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Geochemical assessment of a siliceous limestone sample for cement making

Article in Chinese Journal of Geochemistry · March 2011

DOI: 10.1007/s11631-011-0484-8

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 Chin.J.Geochem.(2011)30:033–039
DOI: 10.1007/s11631-011-0484-8

Geochemical assessment of a siliceous limestone sample for

cement making
Rao D.S.*, Vijayakumar T.V., Prabhakar S., and Bhaskar Raju G.
National Metallurgical Laboratory-Madras Centre CSIR Madras Complex, Taramani, Chennai-600 113, India
∗ Corresponding author. E-mail: [email protected]

Received January 20, 2010; accepted March 1, 2010

© Science Press and Institute of Geochemistry, CAS and Springer-Verlag Berlin Heidelberg 2011

Abstract A low grade siliceous limestone sample from the Jayantipuram mine of Andhra Pradesh, India, has been investigated
for its suitability for cement making. Petrological as well as X-ray diffraction pattern studies indicated that the limestone sample
was crystalline and dominantly composed of calcite and quartz. They are simple in mineralogy, and yet they have variable silica
and lime contents. Geochemical analysis results of twenty five hand picked samples indicated that the limestone from the Jayanti-
puram mine shows a wide range of variations in LOI (29.94% to 40.64%), SiO2 (6.14% to 27.18%), CaO (37.93% to 50.78%),
Al2O3 (0.49% to 2.27%) and Fe2O3 (0.28% to 2.4%). MgO, K2O, Na2O, TiO2 and MnO2 are present in traces. CaO with LOI
shows a strong positive correlation where as CaO with SiO2 shows a strong negative correlation because of mineralogical factors.
The chemical composition of the limestone reflects its mineralogical composition. The distribution of various elements in the
acid-soluble fraction has been studied by the factor analysis method in order to interpret in terms of their mineralogy, sedimentary
environment and diagenesis. Mineralogy, recrystallization and other diagenetic changes are the main factors affecting the distribu-
tion of the elements and their mutual relationships in the limestone. The aim of this paper is also to analyze how significantly the
two parameters, silica modulus and lime saturation factor, influence this low grade siliceous limestone sample from the Jayantipu-
ram mine of Andhra Pradesh, India, for the cement making process from the geochemical data.

Key words Jayantipuram mine; limestone; mineralogy; geochemistry; silica modulus

1 Introduction Zone, 23 per cent in North Zone, 21 per cent in West

Zone and the remaining 8 per cent in East Zone (Minerals
Limestone, a sedimentary calcareous rock, mostly Year Book, 2006; http://siadipp.nic.in/publicat/cement.
composed of calcite with some gangue minerals such as htm). For manufacturing of one ton of cement, a quantity
quartz, feldspar and mica. The major industries which of 1.5 ton of limestone is required. Hence, cement plants
consume limestone are: cement production, metallurgy are necessarily located close to the limestone mines to
(iron and steel making), manufacturing (glass, food minimize the transportation cost. The cement grade
processing, paper making, leather, water purification, limestone deposits are depleting day by day because of
waste water treatment, flue gas desulphurisation, adhe- continuous exploitation of high grade limestone over the
sives, insulation and pH control), agriculture (fertilizers, years. Hence, many of the cement industries in India are
fungicides, animal feed), and construction (mortar, ce- looking for utilization of the existing low grade siliceous
ment, whitewash, building stone) purposes. Limestone is limestone from their captive mines for conservation of
the lifeline for any cement plant because it constitutes mineral resources as well as sustaining environment. But,
the major raw material component. India is endowed the low grade siliceous limestone can not be used di-
with large deposits of limestone. The estimated total re- rectly as it does not meet the required specifications of
serves of limestone are 95.623 billion tones. However, cement making. According to Indian cement manufac-
the limestone deposits are not uniformly distributed in all turers specifications, limestone for cement making,
the States. There is a concentration of about 73 per cent should contain more than 45% CaO; Fe2O3 as well as
of the total reserves in five States, namely, Andhra Al2O3 1% to 2%; free silica less than 8%; combined
Pradesh, Karnataka, Gujarat, Rajasthan and Madhya Na2O+K2O less than 0.6% and P2O5 less than 0.6%.
Pradesh. This concentration is about 48 per cent in South Magnesia contents of the limestone should ideally be less

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34 Chin.J.Geochem.(2011)30:033–039

than 3%, although as high as 5% MgO can be used by factor (LSF): the ratio of CaO and weighted sum of alu-
the cement industry. Magnesia, sulphur and phosphorus mina, silica and ferric oxide, is another important pa-
are regarded as the most undesirable impurities. The rameter that makes a cement plant cost effective. The
presence of phosphorus (P2O5) slows down the setting LSF plays a vital role in cement production because it
time of Portland cement (Minerals Year Book, 2006). In contains CaO, the primary constituent of cement. It has
order to attain these specifications, low grade siliceous been found (Ingram and Daugherty, 1991) that kiln op-
limestone needs to be characterized in terms of their eration and cement quality are improved where the CaO
mineralogy and geochemistry. in limestone is more than 44%. Thus, both high LSF and
Portland cement is produced by the high temperature a low silica ratio contribute significantly to the
reaction of a lime-bearing material (limestone) with one cost-effectiveness of a cement plant. To maintain a con-
containing silica, alumina, and ferrous materials. The sistent supply of suitable limestone grades to a cement
product, which is known as clinker, has four main com- plant, mineralogical as well as geochemical characterisa-
pounds―tricalcium silicate (C3S otherwise known as tion of the limestone is essential.
alite), dicalcium silicate (C2S otherwise known as belite),
calcium aluminate (C3A) and tetracalcium aluminoferrite 2 Geology of the limestone deposit
(C4AF), is afterwards ground with gypsum to give ce-
ment. The quality of cement is determined by the com-
The study area is located in the Jayantipuram
position ratio of these four components. Of these com-
(16°51′30″N to 16°52′45″N latitude and 80°06′15″E to
pounds, C3S and C3A are mainly responsible for the
80°08′00″E) Village, Jaggayyapeta Taluka of Krishna
strength of the cement. High percentage of C3S (low C2S)
District, Andhra Pradesh. The Jayantipuram area lies on
results in high strength, but also high heat generation as
the northeastern margin of the Palnad sub-basin of Kur-
the concrete sets. The reverse combination of low C3S
nool sedimentary basin overlying the Cuddapah Super-
and high C2S develops strength and generates less heat.
group of rocks. The Cuddapah Group is in turn deposited
C3A causes undesirable heat and rapid reacting proper-
over the Achaean basement. The Jayantipuram limestone
ties, which can be prevented by adding CaSO4 to the
deposit forms a part of the Nargi Limestone Formation
final product. C3A can be converted to more desirable
belonging to the Kurnool System. The topography is un-
C4AF by the addition of Fe2O3 before heating, but this
dulating with surface levels varying from 30 to 73 m
also inhabits the formation of C3S. C4AF makes the ce-
above mean sea level. The nearest railway station is Vijay-
ment more resistant to sea water and results in somewhat
awada and the NH-9 is just 3 kilometres away from the
a slower reaction which evolves less heat. Relatively low
site. A seasonal nalla flowing towards southwest is the
grade limestone containing poor CaO can not produce major drainage channel in the area.
sufficient C2S and C3S. Hence, the quality or grade of
limestone not only plays an important role in the
cost-effectiveness of an integrated cement plant, but also 3 Results and discussion
essential for the steady operation of the plant as well as
to achieve optimum plant output. Therefore, the con- 3.1 Characterization
stituents such as calcium oxide (CaO), alumina (Al2O3),
iron oxide (Fe2O3) and silica (SiO2) of the limestone Petrological studies of the limestone sample from the
supplied to the plant be within permissible limits of the Jayantipuam area indicated that the sample is dominantly
specifications meant for cement manufacture. It is an composed of calcite with lesser amounts of quartz, clay
established fact that high SiO2 content in the limestone and rarely some opaque minerals (mostly pyrite). These
has an adverse effect on kiln properties and the kiln is limestone rocks have fine- to medium-grained granular
one of the most important units for the performance of mosaics without any fossils. Calcite is generally
the cement plant. It is monitored in the form of the silica fine-grained but patches of medium- to coarse-grained
ratio (SR) which is the ratio between silica and weighted anhedral calcite are also common. The medium- to
sum of Al2O3 and Fe2O3. As the silica ratio increases, coarse-grained calcite crystals are generally interlocked
more heat is required to run the kiln. Nayak and Mallik and contain inclusions of silicates minerals. Quartz oc-
(2002) have observed that the kiln is more effective curs in the form of subhedral, medium-grained, and de-
where the silica ratio is less than 2.3. The lime saturation trital material. The calcite of this limestone deposit
Chin.J.Geochem.(2011)30:033–039 35

seems to be authigenic in origin and has been precipi- limestone samples from the Jayantipuram area is pre-
tated in-situ. Micro-fractures filled with fine-grained sented in Table 1. Chemical analyses revealed that the
calcite micro-veins which are considered to be diagenetic. limestone samples contain lime as the major constituent,
Clay and iron pyrite in trace amounts are present as
fine-grained disseminated material in many samples. Rao
et al. (2009) studied the siliceous limestone sample from
the same area and reported the same mineralogic results
for this limestone sample.
X-Ray diffractogram of the sample (Fig. 1) revealed
that it contains calcite as the major mineral phase while
quartz as the minor silicate gangue mineral. No other
mineral phases were observed.

3.2 Geochemistry

The chemistry of the cement in general and Portland

cement in particular largely depends upon the geochem-
istry of its raw materials, i.e., limestone. Approximately
75% of the Portland cement raw material consists of lime
(CaO)-bearing material (Lea, 1976). The major and mi- Fig. 1. XRD patterns of three different limestone samples. C. Calcite;
nor elemental chemistry of the randomly hand-picked Q. quartz.

Table 1 Geochemical characteristics of Jayantipuram limestone samples

Sample No. LOI SiO2 Al2O3 Fe2O3 CaO MgO Na2O K2 O TiO2 MnO2
1 34.60 17.60 0.88 1.55 43.51 0.46 0.17 0.23 0.03 0.02
2 34.94 18.44 0.61 0.32 44.23 0.15 0.07 0.18 0.03 0.04
3 35.92 14.76 1.59 0.45 45.24 0.64 0.18 0.34 0.05 0.02
4 40.07 07.70 0.53 0.40 49.29 1.30 0.16 0.18 0.02 0.01
5 30.79 27.18 0.96 0.38 38.90 0.42 0.18 0.27 0.03 0.02
6 35.09 17.93 0.50 0.25 44.35 0.35 0.17 0.18 0.02 0.01
7 36.82 14.69 0.82 0.34 46.12 0.49 0.16 0.24 0.03 0.02
8 34.99 16.79 1.33 0.56 44.33 0.52 0.17 0.39 0.04 0.02
9 35.77 16.17 0.58 0.39 45.46 0.53 0.16 0.20 0.02 0.02
10 35.37 16.89 0.74 0.68 44.67 0.42 0.16 0.23 0.03 0.02
11 37.08 13.82 0.68 0.36 46.59 0.47 0.15 0.21 0.02 0.02
12 37.78 11.95 0.87 0.46 47.36 0.59 0.16 0.20 0.03 0.03
13 36.46 15.42 0.64 0.33 45.72 0.38 0.15 0.22 0.02 0.02
14 34.08 20.33 0.94 0.45 42.61 0.61 0.15 0.23 0.04 0.02
15 31.84 26.28 0.53 0.28 39.68 0.41 0.15 0.19 0.02 0.02
16 34.33 18.01 1.54 0.94 43.22 0.62 0.22 0.36 0.07 0.03
17 34.18 18.22 1.54 0.99 42.81 0.65 0.23 0.38 0.07 0.03
18 34.12 18.32 1.66 1.05 42.87 0.74 0.29 0.37 0.08 0.03
19 33.86 18.84 1.77 1.20 42.52 0.67 0.20 0.41 0.09 0.03
20 33.38 19.35 2.00 1.31 41.93 0.75 0.26 0.47 0.11 0.03
21 32.82 19.70 2.16 1.82 41.17 0.87 0.31 0.48 0.14 0.04
22 31.78 21.34 2.27 2.19 40.13 0.84 0.25 0.50 0.16 0.04
23 31.66 21.47 2.02 1.97 39.93 0.77 0.25 0.46 0.15 0.03
24 29.94 24.59 2.00 2.40 37.93 0.83 0.28 0.40 0.15 0.04
25 40.64 06.14 0.49 0.58 50.78 0.48 0.15 0.16 0.03 0.02
36 Chin.J.Geochem.(2011)30:033–039

followed by Loss on Ignition (LOI) and silica (Table 1). which may be due to the reason that LOI is contributed
Alumina and iron oxide form the minor constituents mainly by the carbonate content of calcite. CaO shows a
while magnesia, alkalis (soda and potash), TiO2 and very strong negative correlation (Table 2) with that of the
MnO2 are present in traces. SiO2, Al2O3, Fe2O3 along silica (Fig. 3). The negative correlation between CaO and
with CaO of the limestone form the main ingredients that SiO2 is because of the fact that the CaO (from calcite)
make up the cement but should be within permissible and SiO2 (from quartz) are from two different mineral
limits. It is apparent that this siliceous limestone sample phases and they are not related. Alumina (Al2O3) in these
can not be used directly for cement industries as the samples ranges from 0.49% to 2.27% and shows nega-
sample contains silica above 8%. LOI of this Jayantipu- tive correlation with CaO and positive correlation with
ram mine limestone sample varies from 29.94% to 40.64 iron, magnesium, soda, potash, titania and manganese
%. The LOI content is mostly contributed by the carbon- oxide which could be due to clay material present in the
ate minerals. limestone samples. Among other constituents that are
The SiO2 content in this limestone varies widely, commonly important is MgO (0.15% to 1.3%) which
ranging from 6.14% to 27.18%, which is contributed by might have been derived either from the magne-
quartz. The lime content varies between 37.93% to sium-containing skeletal debris or due to post deposi-
50.78% and is due to the calcite present in the limestone. tional additions or during diagenesis. The chemical
The CaO content in this limestone shows a strong posi- composition of the limestone reflects its mineralogical
tive correlation (Table 2) with that of the LOI (Fig. 2) composition.

Table 2 Correlation coefficients of constituents of the limestone sample

LOI SiO2 Al2O3 Fe2O3 CaO MgO Na2O K2 O TiO2 MnO2

LOI 01.00

SiO2 −0.97 01.00

Al2O3 −0.61 00.41 01.00

Fe2O3 −0.59 00.38 00.83 01.00
CaO 01.00 −0.97 −0.61 −0.59 01.00
MgO −0.02 −0.14 00.52 00.49 −0.07 1.00
Na2O −0.53 00.35 00.86 00.79 −0.55 0.61 1.00

K2O −0.61 00.42 00.98 00.78 −0.61 0.49 0.84 1.00

TiO2 −0.62 00.42 00.93 00.92 −0.63 0.53 0.84 0.90 1.00

MnO2 −0.52 00.38 00.71 00.69 −0.51 0.16 0.52 0.65 0.76 1.00

Fig. 2. CaO vs. LOI plotting showing positive correlation. Fig. 3. CaO vs. SiO2 plotting showing negative correlations.
Chin.J.Geochem.(2011)30:033–039 37

3.3 Factor analysis depends on the composition of original sediments and

the physico-chemical processes involved. For carbonate
To assist in making geochemical inferences on the sediments diagenesis is essentially the transformation
origin of the limestone of the Jayantipuram mine, major into a stable calcite phase. This could be the reason why
and minor element data were analyzed using the multi- factorial analysis of the geochemical data shows signifi-
variate factor model of correlation matrix (factor model cant factor values (the 2nd factor value; Table 3) of LOI,
of Davis, 1973). This was done after standardization, CaO and SiO2. LOI and CaO forming calcite by
which allowed retention of common factors by minima diagenesis.
or inflection points of eigen values (Sahu, 1982). The
inflection point methods yielded only two common fac- 3.4 Lime saturation factor
tors (Table 3) which were varimax rotated to get geo-
chemical interpretations. The first factor could be related The LSF is a ratio of CaO to the other three main ox-
with sedimentation and the second factor could be re- ides. Applied to clinker, it is calculated as:
lated to diagenesis. The first factor explaining 66.13% of LSF=CaO/(2.8 SiO2 + 1.2 Al2O3 + 0.65 Fe2O3)
total variances is strongly loaded and can be correlated Often, this is referred to as a percentage and therefore
with the source of the sediments, transportation and multiplied by 100 and this is mostly applied to clinkers.
deposition. The elements Mg, Na, K, Ti, Mn, Al, and Fe The lime saturation factor is used for kiln feed control. A
dominantly reflect the clastic sediment contribution. higher LSF makes it difficult to burn raw mix. Reac-
Where as the first factor value shows significant values tivity of the raw mixture for cement making is influenced
for minor elements where by they must have been depos- greatly in pyrolysis. The pyrolysis characteristics of
ited along with carbonate sediments (the 1st factor value; limestone is greatly influenced by the particle size of
Table 3). Diagenesis is a process by which sedimentary calcite crystal, crystal shape that is characteristic of
rocks alter after their deposition. Diagenesis takes place limestone itself and outside impurities such as SiO2,
either by interaction between their constituents or by Al2O3 and Fe2O3 as well as the existence of state of ac-
reaction between their constituents. Similar is the case companying minerals (Park et al., 2004). The LSF con-
for limestones where they undergo some kind of altera- trols the ratio of alite to belite in the clinker. A clinker
tion after initial solidification. Diagenesis is anything with a higher LSF will have a higher proportion of alite
to belite than a clinker with a low LSF. Typical LSF val-
that happens to a sedimentary rock after original deposi-
ues in modern clinkers are 0.92–0.98. Values above 1.0
tion. These alterations include recrystalization, compac-
indicate that free lime is likely to be present in the
tion and cementation. All of these things are considered
clinker. This is because, in principle, at LSF=1.0 all the
part of the diagenetic process. In general, the nature of
free lime should have combined with belite to form alite.
end product of diagenesis
If the LSF is higher than 1.0, the surplus free lime has
Table 3 Factor analysis data from geochemistry nothing with which to combine and will remain as free
Factor-1 Factor-2 Communality lime. In practice, the mixing of raw materials is never
LOI −0.32 −0.94 0.98
perfect and there are always regions within the clinker
SiO2 0.09 0.98 0.96
where the LSF is locally a little above, or a little below,
the target for the clinker as a whole. This means that
Al2O3 0.90 0.36 0.93
there is almost always some residual free lime, even
Fe2O3 0.84 0.34 0.83
where the LSF is considerably below 1.0. It also means
CaO −0.34 −0.92 0.97
that to convert virtually all the belite to alite, an LSF
MgO 0.77 −0.32 0.70
slightly above 1.0 is needed. For the present samples the
Na2O 0.88 0.25 0.83
LSF ranges from 0.5 to 2.8 (Table 4), which indicates
K2O 0.86 0.36 0.88
that the CaO value is highly erratic and needs to be in
TiO2 0.90 0.37 0.95
uniform range for cement making.
MnO2 0.62 0.42 0.56
Eigen value 6.61 1.97 3.5 Silica ratio (SR)
of trace (%) 66.13 19.72
Cumulative of 66.13 85.85 The silica ratio is sometimes called the ‘silica modulus’.
trace (%) The silica modulus has especially great influence
38 Chin.J.Geochem.(2011)30:033–039

Table 4 Lime saturation factor, alumina ratio and silica modulus This is because at an AR of about 1.4, there is more
data
clinker liquid at a lower temperature (Minor constituents
Sample Sample such as MgO can alter this optimum AR). The AR for the
LSF SR AR LSF SR AR
No. No.
present samples ranges from 0.57 to 3.53 (Table 4)
1 0.85 07.24 0.57 14 0.73 14.63 2.09
2 0.84 19.83 1.91 15 0.53 32.44 1.89
3 1.04 07.24 3.53 16 0.82 07.26 1.64 4 Implications in cement making
4 2.19 08.28 1.33 17 0.80 07.20 1.56
5 0.50 20.28 2.53 18 0.79 06.76 1.58 Petrological as well as X-ray diffraction pattern stud-
6 0.87 23.91 2.00 19 0.76 06.34 1.48 ies indicated that the limestone sample was crystalline
7 1.09 12.66 2.41 20 0.73 05.85 1.53 and dominantly composed of calcite and quartz. They
8 0.91 08.88 2.38 21 0.70 04.95 1.19 have a simple mineralogy, and yet they have variable
9 0.98 16.67 1.49 22 0.63 04.78 1.04 silica and lime contents. CaO with LOI shows strong a
10 0.92 11.89 1.09 23 0.63 05.38 1.03 positive correlation whereas CaO with SiO2 shows a
11 1.17 13.29 1.89 24 0.52 05.59 0.83 strong negative correlation because of mineralogical
12 1.36 08.98 1.89 25 2.80 05.74 0.84 factors. Silica modulus and lime saturation factor from
13 1.04 15.90 1.94 geochemistry data indicated that the siliceous limestone
samples from the Jayantipuram mines of Andhra Pradesh,
on burning process and on some cement features. The India, can be utilized for cement making process pro-
silica ratio is defined as: vided they are processed for beneficiation for silica re-
SR=SiO2/(Al2O3 + Fe2O3) moval (to less than 8%) to required level where the CaO
Large variation of silica modulus in the clinker can be can be enriched automatically. Hence, in this limestone
an indication of poor uniformity in the kiln feed. sample if CaO content is increased to more than 45% and
Changes in coating formation in the burning zone, burn- SiO2 content is decreased below 7%, then the low grade
ability of the clinker and ring formations with in the kiln siliceous limestone sample can be utilized for cement
can often be traced to changes of silica modulus in the making. In such a case the existing low grade siliceous
clinker. As a rule, clinker with high silica modulus is limestone samples, which were considered as waste rock
more difficult to burn and exhibits poor coating proper- in various limestone mines, can be effectively utilized
ties. Low silica modulus often leads to ring formations in not only for conservation of mineral resources, but also
cement. A high silica ratio means that more calcium sili- for sustaining environment. The quality up gradation of
cates are present in the clinker and less aluminate and limestone can be done by many ways. One alternative is
ferrite. SR is typically between 2.0 and 3.0 for Portland to crush limestone to be -3mm in size and process it in
cement clinker. The SR governs the proportion of silicate scrubber and classifier, while the other entails grinding
phases in the clinker. The SR for the present samples of raw feed to less than 200 mesh and carry out benefici-
ranges from 4.78 to 32.44 (Table 4) which indicate that ation by froth flotation method (Ananth et al., 1997; Rao
the samples are higher in SiO2 content and needs to be et al., 1997; 2009 and 2010) or by column flotation
brought down to below the specified limits for cement (Vijayakumar et al., 2005).
making.
Acknowledgements The authors are thankful to Director of
3.6 Alumina ratio (AR) National Metallurgical Laboratory, Jamshedpur for his valuable
guidance, encouragement and permission to publish this work.
The alumina ratio is defined as: The authors would like to thank the management of M/s. Madras
AR=(Al2O3)/(Fe2O3) Cements Limited, Chennai and Ramco Research & Development
This determines the potential relative proportions of Centre, Chennai for providing logistic support as well as chemi-
aluminate and ferrite phase in the clinker. An increase in cal analysis of the limestone samples, respectively.
clinker AR (also sometimes written as A/F) means there
will be proportionally more aluminate and less ferrite in References
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