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IS 2000-4 (1985): Methods of chemical analysis of bauxite,Part 4: Determination of ferric oxide [MTD 13: Ores and RawMaterials]

IS : 2000 ( Part 4 ) - 1985

Indian Standard METHODS OF

CHEMICAL ANALYSIS OF BAUXlTE

PART 4 DETERMINATION OF FERRIC OXIDE

( First Revision )

Methods of Chemical Analysis of Ores, Minerals and R.efractories Sectional Committee, SMDC 35

Chairman

Dn L. P. PANDEY

Members

Representing

National Metallurgical Laboratory ( CSIR ), Jamshedpur

lh V. M. C~~OWDIIURY I Alfernafe to ’ Dr L. P. Pandey )

SHR~ G. M. APPA RAO Steel Authority of India Ltd ( Bhilai Steel Plant j, Bhilai

SHXI C. L. SHARMA ( Allernafe ) S~XI J. BANERJEE Steel .4uthority of India Ltd ( Durgapur Steel

Plant \. Dureauur ----~,. -. SHRI A. C. MALLICK ( Alternate )

SHRI S. V. BHA~WAT Khandelwal Ferro Alloys Ltd, Khandelwal Nagar SI~RI D. N. .GUPTA ( Allernale )

SHEI P. BHATTACHAEYA Belpahar Refractories Lid, Belpahar SEI~I P. V. RAO ( Alternate )

SHXI P. K. GHOSAL Kumardhubi Fireclay and Silica Works Ltd, Kumardhubi

SHRI L. N. BANE:~JEE ( Allertiale ) Sr11rr N. B. Guu~ Chowgule & Co Pvt Ltd, Marmugao Harbour SHRI S. S. HONAVAR Italab Pvt Ltd, Madras

SHHI M. V. DAH~OI,I<~I% ( Allernale I ) SHRI J. C. DEY ( Alternate II )

DR C. S. P. IYEX Chairman, SMDC 2 ( Bhabha Atomic Research Centie, Bombay )

Srr~t~ J. R. K. MUX’J’IIY Harz lFu_eF;ctories & Ceramic Works Pvt Ltd, a

SHIGI N. C. SUIA ( Alternate ) DR A. PURUSOTTA~W Geological Survey of India, Calcutta S~rltr M. RAE National Test House, Calcutta

SHRI A. K. DU~TA GIZPT_. ( Alternate ) ( Continued on tage 2 )

I

@ C’ejyright 1986

INDIAN STANDARDS INSTITUTION

This publication is protected under the Indum Copyright Act ( XIV of 1957 i 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 : 2000 ( Part 4 ) - 1985

( Continued from page 1 )

Members Representing

DR J. RAJARAM Essen & Co, Bangalore SHRI K. R AMA KR~SRNA ( Alternate )

SIXRI G. RAJA RAO SIWI D. V. RAMAN

Ferro Alloys Corporation Ltd, Shreeramnagar National Mineral Development Corporation Ltd,

SRRI N. VENKATRAMAN ( Alternate ) Hyderabad

SHRI K. SYAMALA RAO DR B. C. SINITA

Mineral Exploration Corporation Ltd, Nagpur Central Glass & Ceramic Research Institute

SHRI S. Dns GUPTA ( Alternate ) ( CGCRI ), Calcutta

DR Y. P. SRIVASTAVA The Tata Iron & Steel Co Ltd, Jamshedpur DR K. S. R. KRISHNAIAII ( Alternate)

SHRI B. N. TIKOO DR Cn VENKATESWARLU

Department of Atomic Energy, Hyderabad Chairman, SMDC 34 ( Bhabha Atomic Research

SJ~RI K. RA~IIAVENDR.~N, Director ( Strut & Met )

Centre, Bombay ) Director General, IS1 ( Ex-o&cio Member )

Secretaries

SHRI JAGMOHAN SINGII Deputy Director ( Metals ), IS1

SHRI M. L. SITARMA Asistant Director ( Metals ), ISI

2

IS:2000(Part4 )- 1985

Indian Standard METHODS OF

CHEMICAL ANALYSIS OF BAUXITE

PART 4 DETERMINATION OF FERRIC OXIDE

( First Revision )

0. FOREWORD

0.1 This Indian Standard ( Part 4 ) ( First Revision ) was adopted by the Indian Standards Institution on 24 December 1985, after the draft finalized by the Methods of Chemical Analysis of Ores, Minerals and Refractories Sectional Committee had been approved by the Structural and Metals Division Council.

0.2 IS : 2000-1962” which coverd determination of loss on ignition; total silica, non-reactive and reactive silica; alumina; ferric oxide by dichro- mate method, permanganate and calorimetric methods; titania by reduc- tion ( volumetric ) and calorimetric methods; phosphorus; calcium oxide; magnesium and manganous oxide was first published in 1962. While reviewing this,standard the Sectional Committee felt the need for the revision of this standard. On the basis of experience gained during these years the Committee decided to revise this standard into different parts covering determination of each element in a separate part, which on publication would supersede that element given in IS : ZOOO-1962*. This part covers determination of ferric oxide. The other parts are:

Part 1 Determination of loss on ignition

Part 2 Determination of silica ( as SiOz, 0.5 to IO.0 percent )

Part 3 Determination of alumina

Part 5 Determination of titania ( 0.5 to 12.0 percent )

Part 6 Determination of vanadium ( V < 0.1 percent )

Part 7 Determination of phosphorus pentoxide ( PzOs < 0.5 percent )

Part 8 Determination of manganous oxide ( MnO < 0 5 Fercent )

The procedures for determination of CaO, and Mgo in bauxite are at present under investigation and will be given in subsequent parts.

*Methods of chemical analysis of bauxite.

3

_ ._ “... .-- L.. --

IS : 2000 ( Part 4 ) - 1985

0.3 In this revision the committee decided to retain and update the dichromate method, while deleting the permanganate and calorimetric methods.

0.4 In the preparation of this revision due consideration has been given to the facilities available in the country to carry out such analysis.

0.5 In reporting the results 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 witn IS : 2-1960*.

1. SCOPE

1.1 This standard ( Part 4 ) covers the determination of ferric oxide in bauxite.

2. SAMPLING

2.1 Sample shall be drawn and prepared as per the method prescribed in clause 2 of IS : 2000 ( Part 1 )-19851_.

3. GENERAL

3.1 Use of Filter Paper - In this standard, Whatman filter paper with their relative numbers have been prescribed since they are comm- only used’. However, any other suitable brand of filter paper of corres- ponding porosity and of equivalent quality may also be used.

4. QUALITY OF REAGENTS

4.1 Unless specified otherwise, analytical grade reagents and distilled water shall be employed in the test.

5. DETERMINATION OF FERRIC OXIDE BY THE DICHROMATE METHOD

5.1 Outline of the Method - From an aliquot of the main solution [ see 5.3.3 of IS : 2000 ( Part 2 )-1985: 1, RsOs is precipitated by ammonium hydroxide, precipitate is dissolved in hydrochloric acid and ferric iron is then reduced with stannous chloride, excess of which is oxidized by mercuric chloride, the reduced iron is titrated with standard dichromate solution.

*Rules for rounding off numerical values ( revised ). tMethods of chemical analysis of bauxite: Part 1 Determination of loss on ignition

( Jirst revision ) . $Methods of chemical analysis of bauxite: Part 2 Determination of silica (first

revision ).

4

IS : 2000 ( Part 4 ) - 198s

5.2 Reagents

5.2.1 Concentrated Ammonium Hydroxide - rd = 0.90.

5.2.2 Ammonium Chloride - Solid.

5.2.3 Dilute Hydrochloric Acid I I :1 ( u.v ).

5.2.4 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 colution in an air tight, amber-coloured bottle.

5.2.5 Mercuric Chloride Solution - Prepare a saturated solution of mercuric chloride in water.

5.2.6 Sulphuric Acid-Phosphoric Acid Mixture - Add slowly 100 ml of concentrated sulphuric acid to 700 ml of water with constant stirring. Add to this solution 200 ml of syrupy phosphoric acid ( 85 percent ). Cool the solution.

5.2.7 Sodium Diphenylamine Sulphonate Indicator Solution - Dissolve 0.32 g of barium diphenylamine sulphonate in 100 ml of warm water. Add 0.5 g of sodium sulphate, stir, and filter off the precipitate. Store in an amber-coloured bottle. Alternatively, dissolve out 0.20 g of sodium diphenylamine sulphonate in 100 ml of water and store in an amber- coloured bottle.

5.2.8 Standard Potassium Dichromate Solution - ( 0.01 .h’ ) - Dry pure and analytical grade potassium dichromate and transfer in an oven at 110 -& 2°C for about two hours. Cool in a desiccator. From this, weigh out exactly 0.490 4 g to a 1 000 ml volumetric flask carefully through a funnel using water at room temperature. Wash the funnel thoroughly and dissolve the salt completely by shaking until the solution is complete. Make up to the mark and mix well.

5.3 Procedure

5.3.1 Pipette out 100 ml aliquot from the main solution [ see 5.3.3 of IS : 2000 ( Part 2 )-1986* ] in a 400 ml beaker and precipitate Rz03 by ammonium hydroxide in the presence of ammonium chloride ( 2-3 g ), boil and filter. Dissolve the precipitate in hydrochloric acid and reprecipitate mixed hydroxides with ammonium hydroxide and filter using Whatman filter paper No. 41. Wash twice with hot water. Dissolve the precipitate in 250-m] conical flask in 30-40 ml of hot hydrochloric acid and boil the solution, till the solution .is reduced to about 20 ml.

*Methods of chemical analysis of bauxite: .Part 2 Determination of silica (Jirst revision ) .

5

b

IS : 2000 ( Part 4 ) - 1985

Reduce while hot by dropwise addition of stannous chloride solution until the solution becomes colourless. Add 1 to 2 drops in excess. Cool immediately to room temperature. The excess stannous chloride removed by addition of 10 ml mercuric chloride. A silkly white precipitate of mercurous chloride will form slowly. ( In case black precipitate is formed the experiment should be repeated. ) Allow to stand for 2 minutes and dilute to about 150 ml. Add 10 ml of sulphuric acid phos- phoric acid mixture and 3 to 4 drops of indicator solution, and titrate with standard potassium dichromate solution with constant stirring until the green colour changes to deep violet colour. Colour should presist for at least 15 seconds.

, 5.4 Calculation

Ferric oxide, percent = A x I3 x 0.079 85 x 100

-c

where

A = volume in ml of the standard potassium dichromate solution,

B = normality of the standard dichromate solution, and

C = mass in g of the sample as represented by the aliquot taken.

,-