IS 15751: Calcite for ceramic industry

2007·1.2 MB·English

by  Bureau of Indian Standards

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IS 15751 (2007): Calcite for ceramic industry [CHD 9:
Ceramicware]
“!ान $ एक न’ भारत का +नम-ण”
Satyanarayan Gangaram Pitroda
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IS 15751:2007
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Indian Standard
CALCITE FOR CERAMIC INDUSTRY —
SPECIFICATION
ICS 73.060.01; 81.060.01

@ BIS 2007
BUREAU OF INDIAN STANDARDS
MANAK EIHAVAN, 9 BAHADIJR SHAH Z.AFAR MARC
NEW DEL HI I10002”
1[//1(’2007”
Price Group 3
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Ceramicware Sectional Committee, (2HD 9
FOREWORD
This Indian Standard was adopted by the Bureau of Indian Standards, after the draft finalized by the Ceramicware
Sectional Committee had been approved by the Chemical Division Council.
Calcite, the essential mineral in limestone is a naturally occurring calcium carbonate having formula CaCOl,
consisting of 56.03 percent CaO and 43.97 percent C02. Itisnormally white incolour and soft, the hardness being
only 3 in Mohr’s scale. In pottery, calcite is used in glazes. It is used in the manufacture of silica refractories as
mineralizer. In glass industry, it is one of the major raw materials used to introduce CaO in a soda-lime-silica
glass. Calcium oxide increases the mechanical hardness and tensile str-ength of glass and glaze and improves its
durability to acids and to water. In a glaze with abaianced composition, an increase in calcium oxide can reduce
the coefficient of thermal expansion.
This standard contains 4.2, 4.3 and 5.1 which provide for agreement between the purchaser and the supplier,
‘1’hecomposition of the Committee responsible for formulation of this standard is given inAnnex D.
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 ‘Rules for rounding off numerical values (revised)’. The number of significant places retained in the
rounded off value should be the same as that of the specified value inthis standard.
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IS 15751:2007
Indian Standard
CALCITE FOR CERAMIC INDUSTRY —
SPECIFICATION
1 SCOPE 4.3 Si~e
This standard prescribes the requirements and the The grain sizes ofmaterial shall be asagreed tobebveen
methods of sampling and test for calcite suitable for the purchaser and the supplier.
use in ceramic industry. NOTE—Normally,forceramicindustrythegrainsizeisfiner
than 150micron, However,thelumpsmayalsobesupplied.
2 REFERENCES
4.4 Fired Colour
The standards listed below contain provisions which,
through reference in this text, constitute provisions of The colour of fired calcite shall be white or off white.
this standard. At the time of publication, the editions
4.5 Chemical Composition
indicated were valid. All standards are subject to
revisi~n and parties i~ agreements based on this Calcite shall also comply with the requirements
standard are encouraged to investigate the possibility prescribed in Table 1when tested in accordance with
of applying the most recent editions of the standards the method prescribed in Annex B. Reference to the
indicated below. relevant clauses ofAnnex Bisgiven inCO14 ofTable 1.
[s No. Title Table 1 Requirements of Calcite for
323:1959 Specification for rectified spirit Ceramic Industry
(revised)
.9 Characteristics Requirements Methods of
1070:1992 Reagent grade water — Specification No. Test, Refto
(third revision) Clause
(1) (2) (3) (4)
2781:2004 Glossary of terms relating to
ceramicware (second revision) O Residueon 75-micronIS 1.0 B-2
sieve, percent by mass,
4905:1968 Methods for random sampling
MUX
8883 (Part 1): Methods of sam pling chemical and ii) Calcium carbonate (as 97.0 B-3
CaCO,). percent by mass,
2005 chemical product: Part 1 General
Mirz
requirements and precautions (jlrst iii) hlsolublc impurity in 3.0 B-4
revision) hydrochloric acid, percent
bymass,ML:X
3 TERMINOLOGY iv) Iron oxide (as Fe*OJ, 0.5 B-5
percentbymass,Max
For the purpose of this standard, the definitions given v) Losson ignition, percent 44.0 B-6
in IS 2781 shall apply. bymass,Max
vi) Freeiron,percentbymass, 0.05 B-7
M<(X
4 REQUIREMENTS
4.1 Description 5 PACKING AND MARKING
The material shall be in the form of powder or lumps 5.1 Packing
prepared from natural occurring calcite rocks. It shall
The material shall be packed injute bags or as agreed
be free from foreign matter.
to between the purchaser and the supplier.
4.2 Moisture Content
5.2 Marking
Uniess otherwise agreed to between the purchaser and
5.2.1 Each bag shall be marked with the following:
the ~,ljpplier,the moisture content, as received shall not
excecd 2 percent by mass, when determined by the a) Nunc of the manufacturer or his recognized
method prescribed inAnnex A. tr!de-mark, if any;
1
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IS 15751:2007
b) Net mass of content; 6 SAMPLING AND CRITERIA FOR
c) Grain size; CONFORMITY
d) Lot number or batch number in code or 6.1 The representative sample shall be drawn as
otherwise; and prescribed inAnnex C.
e) Month and year of manufacture.
6.2 Test Sample
5.2.2 BIS Certification Marking
Grind.5 to 10g of the sample in a porcelain mortar so
The bags may also be marked with the Standard Mark. that itpasses through 75 micron sieve. Dry to aconstant
mass at 105* 2°C and use itfor thepurpose ofchemical
5.2.2.1 The use of the Standard Mark is governed by
analysis.
the provisions of the Bureau of Indian Standards Act,
1986 and the Rules and Regulations made thereunder.
6.3 Criteria for Conformity
The details of conditions under which the licence for
the use of the Standard Mark may be granted to The lot shall be declared as conforming to the
manufacturers or producers maybe obtained from the requirements ofthis standard, ifall the test results meet
Bureau of Indian Standards. the relevant requirements.
ANNEX A
(Clause 4.2)
DETERMINATION OF MOISTURE CONTENT
A-O PROCEDURE A-1 CALCULATION
M–M, XIOO
Weigh accurately nearest to 0.01 g, about 20 g of the Moisture content, percent by mass= —
M
sample in a tared dish and dry at 105 to 11O“C in an
where
air-oven for 30 min. Cool in a desiccator and weigh.
M = mass ofthe sample taken forthe test, in g;and
Repeat heating and cooling till constant mass is
M,= mass of the sample afler drying, in g.
obtained.

ANNEX B
(Clause 4.5)
CHEMICAL ANALYSIS OF CALCITE
B-O SAMPLING AND PREPARATION OF TEST B-2 DETERMINATION OF RESIDUE ON
SAMPLE 75-MICRON IS SIEVE
B-O.1 The material shall be sampled and prepared for B-2.1 Reagent
chemical analysis as given in 6.1 and 6.2.
B-2.1.1 Ethyl Alcohol- 95 percent (v/v) (see IS 323).
B-1 QUALITY OF REAGENTS B-2.2 Procedure
B-1.1 Unless specified otherwise, pure chemicals and Place 100 gofthe material previously dried to constant
distilled water (see IS 1070) shall be used. mass at 100* 5°C inatared 75-micron IS Sieve. Wash
NOTE—‘Purechemicals’shallmeanchemicalsthat donot by means of a slow stream of running water and then

containimpurities which affecttheresults ofanalysis. with a fine jet of water from awash bottle until all the
2
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IS 15751:2007
material that can pass through the sieve has been where
washed. Wash finally with a small quantity (about
A = mass in g of crucible and CaO residue, in g;
10ml) of ethyl alcohol and then dry the sieve inan air-
and
oven maintained at 100 + 5°C to constant weight.
B = mass of empty crucible, in g.
B-2.3 Report the material on the sieve as the percent
of the air dried material taken. B-4 DETERMINATION OF INSOLUBLE
IMPURITY IN HYDROCHLORIC ACID
B-2.4 Calculation
B-4.1 Procedure
Residue on 75-micron
~x loo Take I g sample dissolved in 25 ml of concentrated
1SSieve, percent by mass =
hydrochloric acid and warm it for 30 min. Allow to
m2
where cool it.Now f~lteritwith Whatman filter paper No. 541.
Wash the filter paper with distilled water till itbecomes
m, =mass of the residue left on the sieve, in g;
clear and free from chloride. Dry the filter paper in a
and
dryer and ignite itinadried and weighed silica crucible
mz= mass of the material taken for test, in g. first at low flame and then raised the temperature for
30 min. Cool itinadessicator and calculate the percent
B-3 DETERMINATION OF CALCIUM
insoluble impurity.
CARBONATE
B-4.2 Calculation
B-3.1 Proc~dure
Insoluble impurity in
B-3.1.1 Dried sample of calcite is taken and weigh
W’3-WXIO0
0.5 g in a watch glass. Transfer the sample to 500 ml hydrochloric acid, percent by mass=
(w*-w)
beaker in which 50 ml (1:1) HC1 is added. Add 50 ml
where
distilled water and boil the solution gently toexpel C02.
Then add about 0.5 g of pure NHdCl and 2 drops of W, = weight of empty crucible,
methyl-red indicator. Heat the contents of beaker to W, = initial weight of crucible with material, and
boiling. Add slowly hot aqueous solution of 4 g Wj = final weight of crucible with material.
ammonium oxalate. Then add dilute ammonia solution
drop-wise till the colour of solution becomes just B-5 DETERMINATION OF IRON OXIDE
yellowish. Allow the precipitate to stand for 1h. Test
B-5.1 Outline of the Method
the supernatant liquid for complete precipitation with
a drop of ammonium oxalate. The orange-red complex produced in acid solution of
the sample (pH 4 to 6) by the addition of
B-3.1.2 Filter off the clean super n atant liquid through
o-phenanthroline is determined photometrically at
Whatman No. 42 filter paper fixed in a funnel. Wash
approximately 510 nm.
the precipitate 2-3 times by recantation with 0.2 percent
cold solution of ammonium oxalate. Transfer the B-5.2 Reagents
precipitate tothe filter cone and wash itwith cold dilute
B-5.2.1 Tartaric Acid Solution — 10percent (m/v).
ammonium oxalate solution until the filtrate isfree from
chloride ions (test with dilute HNO~ and AgNO~ B-5.2.2 Hydroxylarnine Hydrochloride Solution —
solution). Allow the liquid to drain off. Dissolve 1g of the reagent in water. Transfer the
solution to a 100-ml volumetric flask, dilute to the mark
B-3.1.3 Dry the precipitate by placing the funnel inan
and mix well.
air oven at 120°C or on a drying cone. Fold the filter
paper toenclose the entire precipitate. Place this packet B-5.2.3 Ortho-Phenanthroline Solution — Dissolve
inaweighed silica crucible. Ignite the paper by gentle 1gofo-phenanthroline monohydrate in90 ml ofwater
heating and then heat the crucible strongly over aburner with gentle heating and constant stirring. Cool and
flame for about 30 min. Cool the crucible first in air dilute to 100 ml.
and then inadessicator to room temperature and weigh
B-5.2.4 Acetate Buffer — Dissolve 21.5 g of the
it quickly. Repeat the process of heating, cooling and
sodium acetate (CH~COONa, 3H20) in300 ml ofwater
weighing until a constant weight is obtained.
containing 2 ml of glacial acetic acid and dilute to
1000 ml.
B-3.2 Calculation
B-5.2.5 Stundard Iron Solution — Dissolve 0.2 g of
Calcium carbonate
pure iron inconcentrated hydrochloric acid. Dilute the
(as CaCO,), percent by mass = (A-B) x%
solution to about 100 ml. Transfer to a 1000 ml
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IS 15751:2007
volumetric flask, dilute tothe mark and mix well. Dilute coloured test solution to the absorption cell and note
100mlofthis solution to 1000 ml inavolumetric flask. the photometric reading for the test solution. Convett
One millilitre of this diluted solution is equivalent to itto miIligrarns of iron by means ~fthe calibration curve
0.02 mg of iron (as Fe). and calculate the iron oxide content inthe aiiquot taken
inB-5.3.2.
B-5.3 Procedure
B-5.4 Calculation
B-5.3.1 Solution of the Sample — Weigh accurately
about 2 gofthe tinely ground test sample (see 6.2) ina Ferric oxide as
platinum dish. Moisten the sample with 5 ml of water. (as Fe,03), percent by mass = #x O.142 ~
Add 3 ml of dilute sulphuric acid and 20 ml of 1
hydrofluoric acid and evaporate slowly to dryness on where
the sand bath or hot plate in a fime cupboard, taking
M = mass of iron (as Fe) found in aliquot, inmg;
care to avoid spurting. Repeat the process with 10fill
and
ofhydrofluoric acid. Cool, add 2 ml of dilute sulphuric
M,= mass ofthe sample represented bythe aliquot
acid and evaporate as before. Heat the dry residue
taken in B-5.3.2, in g.
cautiously until fumes of sulphur trioxide cease to be
evolved. Raise the temperature to 1000”C and ignite II-6 DETERMINATION OF LOSS ON IGNITION
for 5min. Cool and fuse the residue with 1gof sodium
B-ti.l Procedure
carbonate and dissolve in hydrochloric acid, cool and
dilute to 250 ml in a volumetric flask. Take about so g of the material in China dish and heat
to constant weight at 105 +2°C. Cool itinadesiccator
B.5.3.2 Transfer a 5 ml aliquot of the solution
and keep for subsequent tests.
prepared in B-5.3,1 to a 100 ml volumetric flask. Also
transfer O,1,2, 4, 6, 8and 10 ml each of the standard II-6.2 Heat 1gofthe above dried material inaplatinum
iron solution to seven separate 100 ml volumetric crucible in a muffle furnace at 1000 + 50”C. Cool the
flasks. Then add to each flask 2 ml of tartaric acid crucible and put the contents inadesiccator to constant
solution followed by 2 ml of hydroxylamine mass. The loss inmass denotes loss on ignition and the
hydrochloride solution. Stir well and add 5 ml of percent loss Inay be calculated.
o-phenanthroline solution and 10 ml of acetate buffer
B-7 DETERMINATION OF FREE IRON
solution. Allow to stand for 15 min and dilute up to
the mark with water. Soak about 100 g of the sample in excess of water in a
plastic beaker. Mix the sample with a glass rod by
B-5.3.3 Starting with the blank (Oml) solution transfer
vigorously shaking so asto prevent any settlement. Dip
a suitable portion of the coloured solution, one at a
a bar magnet into the slurry and gently rotate it in the
time, to an absorption cell; record the photometric

slurry, 4 to 5 times. Place the magnet on a clean paper
readings using the light band centred approximately at

and dry at room temperature. Collect the iron filings
510 nm, prepare the calibration curve from these
onthe paper. Weigh the filings using electronic balance
readings against concentration of iron (as Fe).
and note the value. The value isdirectly taken aspercent
B-5.3.4 Similarly transfer a suitable aliquot of the free iron.
ANNEX C
(Clause 6.1)
SAMPLING PROCEDURE FOR CALCITE FOR CERAMIC INDUSTRY
C-1 !WALE OF SAMPLING tinown to consist of different batches of manufacture,
the bags belol]ging to same batch and variety shall be
C-1.1 Lot grouped together and each such group shall constitute
a separate lot.
Al] the bags containing the material in a consignment
and belonging to the same batch of manufacture and of C-1.1.1 Unless otherwise agreed to between the buyer
same grade shall constitute a lot. If the consignment is and tbe seller the number of bags to be selected shall
4
IS 15751:2007
depend upon the size of the lot and shall be in C-3 CRITERIA FOR CONFORMITY
accordance with Table 2.
C-3.1 For individual test, from the test results average
Table 2 Number of Bags to be Selected (X) and range (R) shall be calculated, range being the
difference between the maximum and minimum of the
sl No.ofBagsin No.ofBagstobe test results, and
No. theLot Selected
Sum of the test results
(1) (2) (3) Average (~) =
Number of tests
i) upto 150 3
ii) 151-300 4 The lot shall be declared as conforming to the
iii) 301-500 5 specification with respect to moisture content, if the
iv) 501-1000 7
expression:
v) 100Iandabove 10
(R) (U-L) <0.9
C-1.1.2 The bags shall be selected from the lot at
(X)+ O.6R<U
random and inorder to ensure randomness of selection,
(~)- O.6R2L
the method given in IS 4905 maybe followed.
where U isupper specification limit and Listhe lower
C-2 NUMBER OF TESTS
specification limit.
C-2.1 The bags shall be visually examined for defects
C-3.2 Two tests of moisture content and fired colour
as given in 4.1.
shall pass.
C-2.2 Test for moisture content shall be conducted on
C-3.3 All the composite sample shall meet the relevant
individual sample.
requirement given inTable 1,
C-2.3 For fired colour, two bags shall be selected fi-om
C-3.4 The lot shall be declared as conforming to the
the bags selected as in C-1.1.1 and two individual tests
requirements ofthis standard, ifthe requirements C-3.1
shall be carried out.
and C-3.3 are satisfied.
C-2.4 Tests for all other characteristics inTable 1shall
NOTE-– h casethenumberoftestresultsinthesampleis10,
be conducted on composite sample. theyshill be divided into two sub-groups of fivetest results
each Iaking them consecutively obtained. The rangeof each
C-2.5 For preparation ofcomposite sample and general
sub-group then be determined and mean range shall be
requirements of sampling methods given in IS 8883 calculated by dividing of sum of tbe ranges by two. In the
(Part 1)maybe followed. expression inc-3.1, R shallthenbereplacedbyR,

ANNEX D
(Foreword)
COMMITTEE COMPOSITION
Ceramicware Sectional Committee, CHD 9
Orgarrizution Represerrkrfive{s)
Ccrrtra!Glas & Ceramic Research Institute, Ahmedabad DR K. N. MAITI (Chairman)
All hrdiaPottery Manufacturers Association, Kolkata SHRIS. K. @OSli
SHRI S. CHATTERJEE (Aherrrure)
Centl”al~[ass &Ceramic Research Institute, Kolkata [(REPRESENTATIVE
Cera Sanitaryware Ltd, Kadi, New Delhi SHiW M. K. BHANDARI
!jHRl V. K. JAIN (Alternate)
Chemicals &Allied Products Expcut Inspection Council, SHR!S. K. GHOSN
Ko!kata SHRI K. K.BHATIA(Alfermue)
College of Ceramic Technology, Kolkata RWRESENTATWE

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