IS 8862 (1978): Titanium Dioxide (Anatase Type) for Rubber ... · FOR RUBBER INDUSTRY 0. FOREWORD...

18
Disclosure to Promote the Right To Information 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. इंटरनेट मानक !ान $ एक न’ भारत का +नम-णSatyanarayan Gangaram Pitroda “Invent a New India Using Knowledge” प0रा1 को छोड न’ 5 तरफJawaharlal Nehru “Step Out From the Old to the New” जान1 का अ+धकार, जी1 का अ+धकारMazdoor Kisan Shakti Sangathan “The Right to Information, The Right to Live” !ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता ह Bharthari—Nītiśatakam “Knowledge is such a treasure which cannot be stolen” IS 8862 (1978): Titanium Dioxide (Anatase Type) for Rubber Industry [PCD 13: Rubber and Rubber Products]

Transcript of IS 8862 (1978): Titanium Dioxide (Anatase Type) for Rubber ... · FOR RUBBER INDUSTRY 0. FOREWORD...

Page 1: IS 8862 (1978): Titanium Dioxide (Anatase Type) for Rubber ... · FOR RUBBER INDUSTRY 0. FOREWORD 0.1 This Indian Standard was adopted by the Standards Institution on 10 July 1978,

Disclosure to Promote the Right To Information

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.

इंटरनेट मानक

“!ान $ एक न' भारत का +नम-ण”Satyanarayan Gangaram Pitroda

“Invent a New India Using Knowledge”

“प0रा1 को छोड न' 5 तरफ”Jawaharlal Nehru

“Step Out From the Old to the New”

“जान1 का अ+धकार, जी1 का अ+धकार”Mazdoor Kisan Shakti Sangathan

“The Right to Information, The Right to Live”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता है”Bhartṛhari—Nītiśatakam

“Knowledge is such a treasure which cannot be stolen”

“Invent a New India Using Knowledge”

है”ह”ह

IS 8862 (1978): Titanium Dioxide (Anatase Type) for RubberIndustry [PCD 13: Rubber and Rubber Products]

Page 2: IS 8862 (1978): Titanium Dioxide (Anatase Type) for Rubber ... · FOR RUBBER INDUSTRY 0. FOREWORD 0.1 This Indian Standard was adopted by the Standards Institution on 10 July 1978,
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Page 4: IS 8862 (1978): Titanium Dioxide (Anatase Type) for Rubber ... · FOR RUBBER INDUSTRY 0. FOREWORD 0.1 This Indian Standard was adopted by the Standards Institution on 10 July 1978,
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IS : 8862 - 1978

Indian Standard SPECIFICATION FOR

TITANIUM DIOXIDE ( ANATASE TYPE ) FOR RUBBER INDUSTRY

Rubber Products Sectional Committee, PCDC 13

Chairman Representing

DR D. BANERJEE Escon Consultants Pvt Ltd, Calcutta

Members

SRRI M. L. BAHRANI Ministry of Defence ( R & D ) SERI ANIL .~GARWAL ( Alternate )

SHRI A. K. BANDYOPADHAYA Ministry of Defence ( DGI ) SHRI M. KUMARAN ( Alternate )

SHRI A. T. BASAK Directorate General of Supplies & Disposals, New Delhi

SHRI S. K. BOSE SHRI A GHOSH ( Altcrnats )

DR S. N. CHAKRAVARTY SHRI R. R. PANDIT ( Alternate )

SHRI D. K. CHATTERJEE

DR S. K. ROY ( Alternate ) SHRI 0. P. DHAMIJA

National Test House, Calcutta

Bayer (India ) Ltd, Bombay

Alkali & Chemical Corporation of India Ltd, Rishra

Export Inspection Council of India, Calcutta \ SHRI P. K. CHATTERJEE ( Alternate 1

SHRI K. N. GANESH Indian Petrochemicals Corporation Ltd, Jawahar- nagar

SHRI S. B. GAN~ULI Dunlop India Ltd, Calcutta SHRI P. N. S. MYER ( Alternate )

SHRI A. GEOROE JOHN Madras Rubber Factory Ltd, Madras SHRI K. J. ABRAHAM ( Alternate 1

SHRI LALIT MOHAN JAMNADAS Cosmos India Rubber Works Pvt Ltd, Bombay SHRI PULIN L. KINARIWALA

( Alternate ) ‘&I&I R. C. JHINOAN Indian foil Corporation Ltd, Bombay

SHRI M. K. JAIN ( Alternate ) DR I. V. KRISHNAMURTI National Rubber Manufacturers’ Ltd, Calcutta

SHRI J. CWATTERJEE ( Altmafe ) SHRI S. V. LATHIA Lathia Rubber Manufacturing Co Pvt Ltd, Bombay

SHRI D. P. LATHIA ( Alternate ) SHRI V. N. MAKER All India Rubber Industries Association, Bombay

SHBI M. M. PATEL ( Alternate )

( Continued on page 2 )

@ Copyright 1978 INDIAN STANDARDS INSTITUTION

This publication is protected under the Indian CopFight 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.

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IS : 8862 - 1978

( Continued from page 1 )

Members Representing

DR S. P. MANIK Railway Board, Ministry of Railways SHRI D. N. V. CRELLAM ( Alternate )

Dn W. MILINS Indian Rubber Manufacturers’ Research Association, Bombay

DR C. K. N. NAIR Rubber Board, Kottayam SHRI N. NAOARAJAN Sundaram Industies Pvt Ltd, Madras

SHRI P. VIJAYARAGHAVAN ( Alternate ) SERI S. C. NANDY Bata India Ltd, Calcutta

SRRI SUNIL SARKAR (Alternate ) DR N. V. C. RAO Directorate General of Technical Development,

New Delhi SHRI G. R. INAMDAR (Alternate )

SHRI M. S. SAXENA, Director %eneral, ISI ( Ex-oficio Member ) Director ( P & C )

Secretary

SHRI SATISH CHANDER Deputy Director ( P & C ), IS1

Rubber Chemicals & Compounding Ingredients Subcommittee, PCDC 13 : 5

Conoener

Snnr A. K. SEN CIIAUDHURI Escon Consultants Pvt Ltd, Calcutta

Members

DR M. C. BADRINARAYANA Bayer ( India ) Ltd, Bombay DR S. N. CKAKRAVARTY ( Alternate )

SHEI A. K. BANDY~PADHYA Ministry of Defence ( DGI ) SnRI P. L. Naa ( Alternate )

SHRI B. BANERJEE Indian Rubber Manufacturers’ Research Association, Bombay

Snnr B. BHATTACHARYA Inchek Tyres Ltd, Calcutta SHRI P. K. SARKAR ( filternate)

SHRI S. K. Boar: National Test House, Calcutta DR D. K. DAS ( Alternate )

SHRI D. K. CHATTERJEE Alkali & Chemical Corporation of India Ltd, Rishra

DR S. K. RAY ( Alternate ) L SHRI J. CRATTERJEE National Rubber Manufacturers Ltd, Calcutta

SHRI A. K. BISWAS ( Allenrate ) SHRI R. W. DRARWADKAR United Carbon Yndia Ltd, Bombay SHRI S. B. GANQULI Dunlop India Ltd, Calcutta

SHRI A. SEN ( Alternate ) DR A. S. GHAQ All India Rubber Industries Association, Bombay;

and Mindia Chemicals Ltd, Bombay SHRI S. V. LATHIA ( Alternate ) All India Rubber Industries Association, Bombay SHRI H. B. KINOSLEY Mindia Chemicals Ltd, Bombay

( Alternate )

( Continued on page 14 )

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IS :8862- 1978

Indian Standard SPECIFICATION FOR

TITANIUM DIOXIDE ( ANATASE TYPE ) FOR RUBBER INDUSTRY

0. FOREWORD

0.1 This Indian Standard was adopted by the Indian Standards Institution on 10 July 1978, after the draft finalized by the Rubber Products Sectional Committee had been approved by the Petroleum, Coal and Related Products Division Council.

0.2 Titanium dioxide, anatase, one of the two crystalline forms of titanium dioxide is used in the rubber industry as a white pigment for the manufacture of white and light coloured rubber products. The distinction between the two forms, namely rutile and anatase can be done by X-ray crystallography. The same has, however not been included in the specification as the facilities for doing this test are not widely available.

0.3 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*.

1. SCOPE

1.1 This standard prescribes the requirements and methods of sampling and test for titanium dioxide ( anatase type ) in powder form intended for use as a white pigment in rubber compounds.

2. REQUIREMENTS

2.1 Appearance - The material shall be in the form of a white fine powder, free from lumps, grit and extraneous matter.

2.2 The material shall comply with the requirements given in Table 1 when tested according to the methods listed in co1 4 of the table.

*Rules for rounding off numerical values ( revised ).

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IS : 8862 - 1978

TABLE 1 REQUIREMENTS OF TITANIUM DIOXIDE ( ANATASE TYPE ) FOR RUBBER INDUSTRY

( Clauses 2.2, 4.2 and4.3 )

SL No.

(1) i)

ii)

iii)

iv)

v)

vi)

vii)

viii)

ix)

x)

CHARACTERISTIO REQUIREMENT METHOD OF TEST, REF TO

(2) (3) (4) Colour Close match to the Visual Examination

approved sample

Sieve residue, percent by mass, Max:

3 of IS : 7086 ( Part I )-1973*

a) Through 158 micron 0.01 IS Sieve

b) Through 45 micron 0.05 IS Sieve

Rel;ltz density at 27’C/ 3’85-3.95 4 of IS : 7086 ( Part I )-1973f

pH 6 to 8 5 of IS : 7086 ( Part I )-1973* Moisture content, percent 0’5

by mass, Max 7 of IS : 7086 ( Part I )-1973*

Matter soluble in water, 0.5 percent by mass, Max

8 of IS : 7086 ( Part I )-1973’

Titanium dioxide ( as 98.0 Appendix A TiCs ), percent by mass, Min

Copper, percent by mass, 0’002 Appendix B Max

Iron, percent by mass, 0.04 Appendix C Max

Solubility in ;$ure of To pass Appendix D sulphuric ’ and the test ammonium sulphate

*Methods of sampling and test for rubber compounding ingredients, Part I.

3. PACKING AND MARKING

3.1 Packing - The material shall be packed as agreed between the purchaser and the supplier.

3.2 Marking - Each package shall be securely closed and legibly marked to furnish the following information:

a> Manufacturer’s name and registered trade-mark, if any;

b) Name of the material;

cl Net mass of the material in the package; and

4 Lot, batch number and year of manufacture.

4

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IS : 8862 - 1978

3.2.1 Each package may also be marked with the ISI Certification Mark.

NOTE - 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 safe- guard. Details of conditions under which a licence for the use of the IS1 Certification Mark may be granted to manufacturers or processors, may be obtained from the Indian Standards Institution.

4. SAMPLING AND CRITERIA FOR CONFORMITY

4.1 Sampling - The sampling shall be done as prescribed in 15 of IS : 7086 ( Part I )-1973*.

4.2 Number of Tests - Tests for all the characteristics ( see Table shall be conducted on a composite sample.

4.3 Criteria for Conformity - The lot shall be considered conforming to the specification, the requirements given in Table 1.

if the composite sample satisfies

APPENDIX A [ Table I, Sl No. (vii) ]

DETERMINATION OF TITANIUM DIOXIDE

1)

as all

A-O. GENERAL

A-0.1 Two methods for the determination of titanium dioxide have been prescribed. For routine testing, either Method 1 or Method 2 may be followed but in case of dispute, Method 1 shall be applicable.

A-1. METHOD 1 ZINC REDUCTION METHOD

A-l.0 Outline of the Method - A solution of the dry pigment is made with concentrated sulphuric acid and ammonium sulphate. Titanium is reduced with zinc amalgam in Nakazono reductor and the resulting trivalent titanium is titrated with ferric alum.

*Methods of sampling and test for rubber compounding ingredients, Part I.

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IS : 8862 - 1978

A-I.1 Apparatus

A-1.1.1 .Nakazono Reductor - The apparatus as shown in Fig. 1, consists of a bulb A with a capacity of 500 ml with three stopcocks B, C and D attached. To the stopcock D may be attached, by means of thick rubber tubing E, a small cylindrical flask F of about 50 ml capacity. The stopccck C which is smaller in bore than either of the other two serves to admit carbon dioxide or nitrogen.

Ail dimensions in millimetres.

FIG. 1 NAKAZONO REDUCTOR

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IS:8862 - 1978

A-l.2 Reagents

A-l .2.1 Concentrated Sulphuric Acid - relative density 1.84 ( see IS : 266- 1961* ).

A-1.2.2 Ammonium Sulphate

A-1.2.3 zinc Amalgam - 3 percent, prepared as given below:

Place 50 ml of mercury in a small porcelain dish on a hot water-bath, covering the surface of the mercury with 2 percent ( m/u ) sulphuric acid. Add about 25 g of zinc in small granules. Stir from time to time and replenish the dilute acid with water as required. When all the zinc has disappeared, allow the amalgam to cool and stand for several hours. Finally filter through a Gooch crucible with no asbestos pad. Store the amalgam in glass bottle under 2 percent ( m/v ) sulphuric acid.

A-1.2.4 Standard Ferric Alum Solution - 0.062 5 N, standardized as follows:

Transfer by a pipette 50 ml of the ferric alum solution to be standardized to the Nakazono reductor prepared ready for use as described in A-1.3.2. Displace the air in the reductor by passing carbon dioxide for 3 minutes. Close the taps B and C. Bring the amalgam into intimate contact with ferric alum solution by shaking the apparatus vigorously for 5 minutes. Place the apparatus on a ring stand. Drain the amalgam and pass inert gas as described under A-1.3.4. Titrate it against standard potassium permanganate. The end point is the appearance of light pink colour at least persistent for 30 seconds. the ferric alum solution as follows:

Calculate the strength of

0’1 Strength of ferric alum solution - v X 50

where

V = volume of 0.1 N standard potassium permanganate solution required for titration.

A-1.2.5 Potassium Thiocyanate Solution - 10 percent ( m/v ).

*Specification for sulphuric acid ( reuized ).

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IS : 8862 - 1978

A-l.3 Procedure

A-1.3.1 Weigh approximately 0.5 g of the dried material to the nearest 0.1 mg, into a 250-ml beaker. Add 20 ml of concentrated sulphuric acid and 10 g of ammonium sulphate. Mix carefully and heat on a hot plate to fuming and then over a strong flame until solution is complete, observing caution while examining the solution. Cool the solution, dilute with 100 ml of distilled water, stir and filter, if necessary.

A-1.3.2 Open stopcock C, transfer sufficient quantity of 4 percent sulphuric acid to fill the bottom flask and leave no air space below the stopcock D. Close tap D and add 20 ml of zinc amalgam to A. The reductor is now ready for use.

A-1.3.3 To the amal-gam contained in A, transfer the solution, warmed to 5O”C, which shall not exceed 300 ml in volume. Then pass carbon dioxide or nitrogen for about 3 minutes. Close taps B and C and simultaneously disconnect the carbon dioxide supply. Bring the amalgam into intimate contact with the solution by shaking the apparatus vigorously for 5 minutes, holding it in such a way that the stopcocks are kept shut and in position. The rate of reduction is apparent by develop- ment of the characteristic violet colour of the trivalent titanium.

A-1.3.4 Place the apparatus on a ring stand. Open stocpcock D slightly and allow the amalgam to flow slowly into F. Close D immediately as soon as the amalgam has been completely transferred. With taps B and D open, pass inert gas through D as before, add IO ml potassium thiocyanate solution and titrate with standard ferric alum solution until a faint pink coloration persists for one minute.

A-1.3.5 Facilitate the titration by attaching a piece of very narrow glass tubing to the tip of the burette-with a piece of rubber tubing. The extension passes through stopcock B into the bulb A.

A-4.4 Calculation

Titanium dioxide content, percent by mass

v. x 0.005 = M X 100

where

V = volume in ml of 0.062 5 N ferric alum solution required, and

M = mass in g of pigment taken.

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IS : 8862 - 1978

A-2. METHOD 2 ALUMINIUM REDUCTION METHOD

A-2.0 Outline of the Method - This method is similar to zinc reduction method but easier and quicker to operate. Titanium is reduced to trivalent state by aluminium and titrated against ferric ammonium sulphate using ammonium thiocyanate as indicator.

A-2.1 Apparatus

A-2.1.1 Delivery Tube - made of about 4 mm internal diameter glass tube, bent in such a way as to have a horizontal run of about 150 mm and vertical drop of about 75 mm at one end, and a vertical drop of about 150 mm at the other end.

A-2.1.2 Long Necked Flask - 500-ml capacity.

A-2.2 Reagents

A-2.2.1 Ammonium Sulfihate

A-2.2.2 Sulphuric Acid - relative density 1’84 ( see IS : 266-1961* ).

A-2.2.3 Hydrochloric Acid - relative density 1’19 ( see IS : 265-19627 ).

A-2.2.Q Aluminium Foil - electrolytic grade.

A-2.2.!i Sodium Bicarbonate Solution - saturated.

A-2.2.6 Ammonium Thiocyanate Indicator Solution - prepared as follows:

Dissolve 24’5 g of ammonium thiocyanate in 80 ml of hot water. Filter, cool to room temperature, dilute to 100 ml and preserve in well stoppered, amber coloured bottle.

A-2.2.7 Standard Ferric Ammonium Sulphate Solution - prepared as follows:

Dissolve 30.16 g of fresh ferric ammonium [ FeNHs(S04)z, 12 H20 1

sulphate in 800 ml of water containing 15 ml

of concentrated sulphuric acid. Add 0.1 N potassium permanganate solution until a very slight pink colour is obtained. Dilute to 1000 ml and mix thoroughly. Filter, if necessary. Standardize with 0.190 0 to 0.210 0 g of standard titanium dioxide of known purity prescribed in A-2.3 and calculate titanium dioxide equivalent of solution in grams of titanium dioxide per millilitre of solution as given below:

Titanium dioxide equivalent -= VMXxlo’,

*Specification for sulphuric acid ( revised ). @pccibication for hydrochloric acid ( revised ).

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IS : 8862 - I978

where

M = mass in g of standard titanium dixoide taken for test,

P = percentage of titanium dioxide in standard titanium dioxide used, and

V = volume in ml of ferric ammonium sulphate solution required for titration.

A-2.3 Procedure

A-2.3.1 Weigh accurately about 0’190 0 to 0.210 0 g of the dry material and transfer the same to a 500-ml long necked flask. Add 7 to 9 g of ammonium sulphate and 20 ml of sulphuric acid, mix carefully, heat on a hot plate to fuming and then over a strong flame until solution is complete. Cool and add 120 ml of water and 20 ml of hydrochloric acid. Boil the contents and remove from heat.

A-2.3.2 Insert the short end of the delivery tube into one hole of a two-hole rubber stopper suitable for the long necked flask. Insert a glass rod with a hook at the bottom end in the other hole in such a way that the bottom end shall be nearer to the bottom of the flask when the stopper is fitted into the flask. Attach nearly 1 g of aluminium foil to the bottom end of the rod by coiling it around the rod. Insert the stopper, carrying the rod with foil and delivery tube, into the flask in such a way that the foil is near the bottom of the flask at the same time that the long end of the delivery tube is near the bottom of a 250-ml beaker containing about 150-ml of sodium bicarbonate solution.

A-2.3.3 Heat the flask as soon as the dissolution of aluminium is complete to gentle boiling for 3 to 5 minutes without disturbing the assembly. Cool to 60°C by partial immersion in water and siphon the sodium bicarbonate solution into the flask giving an atmosphere of carbon dioxide over the reduced titanium solution. Withdraw the stopper, rinse the glass rod attached to it with a little water catching the rinsings in the flask. Add 2 ml of ammonium thiocyanate indicator solution and titrate immediately against standard ferric ammonium sulphate solution to a straw coloured end point.

A-2.4 Calculation

Titanium ~dioxide, Vx E x 100 percent by mass =

M

where

V = volume in ml of ferric ammonium sulphate solution used in test,

E = titanium dioxide equivalent ( see A-2.2.7 ) of ferric ammonium sulphate solution in g/ml, and

M = mass in g of material taken for test.

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APPENDIX B [ Table 1, SZ .No. (viii) ]

DETERMINATION OF COPPER

B-l. REAGENTS

B-l.1 Standard Copper Sulphate Solution - Weigh 0’393 0 g of copper sulphate ( CuS04.5H@ ) into a small beaker and dissolve in water. Cautiously add 5 ml of concentrated sulphuric acid ( relative density I.84 ) and transfer to a 1 000 ml volumetric flask. Dilute to the mark and shake to ensure homogeneity. Pipette 10 ml of this solution into a loo-ml volumetric flask, dilute to the mark with water and mix. Each millilitre of the final solution contains 0’000 01 g copper ( as Cu ).

B-1.2 Concentrated Hydrochloric Acid - Relative density l-19 (see IS : 265-1962* ).

B-l.3 Nitric Acid - relative density 1’40 ( see IS : 264-19687 ).

B-l.4 Citric Acid Solution - Dissolve 10 g of citric acid in 100 ml of water.

B-l.5 Ammonium Hydroxide Solution

B-l.6 Sodium Diethyldithiocarbamate - Moisten about 0.01 g of gum tragacanth with about 1 ml of acetone and pour into 1 litre of boiling water. When cool, dissolve in this solution 1 g of sodium diethyldithiocarbamate.

B-2. PROCEDURE

B-2.1 Weigh 5 g of the sample, accurately weighed, into a 200-ml beaker, add 200 ml of concentrated hydrochloric acid and 4 ml of concentrated nitric acid. Cover with glass and heat for one hour with occasional stirring. Dilute to 40 ml with water and add 10 ml of citric acid solution followed by ammonium hydroxide, added dropwise, until the solution is just alkaline to litmus and then 2 ml in excess. and allow to stand for 15 to 20 minutes in warm place.

Bring to boil Filter into a

lOO-ml Nessler cylinder, wash with distilled water until the volume of the filtrate is 70 to 80 ml. Add 10 ml of sodium diethyldithiocarbamate solution and make up to 100 ml with distilled water.

B-2.2 Prepare a blank solution from the same quantities of reagents diluted to 100 ml in a second Nessler cylinder.

*Specification for hydrochloric acid ( rcuised). tspecification for nitric acid ( first rcuision ).

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IS:8862 -1978

B-2.3 By means of a burette add standard copper sulphate solution to the blank, and equal volumes of water to the sample solution until the colour intensities in the two cylinders are identical. Note the volume of copper solution required.

B-3. CALCULATION

B-3.1 Calculate the copper content as follows:

Copper content, percent by mass

I’ )i O*OOl =--_---- M

where

V = volume in ml of standard copper solution required, and

M = mass in g of the sample taken.

APPENDIX C [ Table 1, Sl JVO. (ix) ]

DETERMINATION OF IRON

C-l. REAGENTS

C-l.1 Dilute Hydrochloric Acid - approximately 0.2 N.

C-1.2 Concentrated Hydrochloric Acid - relative density 1.19 ( see IS : 265-1962* ).

C-1.3 Ammonium Persulphate - solid.

C-1.4 Butanolic Potassium Thiocyanate - Dissolve about 10 g of potassium thiocyanate in 10 ml of water at 27 f 2°C. Add n-butyl alcohol to make up to 100 ml and shake vigorously until the solution is clear.

G-I.5 Dilute SulphurZc Acid - 10 percent ( u/v ).

G-I.6 Standard Iron Solution - Dissolve 0.702 g of ammonium ferrous sulphate [ (NH4)2SOIr.FeSO,.GH~O ] in 20 ml of water con- taining 5 ml of concentrated sulphuric acid and dilute with water to 1000 ml. One millilitre of the solution contains 0.1 mg of iron (as Fe).

*Specification for hydrochloric acid (-rrvised ).

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C-2. PROCEDURE

C-2.1 Take approximately 5 g of moisture free sample of titanium dioxide weighed accurately to O-001 g in a 400-ml beaker and boil with 20 ml of dilute hydrochloric acid, till a little acid ( approximately 5mml) is left. Further add 15 ml of concentrated hydrochloric acid and slowly boil till some acid is left as before. Add 20 ml of distilled water and boil for 5 minutes. Filter hot through a filter paper ( Whatman No. 42 or equivalent ) collecting the filtrate in a 400-ml beaker. If the filtrate appear turbid, filter again through the same filter paper, collect- ing the filtrate in another 400-ml beaker. Wash the residue in filter paper several times with hot water, till a drop of washing is neutral to blue litmus paper. Evaporate the total filtrate to less than 75 ml, cool to room temperature and transfer to a loo-ml volumetric flask. Wash the beaker and transfer the washings to loo-ml flask and make up the volume.

C-2.2 Take 20 ml of the solution from the volumetric flask in a Nessler cylinder. Add 30 mg of ammonium persulphate and 15 ml of butanolic potassium thiocyanate and make up to 50 ml. Shake vigorously for 30 seconds and allow the liquids to separate. Carry out a control test in the second Nessler cylinder using 4 ml of standard iron solution and the same quantities of other reagents in the same volume of the reaction mixture. Match the colour produced in the butanol layers after 2 minutes.

C-2.3 The limit prescribed shall be taken to have not been exceeded if the intensity of colour with the sample is not greater than that in the control test.

APPENDIX D [ l-able 1, 5’2 No. (x) ]

SOLUBILITY IN MIXTURE OF SU’3vPHURIC ACID AND AMMONIUM SULPHATE

D-l. PROCEDURE

D-l.1 Dissolve O-2 g of the titanium dioxide in a mixture of 25 ml of concentrated sulphuric acid and 10 g of ammonium sulphate. Add a few drops of hydrogen peroxide. Deep orange colour should develop.

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Page 18: IS 8862 (1978): Titanium Dioxide (Anatase Type) for Rubber ... · FOR RUBBER INDUSTRY 0. FOREWORD 0.1 This Indian Standard was adopted by the Standards Institution on 10 July 1978,

IS : 8862 - 1978

( Continued from page 2 )

Members Rcpresen t ing

SHRI J. N. GHOSA;L Pturdia Chemicals Ltd, Bombay SHRI H. C. VIJAYANATH ( Alternate )

SHRI C. S. INAMDAR Cosmos India Rubber Works Pvt Ltd, Bombay SHRI SEN GUPTA ( Alternate )

SHRI S. M. MEHTA Camphor & Allied Products Ltd, Bareilly SWRI S. N. MEHRA ( Alternate )

SHRI S. C. NANDY Bata India Ltd, Calcutta SHRI S. SARKAR ( Ahrnntc )

DR V. S. VIJAYAN NAYAR Travancore Titanium Products Ltd, Trivandrum SHRI M. M. PATEL Synthetics & Chemicals Ltd, Bombay

SHRI R. P. DUBEY ( Alt.-mate) SHRI V. D. PENDSE Swastik Rubber Products Ltd, Pune

SHRI S. V. TATHAWADKAR ( Alternate ) SHRI P. S. PRATAP I. A. & I. C. Pvt Ltd, Bombay

SHRI C. N. VYAS ( Alternate ) SHRI R. ROY CHOWDHURY Philips Carbon Black Ltd, Calcutta DR S. M. SHETTY Canara Rubber Products Pvt Ltd, Mangalore SHRI D. V. WITTENBAKER Waldies Limited, Calcutta

SHBI A. DEB ( Altcrnate )

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