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( Reaffirmed 1999 )
Indian Standard
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) METHOD OF ANALYSIS OF HYDRAULIC
CEMENT BY ATOMIC ABSORPTION
SPECTROPHOTOMETER
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8 BIS 1990
FOREWORD
This Indian Standard was adopted by the Bureau of Indian Standards on 21 September 1989, after the
draft finalized by the Cement and Concrete Sectional Committee bad been approved by the Civil
Engineering Division Council.
With the advent of large scale cement plants and introduction of sophisticated technology for the
manufacture of cement, it has become absolutely essential to have a precise control in quarrying,
crushing, proportioning of raw materials for raw mix preparation and stable operaiion of the kiln to
get desired quality of clinker. For this purpose, the analytical data of the chemical constituents is
essential at more frequent intervals for necessary corrective actions to be taken. The conventional
methods of chemical analysis, such as gravimetric and volumetric methods which are generally
practised, though accurate and precise, are time consuming resultmg in delay for necessary corrective
actions. In addition to the conventional methods given in IS 4032 : 1985, the technique of atomic
absorption spectrophotometric analysis may be used for routine quality control purposes: The advan-
tages of atomic absorption technique over the conventional analytical methods are its rapidity, relative
freedom from interferences ( which affords high degree of selectivity ) and high degree of sensitivity
for over 60 elements. Application of such rapid analytical methods for analysis of major and minor
constituents of cement for the routine control purposes will be immensely beneficial. With this in
view, the Cement and Concrete Sectional Committee felt necessary to bring out a standard covering
atomic absorption spectrophotometric methods for analysis of hydraulic cement. This standard lays
down the procedure for conducting atomic absorption spectrophotometric analysis of major and minor
constituents of different hydraulic cement. This method may be suitably used for analysis of
clinker as well as raw materials and raw mix used in cement manufacture. In case of dispute or
doubtful marginal values in estimation of elements covered in IS 4032 : 1985, the methods described
in IS 4032 : 1985, shall be taken as refree method.
The composition of the technical committee responsible for the formulation of the standard is given at
Annex A.
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 with IS 2 : 1960 ‘Rules for
rounding off numerical values ( revised )‘.
Is 12813: 1989
Indian Standard
METHOD OF ANALYSIS OF HYDRAULIC
CEMENT BY ATOMIC ABSORPTION
SPECTROPHOTOMETER
1 SCOPE The basis for using absorption to determino atomic
concentration is as follows.
1.1 This standard covers the atomic absorption
spectrophotometric procedure for chemical ana- 4.1.1 Assume a parallel beam of monochromatic
lysis of hydraulic cement and. clinker. radiant energy of intensity lov, at frequency v is
incident on an atomic vapour of path length, 1.
1.2 This method covers the determination of Then, if the intensity of the transmitted beam is
SiO*, A1208, FeaO,, CaO, MgO, NapO, KzO, Iv, the absorption coefficient Kv of the vapour at
MnB03, TIO~ and CrzOs. frequency v is defined by:
NOTE - Compositions are expressed as percent Iv =l0v exp( - Kvl)
oxide but determined as percent elements in the
method. Since the absorption line has a finite half width
Kv will vary with v. However, classical dispersion
2 REFERENCES theory states that the integrated absorption (Kvdv)
is given by the relation:
The Indian Standards given below are necessary
adjuncts of this standard. Kvdv = ( aea/mc ) Nvf
\
IS No. Title whore
m = electronic mass,
IS 264 : 1976 Specification for nitric acid
( second revision ) c = velocity of light,
e = electronic charge,
IS 266 : 1977 Specification for sulphuric acid
( second revision ) NV = number of atoms per cubic centimetre
capable of absorbing radiation of fre-
IS 1070 : 1977 Specification for water for quency v, and
genera1 laboratory use ( second f = oscillator strength.
revision )
4.1.2 This equation is valid only when a transition
Is 3535 : 1986 Methods of sampling hydraulic is initiated from the ground state. NV is essentially
cement (Jirsf revision ) equal to the total number of ato.ms per cubic
IS 4032 : 1985 Method of chemical analysis of centimetre ( NO ). The integrated absorption is
hydraulic cement (first revision ) then proportional to the concentration of free
atoms in the absorbing vapour and is independent
3 SAMPLING of the temperature of the vapour. For most
elements, NV can be replaced by NO which then
3.1 The samples of the cement shall be taken brings about a simple linear relationship between
according to the requirement of IS 3535 : 1986 the integrated absorption coefficient and the
and the relevant standard specification for the type concentration. Since it is difficult to measure the
of cement being tested, The representative sample integrated absorption coefficients, peak absorption
of the cement selected as above shall be thoroughly is measured. In practice, the equation for Iv given
mixed before using. in 4.1.1 is valid only when calibration solutions
are used.
4 OUTLINE OF THE METHOD
4.1.3 Although the integrated absorption is pro-
4.1 In atomic absorption, a sample solution is portional to the concentration of free atoms in
aspirated into a flame through which radiation the absorbing medium and is independent of the
from a line emission source of the element sought temperature of the vapour, the ability of a flame
passes. The monochromatic radiation is absorbed to produce ground state atoms is temperature
in proportion to the concentration of the neutral dependent. The temperature of the flame must be
atoms present. The concentration of the analyte high enough to dissociate the molecules, but not
is obtained by comparison to calibration solutions. so hot as to produce large numbers of ions.
I
IS 12813 : 1989
2
.
IS 12813 : 1989
( Ckse 10.1.2 )
NOTES
1 The typical dilutions indicated in this table is with reference to approximate percentage of constituent
present in standard samples in order to obtain the linearity range given in co1 7 above. However, if
the percentage of constituent in standard sample is different than that indicated, calibration may be done even,
with the same dilutions.
z The precision of lime estimation can be further improved by choosing very close range standard samples for
calibration.
3 The linearity range can be further extended by reducing the path by rotation of the burner or by using
smaller path length burner.
4 Some of the commercially available instruments are having two channel system wherein by use of internal’
standard element which is not present in the sample. the absorbance ratios of lime with internal standard’
element are computed resulting in elimination of dilution errors.
§ In case of calcium and magnesium standards O-1 percent lanthanum/strontium shall be added.
--_-.- __.__-~:_ ,.
IS 12813 : 1989
5
IS 12813: 1989
R’db 3 StamhrdConditions
withWoAhg Rmges for theElements
( Chse 12.1)
iii) Fe 248.3 Air/CIHe Fuel lean. oxi- ,Matrix and Samples and standard 0 - 3’0
dising, blue excess mineral should be matched in
flame acid matrix and acidity
iv) Ca 422.7 Air/GHa Fuel lean, oxi- Depression of Addition of 0.1% La/Sr 0 - 5’0
or diiing, blue signal due to as releasing agent
N,O/GHo flame formation of
oxysalts with
Al, Si, Ti,P
vi) 589'0 Air/C,H, Fpel lean, $te Small ionization Li frpm the flux is 0 - 3.0
$s4nlZ, sufficient to overcome
the interference
vii) K 7665 Air/CaHr ;;;;tan, b;;t Small ionization Li frpm the flux is 0 - 3’0
suffic8ent to overcome
flame l the interference
7
IS 12813: 1989
Membera Reprcserttn~
DR M. RAMAIAH Structural Engineering Research Centre ( CSIR ), Ma&as
DR A. G. MADHAVA RAO ( Alternate )
SHRI A. U. RIJHSINOHANI Cement Corporation of India, New Delhl
SHRI C. S. SHARMA( AIternofe )
SECRETARY Central Board of Irrigation and Power, New Delhi
SHRI K. R. SAXENA( Alternate)
SUPERINTENDING ENGINEER( DESIGNS) Public Works Department, Government of Tamil Nadu
Ex~cur~ve ENGINEER( SMD DIVISION)
( AIternate )
SHRI L. SWAROOP Orissa Cement Limited, New Delhi
SHRI H. BHATTACHARYA
( Alrernate )
SHRI S. K. GUHA THAKURTA Gannon Dunkerly & Co Ltd. Bombay
SHRI S.P. SANKARNARAYANAN
( A/f ernute )
DR H. C. VISV~SVARAYA The Institution of Engineers ( India ), Calcutta
SHRI D. C. CHATURVEDI ( Affornore )
SHRI G. RAMAN. Director General, BIS ( Ex-o&lo Member )
Director ( Civ Engg )
Secretary
SHRI N. C. BANDYOPADRYAY
Joint Director ( Civ Bngg ), BIS
8
IS 12813: 1989
Members Representing
9
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