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है”ह”ह

IS 8767 (1978): Calcium carbonate, precipirated andactivated for paints [CHD 20: Paints, Varnishes and RelatedProducts]

IS : 8767 - 1978 ( Reaffirmed 2009 )

Indian Standard SPECIFICATION FOR

CALCIUM CARBONATE, PRECIPITATED, AND ACTIVATED, FOR PAINTS

Second Reprint OCTOBER 2007 ( Including Amendment No. 1 )

UDC 667.622.114 : 262.2

© Copyright 1978 BUREAU OF I N D I A N S T A N D A R D S MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

Gr 4 August 1978

AMENDMENT NO. 1 NOVEMBER 1987

TO

IS:8767-1978 SPECIFICATION FOR CALCIUM CARBONATE, PRECIPITATED AND ACTIVATED, FOR PAINTS

[ Page 5, Table 1, Sl No, ( i i i ) , c o l 2) -

a) Add the symbol ' + ' a f t e r Oi l abso rp t ion .

b) Add the fo l lowing foo t -no te at the end of the t a b l e :

'+Thie s h a l l , however, be wi th in ± 10 percent of t he approved sample, i f any. '

( CDC 50 ) Printed at Simco Printing Press Delhi, India

IS : 8767 - 1978

Indian Standard SPECIFICATION FOR

CALCIUM CARBONATE, PRECIPITATED, AND ACTIVATED, FOR PAINTS

Raw Materials for Paint Industry Sectional Committee, CDC 50

Chairman

DR R. J . RATHI

Members

SHRI K. L. RATHI ( Alternate to Dr R. J. Rathi )

SHRI S. K. ASTHANA SHRI S. PANDEY ( Alternate )

SHRI S. BHATTACHARYYA

SHRI C. J. BHUMKAR CHEMIST & METALLURGIST-II,

RDSO ASSISTANT RESEARCH OFFICER-II ,

RDSO ( Alternate ) SHRI G. C. DESAI

SHRI M. R. NAIR ( Alternate ) SHRI S. H. DESAI

SHRI R. R. SEQUEIRA ( Alternate ) SHRI O. P. DHAMIJA

SHRI S. N. DATTA ( Alternate ) SHRI G. S. GILL

DR P. K. BHANDARI ( Alternate ) SHRI R. D. KAWATRA

SHRI KULTAR SINGH ( Alternate ) SHRI A. S. KHANNA SHRI T. K. S. MANI

SHRI M. B. SATAYANARAYANA SHRI V. M. NACHANE

DR S. D. YADAV ( Alternate ) SHRI V. C. PANCHAMIYA SHRI B. RAMAMURTI

DR V. S. VIJAYANNAIR ( Alternate ) DR B. SANYAL

SHRI K. K. CHOUDHARY ( Alternate )

Representing

Sudarshan Chemical Industries Ltd, Pune

Ministry of Defence ( DGI )

The Alkali & Chemical Corporation of India Ltd, Calcutta

Asian Paints ( India ) Ltd, Bombay Railway Board ( Ministry of Railways )

Goodlass Nerolac Paints, Bombay

Blundell Eomite Paints Ltd, Bombay i

Export Inspection Council of India, Calcutta

Indian Paint Association, Calcutta

Directorate General of Technical Development, New Delhi

Oil Technologists' Association of India, Kanpur Addisons Paints & Chemicals Ltd, Madras

( Alternate ) Chowgule & Co ( Hind ) Ltd, Bombay

Kamani Metallic Oxides Pvt Ltd, Bombay Travancore Titanium Products Ltd, Trivandrum

Ministry of Defence ( R & D )

( Continued on page 2 )

© Copyright 1978

BUREAU OF INDIAN STANDARDS This publication is protected under the Indian Copyright 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 : 8767 - 1978

( Continued from page 1 )

Members SHRI P. SATYANARAYANAN

SHRI K. C. SEAL SHRI K. S. THAKUR SHRI R. M. TILLU

Representing Development Commissioner ( Small Scale Industries ),

New Delhi National Test House, Calcutta Hindustan Petroleum Corporation Ltd, Bombay Colour Chem Ltd, Bombay

SHRI M. E. MARATHE ( Alternate ) SHRI M. VAITHYANATHAN Indian Dyestuff Industries Ltd, Bombay

SHRI V. R. KARMAKAR ( Alternate ) DR G. M. SAXENA,

Director ( Chem ) Director General, ISI ( Ex-officio Member )

Secretary SHRI R. K. SINGH

Deputy Director ( Chem ), ISI

Pigments and Extenders Subcommittee, CDC 50 : 1 Convener

SHRI K. C. SEAL

Members SHRI S. K. ASTHANA

SHRI A. A. KHAN ( Alternate ) SHRI G. C. DESAI SHRI S. H. DESAI

National Test House, Calcutta

Ministry of Defence ( DGI )

Goodlass Nerolac Paints Ltd, Bombay Blundell Eomite Paints Ltd, Bombay

DR P. G. CHAUDHARI ( Alternate ) SHRI J. N. GHOSAL Sturdia Chemicals Ltd, Rishikesh (UP)

SHRI H. S. VIJAYANATH ( Alternate ) SHRI M. M. GHOSH SHRI V. C. PANCHAMIYA SHRI K. L. RATHI

SHRI H. J . RATHI ( Alternate ) SHRI SUKESH BOSE SHRI R. M. TILLU

Shalimar Paints Ltd, Calcutta Kamani Metallic Oxides Pvt Ltd, Bombay Sudarshan Chemical Industries Ltd, Pune

British Paints India Ltd, Calcutta Colour Chem Ltd, Bombay

SHRI M. E. MARATHE ( Alternate ) SHRI P. N. WAGLE Asian Paints ( I n d i a ) Ltd, Bombay

Panel for Extenders, CDC 50 : 1 : 4 Convener

SHRI G. C. DESAI

Members SHRI V. B. MAZUMDAR ( Alternate

Shri G. C. Desai ) SHRI J. N. GHOSAL

Goodlass Nerolac Paints Ltd, Bombay

to

Sturdia Chemicals Ltd, Rishikesh (UP) SHRI H. S. VIJAYANATH ( Alternate )

SHRI M. M. GHOSH DR R. GOPALAN

SHRI R. K. MANDAN ( Alternate ) SHRI K. S. MEHTA

Shalimar Paints Ltd, Calcutta The Hindustan Mineral Products Co Pvt Ltd, Bombay

Bharat Pulverising Mills Pvt Ltd, Bombay SHRI T. REGHUNANDAN ( Alternate )

SHRI P. N. WAGLE Asian Paints ( India ) Ltd, Bombay

2

IS : 8767 - 1978

Indian Standard SPECIFICATION FOR

CALCIUM CARBONATE, PRECIPITATED, AND ACTIVATED, FOR PAINTS

0. F O R E W O R D

0.1 This Indian Standard was adopted by the Indian Standards Institution on 15 March 1978, after the draft finalized by the Raw Materials for Paint Industry Sectional Committee had been approved by the Chemical Division Council.

0.2 Calcium carbonate, in the form of a fine dry powder, is used as an extender in paint formulations. IS : 63-1961* covers specification for whiting, a naturally occurring form of calcium carbonate used as an ex­tender in paint industry. IS : 2468-1963† covers whiting meant for manu­facture of putty. Precipitated and activated calcium carbonates in the chemically processed form are not so far covered in any Indian Standard for paints. In the light of recent experience in selection and use of exten­ders in paint industry and in view of chemically processed form of calcium carbonate coming into prominence for this purpose, the formulation of this standard was taken up by the concerned technical committee to facilitate procurement of acceptable quality of precipitated and activated calcium carbonates for use as extender in paint industry.

0.3 This standard is one of the series of Indian Standards on calcium carbonate, activated, and precipitated, the other standards published so far are IS : 917-1958‡ and IS : 918-1968§.

0.4 The technical committee responsible for the formulation of this stan­dard was aware of the need for prescribing additional requirements for specific surface area and waterproofing characteristics for activated calcium carbonate. This was, however, not found possible in view of the fact that necessary testing facilities are not available commercially in the country at present. The matter would be reconsidered after such facilities become available.

0.5 This standard contains clause 5.1 which calls for agreement between the purchaser and the supplier.

*Specification for whiting for paints ( revised ). †Specification for whiting for putty. ‡Specification for activated calcium carbonate for rubber industry. §Specification for calcium carbonate, precipitated, for cosmetic industry.

3

IS : 8767 - 1978

0.6 In the preparation of this standard substantial assistance has been derived from data supplied by M/s Sturdia Chemicals Ltd, Rishikesh which is gratefully acknowledged.

0.7 For the purpose of deciding whether a particular requirement of this standard is complied with, the final value, observed or calculated, expres­sing the result of a test or analysis, shall be rounded off in accordance with IS : 2-1960*. The number of significant places retained in the rounded off value should be the same as that of the specified value in this standard.

1. SCOPE

1.1 This standard proscribes requirements and methods of sampling and test for calcium carbonate, precipitated, and activated, intended for use as extender in paint industry.

2. TERMINOLOGY

2.1 For the purpose of this standard, the definitions given in IS : 1303-1963† and IS : 33-1976‡ shall apply.

3. TYPES

3.1 The material shall be of the following two types: a) Type 1 — Calcium carbonate, precipitated; and b) Type 2 — Calcium carbonate, activated.

4. REQUIREMENTS

4.1 The material shall be in the form of fine, white microcrystalline, free flowing powder or in such a condition that it can be reduced to the powder form by crushing without grinding action, under a palette knife. In addi­tion, the activated calcium carbonate shall consist of precipitated calcium carbonate coated with a thin hydrophobic layer of fatty acids or their salts. The material shall be stable in air, free from visible impurities and shall closely resemble the approved sample in colour.

4.2 The material shall also comply with the requirements given in Table 1.

*Rules for rounding off numerical values ( revised ).

†Glossary of terms relating to paints ( revised ).

‡Methods of sampling and test for inorganic pigments and extenders for paints ( second revision ).

4

IS : 8767 - 1978

TABLE 1 REQUIREMENTS FOR CALCIUM CARBONATE, PRECIPITATED AND ACTIVATED, FOR PAINTS

( Clauses 4.2 and 7.1 )

SL No.

(1)

i)

ii)

iii) iv)

v) vi)

vii)

viii)

ix)

x)

xi)

CHARACTERISTIC

(2)

Volatile matter, percent by mass, Max

Rasidue on sieve, percent by mass, Max

Oil absorption Matter soluble in water

( by cold extraction method ), percent by mass, Max

pH value Bulk density

Particle size distribution, percent by mass, finer than 10 microns, Min

Loss on ignition, percent by mass

Insoluble siliceous matter, percent by mass, Max

Calcium carbonate ( as CaCO3 ), percent by mass, Min

Total fatty matter, percent by mass

REQUIREMENT FOR

Type 1 Type 2

(3)

1.0

0.25

30 to 0.3

9 to

(4)

1.0

0.25

80 0.3

10.5 As agreed to bet­ween the purchaser and the supplier 96

43.5 to 44.5 0.2

98

—

*Methods of sampling and test for inorganic revision ) .

—

43 to 46 0.2

94

2.8 to 3.2

METHOD OF TEST, REF TO CL NO. IN

Appendix A IS : 33-1976* (5)

—

—

— –

— —

A-1

A-2

A-3

A-4

A-5

(6)

7

8

9 17

19 15

—

—

—

pigments and extenders for paints ( second

5. PACKING AND MARKING

5.1 Packing — The material shall be packed as agreed to between the purchaser and the supplier.

5.2 Marking — The packages shall be securely closed and marked with the following particulars:

a) Name and type of the material;

b) Name of the manufacturer or his recognized trade-mark, if any;

5

IS : 8767 - 1978

c) Mass of the material; d) Batch No. or Lot No. in code or otherwise; and e) Month and year of manufacture.

5.2.1 The packages may also be marked with the Standard Mark.

NOTE — The use of the Standard Mark is governed by the provisions of the Bureau of Indian Standards Act, 1986 and the Rules and Regulations made thereunder. The Standard 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 BIS and operated by the producer. Standard marked products are also continuously checked by BIS for conformity to that standard as a further safeguard. Details of conditions under which a licence for the use of the Standard Mark may be granted to manufacturers or producers may be obtained from the Bureau of Indian Standards.

6. SAMPLING

6.1 Preparat ion of T e s t S a m p l e s — Representative samples of the material shall be drawn as prescribed under 4 of IS : 33-1976*.

6.2 Criteria for Conformity — A lot shall be declared as conforming to the requirements of this standard if test results of the composite sample satisfy the requirements prescribed under 4.

7. TESTS

7.1 Tests shall be conducted as prescribed in Appendix A and IS : 33-1976*. Reference to relevant clauses of Appendix A and I S : 33-1976* are given in col 5 and 6 of Table 1 respectively.

7.2 Quality of Reagents — 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 results of analysis.

A P P E N D I X A ( Table 1 and Clause 7.1 )

METHODS OF TEST FOR PRECIPITATED AND ACTIVATED CALCIUM CARBONATE FOR PAINTS

A-1. DETERMINATION OF PARTICLE SIZE DISTRIBUTION

A-1.0 Because of the ease of execution and good reproducibility the Andreasen method is included as the referee method. Other methods may,

*Methods of sampling and test for inorganic pigments and extenders for paints ( second revision ).

†Specification for water for general laboratory use ( second revision ).

6

IS : 8767 - 1978

however, be used by agreement between the concerned parties, but in such cases it will be necessary also to agree on appropriate limits.

A-1.1 Principle — The rate of fall of spherical particles through a medium in which they are dispersed is proportional to the square of the particle diameter ( Stokes' law ). The Andreasen method for determination of particle size distribution makes use of this relationship and expressed the particle size distribution in terms of distribution of spherical particles of the same settlement rate. In this determination, a dilute suspension is prepared and the concentration of solids at a fixed point below the surface is determined at a series of time intervals calculated to correspond to certain equivalent spherical diameters.

A-1.2 Apparatus — See Fig. 1.

A-1.2.1 Sedimentation Vessel — of glass about 56 mm internal diameter and having a graduated scale from 0 to 200 mm marked on its side. The zero graduation line shall not be less than 25 mm from the inside base of the vessel and the capacity of the vessel up to the 200 mm mark shall be about 550 to 620 ml.

A-1.2.2 Pipette — fitted with a two-way tap and side discharge tube. The capacity of the pipette to the graduation line is conveniently 10 ml. A bell-shaped dome with a ground glass joint to fit the neck of the sedimen­tation vessel is fused to the pipette. A small vent hole is made in this dome. The inlet to the pipette stem shall be level with the zero line on the sedimentation vessel. The stem from the pipette bulb to the sampling inlet shall be constructed of capillary glass tubing with a bore not less than 1 mm and not more than 1.3 mm. The tube above the bulb shall be 4 to 4.5 mm bore.

A-1.2.3 Constant-Temperature Bath — transparent-sided of at least 15-litres capacity, maintained at a temperature of 27 ± 0.5°C, into which the sedimentation vessel can be immersed up to the 200 mm graduation mark. The bath shall be positioned away from sources of vibration.

A-1.2.4 Mechanical Stirrer — capable of rotating at a suitable speed for complete dispersion ( 1 000 ± 100 rpm is generally suitable ). The stirrer shall be designed to lift the dispersion and to avoid the creation of a vertex.

NOTE — A suitable stirrer may be made from an approximately 40 mm diameter brass disc with four equally spaced cuts, the cut sections being turned upwards at an angle of 30° to the horizontal.

A-1.2.5 Dispersion Vessel — of appropriate dimensions, such as a 1 000-ml gas jar.

A-1.2.6 Balance — having a sensitivity of not less then 0.1 mg.

7

IS : 8767 - 1978

FIG. 1 SEDIMENTATION VESSEL AND PIPETTE

8

IS : 8767 - 1978

A-1.2.7 Drying Oven — capable of being maintained within a tempera­ture range suitable for evaporation of the suspending liquid, for example, 105 ± 2°C for water.

A-1.2.8 Weighing Bottles — wide-mouthed, suitable for evaporation, of capacity not less than 20 ml, or a small laboratory centrifuge and centri­fuge tubes preferably of 20-ml capacity but of not less than 10-ml capacity.

A-1.2.9 Stop-Watch or Stop-Clock

A-1.3 Preparation for the Test A-1.3.1 Calibration of Pipette — Thoroughly clean the pipette. Partly

fill the sedimentation vessel with water. Set the top in the sampling position and by means of a rubber tube suck water into the bulb to the level of the graduation line. Reverse the tap to the discharge position and allow the water to drain into a tared weighing bottle. Apply pressure through the rubber tube to blow any water remaining in the bulb and the discharge tube into the weighing bottle. Weigh the bottle to the nearest 0.001 g and calculate from this mass the internal volume Vp of the pipette.

A-1.3.2 Calibration of Sedimentation Vessel — Thoroughly clean the sedimentation vessel, weigh it, with the pipette in place, to the nearest 0.1 g. Then fill it to the 200 mm mark with water at 27 ± 0.5°C and reweigh. Calculate from the mass of water the internal volume Vs of the vessel.

A-1.3.3 Sample for Analysis — Using 3.5 g of accurately weighed material with 0.07 to 0.14 g of suitable dispersing materials ( see Note ), prepare a dispersion by placing the test portion in the dispersion vessel adding dis­persion solution at 27 ± 0.5°C to give a total volume of about 500 ml and stirring with the mechanical stirrer for 15 minutes. Immediately pour all the suspension into the sedimentation vessel and make up to the 200 mm line with water or aqueous alcohol as appropriate. Transfer the sedimen­tation vessel to the constant temperature bath.

NOTE — Certain sodium salts of polymethacrylates have been found most suitable. Such materials are sold as polysalts, dispex, etc.

A-1.4 Procedure A-1.4.1 Sedimentation — Allow the sedimentation vessel to stand immersed

to the 200 mm mark until it has reached the temperature of the bath. Record this temperature, which shall not differ greatly from that of the room. When temperature equilibrium has been attained, mix the contents thoroughly by placing a finger over the vent hole and inverting the vessel several times. Immediately after mixing, replace the vessel and start the stop-clock or stop-watch.

A-1.4.2 Withdraw from the suspension by means of the pipette a series of samples of volume Vp at depths hn at increasing time intervals after

9

IS : 8767 - 1978

mixing, starting at time t1 corresponding to a particle size of about 20 μm ( calculated in accordance with A-1.4.3 ) and thereafter in progression so that the limiting diameters stand in a 2:1 progression. Alternatively, the samples may be taken at convenient times approximately in a 2 : 1 progression and the exact spherical particle diameters corresponding to each sample calculated. The time to fill the pipette shall be about 20 seconds.

A-1.4.3 Discharge the suspension from the pipette into a tared weighing bottle. When the bulb has drained, remove the rubber suction tube and run 5 to 7 ml of water from an ordinary 10 ml pipette into the bulb of the sedimentation pipette to wash into the weighing bottle any particles adhering to the surface. The stem of the sedimentation pipette shall remain filled with suspension. Dry the contents of the weighing bottle at 105°C until the difference between successive weighings is not greater than 0.1 mg. Calculate the mass of the fraction mn allowing for the mass of dispersing agent, which shall be determined by carrying out a blank test. The determination of different fractions may be carried out by means of chemical methods if that procedure is more suitable.

A-1.4.4 The depth of immersion of the pipette decreases as each fraction is withdrawn. Determine the exact decrease in depth by experiment and allow for it in the subsequent calculation. Suppose that the decrease is 4 mm for each fraction withdrawn, and that initially the depth of immersion of the pipette was 200 mm, then the depth after the first fraction has been withdrawn will be 196 mm, and the mean depth h1 used for calculation of the initial diameter corresponding to the first fraction will be 198 mm. The mean depth h2 for the second fraction will be 194 mm, and so on.

A-1.4.5 Calculation of Withdrawal Time — The withdrawal time, tn, in seconds, for the nth sample is given by the equation:

where

η = absolute viscosity, in newton seconds per square metre, of

the medium;

hn = depth, in millimetres, at which the nth sample extraction

is made;

p1 = density, in megagrams per cubic metre, of the medium;

p2 = density, in megagrams per cubic metre ( or g/cm3 ) of the particle;

g = acceleration due to gravity, in metres per second square; and

dn = limiting stokes diameter, in micrometres, corresponding to the nth sample extraction.

10

IS : 8767 - 1978

A-1.5 Calculation of Cumulative Percentage Undersize — The cumulative percentage by mass, Pn, of particles smaller than each of the limiting stokes diameter dn for each time interval tn is given by the formula;

where mn = mass in g of the fraction corrected for the mass of the

dispersing agent, Vs = volume in ml of the sedimentation vessel, ms = mass in g of the test portion, and Vp = volume in ml of the pipette.

A-1.6 Repetition of Test — Repeat the procedure on a further amount of suspension prepared from the same sample. The results of the test shall be accepted only if the percentages by mass, less than the same limiting stokes diameter, do not differ by more than 4 percent.

A-1.7 Expression of Results — Plot the results of the analysis with the micrometric sizes as abscissae and the percentages undersize as ordinates. From the smooth curve drawn through the points, select the cumulative percentages corresponding to the series required. Repeat the results to the nearest 1 percent.

A-2. DETERMINATION OF LOSS ON IGNITION

A-2.1 Procedure — Weigh accurately about 1 g of the test sample, previously dried at 100 ± 2°C to constant mass into a platinum crucible. Heat the crucible, along with its contents at a temperature of 1 000 ± 25°C in a muffle furnace and ignite for 2 hours, cool in a desic­cator containing phosphorus pentoxide and weigh. Repeat heating, cooling and weighing till constant mass is obtained. Express the loss in mass as the percentage of material taken for the test.

NOTE — Care should be taken to avoid hydration of the quicklime formed.

A-3. DETERMINATION OF INSOLUBLE SILICEOUS MATTER

A-3.1 Reagents

A-3.1.1 Concentrated Hydrochloric Acid

A-3.1.2 Concentrated Sulphuric Acid

A-3.1.3 Hydrofluoric Acid — approximately 40 percent by volume.

11

IS : 8767 - 1978

A-3.2 Procedure — Weigh accurately about 5 g of previously dried test sample and ignite as in A-2.1. Add slowly concentrated hydrochloric acid to dissolve the material. Dilute it to 300 ml, allow to stand for 10 minutes and then filter. Wash the residue with water until free from chlorides ( when tested with silver nitrate solution, the washings should not turn milky ). Ignite the residue with filter paper in a platinum crucible. Cool the crucible, add two drops of concentrated sulphuric acid and then heat to constant mass. Cool in a desiccator and weigh. Add to this, one or two drops of concentrated sulphuric acid and 6 to 7 ml of hydrofluoric acid in two instalments. Dry and then ignite at a temperature of about 850°C for 2 hours, cool it in a desiccator and weigh. Repeat heating, cooling and weighing till constant mass is obtained.

A-3.3 Calculation

Insoluble siliceous matter, percent by mass =

where A = mass in g of the residue after treatment with concentrated

sulphuric acid, B = mass in g of the residue after treatment with concentrated

sulphuric acid and hydrofluoric acid, and

m = mass in g of the sample taken for test.

A-4. DETERMINATION OF CALCIUM CARBONATE

A-4.0 Methods — Two methods have been prescribed for this test, namely, Method A and Method B. Method A is the classical method and Method B is the complexometric method. In case of dispute Method A shall be followed.

A-4.1 Method A

A-4.1.0 Outline of the Method — Calcium is precipitated as its oxalate and dissolved in dilute sulphuric acid and the solution is titrated against permanganate solution.

A-4.1.1 Reagents

A-4.1.1.1 Dilute hydrochloric acid — approximately 5 N.

A-4.1.1.2 Ammonium oxalate solution — saturated.

A-4.1.1.3 Dilute ammonium hydroxide — approximately 5 N and 1 N.

A-4.1.1.4 Dilute potassium permanganate solution — 0.01 N ( approxi­mately ).

12

IS : 8767 - 1978

A-4.1.1.5 Dilute sulphuric acid — approximately 5 N.

A-4.1.1.6 Standard potassium permanganate solution — 0.1 N.

A-4.1.2 Prepared Sample Solution — Weigh accurately about 1 g of sample, previously dried at 100 ± 2°C, into a platinum crucible and ignite as in A-2.1 Transfer the contents of the crucible completely to a 250 ml beaker with a jet of water from a wash bottle. Rinse the crucible with a few millilitres of dilute hydrochloric acid to detach particles adhering to the crucible. Continue addition of acid to the beaker until a total of 40 ml of acid has been added. Heat the solution and boil for about 10 minutes. Cool and transfer completely to a 200-ml graduated flask, add water to make up the volume and mix thoroughly.

A-4.1.3 Procedure — Pipette out 50 ml of the prepared sample solution into a beaker and add 75 ml of water. Heat almost to boiling and add 15 ml of ammonium oxalate solution. To the hot solution, constantly stirred, add dilute ammonium hydroxide (5 N) dropwise until the mixture is strongly alkaline. Let it stand for two hours. Decant the supernatant liquid through a filter paper. Transfer all the precipitate from beaker to the filter paper by addition of cold water. When all the precipitate has been transferred, wash the precipitate in the filter paper first with dilute ammonium hydroxide (1N) and then with cold water until the filtrate does not decolourize dilute potassium permanganate solution in presence of dilute sulphuric acid. Puncture the filter paper and transfer the precipitate to a beaker with a fine jet of hot water. Add about 30 ml of dilute sulphuric acid, heat at 60°C and titrate with standard potassium permanganate solution. Towards the end of the titration introduce the filter paper which was used for filtration into the titration vessel and carry out the titration till the end point is reached. Carry out a blank test with all reagents, following the procedure for the test but without the material.

A-4.1.4 Calculation

Calcium carbonate ( as C2C03 ), percent by mass =

where V1 = volume in ml of standard potassium permanganate

solution used for the test, V2 = volume in ml of standard potassium permanganate solu­

tion used for the blank test,

N = normality of standard potassium permanganate solution, and

M = mass in g of the material taken for the test.

13

IS : 8767 - 1978

A-4.2 Method B

A-4.2.0 Outline of the Method —- The solution of the material, after adjustment of pH, is titrated with EDTA solution using murexide indicator.

A-4.2.1 Reagents

A-4.2.1.1 Dilute hydrochloric acid — approximately 5 N.

A-4.2.1.2 Dilute sodium hydroxide solution — approximately 1 N.

A-4.2.1.3 Standard calcium carbonate solution — 0.01 N. Weigh 0.500 4 g of calcium carbonate, dried at 110°C, and dissolve in the minimum quantity of dilute hydrochloric acid. Make up the volume with water to 1 litre.

A-4.2.1.4 Murexide indicator — Triturate 0.2 g of murexide with 50 g of potassium chloride until a homogeneous mixture is obtained.

A-4.2.1.5 Standard disodium ethylenediamine tetra-acetate ( EDTA ) solution — Weigh 3.7 g of disodium ethylenediamine tetra-acetate dihydrate and dissolve in water. Make up the volume to 1 litre. Standardize the solution against standard calcium carbonate solution as under A-4.2.1.3.

A-4.2.2 Prepared Sample Solution — Weigh accurately about 3 g of previ­ously dried test sample into a platinum crucible and ignite as in A-2.1. Transfer the contents of the crucible completely to a 250-ml beaker with a jet of water from a wash bottle. Rinse the crucible with a few millilitres of dilute hydrochloric acid to detach particles adhering to the crucible. Continue addition of acid to the beaker until a total of 30 ml has been added. Heat the solution and boil for about 10 minutes. Cool and transfer quantitatively to a 500-ml graduated flask. Pipette out 100 ml of this solution and dilute further to 1 litre. Use this diluted solution for test as under A-4.2.3.

A-4.2.3 Procedure — Pipette out 10 ml of the prepared sample solution into a 250 ml conical flask. Add 25 ml of water and 10 ml of dilute sodium hydroxide solution ( pH of the mixture should be more than 12 ). Add 0.3 g of murexide indicator and titrate with standard EDTA solution until the colour changes from red to distinct blue violet.

A-4.2.4 Calculation

Calcium carbonate ( as CaCO3 ), percent by mass =

where V = volume in ml of standard EDTA solution,

N = normality of standard EDTA solution, and M = mass in g of the material taken for the test as in A-4.2.2.

14

IS : 8767 - 1978

A-5. DETERMINATION OF TOTAL FATTY MATTER

A-5.1 Reagents

A-5.1.1 Ether

A-5.1.2 Hydrochloric Acid — approximately 5 N.

A-5.1.3 Acetone

A-5.2 Procedure — Weigh accurately about 5 g of the material in a 400-ml beaker and wet the material by adding a little ether. Cover with a cover-glass and carefully add ( a few millilitres at a time ) 50 ml of hydro­chloric acid. Boil, dilute to about 100 ml with water and cool to room temperature. Transfer to a 300-ml separating funnel, rinse out the beaker with 25 ml of ether and transfer to the separating funnel. Shake gently, release the pressure by inverting the funnel and gradually open the tap. Allow the two layers to separate completely, then run off the aqueous layer into the original beaker. Filter the ether layer through a dry filter paper into a tared conical flask. Transfer the aqueous layer back into the separa­ting funnel and extract twice as before but using 15 ml portions of ether. Filter the combined ether extracts also through the same filter paper and collect the filtrate in the tared conical flask. Finally wash the filter paper with ether, distil the ether until only 5 ml remains in the flask, then add about 5 ml of acetone and evaporate the mixture on a water bath. Dry the residue at 60°C. In order to reduce the drying time to about 15 minutes and minimize volatilization and oxidation of fatty acid, blow through the flask a gentle current of an inert gas two or three times during drying. Cool the flask in a desiccator and reweigh.

A-5.3 Calculation

Total fatty matter, percent by mass =

where A = mass in g of the conical flask containing the dried residue, B = mass in g of the conical flask, and

M = mass in g of the material taken for test.

15

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