materials

Article
The Relation between Concrete, Mortar and Paste Scale Early
Age Properties
Martin Klun, Vlatko Bosiljkov and Violeta Bokan-Bosiljkov *

Faculty of Civil and Geodetic Engineering, University of Ljubljana, Jamova 2, SI-1000 Ljubljana, Slovenia;
martin.klun@fgg.uni-lj.si (M.K.); vlatko.bosiljkov@fgg.uni-lj.si (V.B.)
* Correspondence: violeta.bokan-bosiljkov@fgg.uni-lj.si

Abstract: Microstructure development of concrete, mortar, and paste scale of cement-based material
(CBM) during the early hydration stage has a significant impact on CBM’s physical, mechanical, and
durability characteristics at the high maturity state. The research was carried out using compositions
with increased autogenous shrinkage and extended early age period, proposed within the RRT+
programme of the COST Action TU1404. The electrical conductivity method, used to follow the
solidification process of CBM, is capable of determining the initial and final setting time, and the end
of the solidification process acceleration stage for the paste and mortar scale. Simultaneous ultrasonic
P- and S-wave transmission measurements revealed that the ratio of velocities VP /VS is highly
dependent on the presence of aggregates—it is considerably higher for the paste scale compared to
the mortar and concrete scale. The deviation from the otherwise roughly constant ratio VP /VS for
each scale may indicate cracks in the material. The non-linear correlation between the dynamic and
static elastic moduli valid over the three scales was confirmed. Additionally, it was found that the
static E-modulus correlates very well with the square of the VS and that the VS is highly correlated to



the cube compressive strength—but a separate trendline exists for each CBM scale.



Citation: Klun, M.; Bosiljkov, V.; Keywords: concrete; mortar and paste scale of cement-based material; early hydration stage; microstructure
Bokan-Bosiljkov, V. The Relation development; electrical conductivity; ultrasonic method; standard tests
between Concrete, Mortar and Paste
Scale Early Age Properties. Materials
2021, 14, 1569. https://doi.org/
10.3390/ma14061569 1. Introduction
Formation and development of cement-based materials’ (CBMs) internal structure
Academic Editor: Georgios Savaidis
is a complex process that depends on various influencing parameters—such as the type
of cement, aggregate, water-to-cement ratio, presence of chemical admixtures, and/or
Received: 1 March 2021
Accepted: 19 March 2021
mineral additives, temperature, curing conditions, etc. Immediately after mixing the CBM
Published: 23 March 2021
components into a solid suspension, the cement hydration process starts. During the
process, many chemical and physical changes occur that result first in the change of the
Publisher’s Note: MDPI stays neutral
CBM’s physical state (transition from a quasi-fluid state to a solid-state—setting). After the
with regard to jurisdictional claims in
solid-state is reached, ongoing hydration reactions result in a high state of CBM’s maturity
published maps and institutional affil- that is reflected in the low rate at which the material’s strength and elastic properties are
iations. changing with time. Upon reaching this high state of maturity, the corresponding time
is known as an early hydration period that varies from several hours to a few days or
even weeks, depending on the CBM’s composition and curing conditions. Understanding
microstructure development in CBMs in this early hydration period is fundamental, as it
Copyright: © 2021 by the authors.
has a significant impact on the physical, mechanical, and durability characteristics of CBMs.
Licensee MDPI, Basel, Switzerland.
Among other mechanisms, CBMs can undergo significant volumetric changes from an
This article is an open access article
early age due to an increase in temperature, moisture variations, autogenous shrinkage, etc.
distributed under the terms and These volumetric changes often cause cracks inside the CBM structure or at least induce
conditions of the Creative Commons tensile stresses that reduce the tensile strength of the CBM. Such defects in the CBM can
Attribution (CC BY) license (https:// reduce the long-term safety and durability of reinforced concrete structures [1].
creativecommons.org/licenses/by/ Standard test methods used to evaluate the physical and mechanical characteristics
4.0/). of the CBMs cannot provide enough in-depth knowledge of concrete behaviour during

Materials 2021, 14, 1569. https://doi.org/10.3390/ma14061569 https://www.mdpi.com/journal/materials

Materials 2021, 14, 1569 2 of 24

an early age and throughout its service life. There is a need for continuous monitoring
of critical properties from the start of setting to the mature age of the CBMs. Many new
measurement systems for early-stage testing have been developed in recent years [2]. Ultra-
sonic wave transmission techniques focus on determining different stages during the CBMs
structure formation; they especially focus on the setting (initial and final setting times) and
early age mechanical properties [3–13]. Acoustic emission techniques are used to detect
cement particles’ settlement, segregation, cavitation, migration of water, the formation of
hydrates, and early micro-cracking of CBMs in a fresh state and during the solidification
process [14–18]. Measurement of time-dependent electrical conductivity provides informa-
tion on early age mechanical properties and different stages during the CBMs structure
formation; the influence of aggregate and properties of the interfacial transition zone can
be estimated as well [8,19–23]. Nuclear magnetic resonance is used for the continuous
characterization of the evolving microstructure of various cementitious materials during
the setting process [24–28]. Among the listed measurement systems, ultrasonic techniques,
in particular, have great potential to become standard testing techniques. They can be used
to monitor the solidification process of the CBMs and determine elastic parameters, as well
as evaluate the strength of the early age CBM due to their clear physical basis [2].
In [10,11], the process of setting and hardening was monitored using ultrasonic
transversal or shear wave (S-wave) transmission velocity and dynamic elastic modu-
lus. These two parameters have been proven more CBM setting sensitive than ultrasonic
longitudinal or compression wave (P-wave) transmission velocity. The kinetics of the
dynamic elastic modulus development is tightly linked with the S-wave transmission
velocity development, making the perception of the hardened phase of hydration products
possible. Additionally, simultaneous P- and S-wave transmission velocity measurements
confirmed the correlation between the compressive or tensile strength and dynamic elastic
modulus at the early age of CBMs [12]. These findings indicate that the elastic parameters
are valid solidification indicators, with which the development of other mechanical char-
acteristics of CBMs can be evaluated at an early age. Elastic material parameters are bulk
density-dependent, thus containing additional and variable material parameters, essential
for the mechanical properties of CBMs [13].

2. Research Significance
In this study, advanced non-destructive and standard destructive tests were com-
bined to evaluate properties of CBM at three scales—the concrete scale and “identi-
cal” compositions at the mortar and paste scale. The research was carried out using
materials and compositions proposed within the Extended Round Robin Testing Pro-
gramme (RRT+ ) of the COST Action TU1404: Towards the next generation of standards
for the service life of cement-based materials and structures [1]. The raw materials
were supplied by EDF, France—connected to a broader VerCoRs programme (https:
//fr.xing-events.com/EDF-vercors-project.html accessed on 14 March 2021). The Uni-
versity of Ljubljana (UL) was one of 42 research institutions involved in the RRT+ and
was responsible for mechanical properties testing protocols. An additional task for the
research group was collecting and analysing the mechanical properties test results. Results
of 15 laboratories were available for analyses, predominantly for the VerCoRs concrete
composition with a water-to-cement ratio of 0.52 and specimens aged 7 and 28 days [29,30].
Modified CBM composition (water-to-cement ratio 0.40) was tested as well, but only 3 labo-
ratories reported test results for specimens aged 7 days or less. Moreover, only UL reported
results for the tensile and flexural strength and modulus of elasticity on the paste and
mortar scale. The results obtained by UL showed a decrease in the tensile strength with
increasing age for the paste and mortar scale of the two CBMs during the early hydration
stage [31,32]. As there were no results available for comparison in the RRT+ programme,
the raw materials still available were used for a new, more comprehensive study. It was
designed and conducted to confirm or reject those observations and as proof of concept for
a broader study about the properties of cement and lime-based masonry mortars.
Materials 2021, 14, 1569 3 of 24

This study aims to monitor CBM’s solidification kinetics and the development of
mechanical properties at an early age from up to 7 days. The studied RRT+ cement paste,
mortar and concrete scale compositions are those with a water-to-cement ratio of 0.4 to
increase the autogenous shrinkage of the CBM. The superplasticizer used delayed the
setting of the CBM considerably and thus extended the length of the early age period.
The electrical conductivity measurements were used to follow the solidification process
of a particular CBM, from the state of solid suspension to the age of 7 days. On hardened
specimens that were able to withstand handling operation and self-weight, the transmission
times of ultrasonic P- and S-waves were measured simultaneously and standard destructive
tests were performed to determine both dynamic and static mechanical properties. Based on
the results of the performed tests, the correlations between different mechanical properties
over the three CBM scales and between dynamic and static characteristics were determined
and mutually compared; they were also compared to results obtained by other researchers.

3. Materials and Methods

3.1. Materials and Compositions
The cement used was CEM I 52.5 N CE CP2 NF Gaurain (CCB, Gaurain, Belgium).
The cement’s Blain specific surface area was 4400 cm2 /g, and its density was 3.19 g/cm3 .
The chemical composition of the cement is given in Table 1. The fine aggregate used
was predominantly siliceous (72% of SiO2 and 13% of CaCO3 ) sand of 0–4 mm fraction,
with a density of 2580 kg/m3 and water absorption equal to 0.77%. The coarse aggregate
used was a combination of siliceous-calcareous gravel of a 4–11 fraction (R GSM LGP1)
and 8–16 fraction (R Balloy). The 4–11 and 8–16 fractions density were 2530 kg/m3 and
2580 kg/m3 and water absorption were equal to 2.61% and 2.25%, respectively. The
Los Angeles abrasion coefficient of the gravel fractions was less than 30. The grain size
distribution and appearance of the fractions are given in Figure 1. As an admixture, the
superplasticizer SIKAPLAST Techno 80 (SP) was used to obtain adequate workability of
CBM mixtures.

Figure 1. Grain size distribution and appearance of the 0/4, 4/11.2 and 8/16 fractions.
Materials 2021, 14, 1569 4 of 24

Table 1. Chemical composition of cement.

Oxide (%) SiO2 CaO MgO Al2 O3 Fe2 O3 SO3 Na2 O K2 O Cl

CEM I 21.3 63.8 1.9 3.5 4.3 2.7 0.09 0.59 0.05

Compositions of tested CBM scales, concrete (MOC), mortar (MOM) and cement paste
(MCP) are presented in Table 2. All compositions were prepared with a water-to-cement
ratio of 0.4 and a relatively high SP content to achieve a higher magnitude of autogenous
shrinkage and a higher magnitude of strength at an early age. The three mixtures were
“identical” mixtures on concrete, mortar, and paste scale: MOM was obtained by excluding
the gravel from the MOC, and MCP was obtained with gravel and sand exclusion from the
MOC. As a result, the cement content increased considerably from concrete to mortar and
paste scale when compositions were given per 1 m3 volume (Table 2). The SP percentage
was reduced for the MCP composition to provide the fresh paste mixture’s stability.

Table 2. Composition of cement-based materials’ (CBMs) [33].

Basic Material Type of the Material MCP (kg/m3 ) MOM (kg/m3 ) MOC (kg/m3 )
Cement CEM I 52.5 N 1299 689 439
Dry sand 0–4 mm \ 1212 772
Fully 4–11 mm \ \ 525
saturated gravel 8–16 mm \ \ 424
Admixtures Superplasticizer 5.85 5.85 3.73
Added water * Tap water 514.8 280.1 178.4
weff /c 0.4
* Added water = Effective water (obtained from weff /c ratio) − 0.8 * amount of the Sp (80% of Sp mass is water) +
water theoretically absorbed by the sand (0.77% as a coefficient of absorption).

Details of materials and compositions used to prepare CBMs are available in the
Testing protocols of the RRT+ programme [33].
It is important to note that the properties of the mortar and concrete scale of the
CBM are highly related to the aggregate properties. Recent studies on CBMs have shown
that, besides properties commonly reported for aggregates (such as the geological nature,
density, water absorption and grain size distribution), shape regularity, shape ratio, surface
texture, chemical composition, and LA abrasion resistance are additional parameters that
significantly influence physical and mechanical properties of the CBM [34,35]. There-
fore, the reported results are valid for the aggregates used in this study and should not
be generalised.

3.2. Preparation of Test Specimens and Fresh Properties Testing

All the basic materials, including water, were stored under controlled laboratory
conditions at a temperature of 20 ± 2 ◦ C and relative humidity higher than 60%. The target
temperature of the materials before mixing of CBMs was 20 ◦ C. Each gravel fraction’s
initial water content was measured 7 days before mixing the MOC and the water required
for the fraction to reach a fully saturated surface dry state was added to the aggregate
grains kept in a plastic container. After mixing of aggregate grains and added water, the
container was sealed with a lid. The water content of the 4–11 and 8–16 fractions, before
the mixing of MOC, was 2.76% and 2.56%, respectively and surface water was considered
in calculating the water that was ultimately added to the mixer.
The mixing procedures are described in the Testing protocols of the RRT+ programme [33].
The mixing procedure of MCP closely followed the procedure described in standard EN
196-3 [36], and the procedure of mixing MOM and MOC followed the procedure from
the standard EN 480-1 [37]. For each of the three CBM mixtures, 45 test specimens were
Materials 2021, 14, 1569 5 of 24

made—9 for each testing stage. Tests were carried out in 5 stages; at the ages of 30, 36, 48,
72 h, and 7 days (168 h).
After the mixing of MCP and MOM, the mixture temperature was measured and
consistency was evaluated by flow table test according to the EN 1015-3 [38]. Due to the
MCP’s high flowability, a modified procedure was applied, which excluded dropping
(15-times) of the flow table. The procedure is described in [39] and the obtained value
is referred to as the slump-flow value. Fresh density was evaluated following the EN
1015-6 [40] procedure. After that, mixtures were moulded into prism-shaped moulds with
standard dimensions of 40 × 40 × 160 mm3 . Three specimens were made for every single
test at a particular age. For standard tests of elastic modulus, the standard prism moulds
were halved to dimensions 40 × 40 × 80 mm3 , where EN 196-1 [41] tolerance requirements
were considered (Figure 2). Six specimens with dimensions of 40 × 40 × 80 mm3 were
made for each stage of testing (3 for compressive strength test and 3 for determination of
elastic modulus and σ-ε behaviour in compression).

Figure 2. An example of a set of moulds filled with cement paste (MCP) mixture for testing at a
single age.

In the case of modified ordinary concrete (MOC), the mixture temperature was mea-
sured and consistency and fresh density were evaluated following EN 12350-2 [42] and
EN 12350-6 [43] procedures, respectively. Due to slump values [42] higher than 210 mm
and associated reduced sensitivity of the test method [44], the spread of the specimen
after the slump measurement was recorded as well. The method is similar to that used
for the MCP specimen. For each testing age, three prism specimens with dimensions of
100 × 100 × 400 mm3 , three cube specimens with dimensions of 150 × 150 × 150 mm3 and
three cylinders with a diameter of 100 mm and height of 200 mm (100/200 mm cylinder)
were produced. All the specimens in moulds were stored at relative humidity higher than
95% and a temperature of 20 ± 2 ◦ C. Specimens for determination of elastic modulus and
Poison’s ratio were equipped by double direction strain gauges, measuring longitudinal
and transverse strains simultaneously.
Specimens for measuring temperature and electrical conductivity of mixtures were
cast into the custom-made extruded polystyrene container, and the upper surface was
covered with a polyvinyl sheet to avoid water evaporation, as shown in Figure 3. Inside
dimensions of the container were 5 × 10 × 15 cm3 , to ensure complete immersion of
the sensors into the mixture. For each of the three mixtures, 2 parallel test specimens
were prepared.
Materials 2021, 14, 1569 6 of 24

Figure 3. Custom-made container (left) and moulded specimens prepared for temperature and
conductivity measurements (right).

The custom-made containers were of the same dimensions as those used in [8]. In this
way, the comparison of test results and determination of setting and hardening parameters
of the CBMs at an early age is possible.

3.3. Test Methods

3.3.1. Temperature and Electrical Conductivity Sensor System
Temperature and electrical conductivity in the CBM mixtures were measured with
a commercial Consensor 2.0 system (Consensor B.V., Rotterdam, The Netherlands) [19],
which follows the early age evolution of the CBMs properties as a function of time.
In each polystyrene container, a sensor was positioned at the specimen’s centre,
as shown in Figure 3. In this way, it was completely enclosed with the CBM mixture.
Continuous measurements (in 10-min intervals) of conductivity and temperature for each
CBM mixture started immediately after the mixture was moulded into the polystyrene
container and continued for the first 7 days of CBMs specimens’ setting and hardening.
All that time, containers with specimens were stored in a laboratory under a controlled
temperature of 20 ± 2 ◦ C.

3.3.2. Ultrasonic Method

For measuring the transmission time of longitudinal ultrasonic waves (P-waves) and
ultrasonic shear waves (S-waves), the Proceq Pundit PL-200 device (Figure 4) (Proceq,
Schwerzenbach, Switzerland) was used, with an operating frequency range of 20 kHz to
500 kHz. This range of frequencies is appropriate for the research of building materials [4].
With the ultrasonic method, the dynamic elastic modulus (Ed ), the dynamic Poisson’s ratio
(νd ) and dynamic shear modulus (Gd ) were determined (Figure 5). Measurements were
made on the MCP and MOM specimens with 40 × 40 × 160 mm3 dimensions and on MOC
specimens with 100 × 100 × 400 mm3 , using the shear waves probes with a frequency of
250 kHz. Tests were carried out before standard testing on specimens aged 30, 36, 48, 72 h
and 7 days.
A single MCP, MOM, and MOC specimen was installed between transducers, convert-
ing electric voltage to ultrasonic waves and vice versa. Both transducers have to be firmly
pressed on both sides of specimens to transmit ultrasonic waves directly. Complete contact
between the transducer and surface of the specimen is extremely important to prevent
the ultrasonic signal’s reflection and losses. For this reason, a thin layer of coupling gel
was used. For transducers of ultrasonic P-waves, the coupling gel could be glycerine, but
it has to be a high viscosity gel for S-waves transducers. When measuring the S-wave
transmission time, the transducers’ correct settlement position has to be controlled because
the S-wave signal is the strongest when transducers are parallel to each other. In the
Materials 2021, 14, 1569 7 of 24

opposite case, when transducers are perpendicular to each other, the signal can disappear.
In literature [5,6], the Hilbert transformation algorithm is shown to identify ultrasonic
S-wave transmission. The Hilbert transformation changes the signal into an analytical
shape with a defined amplitude and phase.

Figure 4. Ultrasonic device Proceq Pundit PL-200.

Figure 5. Determination of the dynamic elastic properties using the Pundit device.

Ultrasonic P- and S-wave velocity within a material heavily depends on the material’s
density, elastic modulus, shear modulus and Poisson’s coefficient. Before determining
the elastic properties at different ages, the specimen’s density was calculated according
to the standard EN 1015-10 [45]. The correlation between the mentioned parameters and
ultrasonic wave velocity has been determined for isotropic homogenous materials [46].
In general, the modulus of elasticity E refers to the axial deformation of a material due
to the P-waves, whereas the shear modulus refers to the shear deformation of a material
Materials 2021, 14, 1569 8 of 24

caused by the S-waves [2,47]. The ratio between P- and S-wave transmission velocity is
highly dependent on Poisson’s ratio, which presents the ratio between the axial and shear
deformation [7]. The CBMs are homogenous, isotropic elastic materials; therefore, the
equations for calculating dynamic elastic parameters exist. Index d stands for the dynamic
elastic parameters, and the equations (Equations (1)–(3)) are based on the transmission
velocity of ultrasonic P- and S-waves and bulk density of the material [2,46]:

VP2 − 2VS2
νd = (1)
2 VP2 − VS2

(1 + νd )(1 − 2νd )
Ed = VP2 ρ = 2VS2 ρ(1 + νd ) (2)
(1 − νd )
Ed
Gd = = VS2 ρ (3)
2 + 2νd
where νd stands for dynamic Poisson’s ratio, VP is the transmission velocity of ultrasonic
P-waves, VS is the transmission velocity of ultrasonic S-waves, Ed is the dynamic elastic
modulus, Gd the dynamic shear modulus and ρ is the density of CBM.

3.3.3. Compressive Strength and Tensile Strength

The compressive strength fc for MCP and MOM specimens was assessed follow-
ing the standard EN 1015-11 [48], on the halves of 40 × 40 × 160 mm3 prism, after the
flexural test. For determination of nominal compressive stress, needed for cyclic load-
ing/unloading protocol to determine the modulus of elasticity, the prism specimens of
dimensions 40 × 40 × 80 mm3 were used. An example of compressive tests performed is
shown in Figure 6. The compressive strength of the MOC was determined by following the
standard EN 12390-3 [49], on the 150 mm cube and 100/200 mm cylinder.

Figure 6. An example of MCP cube compression test (left) and MCP prism compression test (right).

Two different methods were used to evaluate the CBMs behaviour in tension: the flexu-
ral test and tensile splitting test. For determination of the flexural strength, the 3-point bend-
ing test was performed. The flexural strength of the MCP and MCM 40 × 40 × 160 mm3
specimen was determined by the standard EN 1015-11 [48], and in the case of the MOC
100 × 100 × 400 mm3 prisms, the procedure in standard EN 12390-5 [50] was followed.
The tensile splitting test was carried out on the prism halves that remained after the flexural
test, following the standard EN 12390-6 [51] (the modified procedure was used for the MCP
and MOM specimens).
Materials 2021, 14, 1569 9 of 24

3.3.4. Static Modulus of Elasticity, Poisson’s Ratio and σ-ε Behaviour in Compression
Static unloading modulus of elasticity (Es ) and static Poisson’s ratio from compression
(νs ) were determined by following a modified protocol [33] of standard EN 12390-13,
method B [52], on 40 × 40 × 80 mm3 prism for the MCP and MOM, and on 100/200 mm
cylinder for the MOC.
In this method, there are 3 loading cycles and the nominal stresses of each cycle, where
the higher nominal stress is σa , the lower nominal stress is σb and the preloading stress is
σp . The preloading stress was equal to the lower nominal stress σb in our study. With the
measured compressive strength fc on the parallel specimens, the preloading and higher
nominal stress were calculated using equations (Equations (4) and (5)).

σp = 0.1 × f c (4)

σa = 0.25 × f c (5)
The loading speed was 1.5 ± 0.125 MPa/s for the MCP and MOM prisms and
0.6 ± 0.2 MPa/s for the MOC composition. Static elastic modulus ES is calculated as
a stress difference divided by longitudinal strain (εL ) difference that corresponds to the
stress difference at the unloading of the third cycle (Equation (6)). Static shear modulus
GS is calculated as a stress difference divided by the absolute value of transverse strain
(εT ) difference that corresponds to the stress difference at the unloading of the third cycle
(Equation (7)). Poisson’s ratio νs is calculated as the absolute value of the transverse strain
difference divided by the longitudinal strain difference (Equation (8)).

∆σ σa − σp
Es = = (6)
∆ε L


ε L (σa ) − ε L σp

∆σ σa − σp
Gs = =  (7)
∆ε T


ε T (σa ) − ε T σp 

∆ε T


ε T (σa ) − ε T σp 
νs = = (8)
∆ε L


ε L (σa ) − ε L σp
After the third cycle of the test was performed, the specimen was loaded to its collapse
(Figure 7). In this way, a compressive stress-strain diagram (σ-ε behaviour) was obtained
for each specimen.

Figure 7. An example of a prism specimen of MCP/ mortar (MOM) (left) and cylinder specimen of
concrete (MOC) (right) after the modulus of elasticity, Poisson’s ratio and σ-ε test.
Materials 2021, 14, 1569 10 of 24

4. Results and Discussion

4.1. Fresh Properties of CBMs
After mixing each of the CBMs, the fresh properties of CBM mixtures were measured.
The results are given in Table 3 for MCP and MOM and in Table 4 for MOC.

Table 3. Fresh properties of MCP and MOM.

Temperature of Mixture Flow Value Density

Fresh Properties of CBM’s
(◦ C) (mm) (kg/m3 )
MCP 19.9 309 1923
MOM 20.1 236 2254

Table 4. Fresh properties of MOC.

Temperature of Mixture Air Content Flow Value Slump Value Density

Mixture:
(◦ C) (%) (mm) (mm) (kg/m3 )
30 h 19.6 2.65 505 250 2370
36 h 18.5 2.7 535 250 2400
48 h 20.2 2.65 565 250 2390
72 h 19.9 2.6 525 254 2360
7d 18.8 2.6 530 250 2380

As expected, the MCP and MOM mixture temperature was very close to 20 ◦ C. The
MCP’s high slump-flow value indicated the paste’s self-compacting ability and density
below 2000 kg/m3 was due to the exclusion of the aggregate particles. The flow value
of the MOM was highly reduced due to the addition of the sand, despite the increased
superplasticizer/cement ratio. However, it was still much higher than 200 mm, which was
the lower limit value for the soft mortar that is cast in the bulk density measuring vessel
without compaction [40]. There was no direct relationship between the MCP and MOM
flow value due to the modified testing procedure applied for the MCP.
MOC fresh properties were measured for five different batches, prepared for different
testing ages of the hardened concrete (Table 4). The fresh MOC temperature was in a
narrow interval of 19.5 ± 1 ◦ C, and the rest of the properties’ repeatability was high. The
flow value (slump-flow) was a better indicator of the MOC consistency than the slump
value. The slump value above 220 mm was not sensitive enough to evaluate a change of
consistency. The MOC concrete can be classified as highly flowable concrete and not far
from the self-compacting ability.

4.2. Time-Dependent Temperature and Electrical Conductivity Development in CBMs

The time-dependent temperatures of two MCP, two MOM and two MOC specimens
within the seven-day measuring period are shown in Figure 8.
There was practically no temperature difference between the curves of the two spec-
imens of individual CBM mixture. However, when comparing MCP, MOM, and MOC
specimens’ temperature curves, it was evident that the cement content of the CBMs pre-
dominantly influenced generated heat and with it the rate of temperature increase and
maximum value of the measured temperature. The custom-made extruded polystyrene
container that obstructed the heat loss through five of six surfaces during the hydration
process was predominantly responsible for the behaviour observed.
The development of physical and mechanical properties of CBMs was influenced by
both time and temperature [53]. Due to significantly different temperature histories of
the CBMs at an early age (Figure 8), the equivalent age method was used to estimate the
MCP, MOM, and MOC’s time-dependent conductivity. For this purpose, the temperature
Materials 2021, 14, 1569 11 of 24

influence on the effective concrete age te was considered, using the Freiesleben-Hansen and
Pedersen (Arrhenius) expression [54], with a constant activation energy of 33.500 J/mol/K
determined by Leusmann et al. [55] for the CBM compositions studied.

Figure 8. Time-dependent temperature for MCP, MOM, and MOC specimens.

MCP, MOM, and MOC specimens time-dependent conductivity (C−t curve) measured
for 7 days is shown in Figure 9. The conductivity is an indicator of the free water inside
the CBM pore structure. The free water content and pore system properties depend on
cement hydration level and initial water content in CBMs. Instantly after mixing, the space
between cement grains (pore system) occupied by water is interconnected; at that point,
the conductivity is a direct indicator of the water content in the cement paste. During
the hydration process, the hydration products may interrupt the connectivity of the pore
system. Consequently, the fast drop of conductivity occurs, which is reflected in the C−t
curves’ steep decrease (Figure 9). The absolute water content of the three CBMs varied;
the MCP mixture has the highest volume of water, followed by MOM and MOC mixtures.
That is why the initial conductivity (before the setting process starts) was the highest in the
MCP specimens and the lowest in the MOC specimens. The increase of the conductivity in
the early period of hydration, observed for the MCP and MOM specimens, can be related
to a dissolution of cement particles in the pore water and associated heat evolution in the
first hours [20,21].
During the structure formation process of the CBM, several stages (initial and final
setting time, percolation of solid phases, de-percolation of water-saturated pores and the
time of the most intensive solidification process) are usually defined based on typical
ultrasonic velocity time-dependent profiles [2]. Vogrič et al. showed [8] that a high degree
of correlation exists between the P-waves ultrasonic velocity-time (VP −t) and electrical
conductivity-time curves. By considering this correlation, the initial setting time (ti ), final
setting time (tf ) and end of the solidification process acceleration stage (inflexion point PT2)
were determined for MCP and MOM specimens (Table 5), using the electrical conductivity-
time curve (C−t) and the rate at which conductivity changes (dC–t curve). Figure 10
illustrates how these parameters were determined for the MCP2 sample. The C-t curves
were not smooth enough for MOC specimens to determine all the parameters, probably
due to much lower cement paste content and coarse aggregate grains. This is in line with
findings related to the VP −t curves where an increase in the aggregate content leads to less
visible substages of the rapid VP increase period [2]. Therefore, only the initial setting was
determined for the MOC specimens, as the time at the rapid drop of the dC-t curve. The
Materials 2021, 14, 1569 12 of 24

final setting time was calculated considering the same setting periods of the MOM and
MOC—which were equal to 90 min.

Figure 9. Time-dependent conductivity (C−te ) for MCP, MOM, and MOC specimens.

Table 5. Characteristics time periods of the CBM solidification process.

Time Periods of the Hydration Process MCP MOM MOC

Initial setting time (h) 13.2; 14.0 14.0 9.5
Final setting time (h) 14.8; 15.5 15.5 11.0
End of the solidification process acceleration stage—PT2 (h) 26; 26.5 26.5; 27 nd

Figure 10. C−te and dC/dt profiles of the MCP2, with the determination of initial and final setting
times and PT2 time.
Materials 2021, 14, 1569 13 of 24

Initial and final setting times (Table 5) are in reasonably good agreement with values
obtained by Staquet [56] for the same CBM compositions: 13.15 h and 14.82 h, respectively,
in the case of the MOM, and 10.15 h and 11.43 h, respectively, in the case of the MOC.
However, the setting times are much higher than in the case of ordinary compositions due
to the retarding effect of the used superplasticizer. This is also true when the inflexion
point PT2 (Figure 10) is considered. The inflexion point PT2 is a good approximation of
the peak value on the calorimetry curve following the induction period. This peak value
occurred at the age of 26 to 27 h for the MCP and MOM compositions and is often related
to complete coverage of the C3 S grains’ surface with the C-S-H “needles” and start of dense
inner products formation [57]. At this stage, CBM is not capable of withstanding loads due
to the specimen’s weight and handling operations. The PT2 time (26 to 27 h) also explains
why during the de-moulding at 24 h, specimens disintegrated.

4.3. Hardened Properties of CBMs

The observation of hardened properties of CBMs began when specimens were able to
withstand loads due to their weight and handling operations. For the studied compositions,
this was only at the age of 30 h. In this chapter, the MCP, MOM and MOC specimens’
mechanical properties are presented at the specimens’ age of 30, 36, 48, 76 h, and 7 days.
The equivalent age approach was not applied since the temperature of the specimens was
not measured.

4.3.1. Ultrasonic P and S Waves Transmission Velocity

The ultrasonic P- and S-wave transmission time was measured for the three CBM
compositions at each specimen’s age. The transmission path length for calculating the
ultrasonic transmission velocity is 160 mm for MCP and MOM specimens and 400 mm
for the MOC specimen. Figure 11 shows the development of the transmission velocity of
ultrasonic P- and S-waves with the specimens’ age.

Figure 11. Development of transmission velocity of ultrasonic longitudinal (VP) and shear (VS) waves.

Shear waves are assumed inexistent in the CBM suspension after mixing since no shear
forces are transmitted in fluids [2]. Thus, the S-waves can propagate in the CBM specimen
only when enough cement hydration products are present to form an interconnected solid
percolation path. This time is often defined as the initial setting time of specific CBM [2]. On
the other hand, the velocity of P-waves at the initial setting time of cement paste is about
1450 m/s [58–60], which is the velocity of the P-waves in water. During the setting and
Materials 2021, 14, 1569 14 of 24

hardening process of CBM, both velocities are continuously increasing and thus present
promising parameters to monitor the solidification process.
By comparing velocities of the P-wave (VP ) at the age of the specimens of 30 h
(Figure 11) to results obtained on the same compositions by [55], it can be concluded
that good reproducibility of the test results exists for the MCP and MOC compositions.
Although an approach with the equivalent age and significantly smaller length of the test
specimens were used in [55], measured average velocities were 2600 m/s and 4150 m/s for
the MCP and MOC specimens, respectively. Values 2500 ± 120 m/s and 3940 ± 50 m/s
were obtained for the MCP and MOC specimens, respectively, in our study. Based on the
same VP measured on the MCP at 30 h, results from [55] can be used to estimate the VP at
initial and final setting, and the PT2 time that presents roughly the start of the decelerated
solidification stage of the MCP as 800 m/s, 1100 m/s and 2250 m/s, respectively. The VP
values of initial and final setting agree with [61].
The P-wave velocity increase with the MCP specimens’ age is approximately constant
(81 to 85 m/s per hour) between the PT2 time and 36 h. After that, the rate of the velocity
increase started to decrease with time considerably. From these results, it can be concluded
that the cement paste’s intense solidification process existed for up to 36 h, which was also
confirmed by [55]. From 36 to 48 h, the increase in VP is highly reduced, and VS is lower
at 48 h than 36 h. This implies the possible presence of cracks inside the MCP specimens,
likely formed due to the cement paste’s autogenous shrinkage. The formation of cracks
can break interconnected solid percolation paths for the S-waves. The ratio between the P-
and S-wave velocities (VP /VS ) is between 1.83 and 1.82 for 30, 72 and 168 h. However, it
is reduced to 1.80 for 36 h and increased to 1.90 for 48 h. It seems that the change of the
otherwise roughly constant VP /VS ratio of the MCP can be used as the measure to detect
damages to the cement composite microstructure.
MOM specimens contain a larger number of solid fractions due to the incorporation of
sand. Thus, higher values of the VP and VS were measured for these specimens (Figure 11).
The VP /VS ratio is close to 1.71 for all but 48 h, where the ratio is increased to 1.73. This
increase may also be due to crack formation, although the extent of the cracks seems to be
much lower due to a smaller volume of cement paste and higher volume stability of the
MOM compared to the MCP.
The highest VP and VS values were measured for the MOC due to the lowest cement
paste content and the highest aggregate grains content, equal to 67%. The VP /VS ratio is
close to√1.70 for all but 7 d (168 h), where the ratio is increased to 1.738. This value is close
to the 3 which is the VP /VS ratio, often reported for stones [2].

4.3.2. Dynamic and Static Elastic Properties of CBM Specimens

The simultaneous determination of the P- and S-ultrasonic wave transmission veloc-
ity makes it possible to determine the dynamic elastic parameters (νd , Ed , Gd ) of CBMs
(Equations (1)–(3)). Those parameters are calculated for nondeformed specimens since
very little force is applied to the specimen during the measurement. On the other hand,
static elastic properties are determined on CBM specimens loaded to 25% to 40% of their
strength—up to the load at which Hook’s law exists between stress and deformation. A
compressive test is most often used to determine those parameters (Equations (6)–(8)).
The difference between static and dynamic Poisson’s ratio for studied CBMs is pre-
sented in Figure 12. For the MCP, νd is close to 0.285 for 30, 72, and 168 h. Lower (0.276) and
higher (0.307) values were measured at 36 and 48 h, respectively. Values of νd below 0.30
are expected for the hydrated cement paste (HCP) since Poisson’s ratio of cement clinker
minerals is 0.3 [62] and that of C-S-H outer and inner gel and of Ca(OH)2 is 0.25, 0.25,
and 0.30, respectively [63]. The effect of formed cracks on the VP and VS values directly
influenced calculated νd at these two ages. The static Poisson’s ratio νs is, as a rule, lower
than the νd and is around 0.25 at the age of the MCP 48 h or higher. On the other hand, at
30 and 36 h, the test results’ standard deviation was so high that the measured average
value could not be applied as a realistic parameter. The presence of autogenous shrinkage
Materials 2021, 14, 1569 15 of 24

cracks can be responsible for the observed behaviour. For MOM prisms, νd is mostly in the
range of 0.240 ± 0.002, except for the 0.247 ± 0.002 value at 48 h. Again, the presence of
cracks in the specimens could influence the observed exception from the rule. The static
Poisson’s ratios νs of the MOM gradually increase, from 0.186 at 30 h to 0.228 at 168 h. A
gradual increase of dynamic and static Poisson’s ratios with the specimen’s age was also
observed for the MOC composition, where νd increased from 0.232 at 30 h to 0.252 at 168 h,
and νs increased from 0.178 at 30 h to 0.196 at 168 h.

Figure 12. The comparison of dynamic and static Poisson’s ratio for CBMs.

The comparison between the dynamic and static E-moduli of studied CBMs is shown
in Figure 13. In general, the elastic modulus is a function of densities of CBMs’ main
components and the interface transition zone between the aggregate and cement matrix.
It is common knowledge that the ordinary aggregate with a density between 2500 and
2700 kg/m3 has the most crucial influence on CBMs’ E-moduli and thus the E-moduli
increase with the increase of volume fraction of aggregate grains; such aggregate was also
used in this study. The dynamic elastic modulus (Ed ), determined by the non-destructive
ultrasonic tests, is generally higher than the static elastic modulus (Es ). When using the
ultrasonic method, only negligible stress occurs in the specimen. Therefore, the specimen
is not exposed to deformation and creep as it is during the static E-modulus test. Even so,
creep deformations do not have a fundamental effect on the static elastic modulus, so the
two methods are comparable [64]. The difference in dynamic and static E-moduli is mainly
because CBMs’ behaviour is viscoelastic, which means that the behaviour of the material
varies according to the strain rate applied during the test [65].
As expected, the lowest E-moduli were measured for the MCP composition, where
there is no difference between Ed and Es values for 30 and 36 h. At the age of 48 h, there
is no increase in Ed , and Es is reduced compared to 36 h. Again, the possible presence of
cracks can be responsible for the observed behaviour. There is another gradual increase in E-
moduli at 72 and 168 h, and Ed values seem to be slightly higher than that of Es . Comparison
to the MCP’s E-moduli determined using the EMM-ARM test method that allows automatic
and continuous evaluation of the property from final setting time forward [29] shows good
agreement of the test results for all specimens’ ages. However, this is probably mainly
because the two moduli are approximately the same for the MCP composition.
A significant difference was obtained between Ed and Es moduli for the MOM com-
positions, with Ed values notably higher (Figure 13). The ratio Ed /Es is the highest at 30
and 36 h (1.32). With an age increase, it started to decrease, to 1.26 at 48 h and finally to
Materials 2021, 14, 1569 16 of 24

1.13 at 72 and 168 h. By comparing Ed values with test results in [56], where the same
MOM composition was tested, 30 h and 36 h values of 23.2 ± 0.6 GPa and 25.3 ± 0.6 GPa,
respectively, are lower than 27.5 GPa and 28.3 GPa, respectively, reported by Staquet [56].
However, already at 48 h, the two Ed are about the same (29.2 ± 0.2 GPa in our study and
30.5 GPa in [56]).

Figure 13. The comparison of dynamic and static modulus of elasticity (E-modulus) for CBMs.

The ratio Ed /Es for the MOC composition follows almost the same pattern as that
observed at the MOM composition. The highest ratio of 1.3 was obtained at 30 h, 36 h and
48 h; at 72 h, a reduction to value 1.23 was observed. Finally, a ratio of 1.13 was obtained
at 168 h. Due to the much higher volume and grain size of aggregate, the moduli of the
concrete composition are considerably higher than those of the MOM. By comparing Ed
values with test results in [56], where the same MOC composition was tested, 30 h and
36 values of 31.2 ± 0.7 GPa and 34.2 ± 0.2 GPa in our study are only slightly lower than
33 GPa and 35 GPa, respectively, obtained by Staquet [56]. Again, at just 48 h, the two Ed
are about the same (36.8 ± 0.5 GPa in our study and 36.8 GPa in [56]). This also shows
that the equivalent age approach would not influence the test results significantly, as this
approach was applied in [56].
When comparing the Es results to the velocities of the shear waves (VS ), the exponen-
tial relation of Es =a·EXP(b·VS2 ), where a and b are constants, results in the highest coefficient
of determination R2 equal to 0.83, 0.98 and 0.90 for the MCP, MOM and MOC, respectively.
Moreover, by considering all test results (for MCP, MOM and MOC compositions), the
correlation of Es = 6.05· EXP 0.255VS2 with R2 equal to 0.97 was obtained. Comparison of

the Ed and Es test results confirms the non-linear correlation between the two properties,
as reported in [2]. By considering all test results, the correlation of Es = 1.16· Ed0.9 with R2
equal to 0.96 was obtained.

4.3.3. Stress-Strain Diagrams of CBMs in Compression

After the 3rd cycle of the unloading elastic modulus test, all the specimens were
loaded to their total collapse. In this way, stress-strain diagrams (σ–ε behaviour) were
obtained. For each tested CBM specimen, the obtained σ–ε diagram is shown in Figure 14.
There are two exceptions where centrical loading was not possible—one MCP specimen
at the age of 36 h and one MOC specimen at 48 h. These results were omitted from the
analyses. The most dispersed σ–ε diagrams for particular age were observed for the MCP
composition, as there is no aggregate in the mixture and the presence of cracks is plausible.
Materials 2021, 14, 1569 17 of 24

These cracks can be present in the specimen before application of load or induced during
the loading due to reduced tensile strength, both due to the autogenous shrinkage. It is also
evident that at ages 48 h and higher, the MCP specimens possess higher deformability than
the MOM specimens, although ultimate stresses are about the same for the particular age
of specimens. A lower Es for the MCP specimens is responsible for the behaviour observed.
Furthermore, MCP specimens show much more brittle behaviour than the MOM and MOC
specimens, especially at ages 72 h and 168 h, where an almost linear behaviour of the MCP
is observed. This is in line with the response shown in [66] for the HCP. As expected, the
nonlinearity of σ–ε diagrams is increased when aggregate is introduced to the mixture.
However, deformability is higher for the MOM specimens than the MOC specimens due to
the lower modulus of elasticity.

Figure 14. Stress-strain diagrams of CBM specimens after unloading elastic modulus test.
Materials 2021, 14, 1569 18 of 24

The non-linear σ–ε behaviour is due to the gradual crack formation in the interface
transition zone (ITZ) between the hardened HCP and aggregate grains. Usually, it is related
to the lower strength of the ITZ due to the locally increased water-to-cement ratio as a
consequence of vibration [66]. CBMs in fresh state possessed highly flowable consistency
and no or minimum vibrations were needed to cast the specimens. Moreover, the MOC
composition showed a brittle response at just 168 h, indicating that ITZ properties were
similar to the bulk HCP ones. Due to the possibility of cracks formation, as a consequence
of the autogenous shrinkage of the HCP, such cracks in the ITZ would have a similar
influence on the σ–ε behaviour as the increased porosity ITZ. The cement binder’s self-
healing capacity can eventually repair these cracks in the non-loaded specimen, resulting
in a more brittle response of the MOC at 168 h.

4.3.4. Strenght Properties of CBM Specimens

The influence of the specimen’s shape on compressive strength development is shown
in Figure 15. As expected, higher strengths were measured on the cube specimens compared
to prismatic or cylindrical 2/1 specimens. The shape conversion factor between the prism
or cylinder and cube is not a constant value for a particular CBM. It seems to be dependent
on the age of the specimen.

Figure 15. The influence of specimen’s shape on compressive strength for MCP, MOM, and MOC.

For the MCP specimens, the shape conversion factor is between 0.78 (at 36 h) and 0.97
(at 30 h) and is close to 0.9 at 48 h, 72 h and 168 h. This factor is much lower for the MOM
composition, ranging between 0.65 (36 h) and 0.78 (72 h). The presence of sand influences
the shape conversion factor. The lowest value of the factor was observed at 36 h for both
CBM compositions. The presence of cracks that influence the strength of the prism more
than the cube strength is a plausible cause for this observation. For the MOC, the shape
factor is between 0.70 (48 h) and 0.88 (168 h), although the other three values are close
to 0.8, which is the conversion factor usually used to calculate the cylinder (150/300 or
200/100 mm) compressive strength, from the 150 mm cube strength.
Direct comparison of the compressive strengths is possible only for the MCP and
MOM compositions due to the same dimensions of specimens used. At 30 h and 36 h,
the compressive strengths of the MCP and MOM were approximately the same when the
2/1 prism was used as a specimen, and the compressive strength is higher for the MOM
composition when the cubic specimen was used. It seems that 2/1 prismatic specimens are
a better choice when the compressive strength of the paste and mortar scale of the concrete
Materials 2021, 14, 1569 19 of 24

is evaluated since they reflect the presence of cracks in the measured strength. Furthermore,
one can conclude that MOM is not adversely affected by the aggregate incorporation, as
reported in [66] since the compressive strength of the MOM is not lower compared to that
of the MCP.
Comparing the MOC compressive strength to that obtained for the MOM composition
is possible only if the shape conversion factor 1.12 is used to calculate the equivalent
compressive strength of the 40 mm cube from the 150 mm cube. The comparison reveals
that the MOC’s compressive strength is higher only for the 30 h and 36 h. At later ages,
however, the compressive strengths of the two compositions are about the same. The
standard cube (150 mm) compressive strength of the MOC reported in [55] is 30 MPa and
51 MPa for 48 h and 168 h, respectively. These values are slightly lower than 35 ± 2 MPa
and 54 ± 2 MPa, respectively, obtained in our study.
When comparing the compressive strength results to the velocities of the shear waves
(VS ), the exponential relation of fC = a × EXP(b × VS ), where a and b are constants, results
in the highest coefficient of determination R2 equal to 0.95, 0.95 and 0.82 for the MCP, MOM
and MOC, respectively.
Flexural and splitting tensile strengths of the tested MCP, MOM and MOC mixtures
are shown in Figure 16. Direct comparison is possible between the MCP and MOM
compositions due to the identical prismatic specimens used. Tensile strength tests are much
more sensitive to the presence of cracks compared to the compression test. For the MCP
composition, tensile strength does not follow the compressive strength increase with the
increase of the specimen’s age. Average values of flexural strength are between 3.14 MPa
(168 h) and 3.96 MPa (36 h), and those of the splitting strength are between 2.40 MPa (30 h)
and 2.94 MPa (36 h). Additionally, a high variation of the test results at 36 h and 48 h
was observed. Observed behaviour is typical for specimens with induced cracks or other
defects. Much higher flexural and splitting tensile strengths were obtained for the MOM
specimens due to the incorporation of the fine aggregate. Average splitting strength values
are gradually increasing with the specimens’ age, from 3.10 MPa (30 h) to 5.98 MPa (168 h).
The situation is different for flexural strength, where the highest average value (7.81 MPa)
and, at the same time, high standard deviation (1.55 MPa) were obtained at 48 h. Moreover,
flexural strength at 168 h was lower compared to that at 72 h. From these results, one
can conclude that the presence of cracks in MOM specimens is reflected in the change of
flexural strength with the age of the specimen. For the MOC composition, flexural strength
gradually increases with the specimens’ age, from 4.14 MPa at 30 h to 6.70 MPa at 168 h.
The situation is different for the splitting strength, where the decrease of strength was
observed from 30 h to 36 h (from average value 1.99 MPa to 1.52 MPa) and approximately
the same average strength of 2.65 ± 0.07 MPa was maintained from 48 h to 168 h.
Observed behaviour is different from that reported in [55] for the same MOC com-
position, where splitting tensile strength was determined on 80/300 mm cylinders and a
gradual increase of the specimen’s strength, from 1.1 MPa at 24 h to 2.2 MPa at 48 h and
3.5 MPa at 168 h, was reported.
As a rule, the development of the flexural and splitting tensile strength with the CBM
age does not follow the compressive test pattern of a particular CBM. There is also a very
poor correlation between the VS and flexural or splitting tensile strength of a particular
CBM. There are only two exceptions—a good linear correlation was obtained at the MOM
between VS and splitting tensile strength (R2 0.92) and at the MOC between VS and flexural
strength (R2 0.95). It can be seen that no rule can be established between the MCP, MOM,
and MOC properties. Several possible influencing parameters are responsible for the
observed behaviour: random presence of cracks, non-adequate shape and dimensions of
specimens to determine early age properties, and the possibility that elastic theory at the
early age of CBMs is not valid for the destructive tests.
Materials 2021, 14, 1569 20 of 24

Figure 16. Flexural (flex) and splitting tensile (tens) strength of MCP, MOM, and MOC.

5. Conclusions
In this study, non-destructive and standard destructive tests were performed to eval-
uate cement-based material properties at three scales—the concrete, mortar, and paste
scale. The research was carried out using materials and compositions proposed within the
RRT+ programme of the COST Action TU1404. The studied compositions have increased
autogenous shrinkage and a highly delayed setting, resulting in an extended early age
period. The electrical conductivity measurements were used to follow a particular cement-
based material solidification process, from the state of solid suspension up to the age of
7 days. On hardened specimens aged 30, 36, 48, 72 h, and 7 days, transmission times of
ultrasonic P- and S-waves were measured simultaneously, and standard destructive tests
were performed to determine both dynamic and static mechanical properties. Based on the
experimental results obtained, the following main conclusions were drawn:
1. The electrical conductivity method used is capable of determining the initial and final
setting time and the end of the solidification process acceleration stage (PT2) for the
MCP and MOM compositions. For the MOC composition, only the initial setting time
was determined. An increase in the aggregate content leads to less visible substages
of the interval, where conductivity rapidly decreases with time.
2. Simultaneous P- and S-wave transmission velocities measurements revealed that the
ratio VP /VS is highly dependent on the HCP and aggregate contents. The highest
ratio of about 1.82 was obtained for the MCP. Lower ratios of 1.71 and 1.70 were
obtained for the MOM and MOC, respectively. The only exception is MOC at 7 days,
where a value of 1.738 was noted. The deviation from the otherwise roughly constant
ratio VP /VS for each CBM may indicate cracks in the material at a particular age.
3. Comparison of dynamic and static elastic moduli, Ed and Es , revealed almost no
difference between the two moduli for the MCP. For the MOM and MOC compositions,
the ratio Ed /Es was changed with the CBM’s age, from about 1.3 at 30 h to 1.13 at 168 h.
Considering all test results (for MCP, MOM and MOC compositions), the non-linear
correlation between the Ed and Es was found to be in the form of Es = 1.16 × Ed0.9
with R2 equal to 0.96. The Es results
additionally correlate very well with the square
of VS , as Es = 6.05 × EXP 0.255VS2 with R2 equal to 0.97.
4. Comparison of dynamic and static Poisson’s ratio, νd and νs , revealed that the value
is approximately 0.285 for νd and about 0.25 for νs when MCP is considered. The νd
value between 0.24 and 0.25 was obtained for the MOM and MOC. Static Poisson’s
Materials 2021, 14, 1569 21 of 24

ratio gradually increased with the specimen’s age. Values from 0.19 to 0.23 were
obtained for the MOM, and from 0.18 to 0.20 for the MOC.
5. Results of compressive strength tests showed 32% higher MOM cube strengths com-
pared to those of the MCP cubes. About the same cube compressive strength was
measured for the MOM and MOC compositions, from 48 h up to 168 h. The cube com-
pressive strength is highly correlated to the velocity of the S-waves (VS ). However, a
separate trendline exists for each CBM tested. This confirms that different parameters
influence the compressive strength and static modulus of elasticity where the same
Es −VS2 tradeline exist for the three CBMs.
6. The comprehensive study using a combination of various non-destructive and de-
structive tests to evaluate the CBM at the three scales shows that evaluating the early
age properties using commonly accepted destructive standard tests and specimens’
shape needs additional validation and possible modifications. Numerical simulations
using reported test results can help solve existing issues.
7. Detection of cracks formed inside the CBM at an early age—such as autogenous
shrinkage cracks—and possible self-healing of those cracks with the CBM’s age is of
utmost importance. Loading the reinforced concrete elements when such cracks are
present in the CBM’s microstructure may lead to the highly reduced service life or
even the collapse of reinforced concrete infrastructure. A change in the otherwise
roughly constant VP /VS ratio can indicate cracks in the CBM for the paste and
mortar scale.

Author Contributions: Conceptualization, M.K., V.B. and V.B.-B.; methodology, M.K., V.B. and
V.B.-B.; validation, V.B.-B.; formal analysis, M.K. and V.B.-B.; investigation, M.K.; resources, V.B.-B.;
writing—original draft preparation, M.K.; writing—review and editing, V.B. and V.B.-B.; visualization,
M.K. and V.B.-B.; supervision, V.B. and V.B.-B.; project administration, V.B.-B.; funding acquisition,
V.B.-B. All authors have read and agreed to the published version of the manuscript.
Funding: The Slovenian Research Agency financially supported research performed through Pro-
gramme Group P2-0185, Research Project J2-9196 and Martin Klun’s PhD project. Materials used were
delivered through the COST Action TU1404 RRT+ programme, financially supported by COST, EU,
EDF, France, CEVA Logistics, Austria and Germany, OeBB Infra, Austria, Staten Vegvesen, Norway,
Schleibinger Gerate, Germany and The Slovenian Research Agency. The authors would also like to
acknowledge the networking support provided by COST Action TU1404.
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Data Availability Statement: Data sharing is not applicable to this article.
Conflicts of Interest: The authors declare no conflict of interest.

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