolution of oxygen gas ceases and
peroxide is destroyed. Remove the crucible and wash down the adhering
solution and decomposed mass into the same beaker, taking help of policc-
man. Cool the solution to room temperature.

A-3.2.1 Filter through No. 40 Whatman filter paper or equivalent.

Wash the residue with water till free from chromate. Dissolve the residue
in hydrochloric acid of minimum quantity and precipitate with sodium
peroxide. Boil off oxygen, filter and wash. Six to eight washings should
be adequate. Combine the filtrates and transfer into 250 ml standard
measuring flask and make up to volume.

A-3.2.2 Take 50 ml of the solution, acidify with dilute sulphuric acid

and add 5 ml more. Add 50 ml of ferrous ammonium sulphate solution.
Add 5 ml orthophosphoric acid and titrate against standard potassium
permanganate solution to the grey end point. Carry out a blank titration
50 ml of the ferrous ammonium sulphate solution with standard potassium
permanganate solution.

A-3.2.3 Calculation

Chromic oxide ( as Cr,O, ),

25*32xJv( V,-I’,)
percent by mass =
M
where
JV =normality of standard potassium permanganate solution,
V, =volume in ml of standard potassium permanganate
solution required for the blank,
T/Z=volume in ml of standard potassium permanganate
solution required for the titration, and
_M =mass in g of the prepared sample taken for the test.

A-3.3 Treat the residue on the filter paper with hot dilute hydrochloric
acid till entirely dissolved. Transfer and dilute to about 200 ml. Add 3-4.g
of ammonium chloride. Heat to boil and add ammonia dropwise till
alkaline. Boil for 4 to 5 minutes. Allow to settle. Filter through NO. 41
Whatman filter paper or equivalent. Wash with hot 0.5 percent ammonium
nitrate solution and finally twice with hot water.

7
IS i 4737 - 1982

A-3.3.1 Dissolve residue on filter paper in hot dilute hydrochloric acid

and transfer into a beaker. Cool and transfer into a 250 ml standard measur-
ing flask. Make up to volume.

A-3.4 Determination of Iron

A-3.4.0 Outline of the Method-Ferric iron is reduced with stannous

chloride excess of which is oxidized by mercuric chloride. The reduced
iron is titrated against standard potassium dichromate solution using
sodium diphenylamine sulphonate solution as indicator.

A-3.4.1 Reagents

A-3.4.1.1 Stannous chloride solution -Dissolve by heating 60 g of pure

stannous chloride in a mixture of 400 ml of concentrated hydrochloric
acid and 600 ml of water until the solution is complete. Cool, add a few
pieces of granulated tin and preserve the solution in an air-tight bottle.

A-3.4.1.2 Mercuric chloride solution - Prepare a saturated solution of

mercuric chloride in water.

A-3.4.1.3 Sulphuric phosphoric acid mixture - Add slowly 150 ml of

concentrated sulphuric acid to 700 ml of water with continuous stirring.
Add to this solution 150 ml of syrupy phosphoric acid. Destroy any oxi-
dizable impurities by adding potassium permanganate solution ( 0. I N )
drop by drop until the pink colour of permanganate persists. Cool the
solution.

A-3.4.1.4 Sodium diphenylamine sulphonate indicator solution - Dissolve

0.2 g of the reagent in 100 ml of hot water.

A-3.4.1.5 Standard potassium dichromate solution - 0.1 N. Dry pure

potassium dichromate at 140 - 150°C for one hour. Cool in a desiccator
and transfer exactly 4.904 g to a one litre volumetric flask carefully through
a funnel using water at room temperature. Wash the funnel thoroughly
and dissoIve the salt by shaking until the solution is complete. Make up
to the mark and mix well.

A-3.4.2 Procedure - Take 100 ml from solution A-3.3.1 in a 500 ml

conical flask. Add 5 ml concentrated hydrochloric acid. Heat to boil. Add
stannous chloride solution dropwise till the solution is colourless. Add two
to three drops of stannous chloride in excess. Cool the solution quickly
to room temperature.

8
 IS : 4737 - 1982

A-3.4.3 Add 10 ml of mercuric chloride solution at a time and stir

the solution. Silky white precipitate of mercurous chloride appears. Allow
to stand for 5 minutes. Add 15 ml of sulphuric-phosphoric acid mixture.
Dilute to about 200-250 ml with cold water. Add three to four drops of
indicator solution. Titrate with standard dichromate solution till colour
of the solution changes to stable blue voilet.

A-3.4.4 Calculation

AxBx7.985
Total iron ( as Fe,O, ), percent by mass = C

where
A = volume of standard potassium dichromate solution required,
B =normality of standard potassium dichromate solution, and
C =mass in g of the sample taken for the test.

A-4. DETERMINATION OF SILICA AND ALUMINA

A-4.0 General - The procedure involves decomposition of finely powdered

chromite sample with perchloric acid. The decomposed material is taken up
with dilute hydrochloric acid filtered and washed. Silica is determined
by hydrofluorization. Hydroxides of iron, aluminium and chromium are
then precipitated out with ammonia, filtered and washed. Calcium and
magnesium are determined in the filtrate. Residue is redissolved in hydro-
chloric acid. Iron is precipitated with addition of sodium peroxide. Alu-
minium is determined from the filtrate after addition of ammonium nitrate.

A-4.0.1 Procedure - Take 0.25 g of finely agated sample i -0.63 micron

IS Sieve ) in a 250 ml beaker. Add 10 ml water and 25 ml of perchloric
acid. Digest at low heat on a hot plate. Then most of black particles dis-
appear, increase heat till copious fumes start ( see Note ). Extract with
20 ml dilute hydrochloric acid and digest. Filter through No. 42 Whatman
filter paper transferring the entire residue and wash on filter paper with
hot water till free from chloride. Collect the filtrate in a 400 ml beaker.

A-4.1 Deter&nation of Silica

A-4.1.0 Outline of the Method - The residue is ignited and silica is deter-
mined by hydrofluorization in presence of 3-4 drops of sulphuric acid.

A-4.1.1 Reagents

A-4.1.1.1 Perchloric acid - 70 percent ( v/v ).

A-4.1.1.2 HydroJuoric acid - 48 percent ( v/v ).

A-4.1.1.3 Dilute su&huric acid - 18 N.

9
IS : 4737 - 1982

A-4.1.2 Procedure - Take the residue as in A-4.0.1 in a previously ignited

and weighed platinum crucible of about 25 ml capacity. Slowly burn off
filter paper. Then ignite in a furnace up to a temperature of 1 000°C. Remove
from the furnace, cool in a freshly charged desiccator and weigh. Repeat
till mass is constant.

A-4.1.3 Add 3 to Bdrops of dilute sulphuric acid and 5 ml hydrofluoric

acid. Heat on a hot plate till dry. Ignite slowly to 1 000°C and weigh.
Repeat hydrofluorization till mass of the crucible is constant. Take final
mass.
Fuse the residue with a little sodium carbonate, take up with dilute
hydrochloric acid and mix with the filtrate as in A-4.0.1.

NOTE - In case black particles of undecomposed chromite persist, dilute with

water, decant off the supernatant solution and retreat the particles with perchloric
acid m the original beaker. Complete decomposition should not take more than
5 to 6 hours. Alternately, decompose @25 g of chromite by fusing with NaaCOs
( 3 g ), take up with dilute hydrochloric acid, evaporate and bake. Extract with
20 ml dilute HCl and proceed as in A-4.0.1.

A-4.1.4 Calculatiou

Silica ( as SiO, ), percent by mass = MZ-M%

M 100
,
where
M2 = mass in g of the residue obtained in A-4.1.2,
h/i,= mass in g of the residue obtained after hydrofluorization
in A-4.1.3, and
M, = mass in g of sample taken for test in A-4.0.1.

A-4.2 Determination of Alumina

A-4.2.0 Outline of the Method-Alumina is determined by separating

as sodium aluminate from the solution of mixed oxides and precipitating
as aluminium hydroxide with ammonium nitrate and igniting to aluminium
oxide.

A-4.2.1 Reagents

A-4.2.1.1 Dilute hydrochloric acid - 5 N.

A-4.2.1.2 Ammonium chloride - Solid.

A-4.2.1.3 AmmoGum nitrate - Solid.

A-4.2.1.4 Dilute ammonium hydroxide - 8 N.

A-4.2.1.5 Dilute sodium hydroxide solution - 10 percent.

10
 IS : 4737 - 1982

A-4.2.1.6 Sodium peroxide - Solid.

A-4.2.2 Procedure -Dilute the filtrate obtained in A-4.0.1 to about

200 ml. Heat to boil after adding 4 g of ammonium chloride. Add with
stirring dilute ammonium hydroxide till a faint ammoniacal smell is
obtained. Boil for a few minutes. Allow the precipitate to settle, filter
through No. 41 Whatman filter paper transferring bulk of the precipitate
on the filter and wash with hot water 6 or 7 times. Dissolve the precipitate
in the same beaker with dilute hydrochloric acid and repeat precipitation of
hydroxides. Wash with hot water collecting the filtrate in the same beaker.

A-4.2.3 Take back the precipitate in the original beaker dissolving in

hot dilute hydrochloric acid. Nearly neutralize with freshly prepared
dilute sodium hydroxide solution. Add 1 to 2 g sodium peroxide. Dilute to
about 200 ml. Heat to boil till evolution of oxygen ceases. Filter through
No. 41 Whatman filter paper or equivalent. Repeat precipitation. Wash
precipitate with hot water.

A-4.2.4 Treat the combined filtrate containing sodium aluminate and

sodium chromate as in A-4.2.3 with 4 to 5 g of ammonium nitrate with
continuous stirring and precipitate aluminium hydroxide. Filter through
No. 41 Whatman filter paper. Repeat precipitation. Wash precipitate on
filter paper with hot 0.5 percent ammonium nitrate solution till free from
chloride. Ignite precipitate on Al@, at about 1 000°C.

A-4.2.5 Calculation

100 XM,
Alumina ( as A&,0, ) percent by mass = ~
M
where
M, =mass in g of the ignited residue, and
M =mass in g of the material taken for test.

A-5. DETERMINATION OF LIME AND MAGNESIA

A-5.0 Outline of the Method - Combined filtrate as obtained in A-4.2.2

is boiled down to less than 100 ml. Aliquots are taken for determination
of calcium and magnesium complexometrically.

A-5.1 Reagents

A-5.1.1 Dilute Hydrochloric Acid - 5 N.

Ab.1.2 Potassium Hydroxide Solution - approximately 10 N. The solution

should be freshly prepared from AR quality potassium hydroxide.

11
IS : 4737 - 1982

A-5.1.3 Buffer Solution ( pH 10 ) -Dissolve 70 g of ammonium chloride

in 200 ml of water, add 570 ml of concentrated ammonia ( density 0.88 -
0.90 ) and dilute to 1 litre.

A-5.1.4 Patton and Keeder’s Indicator-Mix 0.1 g of 2 hydroxy

I-( 2-hydroxy-4-sulpho- 1naphthalzo ) -3-naphthoic acid with 10 g of potas-
sium chloride and grind into a fine mixture in a glass mortar. Preserve in a
well stoppered dry amber coloured glass bottle.

A-5.1.5 Erie Chrome Black T Indicator-Dissolve 0.5 g of Erio Chrome

Black T indicator in 100 ml of rectified spirit and preserve in amber coloured
glass bottle. This indicator should be freshly prepared preferably.

A-5.1.6 Standard ED TA Solution - Weigh 7.444 g of disodium ethylene

diamine tetracetate dihydrate ( EDTA ) and dissolve in deionized water.
Make up the volume to one litre. Mix thoroughly. The solution is 0.02 M.

A-5.1.7 Potassium Cyanide and Hydroxylamine Hydrochloride Pure

A-5.1.8 Deionized Water

A-5.2 Determination of Calcium Oxide

A-5.2.1 Procedure-The combined filtrate as in A-4.2.2 is boiled down

to less than 100 ml cooled and made up to volume 100 ml in a standard
measuring flask. Take two portions of 25 ml each in two conical flask or
white porcelain dish of 100 ml capacity. Add about 5 ml of potassium
hydroxide solution to one flask. Add about 0.2 to 0.4 g P and R indicator
and quickly titrate till the colour changed to violet blue. Note the volume
of EDTA consumed. Add the same EDTA volume less 1 *O ml directly
to the second flask. Add 5 ml of potassium hydroxide solution and about
50 mg each of potassium cyanide and hydroxylamine hydrochloride. Add
0.4 g indicator and immediately titrate with continuous stirring until no
further colour changes and the test solution is clear blue without any tinge
of violet. Volume of EDTA consumed in the final titration should be taken
for calculating CaO percent ( A-5.2.2 ).

A-5.2.2 Calculation

0.11216 V,
Calcium oxide ( as CaO ), percent by mass = M

where
V, =volume in ml of 0.02 M EDTA solution required for final
titration, and
M =mass in g of the material contained in the aliquot of
solution taken for the titration.

12
 IS : 4737 - 1902

A-5.3 Determination of Magnesia

A-5.3.1 Procedure - Take 25 ml aliquot from A-5.1.2 in a white porcelain

dish of 100 ml capacity. Add 25 ml of ammonium chloride and ammonium
hydroxide buffer solution and a few drops of Erio Chrome Black T and
titrate with EDTA solution till the colour changes from wine red to indi-
cator blue.

A-5.3.2 Calculation

v,-VI
Magnesium ( as MgO ), percent by mass = 0.080 62 x 7

where
V, =volume of 0.02 M EDTA solution required for the titra-
tion,
V, =volume of 0.02 M EDTA solution required for the sample
solution, and
M =mass in g of the material contained in the aliquot of solu-
tion taken for the titration.

13