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Effect of lime water on the properties of silica fume blended cementitious


Article  in  Indian Journal of Engineering and Materials Sciences · December 2017


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Indian Journal of Engineering & Materials Sciences
Vol. 24, December 2017, pp. 491-498

Effect of lime water on the properties of silica fume blended

cementitious composite
S Maheswarana*, V Ramesh Kumara, Mohammed Saffiq Rehemana, Smitha Gopinatha,
A Ramachandra Murthya & Nagesh R Iyerb
CSIR-Structural Engineering Research Centre, Taramani, Chennai 600 113, India
Academy of Scientific and Innovative Research, CSIR Campus, Taramani, Chennai 600 113, India
Received 5 August 2017; accepted 16 May 2017
This study is to investigate the setting time and strength properties of cementitious composite mortars blended with silica
fume by the replacement of 10, 20 and 30% of cement with two types of lime water. Concurrently, cement pastes for each of
the above mix proportion are prepared to study the hydration kinetics by using XRD analysis. The ordinary potable water
has been completely replaced with two types of lime water for all the samples except control samples. The results of setting
time experiments show that there is a considerable reduction in the initial and final setting times for both the cases of lime
water and silica fume blended cement pastes compared to control sample. The lime water with ionic level suspension tends
to increase the compaction and early strength of the mortars. Though the lime waters without silica fume reduces the
strength of mortars, the specimens with silica fume and lime water tends to show increase in compressive and split tensile
strengths, influenced by the binary blended cementitious composites which improves both early strength and later strengths.

Keywords: Saturated lime water, Natural lime water, Silica fume, Cementitious composite, XRD, Strength properties

Concrete is a highly heterogeneous material produced innovative and intermixing of existing materials at
by mixture of finely powdered cement, aggregates of component level. It is well known that the concrete, in
various sizes and water with inherent physical, chemical a 2-phase system comprises of cement paste and
and mechanical properties. A reaction between the aggregates (fine and coarse), the aggregates are inert.
cement and water yields calcium silicate hydrate, which The amorphous phase calcium–silicate–hydrate
gives concrete strength and other mechanical properties, (C–S–H) is the ‘‘glue” that holds concrete together.
as well as some more by-products including calcium 1/3 of the pore space is comprised of gel pores and the
hydroxide (CH), ‘gel pores’, Aft (Ettringite), Afm rest are capillary pores. Interfacial transition zone
(Monosulfates) etc. Despite the hydrated cement and (ITZ) is the zone of bonding between cement paste
their by-product materials are available everywhere in and aggregates. Porosity of the paste as well as the
the concrete, the reactions within the concrete during proportion of CH in this zone is considerably higher
setting (fresh state) and hardening (gain strength) are than in the bulk paste. This zone forms the weak link
difficult to control and this is an ongoing problem in the in the concrete, and is usually the site of first
concrete industry. The American Society of Testing and occurrence of cracking in concrete.
Materials (ASTM) defines1 pozzolan as a siliceous or The concrete is the most widely used construction
alumino-siliceous material that in itself possesses little or materials due to its low cost and long durability.
no cementitious value, but in finely divided form and in Generally, the production of every ton of Portland
the presence of moisture will chemically react with cement releases about the same quantity of CO2, a
alkali and alkaline earth hydroxides at ordinary greenhouse gas in to the atmosphere, which is
temperatures to form or assist in forming compounds accounted for 7-8 % of total CO2 emission2,3. Hence,
possessing cementitious properties1. the need for the cement replacement is a primary
Hence, it is imperative for the evolution of new factor in construction industry. With the advent of
materials for improved performance for engineering various supplementary cementitious materials
applications. Newer materials are obtained by (SCMs), construction field has achieved enormous
potential applications by the way of reduction in
*Corresponding author (E-mail: sudha_mahesh@yahoo.com; cement consumption, enhanced properties and
smahes@serc.res.in) reduced carbon foot print. Utilization of these

industrial by-products and/or wastes are either as durability are not reported. It has been studied earlier
cement replacement materials or as aggregates in by some researchers that a high degree of silica fume
concrete presents environmental benefits. For the past agglomeration in cement pastes or mortars due to
three decades, pozzolanic materials showed much inadequate dispersion. This agglomeration of silica
interest in construction for their influence on the fume can reduce its effectiveness on properties of
higher performance of the concrete4,5. The concrete in cement paste and mortar, because of the existence of
fresh as well as in the hardened state, the SF particle clusters and a lower pozzolanic reactivity.
supplementary cementitious materials (SCMs) such as Slurried silica fume is a liquid mixture composed of
silica fume (SF), fly ash (FA), ground granulated blast un-densified powder and water in equal proportions
furnace slag (GGBS), rice husk ash (RHA), by weight, which promises a better dispersion into the
metakaoline (MK) etc improve the pozzolanic activity concrete mix and which has rarely been studied in
and also densifying the concrete by means of packing literature. Rossen et al.16 have studied the
of the solid materials in the system (filler effect) by composition of C-S-H in slurried SF cement pastes,
occupying some of the spaces/pores between the and found that the reduction of portlandite and
aggregate particles. Also, different SCMs have been increase in C-S-H quantity. Zhang et al.17 have
replaced in certain percentages for cement to get new compared the compressive strength of materials made
or improved properties of concrete in addition to of slurried and densified SF (DSF) and noticed that
reduction in carbon foot print and achieved the non-evaporable water content and compressive
great success. strength of paste containing DSF are lower than that
The pozzolanic activity of SF enhanced the containing undensified silica fume. Grist et al.18
hydration activity in cement pastes, because of its showed interest in natural lime-based hydraulic binder
amorphous form with high specific surface area. But with 25% SF by mass of cement and observed that the
it is reported in the literature6-9 that the early age continual increment of compressive strength up to 90
strength cement paste is very low. Beyond 90 days, days of curing. Recently, the strength development of
SF is consumed by CH resulting in improvement of lime–pozzolana pastes with silica fume and fly ash has
later day strength9. Apart from pozzolanic activity of been studied by Koteng et al.19 and they observed that
SF, it also acts as filler in concrete, which fills the lime based pozzolana pastes can reduce the weight of
pores and voids between the cement paste and the structural elements and the overall cost of structures.
aggregates leading to more compaction of concrete10. Other than conventional SCMs of micro-sized
The guideline for the use of SF and its beneficial materials, a series of research studies20-26 were
influence in concrete has been reported by many conducted by using various nano-sized particles such
researchers11. ACI committee11 also suggested the use as nano-SiO221,22, nano-Al2O323,27,28, nano-TiO225,
of SF up to 12% of replacement of cement. Oner nano-Fe2O326 etc towards their effects in the
et al.12 reported that the fly ash reaction needs calcium mechanical properties of concrete. Senff et al.21
hydroxide (CH) crystals to improve concrete investigated the effects on various properties of
properties, they have added lime powder with fly ash. mortar with nano-silica and micro-silica (SF) at
Mira et al.13 observed that the above stated reaction different proportions. The effects of lime water on the
exhibits significant improvement in concrete mechanical and setting properties of nano- Al2O3 up
durability rather than any influence in the to 2% blended cement had higher split strength
development of concrete strength. The treatment of compared to that of the concrete without nano- Al2O3,
concrete with lime is assured by ASTM14, but it when the specimen cured in saturated lime water for
should be used as curing water for mortar cubes. 28 days. At the same time, it was observed that the
Barbhuiya et al.15 observed that the incorporation workability has decreased for fresh concrete
of hydrated lime with silica fume in fly ash concrete, especially cured in lime water27,28 . The effect of lime
there was an improvement in early age compressive water on the properties of non-traditional materials
strength. It was concluded that both the strength and like nano-Zr2O3 incorporated concrete has been
durability of the fly ash concretes could be improved studied by Nazari and Riahi29 and observed that
by the addition of either hydrated lime or silica fume, optimum level of nano- Zr2O3 with 2% replacement
however, the quantification of the hydrated lime and of cement in concrete cured in lime water for 28 days
SF on the long-term strength development and showed the enhancement in strength, but there was

reduction in the setting times as the replacement level water filtrate is obtained by slaking of lime obtained
increases. from calcinations of natural seashells (labeled, LW)
There is hardly any study which clarifies optimum and the second lime water is obtained by dissolving
use and/or consumption of SF in the concrete system commercial calcium hydroxide (Ca(OH)2) (labeled,
at early or later stage. Generally, the pozzolanic LD) received from Merck Millipore, Division of
activity (the chemical reaction of CH crystal with Merck with high purity. The lime water filtrates for
SCMs) starts only after the formation of hydrated calcium hydroxide is obtained from full saturation
product of cement. That is, the formation of CH (~1 g/L) of calcium hydroxide in water. The pH and
crystals occurred after the hydration of C3S and C2S conductivity of the prepared solutions along with
in the cement. It is well known that the hydration of potable water are given in Table 2. The increased
C3S is shorter than C2S hydration; hence there is a conductivity value of the slaked lime water may be
delay in pozzolanic activity. The early pozzolanic due to the mobility of more ions in this particular
activity could be achieved by using hydrated lime of case. Moreover, the alkalinity (higher pH) level of
lime water solution in place of ordinary potable water. lime waters is more than that of potable water and this
Therefore, this study is planned to investigate the will be useful when reacting with SCMs such as SF.
influence of two sources of lime water in the binary The chemical composition of the raw materials is
blended cementitious composites in the paste and analyzed using X-ray fluorescence spectrometer
mortar level. It is also aimed at to find the consistency (Bruker S4 Pioneer). Bruker’s D2 PHASER X-ray
level, setting time properties, hydration process and diffraction (XRD) system, equipped with 1-D
mechanical properties of Portland cement based LynxEye detector is used in the present study and it
composite containing SF and mixed with lime water. employs Cu-Kα radiation (30 kV, 10 mA) with Nickel
filters. A continuous scan of 2θ from 10° to 60° in
Materials and Methods step width of 0.020 and counting time of 0.5 s per step
The cement used for pastes/mortar is 53 grade is performed on less than 25 µm size powder samples.
ordinary Portland cement (OPC) conforming to Experiments are designed to evaluate the
IS: 12269 – 198730 and the physical and chemical performance of Portland cement based materials
properties are given in Table 1. The locally available containing silica fume mixed with W, LW and LD
grade 2 sand conforming to IS: 383-197031 is used. (Table 3). The mix design for binder to sand for
For determination of appropriate water to cement mortars is 1:3. Total of 15 mortar cubes for each
ratio, standard consistency test has been conducted mixes are cast to test the compressive strength for
and water to cement ratio of 0.41 is arrived at. different days, viz., 3, 28 and 90 days (each 5 cubes)
Ordinary potable water is used for control pastes and of curing. The cement pastes for each of the above are
mortar cubes and cylinders. Two types of lime are also mixed to study the hydration kinetics of different
used in lime water filtrate preparation. First lime days of curing using XRD analysis. Concurrently, the
Table 1 — Physical and chemical properties of cement and SF mortar cylinders (50 mm × 100 mm) for each mix are
cast for the similar proportions to study the split
Chemicals Oxide Constituents (%)
tensile strengths for different days, viz., 7 and 28 days
Cement Silica fume
(each mix 6 cylinders) of curing. The polycarboxylate
SiO2 20.24 94.73
Al2O3 5.64 -
based high range water reducing admixture
Fe2O3 4.07 - (HRWRA) is used as superplasticizer (SP) by weight
CaO 63.42 - of cementitious materials to get the uniform
SO3 3.48 0.2 flowability in cube mortars / cylinder mortars. The
Na2O 0.19 0.51 water to binder (cement + SF) ratio for all mixtures is
K2O 0.56 - fixed as 0.4.
MgO + MnO 0.88 -
LOI 1.52 1.5 Table 2 — pH and conductivity measurements of lime waters
Physical properties Solution pH Conductivity,
Color Dark gray Gray Value mS/cm
Specific gravity 3.162 2.15 Potable water 7.678 1.431
Bulk density, g/cm3 1.561 0.13-0.6 Slaked, Natural lime water, LW 9.733 5.142
Fineness passing 40 µm sieve, % 85 92-95 Saturated calcium hydroxide 10.719 1.286
Moisture content, % <1-2 <1 solution, LD

To prepare the mortars containing silica fume, first and 30% and with ordinary potable water compared to
the binders such as cement and silica fume are added to control samples. This may be due to the acceleration
river sand and placed in mixer machine resuming dry of hydration process by silica fume with cement. In
mix for about 2 min. Then the water, which is premixed the case of control with saturated lime water, the
with the superplasticizer, is added and mixing is carried initial setting time is slightly higher because of more
out for 5 min. Finally, the freshly prepared mortar is availability of the calcium hydroxide to react. This
poured into cube moulds of size 70.6 × 70.6 × 70.6 mm. trend has changed with addition of silica fume, that is,
Similarly, the mortar cylinders of size 50 × 100 mm are the IST and FST are reduced considerably because of
cast. After pouring, an external table vibrator is used to consumption of calcium hydroxide by silica fume at
facilitate compaction and decrease the amount of air the early stages as well as later stages. Sellevold
bubbles. The specimens are de-molded after a lapse of et al.32 observed that SF accelerates the hydration of
24 h for moist curing and then cured in water till for the cement during the early stages by providing
testing periods 3, 28 and 90 days. Concurrently, to study nucleation sites where the products of cement
the hydration kinetics by using XRD analysis of the hydration can more readily precipitate from solution.
above mixes in the paste form are also prepared. The
compression test is carried out on 100t UTM under load Semi-quantitative XRD analysis of composite pastes
control. The tensile strength of concrete is evaluated Figures 2-5 show the XRD patterns of pastes of all
using a split cylinder test, in which a cylindrical compositions at 3 and 28 days of curing and the
specimen is placed on its side and loaded in diametrical quantification of the various phases are given in Tables
compression, so as to induce transverse tension. 4-7. The main crystalline phases of calcite

Result and Discussion

The following sections present the properties of
cementitious composites mixed with potable water
(W), saturated lime water (LD) and natural lime water
(LW) solution. Consistency level, setting times,
hydration process and mechanical properties such as
compressive and split tensile strengths are evaluated.
Initial and final setting times
The results of the setting times studied for the
cement composite pastes with partial replacement of
silica fume and with two types of lime waters by
using Vicat apparatus are provided in Fig. 1. It has
been found that there is a reduction in both the initial
and final setting timings (IST and FST) for the
samples with replacement of silica fume by 10, 20 Fig. 1 — Initial and final setting times
Table 3 — Mix proportions of specimens for mortars
Code of mix Cement Silica Fume Sand Water Lime water Superplasticizer, (%)
(kg/m3) (kg/m3) (kg/m3) (kg/m3) (kg/m3)
Control 455 0 1364 181 - 0
CLD 455 0 1364 - 181 0
CLW 455 0 1364 - 181 0
CSF-10 410 45 1364 181 - 0
CSF-20 364 91 1364 181 - 0
CSF-30 319 136 1364 181 - 0
CLDSF-10 410 45 1364 - 181 1.0
CLDSF-20 364 91 1364 - 181 1.5
CLDSF-30 319 136 1364 - 181 2.0
CLWSF-10 410 45 1364 - 181 1.0
CLWSF-20 364 91 1364 - 181 1.5
CLWSF-30 319 136 1364 - 181 2.0

(C- calcium carbonate, CaCO3), Portlandite The XRD patterns and S-Q analysis of hydration of
(P-calcium hydroxide, Ca(OH)2), ettringite (E), gypsum cement pastes of control, CLD and CLW samples are
(G), quartz (Q) are identified. The hydration reaction shown in Fig. 2 and Table 4 gives their quantification
products of cement such as calcium silicates/aluminates values. It is found that the amounts of crystalline
such as C-S-H, C-A-S-H (gehlenite hydrate) including portlandite contents are almost same in all the mixes. It
tobermorite type C-S-H are also evidenced; since the shows that the availability of portlandite crystals is
C-S-H, which is an amorphous phase, its structure more to react with cementitious additives, if any.
cannot be identified exclusively by XRD33, hence it is Similarly, the total quantity of amorphous contents
mentioned in the quantitative analysis tables (Tables such as C-S-H, C-A-H and C-A-S-H etc are equal in all
4-7) as ‘total amorphous contents’ by using TOPAS the cases of mixes. But in the case of samples CSF-10,
academic software (Bruker AXS, Karlsruhe, Germany). CSF-20 and CSF-30, wherein potable water is used, it
The semi-quantitative analyses of XRD of composites is noticed that the consumption of CH crystal
show that the reduction in Portlandite peaks (CH (Table 5 and Fig. 3) and accordingly observed the
crystals), hence the improvement in the C-S-H quantities incremental quantity of amorphous contents in these
in the presence of silica fume at different ages. cases and reduction of CH peaks in the XRD spectrum.
In these cases, there are existence of CH peaks with

Fig. 2 — XRD patterns of Control, CLD and CLW samples for 3 Fig. 4 — XRD patterns of CLDSF-10, CLDSF-20and CLDSF-
and 28 days 30samples for 3 and 28 days

Fig. 3 — XRD patterns of Control, CSF-10, CSF-20 and CSF-30 Fig. 5 — XRD patterns of CLWSF-10, CLWSF-20 and CLWSF-
samples for 3 and 28 days 30 samples for 3 and 28 days

10% and 20% of SF, but complete consumption is only by about 50% at 28 days, because of less
found in 30% SF replacement in 3 days and 28 days of availability of SF to react with CH solution. Similar
curing. These results are supported by those of Ono result has also been observed by Hooton35 that with
et al.34, studied the cement-silica fume system in pastes 20% by volume silica fume replacement, no CH was
and the amounts of CH present after various periods of detectable after 91 days of moist curing at 23°C, while
hydration with different dosages of silica fume. At very 10% silica fume reduced CH by 50% at the same age.
high dosages, almost all CH is consumed by 28 days, In the case of saturated lime water, it is found that
but at 10% replacement of silica fume, CH is reduced the CH crystals for 3 days and 28 days of curing
samples, because of less dosage of SF, its consumption
Table 4 — S-Q analysis for hydration of paste composites CON, also less. Whereas 20% and 30% SF replacement, the
CLD and CLW series consumption of CH is almost completed and there are
Compounds 3 days 28 days no CH crystal for further reaction (Fig. 4 and Table 6).
Control CLD CLW Control CLD CLW Simultaneously, the incremental quantity of amorphous
Calcite (C) 16.69 11.51 11.19 11.91 12.19 15.12 contents is also found in the case of CLWSF series too
Ettringite (E) 1.11 2.05 1.26 0.92 1.13 0.364 (Table 7 and Fig. 5).
Gypsum (G) 3.69 3.69 3.39 3.61 4.39 4.12 Hence, it is concluded from the XRD analysis,
Portlandite (P) 12.57 11.51 12.58 19.09 17.97 15.11 there are two stages of CH crystal consumption and
Quartz (Q) 1.37 0.84 1.03 0.65 1.22 1.1
enhancement in quantity of C-S-H and the like
Other amorphous 64.57 70.42 70.55 63.82 63.1 64.19
contents including materials, which lead to enhancement of strength of
C-S-H, C-A-S-H etc mortar/concrete with similar composition. In the XRD
Table 5 — S-Q analysis for hydration of paste composites Control and CSF series
Compounds 3 days 28 days
Control CSF-10 CSF-20 CSF-30 Control CSF-10 CSF-20 CSF-30
Calcite (C) 16.69 12.06 6.83 11.79 11.91 9.67 11.89 12.55
Ettringite (E) 1.11 2.04 3.57 0 0.92 3.13 4.89 4.38
Gypsum (G) 3.69 3.35 0 0 3.61 2.39 0 0
Portlandite (P) 12.57 7.22 2.39 1.1 19.09 7.11 4.54 0
Quartz (Q) 1.37 0.61 0.44 0.55 0.65 1.47 0 0
Other amorphous contents including 64.57 75.72 86.77 86.56 63.82 76.23 78.68 83.07
C-S-H, C-A-S-H etc
Table 6 — S-Q analysis for hydration of paste composites CLDSF series
Compounds 3 days 28 days
Calcite (C) 24.95 11.43 9.58 12.27 9.76 12.33
Ettringite (E) 1.02 3.36 2.52 0.64 4.02 2.09
Gypsum (G) 3.43 3.04 0 4.15 4.18 0
Portlandite (P) 5.15 1.86 0 9.15 0 0
Quartz (Q) 1.89 0.47 0 0.52 0.24 0.29
Other amorphous contents including 63.565 77.84 87.9 73.28 81.8 85.29
C-S-H, C-A-S-H etc

Table 7 — S-Q analysis for hydration of paste composites CLWSF series

Compounds 3 days 28 days
Calcite (C) 12.65 6.99 8.54 10.44 9.79 15.37
Ettringite (E) 3.35 3.59 3.15 3.69 3.1 2.51
Gypsum (G) 3.45 1.02 0.64 4.01 2.64 1.88
Portlandite (P) 9.51 5.51 0.55 9.27 4.02 0.64
Quartz (Q) 0.64 0.25 0.2 0.17 0.95 0.2
Other amorphous contents including 68.4 79.66 88.31 71.42 79.14 82.75
C-S-H, C-A-S-H etc

As predicted by the Nazari and Riahi25, the reduction

in the strength of cementitious composites with lime
water curing is observed in this study due to more
availability of Ca(OH)2 presence. The increase of
compressive strength is noticed in two stages, viz., early
(3-day) and later day strength (90-day) compared to
control mortars. This is due to the early consumption of
added calcium hydroxide solution by silica fume to form
additional C-S-H. This has been confirmed by semi-
quantitative analysis of XRD of cement composite
pastes of similar mix proportions. There is a continual
improvement of compressive strength observed for 28
days cured samples. After 28 days, the hydration
Fig. 6 — Comparison of compressive strength of various
composite mortars for 3, 28 and 90 days
reaction of cementitious composites are almost
saturated, the subsequent strength gain is observed to be
generally low. But in the second stage, that is 90 days
cured samples, the further strength increments observed
because of consumption of the by-product of cement
hydration, namely the calcium hydroxide by silica fume.
It is also noted that the saturated lime water (CLDSF
series) with 20% silica fume (strength gain of 17% over
control) and natural lime water (CLWDSF series) with
30% silica fume replacements (strength gain of 16%)
provided higher compressive strength compared to
control mortars (Fig. 6). This incremental effect could be
due to the additional formation of C-S-H in the cement
moiety during subsequent hydration.
Fig. 7 — Comparison of split tensile strength of composite Split strength development for mortar mixes
mortars for 7 and 28 days Development of split tensile strengths of cylinder
analysis of all the mixes shown that the quantity of mortars incorporating lime water and SF are higher
calcite throughout equally, which act as an inert filler than the samples without SF and lime water. The split
material and mere presence of numerous fine tensile strength enhancement for lime water influenced
particles-whether pozzolanic or not, it has an binary blended cementitious composite show 21-28%
accelerating effect on the cement hydration. over control samples after 28 days curing. That is, for
both the types of composites, as the compressive
Compressive strength development for mortar mixes strength increases, the tensile strength also increases
It is observed that there is no change in the (Fig. 7). It is observed from this study, the early
compressive strength while using lime waters (CLD strength gain is almost similar to the control samples,
and CLW) alone, whereas there is a considerable whereas 28 days split tensile strength, increment in
strength gain for the samples CSF10, 20 and 30 with strength is observed. This shows a clear indication of
potable water (W) than control for all the days, viz., 3, improved binding properties between the blended
28 and 90 days of curing. The early strength gain for composites such as cement-SF-lime water.
the cases of CLDSF and CLWSF series is observed
over control mortars, particularly a strength gain in Conclusions
the range of 13-34% for the samples CLDSF-30 and This work is a preliminary investigation to study the
CLWSF-30. This trend is continuing up to 28 days of effect of two different lime water on the properties of
curing. This is evident that the increase in percentage silica fume blended cementitious composites. The use of
addition of SF attributes to increase the early strength lime water with silica fume mixed Portland cement
of the cement mortar cubes when compared to 3rd day based composites affects both setting time and
strengths of control mortars. compressive and split strengths of the mortar specimens.

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27 Nazari A & Riahi S, J Compos Mater, 45 (2011) 1059-1064.
with cement and enhancement of compressive and split 28 Nazari A & Riahi S, J Compos Mater, 45 (2010) 1165-1172.
strength of the composite mortars. 29 Nazari A & Riahi S, J Compos Mater, 45 (2011) 639-644
30 IS: 12269-1987. Specification for 53 Grade Ordinary
Portland Cement.
The researchers of CSMG, AML and STL of 31 IS: 383-1970. Specification for Course and Fine Aggregates
CSIR-SERC are greatly acknowledged for the useful from natural sources for concrete
discussion and suggestions provided during the course 32 Sellevold E J, Badger D H, Klitgaard J K & Knudsen T, Silica
of the investigations. Fume-Cement Pastes: Hydration and Pore Structure.
Condensed Silica Fume in Concrete, Proc Nordic Research
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