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Abstract: Research using marble powder as a partial replacement of cement in concrete has gained a lot of attention recently. In this paper,
the effect of dried marble powder on particle packing of concrete has been demonstrated. Experimental investigations have been conducted on
the effect of marble powder on hydration reaction, strength activity index, and possible reasons for the gain in strength. In addition, statistical
methods were used to develop two mathematical models for marble powder incorporated in concrete using experimental values. In the first
model, the ratios of 28-day compressive strength between concrete with cement partially replaced by marble powder and control concrete
have been related to marble powder replacement percentage. In the second model proposed, modified and simplified relationships for the
water-cement law when cement is partially replaced by marble powder have been provided. The first model was validated for both standard
cubes and cylinders used for testing by researchers and the predictions showed only 7.15% error as compared with the experimental values.
The second model might serve as a useful tool for mix proportioning of concrete mixes incorporating marble powder in concrete. Finally,
based on a review of the literature and experimental results, a set of guidelines has been proposed for the use of marble powder as a partial
replacement of cement in concrete. DOI: 10.1061/(ASCE)MT.1943-5533.0002631. © 2019 American Society of Civil Engineers.
Author keywords: Concrete; Marble powder; Compressive strength; Modeling; Regression analysis.
In most of the studies, high levels of calcite were used, such that a certain percentage, the fillers start acting as diluents, thus reduc-
most of it acts as a filler. Bessey (1938) discovered monocarboa- ing the compressive strength as compared with control concretes
luminate (Mc) and it was successfully synthesized by Carlson and (Soroka and Stern 1976). Some factors such as the particle size
Berman (1960). The reactivity of calcite in limestone has been well distribution (PSD) and particle-packing density of the mix, the type
established. The hydration of ordinary portland cement (OPC) of cement, and the usage of plasticizer also are significant for the
blended with 20% calcium carbonate was investigated by Bonavetti properties of the fresh and hardened concrete (Tikkanen et al.
et al. (2001). At 3-day hydration, monocarboaluminate and ettrin- 2014). Therefore, it is necessary to study the role of marble powder
gite were detected. However, at the end of 28 days, the presence of as filler using particle-packing analysis and to check whether cal-
ettringite was almost negligible and monocarboaluminate along cite in marble powder takes part in reaction with C3 A in cement.
with monosulfate were found. Finally, after 90 days, monocarboa- For materials like fly ash and rice husk ash, prediction models
luminate and ettringite appeared as the stable hydration products are already available in the literature (Chopra et al. 2016; Pathak
and monosulfoaluminate disappeared. Damidot et al. (1994) also et al. 2012; Topçu and Sarıdemir 2008). Abrams’ and Bolomey’s
found similar results because hemicarboaluminate was not found in law were modified and a new model was developed by Štefan
the presence of calcium carbonate. Sprung and Siebel (1991) inves- (1991) for silica fume concrete. A prediction model for compres-
tigated the strength development of different limestone-blended sive strength of silica fume concrete using 150 × 300 mm cylinders
cement concretes. It was found that concrete with up to 20% lime- was developed by Gutierrez and Canovas (1996) in which the ef-
stone had similar performance as compared with the control con- ficiency of silica fume was considered constant. However, Ganesh
crete. The effect of different fillers on the compressive strength was Babu and Prakash (1995) reported that the efficiency of silica fume
examined by Soroka and Setter (1977). They demonstrated that depends on the levels of cement replacement. Bhanja and Sengupta
cement samples with limestone had the largest gain in strength as (2002) formulated a regression model involving nondimensional
compared with some pozzolanic fillers. In the early-age samples, a parameters for prediction of 28-day compressive strength for differ-
maximum increase of about 10% in strength on substituting cement ent types of specimens. Similarly, the law for water:cement (w/c)
by limestone was observed. It was concluded that the main reason ratio formulated by Abrams (1918) considered w/c ratio as the only
for increase in strength could be accelerated cement hydration due governing factor affecting the compressive strength of concrete.
to the availability of crystallization nuclei provided by the fillers, However, with the inclusion of mineral admixtures this law is no
rather than being caused by a chemically induced strength gain due more valid because both w/c ratio and percentage replacement of
to the formation of carboaluminate as shown in Eq. (1) the material have an effect on the strength parameter. Therefore, the
C3 A þ CaCO3 þ 11H2 O → C3 A • CaCO3 • 11H2 O ð1Þ conventional formulation needs to be modified according to the
pattern observed for different materials. Oluokon (1994) proposed
Thus, calcite is found to serve two functions, one of which is a modified w/c law for fly ash use in concrete. Bhanja and Sengupta
actively participating in the hydration process and the other as inert (2003) formulated a law for silica fume incorporating the efficiency
filler. Matschei et al. (2007) also showed that a large part of calcium factor of silica fume. No such law is available for marble powder in
carbonate is reactive and it affects the distribution of lime, alumina, the literature. Therefore, there is a need for formulation of compres-
and sulfate. sive strength prediction model and a new w/c law for inclusion of
Bentz et al. (2015) conducted an investigation on the influence waste marble powder in concrete. This paper addresses these two
of both conventional limestone aggregates and fine limestone pow- gaps and is an extension of the work presented by Singh et al.
der on the performance of concrete. It was observed that a favorable (2017e).
surface for nucleation and growth of calcium silicate hydration gel
at early ages was provided by fine limestone powder in the form
of calcite. That in turn accelerates and amplifies silicate hydration, Research Significance
and also provides a source of carbonate ions to participate in reac-
tions with the aluminate phases present in the cement. However, In this paper, the effect of marble powder on particle packing of
another polymorph of CaCO3 aragonite exhibited a different crystal concrete is demonstrated. Experimental investigations to study the
(and surface) structure that was not found to accelerate or amplify effect of marble dust on hydration reaction, strength activity index,
silicate hydration at a similar particle size or surface area. Even and exploring possible reasons for the gain in strength have been
though these two forms of CaCO3 , i.e., calcite and aragonite, have conducted. The novelty of this paper is that it deals with develop-
similar solubilities in water, aragonite enhances the reactivity of the ment of statistical methods, developing two mathematical models
aluminate phase by forming carboaluminate. A total of 10% lime- for marble powder incorporated in concrete. In the first model, the
stone could replace an equivalent volume of cement in 100% OPC ratios of 28-day compressive strength between concrete with ce-
concretes without any loss in performance of concrete. Fine pow- ment partially replaced by marble powder and control concrete
ders have been found to show three different types of effects of have been related to marble powder replacement percentage. The
properties of hardened concrete (Tikkanen et al. 2014): expression that has been derived is on the basis of strength ratios and
• They may take part in a chemical reaction such as hydraulic or not on the absolute values of strength. In the second model, modi-
pozzolanic effects (Larbi 1993); fied and simplified relationships for w/c law when cement is
Fig. 1. Particle size distribution of cement. Fig. 3. Particle size distribution of coarse aggregate.
Fig. 4. (a) XRD of marble powder; (b) thermogravimetric analysis of marble powder; (c) SEM of marble powder showing elements; and (d) EDS of
marble powder showing elements.
the particle size distribution of coarse aggregate. The mineralogical (EDS) extension was performed on marble dust, showing lime as
composition of dried marble powder was found using powdered the main constituent of the powder as shown in Figs. 4(c and d),
XRD analysis in the Physics Department of the Birla Institute respectively.
of Technology and Science (BITS), Pilani, with an X-ray source
of Cu Kα radiation (λ ¼ 1.5418 Å) for diffraction angle varying Procedures
from 10° to 80° in 2θ ¼ 0.020° at 2° per minute. The peak phases
were identified using software named Match! version 3.7.0, which Particle Packing
was developed by . An open crystallography database with an ex- Efficient particle packing is required for concrete to achieve im-
tension for cement-based materials was used to match the peaks. proved mechanical strength and durability. The literature shows
Mainly calcite and dolomite were present in crystalline phases as that marble powder has been mainly found to give a filler effect by
shown in Fig. 4(a). Table 1 shows the chemical composition of mar- providing efficient particle packing in concrete mix (Aliabdo et al.
ble powder from an X-ray fluorescence (XRF) test. A very small 2014; Gupta et al. 2008; Shirulea et al. 2012; Singh et al. 2017e).
percentage of silica and alumina are present in the raw material, As a demonstration, the concrete mix was designed for M20 with
which would not help it in taking part actively in the hydration pro- minimum amounts of cement according to IS 10262 (BIS 2009).
cess for formation of calcium silicate gels as observed by Aliabdo Marble powder as partial cement-replacing material was used be-
et al. (2014) and Vardhan et al. (2015). Thermal analysis of marble cause of its fineness. The compositions of the mixtures and their
powder showed the presence of calcium carbonate as the main con- reference mixture are presented in Table 3. The PSD of the cement,
stituent. For temperature in the range of 740°C–800°C, a steep loss sand, and marble powder is given in Figs. 1 and 2. Coarse aggre-
in weight was detected due to the decomposition of calcite, which gates are taken as passing through 20- and 10-mm sieves in a ratio
is an endothermic reaction as shown in Fig. 4(b). A scanning elec- of 65%–35% and their PSD is given in Fig. 3. The particle-packing
tron microscope (SEM) with energy-dispersive X-ray spectroscopy analysis was done using EMMA software. It helps in calculating
and displaying the PSD of a mixture of components. It applies a The procedure used was as follows: Three mortar blocks were
model’s best-fit particle packing based on the Andreasen model by cast for 3, 7, and 28 days of curing, respectively. Cement content
Andreasen and Andersen (1930) for making efficient particle pack- was taken as 200 g of cement mixed with 600 g of sand according
ing. Particle size distribution modulus, q, given by Eq. (1), was to IS 650 (BIS 1991) as 600 g, i.e., a ratio of 1∶3 for cement and
defined by Andreasen while modeling PSDs that would serve as sand according to IS 4031 Part 6 (BIS 1988). Water content was
a measure of the contribution of the various ingredient size classes taken according to the standard consistency of cement paste, which
that compose the mixture to the overall particle size distribution. In was 31%. Mortar pastes were then mixed and cast in 50-mm molds.
Eq. (2), CPFT is the cumulative percent of particles finer than a All blocks were demolded after 24 h and placed in a tap water bath
given particle size D, and Dl is the size of the largest particle at 23°C for curing. After removing them from the bath they were
surface dried and finally tested for compressive strength. The
Dq strength activity index (SAI) is therefore reported according to
CPFT ¼ × 100 ð2Þ
Dl Eq. (3)
A
The distribution modulus is the slope of the line tangent to the SAI ¼ × 100 ð3Þ
B
CPFT curve plotted on a logarithmic scale. This is a simple-to-use
tool that allows the control and optimization of the composition of where A = compressive strength of the mix sample (MPa); and
the different size classes in any given particulate system. Using the B = strength of the control mortar (MPa).
EMMA software, mixtures composed of several discrete size classes Generally for pozzolanic materials, SAI results greater than
can be easily built as a function of a desired modulus, q. Small var- 0.80 after 28 days are indicative of a positive pozzolanic activity
iations in the composition can create significant changes in the for FA for a cement replacement of 30%. ASTM C186 (ASTM
model line slope and the properties of the particle size distributions. 2015) requires a SAI greater than 0.75 after 7 and 28 days for
The q value gives the slope of the target line on the graph. For FA and natural pozzolans at a cement replacement level of 20%.
the present case a q value of 0.34 was selected, which represents a Table 4 shows the mix proportions used for the three cases.
target slump range of 110–130 mm. The software EMMA has pre-
loaded CO2 emission values for each raw material used in the mix Heat of Hydration
in its inventory. Therefore, evaluating it gives an output of how The heat of hydration for cement pastes with a w/b ratio of 0.5
much CO2 would be emitted in creating the mix. The software also was measured using an isothermal conduction calorimeter in the
helps in calculating the CO2 emissions on production of concrete. Chemical Engineering Department of BITS Pilani according to
ASTM C186 (ASTM 2015). The values were measured for the first
Strength Activity 24 h of hydration at a control temperature of 20°C.
In order to test whether marble powder acts only as a filler material
or any reaction takes place between calcite in marble and tricalcium Carboaluminate Formation
aluminate (C3 A) in cement, a strength activity test was conducted. As discussed in the “Introduction,” a reaction of CaCO3 with
Three cases were devised for preparing cement mortar blocks: C3 A forming monocarboaluminate takes place. For analyzing this,
1. 100% cement and standard silica sand; samples crushed in a strength activity test were immersed in
2. 90% cement and 10% silica sand, with the gain in strength due acetone for 24 h to stop hydration, and then ground to a fine powder
to 90% cement and the filler effect of sand; and before testing. They were tested with powdered XRD analysis in
3. 90% cement and 10% marble powder, with the gain in strength the Physics Department of BITS Pilani with an X-ray source of
due to 90% cement and the filler effect of marble powder. If any
extra gain in strength was observed, it would indicate the pos-
sibility of a chemical reaction taking place.
Cases 2 and 3 have been planned in such a way that the material Table 4. Mix proportions for different cases
replacing cement is of the same particle size distribution. One Component
material, i.e., silica sand (standard sand), is chemically inert, which
is already well established. However, the aim of the study is check Cement Sand Silica Silica Marble
Mix (g) (g) sand (g) sanda (g) powdera (g)
whether marble power reacts similarly to the compounds present in
cement, i.e., whether it takes part in the hydration process or not. Case 1 200 600 — — —
Both marble dust and silica sand would exhibit some filler effect Case 2 180 — 600 20 —
because of their particle size distribution. Case 3 190 — 600 — 20
Therefore, if any extra strength is found in the case with marble a
Particle size distribution of marble dust and silica sand replacing cement
powder, it would hint of a chemical reaction taking place. was taken as the same.
uniform. This was done to study the change in properties of con- be attributed to the fines present in marble powder, which vary in
crete essentially due to incorporation of marble powder in concrete. the particle size range of sand to finer than cement as shown in
Workability was kept constant at 100-mm slump with the use of Figs. 1 and 2, thus they help in providing efficient particle packing
superplasticizer so that the compaction energy remained the same. in concrete. Positive results for increased compressive strength for
The four water:binder ratios used were 0.35, 0.4, 0.45, and 0.5. the same mix design have been demonstrated by Singh et al.
Cement was partially replaced by dried marble powder by weight (2017e). In addition, a decrease in CO2 emissions by 5.2% from
(1∶1) at 5%, 10%, 15%, 20%, and 25% of the total binder content. 510.92 to 475.92 kg=m3 was found on replacing 10% cement by
The mix proportion adopted was C∶FA∶CA ¼ 1∶1.63∶3.02. Mix de- marble powder. However, tests were still conducted to investigate
sign was done according to IS 10262 (BIS 2009). Cement content whether any chemical reactions were taking place in the system.
was varied from 450 to 350 kg=m3 , with water kept constant at
around 160 kg=m3 .
Strength Activity
Compressive strength was measured for mainly two types of
specimens according to the standards—150-mm cubes according The results for strength activity showed additional increase of
to IS 516 (BIS 1959) and 150 × 300 mm cylinders according to strength in samples containing marble powder instead of silica
ASTM C39 (ASTM 2016d). Testing of all the samples was done sand. The strength ratio for samples at the end of 28 days was
after pond curing for 28 days. The values of strength reported were higher by almost 13%, indicating that a chemical reaction is taking
an average of nine samples. A total of 300 samples were tested and place. However, because very little amounts of silica and alumina
values were analyzed for statistical modeling. were found to be present in the marble powder, X-ray diffraction
tests were performed to determine the reason for the gain in
strength. Table 5 shows the strength activity test results.
Results and Discussion
Heat of Hydration
Particle Packing
The addition of marble dust was found to influence the hydration of
The straight line in Fig. 5 is the target [best-fit particle packing the cement paste as shown in Fig. 6. An increased rate of hydration
based on the Andreasen Model by Andreasen and Andersen was found for the sample with 10% marble dust as partial replace-
(1930)], and the irregular line represents the particle-packing curve ment of cement by weight. Tikkanen et al. (2014) also observed an
of the design mix. When the particle-packing line is above the tar- increase in degree of hydration on the addition of mineral powders
get line, it shows that too much material of that size is present in the like limestone or quartz in concrete as compared to the control
mix, and when below there is very little of that material present. mixes. The reason for increased heat of hydration could be the pro-
The results of the mix with 10% replacement of cement by marble vision of nucleation sites by the extra-fine particles of waste marble
Fig. 5. PSD for (a) control concrete mix; and (b) concrete mix with 10% marble powder.
deviation.
attributed to the acceleration effect of marble powder on the hy-
dration process, which is related to the formation of calcium car-
boaluminate hydrates. Also, the increased binding capacity of
carboaluminate is likely due to its compact structure as described
by Bonavetti et al. (2001). Singh et al. (2017e) demonstrated the
compaction and decreased porosity of concrete on use of marble
powder using SEM images. This is also in agreement with the work
of Kakali et al. (2000).
Statistical Analysis
Fig. 7. XRD of samples with (a) cement only; and (b) 10% marble powder. P = portlandite [CaðOHÞ2 ]; CS/CSH = calcium silicate hydrate;
C3 A = tricalcium aluminate; Mc = monocarboaluminate; and SO4-Aft = ettringite.
Aliabdo 0.5 0 40 — —
et al. 5 43 41.35 3.84
(2014) 7.5 44 41.71 5.21
10 44.1 41.79 5.23
15 43.5 41.15 5.41
Arshad 0.45 0 31.27 — —
et al. 10 32.76 32.32 1.33
(2014) 15 33.12 32.67 1.36
20 33.14 32.17 2.94
Fig. 9. 28-day compressive strength and percent marble powder. 25 29.16 30.81 −5.66
Rana 0.38 0 50 — —
et al. 10 51.1 51.68 −1.14
(2015) 15 49 52.24 −6.61
provide the desirable strength. A similar observation was made by 20 48 51.43 −7.15
Singh et al. (2017e) and Aliabdo et al. (2014). 25 49 49.27 −0.54
The results obtained from the experimental procedure were used
to formulate a model relating w/b ratio and marble powder content
to the compressive strength of the mix. No such model has been
reported in the literature to date. For the present investigation, the
factors taken into account that affect the strength of concrete are
w/b ratio and marble powder content.
A new relation for compressive strength and w/b ratio is given
according to Eq. (5)
w ms
log CS ¼ a1 þ a2 þ a3 log CS
cm c
w mp
¼ a1 þ a2 þ a3 ð5Þ
cm c
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