Early Age Properties of Self-Compacting Concrete - Effects of Fine Aggregate and Limestone Filler - Thesis

Early age properties of
self-compacting concrete
– Effects of fine aggregate and limestone filler
OSKAR ESPING
Department of Civil and Environmental Engineering

Building Technology
CHALMERS UNIVERSITY OF TECHNOLOGY
Göteborg, Sweden 2007
THESIS FOR THE DEGREE OF DOCTOR OF PHILOSOPHY
Early age properties of self-compacting

concrete
- Effects of fine aggregate and limestone filler
OSKAR ESPING

Building Technology
CHALMERS UNIVERSITY OF TECHNOLOGY
Early age properties of self-compacting concrete
OSKAR ESPING
ISBN 978-91-7291-890-0
© Oskar Esping, 2007
Doktorsavhandlingar vid Chalmers tekniska högskola

Ny serie nr 2571
ISSN 0346-718X

Building Technology
Chalmers University of Technology
SE-412 96 Göteborg
Sweden
Telephone: +46 (0)31-772 1000
http://www.chalmers.se
Chalmers Reproservice
II CHALMERS, Civil and Environmental Engineering

Early age properties of self-compacting concrete
Oskar ESPING
Building Technology
Chalmers University of Technology
ABSTRACT
Self-compacting concrete (SCC) is a sensitive mix, strongly dependent on the composition
and the characteristics of its constituents. It has to possess the incompatible properties of
high flowability together with high segregation resistance, a balance made possible by the
dispersing effect of water-reducing admixture combined with cohesiveness produced by a
high concentration of fine particles. These fines and their effects on the early age
properties of the SCC have been in focus in this present dissertation.
The effect of the specific surface area of gravel and limestone filler on the rheology of
SCC was evaluated. Performed experiments clearly demonstrated that traditional methods
for geometric characterization of the fines (size distribution, water absorption, fineness
modulus, etc.) are not sufficient to ensure consistent quality of SCC. By measuring the
specific surface area with a simplified gas adsorption method, BET(H2O), it was found that
the specific surface area of a normal gravel, accepted by traditional methods for production
of SCC, can vary up to 7000 m2/kg. A model is proposed, based on an assumption that 30
full molecular layers of water covering the particle surface are required to provide
lubrication sufficient to create flowability, where a change in specific area is translated to a
change in water demand for the concrete mix. It is suggested that an increase in
BET(H2O)-area of 1000 m2/kg corresponds to an increase in water demand by
approximately 0.85% by mass of the filler or gravel content for constant flowability.
Furthermore, the influence of mix design and fines BET(H2O)-area on the SCC’s early-age
deformation was demonstrated. The autogenous (sealed) deformation was measured with a
specially developed concrete dilatometer, together with capillary pore pressure and
temperature. It is suggested that that autogenous shrinkage and rate of evaporation are the
main factors promoting the risk of plastic shrinkage cracking. An increased particle surface
decreased the rate and magnitude of evaporation, and consequently reduced the plastic
cracking tendency, despite an increase in autogenous shrinkage.
Key words: self-compacting concrete, rheology, autogenous deformation, plastic

shrinkage, pore pressure, limestone filler, specific surface area, BET
CHALMERS, Civil and Environmental Engineering III

APPENDED PAPERS
The work presented in this doctoral thesis is based on the following papers, referred to in
the text by their Roman numbers:
I. Slump flow values vs. Bingham parameters for high flowable mortars and
concretes
Esping O., Accepted for publication in 5th International RILEM Symposium on
Self-Compacting Concrete, 3-5 September 2007, Ghent, Belgium, 2007.
II. Methods for characterisation of fillers and fines for self-compacting concrete
Esping O., 3rd International RILEM Symposium on Self-Compacting Concrete,
PRO 33, 17–20 August, pp 208-219, Reykjavik, Iceland, 2003.
III. SCC flowability: Effect of changes in particle surface area, and how to
compensate for this
Esping O., Accepted for publication in 5th International RILEM Symposium on
Self-Compacting Concrete, 3-5 September, Ghent, Belgium, 2007.
IV. Investigation of autogenous deformation in self-compacting concrete

Esping O., International RILEM conference on Volume Changes of Hardening
Concrete, 20-23 August, pp 273-282, Lyngby, Denmark, 2006.
V. Investigation of early age deformation in self-compacting concrete

Esping O., Löfgren I., 2nd International Symposium on Advances in Concrete
Ccience, 11-15 September, Quebec, Canada, 2006.
VI. Effect of limestone filler BET(H2O)-area on the fresh and hardened

properties of self-compacting concrete
Esping O., Submitted for publication in Cement and Concrete Research, 2007
IV CHALMERS, Civil and Environmental Engineering

CONTENTS
ABSTRACT III
APPENDED PAPERS IV
CONTENTS V
NOTATIONS VIII
1 INTRODUCTION 1
1.1 Background 1
1.2 Objective and limitations 2
1.3 Disposition of the thesis 3
1.4 Original features 3
2 RHEOLOGY 5
2.1 Introduction 5
2.2 Particle suspensions 7
2.3 Measuring techniques 22
2.4 Concluding remarks 27
3 EARLY-AGE DEFORMATION 29
3.1 Introduction 29
3.2 Plastic shrinkage cracking 31
3.3 Mechanisms of early-age deformation 32
3.4 Measuring techniques and methods 42
4 EXPERIMENTAL WORK 49
4.1 Introduction 49
4.2 Materials and mix design 50
4.3 Particle quantifications 53
4.4 Mortar and concrete quantifications 62
CHALMERS, Civil and Environmental Engineering V

5 FINAL DISCUSSION AND CONCLUSIONS 73
5.1 Discussion 73
5.2 General conclusions 75
5.3 Suggestions for future research 76
6 REFERENCES 79
APPENDIX A: BET(H2O) 91
APPENDIX B: CONCRETE DIGITAL DILATOMETER 99
APPENDIX C: CONCRETE CRACKING RING TEST 105
APPENDIX D: GLOSSARY 111
PAPER I: SLUMP FLOW VALUES VS. BINGHAM PARAMETERS

FOR HIGH FLOWABLE MORTARS AND CONCRETES
PAPER II: METHODS FOR CHARACTERISATION OF FILLERS AND

FINES FOR SCC
PAPER III: SCC FLOWABILITY: EFFECT OF CHANGES IN PARTICLE

SURFACE AREA, AND HOW TO COMPENSATE FOR THIS
PAPER IV: INVESTIGATION OF AUTOGENOUS DEFORMATION IN

SCC
PAPER V: INVESTIGATION OF EARLY AGE DEFORMATION IN SCC
PAPER VI: EFFECT OF LIMESTONE FILLER BET(H2O)-AREA ON THE

FRESH AND HARDENED PROPERTIES OF SCC
VI CHALMERS, Civil and Environmental Engineering

ACKNOWLEDGEMENT
The work presented in this doctoral thesis is one of the two outcomes of the project
“Industrial building with in-situ cast concrete – New concepts”, which was made possible
by a donation from Thomas Concrete Group / AB Färdig Betong to Chalmers University of
Technology. The work has been conducted at the Department of Civil and Environmental
Engineering (Chalmers University of Technology) and at the research centre of Thomas
Concrete Group in Göteborg, during the period 2001-2007. During the first years this
thesis was carried out under the supervision of Professor Lars-Olof Nilsson now at Lund
University of Technology, and during the remaining years under Professor Tang Luping
at Chalmers University of Technology. Professor Per-Erik Petersson at the Swedish
National Testing and Research Institute has acted as assisting supervisor. I am most
grateful for their support and assistance.
Grateful thanks are also addressed to:
☺ Annika Wirje, Färdig Betong AB
☺ Jan-Erik Lindqvist, Swedish National Testing and Research Institute
☺ Martin Hansson, Sika
☺ Mats Karlsson, Thomas Concrete Group AB
☺ Mette Geiker, Technical University of Denmark
☺ Olafur Wallevik, The Icelandic Building Research Institute
☺ Peter Billberg, Swedish Cement and Concrete Research Institute
☺ Sten Rodenstam, Nordkalk AB
Special thanks are due to Thomas Concrete Group and AB Färdig Betong for their
generous donation, support and confidence in me.
I would like to extend my special thanks to Ingemar Löfgren and Professor Tomas Kutti
at Thomas Concrete Group AB for their involvement in this work, and for their
indispensable help, guidance, encouragement and always valuable advice.
Finally, I would like to thank my future wife, Lotta, and children Albin and Elin, for
supporting and having patience with me during my doctoral studies.
It is my hope that this paper will be reviewed critically. Any viewpoints, comments and
suggestions about the text should be directed to me.
By the nature of an experimental investigation, each question is often answered with many
new questions. And with knowledge arises a question whether the experimental course of
action could be made in a more proper way. It ought to be noted that the purpose of a PhD
study is educational, and that the work presented in this doctoral thesis is mainly intended
as a personal learning process, not to produce unique or useful results. Yet it has to be
performed with a scientific approach and to fulfil certain requirements of quality, which I
hope to have achieved for the benefit of future research.
Göteborg, February 2007
CHALMERS, Civil and Environmental Engineering VII

NOTATIONS
Symbol Description Unit

A area [m2] [mm2]
A Arrhenius constant of the liquid [Pa·s]
Am monolayer adsorbate molecule area [m2]
C BET-constant related to the heat of adsorption [-]
d nominal size [mm]
d max maximum grain size [mm]
di mean particle size from two contiguous sieves [m]
D diameter [m] [mm]
Dcircle circle diameter with the same area as measured area [m]
De Deborah number [-]
Dmax length of the major axis [m]
Dmin length of the minor axis [m]
E evaporation [kg/m2]
E0 fluid activation energy [J/mol]
Ep deformation coefficient [-]
F cumulative retained material on specified sieve size [weight-%]
fc compressive strength [MPa]
f c0 compressive strength “without” pores [MPa]
Fm Feret diameter [m]
FM fineness modulus [-]
k constant for the effect of porosity on comp.strength [-]
k constant for the effect of particles >0.5 mm [-]
l length [mm]
l0 specimen initial length [mm]
M torque [N·m]
M molecular weight of adsorbate (~0.018 kg/mol for water) [kg/mol]
m mass weight [kg] [g]
mc mass of container [kg] [g]
mdry mass of oven dry specimen [kg] [g]
na number of objects per unit area [pcs/m3]
nH 2O number of layer water molecules adsorbed [pcs]
N Avogadro´s number (6.022·1023 molecules per mol) [mol-1]
pw partial water vapour pressure [Pa]
ps partial water vapour pressure at saturation [Pa]
p / po relative pressure [-]
P perimeter [m]
Pw pore water pressure [Pa]
P pressure [Pa]
VIII CHALMERS, Civil and Environmental Engineering

P porosity [-]
po partial pressure at saturation [Pa]
Q volumetric flow rate [m3/s]
r correlation coefficient [-]
r meniscus radius [m]
r interparticle distance [Å]
R radius [m]
R universal gas constant (R=8.314) [J/(mol·K)]
Ri radius of inner cylinder [mm]
Ro radius of outer cylinder [mm]
Rp relative flow area [-]
RH relative humidity [%][-]
S specific surface area [m2/kg], [m2/m3]
SF slump flow spread diameter [mm]
S BETH 2O specific surface area by BET(H2O) [m2/kg]
S' BETH 2 O approximated SBETH2O-area for the whole mass fraction [m2/kg]
SN2 specific surface area by BET(N2) [m2/kg]
S blaine specific surface area by blaine [m2/kg]
S SEM specific surface area by image analyze from SEM [m2/kg]
S size specific surface area by size distribution [m2/kg]
SP superplasticizer content [kg/m3]
t time [sec]
t time from water addition to mix [hours]
T temperature [°C], [K]
TX thixotropy [Pa/s]
T 50 time to 500 mm spread [sec]
u moisture content [kgw/kgmtrl]
V volume [m3]
w/ c water cement ratio [weight%]
w average crack width [mm2]
We evaporable water [kg/m3]
x fitting parameter (2.5 for spheres) [-]
xm monolayer capacity [-]
x05 mass fraction passing 0.5 mm sieve [-]
X adsorption isotherm [kg/kg]
y BET adsorption isotherm [-]
α angle [rad] or [º]

βp retained water ratio [-]
∆l specimen change in length [µm]
∆m sample weight loss due to drying [kg]
δ phase lag (loss angle) [rad]
ε strain [10-6m/m]
γw surface tension of air-water interface (~0.074 n/m) [N/m]
CHALMERS, Civil and Environmental Engineering IX

γ& shear rate [1/s]
η viscosity [Pa·s]
η app apparent viscosity [Pa·sA]
ηc viscosity of the fluid phase [Pa·s]
η pl plastic viscosity [Pa·s]
η∞ constant viscosity near infinite shear rate [function dependent]
η0 constant viscosity near zero shear rate [function dependent]
ρ density [kg/m3]
σ shear stress [Pa]
σ app apparent yield stress [Pa]
σs static yield stress [Pa]
σy yield stress [Pa]
σ0 Bingham yield stress [Pa]
σ0 stress amplitude [Pa]
σ 0* apparent Bingham yield stress [Pa]
γ0 strain amplitude [-]
ϕ volume fraction of solid particles [-]
ϕm maximum possible volume fraction of solid particles [-]
ϑ air velocity [m/s]
ω angular frequency [rad/s]
Ω angular velocity [rad/s]
Abbreviation Description
A aggregate
ACC accelerator
C cement
BET Brunauer, Emmet, and Teller
CDD concrete digital dilatometer
CH calcium hydroxide
C-S-H calcium silicate hydrate
COV coefficient of variance
F filler
H2O (see W)
LOI loss of ignition
N2 nitrogen
P powder
RE retarder
SCC self-compacting concrete
SEM scanning electronic microscopy
SF silica fume
Size size distribution
SP superplasticizer
SRA shrinkage reducing admixture
W water
X CHALMERS, Civil and Environmental Engineering

Chapter 1 – Introduction
1 INTRODUCTION
1.1 Background
Cement-based materials are the most abundant of all man-made materials and are among
the most important construction materials, and it is most likely that they will continue to
have the same importance in the future. However, these construction and engineering
materials must meet new and higher demands. When facing issues of productivity,
economy, quality and environment, they have to compete with other construction materials
such as plastic, steel and wood. One direction in this evolution is towards self-compacting
concrete (SCC), a modified product that, without additional compaction energy, flows and
consolidates under the influence of its own weight.
The use of SCC offers a more industrialised production. Not only will it reduce the
unhealthy tasks for workers, it can also reduces the technical costs of in situ cast concrete
constructions, due to improved casting cycle, quality, durability, surface finish and
reliability of concrete structures and eliminating some of the potential for human error.
However, SCC is a sensitive mix, strongly dependent on the composition and the
characteristics of its constituents. It has to possess the incompatible properties of high
flowability together with high segregation resistance. This balance is made possible by the
dispersing effect of high-range water-reducing admixture (superplasticizer) combined with
cohesiveness produced by a high concentration of fine particles in additional filler material
[1]. The main mechanisms controlling this fine balance are related to surface physics and
chemistry; hence, SCC is strongly dependent on the activity of the admixtures, as well as
on the large surface area generated by the high content of fines [2]. Fresh SCC, like all
cementitious materials, is a concentrated particle suspension with a wide range of particle
sizes (from 10-7 to 30 mm for concrete). The particles are affected by a complex balance of
interparticle forces (i.e. interlocking, frictional, flocculation, colloidal, van der Waals, and
electrostatic forces), generating a time dependence and viscoplastic non-Newtonian
behaviour. In addition, the concretes have irreversible time-dependent properties as a result
of the chemical reactions [3].
Since the ratio of surface area to volume increases exponentially with particle irregularity
and decreased size, this area has a predominant effect on fresh and hardened concrete [4]-
[7]. Particles with apparently similar grading can provide significantly different effects on
concrete properties. These differences can be related to the fineness, shape, surface texture,
porosity, etc. If the particles provide a large specific area, a large quantity of water will be
adsorbed on the particles’ surfaces and less water will be available to lubricate and disperse
the particles, which is needed to provide flowability [8]. This adsorption will also influence
the development of negative capillary pore pressure, causing the paste to contract [9].
These contracting capillary forces are inversely proportional to the meniscus radius, and
hence the capillary tension stresses increase with decreasing pore sizes and interparticle
spaces. As a consequence of the large surface area generated by the high concentration of
powder material, and the retarding effect of superplasticizer, the SCC may develop a large
autogenous shrinkage and thus a high plastic shrinkage cracking tendency [10].
CHALMERS, Civil and Environmental Engineering 1

As aggregates represent 60-80% of the total volume of concrete, it is obvious that their
influence on the fresh and hardened concrete is substantial. Properties of fine particles (<63
µm) and their influence are often neglected, because traditional standard methods for
characterizing aggregates are deficient. The content of fine particles, by volume or weight,
is often small but the number of particles and their total surface area are large. A content of
3 vol-% of particles finer than 63 µm (EN 933-1, or 75 µm according to ASTM C33) is
considered harmful, but these particles and their surface properties may have a
considerable influence on the quality of the concrete, in either fresh or hardened state [8].
Powder material (filler, cement, etc.) is traditionally characterized by its size distribution
and specific surface area by Blaine. Due to the methodology, where the surface area is
determined by air permeability, based on packed spherical particles, information about the
shape, texture and surface porosity is neglected [5][11]. An irregular and porous particle
can provide a considerably larger surface area, accessible to water, than a spherical one
(see Figure 1). Under real conditions, a particle external surface can be as much as 1000
times greater that that of a sphere with equal volume [12]. Other, possibly more correct,
methods for geometric characterization, such as the BET with nitrogen gas or image
analysis, are more seldom used due to their complexity and high cost.
Hence, to be able to offer a high-quality product, it is imperative to have understanding and
knowledge of how the constituents affect the concrete’s fresh and hardened properties, and
how to characterize the concrete and its constituents’ properties.
Specific surface area - Particel geometry
70000
60000
50000 sphere
Area, S [m 2/m 3 ]
Irregular (5x)
40000
Irregular (10x)
30000
20000
10000
0
0.001 0.01 0.1 1
Size, D [mm] (log)
Figure 1. The enlarging effect of size (logarithmic) and shape on specific surface area,
illustrated with a spherical particle and an irregular one (with same section area but 5 and
10 times larger perimeter).
1.2 Objective and limitations

The main objective of this study was to gain more understanding and knowledge regarding
basic mechanisms that govern the rheological and time-dependent characteristics of
cementitious materials. A further aim has been to investigate the possibility to find a tool
for quality control of the constituents in order to detect, and to compensate for, variations
in the materials that adversely affect the flow behaviour and early-age deformation of self-
compacting concrete. Combinations of cement, fillers and aggregates normally used in
Sweden, together with a superplasticizer, were used. The effect of limestone fillers and the
fine part of aggregates has been in focus. In this work, the properties studied were mainly
particle characteristics, the rheology of suspensions, and autogenous deformation. Thus,
2 CHALMERS, Civil and Environmental Engineering

admixtures (especially the superplasticizer) predominate for the properties of fresh SCC,
and their effects have not been examined in this work. Nether have the thermal effects on
early-age deformation been considered. Methods for evaluation of specific surface area,
and correlation of measurement results from these methods with flow behaviour of mortars
and concretes, comprised a main topic. The concrete is structurally divided into two stages:
early age and long term, where early age is limited to 24 hours from mixing.
Rheologically, the concrete is also divided into two stages: fresh and hardened, where the
concrete (or mortar) is considered to be fresh as long as the matrix of suspended particles
is, or can be turned into, a liquid.
1.3 Disposition of the thesis

This thesis consists of an introductory text and six papers (Papers I to VI). The
introductory text, divided into three main parts (Chapters 2 to 4), gives a more
comprehensive description of the subjects treated and measuring methods used in the
appended papers.
First, an introduction to the rheology of particle suspensions and the factors affecting it is
presented in Chapter 2. Rheological characteristics, models, and methodology for
measuring the rheology are defined here, with cementitious materials in focus.
In Chapter 3 an introduction to early-age volume change of cementitious materials is
presented. Basic mechanisms and some general methods and principals for evaluating the
unrestrained early age shrinkage are described.
The experimental methods and materials used in the appended papers are presented in
Chapter 4. A more detailed description of the experimental setups is given here,
complemented with some analysis of the methods. Further description of the methods,
unique for this work, can be found in Appendices A, B and C.
In Chapter 5, discussions, conclusions and suggestions for future research are presented.
1.4 Original features

The main original features of this doctoral thesis may be summarized as follows:
o The particles’ specific surface area by BET has been shown to provide a good
correlation with mortar and concrete flowability (slump flow, yield stress and
viscosity), whereas other traditional methods characterizing the particle size,
geometry and surface area did not.
o The simplified BET method, using water vapour as adsorbate, was proven high
potential means of geometrical characterization for fillers and fine aggregates.
o It was shown that a change in fillers’ or fine aggregates’ BET(H2O)-area can be
used to calculate the change in mixing water for constant flowability of SCC.
o A potential method for determining the concrete’s linear autogenous deformation,
with the ability to start measuring in the liquid state before set, has been presented.
o The effect of mix design and BET(H2O)-area on the concrete’s capillary pore
pressure, autogenous deformation, and plastic shrinkage cracking tendency was
demonstrated in experiments.


Chapter 2 – Rheology
2 RHEOLOGY
2.1 Introduction
Rheology is defined as the science of deformation and flow of matter, and describes the
interrelation between force, deformation, and time [13]-[15]. It is normally applied to more
or less fluid materials, or materials that exhibit a time-dependent response to stress. An
important issue of rheology is the definition and classification of materials. One way to
characterize a material is by its relaxation time, i.e. the time required to reduce a stress in
the material by flow (see Table 1). Glass, for instance, is usually defined as a solid
material, but over a longer times perspective it flows like a liquid, although extremely
slowly.
Table 1. Classification of materials state in terms of their relaxation time (at 20ºC).
Gases Liquids Solids
Relaxation time [seconds] <10-6 10-6 – 100 >100
Another way of defining materials rheologically is by their flow characteristics, with a
classification into viscous, elastic and viscoelastic. Gases and many liquids are defined as
viscous. An ideal fluid is unable to store any deformation energy; when subject to stress, it
flows and the deformation energy is dissipated as heat (resulting in a rise of temperature).
Solids, on the other hand, can be described as elastic materials. Ideal elastic material stores
all imposed deformation energy, and will consequently recover totally upon a stress
release. But a large number of materials are viscoelastic (both viscous and elastic), i.e. they
store some of the deformation energy in their structure while some is lost by flow. The
simplest model describing an ideal fluid’s flow characteristics, and the basis for classical
fluid mechanics, is Newtonian – with a linear relationship between shear stress (σ) and
shear rate ( γ& ), and with zero stress at zero rate. This behaviour is analogous to Hookean
behaviour for a solid (see Figure 2). However, many important fluids, such as polymers,
blood, foods, cosmetics, and concretes, show non-Newtonian plastic behaviour, in which
flow only initiates above some level of stress (i.e. yield stress), and once flow begins the
relationship between shear stress and shear rate is linear or non-linear. The non-linear
materials can be either shear-thinning or thickening, with or without yield stress. Materials
with thickening behaviour are not very common, especially among particle suspensions.
Shear stress, τ [Pa] Shear stress, σ [Pa]
Hookean Newtonian
Elasticity, G [Pa] Viscosity, η [Pa s]
•
Shear strain, ε [-] Shear rate, γ [1/s]
Figure 2. The Hookean behaviour in which stress is proportional to strain versus the
Newtonian behaviour in which stress is proportional to shear rate.

Some materials also have a time dependence due to a flocculated microstructure, where the
flow characteristics are influenced by the shear history of a material. These types of
materials are usually defined as thixotropic or anti-thixotropic. In general, equilibrium
measurements are desired, and the time dependence is minimized by pre-shearing the
material and destroying the sample’s structure in the test [13]-[15].
A suspension with a wide range of particle sizes comprises a complex balance of
interparticle forces (i.e. interlocking, frictional, flocculation, colloidal, van der Waals, and
electrostatic forces), which generates this time dependence and viscoplastic non-
Newtonian behaviour [4][13][16]-[18].
Other factors which affect the flow behaviour are the temperature, pressure, and pH. It is
generally desirable to maintain these at constant levels throughout an experimental
procedure, and this is normally done. The effect of pressure can be neglected, as it is very
small at atmospheric pressure [13].
The viscosity of different materials varies in a wide range (Table 2) as do the shear rates
they may be subjected to in different industrial processes (Table 3). To be able to
characterize a fluid, a proper model to mathematically describe the rheology must be
selected, together with a suitable instrument for measurements under realistic conditions.
In the literature, there are several theoretical models, instruments and measuring
techniques proposed to evaluate the flow behaviour of non-Newtonian fluids.
Table 2. Viscosity of some familiar Table 3. Typical range of shear rates of
materials at room temperature [13][19]. some familiar processes [13].
Viscosity Shear rate
Liquid Process
η [Pa·s] γ& [s-1]
Glass 1040 Lubricating 103 - 107
Asphalt 108 Rubbing 104 - 105
Molten polymers 103 Spraying and brushing 103 - 104
SCC 102 Mixing and stirring 10 - 103
Syrup 10 Chewing / swallowing 10 - 102
Mortar 1 Pumping / pipe flow 1 - 103
Olive oil 10-1 Extruding 1 - 102
Water 10-3 Levelling 10-2 - 10-1
Air 10-5 Sedimentation 10-6 - 10-3
The rheological properties of cementitious materials (cement paste, mortar and concrete)
are mainly influenced by the following factors [5][20]-[24]:
a) Water content.
b) Amount of filler and aggregate, its particle shape, surface texture, porosity, size, and
size distribution, and consequently the particle packing and specific surface area.
c) Type and amount of cement and cement replacements
d) Amount of entrained air, and bubbles’ size.
e) Presence and efficiency of admixtures affecting the properties of adsorbed water
layer and particle dispersion.

f) Temperature.
g) Degree of hydration.
h) Time elapsed after mixing.
i) Mixing procedure.
Here, the water content and specific surface area are the two single most important factors
influencing the rheological properties of cementitious materials [5][22].
The objective of this chapter is to present, through a literature review, an introduction to
the rheology of particle suspensions and the factors affecting it. Flow behaviours,
rheological characteristics, models, and methods for measuring the rheology of fresh
cementitious materials are in focus.
2.2 Particle suspensions

Because suspensions of solid particles in a liquid generally behave as fluids, it is often
useful to characterize their rheological behaviour [13]-[15]. The two main factors affecting
the rheology of particle suspensions are the volume fraction of solid particles in the
suspension, and the extent to which the particles are flocculated [20]. The effect of
flocculation is most pronounced for colloidal particles (i.e. particles in size range 20µm -
1ηm). The forces are fairly weak, so by applying a stress the flocculated network can easily
be broken and the suspension will start to flow. For very dilute suspensions, the
interparticle forces are negligible, and Newton's law can be applied. When the effect of a
small increase of the volume fraction of solids (φ) merely increases the viscosity (η), it can
be defined by the Einstein equation as follows:
η = η c ⋅ ( 1 − 2.5 ⋅ ϕ ) (Eq. 1)
where ηc is the viscosity of the suspending medium. However, the Einstein equation and
Newtonian model are not suitable for fluids with a high concentration of particles, such as
paste, mortar, and concrete. As the volume fraction is increased above a few percent,
viscosity increases progressively. Several equations have been proposed to better describe
the full relationship between volume fraction and viscosity, taking into consideration the
maximum packing fraction of solids (φm) and the shape of the solids by applying a fitting
parameter (x), where the Krieger-Dougherty relationship (Eq. 2) is commonly used for
colloidal suspensions [20][25].
η = η c ⋅ ( 1 − ϕ / ϕ m ) − x⋅ϕ m
(Eq. 2)
For highly concentrated colloidal suspensions with a mix of particles with different
properties (size, shape and surface properties), such as cementitious materials, the viscosity
tends to be more complex when described mathematically. For these types of materials
there is a fine balance between the interparticle forces (e.g. van der Waals attraction,
electrostatic and steric repulsion, interlocking, friction, etc.) causing a non-Newtonian
viscoplastic flow behaviour [13][19].
The effect of w/c on paste viscosity is usually defined by the Krieger-Dougherty equation
(Eq. 2), whereas the effect of w/c on yield stress (σy) can be described by the power law:
σ y = A ⋅ ϕ B [Pa] (Eq. 3)

where φ is the volume fraction of solids, and A and B are a constants (typically in the range
of A is 2–4). Another way to express the yield stress is to consider also interparticle forces
that are responsible for flocculation. The effect of w/c on yield stress (σy) can then be
calculated as:
ϕB
σ y = A⋅ 2
⋅ Φ max
'
[Pa] (Eq. 4)
r
where r is the particle radius, and Φ’max is the maximum interparticle force (maximum
slope of the pair potential) [25][26].
2.2.1 Interparticle forces

Particle suspensions’ rheology is affected by macro-level factors like particle size, size
distribution, shape, texture, density, water content, etc., and micro-level forces such as
capillary, flocculation, colloidal and true solution forces [4][13][16]-[18]. The forces
interacting between suspended particles of different sizes can be categorized as shown in
Figure 3.
Effect of particle forces
Coherence:
Flowability:
Liquid-need:
Attraction:
Repulsion:
Size [mm]: 30 1 0.1 2·10-4 10-6 10-7

Forces: Mechanical Capillary Flocculation Colloidal Solution
Figure 3. Illustration of how particles of a certain size group under forces (x axis) are
acting in a suspension, in terms of coherence, flowability, need of liquid, and
attraction/repulsion (y axis). The magnitude is only relative within each property [18].
At macro-level there are interlocking and friction forces, and at micro-level there is a fine
balance between attractive and repulsive forces. The main attractive forces are collectively
called the van der Waals force (sometimes called London dispersion force), a short-range
electromagnetic and relatively weak force interacting between two bodies. The van der
Waals force arises from the polarization of molecules or particles into dipoles. This
includes forces that arise from fixed or angle-averaged dipoles (Keesom forces) and free or
rotation dipoles (Debye forces) as well as shifts in electron cloud distribution (London
forces) [4][27]. The main repulsive force is the force which the electrical double layer
gives rise to, and which acts between charged bodies with a potential difference.
The net result of these attractive and repulsive electric forces of suspended particles creates
an energy barrier as they approach each other [4]. The consequent potential energy, as a

function of interparticle distance (r), is illustrated in Figure 4. At a small separation

distance (r=r0), a deep potential energy trough is encountered, where the net force is zero
and the particles are at an equilibrium distance apart, causing the matrix to flocculate. To
make r smaller or larger than ro a dispersing or compressing force must be applied.
Depending on the balance of forces, a much less deep secondary minimum, with zero net
force, can exist at a larger interparticle distance (r=r0´) [14][28]. At this point the
flocculated particles can more easily be separated by an applied shear. Still, if this
secondary minimum is deep enough, relatively strong flocs can be formed. This is
considered to be the basis for the thixotropic behaviour of particle suspensions [29].
Since the ratio of surface to volume is inversely proportional to linear dimension, the effect
of these attractive and repulsive forces also increases as the particles become smaller and
their specific surface area increases.
Cementitious materials are highly

concentrated composite systems with a wide
range of particle sizes (from 10-7 to 30 mm for Repulsing r
+
concrete), where the fresh mix comprises a forces
Potential energy
complex balance of interparticle forces Interparticle
r0 r0’ distance, r
generating a suspension with viscoplastic non-
Newtonian behaviour. All these interacting
forces depend on the shape of the particles, Secondary
their size, concentration, and surface Attracting minimum
forces
properties, but also on the water content of the
-
suspension [4][18][19][28]. For cement-based Primary minimum

materials the balance between the flocculation
and colloidal forces acting between particles Figure 4. Illustration of the potential
in the size range from 0.1 mm down to 1 ηm energy as a function of interparticle
is predominant. distance.
In a matrix of the smallest particles, good coherence is accompanied by good fluidity (see
Figure 5). In a system with a wide range of particle sizes and all the forces working
together, the smallest particles with their good flowability now cause sedimentation of the
larger particles in the fluid matrix, and thus a bad coherence of the total mass. Hence, for
optimum coherence with strong flocculation, flowability is poor. This flowability can be
increased by adding more water as well as by increasing the amount of the smallest
particles, but at the price of decreased coherence. Thus, there is a compromise between
fluidity and coherence. Figure 5 illustrates how each group of particle sizes is affected by
another, in terms of coherence, flowability and need for water [4][18][24].
Hence, for a given mortar or concrete mix, the flowability can be adjusted on macro-level
by grading, shape and water content etc., and on the micro-level by the ratio between the
flocculation and colloidal forces. Stronger colloidal forces and weak coherence generate
better flowability, a smaller compaction energy need and a larger separation tendency [18].

Interacting forces of composite particle systems
Coherence:
Flowability:
Water-need:
Size [mm]: 30 1 0.1 2·10-4 10-6 10-7

Forces: Mechanical Capillary Flocculation Colloidal Solution
Figure 5. When a suspension incorporates a mix of particle sizes, the forces are acting
together. The figure illustrates how this balance of different size groups forces (x-axis)
affects coherence, flowability and need for water (y-axis). The magnitude is only relative
within each property [18].
To increase a fresh cementitious material’s flowability, regarding the interparticle forces,

one can [4][18][24]:
Choose a better total weighted grading curve (more densely packed structure).
Choose more rounded and smoother particles (with smaller interlocking and surface
area).
Increase the water content (which separates the particles).
Vibrate the material (which de-flocculates it temporarily).
Add de-flocculation agent with high zeta-potential (which increases the double-layer
effect).
Add very fine particles (<10-5 mm) with positively charged zeta-potential, e.g. silica
fume and fines in fly ash (colloidal repelling particles).
Add air-entraining agent (small air bubbles acting like ball-bearings).
Add a surface-active agent (giving electrostatic and/or steric hindrance).
Add admixtures that decrease the water’s surface tension (which decreases
flocculation).
Add large molecules which are adsorbed onto the cement particles (giving steric
hindrance).
There is also sometimes a need to increase the coherence in order to create robustness and
segregation resistance; therefore flocculating or thickening admixtures are used (to de-
charge the double layers or immobilize the water phase).

2.2.2 Flow characteristics

Suspensions and solutions, under steady shear Shear stress, σ [Pa] 3c)
flow conditions (equilibrium state), may
exhibit certain behaviours over a limited σ0* 3b)
range of shear rates. Additionally, some σ0 3a)

materials may exhibit more than one distinct
2b)
behaviour over different shear rate regions of
the flow curve. Several types of behaviour 2a)
can be classified according to their 1
characteristic shape (see Figure 6). The σapp
following classification system [30] covers
the most frequently encountered flow types, •
Shear rate, γ [1/s]
divided in terms of Newtonian, general non-
Newtonian, and viscoplastic non-Newtonian Figure 6. Flow types illustrated as
fluids: curves and their characteristic shape.
1. Newtonian: Viscosity is constant with shear rate changes.

2. General non-Newtonian:
a) Shear-thickening: Viscosity increases continuously as shear rate grows.
b) Shear-thinning (pseudoplastic): Viscosity decreases continuously with shear rate.
3. Viscoplastic non-Newtonian fluids:
a) Shear-thinning with yield-response: Viscosity decreases continuously with shear
rate once the apparent yield stress (σapp) has been exceeded.
b) Bingham plastic (ideal): Above the Bingham yield stress (σ0) the differential
viscosity is constant and is called the plastic viscosity.
c) Bingham plastic (non-ideal): Above the apparent yield stress the viscosity
decreases continuously and approaches a constant value with increasing shear rate.
Extrapolation of the flow curve from the linear region (plastic region) to the stress
axis gives the apparent Bingham yield stress ( σ 0* ) and the plastic viscosity.
Newtonian Fluids
In the simplest type of flow, termed Newtonian, the material’s viscosity is constant and
independent of the shear rate [13][14]. That is, when shear stress (σ) is plotted against
shear rate ( γ& ) at a given temperature, the plot shows a straight line with a constant slope
that is independent of shear rate (see Figure 6). This slope is called the Newtonian
viscosity (η) of the fluid. The simplest constitutive equation is Newton’s law of viscosity:
σ = η ⋅ γ& [Pa] (Eq. 5)
From this it may be seen that a single point measurement, with a corresponding pair of
values of σ and γ& , would serve to rheologically define a Newtonian fluid.
All gases and common liquids such as ethanol, water and most oils are Newtonian. Also,
liquids with low molecular weight and solutions of substances with low molecular weight
in liquids, e.g. aqueous solutions of sugar or salt, are usually Newtonian.

General non-Newtonian Fluids

Any fluids that do not obey the Newtonian relationship between shear stress and shear rate
are non-Newtonian. The subject of rheology is generally devoted to the study of the
behaviour of such fluids. Suspensions of fine particles are usually non-Newtonian [13][14].
In the case of general non-Newtonian fluids, the slope of the shear stress versus shear rate
plot is not constant. When the viscosity of a fluid decreases with increasing shear rate, the
fluid is called shear-thinning (pseudoplastic). In the opposite case where the viscosity
increases as the fluid is subjected to a high shear rate, the fluid is called shear-thickening.
The term dilatant is commonly used for shear-thickening, although this usage is strictly
incorrect. Dilatancy is a property that usually is associated with suspension of irregularly
shaped particles, in which the liquid exhibits an increase in volume while being sheared.
Viscoplastic non-Newtonian Fluids
The other important class of non-Newtonian fluids is a viscoplastic fluid. This is a fluid
which will not flow when a very small shear stress is applied. The shear stress must exceed
a critical value known as the yield stress for the fluid to flow [13][14]. For example, when
opening a tube of toothpaste, an adequate force has to be applied in order to make the
toothpaste start to flow. Therefore, viscoplastic fluids behave like solids when the applied
shear stress is less than the yield stress. Once the applied shear stress exceeds the yield
stress, the viscoplastic fluid flows just like a normal fluid. Examples of viscoplastic fluids
are blood, paint, mayonnaise, toothpaste, grease, foods, and mortar and concrete.
Once the yield stress has been exceeded, the slope of the shear stress versus shear rate
curve may be either constant or non-constant. If the fluid obeys a yield value and has a
constant viscosity it is called Bingham-plastic, and if the viscosity is non-constant it is
called shear-thinning and shear-thickening with yield response.
2.2.3 Rheological models

By using a mathematical relationship, a fluid can be rheologically characterized by a small
number of coefficients (e.g. viscosity and yield stress).
The models that are presented in this section are used to characterize the non-Newtonian
behaviour of fluids in equilibrium, under steady shear flow conditions at constant pressure
and temperature. A large number of models have been reported in the literature, but only
those which are applicable to the study of the rheology of particle suspensions have been
included [13]-[15][26][28][31]-[35].
In the literature, several theoretical models used to describe the non-Newtonian flow
behaviour can be found. The most frequently used fundamental models are the Power-law,
Bingham and Herschel-Bulkley.
These models are well suited to studying materials over a small shear range or where only
a simple relationship is required. But many materials will start to deviate from these
relationships over a sufficiently large shear range. To be able to give a more realistic
prediction of flow over a wider range of conditions, as enhancements to the fundamental
models, other relationships have been developed. More detailed description and alternative
expressions can be found in the cited literature.
For mortar and concrete, the Bingham model is considered by many researchers to be the
most useful. This can be explained by its simplicity (with only two parameters), and by the

fact that materials of this type, over a limited range of shear rates, correspond quite closely
to the model [24][28]. However, it ought to be noted that there are no fluids which behave
like an ideal Bingham material. This is only a generalized model to be used for non-ideal
Bingham materials [36]. For cement paste, there are disagreements as to which model best
describes the flow behaviour. These types of highly concentrated suspensions,
incorporating a high ratio of colloidal particles (i.e. particles smaller than approx. 1µm),
tend to show a more pseudo-plastic shear-thinning behaviour at equilibrium flow. In the
literature, different models have been proposed but the Bingham model and the Herschel-
Bulkley model tend to be best suited for cement pastes [25][28][34][37][38]. The Bingham
model is better suited for pastes with high water-to-cement ratio (w/c) than for those with
low w/c [25]. When superplasticizer is added, paste tends to show Newtonian behaviour at
low concentrations and viscoplastic behaviour at high concentrations [26]. SCC, however,
has been suggested to a have a shear-thickening behaviour with a yield, and the rheology
parameters are to be defined by the Herschel-Bulkley model (with A>1) [39]. Others
consider the apparent shear-thickening behaviour of SCC to be an artefact from the
experimental setup, caused by a lack of steady state during the measurement, where the
structure of flocculated colloidal particles has not been broken [40][41].
Typical values of yield stress and plastic viscosity for some cementitious materials, defined
by the Bingham model, are shown in Table 4. For SCC, it cannot be at the lower limits of
yield stress and viscosity simultaneously, since it would separate.
Table 4. Typical range of yield stress (σ0) and plastic viscosity (ηpl) for cement paste,
mortar, “normal” concrete (NC and flowing NC), and self-compacting concrete (SCC),
defined by the Bingham model [5] [19] [42].
Paste Mortar NC Flowing NC SCC
σ 0 [Pa]: 10−50 10−100 400−2000 100-400 10−100
η pl [Pa s]: 0.01−1 1−5 50−100 20-100 20−150
Power-law (or Ostwald-de Waele)

Many non-Newtonian materials undergo a simple increase or decrease in viscosity as the
shear rate is increased. One of the most widely used forms of the general non-Newtonian
constitutive relation is a power-law model, a two parameter model expressed as:
σ = η app ⋅ γ& A [Pa] (Eq. 6)
where σ is the shear stress, ηapp is a non-Newtonian apparent viscosity defining the
consistency of the fluid, and A is the power-law model constant indicating the degree of
non-Newtonian behaviour (the greater the departure from unity, the more pronounced the
non-Newtonian properties of the fluid).
The power-law model does not handle viscoelastic materials with a yield stress. If A<1, a
shear-thinning fluid is obtained, which is characterized by a progressively decreasing
apparent viscosity with increasing shear rate – whereas if A>1, it is a shear-thickening
fluid, and when A=1 it is a Newtonian fluid. These three types of power-law models are
illustrated in Figure 7. The power-law model is good for describing a material’s flow
within a small range of shear rates, but fails to describe the viscosity of many non-
Newtonian fluids in very low and very high shear rate regions (e.g. for suspensions, η goes
to infinity at a very low shear rate and becomes constant at a very high shear rate), nor
does the model handle viscoelastic materials with a yield.

Shear stress, σ [Pa] 3a) Herschel-Bulkley, A<1 (shear-thinning with yield)

3b) Bingham (or Herschel-Bulkley when A=1)
2b) Power-law, A<1 (shear-thinning)
1) Newtonian (or Power-law when A=1)
2a) Power-law, A>1 (shear-thinning)
σapp
σ0 Viscosity, η [Pa s]
2a)
•
1) 3b)
2b) 3a)
•
Figure 7. Flow curves of Power-law, Bingham and Herschel-Bulkley models.
Bingham
Some materials exhibit an infinite viscosity until a sufficiently high stress is applied to
initiate flow. Above this stress the material then shows simple Newtonian flow. The
simplest model covering these types of viscoplastic fluids with a yield response is the ideal
Bingham model, and is expressed by the following two parameter equation:
σ = σ 0 + η pl ⋅ γ& {σ > σ 0 } [Pa] (Eq. 7)
where ηpl is the model coefficient of plastic viscosity, and γ& is the shear rate. σ0 is the
constant which is interpreted as yield stress, and which often is referred to as the Bingham
yield stress or simply the yield stress of the material. The Bingham model can describe the
viscosity characteristics of a fluid with yield stress whose viscosity is independent of shear
rate, as shown in Figure 7. Therefore, the Bingham plastic model does not have the ability
to handle the shear-thinning characteristics of general non-Newtonian fluids.
Many concentrated particle suspensions and colloidal systems, such as mortar and
concrete, show Bingham behaviour at limited ranges of shear rate.
All rheological measurements presented in the appended papers (Paper I, II, III and VI), on
both mortars and concretes, were performed with the Bingham model.
Herschel-Bulkley
The Herschel-Bulkley model is a three-parameter model used to describe viscoplastic
materials exhibiting a yield response with a shear-thinning relationship above the yield
stress. It is a combination of Power-law and Bingham, and is expressed as:
σ = σ app + ηapp ⋅ γ& A {σ > σ app } [Pa] (Eq. 8)
where σapp is the constant that is interpreted as apparent yield stress, ηapp is the model
coefficient of apparent viscosity, γ& is the shear rate, and A is the model constant indicating
the degree of non-Newtonian behaviour (the greater the departure from unity, the more

pronounced the non-Newtonian properties of the fluid). When A=1, Herschel-Bulkley is

reduced to the equation for Bingham (see Figure 7). The Herschel-Bulkley model tends to
give a more realistic prediction of flow over a wider range of conditions than the Bingham
model. It is often applied to industrial fluids (e.g. biological fluids, food and cosmetics),
where it is used for specifying conditions in the design of process plants.
2.2.4 Yield stress measurement

Whether yield stress is a true material property or not is a controversial issue [14].
However, there is generally an acceptance of its practical usefulness in engineering design
and operation of processes where handling and transport of industrial suspensions are
involved. For example, the minimum pump pressure required to start, the resistance to
initiating flow, the segregation of aggregates, and entrapment of air in cementitious
materials are typical problems where the knowledge of the yield stress is essential.
Numerous techniques have been developed for determining the yield stress, both directly
and indirectly [14][15][20], based on the general definition of the yield stress as the stress
limit between flow and non-flow conditions. Indirect methods simply involve the
extrapolation of shear stress vs. shear rate data to zero shear rate, with or without the help
of a rheological model. Direct measurements generally rely on some independent
assessment of yield stress as the critical shear stress at which the fluid yields or starts to
flow.
Various techniques have been introduced for measuring the yield stress directly and
independently of shear stress vs. shear rate data [14][15][20]. Although the general
principle of the yield stress as the stress limit between flow and non-flow conditions is
often used, the specific criterion employed for defining the yield stress seems to vary
among these techniques. Constant shear stress rheometers provide the most direct method
for making the measurement, where the stress is progressively increased, yield is reached,
and flow initiates. Furthermore, each direct technique appears to have its own limitations
and sensitivity, so that no single technique can be considered versatile or accurate enough
to cover the whole range of yield stress and fluid characteristics.
The value obtained by the extrapolation of a flow curve is known as “apparent” (or
“extrapolated”) yield stress, whereas yield stress measured directly, usually under a near-
static condition, is termed a “static” (or “true”) yield value. In a strain-stress measurement,
the static yield stress (σs) can be evaluated either from the point where the elastic response
starts to diverge from its linearity, or at the peak stress just before the material’s elastic
structure breaks and turns into a plastic state (see Figure 8) [29]. However, it can be
problematic to find the exact point where the response starts to diverge from linearity, as it
usually is not a distinct point. Moreover, in a strain-stress measurement the value of static
yield stress depends on the applied rate of shear strain (or shear stress when measuring the
strain).

Shear strain, ε [-] Shear stress, σ [Pa]

Elastic response
σs Peak level
σs
Load Respons
Time, t [sec] Shear strain, ε [-]
Figure 8. Determination of static yield stress (σs), by a strain-stress measurement, either

from the point where the elastic response starts to diverges from its linearity, or at the
peak stress.
The indirect determination of the yield stress simply involves the extrapolation of
experimental shear stress vs. shear rate data to zero rate (see Figure 9). The extrapolation
may be performed graphically or numerically, or can be fitted to a suitable rheological
model representing the fluid.
Direct data extrapolation is a procedure to extend Shear stress, σ [Pa]

the flow curve at low shear rates to zero shear rate,
x
and take the shear stress intercept as the yield xx
stress value. The technique is only relatively Bingham
x
x
straightforward if the shear stress vs. shear rate x
x
x
data are linear and there is no plug flow. With x
σ0
non-linear flow curves, as shown in Figure 9, the x
x
data may have to be fitted to a polynomial σapp Curve fit
equation followed by the extrapolation of the
resulting curve fit to zero shear rate. The yield Shear rate, •γ [1/s]
stress value obtained obviously depends on the Figure 9. Determination of
lowest shear rate data available and used in the apparent yield stress (σ0 and σapp)
extrapolation. Thus, it is imperative that some by extrapolation from a curve fit,
checking procedure should be carried out to and by applying a rheological
ascertain the reliability of the low shear rate data model. In this illustration a 3rd-
before extrapolation is made. Thixotropic order polynomial curve fit and
materials with a high yield stress tend to provide the Bingham model are applied
non-steady shear flow and plug flow due to to measurements in a flow curve.
structural build-up at low shear rate.
A more convenient extrapolation technique is to approximate the experimental data with

one of the viscoplastic flow models. Many researchers appear to prefer the Bingham model
which postulates a linear relationship between shear stress and shear rate. However, since a
large number of yield stress fluids, including suspensions, are not Bingham-plastic except
at very high shear rates, the use of the Bingham plastic model can lead to unnecessary
over-prediction of the yield stress, as shown in Figure 9 [14][43].
Extrapolation by means of the nonlinear Casson model can be used from a linear plot of
γ& versus σ . The application of the Herschel-Bulkley model is less certain although
systematic procedures for determining the yield stress value and the other model
parameters are available. Even with the most suitable model and appropriate technique, the
yield stress value obtained cannot be regarded as an absolute material property because its

accuracy depends on the model used and the range and reliability of the experimental data
available. Several studies [14] have shown that a given fluid can be described equally well
by more than one model and, hence, can have different yield stress values.
It has been shown by many investigators that the empirical tests to some extent provide
information about the concrete rheology. Slump has for a long time been considered to be a
unique function of yield stress (Bingham), without influence by plastic viscosity [44]-[60].
More recently the horizontal flow spread, rather than the vertical slump, has been used to
calculate the yield stress [24][61]-[63]. Usually these correlations concern concretes in a
small range of flowability (e.g. HPC, SCC), and are not valid for other or wider ranges.
Often the correlation is purely empirical, but there are also some physical models proposed
to explain the relationship. The viscosity, on the other hand, is generally considered to
correlate with empirical tests recording the flow time. For SCC, this connection is usually
made with the slump flow spread time to 500 mm (T50) or V-funnel time [64]-[66].
In Paper I experimental results are presented, addressing the interaction between the slump
flow spread, flow time (T50), yield stress (σ0) and plastic viscosity (ηpl). It was shown that
the slump flow spread is not a unique function of yield stress, but rather a more complex
function of both yield stress and viscosity. However, the spread proved to be much more
closely related to the yield stress than to the viscosity, especially at high viscosity, whereas
the T50 time was connected more equally with yield stress and viscosity. These relations
are illustrated in Figure 10.
1000 1000
800 800
Slump flow [mm]
Slump flow [mm]
y = -124.65Ln(x) + 1071.82
600 2 600
R = 0.89
400 400
200 200
0 200 400 600 0 50 100 150 200
Yield stress [Pa] Viscosity [Pa s]
25 25
20 20
15 15
T50 [s]
T50 [s]
10 10
5 5
0 0
0 50 100 150 0 50 100 150
Yield stress [Pa] Viscosity [Pa s]
Figure 10. Measures of slump flow values vs. rheological parameters, individually, for
~550 mixtures with a wide range of consistency.

The following approximate models for calculating the relative slump flow area (Rp) and
the slump flow spread time T50 (in seconds) for flowable concretes (and mortars), over a
wide range of consistencies, was proposed:
( H / 6 )2
Rp ≈ (Eq. 9) R p = ( D / D0 ) 2 − 1 (Eq. 10)
ln( η pl + 2 ) ⋅ σ 0
T 50 ≈ 0.002 ⋅ σ 0 ⋅ η pl (Eq. 11)
where ηpl is the plastic viscosity, σ0 the yield stress, H the cone height (300 mm for
Abram’s cone), D the measured spread diameter in millimetres, and D0 the flow cone
bottom diameter (200 mm). The models are purely empirical and are deficient in units.
They are only intended to roughly illustrate the interaction between the rheological
parameters and slump flow values.
In the literature it is not generally agreed that slump flow is a unique measure of concrete
yield stress [67]-[73]. It has been noted that the correlation is weak, or that relation
between yield stress and slump flow, without taking viscosity into account, does not show
a satisfactory fit. In Figure 11, typical values for SCC, presented by Nielsson and Wallevik
[67], are plotted in the diagram from Paper I showing the correlation between the
measures of slump flow values and rheological parameters.
120 550 mm 600 mm 650 mm 700 mm
>700 mm
600-700 mm
90 500-600 mm
Yield stress [Pa]
500-600 mm
60
30 600-700 mm
>700 mm
0
0 50 100 150
Viscosity [Pa s]
Figure 11. The slump flow spread (mixtures with a spread <500 mm are excluded) and
Bingham rheology parameters (yield stress and plastic viscosity) for SCC from Paper I,
complemented with typical values for SCC from [67].
2.2.5 Time dependence

Some materials have a reversible time dependence, where the flow characteristics are
influenced by the shear history of a material. At rest the material regains its original state.
These types of materials are usually defined as thixotropic or anti-thixotropic. If there is a
reversible recovery of viscosity with time, it is referred to as thixotropy – and if the
recovery results in a decrease in viscosity, it is termed anti- or negative thixotropy
(sometimes referred to as rheopexy, although this is not the preferred term). The effects of
thixotropy and anti-thixotropy are illustrated in Figure 12.
Cementitious materials generally shows time-dependent reversible flow behaviour,
referred to as thixotropy. Other well-known examples of thixotropic materials are: yoghurt,
ketchup, mayonnaise, wall paint, and clay.

The phenomenon of thixotropy rises from the

microstructure of the matrix system [14], due
•
to aggregation and flocculation of suspended
particles and the time taking to change this Load
microstructure. In such a system, interaction
occurs between the particles as a result of the
attraction due to van der Waals forces and
Shear stress, σ [Pa]

repulsion due to electrostatic and steric effects.
The stability of the structure depends upon the
existence of a potential energy barrier which
prevents the particles from approaching close Thixotropic
to one another. In this way, the weak physical

bonds between the particles give rise to

aggregation. As the suspension is sheared, the
weak physical bonds among particles are
ruptured, and the network among them breaks
down into separate aggregates, which can Anti-thixotropic
disintegrate further into smaller fragments Time, t [s]

(small aggregates or flocs), whereas if the
suspension is at rest the particle aggregation Figure 12. When gradually ramping
can re-flocculate and form again. These shear- down, the structure breaks down or
induced changes in microstructure take time rebuilds, whether it is thixotropic or
and, if fully reversible, are referred to as anti-thixotropic, and whether at high
thixotropy [4][14][19][32][74][75]. The time or low load. The figure illustrates a
for structural breakdown is normally shorter controlled rate; with controlled
than the time for structural build-up [29]. stress, the effect is the opposite.
It should be noted that these changes are purely time related and the materials flow
characteristics need to be studied as well. It is possible that a material could be both
thixotropic and shear-thickening or shear-thinning.
In order to characterize the rheology of cementitious materials and other time-dependent
material, one has to be aware of these effects. It is necessary to study the time dependence
of the material in order to design a conditioning regime. To be able to compare
measurements in common references, it is important to take steps to pre-condition the
sample. The best method for this purpose is to pre-shear the sample for a time sufficient to
destroy any structure (flocculated colloidal particles) [41]. One way to do this is to start at
a high shear rate for a sufficient time, followed by measuring stress while decreasing the
strain rate from high to low. Another method is to initiate each measurement with a
constant shear, applied for a time sufficient to reach equilibrium (within acceptance)
[14][28]. At low strain rates a suspension may be very slow to reach equilibrium.
There are many methods proposed, based on rheological measurements, for how to
characterize the time dependence. However, the quantification of thixotropy in absolute or
fundamental terms is problematic, as it depends on the shear history of the material as well
as the method used to measure and evaluate the thixotropy; hence the thixotropic value is
often only relative. A commonly used technique to determine the thixotropy is to measure
the time needed for a structural breakdown [28]. This is usually done by applying a
constant shear rate (or stress), and recording the time for the measured shear stress (or rate)
to reach an equilibrium state (within acceptance); see Figure 14. As the breakdown time
depends on the size of the applied shear, the test can be performed at different specific

levels of rate (or stress), respectively. A method to characterize the material’s thixotropy
with a single value [76][77], when using different levels of shear, is to determine the area
between the curves of initial shear stress and equilibrium shear stress (see Figure 13).
Shear stress, σ [Pa] Shear stress, σ [Pa]
Initial shear stress

Initial shear stress
Equilibrium
shear stress Thixotropic
area [Pa/s]
Equilibrium
shear stress
•
Time, t [sec] Shear rate, γ [1/s]
Figure 13. Thixotropy represented by the evaluated area between the curves of initial
shear stress and equilibrium shear stress
Another popular method, especially for cementitious materials, is to quantify the time
dependence by the area of a flow hysteresis. This area represents the energy needed to
break down the structure [78]. In a typical rheometric test, shear stress or shear rate is
ramped at a fixed speed up to a maximum value, then ramped back down at the same speed
to the beginning (see Figure 14). In hysteresis, one flow curve lies above the other,
forming a continuous loop whose internal area depends on the shear and thermal history of
the material, and on how rapidly the stress or shear rate was ramped. Not all researchers
agree that the area of a flow hysteresis in measurements of stress as a function of rate
represents any material characteristics. The first method, where the stress is measured
directly as a function of time at some strain rate, is considered to better reflect the
thixotropic behaviour [28].
Shear stress, σ [Pa] Shear rate, γ [1/s]
Shear stress, σ [Pa] Shear rate, γ [1/s]
• •
Thixotropic
area [Pa/s]
Thixotropic
time [s]
•
Time, t [s] Time, t [s]
Figure 14. Thixotropy quantified by the area of the flow hysteresis when the shear rate is
ramped up and down, or alternatively by the time to steady-state (equilibrium) flow at
constant shear rate.
In Paper II, a thixotropic measurement on mortars was performed, using the latter method
with the area of the flow hysteresis.
There is no general agreement that the thixotropy can be evaluated by measuring structural
breakdown, nor that methods based on the calculated area represent any material
characteristics [28]. The structural build-up at rest, rather than the breakdown, is proposed
to better represent the material’s true thixotropic behaviour [29], and it is to be monitored
without breaking down the structure. Furthermore, the elastic region of a viscoelastic
material is proposed to represent the structure; hence it is to be characterized by a strain-

stress measurement where the structure corresponds to the peak stress (the static yield
stress), just before the material’s elastic structure breaks and turns into a plastic state (see
Figure 8). However, it can be problematic to avoid a structural breakdown when
measuring this peak level. Moreover, the peak level is dependent on the applied rate of
shear strain (or shear stress when measuring the strain).
Another non-destructive method to measure the material’s structure, represented by its
elastic region, is by an oscillating rheology test. The deformations are small and kept
within the linear viscoelastic region, so the structural build-up can be monitored over a
time period without destroying the structure. In a typical oscillation test, illustrated in
Figure 15, the applied periodic stress (σ) and the resulting strain (γ) can be described as:
σ = σ 0 ⋅ cos( ω ⋅ t ) [Pa] (Eq. 12) γ = γ 0 ⋅ cos( ω ⋅ t − δ ) [-] (Eq. 13)
where σ0 is the stress amplitude, γ0 is the strain amplitude, ω is the angular frequency, t is
the time, and δ is the phase lag (loss angle) [14][79]. For an ideal solid the phase angle will
be δ=0, whereas for a Newtonian fluid with a purely viscous response it will be δ=2π
(=90°). The materials rheological characteristics are described in terms of the shear storage
modulus G’ (representing the elastic response of the material), and the shear loss modulus
G” (representing the irreversible viscous response) can be calculated as:
G' = σ 0 / γ 0 ⋅ cos( δ ) [Pa] (Eq. 14) G" = σ 0 / γ 0 ⋅ sin( δ ) [Pa] (Eq. 15)
Strain, γ [-]
Stress, σ [Pa] Phase angle, δ [rad]
σ0
γ0
Time, t [sec]
Resulting strain, γ [-]

Applied stress, σ [Pa]
Figure 15. Principle of oscillatory measurement of a viscoelastic fluid.

To quantify thixotropy in absolute or fundamental terms is problematic, as the methods are
dependent on the shear history of the material as well as the method used to measure and
evaluate the thixotropy. Therefore, the thixotropic value will only be relative.
For suspensions subjected to chemical reactions, particles absorption, etc., causing an
irreversible time dependence, it is important to exclude these effects from those which are
reversible. Cementitious materials have a time-dependent irreversible behaviour, which is
not to be confused with the time-dependent reversible flow behaviour (i.e. thixotropy).
Hydration produces a type of hysteresis, where the stress during the subsequent
measurement is higher than during the former measurement [26][28]. These changes are
not reversible. The same phenomenon can be observed in the time-dependent water
adsorption on particles’ surfaces and the absorption into the particles. A porous particle
with a rough surface texture generates a more delayed adsorption than a smooth non-
porous particle. Also the loss of water due to evaporation will have the same effect as the
adsorption (and absorption). Another feature causing an irreversible behaviour is the loss
of dispersing efficiency of the superplasticizer and other water reducing admixtures. A
feature also producing a hysteresis, observed with cementitious materials, is an irreversible
structural breakdown on first mixing. This is not thixotropy (it is not reversible), but it
could easily be confused with thixotropy if the reversibility were not assessed. Usually
these effects are classified as irreversible structural breakdown.

There is no general agreement that the true Yield stress, σo and σs [Pa]
thixotropy can be evaluated by measures of Static yield stress (σs)
structural breakdown, but rather methods using Thixotropic
structural build-up at rest are to be used [29]. This area [Pa·s]
Dynamic yield
is proposed to be characterized by a non- stress (σo) Reversible
destructive method, for example by the peak stress structure
(see Figure 8) in a strain-stress measurement [29].
To exclude the time-dependent irreversible Non-reversible
structure
behaviour from the reversible (thixotropic), the
static yield stress is to be related to the dynamic Time, t [sec]
yield stress (e.g. by Bingham, without thixotropic

Figure 16. Principle for de-
effects). The reversible part of the structure can
termining the thixotropic area of
then be evaluated from the area between the
the reversible (time-depending)
curves of static and dynamic yield stress versus
structure.
time (see Figure 16).
2.2.6 Temperature dependence

Temperature has a dramatic effect on the viscosity of any liquid, including particle
suspension as a whole, and its suspending media. The viscosity of fluids is usually found to
decrease with an increase in temperature [13], assuming that no physical/chemical changes
are being induced by the applied heat energy. Liquids with higher viscosities generally are
more temperature-sensitive. By using the Arrhenius relationship, a Newtonian liquid’s
change in viscosity with temperature can be calculated approximately as:
E0
η = A⋅e R ⋅T (Eq. 16)
where A is a constant, E0 is the fluid activation energy in J/mol, R is the gas constant, and T
is the absolute temperature in Kelvin. For water at 20°C, the equation can be
approximately written as:
η = 5.5 ⋅ e ( −2520 / T ) (Eq. 17)
To maintain ±1% accuracy in the measurements of viscosity, at 20°C, the sample then
must hold the temperature to ±0.3°C. For particles suspended in water, the viscosity rises
with concentration and the temperature dependence increases. Consequently, precise
control of the sample temperature is necessary to measure viscosity accurately.
2.3 Measuring techniques

To establish the fundamental rheological measurements for non-Newtonian fluids, a
rheometer is to be used. Numerous types of this instrument have been proposed for
evaluation of the dynamic viscosity and yield stress of such materials. A rheometer is used
to measure both viscosity and yield stress of a material, whereas a viscometer measures
only the viscosity since these instruments do not measure the shear stress and shear rate
simultaneously of a fluid at a given point. In order to determine real values of stress and
rate (at the same point) an absolute instrument is needed, where the determination is made
on the basis of a known mathematical description of flow occurring in the instrument and
on the basis of its geometry.

The measuring techniques can be divided into four principal ones, as shown in Figure 17.
Shearing parallel Rotating concentric Rotating Capillary tube

plates cylinder parallel plates
Figure 17. Illustration of the four main rheological techniques.

Numerous more or less empirical techniques have also been proposed. The most basic type
is the cup method, where the time that it takes to empty a cup with a defined hole in the
bottom gives a measure of the viscosity. Other types use a penetration rod, ball, etc., where
a falling objects with a defined density penetrates the samples. These types of kinematic
viscometers are only appropriate for making comparative studies, as the shear rate is not
fully controllable, and they are excluded from this study [14][13][28][80][15].
In order to determine the rheological properties of a Herschel-Bulkley

non-Newtonian fluid, a multipoint flow curve has to
be measured. A single point on the flow curve does
not describe this material correctly. Two fluids with Bingham
completely different rheological properties may
Viscosity (Newton)
generate the same value of viscosity at a given value
of shear rate if the flow curves intersect at this point Shear rate, •γ [1/s]
(see Figure 18).
A schematic illustration of the principal techniques Figure 18. Two flow curves
for measuring the viscosity and yield stress of non- intersecting, generating the
Newtonian fluids is shown in Figure 19. same value of viscosity at a
single measurement point.
Rheometers
Viscosity measurements Yield stress measurements
Drag flow Pressure driven flow Indirect methods Direct methods
Rotating rheometer Data Model

extrapolation extrapolation
Concentric Cone & Parallel Capillary tube

cylinder plate plates rheometer
Figure 19. Rheometers’ principal techniques for determining the viscosity and yield stress.
Most of these rheometers can produce viscosity measurements at a specified, constant
shear rate or shear stress (normally a constant shear rate is applied). Therefore, in order to
measure the viscosity over a range of shear rates, one needs to repeat the measurement by
varying either the pressure in the reservoir tank of the capillary-tube rheometer, or the

rotating speed (or torque) of the cone or cup in the rotating rheometers. In addition, since
these tests are to be performed at a stationary state, the capillary-tube rheometer is not very
applicable to a thixotropic fluid like fresh cementitious materials where the samples are to
be pre-sheared before measuring. For the yield measurement of viscoplastic materials, the
indirect methods are preferred rather than direct methods, for practical reasons [43]. Thus,
the direct methods will not be rigorously discussed.
In a rotational rheometer, the fluid sample is sheared as a result of the rotation of a cylinder
or cone. The shearing occurs in a narrow gap between two surfaces, usually one rotating
and the other stationary. Three frequently used geometries are: the coaxial (concentric)
cylinder, the cone-and-plate, and parallel plates. The coaxial cylinder is the most
commonly used [14].
In a capillary-tube rheometer, the fluid is made to flow through a capillary tube and the
rates of flow under known pressure differences are measured. This method is commonly
used in the process industry, where the apparatus can be installed in series with the flow.
Standardized measuring geometry for the different rheometers can be found in DIN 53018,
DIN 53019, ISO 2884 and ISO 3219.
2.3.1 Rotational rheometer, concentric cylinder

In a concentric (coaxial) cylinder system the inner cylinder is often referred to as a bob,
and the external one as a cup. The shear rate is determined by geometrical dimensions and
the speed of rotation. The shear stress is calculated from the torque and the geometrical
dimensions. By changing the speed of the rotating element, different torques can be
obtained (or different rotation when changing the torque), which are used for the
determination of the shear stress / shear rate curve. Figure 20 shows a typical coaxial
cylinder system that has a fluid confined within a narrow gap (Ri/Ro≥0.99) between the
inner cylinder rotating at an angular velocity ( Ω ), and the stationary outer cylinder
(normally it is the inner one that rotates).
With the concentric (coaxial) cylinder system, Ω

the shear profile over the gap will not be linear;
thus, ambiguity arises over the best value to
use for the effective mean radius (Ra) in the
H
calculation of shear stress and shear rate. The
shape of the profile is governed not only by the
geometrical dimensions, but also by the flow
characteristics of the fluid [15]. For a known Ri
flow characteristic an approximate solution can gap Ra
be found and the analysis of data will not
involve differentiation calculations. E.g. for a Ro
Bingham fluid, the so-called Reiner Riwling
equation can be used, provided that there is no Figure 20. Principle of a con-centric
plug flow over the profile and that the gap is cylinder rheometer. In this example
sufficiently narrow. the bob is rotating.
For particle suspensions, such as cementitious materials, there are well-established rules
for the geometry of apparatus and sample to ensure that rheological measurements are
reliable. The chief rules are that any dimension should be at least 10 times the size of the

largest particles (Ro-Ri≥10·Dmax) and that the ratio of outer to inner cylinder radius should
be less than 1.2 [14][19][28]. It can be noted that this is not the narrow gap that is required
to generate a known shear profile (Ro/Ri≤1.01), but in order to have manageable
equipment the maximum ratio of radii is set to 1.2 without generating too large errors. E.g.
if 0.5 mm particles and a narrow gap are to be used, the diameters of the inner and outer
cylinders would have to be approximately 1 metre. Wide-gap (Ro/Ri>1.2) concentric
cylinder rheometers exist, but the calculation of shear stress and rate requires broad
assumptions concerning these parameters over the range of shear across the gap. Thus,
small-gap (Ro/Ri≤1.2) rheometers are preferable because they do not require large
assumptions, and they also decrease the risk of plug flow [20][26][28].
For a viscoelastic fluid, at low shear rate, there is always a risk of plug flow. If the shear
stress falls below the yield value (see Figure 22). The velocity gradient over the profile
will change, and there will be a part of the material without velocity. The gap where flow
occurs will then be reduced to an indeterminable value, so the calculations of angular
velocity and torque into shear rate and shear stress will not be valid. With a rotating inner
cylinder, the plug of solid material will appear at the outer cylinder and at the inner
cylinder when the outer is rotating. In a flow curve (shear rate versus stress), plug flow will
be manifested as loss of shear stress in the low shear rate region. For a Bingham fluid, the
measured values at low shear rates will diverge from the linear curve (similarly to the non-
ideal Bingham-plastic behaviour in Figure 6, curve 3a); hence these values are to be
excluded. The lower limit of the angular velocity (Ω), where all material is sheared in the
gap, for a Bingham fluid, can be calculated as [28]:
Ω = [( Ro / Ri ) − 1]2 ⋅ σ 0 / η pl (Eq. 18)
The end-effects, where shear is

generated at the bottom of the inner
cylinder, can be tackled by entrapping
air at the bottom of the inner cylinder if
it has a concave shape, or else by
making the end of the inner cylinder
bottom into a cone-and-plate geometry
and incorporating this in the equations.
The wall-slip, where a lubricating slip-
layer is formed at the surface of the
inner cylinder (see Figure 23), can be
avoided by grooving the surface or
designing the bob as a vane (see Figure Figure 21. Photo showing cylinders (bob)
21). However, a vane may introduce a with different geometries. From left: cone-
complex flow (e.g. turbulence). and-plate, concave, grooved and vane.
For mortars and pastes, the grooved inner cylinder and the vane have been shown to
provide stable measurements and equal results, whereas the smooth (conical and concave
in Figure 21) gave deficient measurements with a shear-thinning behaviour (indicating
wall-slip) and with a larger scatter.

Lubricating slip-layer
Ro
”plug” Ω
Ri
Ω
Complete Incomplete
flow flow
Shear stress σ
σ < σ0
γ·
Shear rate
(velocity)
Figure 22. Illustration of plug flow, with a Figure 23. Illustration of wall-slip, with a
section of solid material at the outer lubricating slippage layer of suspending
cylinder (when the inner rotates), where media formed at the surface of the inner
the shear stress is below the yield value. cylinder.
For cementitious materials, the concentric (coaxial) cylinder is the most commonly used
system for rheological measurements, usually with some type of grooved or ribbed surface
on the inner or outer cylinder (or both). Also the vane type is commonly used for
cementitious materials. A well-known commercial apparatus using this system is the BML
rheometer for concrete. In the appended papers, the rheological measurements on mortars
and concretes were performed using a concentric system.
2.3.2 Rotational rheometer, cone-and-plate

The common feature of a cone-and-plate rheometer
is that the fluid is sheared between a flat plate and a Ω
cone with a low angle (see Figure 24). The cone-
and-plate system produces a flow in which the shear α
rate is very nearly uniform everywhere in the liquid,
provided that the gap angle (α) is small. Typically, R
this angle is not to be larger than 4º [13][15][80]. For
cementitious materials, the cone-and-plate system is
Figure 24. Principle of a cone-
seldom used, as the narrow gap close to the centre
and-plate rheometer.
will make the particles cause interference.
2.3.3 Rotational rheometer, parallel-plates

The rotating parallel-plates rheometer is similar to
the cone-and-plate system. The fluid is sheared Ω
between a stationary and a rotating flat plate (see
Figure 25). In this system the gap between the plates h
can be adjusted to fit the fluid, which is preferable
for particle suspensions. However, in contrast to the R
cone-and-plate system, the parallel plates do not
provide a shear rate that is uniform over the radius,
Figure 25. Principle of a rotating
which consequently makes it inappropriate for non-
rheometer with parallel-plates.
Newtonian fluids.

A well-known commercial apparatus using the rotating parallel-plates system is the

BTRHEOM rheometer for concrete.
2.3.4 Capillary-tube rheometer

In a capillary-tube rheometer (see Figure 26), the fluid is forced through a cylindrical
capillary tube with a smooth inner surface. The flow parameters have to be chosen in such
a way that the flow may be regarded as steady-state, isothermal, and laminar. The ratio of
the capillary length (L) to its inner radius is to be large so the end-effects occurring in the
entrance and exit regions of the capillary tube can be neglected. Knowing the dimensions
of the capillary tube (i.e., its inner diameter and length), one can determine the functional
dependence between the volumetric flow rate and the pressure drop (∆P) due to friction.
By applying various values of pressure drop (or flow rate), the flow curve of the fluid can
be determined.
The principle of a capillary-tube rheometer is based on the so called Hagen-Poiseuille
equation, valid for Newtonian fluids. Since the viscosity of a Newtonian fluid does not
vary with flow or shear, only one measurement at any flow velocity is needed. However,
for non-Newtonian fluids, it is more complicated as the viscosity may vary with flow
velocity (or shear rate). Consequently, one needs to vary the pressure in the reservoir in
order to change the shear rate, a time-consuming procedure. After each run, the pressure
should be reset to a new value to obtain the relation between flow rate and pressure drop.
∆P
2·R
Figure 26. Principle of capillary-tube rheometer.
2.4 Concluding remarks

Some concluding remarks concerning the rheology of fresh cementitious materials (paste,
mortar and concrete) can be made as follows:
The most important factors affecting the rheological properties are the water content,
and the particles’ specific surface area and packing. Other influential properties are the
particle size distribution, shape, and surface texture.
Cementitious materials are widely recognized to show a viscoplastic non-Newtonian
behaviour due to the complex balance of interparticle forces. The flow characteristic
mainly depends on concentration of particles and on the extent to which content
particles are flocculated. The particles cover a very broad size range, from micron-
sized cement and silica fume particles to centimetre-sized aggregates, but flocculation
is only important for the finer particles.
It is important to be aware of the time-dependent, reversible and irreversible,
phenomena that these materials show (e.g. thixotropy, hydration, mixing, adsorption),

and rheological tests are to be performed at steady shear (equilibrium conditions).

When evaluating the development of thixotropy over time, the irreversible part must be
measured and excluded from the reversible.
In order to determine the rheological properties of a non-Newtonian/viscoplastic fluid,
a multipoint flow curve has to be measured; hence a single point on the flow curve
does not describe this material completely. It is preferable to use a controlled
multipoint shear rate technique.
The Bingham model is the most frequently used, and probably the best suited, model to
describe the rheology of these types of materials. It is simple (with only two
parameters), and over a limited range of shear rates it is confirmed quite well. For
highly concentrated colloidal systems, such as cement paste with low w/c, the
Herschel-Bulkley model might be more suitable.
The slump flow spread and T50 time are not a unique function of yield stress and
viscosity respectively, but rather a more complex function of both where neither yield
stress nor viscosity can be neglected. The spread has proved to be more closely
connected with the yield stress than the viscosity (~3 times), especially at high
viscosity, whereas the T50 time was connected more equally with yield stress and
viscosity.

Chapter 3 – Early-age deformation
3 EARLY-AGE DEFORMATION
3.1 Introduction
When a porous body loses water to the ambience, contraction will take place. For
cementitious materials there will also be an additional shrinkage caused by the chemical
reactions (hydration, carbonation, etc.). Since the rigidity, as well as the effect of different
chemical reactions, changes with time, it is convenient to distinguish between early-age
and long-term behaviour, where early age is limited to 24 hours from mixing and long-
term refers to the time beyond. However, there is not a well-defined and distinct transition
but rather a continuous transformation from a plastic to a rigid state. Shrinkage of a
cementitious material will start as soon water is added, due to the chemical reaction and
also due to the loss of water by evaporation (if not prevented). In the initial fresh state,
when the concrete is still a fluid, the volumetric shrinkage will, fully or partly, result in a
vertical displacement (settlement) [81][82]. This deformation does not result in any
stresses and is often ignored in the design of concrete structures, since it is considered to be
less than the subsequent deformations or is considered not important. Moreover, in the
fresh state, shrinkage measurements are difficult to perform without involving the effect of
gravity (bleeding, segregation, etc.) which, in addition, is not isotropic.
Yet in order to elucidate the mechanism of early-age deformations, and in view of the fact
that they are greatest up to an age of 12 hours, these deformations should be investigated
and may have to be taken into account. The governing mechanisms of the total shrinkage,
distinguishing between early age and long term, are illustrated in Figure 27. It ought to be
noted that there are also structural and environmental factors that simultaneously can cause
expansions, e.g. alkali silica reactions, delayed ettringite formation, expansive cements,
sulphate attack, thermal changes and reabsorption of water. There is generally an interplay
between the mechanisms of contraction and expansion, but often the contracting part is
predominant. However, the mechanisms of expansion have not been considered in this
work. Neither are the long-term deformations further explored.
Total shrinkage
Early age (<24 hours) shrinkage Long term (>24 hours) shrinkage
Plastic shrinkage Thermal dilatation Drying shrinkage
Autogenous shrinkage Evaporation External absorption Carbonation shrinkage
Chemical shrinkage Hydration
Figure 27. Illustration of the driving mechanisms of the total shrinkage, not considering
the mechanisms of expansion, or including the structural restrain.

Shrinkage, especially at early age, has become of great concern, due to recurrent problems
with cracking in concrete structures. Conditions such as reduced maximum aggregate size,
increased amount of fines, presence of retarding admixtures, increased binder content, and
deficient covering and curing all contribute to these problems. In recent research there has
been a growing interest in the area of autogenous and plastic shrinkage, as well as how to
control and counteract the early-age shrinkage. A “hot topic” today is e.g. the use of
superabsorbent polymer for internal curing [83]-[88].
There are two main driving forces for early-age shrinkage [81]: (1) evaporation shrinkage
(or early-age drying shrinkage) due to loss of water from the fresh concrete, and (2)
shrinkage due to hydration and chemical reactions producing autogenous shrinkage. Yet
under sealed conditions, if evaporation is prevented, the early-age shrinkage is a result of
the autogenous shrinkage. However, temperature dilation may also contribute (e.g. when
cooling the surface), as well as the external suction of water (absorption) by the formwork
material or by the sub-base. Accordingly, cracking in the initial phase is a product of
several factors. Thus, it is important to separate the mechanisms into those that are
dependent on environmental conditions (e.g. evaporation of water from the surface) and
those that occur without moisture transfer to the ambient and which are associated with the
autogenous deformation of the material.
During the early age, here defined as the firs 24 1. Plastic

hours from mixing, the concrete undergoes three Water
more or less distinct structural phases [89]-[91]:
Cement grains
1. Plastic: a liquid state where the concrete is
2. Semiplastic
plastic with viscoelastic behaviour, and is still
workable. Solid grains
(aggregate/filler)
2. Semiplastic: after initial setting, the concrete
will undergo a transition stage of early
stiffening from fluidity to rigidity, where a 3. Rigid
self-supporting skeleton starts to form. Solid hydrates
3. Rigid: at the final hardening stage, initiated
Gas voids/pores
by the point of final setting, the concrete’s
strength starts to develop from the continuing
hydration. Figure 28. Illustration of
structural development.
The term “plastic shrinkage” refers to the periods (1 and 2) until the point of final set
[22][23][89]. However, neither the initial nor the final set is a distinct and well-defined
physical state, but merely a gradual change of structure due to hydration. The points of
setting are often arbitrarily chosen, referring to measures from empirical methods. As the
point of final set is arbitrarily determined, so is the period of plastic shrinkage. However,
this period is often simply given a general time (e.g. 12 or 24 hours). Commonly used
methods for determination of setting (initial and final) are the Vicat needle method (EN
196-3) and the penetration resistance method (ASTM C403). There are also ultrasonic
techniques proposed for better prediction of setting time [92]-[94].

3.2 Plastic shrinkage cracking

Plastic shrinkage cracking is not a physical deformation, but an effect of a rather complex
sequence of overlapping deformation mechanisms. The main underlying mechanisms for
early-age deformation follow this section.
Plastic shrinkage is defined in the literature as the shrinkage of fresh concrete, exposed to
drying, that takes place during the time to final set, while the concrete is “plastic” [23]. The
duration is usually short and ends when the concrete has reached its final set. If the
shrinkage is non-uniform, or if there is restraint, tensile stresses develops which may result
in cracking as the concrete has a poorly developed tensile strength and strain [95]; see
Figure 29. These cracks are usually referred to as “plastic shrinkage cracks”. The prevalent
theory is that plastic shrinkage is directly caused by evaporation of water from the concrete
surface; i.e. if the amount of water lost to the ambient exceeds the amount of water brought
to the surface by bleeding, and if it is large, plastic shrinkage cracking may occur [22][23].
Care is to be taken to protect the surface against drying, although experience in the use of
concretes with low w/c, or with silica added, has revealed that severe cracking may occur
in spite of proper protection (curing membrane, plastic sheets, water spray, etc.), testifying
to a large autogenous shrinkage [10][96]. Hence, most likely the cracking caused by plastic
shrinkage is also a result of the autogenous shrinkage and thermal dilatation. Moreover, it
can be difficult to distinguish between the plastic shrinkage cracks and cracks caused by
thermal dilation, vertical displacement (settlement), early-age evaporation or autogenous
shrinkage. Generally, cracks due to autogenous shrinkage develop uniformly through the
concrete member, whereas cracks from evaporation are initiated at the outside surface and
progress inward. For concretes where the paste generates a large chemical shrinkage (e.g.
low w/c, addition of silica fume), the autogenous part of the plastic shrinkage can be
significant, whereas when the chemical shrinkage is small (e.g. high w/c) the shrinkage due
to evaporation tends to be predominant [91].
The environmental factors that promote early- 10,000

Tensile strain at failure, εtu, [10-6 m/m]
age cracks are wind speed, air temperature,

solar radiation and the relative humidity. These
factors, together with the temperature of the 1,000
concrete, govern the rate of evaporation from
the concrete (see section 3.3.6). It is generally
suggested that if the evaporation exceeds 1.0
kg/m2/h there is a significant risk of cracking, 100
but cracks may occur also at evaporation rates
lower than 0.5 kg/m2/h. Moreover, for low w/c
or w/b concretes cracking may develop in spite
10
of proper protection. It has therefore been
1 10 100
suggested that if the early-age shrinkage Age [hours] at 20ºC
magnitude exceeds 1000 µm/m, there is a high
risk of cracking [97][98]. This corresponds well Figure 29. Relationship between
to the American Concrete Institute guidelines tensile strain capacity and age of
(ACI 209-92) where it is stated that cracks may concrete, based on Kasai et al. [95].
occur for shrinkage of about 400–1000 µm/m.
Moreover, this seems to be consistent with the
actual tensile strain capacity of the concrete
when cracking usually occurs; see Figure 29.

3.3 Mechanisms of early-age deformation

3.3.1 Hydration and development of microstructure
The hydration of Portland cement is a complex sequence of overlapping chemical reactions
between clinker components, calcium sulphate and water, leading to setting and hardening.
The process that occur can be divided in five stages as follows [22][26]; see Figure 30. As
soon as C3S (in the cement) and water come in contact, reactions start to occur, releasing
calcium and hydroxyl ions into the solution, generating an outburst of heat (Stage I). After
this initial stage an induction period (or dormant period) is entered (Stage II), where the
dissolution continues and pH reaches a high value (~12.5). During this induction period
not much hydration takes place, but this does not mean that the paste is “dormant” with
respect to volume changes. After a certain critical value of calcium and hydroxide ions is
reached, there is a rapid crystallization of CH (calcium hydroxide) and C-S-H (calcium
silicate hydrate) followed by a rapid reaction (Stage III). In this acceleration stage there is
an onset of transformation to rigidity, with the initial set somewhat after the transition from
Stage II while the final set occurs just before the peak between Stages III and IV. In the
following stages (IV and V), there is a continuous formation of hydration products, yet the
rate of reaction is slowing down. In the final stage (V) there is only a slow formation of
products and the reaction is diffusion-controlled.
The degree of hydration refers to the amount of cement reacted relative to the total amount
of cement. To obtain full hydration in a closed cement-paste system, the water and space
needed corresponds to a w/c ratio of 0.42 [100]. However, this level can vary from 0.36 to
0.48, depending on cement type [8]. At lower w/c ratio, hydration stops due to lack of
water and the remaining cement will be unhydrated. E.g. at w/c 0.21 only 50% of the
cement will be fully hydrated [4]. However, if water is allowed to penetrate into an open
system of hardening cement paste, the w/c ratio for full hydration is reduced to
approximately 0.36.
Dissolution:
Rate of heat evolution
Final set
ettringite formation
Rapid formation Diffusion-controlled
of C-S-H and CH reactions
Induction period: Formation of
increase in Ca2+ monosulfate
concentration
Initial set
I II III IV V
~10 minutes ~4 hours ~12 hours ~24 hours Time of hydration
~2% ~15% ~30% Degree of hydration
Figure 30. Schematic representation of heat evolution during hydration of cement and
water, based on Gartner et al. [101].
In Figure 31, the products associated with the stages of cement hydration and the change
of porosity and permeability can be seen. The setting process is the consequence of a
change from a concentrated suspension of flocculated particles to a viscoelastic skeletal
solid capable of supporting an applied stress; see Figure 32. Setting is controlled primarily
by the hydration of C3S and occurs when the induction period is terminated by a rapid
hydration of C3S leading to a fast temperature rise of the concrete (Stage III) [22].

As the hydration proceeds, capillary C-S-H

pores are gradually emptied and (short fibres)
hydration products progressively fill
the void spaces in the cement paste. Porosity CH
As the pores will be smaller, or Permeability
consumed, the total volume of pores
C-S-H (long fibres)
(porosity) will decrease. This leads C4(AF)H13
Ettringite
to decreased permeability and to
increased strength and durability of Monosulphate
the cement paste [90]. The pores in
the paste are typically in the size 0 5 30 1 2 6 1 2 7 28 90
range of 2·10-9 to 1·10-5 metre, minutes hours days
where the smallest are distinguished Time of hydration
as gel pores and the larger as I & II III & IV V
capillary pores [99]. Larger pores
are associated with air voids. Figure 31. Products associated with the stages
of hydration, based on Locher et al. [102].
However, not only the w/c ratio will influence the hydration, but also a number of
parameters such as: the composition and fineness of the cement (the main clinker
components); addition of supplementary materials (such as fly ash and silica); admixtures
(super plasticizer, accelerator, retarder, etc.); and the temperature.
Concentrated suspension Formation of a layer of Nucleation and early Rapid formation of ‘C-S-H’
of flocculated particles ettringite or ‘AFt’ and formation of ‘C-S-H’. leading to solidification and
‘CH’. Possible particle Continued formation of creation of capillary pores
agglomeration ‘AFt’. Particle agglomeration
cement
water
AFt and CH Outer C-S-H AFt

C-S-H needles
Gel Outer C-S-H
First minutes (Stage I): Induction period (Stage II): Acceleration period (Stage III):
wetting and mixing agitation, transport, placing, setting and early hardening
and finishing
Figure 32. Schematic representation of the early microstructural development [91].
3.3.2 Chemical shrinkage

In the literature, chemical shrinkage is also referred to as Le Chatelier contraction, named
after the French scientist who in 1900 first observed the phenomenon [90]. Chemical
shrinkage is the result of the reactions between cement and water, which lead to a volume
reduction; the reactions of reactive fillers (pozzolanic) are also considered. The basic
principle of chemical shrinkage is that the volume occupied by the hydration products is
less than the sum of the volumes of the constituents (cement, pozzolan and water) before
hydration [82]. According to Powers & Brownyard [100], when water reacts with the

cement ~25% of its initial volume is lost, and 1 gram of cement will consume 0.23-0.25
grams of water when fully hydrated. Hence, the chemical shrinkage amounts ~6 ml per 100
gram of cement reacted.
The basic reactions of cement clinker are generally defined by four reactions of C3S, C2S,
C3A and C4AF. Each of these reactions requires water, is exothermic, and results in a
different decreased volume of the reaction products [97]. The contribution from each of
these four phases to the chemical shrinkage is given in Table 5.
Chemical shrinkage is a microscopic internal volume

reduction, not considering the air in the capillary Table 5. Approximate
pores (porosity) [82]. At the stage where the paste is chemical shrinkage for the
liquid-like, without a restraining skeleton and empty individual reacted phases in
pores, the chemical shrinkage will be equal to the cement [89][103].
external bulk deformation [103][104]. However, at the Vcs
stage when the self-supporting skeleton of hydration [ml/100g]
products starts to form (initial set) the external and
C3A 17.85
internal chemical shrinkage will diverge, since the
C4AF 11.13
rigidity of the paste restrains the volume change [90].
C3S 5.32
This external deformation (for a sealed system) is
C2S 4.00
referred to as autogenous shrinkage (see Figure 33).
I. Placing/casting
Chemical
shrinkage
Chemical
II. Initial set shrinkage
Shrinkage
Empty pores
Chemical
III. Hardening
shrinkage
Initial set
Autogenous shrinkage Autogenous
shrinkage
Time Hydration products Cement Water Empty pores
I. II. III.
Figure 33. Principle of autogenous and chemical shrinkage for a cement paste under
sealed conditions.
As mentioned, the chemical shrinkage begins immediately when mixing cement and water
and the rate of shrinkage is highest during the first hours. Chemical shrinkage is suggested
to be almost linearly proportional to the degree of hydration (except for the very initial
hydration) [105][106]. It has also been shown that the chemical shrinkage correlates
linearly with the strength development, once the paste has set [107]. Factors such as
temperature, w/c, cement fineness, C3A and C4AF content, and the efficiency of cement
dispersion will have a significant effect on the rate [23]. Also additives such as chemical
and mineral admixtures and pozzolans will influence the chemical shrinkage [22].

3.3.3 Autogenous shrinkage

Autogenous shrinkage was first described by Lyman in 1934 [112] as a factor contributing
to the total shrinkage, yet difficult to access. Davis [113] reported in 1940 measurements of
autogenous shrinkage in the range 50-100 µm/m after 5 years of hardening. Compared
with the thermal deformations and drying shrinkage this was considered to be relatively
small, which is why historically little attention has been paid to the autogenous shrinkage
[114]. However, many concretes today tends to develop a substantial autogenous
shrinkage, due to the usage of chemical admixtures, low w/c, and high content of binder
and filler material (e.g. high strength and self-compacting concrete).
Autogenous deformation may be defined as the unrestrained external bulk deformation
taking place under isothermal and sealed conditions [104][108]., in other words with (1) no
external forces or restraint acting on the material, (2) no exchange of matter with the
surroundings (e.g. no evaporation), and (3) no variation in the temperature.
In the literature, a large number of terms for autogenous shrinkage can be found, such as:
bulk shrinkage, external volume change, total or external chemical shrinkage, hydration
shrinkage, and self-desiccation shrinkage [89][104][109]. The deformation may be either a
shrinkage or an expansion (in length or volume). In this work, shrinkage is defined as a
negative strain and expansion as a positive strain. Mostly, autogenous deformation is
shrinkage, but any re-absorption of bleed water and/or absorbed water in the aggregates, as
well as some early chemical reactions (e.g. ettringite formation), may cause an autogenous
swelling [110].
The autogenous shrinkage originates from the chemical shrinkage, though it also involves
the effect of the internal restraining structure and the contracting empty capillary pores.
Whether the macroscopic bleeding (and re-absorption) is to be taken in account, or whether
it only concerns homogeneous materials, is not clear [104].
As long as the concrete is fluid, autogenous shrinkage is considered to be equal to the
chemical shrinkage. But once the self-supporting skeleton starts to form, the autogenous
will diverge from the chemical [81][103][108][114][115]. Autogenous shrinkage before
setting is not necessarily isotropic. It may be converted, fully or partly, to a vertical
displacement. In a horizontal beam or slab, these volume changes will show up as vertical
settlement without any linear horizontal deformation [105][116]. This part of the
autogenous shrinkage is therefore sometimes referred to as setting shrinkage [111].
However, at the stage where the concrete starts to behave like a visco-elastic material, with
a rigid self-supporting skeleton, the deformation of the specimen will become isotropic,
and a linear contraction can be observed [81][103][117]. From being equal, the rate of
autogenous shrinkage will be approximately 1/10 of the rate of chemical shrinkage [110].
There is no general agreement on whether the autogenous deformation is to be referred to
the full period of hardening starting from water addition [117][118] or to the period in
solid state from the time where a structure starts to form i.e. initial or final set. The latter
point of set is sometimes referred to as the time zero (t0) [119]-[122]. Neither is there
general agreement on how to define or measure the point of set. However, as this point is
not a well-defined physical state but rather a continuous transformation from a liquid to a
solid state [104], and as the shrinkage is highest up to an age of 12 hours [118], it is
suggested that autogenous measurement is to be started as soon as possible after mixing.
Moreover, autogenous deformation refers to the deformation under autogenous conditions
(unstrained, sealed and isothermal), and does not refer to whether the system has set or not
[104]. In literature the reported magnitude of autogenous deformation varies enormously,

which reflects the difficulties in the interpretation of the results based on different
techniques [81][111][123].
The pattern of autogenous deformation, exemplified in Figure 34, comprises three distinct
stages which can be defined as: (1) plastic, (2) semiplastic and (3) rigid, separated by the
time to initial and final set [91]. In literature, other terms for these stages can be found, e.g.
liquid / skeleton formation / hardening [89]. Also the four stages: initial / induction /
acceleration / deacceleration, connected with the chemical reactions, can be found [125]. It
has been suggested [81] that, when measuring the autogenous shrinkage, the setting (initial
and final) will be manifested as a change of the slope of the deformation. Initially the
autogenous shrinkage originates from the chemical shrinkage, whereas once the concrete
sets the development of a contracting capillary pore pressure will contribute to the
subsequent deformation (see Figure 34) [116].
Plastic Semiplastic Rigid
Self-supporting skeleton starts to form

Deformation, Pressure & Temp
Initial set
Final set
Pore pressure (measured)
Autogenous deformation (measured)
Temperature (measured)
Chemical shrinkage (assumed)

0 ~6 ~12 ~18 ~24
Time (from mix) [hours]
Figure 34. Illustration of early-age autogenous deformation and the corresponding

development of temperature, capillary pore pressure (based on measurements of a SCC
with w/c 0.45, from [91]).
There are numerous factors which have an impact on the autogenous shrinkage. Factors
increasing the chemical shrinkage need not cause a larger autogenous shrinkage, since
some of these will shorten the time to set and/or generate a more rigid restraining structure.
E.g. the effect of cement fineness, content of C3A and C4AF, and temperature is not a
matter of course. In addition to the chemical shrinkage, the autogenous shrinkage will be
influenced by the internal restraint from aggregates. However, when the rate of chemical
shrinkage is high, so is the rate of autogenous shrinkage, especially at early age. The
autogenous shrinkage tends to increase with [23][91]:
o high binder content,
o low w/c
o low content of aggregate (especially the coarse fraction),
o addition of silica, and
o presence of chemical admixtures with a retarding effect.
The autogenous shrinkage may also be reduced by addition of accelerator, shrinkage-
reducing admixture, or internal curing (saturated aggregates, superabsorbent polymer). The
effect of different mix designs on the autogenous deformation is exemplified in Figure 35.

0 6 12 18 24 0 6 12 18 24 0 6 12 18 24
Autogenous deformation [10 m/m]
0 0 0

w/c 0.67 50% (8-16)
-6
-6
-6
w/c 0.55 -200 40% (8-16)
-400 0% Silica -200
5% Silica 30% (8-16)
-400 10% Silica 20% (8-16)
-800 -400
w/c 0.45 -600
w/c 0.38
-1 200 -800 -600

Time [hours] Time [hours] Time [hours]
(a) (b) (c)

0 6 12 18 24 0 6 12 18 24 0 6 12 18 24
0 0 0

0.6% SP Accelerator
-6
-6
2% SRA
-6
Ref.
0.8% SP -200
-200 -200 1% SRA Retarder
1.0% SP 0% SRA
-400
-400 -400
-600
-600 -600 -800

(d) (e) (f)

Figure 35. Measures of autogenous deformation on SCC (from [124]) and the effect of (a)
w/c, (b) silica, (c) content of coarse aggregate of total aggregate, (d) superplasticizer
dosage, (e) shrinkage-reducing admixture, and (f) accelerator and retarder.
3.3.4 Capillary pore pressure

When a concrete dries out due to qev Air
evaporation, if the rate of evaporation Pa
exceeds the rate of free internal water γ γ
transported to the surface, the Particle
concrete surface will dry out. This Pw
leads to the formation of numerous Water
water menisci (with a curved surface) Figure 36. Illustration of the formation of
between the particles near the menisci between particles near the surface
surface; see Figure 36. due to evaporation.
Since the fluid pressure is less on the convex side of a meniscus than on the concave side,
the creation of water menisci results in a negative pressure in the pore water and
contraction forces between particles [4]. Consequently, the average distance between the
particles tends to be reduced and the paste contracts [9]. These contracting capillary forces
are in inverse ratio to the meniscus radius, and hence the capillary tension stresses increase
with decreasing pore sizes and interparticle spaces (e.g. with low w/c, high cement

fineness, additions of fines, etc.). For a concrete where evaporation is prevented, a negative
capillary pressure will also start to develop, but only once the hydration commences and
the concrete sets [89]. As a solid skeleton starts to form the chemical shrinkage is not
totally transformed into external volume change and, if the water supply is restricted,
empty pores will be formed inside the paste, and contracting water meniscus are created
(see Figure 33 and Figure 34). At the stage where the concrete starts to set (initial set) both
the capillary pore pressure and the temperature reaches an accelerating phase (see Figure
34 and Figure 37), which indicates that the dormant period is ended and that the cement
hydration accelerates [91]. Initially (before setting), when the concrete is liquid-like,
without restraining skeleton and empty pores, the pore pressure is zero [116]. According to
Wittman [9] the action of capillary pore pressure the cause of plastic shrinkage.
Typical development of pore pressure is shown in Figure 37. As can be seen, the pore
pressure develops more rapidly in an evaporating concrete than in a sealed one. The
accelerating phase of pore pressure starts at 5-6 hours from mixing for a sealed concrete,
whereas for an evaporating one it accelerates at 3-4 hours [91]. It can also be noted (in
Figure 37) that the initial cracking, due to plastic shrinkage, which coincides with the
accelerating phase of the pore pressure (3-4 hours from mixing). Furthermore, a pressure
close to the exposed surface is ahead of a lower pressure. However, for SCC’s with a high
w/c (>0.55) these differences are smaller, and for standard concrete the pressure at the
different distances from the surface will develop almost equally in time [91]. This can be
explained by the concrete’s ability to transport water to the surface in relation to the
evaporation [116]. Thus, for a denser and less permeable matrix the internal transport of
water to the area close to the surface, having a larger capillary tension (due to evaporation),
will be restricted. Whereas for a more porous and permeable matrix the balancing of the
differences in pore pressure, and the transport water to the surface, will be faster and the
pressure will be more uniform through the section.
Max Max
Temp.
Pore Pore pressure (low)

pressure
Pore pressure (high)
Initial set
Evaporation
Autogenous
deformation Temperature
Strain
Final set
Initial crack
Min Min
0 5 10 15 20 0 5 10 15 20
Time (from mix) [hour] Time (from mix) [hour]
Figure 37. Typical measurementss of pore pressure and temperature development, for a
SCC with w/c 0.55. To the left, pore pressure and temperature together with the
autogenous deformation, and to the right with the strain and evaporation (ring test). The
axes have been normalized against maximum and minimum values.
The capillary pore pressure (Pc) that is generated can be described by the Gauss-Laplace’s
equation (Eq. 19) which relates the pressure to the capillary radius, and by the Kelvin’s
equation (Eq. 20), which relate the pressure to the relative humidity (RH). The capillary
pore pressure is, by definition, the differences between the pressures in the fluid that lies

on the concave side of the surface (in this case the air pressure, Pa) and in the other fluid
(in this case the water pressure, Pw) [116]; see Figure 36.
2 ⋅γ w ⎛1 1⎞
Pc = Pa − Pw = − = −γ w ⎜⎜ + ⎟⎟ [Pa] (Eq. 19)
r ⎝ r1 r2 ⎠
2 ⋅γ w ⋅ M w 2 ⋅γ w ⋅ M w ⎛ 1 1 ⎞
ln(RH ) = − =− ⋅⎜ + ⎟⎟ [-] (Eq. 20)
ρw ⋅ R ⋅T ⋅ r ρ w R ⋅ T ⎜⎝ r1 r2 ⎠
where γw is the surface tension of the capillary water (~0.074 N/m); r is the mean curvature
of the surface; r1 and r2 are the principal radii of curvature in metre (see Figure 39, R is the
ideal gas constant (8.314 J/mol K); T is the absolute temperature in Kelvin (20°C≈293K);
Mw is the molar mass of water (~0.018 kg/mol); and ρw is the density of water. By
combining the two equations, and setting Pa equal to zero (= atmospheric pressure) and r1
equal to r2, the following relationship is obtained:
ρw ⋅ R ⋅T
Pc = ⋅ ln(RH ) [Pa] (Eq. 21)
Mw
This equation (Eq. 21) shows that a small 1 000 000
reduction in RH will lead to very large Capillary pore pressure [kPa]
100 000
capillary pressure; see Figure 38. Yet, the
pressure can only develop if there are partly 10 000
empty pores available in the system. Once 1 000
the matrix sets and the pores lose their
100
internal water (by hydration, evaporation,
etc.) the pores loses their internal water, 10
starting with the largest pores, and RH will 1
start to drop [100]. In addition, the 0 0.5 1
dissolution of salts into the pore water will Relative humidity, RH [-]
increase the alkalinity (i.e. concentration of
OH- ions, mainly from KOH and NaOH) and Figure 38. Relation between RH and
consequently reduce the RH. This reduction capillary pore pressure (at 20°C),
will be 1-3%, depending on the cement based on the Kelvin equation. Note,
composition and w/c ratio [126]. pressure is negative and logarithmic.
Based on the assumption that the capillary pores in the paste are typically in the size range
of 0.01 to 5 µm [90], the pore pressure calculated with Kelvin’s equation (Eq. 20) will
roughly be in the rage of -10 kPa and -10 MPa. If the gel pores, down to 2 nm [99], were
included, the pore pressure would theoretically be as low as -100 MPa.
r1
r1
r2 r1 r2 r*2 r*2
r1
∆Pc
Figure 39. Schematic representation of liquid filled joint between two spherical particles
at the surface.

According to Powers [4] the maximum negative capillary pore pressure, Pc,max, developed
in a cement paste mixture is indirectly proportional to the w/c:
γw ⋅S
Pc ,max = −1 ⋅ 10 3 ⋅ [Pa] (Eq. 22)
wc
where S is the mass specific surface area of the cement [m2/kg] measured with Blaine.
Assuming S = 350 m2/kg, and w/c ratio 0.55, the capillary pressure calculated with
equation (Eq. 22) will be -45 kPa, in a fully hydrated cement paste. However, this is not
near the theoretical lower limit of -100 MPa [128] in the smallest pores in the gel.
Many factors have an impact on the pore pressure development, related to the evaporation
as well as to the hydration. That the rate of hydration (apart from the rate of evaporation)
plays an important role for how the capillary pressure develops is shown in Figure 40,
where concretes with accelerator and retarder, and with different superplasticizer dosage,
change the time of the pressure drop. It should be noted that the time to, and magnitude of,
maximum underpressure are often not possible to evaluate, due to a collapse (loss) of
measured pressure at random times. This effect is usually referred to as the breakthrough
pressure [9][116], and is the effect of air penetrating the pressure transducer, as the
surrounding water menisci cannot find stable positions in the region adjacent to the
measuring point.
0 0 0
Pore pressure [kPa] -20

Pore pressure [kPa]
Pore pressure [kPa]
-20 -10
Accelerator -40
-40 Ref. -20 1.0% SP
-60
0.6% SP
Retarder
-60 -30 -80 Evaporating
0.8% SP Sealed
-100
-80 -40
0 2 4 6 8
0 2 4 6 8 0 2 4 6 8
Time (from mix) [hours] Time (from mix) [hours] Time (from mix) [hours]
(a) (b) (c)

Figure 40. Measurements of capillary pore pressure on SCC with w/c 0.67 (from [91]),
and the effect of (a) accelerator and retarder, (b) superplasticizer dosage, and (c) being
sealed/unsealed.
3.3.5 Disjoining pressure

Water will be adsorbed in the narrow spaces
and on the particles and the C-S-H surfaces at Pd
all relative humidities. The thickness of the Menisci
adsorbed water film increases with an
increasing RH. In locations where the distance
between two particles/surfaces is hindered, the Hindered adsorption
adsorption of water molecules may induce
pressure and cause expansion (see Figure 41). Figure 41. Illustration of disjoining
pressure

This pressure, called disjoining pressure, will rise with an increase in RH of the system and
lead to an expansion. Consequently, when the system dries out and RH is reduced the
particles will contract [129][130]. The disjointing pressure concerns aggregations in which
the smallest interparticle distance is much smaller than the particles [4], and is active in the
area of hindered absorption where the distances between the surfaces are smaller than two
times the thickness of free adsorbed water layer (~20Å at 100%) [22] [130]. The
disjointing pressure develops steady in the range between 100% and around 40% [131],
and shows an RH dependency similar to the capillary stress. It increases with increasing
thickness of the adsorbed water between the particles (i.e. increased RH) until it exceeds
the van der Waals’ attraction, when the particles will be forced apart. Therefore, on first
drying and lowered RH, the decreasing disjoining will case the particles to be drawn
together by the van der Waals’ forces, and there will be net volume shrinkage [22].
However, there is not a general agreement that the disjointing pressure has a significant
influence on the autogenous shrinkage of cementitious materials [125].
3.3.6 Evaporation shrinkage

The evaporation shrinkage (or “early-age drying shrinkage”) referees to the volume
reduction due to the loss of water to the surroundings, without involving the autogenous
shrinkage. Although it is not included, the effects are the same as the shrinkage caused by
external suction of water (absorption) by the formwork material or by the sub-base. At the
initial stage where the concrete is liquid-like, without a restraining skeleton and empty
pore, the loss of water due to evaporation will be equal to an external bulk volume
reduction, and fairly constant. Moreover, the evaporation is close to the evaporation from a
free water surface, yet dependent on the rate of bleeding. However, for SCC and other high
performance concretes, containing a large quantity of fines (and binders), the ability to
bleed is restricted.
Once the concrete sets the transport properties changes and slow down the evaporation.
During the drying, the larger pores are the first ones to lose their internal water [127].
Moreover, due to the contraction and the development of hydration products the pores will
be smaller, or consumed, and the total volume of pores (porosity) will decrease, and so will
the permeability [89]. This effect is illustrated in Figure 42 where the effect of w/c on the
evaporation is shown.
Parallels can be drawn to the development of autogenous deformation, but instead of the
internal consumption of water and chemical shrinkage, the water is externally lost by
evaporation. However, the evaporation also has a cooling effect by water transforming to
vapour (“evaporate cooling”) which lowers the concrete’s temperature near the surface
(depending on the temperatures, vapour pressure, evaporation, etc.). When comparing the
temperature development in sealed concrete specimens with evaporation, a difference of
approximately 2-5°C can observed during the first hours from mixing (see Figure 43) [91].

4 30
Water Sealed
Concrete temperature [C°]

w/c 0.67
3
Evaporation [kg/m ]
2
25
w/c 0.55
2
w/c 0.45 20
1 w/c 0.38
Evaporatin
0 15
0 6 12 18 24 0 5 10 15 20
Time [hours] Time (from mix) [hour]
Figure 42. Example of evaporation from Figure 43. Temperature development for
SCC with w/c from 0.38 to 0.67, exposed to a sealed SCC (w/c 0.55) exposed to air
air with 4.5 m/s, 35% RH and 23°C. at 4.5 m/s, 35% RH and 23°C [91].
The concrete’s surface temperature and its

ability to transport water to the surface in
early age are dependent on a rather complex
sequence of interconnecting mechanisms
changing with time, and are not often
considered. Neither are the concrete’s
surface texture and the geometry of the
pores at the surface considered [116].
Normally, and for practical reasons, it is the
environmental factors (air velocity, air
temperature and RH) and the concrete
temperature that generally are used to
evaluate the evaporation in early age
(Figure 44). In addition, recommended Figure 44. Commonly used “tool” to
limits of evaporation rate are sometimes estimate the rate of evaporation from the
given (see section 3.2) in order to lower the concrete surface at early age (ACI 305).
risk of plastic shrinkage cracking.
3.4 Measuring techniques and methods

3.4.1 General
Only the basic techniques and general methods for evaluating the unrestrained
deformations at early age are described here. An overview is given of some methods and
principles for measuring:
1. Chemical shrinkage
2. Autogenous shrinkage
3. Plastic shrinkage
Methods limited to measurement in the hardened state, i.e. only to be conducted after
setting or demoulding, have not been considered. Nor have the restrained shrinkage test
methods (e.g. ring tests, plate tests, longitudinal tests etc.), or the methods associated with
deformations due to temperature dilation. An inventory of testing techniques and

methodologies of restraint shrinkage and early-age cracking can be found in TC 181-EAS

(RILEM report 25), and in an article by Bentur & Kovler [132]. Moreover, the restraint
shrinkage test methods can not measure prior setting, as the sample must have a certain
strain capacity in order to be externally restraint.
The shrinkage due to evaporation cannot be measured alone, since shrinkage
measurements on cementitious material will involve the chemical shrinkage from
hydration. However, at the initial stage where the concrete is liquid-like, without a
restraining skeleton and empty pores, the lost volume of water due to evaporation will be
equal to an external bulk volume reduction (manifested as a vertical displacement).
Moreover, the evaporation shrinkage, as well as the plastic shrinkage, is only relative as it
strongly depends on a number of factors related to the sample’s geometry and
environmental conditions. A possible method to evaluate the evaporation shrinkage could
be to use the differences between measured plastic and autogenous shrinkage, together
with measurements of the settlement.
There are a large number of proposed methods for determining the early-age unstrained
deformation. Yet, no standardized methods are available, except for the chemical shrinkage
of cement paste (e.g. ASTM C1608). However, a new standard test method for autogenous
linear deformation (strain) of cement paste and mortar is proposed as an ASTM standard
(C157/C157M). This method, presented by Jensen & Hansen [133], uses a corrugated
mould system, developed in order to start measurement when the mortar (or paste) is fresh.
To measure the deformation in early age is a sensitive task, and many of the methods
suffer from large disadvantages and errors. Moreover, in early age the deformation is often
dependent on a rather complex sequence of interconnecting mechanisms, changing with
time. In literature the reported magnitude of early-age deformation varies enormously,
which reflects the difficulties in the interpretation of the results based on different
techniques and methods [81][111][123]. Moreover, these differences are promoted by the
fact that there is no general agreement on when to start measuring or how to define or
verify this starting point. This has been pointed out in section 3.3.3.
The methods can be divided, by their principal measuring techniques, into (1) linear
deformation measurements and (2) volumetric deformation measurements [81][104]. Both
kinds of methods ought in theory to give analogous results. However, even under carefully
controlled conditions, volumetric measurements can yield up to 5 times higher results than
the linear techniques [81][104]. In the literature, there is no general agreement clarifying
this problem [123].
3.4.2 Chemical shrinkage measurement

Chemical shrinkage is a microscopic internal (absolute) volume reduction, not considering
the air in the capillary pores (porosity) [82]. Hence, only volumetric measurements can be
applied. Water must be allowed to fully penetrate into the material, preventing any pores
from being emptied, so the thickness of the sample must be relatively small (maximum
t=10 mm [134]). If the specimen is too thick, intrusion of water (on which the
measurement is based) will be worsened and measurement faults appear [135]. However,
for more diluted cement pastes, larger samples can be used [136]. The chemical shrinkage
is directly proportional to the volume of water that the cement paste will absorb during its
hydration [137]. The shrinkage can be measured in two fundamentally different ways: by
dilatometry or by reduced buoyancy [89]. Both methods include an external water source

in contact with the cement paste sample. Bovin et al. [106] have shown that there is a high
correlation between the two ways of measuring.
The dilatometric method was initially developed by Le Chatelier [138] . This method
consists of immersing a given mass of cement paste in a glass flask, e.g. of “Erlenmeyer
flask” type, filled with water and surmounted by a graduated capillary tube (see Figure
45). The flask is to be placed in a thermostable bath at constant temperature (usually at
20°C). The decrease in volume of water, gradually consumed by the hydration reaction, is
manually read on the capillary tube at regular intervals [139].
The buoyancy method is based on the same principles as the dilatometric method, but
instead of following the volume of consumed water directly, the sample’s reduced
buoyancy is recorded (see Figure 45). Based on Archimedes’ principle, the water
submerged sample will register a volume reduction by weight [106][136][140][141]. An
advantage of this method is that the reading can be logged.
Thermo stable bath
0.001 g Balance
Graded tube
Plug Cup
Flask Membrane (oil)
Water Water
t Cement paste Cement paste
Dilatometry Reduced buoyancy
Figure 45. Principles of measuring techniques, by dilatometry or by reduced buoyancy, for

chemical shrinkage of cement paste.
3.4.3 Autogenous shrinkage measurement

Methods for autogenous shrinkage measurements can be of either linear type or volumetric
type. However, not many linear test methods are able to handle anisotropic volume
changes, i.e. on cementitious materials in fresh state. Moreover, most methods are
designed to be used on mortar and cement paste, and not on concrete. Measurements of
autogenous deformation, both linear and volumetric, are very sensitive to bleed water in
the sealed samples. Since the bleed water may be reabsorbed after setting by the cement
paste, the linear shrinkage will reduce or even cause expansion [116]. For volumetric
shrinkage, the effect of reabsorbed bleed water on the external volume will be the opposite,
since the effect of loss of water is much larger than the expansion from absorption
[133][142]. Hence, the presence of bleed water will overestimate the autogenous shrinkage
when measuring volumetrically, and underestimate it when measuring linearly. In order to
avoid bleeding, rotating the sample prior to setting has been proposed [111][143][144].
Volumetric measurement of autogenous shrinkage is generally performed on samples,
mainly cement paste and mortars, in a tight flexible rubber/latex membrane submerged in a
thermally stable bath of water (or e.g. silicone oil); see Figure 46. The sample’s change in
volume is measured by the amount of water displaced by the immersed sample, usually by
measuring the change in weight (reduced buoyancy, according to Archimedes’ principle)
[143][145]. The membrane type is selected to withstand alkali and to be tight enough not to
allow water to penetrate. The advantage of this method is that continuous measurement can

be commenced immediately after casting. However, in addition to the effect of bleeding

water, entrapped air between the membrane and the sample will, once set, be sucked back
into the cement paste, causing errors in the measurement (e.g. overestimated shrinkage)
[114]. Care must be taken when filling the membrane, to avoid the entrapment of air.
Furthermore, the pressure excreted on the sample by the elastic membrane and by the
surrounding liquid may brake the growth of crystals and weaken the initial skeleton of the
cement paste, and consequently increase the shrinkage during setting [125][133].
It has been shown that, before the Balance

0.001 g
formation of self-supporting skeleton
and gas-filled pores, there is good Thermo stable bath
agreement between the chemical and Flexible tight
autogenous shrinkages when membrane
determined by the reduced buoyancy
technique [81][108][145][144]. Still, Sample
once hydration products start to form
(initial set), the chemical and
autogenous shrinkages will diverge.
This will verify the model for cement Figure 46. Illustration of volumetric
pastes, presented in section 3.3.2, autogenous shrinkage measurement by
Figure 33. reduced buoyancy technique.
Linear autogenous measurements, at early age, are generally performed on samples in a

rigid mould with low friction [81][108][111]. Usually the mould is of prism or beam type,
but also slabs or cylinders type occur. An overview of different methods for linear
measurements of autogenous shrinkage can be found in literature [111][123][146]. The
size of the sample is dependent on the maximum grain size (i.e. if paste, mortar or
concrete). The mould is to be temperature-controlled (e.g. circulating cooling liquid) or
placed in a thermostable bath. However, for large samples it can be problematic to achieve
isothermal conditions (constant temperature). The length change of the sample is usually
recorded by displacement transducer, or by non-contact transducers (e.g. laser technique),
at the end of the specimen or at rods/bars imbedded in the fresh cast (see Figure 47). Also
imbedded strain gauges have been proposed for linear measurements [125][147]. It is
important that the exposed surface is sealed/covered (e.g. by diffusion-tight plastic or
aluminium foil) immediately after finishing, preventing any evaporation. However, none of
these linear methods have the ability to measure before setting, as the material must have
some degree of rigidity; hence it is proposed that the tests should be complemented with a
transducer (contact/non-contact) recording vertical displacement (settlement) [145]. This
displacement can be measured on a small plate placed on the surface of the specimen
[148]. By simultaneously measuring the vertical and horizontal displacement, the
volumetric shrinkage can be calculated for the whole period of early-age shrinkage.

Thermo stable bath Cover/sealing (e.g. plastic foil)

Displacement transducer Low friction surface (e.g. teflon foil)
Measuring rod Mould
Specimen
l0
Figure 47. Principle of linear autogenous shrinkage measurement on prism/beam with

displacement transducers recording the change in length at the end of the sealed sample.
In addition, linear measurement of autogenous shrinkage can be performed on samples cast
in a corrugated tight tube. The corrugation permits the tube to deform easily in the
longitudinal direction, whereas the geometry of the cross section is well defined. Before
set, the tube will transform the volumetric deformation into a linear deformation. However,
as the cementitious material undergoes transition from a fluid to a rigid state, the
deformation will become isotropic. Thus, continuous measurement can be commenced
immediately after casting. The tube is to withstand alkali and be tight enough not to allow
water/air to penetrate (e.g. PVC, polyethylene). To measure under isothermal conditions,
the sample is to be submerged in a thermally stable bath of water (or e.g. glycol, silicone
oil); see Figure 48. Linear autogenous deformation using a corrugated tube mould has been
proposed for cement paste, mortar and concrete [133][149]-[151]. For pastes and mortars,
smaller tubes are to be used, whereas for concrete the tube must have a larger diameter (~5
times the maximum grain size). Moreover, measurements can be performed in vertical or
horizontal position, although linear might be preferable as the vertical position can
introduce errors from bleeding and segregation. A setup for concrete is exemplified in
section 4.4.3.
Displacement transducer Corrugated tight mould
End cap Specimen Thermo stable bath
l0
Figure 48. Illustration of a linear autogenous shrinkage measurement on corrugated tube

mould with displacement transducers, recording the change in length at the end.
The autogenous shrinkage measurements, presented in the appended papers (Paper IV, V,
IV and VI), were performed using the latter linear technique with a corrugated tube mould.
3.4.4 Plastic shrinkage measurement

Plastic shrinkage incorporates most of the mechanisms of early-age deformation. The
plastic shrinkage will mainly be governed by the autogenous shrinkage and the shrinkage
due to evaporation [82][91][108]. However, when measuring the plastic shrinkage, thermal
dilatation from hydration and the evaporation cooling (by water transforming from liquid

to gas) will also contribute to the total deformation. Moreover, the plastic shrinkage is only
a relative measure as it strongly depends on a number of factors related to the sample’s
geometry and environmental conditions [23]. Thus, these factors are to be controlled and
well defined. Methods proposed for plastic shrinkage measurements (e.g. ASTM
C157/C157M and C426) need a certain level of rigidity in order to measure the shrinkage,
and usually do not consider the deformation during the first 24 hours after casting [118].
For early-age plastic shrinkage, measurement is to be started prior to demoulding. For
concrete, a method has been proposed [145][152][153] for measuring the linear plastic
shrinkage on slab-type samples in a rigid mould. This is performed analogously to the
linear autogenous deformation, but the top surface is exposed to drying at controlled
ambient condition (air velocity, RH and temperature). As the material must have some
degree of rigidity, tests are complemented with a transducer recording vertical
displacement (settlement). By simultaneously measuring the vertical and horizontal
displacement, the volumetric shrinkage can be calculated for the whole period of early-age
shrinkage. Furthermore, complementary measurements of weight loss can be recorded by
placing the sample on a balance, in order to evaluate the evaporation (see Figure 49).
Displacement
Measuring rod
Low friction surface transducer (vertical) Fan
Mould (e.g. teflon foil) Thermo couple
Displacement v, T, RH
transducer
Specimen 0.001 g Balance
Figure 49. Principle of linear plastic shrinkage measurement on a slab exposed to drying,
with displacement transducers recording the vertical and horizontal deformation.

Some concluding remarks concerning the early-age shrinkage of fresh cementitious
materials (paste, mortar and concrete) can be made as follows:
o There are two main driving forces for early-age shrinkage: (1) drying shrinkage due
evaporation, and (2) chemical shrinkage due to hydration. However, temperature
dilation may also contribute, as well as the external suction of water by the formwork
material or by the sub-base. Accordingly, cracking in the initial phase is a product of
several mechanisms.
o To elucidate the mechanism of early-age deformations, the underlying mechanisms,
such as capillary pore pressure, temperature and structural development, are to be
investigated and taken into account.
o At the stage where the paste is liquid-like, without restraining skeleton and empty
pores, the chemical shrinkage will be equal to the external bulk deformation.
However, at the stage when the self-supporting skeleton of hydration products starts
to form (initial set) the external and internal chemical shrinkage will diverge, since
the rigidity of the paste restrains the volume change. This external deformation (for a
sealed system) is referred to as autogenous shrinkage.

o Early-age shrinkage can either be measured linearly or volumetrically, both

techniques having advantages and disadvantages. The main difference is that linear
techniques usually need a certain level of rigidity of the sample on order to start
measuring. Moreover, even under carefully controlled conditions the volumetric
technique produces up to 5 times higher measuring results.
o Bleed water may introduce large errors to the shrinkage measurements, and care are
to be taken in order to avoid segregation and bleeding. Volumetric measurements are
especially sensitive for bleed water and entrapped air, causing an overestimated
shrinkage. Whereas, in linear measurements the reabsorbed bleed water may lead to
underestimation of the shrinkage.
o Autogenous deformation refers to deformation under autogenous conditions
(unstrained, sealed and isothermal) and do not refer to whether the system have set or
not. Moreover, as the point of set is not a well-defined physical state but rather a
continuous transformation from a liquid to a solid state, often arbitrarily chosen. And
as the shrinkage is highest up to an age of 12 hours, it is suggested that autogenous
deformation is to be referring to the whole period of hardening from mixing. Also
this offers the possibility to register the time of setting.
o Linear measurements, started prior setting, are a sensitive task. It is not only
associated with large scatter, it also somewhat ambiguous since the length is not
defined in a fluid system. At the initial stage where the concrete is liquid-like,
without a restraining skeleton and empty pore, the volumetric shrinkage will manly
turn into a vertical displacement (settlement).
o By simultaneously measuring the vertical and horizontal displacement, the
volumetric shrinkage can be calculated for the whole period of early-age shrinkage.
Alternatively, linear measurement can be performed on samples cast in a flexible
mould with a well defined cross section. Hence, before set the tube will transform the
volumetric deformation into a linear deformation.

Chapter 4 – Experimental work
4 EXPERIMENTAL WORK
4.1 Introduction
Complementary information concerning the experimental methods and materials used in
the appended papers is presented in this chapter. Further, a more detailed description is
provided, and some further analysis of the methods and the results is made.
In Paper I the influence of Bingham rheology parameters on the slump flow values of self-
compacting concrete and mortar is evaluated, and it addresses the complex connection
between the slump flow spread, flow time (T50), yield stress and plastic viscosity. A large
number of more or less self-compacting mortars (~200 mixtures) and concretes (~550
mixtures) with a wide range of consistency were used. The mortar rheology was measured
by using a Bohlin CVO200 rheometer with concentric setup, and for concrete a ConTec
Visco5 rheometer was used.
In Paper II the properties of eight different fillers (seven limestone and one glass filler)
and their influence on the rheology of self-compacting mortar are evaluated. The mortar
rheology and slump flow were measured using the same setup as in Paper I. Traditional
methods for determining the surface area of filler material were used, such as the area from
size distribution (laser diffraction), by image analysis (SEM), Blaine, and by BET(N2). In
addition, a simplified method called BET(H2O) was used. Geometrical properties such as
F-shape, F-circle and Compactness were determined from image analysis (SEM), and the
fillers’ retained water ratio and deformation coefficient were measured.
In Paper III the effect of the specific surface area of gravel and limestone filler on the
rheology of self-compacting concrete is evaluated. The area was measured with the
BET(H2O) method, as in Paper II. The differences in BET-area were used as a basis for
calculation of the water demand for the concrete mixes. The concrete rheology and slump
flow were measured using the same setup as in Paper I. The mix design and its
constituents comprised typical materials and compositions for SCC in Sweden. A 0-8 mm
natural gravel, collected at five different occasions, was used, as well as five limestone
fillers with different geological origins.
In Paper IV the influence of fineness of concrete constituents on early-age (<24 h)
autogenous shrinkage is investigated. The experiments were conducted on SCC,
incorporating the same five limestone fillers as in Paper III. Tests were also conducted on
corresponding mixes without cement, i.e. without chemical shrinkage. A newly developed
concrete dilatometer was used, generating measurements of linear autogenous (sealed)
deformation of the concrete cast in a vapour-proof flexible tube mould. Temperature and
pore pressure were simultaneously measured on the sealed samples together with the
deformation.
In Paper V the influence of mix design on autogenous deformation (with the same method
as in Paper IV) and crack tendency due to plastic shrinkage are evaluated. For the crack
tendency test, a modified ring-test method was used where the concrete specimens were
exposed to early drying conditions while restrained by an inner steel ring. A large number
of different SCC constituents and mix compositions were investigated: e.g. w/c-ratio from

0.38 to 0.67, silica fume, and different admixtures. For comparison, tests with standard
concrete were also made.
Paper VI summarizes Papers II-V, with the focus on the five limestone fillers with
different BET-area and their effect on the fresh and hardened properties of self-compacting
concrete (SCC). Complementary tests of compressive strength (28 d) were made.
4.2 Materials and mix design

The mix design comprised typical compositions for SCC (in Sweden), and the constituents
used are all available products on the Swedish market, with some exceptions. However, in
Paper I, some materials used are unique. In this case the mixture’s composition was not
considered, as only the measures of flowability were of interest. Fore instance, different
cements, mineral and chemical admixtures were used. Neither were all mixes self-
compacting, but they still had the ability to generate a measurable slump flow spread.
In Paper II one of the seven limestone fillers, the one named “L180X” from Nordkalk, is
not a commercial product. Furthermore, the filler named “MicroFiller” (ground recycled
glass), from SGÅ, is no longer produced.
The SCC mixes were designed to have a water-to-filler ratio (w/f) by volume close to 1.0
[154]. In this calculation, all solid material smaller than 0.125 mm was included as filler.
The following two materials, typical for all mixtures (except for Paper I), were used:
o Cement, type CEM II/A-LL 42.5R, “Byggcement Std PK Skövde”, Cementa.
o Superplasticizer, polycarboxylate ether-based type, “Sikament 56”, Sika.
The mortar recipes in Papers I and II are based on “normal” SCC, where the proportions
were scaled down to a maximum grain size of 0.5 mm. This scaling was made, thus with
some modifications for appropriate consistency, according to the following factors:
o 95% water
o 60% superplasticizer
o 100% cement and filler
o 50% natural gravel (0-8 mm), with dmax = 0.5 mm.
o 0% coarse aggregate (8-16 mm)
The limestone fillers used, all of ground type, were G100
G200
selected for their differences in size distribution (Filipstad)
and geological origin, thus providing variations in
L25
size, surface area, shape, surface porosity and L40
texture. The location of the quarries where the L180X
(Köping)
limestone fillers originated from is illustrated in
Figure 50, and their chemical composition is given L10
in Table 6. One of the coarsest fillers, the “L70”, L70
L180
was also the one with the largest specific surface (Uddagården)
area by BET. An explanation for the large area
L15
may be the apparently porous structure of the L190
particles available for water to be adsorbed (see (Ignaberga)
Figure 51). Compared with the filler “L40”, used
as reference, the area by BET(H2O) for “L70” was Figure 50. Location of the
~3.4 times larger. limestone quarry’s in Sweden.

Figure 51. Pictures of limestone fillers, taken with SEM. The pictures edge length
corresponds to 0.5 mm. To the left, the relatively coarse “L70” filler with a large specific
surface area. To the right, the “L40” filler which was used as a reference.
Table 6. Chemical composition of the limestone fillers, in percentage.

L10 L15 L25 L40 L70 L180 L180X L190 G100 G200
CaO 48.7 49.1 51.2 50.2 46.8 47.4 50.0 51.5 52.9 52.5
SiO2 6.8 9.9 3.7 5.2 8.3 8.0 5.5 5.4 3.8 3.5
Al2O3 2.3 0.63 0.89 1.2 2.7 2.8 1.2 0.42 0.83 0.85
Fe2O3 1.10 0.25 0.78 1.00 1.4 1.40 0.95 0.19 0.9 0.7
MgO 0.63 0.44 1.40 1.60 0.61 0.68 1.54 0.45 6.70 4.50
K2O 0.55 0.33 0.23 0.30 0.63 0.65 0.33 0.19 0.19 0.15
LOI 38.7 39.1 41.1 40.5 37.7 37.6 40.6 41.2 40.0 40.0
In Paper III, a natural gravel (0-8 mm) named “Hol” was used. Samples (~100 kg) were
collected over a period of 4 months at regular intervals from the daily production at a
concrete plant. The deviations of standard quantification measures for natural gravel (size
distribution, water absorption, density, petrography, modulus of fineness and silt content
according to EN standards) were within acceptance. For each sample, the specific surface
area was measured by BET(H2O). Five representative samples were then chosen, having a
wide range of BET-area (see Figure 52). Geometrical properties such as F-shape, F-circle,
Compactness and surface area were determined by image analysis on SEM pictures. No
significant differences between the five samples were detected (see Figure 53). Neither did
the petrography analyse show significant differences (see Table 7)
Table 7. Petrography analysis of the natural gravel “Hol”, for particles in the size range
0.125-0.5 mm (values in percentage of total number of particles analyzed).
Granite Quartz Feldspar Mica Amphibolite Porphyry Clay slate Opaque
Sandstone minerals
F(ref) 17 40 36 3 3 0,4 0.8 0.6
G 15 49 29 1 3 0,2 0.6 0.4
H 15 43 33 2 3 0,8 1 0.8
I 17 37 38 2 5 0,2 0.8 0.8
J 19 39 35 1 4 0,6 0.8 0.6

Compactness
3 400
J 1.0 F-shape 65 000
Compactness, F-shape, F-circle [-]

H F(ref)
F-circle
Specific surface area [m /m ]

3 200
3
I 0.9 Surface area
2
BET(H2O) [m /kg]
3 000
60 000
2
G 0.8
2 800
0.7
2 600 55 000
2 400 0.6
2 200 0.5 50 000

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 F(ref) G H I J
Figure 52. Regular measures (4 months) of Figure 53. F-shape, F-circle,

specific surface area by BET(H2O) for the 0- Compactness and surface area
8 mm natural gravel “Hol”, and the five determined by image analysis (SEM),
selected samples (F to J). for particles of sizes up to 0.125 mm
Each mortar mix was prepared in batches of 0:00 1 WATER

0.5 to 1.0 litres, using a 4.73 litre Hobart 30 sec I. 140 rpm 2 CEMENT
laboratory paddle mixer (see Figure 55). 0:30 3
The mixing sequence is based on ASTM 30 sec I. 140 rpm
SAND &
FILLER
C305, and is illustrated in Figure 54. 1:00
stop/start
SP
4
The concrete mixes were made in batches of 30 sec II. 285 rpm
30 to 60 litres, mixed in a BHS-60 twin- 1:30

stop
5
(15 sec)
shaft paddle mixer (see Figure 55) for four (SCRAPE)
minutes after all water was added to the 90 sec 0 rpm
premixed dry materials. The chemical 3:00

start
6
admixtures (e.g. superplasticizer) were
60 sec II. 285 rpm
added directly after the mixing water.
stop
4:00 7
Figure 54. Mixing sequence (mortar).
Figure 55. Photo showing the mixers. To the left is the Hobart mixer used for the mortars,
and to the right the BHS mixer used for the concretes.

4.3 Particle quantifications

4.3.1 Surface area from size distribution
The specific surface area (S) is a single parameter to describe particles’ total area available
for surrounding media. One way to evaluate S is to assume the particle geometry and
calculate the area from the size distribution (grading curve). Hence, the surface area
generated by the particles’ shape, porosity and texture will not be taken into consideration.
Moreover, the contribution from the smallest fraction will be underestimated. The content
of fines might be small, but the number of particles can be large and, consequently, so will
the total surface area (see Figure 1).
In Paper II the sample’s specific surface area from size distribution was determined, both
on the basis of results from the laser diffraction analysis (Ssize) and from the image analysis
with scanning electronic microscope (SSEM).
The Ssize was calculated (BS 4359 standard) [4][155]-[127] by assuming consistently
cubical or spherical and smoothed particles with uniform density (ρ), as:
A Size distribution
S size = = 50
ρ ⋅V m4
6 ∑ ( mi ⋅ d i )
40
2
Staying [weight-%]
= ⋅ [m2/kg] (Eq. 23)

ρ ∑ ( mi ⋅ di )
30
3
m3
20
The particle size ( d i ) is represented by an

m2 10
average value from the two contiguous m1
0
sieves´ nominal sizes (di and di+1), as: 0 0.063 0.125 0.25 0.5
d1 d2 d3 d4
d i = d i ⋅ d i +1 [m] (Eq. 24) Size [mm]
Figure 56. Volume retained material

The mass of material (mi) in this fraction is (mi) and its average size ( d i ), in a
represented by the percentages of retained
linear grading curve, for calculation
material by weight on the smaller contiguous
of specific surface area (Ssize) from
sieve (see Figure 56).
size distribution.
The size distribution from the image analysis (SSEM) was determined according to the
Nordtest method NT BUILD 486, a method based on measurements of the maximum Feret
diameter (Fm) of 2D intersected 3D particles, where the total number of 2D objects per
unit area in size class i (nai) is calculated as:
k
nai = ∑ p j ⋅ n j ⋅ H j [pcs/m2] (Eq. 25)
j =1
where k is the number of classes and pj is the probability that a 3D particle of size H j will
be observed as a 2D object in size class i. nj is the number of 3D objects and H j is the
geometrical mean size in class j.
The SSEM was calculated, assuming cubical particles (shape factor 0.668) with uniform
density (ρ), as [4]:

6 ∑ ( Dcircle,i )
2
A
S SEM = = ⋅ [m2/kg] (Eq. 26)
ρ ⋅ V ρ ∑ ( Dcircle,i )
3
where Dcircle is the diameter of a circle with the same area as Area, A
measured (see Figure 57), and was computed as:
Dcircle = 2 ⋅ A / π [m] (Eq. 27) Dcircle
where A is the particle cross-section area.

Figure 57. Dcircle.
Even though the laser diffraction and the scanning electronic microscope (SEM) recorded
relatively small particles, the calculated area was still 10 to 100 times smaller than the area
measured with the BET method. This proves the significance of the particles’ shape,
porosity and texture of the surface area. Furthermore, in Paper II it was shown that the
correlation between the specific surface areas from size distribution (Ssize and SSEM) and by
BET was poor, whereas the correlation with Blaine was strong. The relationship with the
rheology measures was also poor.
4.3.2 Specific surface area by BET(N2)

A commonly used method to determine the specific surface area of powders is by gas
adsorption methods. By using BET theory (named after its originators Brunauer, Emmett,
and Teller [158]), the surface area can be determined from knowledge of the size and
number of the physically adsorbed gas molecules. This is a more direct method of
determining the specific surface area (S), which is deduced from the area occupied by the
volume of gas required to cover and form a monolayer on the surface of the sample. This
area is normally much larger than the surface area determined by air permeability (i.e.
Blaine) [127][157].
In Paper II the fillers specific surface

area by BET(N2) was determined by
the multipoint method, using nitrogen
gas as adsorbate at different relative
pressures and constant temperature (-
196°C). The test was performed
according to ISO 9277 standard, by
Norkalk AB (limestone filler
producer) (see Figure 58) and by SP
(Swedish National Testing and Figure 58. Photo showing a Micromeritics
Research Institute) both using a analyzer, to determine the multipoint BET
Micromeritics BET analyzer. surface area by flowing gas technique.
The results, presented in Paper II, show that the effect of specific surface area by BET(N2)
for different filler materials on the mortar’s rheology was significant, and that the BET-
area (with N2 as well as with H2O) was the parameter that corresponded best to the
rheological parameters.

4.3.3 Specific surface area by BET(H2O)

Nitrogen is the most commonly used operating gas when determining the specific surface
area by gas adsorption methods. But other gases can also be employed, provided that they
are physically adsorbed by weak bonds at the surface of the solid (i.e. van der Waals
forces): e.g. argon, benzene, krypton, butane, toluene, paraffin, freon, as well as water
[127][157].
By applying BET theory with water vapour as adsorbate, and with the approximation that
the relative pressure (p/p0) has the nature of relative humidity (RH) at 20°C, the BET
equation can be presented as [159]:
RH 1 (C − 1)
= + ⋅ RH [kg/kg] (Eq. 28)
u ⋅ ( 1 − RH ) x m ⋅ C xm ⋅ C
where xm is the monolayer capacity (i.e. the
weight of the gas required for monolayer
y [kg/kg]
coverage), C is a constant related to the
heat of adsorption, and u is the moisture b
content (i.e. the weight of the adsorbed gas) a
defined as: 0.113 0.331
RH [-]
(m − mdry )
u= [kg/kg] (Eq. 29)
mdry Figure 59. BET-plot with the
intersection point (a) and slope (b)
where m and mdry are the sample weight in calculated from the linear relation-ship
adsorbed and dry condition. between y and RH.
By using a so-called BET-plot (see Figure 59), where the adsorption isotherm (y) is plotted
against RH, a linear relationship is created with the intersection point (a) and slope (b) as:
y = a + b ⋅ RH [kg/kg] (Eq. 30)
RH
y= [kg/kg] (RH {0;1}) (Eq. 31)
u ⋅ ( 1 − RH )
1 ( C − 1)
a= [kg/kg] (Eq. 32) b= [kg/kg] (Eq. 33)
xm ⋅ C xm ⋅ C
From this BET-plot, a and b can be determined (graphically or by linear regression), and
the two unknowns xm can be derived as:
1
xm = [kg/kg] (Eq. 34)
a+b
The specific area (S) is directly proportional to the amount of monomolecular adsorbate, as
[156]-[157][160]:
xm ⋅ N
S= ⋅ Am [kg/kg] (Eq. 35)
M
where N is Avogadro´s number (6.022·1023 molecules per mol), M is the molecular weight
of the adsorbate (for water 18.016·10-3 kg per mol), and Am is the area occupied per
molecule of adsorbate in a monolayer. For water, Am is approximately 10.6·10-20 m2 per
molecule [26][156][127][159]. As a perspective, one litre of water in one molecule layer

will cover 3,546,000 m2. From this, the specific surface area by BET, with water as
adsorbate, can be calculated as:
3.54 ⋅ 10 6
S BETH 2 O = [m2/kg] (Eq. 36)
a+b
It should be noted that adsorption is not the same for moisture as for nitrogen gas. The
water molecule is smaller than the nitrogen molecule (10.6 Å2 for water, and 16.2 Å2 for
nitrogen), and has larger affinity forces (of attraction) due to its two-polar covalent bonds
(see Figure 60). Consequently, the water molecule can penetrate into more narrow spaces
(pores and texture) and will be more strongly adsorbed to the particles surfaces, relative to
the nitrogen molecule. A larger quantity of absorbed molecules, in a single layer, will
generate a larger BET-area. However, using water (moisture) is probably closer to real
conditions for materials for concrete production than using nitrogen gas.
H 2O + N2
H Adsorbed
molecules
+ N N
H O
-
Mono-layer
(~3.5Å for water)
Figure 60. The polar water (H2O)
molecule versus the non-polar
nitrogen (N2). Figure 61. Molecules adsorbed onto a surface
Usually a second layer is formed before 0.01
the monolayer is complete (see Figure L180

61), but in the area of 0.05<p/p0<0.40 the 0.008
BET-plot usually shows a linear relation
m oisture content [kg/m ]
3
and a monolayer theory can be adopted 0.006

Natural gravel 0-1
[127][160]. Moreover, no appreciable
capillary condensation can take place 0.004
below 0.4, which is the criterion for the
BET theory [161]. Thus, to be able to use 0.002
BET theory with moisture as a
monomolecular adsorbate, the RH must Microfiller L40
0
be restricted to approximately 5-40% (at 0 10 20 30 40 50
20ºC). In Figure 62 the measurements of RH [%]
the adsorption isotherm for different
fillers and natural gravel at RH up to Figure 62. Adsorption isotherm for two
40% are given. It can be seen that there is limestone filler (L40 and L180), a glass
a linear relation within 10-40%, which filler (Microfiller) and a natural gravel (0-
indicates a monolayer adsorption in this 1 mm).
region.
The technique of using the BET method with moisture (water) instead of nitrogen gas has
been applied by several researchers [4][156][127][159][162]-[165]. In the literature, it can
be seen that during the 1960s and early 1970s there was a vigorous debate on whether
water vapour should be used as BET-adsorbate. Traditionally, when using BET with water,
the focus has mainly been on internal porosity (e.g. to determine the pore size distribution
in a C-S-H gel) and not on external particle surface. Neither has the simplified method,
with different relative humidity instead of pressurized vapour, been used for particles.

The sample particles’ specific surface area by

BET(H2O) was determined gravimetrically by the
simplified multipoint BET method, using water (as
moisture) as adsorbate at different relative humidities
(RH). Initially, the test was performed with a “two-
pressure” humidity generator (see Figure 63) where the
specimens were conditioned in air vaporized at several
levels (from 6 to 50% RH). Later, all tests were
performed with climate boxes at 11.3% and 33.1% RH,
achieved with LiCl and MgCl2 saturated salt (binary)
solutions (see Figure 64). To ensure linearity, KC2H3O2
can be used for 23.1% RH as a third climate.
The sample size was approximately 100 g, the weight Figure 63. Thunder 2500, a
was measured by a precision balance with 0.001 g "two-pressure" humidity
readability, and the sample was oven dried at 105ºC. generator, for climates
The samples were conditioned in each climate for with high accuracy.
approximately four days, at 20ºC.
Saturated salt solution
Sample
Box with tight lid
Fan
Net
Figure 64. Photo of climate boxes with RH 11.3% (LiCl) and 33.1% (MgCl2) RH (left) and
their principle design (right).
The time for the samples to be conditioned and reach steady state within acceptance was
evaluated to be 3-5 days, depending on how large an area the material has. In Figure 65, it
is shown how the oven dried samples, exposed to 50% RH, increase in moisture content
with time. However, this is a relatively high RH.
0.5%
L10
L15
0.4%
Moisture content [%]
L25
0.3% L40
L180
0.2% L180X
L190
0.1%
MF
B15
0.0%
1 10 100 1000 10000
Time [hour]
Figure 65. Changes of moisture content with time, for seven limestone fillers: a glass filler
and a natural gravel (0-1 mm), conditioned at 50% RH. The time scale is logarithmic.

The repeatability was evaluated, using two different natural sands (1 and 2). Ten
repetitions were made, with double samples. New samples (2x100 g) were taken between
the runs. The results are presented in Figure 66. For each sample the coefficient of
variance (COV) was lower than 1.82%. A tendency can be observed, indicating that there
is a systematic error, yet not very large. There are numerous sources that can cause this
error, such as the conditioning time, weighing of oven-dried samples, measuring order, and
room temperature. No further investigation of this was made.
3600
1(average) 1a, COV 1.82%
2
3349 m /kg 1b, COV 1.55%
3500 1(average)
COV 1.65%
S(BETH2O)[m /kg]
3400
2
3300
3200 2(average) 2b, COV 1.45%

2
2(average)
3298 m /kg 2a, COV 1.73% COV 1.67%
3100
Figure 66. Repeatability for the BET(H2O)-area, using double samples of two different
natural sands (0-0.5 mm). New samples (2x100 g) were taken between runs.
For gravel/aggregate, the removed particles not passing the 0.5 mm sieve can be
compensated for, but only very approximately. The BET(H2O) area (S´BETH2O) per unit
specimen mass is then calculated for the whole size fraction and approximated as:
m05
S ' BETH 2O = S BETH 2O ⋅ ( x05 + k ⋅ ( 1 − x05 )) [m /kg] [-]
2
(Eq. 37) x05 = (Eq. 38)
mtot
where k is a factor compensating for the removed particles not passing the 0.5 mm sieve,
x05 is the mass fraction passing the 0.5 mm sieve, m05 is the mass passing 0.5 mm, and mtot
is the total mass. If there is only a small amount passing the 0.5 mm sieve, the calculation
of S´BETH2O is not valid. In a series of measurements on four different 0-8 mm gravels
(naturals, sea sand and crushed), the area was measured on the fraction passing 0.5 mm as
well as on the whole fraction. The test was repeated three times, in order to ensure correct
measurements. The gravel’s size distribution is shown in Figure 67, and the measured
BET-area and factor is given in Table 8. For gravels with a maximum grain size up to 8
mm the factor was approximated to k ≈ 0.5.
100%
Table 8. Measures of BET(H2O)-area for the
80% fraction passing 0.5mm and the whole fraction,
Passing [%]
60% used for the evaluation of factor k.

Natural 1
40%
Natural 2
Gravel <0,5mm SBETH2O S’BETH2O k
20% Sea sand (0-8mm) [%] [m2/kg] [m2/kg] [-]
Crushed Natural1 26% 4142 2375 0.42
0%
Natural2 50% 8162 6320 0.55
Sea sand 65% 1287 1101 0.59
3
5
25
16
5
0
1
2
4
8
06
12
0.
0.
0.
0.
Size [mm]
Crushed 34% 4815 3102 0.46
Figure 67. Size distribution Average 0.51

In Paper II it was shown that the granular characteristics with the highest single correlation
was found between the BET(N2) and BET(H2O) measures (specific area). Although the
measured values are not equal, the linear relationship is good.
40 000
One has to be aware of the differences in
size and polarity of the water and nitrogen
S BET(H2O) [m /kg]
30 000
molecules. Tests have also been made on y = 1.554x
2
fines (<1.0 mm) sieved from different 20 000
2
R = 0.994
aggregates, with the same good
relationship. It was found that the 10 000
BET(H2O) was 1.55 times larger than
0
BET(N2), see Figure 68.
0 5 000 10 000 15 000 20 000
2
For binders of cement type, the BET(H2O) SBET(N2) [m /kg]
method did not supply reliable measures
Figure 68. The linear relation between
due to the nature of hydration, and is
measures of BET-area with N2 and H2O.
therefore not recommended.
The results from the flowability measurements in Papers II and III for mortars and
concretes show significant differences between the samples, which were strongly reflected
by the differences in BET(H2O)-area. There was a strong connection between the
BET(H2O)-area and the rheological parameters and slump flow values.
When there is a change in the dry material’s specific surface area, and as this area has to be
covered with water in order to create mobility, the concrete water demand will change.
One way to compensate for these variations in filler or fine aggregate, presented in Paper
III, is to consider the specific area by BET(H2O) and translate this to a change in water
demand of the concrete mix. With the assumption that 1 litre of water in one molecule
layer covers 3,546,000 m2, the change in mixing water (∆W) due to a change in specific
surface area (∆SBETH2O) can be calculated as:
nH 2O
∆W = ∆S BETH 20 ⋅ ⋅ m mtr [litre/m3] (Eq. 39)
3.546 ⋅ 10 6
where mmtr is the mass of the dry material of the mix, and nH2O is the number of full water
molecular layers covering the particle surfaces required to provide sufficient dispersion for
flowability. Based on numerous experiments, a suitable value was found to be nH2O ≈ 30
layers. This can be compared to the 5-20 molecular layers of water adsorbed at high
relative humidity, proposed in literature [4][156][127][159][166][167] or as much as 60
molecules in thickness [20]. Furthermore, it was shown that the free water content,
available to provide flowability, in 1 m3 SCC mix can vary by several litres due to
differences in apparently equivalent fine aggregates. In [5] it was found that a natural
gravel collected at different spots in a gravel pit, with small differences in grading, can
vary in BET(H2O)-area by ~7000 m2/kg. A change in BET-area of 1000 m2/kg corresponds
to approximately 0.8% moisture content of the gravel. E.g. a SCC with 1000 kg gravel (0-8
mm) that increases by 10000 m2/kg in area will need 8.5 litres of extra water, in order to
retain its consistency.
In Papers IV and IV the BET(H2O)-area was shown to influence – apart from the
flowability and water requirement – the pore pressure development, autogenous
deformation, plastic shrinkage and compressive strength. Limestone filler with larger BET-
area increased the rate and magnitude of autogenous shrinkage, primarily in the plastic
region, without affecting the temperature development and the times to initial and final set.

Increased particle surface area decreased the rate and magnitude of evaporation, and
reduced the plastic crack tendency. In addition, a larger BET-area gave rise to a higher
compressive strength. When adding extra water to the mix, compensating for the loss of
flowability due to increased particle surface area, the crack tendency increased
significantly, the autogenous shrinkage decreased and the compressive strength was
lowered.
For more details and a methodology description of the BET(H2O)-method, see Appendix A.
4.3.4 Specific surface area by Blaine

The surface area of powder can be
determined by measuring the pressure
drop of fluid flow through a packed
powder bed. The most frequently used
apparatus is the Blaine, which is a
standard test method for characterizing
the fineness of hydraulic cement by air
permeability.
In Paper II, the fillers’ fineness, in terms
of specific surface area, was determined
by the Blaine method (Sblaine). The test
was made according to the SS 134222
(similar to ASTM C204) standard, with a
Tonindustrie instrument (see Figure 69).
Comparative measurements on the fillers Figure 69. The Blaine apparatus for
were performed by Norkalk AB, using a determining powder fineness, in terms of
ToniPerm instrument. specific surface area.
A strong correlation was found between the calculated specific area (from size
distributions) and the area measured with Blaine, whereas the correlation with the BET-
area was weak. This indicates that Blaine is mainly a measure of size and size distribution,
based on theoretical spherical particles. However, it should be noted that great variation
was observed between values measured on the same specimen, especially between those
performed by different persons (and equipment used).
Furthermore, the results presented in Paper II, shows that the effect of specific surface area
by Blaine for different filler materials showed a poor correlation with the mortar’s
rheological parameters.
4.3.5 Image analysis

Image analysis refers to a computer analysis of digital images, where a large number of
particles, each with numerous parameters, are generated. The image analysis unit has the
capability to generate an array of chords across the particle to arithmetically define
geometrical quantification, e.g. of shape and size.

The image processing and analysis were made,

in Paper II, with the software “UTHSCSA
Image Tool”. The samples were epoxy-
moulded and polished. The images were made
by a low-vacuum scanning electron
microscope (SEM), type Jeol 5310LV (see
Figure 70), at Swedish National Testing and
Research Institute (SP). For a representative
sample, approximately 15,000 particles from
four different digital pictures with 2016·2016
pixels size were used. The following shape Figure 70. Images generated by
factors were calculated as (Eq. 40) to (Eq. 42). SEM.
F-shape: the ratio of the length of the minor a) Dmin

axis (Dmin) to the length of the major axis Dmax
(Dmax). If the elongation is 1, the object is
roughly circular or square (see Figure 71).
The F-shape is computed as:
Dmin Dmax [-] (Eq. 40)
b) Area (pe.) Perimeter
F-circle: the ratio of measured area to the area Area (ci.)
of a circle with the same perimeter as
measured. At 1, the object is circular (see
Figure 71). The F-circle is computed as:
4 ⋅ π ⋅ Area
[-] (Eq. 41)
Perimeter 2 c)
Dmax
Compactness: the ratio between the diameter of
a circle with the same area as measured (Dcircle)
and the maximum elongation (Dmax) of the Dcircle
measured area. At 1, the object is circular (see

Figure 71). The Compactness is computed as:
Figure 71. Geometrical measures
2 ⋅ Area / π for calculation of F-shape (a), F-
[-] (= Dcircle / Dmax) (Eq. 42)
Dmax circle (b) and Compactness (c).
The results, in Paper II, show that the correlations between the shape factors (F-shape, F-
circle and Compactness) are good. This was expected since the values used for calculation
have much in common. Thus it ought to be pointed out that F-shape is more a measure of
shape, F-circle is more a measure of texture, and Compactness is somewhere in between.
The correlation with other granular characteristics (calculated surface area, BET-area and
Blaine) was poor, and so was the connection with the mortar’s rheological parameters.
The quantification by image analysis can be problematic, as the method is strongly
dependent on a large number of factors, such as: sample preparation, microscope
performance, photo quality (sharpness), resolution, number of particles, analyzing
software, threshold technique, etc. Since the threshold was made manually, the results can
be somewhat arbitrary.

4.3.6 Retained water and water sensitivity

When a sufficient amount of water is provided to the powder, the interacting forces
decrease, the particles start to disperse, and deformation arises by its own gravity.
Okamura et al. [168] found that there was a linear relationship between the water-to-
powder ratio and the relative spread flow, which can be used to empirically characterize
the powder’s response to water addition.
In Paper II, this method was used to quantify Mini-slump cone Sample
the different fillers’ retained water ratio (βp) ØD=700/100 mm Table (non-
H=60 mm adsorbent)
and deformation coefficient or sensitivity (Ep).
A mini-slump test was used to measure the Spread
flow spread. The relative flow area (Rp), at diameter
different water-to-powder ratios by volume
(Vw/Vp), was calculated as:
Figure 72. The mini-slump and the
D2 measurements of spread flow
R p = 2 − 1 [m2/m2] (Eq. 43)
D0 diameter (in four directions).
where D is the average spread diameter,
calculated in four directions and D0 is the base Vw/Vp [-]
diameter of the cone (see Figure 72).
The measure of retained water ratio (βp) can be Ep
considered as the amount of water, adsorbed on
the particle surfaces and filling the voids in the βp
particle system, needed to initiate flow. The Rp [-]
deformation coefficient (Ep) is a measure of the
sensitivity to a change in water content [169]. Figure 73. The evaluation of βp and
βp is represented by the interception point and Ep from the linear relationship of the
Ep the slope, from the linear relationship ratio of water to powder (Vw/Vp) and
between Vw/Vp and Rp (see Figure 73). relative spread flow (Rp).
Results, in Paper II, show a strong correlation between the fillers’ retained water ratio (βp)
and the mortar slump flow spread, whereas the deformation coefficient (Ep) correlated with
the specific surface area from size distribution and with the Blaine area. Theoretically, the
fillers’ retained water ratio (βp) should reflect the ability to adsorb water, and correlate
with the BET(H2O)-area; but this correlation was poor. In addition, the fillers’ water
absorption (with particles passing the 0.063 mm sieve removed) was determined in
according to EN 1097-6, a method mainly designed for aggregates. But as the coefficient
of variance was high (~25% when repeated four times) these measurements are not
presented. Still, the water absorption showed a correlation with the BET(H2O)-area.
4.4 Mortar and concrete quantifications

4.4.1 Slump flow test
The oldest and most frequently used test today is the slump cone test, which, associated
with the Abram’s cone, has its origin in the USA around 1910 [170]. For high-flowable
concretes and mortars, the slump cone is used to measure the spread (slump flow), rather
than the vertical drop.

For the mortars, in Papers I and II, slump

flow measurement was carried out by using a
mini-slump cone (see Figure 74). The
average spread flow diameter, from two
perpendicular directions, was measured (in
millimetres). No compaction was needed (as
in EN 1015-2 and ASTM C230 standard), as
the mortar mixes were highly flowable.
For the concretes, all more or less self- Figure 74. Mini-slump flow test with
compacting, slump flow measurement was mortar (spread).
carried out using a traditional slump cone
(EN 12350-2 or ASTM C143, but without
compaction; see Figure 75). In addition to
the slump flow spread (average), the time
from lifting the cone to when the flow spread
reached a 500 mm circle was recorded,
referred to as T50 and stated in seconds.
The concrete slump flow test (spread and
T50) was used in Papers I, III and VI.
Moreover, in Paper I slump flow values
(concrete and mortar) were used for
evaluation of the relation to the rheology Figure 75. Slump flow test with
parameters (yield stress and viscosity). concrete (spread and T50).
4.4.2 Rheology
For a more scientific approach, a rheometer can be
used (see section 2.3). Unlike the measurements of
qualitative tests (e.g. slump flow), the rheological
parameters are fundamental physical quantities,
mutually independent and not dependent on
operator or equipment. The most established
parameters used to define mortar and concrete
rheology are the yield stress and plastic viscosity in
the Bingham equation [24][28] (see section 2.2.3) . Figure 76. The Bohlin CVO200.
For the mortars (in Papers I and II), a Bohlin
CVO200 rheometer was used, with a fixed outer
cylinder (cup) of diameter Do=30 mm and a
measuring rotating inner cylinder (bob) of diameter
Di = 20 mm, providing a gap of 5 mm (see Figure
76). For the concretes, (in Papers I, III and VI) a
ConTec Visco5 was used, with a rotating outer
cylinder of diameter Do=290 mm and a measuring
fixed inner cylinder of diameter Di=200 mm,
providing a gap of 45 mm (see Figure 77). Figure 77. The ConTec Visco5.

The two rheological parameters of plastic viscosity (ηpl) and yield stress (σ0) were
evaluated in accordance with the Bingham model, see (Eq. 7), at a controlled shear rate
( γ& ) at 20ºC. In addition, the experimental setup for mortars was initiated with a linear
up/down loop for a thixotropic evaluation, represented by the area in hysteresis (see Figure
14). The experimental geometry and measuring sequence is illustrated in Figure 78.
Thixotropy is not strictly a rheological definition, nor an absolute or fundamental term, but
a quantification of reversible time-dependence (see section 2.2.5). A typical measure of
mortar rheology is shown in Figure 79. The measure of segregation was used as a criterion
for acceptance (measures rejected when >10%).
60 No logging
Mortar sample
Logging
Shear rate [1/s]
45
H=37.5 mm
30
Rotating and
15 measuring
inner cylinder
0 Ri=10 mm Fixed outer
0 10 20 30 40 50 60 70 80 90 Ro=15 mm cylinder
Time [s]
8 No logging Ro=145 mm
Concrete
Logging Ri=100 mm sample
Shear rate [1/s]
4
H=140 mm
2 Measuring
inner cylinder
0 Rotating
0 10 20 30 40 50 60 outer cylinder
Time [s]
Figure 78. The measuring sequence for the Bingham evaluation (followed by segregation
estimation) and schematic illustration of the rheometers. For mortar the Bohlin CVO200
was used, and for concrete the ConTec Visco5. The sequence for mortars begins with a
linear up/down loop for a thixotropic evaluation.
1
2
Thixotropic area 3
Segregation [%]
Thixotropy [Pa/s]
Segregation
Viscosity, ηpl [Pa·s]
Yield stress, σo [Pa]

Yield stress and plastic viscosity (Bingham)
•
Figure 79. A typical measurement with mortar and the methodology evaluating the
Bingham parameters and thixotropy (and segregation).

4.4.3 Autogenous deformation

Autogenous deformation is the unstrained bulk deformation of a closed system (under
sealed conditions) at a constant temperature (isothermal), i.e. without exchange of matter
with the exterior (e.g. loss of water) [104]. Fundamental measurements of autogenous
deformation can be made with volumetric or linear techniques, the latter having been used
in this study. More general details are given in section 3.3.3.
In Papers IV, V and IV, autogenous linear deformation was monitored by a concrete digital
dilatometer (CDD), developed in order to start measurement before setting, when the
concrete is fresh. The method is a modification of the CT1 digital dilatometer for pastes
and mortars; see Jensen & Hansen [133]. The CDD sample consists of a concrete
specimen, cast in a steel coil-reinforced vapour-proof flexible polyurethane tube with inner
diameter of ~82 mm and specimen length ~400 mm, sealed with hose clamps and O-ring-
equipped PVC end-caps. The mould is placed in a mechanically stable measuring rig and
the unrestrained, time-dependent, linear bulk deformation is recorded by a digital gauge
(Mitutoyu 543-450B, resolution 1 µm and accuracy 3 µm). The test, containing three
complete CDD setups, was performed in a thermostable room at 20±1ºC, where the
recording was started at 30 minutes from water addition and logged with an interval of 5
minutes for a period of 24 hours or more. The equipment and apparatus for a typical test
are shown in Figure 81.
Due to greater stiffness of the mould in the 0%

radial direction than in the longitudinal, the y = 0.338x
flexible mould transforms most of the -1%
Length change (strain)
volumetric deformation into a linear

y = 0.796x
deformation when the concrete is in the fluid -2%
y=x R2 = 0.9999
state. Based on an experimental evaluation,
-3%
using water as matter, the ratio between linear
and volumetric deformation for a liquid was 3-D tube (calculated)
-4% Fluid (measured)
determined to be approximately 0.8 for the
1-D tube (calculated)
equipment (see Figure 80). As the concrete -5%
undergoes transition from a fluid to a rigid 0% -1% -2% -3% -4% -5%
state, the deformation becomes isotropic. But Volume change
as the setting point is not a well-defined
physical state but rather a continuous Figure 80. The ratio between linear
transformation from a liquid to a solid state and volumetric deformation for the
[104], no correction for this was made. The mould. Filled with a Newtonian fluid
experiments were supplemented with the ratio follows the measured ratio,
measurements of temperature and pore but once rigid the ratio will follow the
pressure placed in the centre of the core. calculated 3-D deformation.

Mould length 460 mm

Specimen length 400 mm Didital gauge
Mould diameter 82 mm 1/1000 mm
Adjustable
fixture
0 001
Fixed end-cap Hose-clap Flexible PU-tube Moving end-cap Measuring rig
0 001
Figure 81. Photo and illustration of the Concrete Digital Dilatometer (CDD), with
supplemented measurements of temperature and pore pressure.
For more details and a methodology description of the CDD-method, see Appendix B.
The result from a test is presented graphically and the development of deformation (mean
value from two or more tests) is plotted against time. Moreover, a number of deformation
factors were evaluated with a model presented in Figure 82. For concrete, the deformation
pattern comprises three distinct stages which can be defined as [91]: plastic, semiplastic
and rigid period. In the plastic (1) and semiplastic (2) periods, the rate of deformation
(dε/dt1 and dε/dt2), period time (t1 and t2) and deformation (ε1 and ε2) are evaluated from
the deformation/time graph. In the rigid period (3), the rate of deformation (dε/dt3) is
evaluated between 48 and 72 hours from water addition. The time (t) is related to the time
when the mixing water was added to the premixed solid material (including the cement).
As the measuring was started after 30 minutes, and as the initial deformation tends to be
linear up to 2 hours from mix, the curve was extrapolated to the time zero.
For the SCC mixes used in this work, the transition from plastic to semiplastic (t1) takes
place at ~6 hours after water addition and the transition to rigid period (t1 + t2) at ~12
hours. Compared to traditional concrete without addition of superplasticizer, the self-
compacting concrete (SCC) tends to be retarded for about one hour [91].

Deformation (strain) [10 m/m]

dε/dt1
ε1
Initial set
-6
ε1
dε/dt2 Final set
ε2
ε1+ε2 dε/dt3
t1 t1+t2
Time, t [hour]
2. Semi-
1. Plastic 3. Rigid
plastic
Figure 82. Model of how the deformation parameters are evaluated from the linear
autogenous deformation measurements, where the deformation is divided into
plastic/semiplastic/rigid periods.
It should be pointed out that linear measurement of autogenous deformation on a concrete
mix before setting, when the concrete is fresh, is a very sensitive task and must be made
with great care. A mean value from two or more tests, each with three complete CDD
setups, was used. A typical measurement (with three setups) generated a coefficient of
variance (COV) below 10% (see Figure 83). What can also be noted in Figure 83 is the
pattern of autogenous deformation, comprising the three distinct stages (plastic, semiplastic
and rigid), separated by the time to initial and final set, and manifested by a plateau in the
curve. Mortar, on the other hand, showed a different behaviour. In Figure 84, no
semiplastic region and distinct point of initial set could be observed, but merely a plastic
and a rigid period separated by a single point of set. Moreover, mortars generated more
stable measures with a smaller deviation (COV <5%), but then the magnitude of
deformation was also approximately two times that of the concretes.
It might seem that the development of autogenous shrinkage ends at final set, but it is
merely slowing down. In long-term measurements, following final set the autogenous
shrinkage after 9-12 months was approximately equal in magnitude as prior setting.
0 12% 0
Deformation [10 m/m]
COV -300
-200 8%
-6
-6
COV
-600
-400 Deformation 4%
(average) -900
-600 0% -1200
0 6 12 18 24 0 6 12 18 24
Figure 83. Autogenous deformation Figure 84. Autogenous deformation for a

measures and COV for a SCC (w/c 0.55). mortar (w/c 0.45 and dmax 8 mm).

For standard concrete (i.e. without additional filler and superplastisizer) a different
behaviour was also shown. In Figure 85 it can be seen that the initial shrinkage is
approximately half the shrinkage the SCC generates. And between initial and final set
(semiplastic region), the standard concrete generated much less shrinkage than the SCC.
These differences might be explained by the effects of the limestone filler and
superplasticizer. When limestone is added to a concrete, the initial induction period (or
dormant period) is shortened and an extra peak of hydration will occur [171]-[175]. This
phenomenon is explained by the surfaces of the filler material acting as nucleation sites for
the early reaction products of CH and CSH, which accelerates the hydration of cement
clinkers (especially C3S) [176]-[179]. In addition, if the cement has a significant amount of
tricalcium aluminate (C3A), calcium carboaluminate will be produced from the reaction
between calcium carbonate (CaCO3) from the limestone and the C3A [180]-[186], which
will also accelerate the hydration. On the other hand, the superplasticizer used for the
SCCs retarded the mixes by approximately one hour.
In Figure 83 and Figure 85 it can be noted 0

that slightly ahead of the final set (12-13
hours) there is a local dip in the Deformation [10 m/m] Standard concrete
deformation, which can be explained by
-200
the fact that this point coincides with the
-6
peak in the temperature development (see

Figure 37). The temperature, in the core SCC
of the sample, changed by approximately -400
5°C. Compensations for this are possible,
but are not an easy task as the thermal
expansion coefficient (TEC) for concrete
is changing with time, especially at early -600
ages. The TEC for concrete is roughly 0 6 12 18 24
20·10-6 1/°C up to and including initial set, Time [hour]
and 10·10-6 1/°C at final set [187]-[190],

Figure 85. Autogenous deformation
whereas for the rig it is 17.3·10-6 1/°C
measures for a standard concrete and a
(stainless steel). Hence, no compensation
SCC (both with w/c 0.55).
for the change in temperature on the
deformation was made.
When developing the equipment, complementary tests were performed, evaluating the
effect of gravity on the measurements of autogenous deformation. Measurements with the
sample placed in 0 (horizontal), 30 and 60 degree positions show no significant differences
(see Figure 86), so the horizontal position was chosen for the method. However, to ensure
unrestrained conditions, a double layer of low-friction paper (teflon type or baking-tray
paper) was placed between the rig and the sample. In a series of tests, using a similar
dilatometer, and thus with a smaller tube, Mounanga et al. [150] evaluated the effect of the
mould’s position on the linear autogenous deformation on self-compacting mortars. It was
found that a vertical position generated more than three times the shrinkage that a
horizontal one did. This effect was mainly explained by sedimentation and bleeding of the
mortars.


-200
-6
0° (horizontal)
30°
-400
60°
-600
0 6 12 18 24
Time (from mix) [hour]
Figure 86. The effect of gravity on the measurements, by placing the rig in different angles.
4.4.4 Plastic shrinkage cracking tendency

For a general description of plastic shrinkage cracking, see section 3.2.
In Papers IV, V and VI a ring-test method was used for the determination of the cracking
tendency of concrete at early ages, as shown in Figure 87. The test method is a
modification of the NORDTEST-method NT Build 433 developed at NTNU/SINTEF by
Johansen and Dahl [191]. The main deviations from the Nordtest method are: the samples
thickness, the environmental conditions, and the method for evaluating the crack tendency.
The test method consists of a ring-shaped specimen of concrete cast between two
concentric steel rings with diameter 300 and 600 mm, and with a thickness of 80 mm. The
steel rings have ribs attached to provide crack initiation and are fixed to a stiff base plate
with a smooth surface (coated with a thin layer of oil). After casting, the ring specimens
are placed in an environmental stable room with 23±2ºC air temperature and 35±5% RH.
Air funnels are positioned over samples, exposing the surfaces to a constant air velocity of
4.5 m/s. The shape (angle) of the funnel is designed to generate a uniform velocity over the
whole surface. For each test a set of three ring specimens was used.
Fan Base plate
Steel rings
Climat
conditions:
23±2°C Concrete
35±5%RH specimen
PT100
Air velocity
Strain gauges
4.5 m/s
Pressure gauges
20 mm Steel ribs
80 mm
20 mm
ø300 mm Scale
ø600 mm
Figure 87. Illustration and photo, showing the test arrangement for the determination of
the cracking tendency.

The measurements start 60 minutes after mixing and the temperature, the weight loss and
the restraint strain are continuously recorded. After 20 hours of drying, the rings are taken
out of the rig and the cracking tendency is evaluated as the average total crack area (crack
length x crack width) on the concrete surface of each of the three specimens. The crack
width was measured with a crack microscope (to an accuracy of 0.05mm) and the crack
length was measured with a digital measuring wheel (to an accuracy of ±1mm). The
weight change was recorded, for one of three samples, using a scale (load cell based) with
accuracy better than 0.03% for a weight of 100 kg (minimum detectable weight change 20
g). The concrete temperature was measured using both a thermo thread, placed in the
specimen, and a PT100 sensor mounted on the inner ring. To monitor the stress build-up of
the concrete and the time when the cracks would appear, strain gauges were mounted (in
full bridge) on the inner steel ring. The air temperature and relative humidity in the room
were measured using a Visala sensor. In addition, the capillary pore pressure was measured
(at 20 and 60 mm depth). Plastic shrinkage is considered to be related to the capillary
pressure in fresh concrete [9][89][116]. The data (strain, pore pressures, weight,
temperatures and RH) were logged every minute using a data logger (PC-logger3100i from
INTAB).
For more details and a methodology description of the ring-test method, see Appendix C.
The method is intended for laboratory use and the test results are purely relative. They
cannot be directly transferred to predict the extent of cracking which will occur in practice
under the prevailing field conditions. Still, the underlying mechanisms can partly be
quantified in terms of temperature and pore pressure development. In order to verify the
ring-test method, Löfgren & Esping [192] conducted a field study in which the cracking
tendency was evaluated on the ring-test specimens, and on larger slab elements that were
both cast outside and exposed to the environment. A series of one reference and six
different SCC’s were used. The experimental results (see Figure 88) showed a strong
correlation (close to unity) between the ring-tests performed in the laboratory and the field
study (both the ring-test and the slab specimens).
3
Ring (field)
Relative crack area [-]
Slab (field)
2 Ring (lab)
0
Mix 1(ref) Mix 2 Mix 3 Mix 4 Mix 5 Mix 6 Mix 7
Figure 88. Comparison of the relative crack areas between the field study (the ring-tests
and the slabs) and the ring-tests of the laboratory study.
4.4.5 Capillary pore pressure

When the concrete dries out due to evaporation, the loss of water from the paste generates
negative capillary pressure, causing the paste to contract [9], which in turn will lead to an
external shrinkage. For a cementitious material where evaporation is prevented, a

contracting negative capillary pressure will also develop, thus uniformly through the
member, but only once the hydration commences and the structure sets [89]. As long as the
concrete is plastic the capillary pore pressure undergoes only small changes. However, at
the stage where the concrete starts to set (initial set), and a restraining skeleton of hydration
products are formed, the capillary pore pressure reach an accelerating phase.
In Papers IV, V and VI, pore pressure was measured with pore pressure transducers (Model
AB 0-15 PSIG from Data Instruments 0-100 kPa / overload 200 kPa), connected to a de-
aired water filled system with a 50 mm long needle (cannula type) with an external/internal
diameter of 0.7/0.4 mm (see Figure 89). The test was performed according to a procedure
developed by Radocea [116]. The data were logged every minute using a data logger (PC-
logger3100i from INTAB). The measurements were performed on sealed samples (in
specimens for autogenous deformation), and on samples exposed to drying (ring-test).
De-aired water
filled system
Sample
Needle (cannula)
L 50 / Ø 0.4 mm
Pressure gauge
Figure 89. Picture and schematic illustration of pressure gauge and the needle used to
measure the capillary pore pressure in the concrete.
It should, however, be pointed out that this test technique is highly sensitive to local
conditions. This sensitivity manifests itself in, for example, a loss of pressure at a random
point in time. This point was named by Wittman [9] as the breakthrough pressure.
The breakthrough pressure probably occurs
0
with local disturbances at the needle tip, such
as destruction of the water menisci by air
Pore pressure [kPa]
pores, which relieves the pressure. As a result, -30

the maximum recorded pressure may not be breakthrough
representative for the concrete. In most of the -60
pore pressure measurements a breakthrough
point was reached, usually at negative pressure -90
in the range of 60 to 100 kPa. Occasionally
measurements as low as 110 kPa were
-120
recorded without showing a breakthrough (see
0 5 10 15 20
Figure 90). Lower pressures may not be Time (from mix) [hour]
possible, due to the fact that water at 20°C
starts boiling at 101.3 kPa. If possible, a media Figure 90. Example, showing the
with a higher boiling point, instead of water development of pore pressure for a
(e.g. silicone oil), can be used in the measuring SCC (w/c 0.55).
system.


Some concluding remarks concerning the experimental methods and materials used in the
appended papers can be made as follows:
o The quantification by image analysis was found to be complicated. The method is
strongly dependent on a large number of factors, such as: sample preparation,
microscope performance, photo quality (sharpness), resolution, number of particles,
analyzing software, threshold technique, etc.
o The shape factors, F-shape, F-circle, and Compactness, are mainly a measure of
particles’ circularity, and the correlation with rheology was poor.
o The different fillers’ retained water ratio (βp) and deformation coefficient or
sensitivity (Ep) show weak correlation with mortars’ rheology.
o Specific area calculated from size distribution and measured by the Blaine method is
somewhat deficient. It is mainly a measure of size and size distribution, deduced for
theoretical spherical particles, and shows a weak correlation with rheology.
o The BET(H2O) method for characterization of specific surface area has proven large
potential. It is simple and inexpensive, and has provided stable and reliable values. It
has also shown a strong correlation with the rheological properties and with the
traditional BET(N2).
o The concrete dilatometer (CDD) is a potential method for linear measurements of
autogenous deformation for concrete at early ages. It has the advantage that
measurements can be started before setting, when the concrete is fresh. It is also
relatively simple and has been shown to provide stable and reliable results.
o From measurements of temperature and pore pressure development, the underlying
mechanisms of autogenous shrinkage could be verified.
o A high correlation was found between the results of the ring-tests performed in the
laboratory and the field study, and between the ring-test specimens and the slab
specimens.

Chapter 5 – Final discussion and conclusions
5 FINAL DISCUSSION AND CONCLUSIONS
5.1 Discussion
The distinguishing characteristic of self-compacting concrete (SCC) is its ability to flow
and consolidate under the influence of its own gravity weight. Yet it is a sensitive mix,
strongly dependent on the composition and the characteristics of its constituents.
Moreover, it has to possess the incompatible properties of high flowability together with
high segregation resistance – a balance made possible by the dispersing effect of high-
range water-reducing admixture (superplasticizer) combined with cohesiveness produced
by a high concentration of fines. However, the large specific surface area of the additional
filler material and the retarding effect of the superplasticizer will also promote the
autogenous (sealed) shrinkage and increase the risk of early-age cracking.
In this thesis, a literature review and experimental work were carried out in order to study
the rheology and early-age deformation of cementitious materials and factors affecting
them. The main conclusion from this work is that, due to the large surface areas involved,
quantification of geometrical and surface properties (size, shape, porosity and texture) of
fillers and the fine part of the aggregates is essential for the ability to control early-age
properties, such as workability and plastic shrinkage cracking, in the production of SCC.
In addition to the size and size distribution, the particles’ external characteristics were
found to be of major importance, especially their shape and texture. These characteristics
of three-dimensional bodies are rather difficult to describe, and it is therefore convenient to
use the total surface area as a single parameter. The surface area strongly reflects the water
requirement that is needed to create fluidity for the concrete. A commonly used method to
determine the specific surface area is the BET method, by which the area is deduced from
the amount of monolayer-adsorbed gas. The main difference between the BET method and
other traditional methods (e.g. that of Blaine) to determine the particles’ specific surface
area is that the BET provides more of a “real” surface area, as it includes shape and surface
properties, while most others are based on the assumption that all particles are spherical
and non-porous. For example, a coarser filler or gravel can provide a larger BET-area than
a finer one, due to differences in surface texture and accessible porosity. However, not
only the surfaces are to be covered with suspending media to generate fluidity; the voids in
between the particles are to be filled, and hence the particles’ packing will also have a
major influence on the flowability.
A simplified adsorption method, the BET(H2O) with water vapour as adsorbate, for
characterization of particles’ specific surface area was introduced, and is proposed as a
potential means of geometrical characterization for fillers and gravels. It is simple and low-
cost, and has provided stable and reliable values. It has also shown a strong correlation
with the traditional BET with nitrogen gas, as well as with the rheological properties.
Furthermore, it was shown that it is possible to calculate the extra water needed to
compensate for changes in filler and fine aggregates’ BET(H2O)-area, in order to produce
SCC with small variations in flowability. An increase in BET(H2O)-area of 1000 m2/kg
corresponds to a need for additional water of approximately 0.85% by mass of the gravel
(or filler) content for constant flowability. E.g. a SCC with 1000 kg gravel (0-8 mm) that
increases by 1000 m2/kg in area will need 8.5 litres of extra water, in order to retain its

flowability. In cases where traditional methods for geometrical characterization (size

distribution, water absorption, fineness modulus, etc.) are kept within acceptance, a normal
gravel for concrete can vary by up to 7000 m2/kg in surface area.
In the presented work, the influence of the BET(H2O)-area and the mix design on the
early-age deformation was investigated. The linear autogenous deformation was measured
with a specially developed concrete dilatometer (the CDD), with the ability to measure
before setting, when the concrete is still fresh. The plastic shrinkage cracking tendency was
evaluated by a modified ring-test method. To verify the underlying mechanisms of early-
age deformation (autogenous and plastic shrinkage), the development of capillary pressure
and temperature was recorded. In addition, to follow the concrete’s stress development and
the time of cracking in the ring-test, the restraint strain on the inner ring was monitored.
It was found that, as long as the concrete is plastic, the autogenous shrinkage developed
rapidly and almost linearly with time. During this period the temperature and capillary pore
pressure underwent only small changes. However, the rate of the shrinkage was
temporarily slowed down, indicating an initial setting of the concrete. For the SCCs used in
this work, this plateau was reached at approximately 6 hours. At this point in time, both the
capillary pore pressure and the temperature reached an accelerating phase, which indicated
that the dormant period was ended and that the cement hydration accelerated. At about 12
hours, a final setting was reached which, for the shrinkage, was manifested in a second
plateau slightly ahead of the temperature peak. After this break point, the following
shrinkage developed much more slowly.
For the concretes exposed to drying, it was found that the plastic shrinkage cracking
usually started at, or slightly after, initial set. The formation of plastic shrinkage cracks is
attributed to the development of capillary pore pressure due to the movement or loss of
water. However, the rate of evaporation strongly depended on the mix composition and
was not always the governing factor for the cracking tendency. Depending on the
characteristics of the concrete, different mechanisms were found to be responsible. For
concrete with a high w/c-ratio, evaporation was the governing cause, whereas for concrete
with a low w/c-ratio (or with the addition of silica) the autogenous shrinkage proved to be
the dominant cause. A minimum in crack tendency was found at w/c 0.55. For the mixes
with retardation (e.g. retarder or high superplasticizer dosage), both the autogenous
shrinkage and evaporation increased, and consequently so did the crack tendency.
With an increased particle surface area (by BET method), the rate and magnitude of
autogenous shrinkage increased, primarily in the plastic region, without affecting the
temperature development and the times to initial and final set. It also decreased the rate of
evaporation, lowered the plastic cracking tendency, and generated a higher compressive
strength. When adding extra water to the mix, compensating for the loss of flowability due
to increased particle surface area, the effect was the opposite (i.e. increased crack
tendency, decreased autogenous shrinkage and lower compressive strength). This indicates
that that the BET-area is not only characterizing the particle’s external surface area, but
partly also the internal area (porosity). If the mixing water is absorbed or sufficiently
bound to particles the effective w/c ratio will decrease, increasing the compressive
strength. Moreover, with an increased area, the increased nucleating will also contribute to
a higher strength.
Finally, the corresponding mixes without cement appeared to generate a large
“autogenous” shrinkage, despite the absence of chemical reaction of cement and water
(hydration). However, in these mixes, the cement was replaced with equal volume of filler,
why the effect of filler was enlarged. At 24 hours the shrinkage was, after a small initial

swelling, approximately in the same magnitude after 24 hours as for the SCC’s with
cement. However, the SCC’s generated no swelling and almost all shrinkage before final
set (~12 hours), whereas for the mixes without cement the rate of shrinkage was lower in
this period. Moreover, once set the rate of deformation for the SCC’s significantly slowing
down. This indicates that not only the hydration (chemical shrinkage) is the driving
mechanism of autogenous shrinkage for concrete, but also the constituent’s
adsorption/absorption will contribute, especially in the fresh state before setting. For
cement paste, prior initial set, the chemical shrinkage might be equal to the autogenous
shrinkage. But once more or less porous particles (filler and aggregate) are introduced to
the mixture the adsorption/absorption will properly introduce an additional shrinkage.
5.2 General conclusions

The main conclusion of this dissertation can briefly be summarised as follows:
o Due to the importance of their large surface area, geometrical quantification of filler
and the fine part of aggregate is essential for the ability to control physical properties,
such as workability and plastic shrinkage, in the production of SCC.
o The specific surface area, quantified by BET technique, has been shown to be the
single most important granular measure concerning the mortar and concrete
flowability (rheology and slump flow) and its time dependency (loss of consistency
and thixotropy), which can be explained by the fact that BET surface area comprises
important factors such as particles fineness, shape, porosity and surface texture.
o Other geometrical characterizations, such as shape factors (F-shape, F-circle, and
Compactness), fineness modulus and specific area calculated from size distribution
and measured by Blaine was somewhat deficient and showed consistently small
differences between the samples. It was difficult to draw reliable conclusions on the
basis of these results, and their correlation with flowability was generally poor.
o The BET (H2O), a simplified gas adsorption method for characterisation of fillers
and aggregates containing fines for SCC, was introduced. The BET (H2O) has
proven high potential. It is simple, low cost, and has provided stable and reliable
values. It has also shown a strong correlation with the rheological properties and with
the traditional BET (Nitrogen).
o It was shown that the free water content, available to provide flowability, in 1 m3
SCC mix can vary by several litres due to differences in apparently equivalent fine
aggregates. Moreover, the specific surface area of normal gravel, accepted by
traditional methods for production of SCC, can vary up to 7000 m2/kg.
o It was demonstrated how an increase in BET(H2O)-area of 1000 m2/kg corresponds
to an increase in water demand by approximately 0.85% by mass of filler or gravel
content for constant flowability. E.g. a SCC with 1000 kg gravel (0-8 mm) that
increases by 1000 m2/kg in area will need 8.5 litre extra water, in order to retain its
consistency.
o A specially developed concrete dilatometer for linear measurements of autogenous
(sealed) deformations was introduced. It has the advantage that measurements can be
started before setting, when the concrete is fresh. It is also relatively simple and has
been shown to provide stable and reliable results. The method and the underlying
mechanisms were verified by parallel measurements of capillary pore pressure.

o Increased particle surface area did not only decrease the SCC flowability, it also
decreased the rate and magnitude of evaporation and consequently reduced the
plastic crack tendency, despite an increased autogenous shrinkage. Moreover, an
increased area resulted in a higher compressive strength. However, with additional
water for constant flowability, compensating for the differences in BET(H2O)-area,
evaporation and plastic cracking tendency was increased significantly, and strength
was reduced.
o For concrete with a high w/c-ratio, evaporation was shown to be the main governing
mechanism for plastic shrinkage cracking, whereas for concrete with a low w/c-ratio
the autogenous shrinkage proved to be dominating. For mixes with retardation, both
the autogenous shrinkage and evaporation increased, and consequently so did the
crack tendency.
o It is proposed that not only the hydration (chemical shrinkage) is the driving
mechanism of autogenous shrinkage for concrete, but also the constituent’s
adsorption/absorption will contribute, especially in the fresh state before setting.
5.3 Suggestions for future research

Materials science is a fundamental field within the area of civil engineering. Although the
research and literature relating to early-age properties of cementitious materials are
extensive, there are still questions to be answered and further research is needed. In
general, if the early-age behaviour and properties are to be better understood, it is
necessary to increase the knowledge and understanding of the mechanisms of interparticle
forces and how they are acting in this complex composite mix.
For measurements of flowability and early-age deformation there is a need of general
guidelines, standards and recommendations. Methods, methodologies, apparatus, models,
etc. have to be defined. For flowability measurements of SCC there are well-established
empirical test methods, whereas there is no general agreement on how to rheologically
characterize the concrete. Surprisingly, for mortars and pastes there are even wider
disagreements. Neither is there general agreement on how to define and characterize the
time-dependent reversible (thixotropic) and irreversible behaviour. In the area of early
deformation, there is even greater disagreement on what and how to measure. As several of
these measures are only relative, general guidelines and standards are needed. Furthermore,
the terminology and definitions are somewhat inconsistent and deficient. In the area of
particle characterization, there are well-established guidelines and standardized methods,
but still there is a lack of simple methods for quality control of the properties of filler and
fines that have a clear connection with the fresh concrete behaviour.
Focusing on the matters identified in this work, the following suggestions for future
research are made.
(1) Develop a methodology to perform measurements with the BET(H2O) method in a
shorter time (normally a measurement takes at least 6-8 days). The working effort is not
large, but it might be preferable to speed up the procedure. A suggested method is to do the
conditioning at lower pressure. By placing the samples in the desiccator with the saturated
salt solution and evacuating the air, the process of adsorption will be faster and the time to
equilibrium shorter. Another suggested method, to speed up equilibrium formation, might
be to perform the conditioning of samples at a higher temperature. A third method could

perhaps be to follow the sample’s weight as a function of time, frequently and long enough
to produce a smooth curve with a clear tendency, and extrapolate to an equilibrium state.
(2) Evaluate the effect of particles’ (filler, gravel and aggregate) adsorption/absorption
with time on the autogenous shrinkage of mortars and concretes. The hydration is, in
general, considered to be the single driving force of autogenous shrinkage. But the
measurements (in Paper IV) on mixtures without cement indicated a substantial
“autogenous” shrinkage, after an initial swelling. Consequently, the contribution of
adsorption/absorption to the autogenous shrinkage ought to be significant, especially in the
fresh state, before initial setting. More measurements need to be made, using different
compositions and materials, and to be complemented with pore pressure measurements on
mixtures without cement.
(3) Develop methodology for measuring the plastic shrinkage, using the concrete
dilatometer (CDD) with an open system where the samples are exposed to evaporation. If
the measurements are made simultaneously with the sealed system, the evaporation
shrinkage can be extracted from the plastic shrinkage. Yet the plastic shrinkage will only
be relative, and so will the evaporation shrinkage, as these measures will depend on the
geometry and diffusion coefficient of the mould, exposed area, air velocity, RH,
temperature, etc.
Within this work, an attempt was made
to measure the plastic shrinkage with (b)
the CDD, by replacing the PE-tube with
a felted cloth (geotextile/fabric; see
Figure 91). But as this mould did not
have the radial stiffness (e.g. from
corrugation and steel wire coil), the (a)
shrinkage in the plastic stage was
mainly transformed to vertical
displacements and almost no linear
measurements were recorded in this
stage. Hence, the open (diffusion)
mould needs to be designed with a Figure 91. Measurements with the CDD: (a)
relation between the volumetric, radial under sealed conditions, and (b) when
and longitudinal deformations, equal to exposed to evaporation (plastic shrinkage).
the sealed mould.
In the present study, the fundamental mechanisms affecting the rheology of cementitious
materials were theoretically reviewed. However, to be able to practically use and apply
these theories in “reality”, a large experimental study needs to be made and the results
compared with those in the literature. The study should focus on the mix design of high-
flowable concretes (e.g. SCC), in which the proportions of the constituents and their
properties are of major importance. Recommendations or instructions for how the
proportions and properties affect the workability/rheology of concrete should be given, e.g.
by designing a flow diagram with orientation (see Figure 92). Also how different measures
of the constituents, by specific methods, affect the workability/rheology are to be given. To
be able to ensure the quality and hopefully lower the cost in the production of SCC, such a
guideline could be a helpful tool.

FLOW DIAGRAM
+Silica/Cement +Cons. loss +Sand/Stone +Cement
+Cement fineness +Filler & fines
+Irregularity
Yield stress, σ0 [Pa]
+Elongation
+Air
+Paste volume
+Water +Flyash/Cement +SP +Slagg/Cement
Viscosity (plastic), ηpl [Pa·s]
Figure 92. Illustration of a flow diagram, showing how changes in proportions and
properties of constituents may affect the flow behaviour (rheologically in terms of the
Bingham parameters σ0 and ηpl) of fresh concrete. This is a potential aid in mix design,
showing how to best orientate towards a desired point of consistency.

Chapter 6 – References
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and technology”, New Jersey, 1995.
[166] Badmann R., Stockhausen N., Setzer M.J., “The statistical thickness and the chemical
potential of adsorbed water films”, Journal of Colloid and Interface Science, Vol. 82(2), pp.
534-542, 1981.
[167] Hagymassy J., Brunauer J.R., Mikhail R.S., “Pores structure analysis by water vapour
adsorption”, Journal of Colloid and Interface Science, Vol. 29(3), pp. 485-491, 1969.
[168] Okamura H., Ozawa K., “Mix design for self-compacting concrete”, Concrete Library of the
JSCE, No 25, pp. 107-120, June, (Translation from Proceedings of ISCE, No 496/V-24,
1994.8), 1995.
[169] Domone P. L., Chai H., “Testing of binders for high performance concrete”, Cement and
Concrete Research, Vol. 27(8), pp. 1141-1147, 1997.
[170] Bartos P., Sonebi M., Tamimi A.K., “Workability and rheology of fresh concrete:
Compendium of tests”, RILEM, France, 2002.
[171] Billberg P., “Influence of filler characteristics on SCC rheology and early hydration”, 2nd
International RILEM Symposium on Self-Compacting Concrete, Japan, pp. 285-294, 2001.
[172] Poppe A.M., Schutter D.G., “Modelling of the heat development during cement hydration in
self-compacting concrete”, Proceedings of the 4th International RILEM Symposium on Self-
Compacting Concrete, pp. 271-277, Chicago, 2005.
[173] Sari M., Prat E., Labastire J.K., “High strength self-compacting concrete - Original solutions
associating organic and inorganic admixtures”, Cement and Concrete Research, Vol. 29(6),
pp. 813-818, 1999.
[174] Sharma R.L., Pandey S.P., “Influence of mineral additives on the hydration characteristics of
ordinary Portland cement”, Cement and Concrete Research, Vol. 29, pp. 1525-1529, 1999.
[175] Ye G., Lui X., Schutter D.G., Poppe A.M., Taerwe L., “Influence of limestone powder used
as filler in SCC on hydration and microstructure of cement pastes” Cement and Concrete
Composites, Vol. 29, pp. 94-102, 2007.
[176] Lawrence P., Cyr M., Ringot E., “Mineral admixtures in mortars effect of type, amount and
fineness of fine constituents on compressive strength”, Cement and Concrete Research, Vol.
35, pp. 1092-1105, 2005.
[177] Nomat A., “Interactions between chemical evolution (hydration) and physical evolution
(setting) in the case of tricalcium silicate”, Materials and Structures, Vol. 27, pp. 187-195,
1994.
[178] Sari M., Prat E., Labastire J.K., “High strength self-compacting concrete - Original solutions
associating organic and inorganic admixtures”, Cement and Concrete Research, Vol. 29(6),
pp. 813-818, 1999.
[179] Soroka I., Setter N., “The effect of fillers on strength of cement mortars”, Cement and
[180] Bonavetti V.L., Rahhal V.F., Irassar E.F., “Studies on the carboaluminate formation in
limestone filler-blended cements”, Cement and Concrete Research, Vol. 31, pp. 853-859,
2001.

[181] Ingram K.D., Daugherty K.E., “A review of limestone addition to Portland cement concrete”,
Cement and Concrete Composites, Vol. 13, pp. 165-170, 1991.
[182] Péra J., Husson S., Guilhot B., “Influence of ground limestone on cement hydration”, Cement
and Concrete Research, Vol. 21, 99-105, 1999.
[183] Soroka I., Stern N., “Calcareous fillers and the compressive strength of Portland cement”,
[184] Taylor H.F.W., “Cement Chemistry”, 2nd Edition, Thomas Telford Publications, London,
1997.
[185] Tsivilis S., Chaniotakis E., Badogiannis E., Pahoulas G., Ilias A., “A study on the parameters
affecting the properties of Portland limestone cements”, Cement and Concrete Composites,
Vol. 21, pp. 107-116, 1999.
[186] Vuk T., Tinta V., Gabrovek R., Kaui V., “The effects of limestone addition, clinker type and
fineness on properties of Portland cement”, Cement and Concrete Research, Vol. 31, pp.
135-139, 2001.
[187] Hedlund H., “Stresses in high performance concrete due to temperature and moisture
variations at early ages”, Licentiate Thesis, Luleå University of Technology, 1996.
[188] Ozawa M., Morimoto H., “Estimation method for thermal expansion coefficient of concretes
at early ages”, Proceedings of the International RILEM Conference on Volume Changes of
[189] Sellevold E.J., Bjøntegaard Ø., “Thermal expansion coefficient of cemen paste and concrete -
Effect of moisture content”, Proceedings of the Conference on Advances in Cement and
Concrete, pp. 27-37, Colorado, 2003.
[190] Schutter D.G., “Thermal properties”, RILEM report 25: Early Age Cracking in Cementitious
Systems, RILEM TC181-EAS, pp. 121-125, 2002.
[191] Johansen R., Dahl P.A., “Control of plastic shrinkage of cement”, Proceedings of the
Conference on Our World in Concrete and Structures, Singapore, 1993.
[192] Löfgren I., Esping O., “Early age cracking of self-compacting concrete”, Proceedings of the
International RILEM Conference on Volume Changes of Hardening Concrete: Testing and
Mitigation, pp.. 251-260, Lyngby, 2006.
Standards, recommendations and other description of test methods:

(Note, standards are not referred to by a given index number, but merely by their ID.)
ACI 116R-90, “Cement and concrete terminology”, American Concrete Institute, ACI Manual of
Concrete in Practice, Part 1, 2000.
ACI 209-92, “Prediction of creep, shrinkage, and temperature effects in concrete structures”,
Farmington Hills: American Concrete Institute , 1997.
ACI 305, “Hot weather concreting”, ACI Manual of Construction Practice, Part 2, Farmington
Hills: American Concrete Institute , 2002
ASTM 04.02, “Construction: Concrete and Aggregates”, Annual Book of ASTM Standards, Vol.
04.02, 2000.
ASTM C33, “Standard specification for concrete aggregates”, Annual Book of ASTM Standards,
Vol. 04.02, 2000.
ASTM C157, Standard test method for length change of hardened hydraulic-cement mortar and
concrete”, Annual Book of ASTM Standards, Volume 04.02, 2002.

ASTM C230-90, “Standard Specification for Flow Table for Use in Tests of Hydraulic Cement”,
Annual Book of ASTM Standards, Volume 04.02, 2002.
ASTM C204-00, “Standard test method for fineness of hydraulic cement by air permeability
apparatus”, 2002.
ASTM C403, “Test method for time of setting of concrete mixtures by penetration resistance,
Annual Book of ASTM Standards, Vol. 04.02, 2002.
ASTM C426-06 Standard test method for linear drying shrinkage of concrete masonry units,
ASTM C1608-06, “Standard Test Method for Chemical Shrinkage of Hydraulic Cement Paste”,
BS 4359, “Determination of specific surface area from particle size distribution”, British standard,
1973.
BS 5168:1975, “Glossary of rheological terms”, British Standard Institution, 1975.
DIN 53019, “Viscometry; Determination of viscosities and flow curves using standard design
rotary viscometers with a standard geometry measuring system”, 1976.
EN 196-3, “Methods of testing cement - Part 3: Determination of setting time and soundness”,
2005.
EN 933-1, “Tests for geometrical properties of aggregates - Part 1: Determination of particle size
distribution - Sieving method”, 2004.
EN 933-2, “Tests for geometrical properties of aggregates - Part 2: Determination of particle size
distribution - Test sieves, nominal size of apertures”, 1996.
EN 1015-2, “Bulk sampling of mortars and preparation of test mortars - Part 2: Bulk sampling of
mortars and preparation of test mortars”, 2006.
EN 1015-3, “Methods of test for mortar for masonry - Part 3: Determination of consistence of fresh
mortar (by flow table)”, 1999.
EN 1097-6, “Tests for mechanical and physical properties of aggregates - Part 6: Determination of
particle density and water absorption”, 2000.
EN 12350-2, “Testing fresh concrete - Part 2: Slump test”, 2000.
ISO 2884, “Paints and varnishes: Determination of viscosity using rotary viscometers - Cone-and-
plate viscometer operated at a high rate of shear”, 1999.
ISO 3219, “Plastics; Polymers/resins in the liquid state or as emulsions or dispersions -
Determination of viscosity using a rotational viscometer with defined shear rate”, 1993.
ISO 9277, “Determination of specific surface area of solids by gas adsorption using BET method”,
1996.
NT BUILD 433, “Concrete: Cracking tendency – Exposure to drying the first 24 hours”, Nordtest,
1995.
NT BUILD 486, “Aggregates: Size distribution”, Nordtest, 1998.
RILEM report 25, “Early Age Cracking in Cementitious Systems, TC181-EAS, RILEM Technical
Committee, 2002.
SS 132126, “Concrete testing - Aggregate - Modulus of fineness”, 1986.
SS 134222, “Methods of testing cement - Determination of fineness”, 1990.

Appendix A - Specific surface area by BET(H2O)
APPENDIX A: BET(H2O)
DETERMINATION OF SPECIFIC SURFACE AREA OF FILLER AND FINE
PART OF AGGREGATE BY BET METHOD WITH WATER ADSORPTION.


BET(H2O):
DETERMINATION OF SPECIFIC SURFACE AREA OF FILLER AND FINE
PART OF AGGREGATE BY BET METHOD WITH WATER ADSORPTION
Key words: surface area, BET, adsorption, powder, filler, aggregate.
1 SCOPE 3 REFERENCES
This description provides guidelines for [1] Brunauer S., Emmet H. P., Teller., “Adsorption
determination of specific surface area by the of gases in multimolecular layers”, American
BET(H2O) method. The principle is based on the Chemical Society, 1938.
method of Brunauer, Emmet and Teller [1], where
[2] Gregg S. J., Sing K. S. W., “Adsorption, surface
the area is given by the number of physically
area and porosity”, New York, 1967.
adsorbed gas molecules formed in a monolayer.
For a general description of the BET method see Standard: ISO 9277, “Determination of the specific
ISO 9277, and for the physics and applications of surface area of solids by gas adsorption using the
gas adsorption see Gregg and Sing [2]. The BET method”, 2002.
measurements of BET area are normally
conducted volumetrically with nitrogen gas (N2), but Standard: EN 933-1, “Tests for geometrical
in this case it is gravimetrically with water vapour properties of aggregates - Determination of particle
size distribution - Sieving method”, 2004.
(H2O) as adsorptive gas. By using the relationship
between the relative humidity and the adsorbed Standard: EN 1097-5, “Tests for mechanical and
weight per unit specimen mass the surface area is physical properties of aggregates - Determination
calculated (in m² per kg). The BET(H2O)-area is of the water content by drying in a ventilated oven”,
generally much larger than the area determined by 2004.
air permeability (e.g. Blaine), and slightly larger
than the BET(N2)-area due to the differences in Standard: EN 932-1, “Tests for general properties
polarity and molecular size. of aggregates - Methods for sampling”, 1997.
For concrete, particle concentration and size Standard: EN 932-2, “Tests for general properties
distribution strongly influence the workability since of aggregates - Methods for reducing laboratory
its matrix consists of a suspension of smaller samples”, 2004.
particles filling the hollow spaces between the
coarser ones. To decrease the internal friction and
generate mobility, the particle surfaces are to be 4 NOTATIONS
covered with water and the voids in the system to 4.1 Definitions
be filled. Other important properties affecting the
workability are the particle shape, porosity and Adsorbate; A substance that is adsorbed at the
surface texture. Since surface area/volume ratio interface of a substrate material.
increases exponentially with particle irregularity Adsorbent; The substrate material onto which a
(shape, surface texture and porosity) and substance is adsorbed.
decreased size, quantification of geometrical
properties of fillers and the fine part of the Adsorption; Enrichment of adsorptive at the
aggregates is essential for the ability to control external and accessible internal surfaces of a solid.
physical properties, such as workability.
Adsorptive; A measuring gas to be adsorbed.
Adsorption isotherm; A graphical representation of
2 FIELD OF APPLICATION the relationship between the bulk activity of
adsorbate and the amount of adsorbate at constant
The BET(H2O) test method is only to be applied for temperature.
laboratory use on fillers and fine part of aggregates.
Cement and other powders reacting with water are BET; A model to determine the surface area from
not to be analyzed. Maximum particle size is 0.5 the physical adsorption of a gas on a solid surface,
mm. If the material incorporates particles up to 8 named after Brunauer, Emmett & Teller.
mm, these are to be removed and compensated Specific surface area; The ratio of total (external
for. For materials with particles larger than 8 mm, and corresponding internal) surface area per unit
the BET(H2O) method is not recommended. weight or unit volume.

4.1 Symbols • A desiccator or airtight cabinet with desiccant, to

be used for the cooling stage. Silica gel with colour
dmax maximum grain size, in millimetres [mm] indicator is a suitable desiccant.
k factor compensating for the particles not NOTE 1: If a desiccator or cabinet with desiccant is
passing the 0.5 mm sieve (k ≈ 0.5) not available, thermal insulation can be used to
protect the balance from the sample heat. A cork
m mass of specimen, in grams [g] mat can be suitable.
mc mass of container, in grams [g]
• Precision balance of suitable capacity (100 g
mdry mass of oven dry specimen, in grams [g] sample + container), with 0.001 g readability and
0.005% accuracy of the sample mass.
RH relative humidity, in the range of 0-1 [-]
• Ventilated drying oven, thermostatically
SBETH2O specific surface area by BET(H2O), in
controlled to a temperature of 110±5°C.
square meters per kilogram [m2/kg]
• 2 sets of airtight boxes, equipped with a tight lid,
S’BETH2O approximated BET(H2O)-area for the
fan, supporting grid/net and shallow tray that
whole mass fraction (up to 8 mm)
occupies most of the bottom for the saturated salt
u moisture content, in kilograms of water solutions (see Figure 1a).
per kilogram dry of material [kg/kg]
• Salts, lithium chloride (LiCl) for 11.3% RH and
x05 mass fraction passing 0.5 mm sieve [-] magnesium chloride (MgCl2) for 33.1% RH. The
amount of salt needed is dependent on the size of
the box, where the shallow tray is to be filled to ~3
5 METHOD OF TESTING mm depth.
5.1 Principle • 1 set (2 off) of containers for each material,
large enough to store the ~100 g double sample.
The specific surface area is determined by The container must be open, heat-resistant and
deducing the area from the volume of gas required made of non-adsorbent material. E.g. a 300 ml food
to form a monolayer on the surface of the sample. tin of thin alumina without lid.
By using BET theory, the area can be calculated
from knowledge of the size and the number of
physically adsorbed gas molecules.
5.3 Preparation of equipment and test
With the BET(H2O), the specific surface area of specimen
fillers and fine part of aggregate is determined
gravimetrically by a multipoint method, using water 5.3.1 Saturated salt solutions
vapour (moisture) as adsorbate at different relative The dry salt is to be spread to about 3 mm depth in
humidity (RH). The test is to be performed at 20ºC the shallow tray. More than one tray can be used in
with climate boxes with 11.3% and 33.1% RH, order to occupy most of the bottom of the climate
achieved with LiCl and MgCl2 saturated salt box. Water is added to moisten the salt, but not
solutions (see Figure 1a). The oven-dried double more than to make it look damp. If all salt is
samples, approximately 2x100 g, are conditioned in dissolved (i.e. no visual salt) too much water has
11.3% RH followed by 33.1% for minimum 4 days been used, in which case add more dry salt.
in each climate. The weight of the dry and
conditioned samples is measured by a precision 5.3.2 Sample
balance with 0.001 g readability. By plotting the The recommended specimen size is approximately
BET(H2O) adsorption isotherm as a linear function 100 g. For gravel/aggregate the sample is to be
of the RH, and evaluating the intercept and slope, collected in accordance with EN 932-1, and
the specific surface area (SBETH2O) can be calculated reduced according to EN 932-2. All grains not
(see Figure 1b). passing the 0.5 mm sieve (see EN 933-1) are to be
removed, and the masses of the passed and
retained materials are to be weighed and recorded.
5.2 Equipment The sample is to be made in pairs, to ensure
Required equipment for a typical test: precision. The maximum number of specimens to
be tested simultaneously depends on the size of
• Thermally controlled room or chamber with an the climate boxes and the sample containers.
air temperature of 20±2ºC.

5.4 Procedure g) Weigh the sample and determine the mass

(m1) by subtracting the mass of the tray (mc) from
5.4.1 Running the test the measured weight. Place the sample in the
a) Weigh and record the mass of the empty climate box with 33.1% RH (MgCl2). The
containers (mc). The containers must be clean and conditioning procedure is the same as for the
dry, and numbered with a marker. 11.3% RH conditioning.
NOTE 2: Two containers for each material are h) Weigh the sample and determine the mass
needed as the sample is to be made in pairs, to (m2) by subtracting the mass of the tray (mc) from
ensure precision. the measured weight.
b) If the materials contain grains larger than 0.5 NOTE 6: Keep the lids of the boxes as closed as
mm these are to be removed by sieving. The possible between the weighing of samples. The
masses of the passed and retained materials on saturated salt solution can be reused a large
the 0.5 mm sieve (see EN 933-1) are to be number of times. Just ensure that the salt is
weighed and recorded. sufficiently moistened, but not fully dissolved.
Adjust by adding extra salt or water if needed.
c) The ~100 g specimens (two per material) are
to be placed in each container. NOTE 7: It is also possible to determine the dry
mass of the test portion (see d to f) as a final step
d) The samples and the desiccant are to be instead. For higher precision and lower error, the
placed in the ventilated drying oven with a dry mass can be determined both initially and
temperature of 110±5°C. The time to dry depends finally (and the mean value reported). The dry
on the sample’s size, fineness, porosity and mass should not differ by more than 0.01%.
moisture content. A minimum time of 4 hours is
recommended. 5.4.2 Finishing the test
e) The samples and the desiccant are to be The measured masses (mdry, m1, and m2) for each
placed in the desiccator or airtight cabinet. The test portion are to be transferred to a computer for
time required for the cooling stage depends on the calculation and evaluation.
size and number of samples, the tightness of the
cabinet, balance heat sensitivity, etc. Time less
than 2 hours is recommended. 5.5 Expression of results
NOTE 3: It is also possible to weigh a sample The BET(H2O) surface area per unit specimen
immediately after removing it from the oven if the mass is calculated as:
balance is sufficiently protected from the sample
heat (with e.g. a cork mat). 3.54 ⋅ 10 6
S BETH 2 O = [m2/kg] (Eq. 1)
f) Weigh the samples and determine the dry a+b
mass of the specimen (mdry) by subtracting the where a is the interception point and b the slope of
mass of the tray (mc) from the weight. Directly place the curve from the linear relationship between the
the sample in the climate box with 11.3% RH (LiCl). BET(H2O) adsorption isotherm and relative
The time for the test portion to be conditioned is a humidity (see Figure 1b). The adsorption isotherm
minimum of 3 days, preferably 4-5. The box is to be (y) is calculated as:
placed in a thermally controlled room or chamber
with an air temperature of 20±2ºC. RH
y= [kg/kg] (Eq. 2)
NOTE 4: The time when the sample is exposed is
u ⋅ ( 1 − RH )
crucial, and is to be kept as short as possible. where RH is the relative humidity (0.113 and
NOTE 5: In some cases where the particles are 0.331), and u is the moisture content of the
very fine (e.g. silica fume) or very porous, a longer conditioned specimen. The moisture content is
time is needed for conditioning. The time required calculated as:
to achieve constant mass for a specific type of
(m − mdry )
material, or particle size, can be determined by u= [kg/kg] (Eq. 3)
successive weighing at least 12 h apart and seeing mdry
that the mass does not differ by more than 0.005%.
where mdry is the mass of the oven-dry specimen
and m the mass of the conditioned specimen (m=m1
for 11.3% and m=m2 for 33.1%).

For gravel/aggregate, the removed particles not 6 TEST REPORT

passing the 0.5 mm sieve are to be compensated
for. The BET(H2O) surface area per unit specimen The report is to include necessary information from
mass calculated for the whole size fraction is among the following:
approximated as: a) Document ID (name, no., test method, etc.).
3.54 ⋅ 10 6
b) Date and time.
S ' BETH 2O = ⋅ (x05 + k ⋅ ( 1 − x05 )) (Eq. 4)
a+b c) Performer ID (name and address).
where k is a factor compensating for the removed d) Material ID, supplier and characteristics.
particles not passing the 0.5 mm sieve. For
gravels/aggregates with a maximum grain size up e) Date, location and method of sampling.*
to 8 mm, k ≈ 0.5 [-]. The mass fraction passing the f) Mass fraction passing 0.5 mm sieve (x05),
0.5 mm sieve is calculated as: expressed in percentage [%].*
m05 g) Maximum grain size (dmax), expressed in
x05 = [-] (Eq. 5) millimetres [mm].*
mtot
h) Mass of the analyzed specimen, expressed in
where m05 is the mass passing the 0.5 mm sieve grams [g].
and mtot is the total mass.
i) Specific surface area (SBETH2O), expressed in
Note 8: If there is only a small amount passing the square metres per kilogram [m2/kg].
0.5 mm sieve, the calculation of S´BETH2O is not valid.
For x05<0.1 the method is not recommended. j) Specific surface area for the whole size
fraction (S´BETH2O), in square metres per
It is not necessary to graphically plot the kilogram [m2/kg].*
relationship between the isotherm (y) and RH in
order to evaluate the variables a (interception) and k) Deviation in surface area, based on the double
b (slope). By using Eq. 2, Eq. 3 and the linear specimen results, expressed in percentage
relationship: [%].
y = b ⋅ RH + a [-] (Eq. 6) l) Time of conditioning in each climate,
expressed in days.
a and b can be calculated as:
m) Any deviation from the test method.
⎛ 0.1934 0.2565 ⎞⎟
a = mdry ⋅ ⎜ − n) Relevant visual observations and personal
⎜ ( m − m ) ( m − m ) ⎟ (Eq. 7) judgments and interpretations.
⎝ 1 dry 2 dry ⎠
⎛ 2.2696 0.5844 ⎞⎟ o) Date and signature.

b = mdry ⋅ ⎜ −
⎜ ( m − m ) ( m − m ) ⎟ (Eq. 8) Note 10: * only for gravel/aggregate, where also
⎝ 2 dry 1 dry ⎠
both SBETH2O and S´BETH2O are to be reported.
The specific surface area (SBETH2O) is to be
presented as a mean value based on the double
specimen results, together with a calculated 7 EXAMPLES
deviation.
To give an idea of the magnitude of the specific
Note 9: Adsorption is not the same for moisture as surface area by BET(H2O) for different materials,
for nitrogen gas. The water molecule is smaller the following approximate values are given:
than the nitrogen molecule (10.6 Å2 for water, and
16.2 Å2 for nitrogen), and has larger affinity forces Material SBETH2O S´BETH2O
(of attraction) due to its two-polar covalent bonds. [m2/kg] [m2/kg]
However, using water (moisture) is probably closer Limestone filler ~2 000
to real conditions in concrete production than using
Fly ash ~3 000
nitrogen gas. Silica fume ~20 000
Natural gravel (0-8 mm) ~4 000 ~2 500
Sea-sand (0-4 mm) ~1 500 ~1000


Box with tight lid Samples (2x)
y [kg/kg]
b
Fan
a
Net
0.113 RH [-] 0.331
(a) (b)
Figure 1. (a) Schematic illustration of climate box, and (b) the BET-plot with adsorption isotherm as a linear
function of RH.


Appendix B – Concrete digital dilatometer
APPENDIX B: CONCRETE DIGITAL DILATOMETER

LINEAR MEASUREMENT OF AUTOGENOUS DEFORMATION
IN FRESH AND HARDENING CONCRETE.


CONCRETE DIGITAL DILATOMETER (CDD):

LINEAR MEASUREMENT OF AUTOGENOUS DEFORMATION IN FRESH
AND HARDENING CONCRETE
Key words: Concrete, shrinkage, autogenous
1 SCOPE 4 NOTATIONS
This test method covers determination of concrete 4.1 Definitions
autogenous deformation. It has the ability to start
measurements before setting, when the concrete is Linear deformation; the relative change in length
fresh. The method is a modification of the CT1 due to shrinkage or expansion, referred to the
digital dilatometer for pastes and mortars. specimen’s original length.
As the use of high-performance and self- Autogenous deformation; the unrestrained, time-
compacting concrete has increased, problems with dependent bulk deformation of fresh and hardening
early-age shrinkage and cracking have become sealed concrete at a constant temperature.
significant. Conditions such as reduced water- Shrinkage; when the deformation is a contraction, it
cement ratio, reduced maximum aggregate size, may be referred to as shrinkage, e.g. autogenous
increased amount of fines, and increased binder shrinkage.
content all contribute to these problems. Compared
with drying shrinkage, which generally occurs from Chemical shrinkage; under sealed conditions, the
the outer surface of the concrete inward, cement paste hydration products occupy less
autogenous shrinkage develops uniformly through space than the original reactants. Most factors
the concrete member, but can be more likely to causing the autogenous shrinkage are chemical.
cause cracking, because it develops more rapidly
and occurs when the cement paste is young and
has poorly developed mechanical properties. 4.1 Symbols
l0 length of specimen at time of casting (when

2 FIELD OF APPLICATION measurements start), in millimetres [mm].
With the concrete digital dilatometer test, the fresh ∆l change in length of specimen at time t, in
and hardening concrete linear autogenous micrometres [µm].
deformation is evaluated. t time after mixing (when measurements
The test is only to be applied for laboratory use. start), in hours and minutes [hh:mm].
Maximum coarse aggregate size is 16 mm. ε relative change in length, defined positive
for shrinkage (negative for swelling), in
A concrete digital dilatometer (CDD) test is microstrain [µm/m].
preferably combined with:
T concrete cross section temperature, in
• Cracking tendency ring-test (NT BUILD 433) for degrese Celsius [ºC]
concrete.
• Digital dilatometer (CT1) test for cement paste. 5 METHOD OF TESTING

5.1 Principle
3 REFERENCES The concrete digital dilatometer is a test method for
CT1 digital dilatometer: Jensen O. M., Hansen F., evaluation of linear autogenous deformation of
“A dilatometer for measuring autogenous fresh and hardening concrete at sealed conditions
deformation in hardening Portland cement paste”, and constant ambient temperature.
Materials and Structures, Vol. 28(181), pp. 406- The concrete is cast in a vapour proof steel coil
409, 1995. reinforced flexible polyurethane (PU) tube mould
Sampling procedure: EN 12350-1, ASTM C172 or with inner diameter 82 mm and specimen length
NT BUILD 191. ~400 mm.
Cracking tendency test: NT BUILD 433.

The mould is placed in a mechanically stable 5.3.5 Casting

measuring rig, where the unrestrained, time-
dependent bulk deformation is recorded by a digital The specimen must completely fill the mould. If
gauge (1/1000 mm) at thermally controlled ambient needed, compaction by vibration.
conditions (20ºC) for a period of 24 hours or more. If temperature sensors - place one in the centre
The method is illustrated in Figure 1. and one at the surface of the mould cross-section.
The second end-caps (fixed end) are to be fitted to
the PE-tube with a house-clamp.
5.2 Apparatus
Required equipment and apparatus for a typical
test: 5.4 Procedure
• Thermally controlled room or chamber with an 5.4.1 Starting the test

air temperature of 20±1ºC. a) The specimen is to be placed in the measuring
• 2 or 3 complete CDD setups (mould consisting rig.
of PE-tube, end-caps, fixture and hose-clamps b) The mould is to be adjusted and fixed to the
and measuring rig), as shown in Figure 1. rig so that the digital gauge contact point is in
starting position.
• 1 set (2 off) of recording temperature sensors.
c) Reference length l0 (mould length excluding
• Table vibrator.
the end-caps, i.e. specimen length) is to be
• Ruler or gauge graded in 1/1 mm. measured to 1/10 mm.
• Stopwatch, measuring 1/1 sec (if manual d) The digital gauge is to be re-zeroed and its
reading of change in length). recording phase (time t and length change ∆l)
started.
e) If temperature sensors: start temperature T
5.3 Preparation of test specimen recording.
5.3.1 Mould The test must be performed in a thermally
The first end-cap (moving end) is to be fitted to the controlled room or chamber with an air temperature
PE-tube with a house-clamp. The mould is to be of 20±1ºC.
placed in a vertical support rack (e.g. a piece of The starting procedure (a-d) is to be performed
duct) to ensure stability during casting. within 20-30 minutes from adding water to the mix.
This time is to be noted. The initial measurements
are sensitive and it is recommended to let the
5.3.2 Mix sample set (or rest) in the rig for 10 minutes before
starting the measurements.
Concrete constituents’ volume is to be calculated to
1/1000 litre. Dry aggregate is preferable.
5.4.2 During the test
5.3.3 Mixing If manual reading, continuously record the time t,
length change ∆l and concrete temperature T.
A suitable concrete mixing method, mixer and
Enough sampling frequency is to be selected for
volume are to be selected and documented. No
smooth curve of shrinkage development.
standards are available.
Visual observation of specimen straightness;
possible curviness is to be measured and noted.
5.3.4 Sample
The sample size is 2.2 litres and is to be collected 5.4.3 Finishing the test
in accordance with EN 12350-1, ASTM C172 or NT
BUILD 191. Recording phase (t, ∆l and T) stops. Values are to
be transferred to computer for calculation and
Maximum coarse aggregate size is 16 mm. evaluation.

5.5 Expression of results c) Performer ID (name and address).

The shrinkage, ε, for each test specimen is to be d) Test object ID.
calculated as: e) Purpose of test.
∆l f) Concrete ID (producer, recipe, etc.).
ε= ⋅ 10 6 [in parts per million, e.g. µm per m]
l0 g) If relevant, concrete and/or air temperature.
The results are to be calculated as a mean value of h) Method of sampling.
two or three tests, and are to be given in
i) Time from water addition to sampling start.
microstrain with two significant digits.
j) Reference length (l0), i.e. specimen length.
The shrinkage must be corrected for the recorded
concrete cross section temperature (T). Adequate k) Storage conditions.
thermal expansion coefficient is to be applied.
l) Test results (t, ∆l and T).
The development of shrinkage (ε) with time (t) is to
m) Relevant visual observations (e.g. sample
be presented graphically.
curviness) and personal judgments and
interpretations.
6 TEST REPORT n) Any deviation from the test method.
The report should include necessary information o) Graphic presentation of shrinkage (ε)
from among the following: development with time (t).
a) Document ID (name, no., test method, etc.). p) Inaccuracy and/or uncertainty of test results.
b) Date and time. q) Date and signature.
Mould length 460 mm

Specimen length 400 mm
Didital gauge
Mould diameter 82 mm 1/1000 mm
Adjustable
fixture
0 001
0 001
Figure 1. Principe of the Concrete Digital Dilatometer (CDD) for autogenous measurement.


Appendix C - Concrete cracking ring test
APPENDIX C: CONCRETE CRACKING RING TEST

CRACKING TENDENCY MEASUREMENT DUE TO DRYING
DEFORMATION THE FIRST 24 HOURS


CONCRETE CRACKING RING TEST:

CRACKING TENDENCY MEASUREMENT DUE TO DRYING DEFORMATION
THE FIRST 24 HOURS
Key words: Concrete, cracking, shrinkage, drying
1 SCOPE 3 REFERENCES
This test method covers determination of concrete Sampling procedure: EN 12350-1, ASTM C172 or
cracking tendency at early ages. The test is NT BUILD 191.
performed on 3 restrained ring-shaped specimens,
Cracking tendency test: NT BUILD 433
exposed to an air stream of defined velocity,
temperature and relative humidity, for the first 24
hours after casting.
4 NOTATIONS
The principle of the test is that the concrete sample
is cast around a restraining inner steel ring, causing 4.1 Definitions
a development of tangential stresses, which if Shrinkage: when the deformation is a contraction, it
sufficiently high may lead to cracking. The may be referred to as shrinkage, e.g. autogenous or
evaluation is based on characterization of the cracks drying shrinkage.
in terms of average total area in the three samples.
Autogenous shrinkage: the unrestrained, time-
The method is a modification of the Nordtest method dependent bulk deformation of fresh and hardening
“NT BUILD433”. sealed concrete at a constant temperature.
Problems with early-age shrinkage and cracking Chemical shrinkage: under sealed conditions, the
have become significant. Conditions such as cement paste hydration products occupy less space
reduced maximum aggregate size, increased than the original reactants. Most of the factors
amount of fines, presence of retarding admixtures, causing the autogenous shrinkage are chemical.
increased binder content and deficient covering and
curing all contribute to these problems. Evaporation shrinkage: when water evaporates from
the fresh and hardening concrete, tensile stress
Most probably the plastic shrinkage also consists of builds up in the capillaries, causing the concrete to
autogenous shrinkage. Compared with autogenous contract. In early stages; drying shrinkage can be
shrinkage, which generally develops uniformly defined as plastic shrinkage.
through the concrete member, shrinkage due to
evaporating occurs from the outer surface of the
concrete inward, causing cracks that develop 4.1 Symbols
rapidly, and occurs when the cement paste is young
and has poorly developed mechanical properties.
n number of cracks of each specimen.
l length of each crack, in millimetres [mm].
2 FIELD OF APPLICATION w each crack average width, in millimetres
With the “Concrete cracking ring test”, the plastic [mm].
and hardening concrete cracking tendency can be A average total crack area calculated from two
used for an evaluation of different types of concrete ore more samples, in sq. millimetres [mm2]
exposed to early drying.
t time after mixing, in hours [h].
The test is only to be applied for laboratory use,
where the method information is relative and cannot ∆m sample weight loss due to drying, in
predict the extent of cracking which might occur kilograms [kg].
under prevailing conditions. E sample evaporation, in kilograms per sq.
Maximum coarse aggregate size is 16 mm. metre [kg/m2].
The concrete cracking ring test is preferably v air velocity, in metres per second [m/s].
combined with: RH air relative humidity, in percentage [%].
• Volume or linear measurement of autogenous Ta air temperature, degrees Celsius [ºC].
deformation, e.g. Concrete Digital Dilatometer
(CDD) test for concrete. Tc concrete temperature, degrees Celsius [ºC].

5 METHOD OF TESTING 5.3 Preparation of test specimen

5.1 Principle 5.3.1 Mould
When water evaporates from the fresh concrete, the The inner and outer steel rings are fixed on a stiff
concrete tends to contract, and as contraction is base steel plate with a smooth surface. The steel
restrained, tangential tension develops across a rings are to be covered with a thin layer of form oil
section of the ring specimen. The extent of cracking and the base plate is not to be oiled.
depends both on the magnitude of the tensile forces
and on the strain capacity of the concrete.
The concrete is cast between two concentric steel 5.3.2 Mix
rings with diameters 300 and 600 mm, and with a Concrete constituents by dry weight are to be
depth of 80 mm; see Figure 1. The steel rings have recorded. Max. coarse aggregate size is 16 mm.
ribs attached to provide crack initiation and are fixed
to a stiff base plate with a smooth surface. After
casting, the ring specimens are positioned under air 5.3.3 Mixing
funnels with a 10 mm opening between the concrete
surface and the funnel along the circumference of A suitable concrete mixing method, mixer and
the outer ring. The funnel is shaped to provide equal volume are to be selected and documented. No
wind velocity across the concrete surface of 4.5 m/s. standards are available.
The test is to be performed at stable and constant
environmental conditions, where one of the samples
is to be placed on a balance. 5.3.4 Sample
The cracking tendency is evaluated from crack The sample size is 17 litres (x3) and is to be
length and average width measurements on the collected in accordance with EN 12350-1, ASTM
concrete top surface. C172 or NT BUILD 191.
5.2 Apparatus 5.3.5 Casting

Required equipment and apparatus for a typical test: The concrete is to be sampled from the mixer
immediately after the end of mixing period. The
• Thermal and humidity-controlled room or casting of 3 ring specimens must be accomplished
chamber with a constant air temperature of within 30-45 minutes after water addition.
T=20±1ºC and relative humidity of RH=35±5%.
The conditions’ magnitudes are not absolute, The specimen must completely fill the mould (to the
but these are preferable. top of the inner and outer steel rings). If needed,
compact by vibration. Top surfaces are to be
• 3 complete mould setups for ring specimen, as smoothed in a corresponding manner.
shown in Figure 1.
• 3 sets of air funnels, including fan and ducting,
as shown in Figure 1. 5.4 Procedure
• Balance (load cell) with manual reading or 5.4.1 Starting the test
automatic recording of weight changes.
a) One of the specimens is to be placed on the
• Devices and instrumentation for manual reading balance.
or automatic recording of: b) Each specimen’s horizontal position is to be
- air velocity ensured (if unsure, use a water level).
- temperature and relative humidity of air
- concrete temperature. c) One concrete temperature sensor is to be
placed in the centre of the mould cross-section.
• Ruler or measuring wheel graded in 1/1 mm.
d) The air funnels are to be placed in such a way
• Water level. that the opening between the concrete surface
• Stopwatch, measuring 1/1 sec. and the funnel edge is uniform (10 mm) along
the whole circumference of the outer steel ring.

e) The fans are to be started 55 minutes after 5.5 Expression of results

water addition. Velocity over the concrete
surface is to be ensured (4.5 m/s) The total crack area for each ring is to be calculated
as the accumulated sum over each average crack
f) The recording phase (time t, concrete width multiplied by its length. The average total
temperature Tc, specimen weight loss ∆m, air crack area (A) is expressed by the average area for
temperature and humidity Ta and RH) is to be 3 rings, rounded to the nearest 0.1 mm, as:
started 60 minutes after water addition.
3 n
The test is to be performed in a thermal, humidity-
stable and controlled room or chamber with an air
∑( ∑( l
j =1 i =1
i ⋅ wi ) )
temperature of 20±1ºC. and relative humidity of A= [mm2]
3
35±5%.
The water evaporation (E) is calculated by the
The starting procedure (a-d) is to be performed
quotient of weight loss (∆m) and ring surface area:
within 60 minutes from water addition, if not this time
is to be noted. ∆m
E= [kg/m2]
0.212
5.4.2 During the test The development of concrete temperature (Tc) and
evaporation (E) with time (t) is to be presented
If manually reading, continuously record the time t,
graphically.
concrete temperature Tc, specimen weight loss ∆m,
air temperature and humidity Ta and RH. Enough
sampling frequency is to be selected for a smooth
curve of temperature and weight loss development 6 TEST REPORT
(less than 1/2 hours interval). The report is to include necessary information from
Visual observation of specimens throughout the 24 among the following:
hours can be made in order to describe the crack a) Document ID (name, no., test method, etc.).
development. The type, orientation and time of
occurrence of cracks can then be noted. b) Date and time.
c) Performer ID (name and address).
5.4.3 Finishing the test d) Test object ID.
The recording phase (t, Tc, ∆m, Ta and RH) stops. e) Purpose of test.
Values are to be transferred to computer for f) Concrete ID (producer, recipe, etc).
calculation and evaluation.
g) Identification of the test equipment and
instruments used.
5.4.3 Crack measurements h) Method of sampling.
The ring specimens should normally be examined i) Time from water addition to sampling start/stop
after 24 hours’ exposure, and surface cracks with an and crack measuring.
approximate radial orientation should be identified
j) Air velocity (v), temperature (ta) and humidity
and marked in an adequate way. The average width
(RH) during the test.
(w) and length (l) of each crack are to be measured
and recorded. The width measurements shall be k) Test results: number of cracks (n), total crack
performed by the use of the magnifying glass and area (A) and graphical presentation of concrete
readings by interpolation to the nearest 0.02 mm. It temperature and evaporation (t, Tc and E).
is recommended that a lower crack limit is 0.05 mm.
The main crack pattern of each ring can be recorded l) Relevant visual observations and personal
by photo or sketched by drawing. judgments and interpretations.
The standard procedure also includes recording of m) Any deviation from the test method.
weight loss and temperature development. These n) Inaccuracy and/or uncertainty of test results.
parameters give useful information about the
evaporation of water, and serve as a control for o) Date and signature.
identical tests as well.

Air flow 310 m3/h
Fan
Adjustable damper
Duct ø100 mm
Transparent air funnel

Min 1000 mm
Distances 10 mm
Steel rings ø600/300 mm
Air velocity 4.5 m/s
Base plate with

smooth steel surface
Test arrangement
30°
120°
Distances
h=10 mm
Transparent, e.g.
Plexiglass, t=4 mm Steel ribs 80 x 25 x 3 mm,
25
12 pcs on outer & 3 pcs on inner ring
11°
51
80
ø100
6
ø612
ø300 (outer)
ø600 (inner) 6
Transparent air funnel Ring mould setup
Figure 1. Principe of the concrete cracking ring test for cracking tendency measurement.

Appendix D - Glossary
APPENDIX D: GLOSSARY
The following terminology, related to the subject matter in this work, has been adopted.
Thus some modification from its origins is made (see references at end of this appendix).
This glossary is intended as a reader’s aid. The explanations given here are not rigorous
definitions and should not be regarded as such. Formal definitions may be found in
documents such as:
o ASTM Standard C125 “Standard terminology relating to concrete and concrete
aggregates”
o British Standard BS5168 “Glossary of rheological terms”
o ACI Manual 116R “Cement and concrete terminology”
o European standard EN 197-1 “Cement”, EN 206-1 “Concrete”, EN 934-2
“Admixtures for concrete”, EN 12620 “Aggregates for concrete”
Definitions regarding fresh concrete and mortar and its constituents are fairly well defined
in literature and standards. However, an established and standardized terminology is
somewhat more deficient regarding the subject of early-age deformation, and especially
autogenous deformation.
admixture: A material other than water, aggregates, and cement, that is used as an ingredient of
concrete and is added to the bath before and during the mixing operation.
adsorbate: A substance that is adsorbed at the interface of a substrate material.
adsorbent: The substrate material onto which a substance is adsorbed.
adsorption hysteresis: The adsorption and desorption curves’ deviation from one another. Generally
explained as due to the ink-bottle effect.
adsorption isotherm: A graphical representation of the relationship between the bulk activity of
adsorbate and the amount of adsorbate at constant temperature.
adsorption: Development at the surface of a solid of a higher concentration of a substance than what
exists in the bulk of the medium. For aggregate, concrete and cement, adsorption is the formation of a
layer of water at the surface of a solid held by either physical and/or chemical forces.
aerosol: Droplets or particles dispersed in a gaseous phase.
aggregate: Granular material, such as sand, gravel, crushed stone, or crushed concrete, used with a
hydraulic cementing medium to produce either concrete or mortar.
aggregation: A general term defined as any process by which particles collect to form a cohesive mass
or cluster structure.
anti-thixotropy: See negative thixotropy.
apparent density: The density of loose or compacted particulate matter determined by dividing actual
weight by volume occupied; apparent density is always less than true density of a material comprising
the particulate matter, because volume occupied includes the space devoted to pores or cavities between
particles (see apparent particle volume).
apparent particle volume: The total volume of the particle excluding open pores, but including closed
pores.
apparent viscosity, The quotient of shear stress divided by shear rate when the this quotient is

dependent on rate of shear ( η app = ∂σ / ∂γ& ).

apparent yield stress: For non-ideal viscoplastic materials (e.g. concrete), where the yield stress is
indefinite. An apparent yield stress can be defined by extrapolation from the linear shear rate of the
flow curve to the shear stress axis (see Bingham model).
autogenous shrinkage: The unrestrained, time-dependent bulk deformation of fresh and hardening
sealed homogeneous cement paste, mortar or concrete at a constant temperature (isothermal).
BET: A gas adsorption technique for determination of the specific surface area of porous materials,
named after Brunauer, Emmett and Teller. The BET surface area is the area on which gas molecules,
such as N2 or O2, can adsorb.
Bingham model: A mathematical model used for describing viscoplastic flows exhibiting a yield
response. The ideal Bingham material is an elastic solid at low shear stress values and a Newtonian
fluid above a critical value called the yield stress. The plastic viscosity region exhibits a linear
relationship between shear stress and shear rate, with a constant plastic viscosity ( σ = σ 0 + γ& ⋅ η pl ).
Fresh cement paste, mortar or concrete, under certain conditions, and the Bingham model are
traditionally used for defining the rheological properties.
Blaine fineness: The fineness of granular materials such as filler, cement and pozzolan, expressed as
total surface area in square centimetres per gram, determined by the Blaine air-permeability apparatus
and procedure.
bleeding: The separation of water or paste from a fresh mix, usually caused by the settlement of the
solid constituents. Bleeding is sometimes considered a form of segregation.
Brownian motion: The random movement of small particles in a dispersed phase due to bombardment
by molecules of the surrounding medium (see colloidal).
bulk density: The mass of a material per unit volume (including solid particles, voids and pores).
Compaction increases bulk density by reducing pore spaces. Bulk density is used interchangeably with
unit weight.
cement paste: Constituent of concrete, consisting of cement and water.
cement: A powdery substance made by burning, at a high temperature, a mixture of clay and limestone
– producing lumps called “clinkers” which are ground into a fine powder consisting of hydraulic
calcium silicates.
chemical shrinkage: Under sealed conditions, the absolute volume reduction associated with the
hydration reactions in cementitious materials. The products of hydration occupy less space than the
original reactants. Most of the factors causing the autogenous shrinkage are chemical.
coarse aggregate: A general term for aggregate of such size that it is substantially retained on a sieve
of specified size, commonly 8.0, 4.0 or 4.75 mm.
cohesiveness: Ability of mix to resist segregation during transportation and placement.
colloidal: State of subdivision implying that the particles have at least in one direction a dimension
roughly between 1 nm and 1 ?m. Colloids are significantly affected by Brownian motion when
suspended in a liquid.
compactness: A shape measure, calculated as the ratio between the diameter of a circle with the same
area as measured and the maximum elongation of the measured area. At 1, the object is circular.
concrete: A composite material that consists essentially of a binding medium in which are embedded
particles or fragments of relatively inert material filler. In Portland cement concrete, the binder is a
mixture of Portland cement and water; the filler may be any of a wide variety of natural or artificial
aggregates.
consistency: The relative mobility or ability of fresh concrete or mortar to flow, usually measured with
free flow techniques (e.g. slump for concrete and slump flow for mortar).
continuous phase: Constituting the medium, a phase that exhibits continuity throughout the dispersion.
E.g. the liquid in a suspension.

creep: The response of a material to the instantaneous application of a constant stress.

Deborah number: The ratio of a characteristic relaxation time of a material to the duration of the
observation. In equilibrium flow, the effective duration of the experiment is infinity, and De=0.
deformation coefficient: A measure of the sensitivity of increased water content.
deformation: Movement of parts or particles of a material body relative to one another such that the
continuity of the body is not destroyed, resulting in a change of shape, volume or both.
density: Mass per unit volume. For concrete and mortar density, the bulk density is normally
substituted, but for the constituents it is the density of solids or the apparent density (interchangeably
with specific gravity).
desorption: The process by which the amount of an adsorbed substance is reduced.
dilatant: A property often associated with suspension of irregularly shaped particles, in which the
liquid exhibits an increase in volume while being sheared. The term 'dilatant' is commonly used in
practice to indicate shear-thickening, although this usage is strictly incorrect.
disjointing pressure: Repulsing pressure due to adoption of water molecules acting in locations where
the distance between two surfaces is restricted. The forces acts in the range of 40-100% RH, increasing
with increased RH.
dispersed phase: In a dispersion, the phase that is distributed in the form of discrete discontinuities
(particles, droplets or bubbles).
dispersion: A two-phase system in which discontinuities of any kind (solid, liquid, gas) are dispersed in
a continuous phase of a different composition or state. In the field of cementitious materials, dispersion
is used to describe a suspension of solid particles in a liquid medium (see suspension).
drying shrinkage: Contraction caused by the loss of water from the hardened cementitious material.
Similar to the term 'evaporation shrinkage', but reserved for hardened state.
elastic: A conservative property in which part of the mechanical energy used to produce deformation is
stored in the material and recovered on release of stress.
electrical double layer: A model for the situation at a charged solid surface in solution, where ions of
opposite charge are attracted to the surface but try to diffuse away and remain uniformly distributed in
the solution, resulting in two plates of an electrical condenser ? the charged surface and a balancing
charge in solution spread over a short distance from the surface.
elongation: A shape factor, defined by the ratio of length to width of a rectangle with sides parallel to
the longest dimension of particles.
emulsion: A dispersion consisting of two or more liquid phases.
equilibrium (steady-state) flow: Condition under which constant stress or shear rate is maintained for
sufficient time to allow a steady state to be achieved in a fluid containing time-dependent structure
(such as concrete). An equilibrium flow curve can be used to characterize the time-dependent flow
properties of a material (e.g. thixotropy).
error: Result of a measurement minus the value of the measurand.
evaporable water: Water set in cement paste present in capillaries or held by surface forces; measured
as the water removable by drying under specified conditions.
evaporation shrinkage: When water evaporates from the fresh and hardening cementitious materials,
tensile stress builds up in the capillaries, causing the cement paste, mortar or concrete to contract.
Evaporation shrinkage is generally reserved for the loss of water at early ages, whereas drying
shrinkage is reserved for the long-term loss.
F-circle: A shape measure, calculated as the ratio of measured area to the area of a circle with the same
perimeter as that measured. At 1, the object is circular.
Feret diameter: Geometrically defined as the perpendicular distance between parallel lines tangential
to the perimeter at opposite sides of a 2D object in a certain direction. When measuring the Feret
diameter in several predetermined directions, the obtained maximum value is the maximum Feret
diameter.

filler: A general term for very fine granular material of solid material, usually inert and less than
roughly 0.125 mm, which occupies space and may improve physical properties or lower costs. Filler
can either be an additive or a fine fraction of aggregate (see powder).
filling ability: The concrete's ability to flow into and fill the mould.
final setting: Structural phase of the cementitious system matrix transforming to a true rigid, controlled
by its hydration. The final setting is manifested by an increasing strain capacity and a distinct decreased
rate of autogenous deformation. At the transitional period between initial and final set, the matrix
changes from true fluidity to true rigidity state.
fine aggregate: A general term for aggregate of such size that it substantially passes a sieve of specified
size, commonly 8.0, 4.0 or 4.75 mm.
fineness modulus: An index of fineness or coarseness of an aggregate sample. An empirical factor
determined by adding total percentages of an aggregate sample retained on each of a specified series of
sieves, and dividing the sum by 100.
fines: Material in aggregate finer than a given sieve, usually the 0.125 or 0.074 mm sieve (see powder).
Used for expressing the amount of fine aggregate in a concrete mixture as a percent by absolute volume
of the total amount of aggregate.
flocculation: The process by which particles in a suspension are mutually attracted by a combination of
van der Waals and electrostatic forces, stick together to form agglomerates and either settle out of the
suspension as flocs or form a three-dimensional network throughout the suspension.
flow curve: A graphical representation of the material's flow behaviour in which shear stress is related
to shear rate. The flow curve is a type of rheogram.
flow hysteresis: A condition resulting from differences in the rate of energy dissipation due to shear
history. In a typical rheometric test, shear stress or shear rate is ramped at a fixed speed up to a
maximum value, and then ramped back down at the same speed to the beginning. In hysteresis, one
flow curve lies above the other, forming a continuous loop whose internal area depends on the shear
and thermal history of the material, and on how rapidly the stress or shear rate was ramped. If the
down-curve lies below the up-curve, then it is referred to as a thixotropic loop, whereas if the down-
curve lies above the up-curve, then it is called a negative thixotropic loop. The area enclosed in this
loop is a commonly used measure of thixotropy/anti-thixotropy.
flow: Time dependent irrecoverable deformation.
flowability: A measure of the consistency of freshly mixed concrete, mortar, or cement paste. Usually
expressed in terms of spread diameter of a slump flow test (see workability).
fluidity: The reciprocal of viscosity.
free moisture: Moisture having essentially the properties of pure water in bulk; moisture not absorbed
by aggregate. See also surface moisture.
F-shape: A shape measure, calculated as the ratio of the length of the minor axis to the length of the
major axis. If the elongation is 1, the object is roughly circular or square.
grading: See size distribution.
grout: A mixture of cementitious material and water, with or without aggregate, proportioned to
produce a pourable consistency without segregation of the constituents; also, a mixture of other
composition but of similar consistency.
Herschel-Bulkley: A three-parameter rheological model used to describe viscoplastic materials
exhibiting a yield response with a shear-thinning relationship above the yield stress.
hydration: Chemical reaction which takes place as a result of combining cement and water. Maximum
hydration equals maximum potential strength of cementitious materials.
initial setting: Transition phase of cementitious system when the matrix changes from a concentrated
suspension of flocculated particles to a viscoelastic skeletal solid capable of supporting an applied
stress. At initial setting, capillary pore pressure rises significantly. Before initial setting, the chemical
shrinkage is equal to the autogenous shrinkage, and furthermore, the total shrinkage will transform into

settlement.
linear deformation: The relative change in length due to shrinkage or expansion, referred to the
specimen origin length.
liquid phase: Consisting of a condensed fluid, e.g. the dispersion or suspending media in a suspension.
mixing water: The water in freshly mixed sand-cement grout, mortar, or concrete, exclusive of any
previously absorbed by the aggregate (e.g., water considered in the computation of the net water-cement
ratio). See also surface moisture.
mobility: An ability of a fresh mix to flow and fill formwork or other container spaces.
moisture content of aggregate: The ratio, expressed as a percentage, of the weight of water in a given
granular mass to the dry weight of the mass.
monolayer adsorption: Adsorption in which only a single layer of molecules becomes adsorbed at an
interface. In monolayer adsorption, all adsorbed molecules are in the position of closest approach to the
substrate surface.
mortar: Concrete with essentially no aggregate larger than about 4 mm, i.e. a mixture of cement, sand
and water.
negative thixotropy: A reversible time-dependent increase in viscosity at a particular shear rate.
Shearing causes a gradual growth in structure over time (see flow hysteresis).
Newtonian: A flow model of fluids in which a linear relationship exists between shear stress and shear
rate, where the coefficient of viscosity is constant with shear rate ( σ = γ& ⋅ η ).
particle phase (or solid phase): The particles in a suspension, gel or aerosol.
particle size distribution: The division of particles of a graded material among various sizes; for
concrete materials, usually expressed in terms of cumulative percentages larger or smaller than each of
a series of diameters or the percentages within certain ranges of diameter, as determined by sieving.
particle: Any condensed-phase three-dimensional discontinuity in a dispersed system may generally be
considered a particle. The term is normally used in reference to solid materials. An aggregate may also
be regarded as a particle.
passing ability: The concrete's ability to flow through narrow spaces and prevent blocking around
reinforcements.
paste: The fraction of concrete comprising powder (including cement), water, air and admixtures.
plastic shrinkage: Net sum of early-age volume changes, including autogenous shrinkage and
shrinkage due to loss of water caused by evaporation, the aggregates' and filler materials' adsorption and
absorption, and suction of water by sub-base or formwork material.
plastic viscosity: The excess of shear stress over yield stress divided by the shear rate (see Bingham
model). In a flow curve, the viscosity is represented as the slope of the curve. For concrete, mortar or
other non-Newtonian materials, the term is often used synonymously with viscosity.
plastic: The property of a solid body that is in the elastic state when the stress is below a critical value,
termed the yield stress, and in plastic state when this value is exceeded.
plasticizer: An admixture which increases workability/flowability of freshly mixed mortar or concrete
without increasing water content. Also known as water-reducing admixture because it can maintain the
same workability/flowability of the mix with reduced water content.
plug flow: Flow in a pipe of a material that possesses a yield value (see yield stress). Because of the
existence of the yield value, flow starts near the surface of the pipe and the material flows forward as a
solid plug (i.e. the core of the material has a zero velocity gradient).
porosity: The ratio, usually expressed as a percentage, of the volume of voids in a material to the total
volume of the material, including voids.
Portland cement: A finely pulverized clinker produced by burning mixtures containing lime, iron,
alumina, and silica at high temperature and in definite proportions, and then intergrinding gypsum to
give the properties desired.

powder: A general term for relatively dry, undispersed accumulation of very fine granular material of
solid material including cement and those having a fineness equal to cement. Maximum dimension in
any given direction is less than roughly 0.125 or 0.074 mm. It will also include this size fraction of
aggregate.
precision: The degree of agreement within a set of observations or test results obtained as directed in a
test method.
pseudoplastic: See shear thinning.
relative humidity: The ratio of the quantity of water vapour actually present to the amount present in a
saturated atmosphere at a given temperature; expressed as a percentage.
relaxation time: A time characterizing the response of a viscoelastic material to the instantaneous
application of a constant strain.
repeatability: Variability of independent test results obtained on the same material, with the same
equipment, and by the same operator.
reproducibility: Variability of the replicated results of same test method, obtained on identical material
performed by different operators using different equipment.
retained water ratio: The amount of water, adsorbed on the particle surfaces and filling the voids in
the particle system, needed to initiate flow.
retardation time: A time characterizing the response of a viscoelastic material to the instantaneous
application of a constant stress.
rheology: The science of the deformation and flow of matter.
rheometer: An apparatus for measurement of rheological properties.
rheopexy: An effect by which a material recovers some of its pre-sheared viscosity at a faster rate when
it is gently sheared compared to when it is allowed to stand. The term 'rheopexy' is commonly used in
practice to indicate negative thixotropy, although this usage is strictly incorrect.
robustness: The concrete's ability to resist deviation in the constituents' proportions (water, cement,
aggregate and additives) and properties (gravel moisture content, aggregate grading, etc.).
roundness: The ratio of the average radius of curvature of the several edges of corners of a particle to
the radius of curvature of the maximum inscribed sphere.
sand: The fine granular material (usually passing the 4 mm sieve and predominantly retained on the
0.125 mm) resulting from the natural disintegration of rock, or from the crushing of friable sandstone.
saturation: The condition of coexistence in stable equilibrium of either a vapour and a liquid or a
vapour and solid phase of the same substance at the same temperature. Applied to aggregate or
concrete, the condition such that no more liquid can be held or placed within it.
segregation: A loss of uniformity of fresh concrete mix. A separation of one or more of the constituents
of the mix with consequent non-uniform proportions.
self-compacting concrete: A modified standard concrete that, without the influence of additional
compaction energy, flows, de-airs and completely fills the formwork only under the influence of its
own gravity weight. It has to combine high fluidity with a high segregation resistance and has to be able
to carry coarse aggregate grains through narrow spaces.
self-desiccation: Lowering of internal relative humidity in a closed isothermal cement paste system due
to the consumption of capillary water and the chemical shrinkage from progress of cement hydration.
separation: The tendency, as concrete is caused to pass from the unconfined ends of chutes or
conveyor belts, for coarse aggregate to separate from the concrete and accumulate at one side; the
tendency, as processed aggregate leaves the ends of conveyor belts, chutes, or similar devices with
confining sides, for the larger aggregate to separate from the mass and accumulate at one side; the
tendency for solids to separate from the water by gravitational settlement. See also bleeding and
segregation.
setting: Onset of solidification in a plastic cement paste system. The beginning of solidification,
referred to as initial set, marks the point in time when the paste loses its plasticity, becomes unworkable

and is capable of supporting an applied stress.

settlement: Vertical displacement in cementitious materials before initial setting, which is caused by
bleeding, chemical shrinkage, etc.
shear rate: The change of shear strain with time (dγ/dt). For fluids, the shear rate, rather than the strain,
is generally used in describing flow.
shear strain: The relative deformation of shear divided by the separation distance of shearing forces.
Alternatively, the shear strain can be defined as tan(θ), where θ is the angle of deformation.
shear stress: The component of stress that causes successive parallel layers of a material body to move,
in their own planes, relative to each other.
shear thickening: An increase in viscosity with increasing shear rate during steady shear flow (not to
be confused with dilatant).
shear thinning: A decrease in viscosity with increasing shear rate during steady shear flow.
shear: The relative movement of parallel adjacent layers.
shrinkage: When the deformation is a contraction, it may be referred to as shrinkage, e.g. autogenous
or drying shrinkage.
sieve analysis: The classification of particles, particularly of aggregates, according to sizes as
determined with a series of sieves of different openings.
size distribution: The distribution of particles of granular material among various sizes, usually
expressed in terms of cumulative percentages larger or smaller than each of a series of sizes (sieve
openings) or the percentages between certain ranges of sizes (sieve openings). Also named grading.
slump flow test: A commonly used consistency test method for determination of vertical slump flow
spread and velocity of highly flowable concrete and mortar, expressed in terms of average spread
diameter and flow time. Also named spread flow cone test.
slurry: A concentrated cement-based particulate suspension.
sol: A liquid dispersion containing particles of colloidal dimensions.
specific surface area: The total (external and corresponding internal) surface area per unit weight or
unit volume.
sphericity: The degree to which a particle approaches a spherical shape, defined as the ratio between
the diameter of a sphere with the same volume as the particle and the diameter of the circumscribed
sphere.
stability: The concrete's capability of retaining homogeneous, i.e. resisting segregation and bleeding
during handling or placing of the mix. Also named segregation resistance.
stress growth: An increasing stress vs. time or modulus vs. time function is termed stress growth, when
an instantaneous and constant strain (or shear rate) is applied to a material while stress is measured over
time.
stress relaxation: A decreasing stress vs. time or modulus vs. time function is termed stress relaxation,
when an instantaneous and constant strain (or shear rate) is applied to a material while stress is
measured over time.
stress: Force per unit area (σ=F/A).
structure: In rheology, structure is a term that refers to the stable physical bounds between particles in
a fluid. These bounds result in aggregates, flocs or network structures, which impact the fluid and
provide elastic and plastic properties.
subsidence: See settlement.
superplasticizer: A high-efficiency plasticizer (see plasticizer).
surface moisture: Water retained on surfaces of aggregates capable of mixing with Portland cement in
concrete; distinguished from absorbed moisture, which is contained inside the aggregate particles.
surface texture: Degree of roughness or irregularity of the exterior surfaces of aggregate particles or

hardened concrete.
surface voids: Cavities visible on the surface of a solid. See also porosity and surface texture.
suspension: A liquid in which solid particles are dispersed (see dispersion).
thixotropy: A reversible time-dependent decrease in viscosity at a particular shear rate. Shearing causes
a gradual breakdown in structure over time. The thixotropy is a measure of applied work needed to
break down the structure. In a flow curve, the thixotropy causes a flow hysteresis effect (see flow
hysteresis). Note that thixotropy is a reversible phenomenon; the term is often used wrongly in concrete
technology to describe an irreversible change.
van der Waals force: A short-range electromagnetic force interacting between two non-polar
molecules (or atoms), where the force arises when the molecules become polar for a short time because
their electrons are in constant motion. This motion is usually balanced or symmetrical around the non-
polar molecule, but if the electrons are briefly disturbed their negative charge may increase at one part
of the molecule, creating a positive charge on another part of the molecule. The molecule becomes a
dipole for a short time until the electrons rebalance, disturbing electrons in neighbouring molecules,
turning them into dipoles as well. The force also acts between macroscopic bodies, as particle-particle
and particle-surface, where if two solid surfaces are brought close together, all the atoms in the surface
zones will contribute to the forces of attraction. The van der Waals forces are much weaker than the
force that arises from electrostatic charged particles, but are strong enough to hold some particles
together.
vapour pressure: The pressure exerted by a vapour that is calculated from relative humidity and
temperature. The higher the humidity, and the higher the temperature in degrees Celsius, the greater the
vapour pressure exerted.
viscoelastic: A time-dependent property in which a material under stress produces both a viscous and
an elastic response. A viscoelastic material will exhibit viscous flow under constant stress, but a portion
of mechanical energy is conserved and recovered after stress is released.
viscoplastic: A hybrid property in which a material behaves like a solid below some critical stress
value, the yield stress, but flows like a viscous liquid when this stress is exceeded. Often associated
with aggregated particle suspensions (e.g. mortar and concrete).
viscosity: The property of a Newtonian material to resist increased deformation increasingly with
increasing rate of deformation. It is determined as the ratio of shear stress to shear rate ( η = σ / γ& ) in a
steady flow. For concrete or other non-Newtonian materials, often used synonymously with plastic
viscosity (or apparent viscosity).
viscous: The tendency of a liquid to resist flow as a result of internal friction.
water-cement ratio: The ratio of the amount of water, excluding only that absorbed by the aggregates,
to the amount of Portland cement in a concrete or mortar mixture; preferably stated as a decimal by
weight.
workability loss: The amount by which the workability of freshly mixed concrete changes during a
period of time after the initial mixing. Traditionally expressed in terms of the decrease in spread
diameter of a flow cone test.
workability: A general term relating to behaviour of fresh concrete, comprising a number of
characteristics of parameters obtained from different tests. A commonly used definition is: “that
property of freshly mixed concrete or mortar which determines the ease with which it can be mixed,
placed, consolidated and finished”. Usually expressed in terms of spread diameter of a slump flow test
(see flowability).
yield stress: A critical shear stress value below which an ideal plastic (Bingham-plastic) or viscoplastic
material behaves like a solid (i.e., will not flow). Once the yield stress is exceeded, a plastic material
yields (deforms plastically) while a viscoplastic material flows like a liquid. For non-ideal viscoplastic
materials (e.g. concrete), where the yield stress is indefinite, an apparent yield stress can be defined by
extrapolation from the linear shear rate of the flow curve to the shear stress axis (see Bingham model).
Z-potential: A suspended charged particle in a solution attracts ions of opposite charge to those at its

surface, where they form the Stern layer. To maintain the electrical balance of the suspending fluid, ions
of opposite charge are attracted to the Stern layer. The potential at the surface of the part of this diffuse
double-layer of ions that can move with the particle when subjected to a voltage gradient is the zeta-
potential. The magnitude of the Z-potential is approximately proportional to the surface charge on the
particle.
References:
Bartos P., “Fresh concrete: Properties and tests”, Department of Civil Engineering, Paisley College,
Scotland, 1992.
Bentur A., “Terminology and definitions”, RILEM report 25: Early Age Cracking in Cementitious
Systems, RILEM TC181-EAS, pp. 13-15, 2002.
EFNARC, “Specifications and guidelines for self-compacting concrete”, European Federation for
Specialist Construction Chemicals and Concrete Systems, Farnham, 2002.
EFNARC , “European guidelines for self-compacting concrete: Specification, production and use”,
European Federation for Specialist Construction Chemicals and Concrete Systems, Farnham, 2005.
Hackley V. A., Ferraris C. F., “Guide to rheological nomenclature: Measurements in ceramic
particulate systems”, NIST special publication, No 946, National Institute of Standards and
Technology, Washington, 2001.
Hackley V. A., Ferraris C. F., “The Use of Nomenclature in Dispersion Science and Technology”,
NIST publication No 960-3, Washington, 2001.
Holt E.E., “Early age autogenous shrinkage of concrete”. Technical Research Centre of Finland,
VTT Publications 446, 2001.
Jensen O.M., “Autogenous phenomena in cement-based materials”, Department of Building
Technology and Structural Engineering, Aalborg University, Denmark, 2005.
Jillavenkatesa A., Dapkunas S.J., Lum L-S.H., “Particle Size Characterization”, NIST, Puplication
No 960-1, Washington, 2001.
Lura P., “Autogenous deformation and initial curing of concrete”, Technical University of Delft,
Netherlands, 2003.
Mehta K.P., Monteiro P.J.M., “Concrete: Structure, properties, and materials”, 3rd Ed., McGraw-
Hill, 1993.
Mindess S., Young J.F., Darwin D.,”Concrete”, 2nd ed., Pearson Education Inc., 2003.
Swedish Concrete Association, “Self-compacting concrete -Recommendations for use”, Report No.
10, Svenska Betongföreningen, 2002.
Tattersall G.H., Banfill P.F.G., “Rheology of fresh concrete”, Pitman, London, 1983.
Tattersall G.H., “Workability and quality control of concrete”, E&FN Spon, London, 1991.
Tazawa E-I., ”Autogenous Shrinkage of Concrete”, Taylor and Francis, 1999.


Paper I - Slump flow values vs. Bingham parameters
for high flowable mortars and concretes
PAPER I: SLUMP FLOW VALUES VS. BINGHAM

PARAMETERS FOR HIGH FLOWABLE
MORTARS AND CONCRETES
Esping O., “Slump flow values vs. Bingham parameters for high flowable mortars and
concretes”, Accepted for publication at 5th International RILEM Symposium on Self-
Compacting Concrete, 3-5 September 2007, Ghent, Belgium, 2007.
SLUMP FLOW VALUES VS. BINGHAM PARAMETERS FOR HIGH

FLOWABLE MORTARS AND CONCRETES
Oskar Esping
Dep. of Civil and Environmental Engineering, Chalmers University of Technology, Sweden.
Abstract
In the present work, the influence of Bingham rheology parameters on the slump flow
values of self-compacting concrete and mortar has been evaluated. The objective was to
present experimental results, without any physical validation, addressing the complex
connection between the slump flow spread, flow time (T50), yield stress and plastic
viscosity. A large number of more or less self-compacting mortars (~200 mixtures) and
concretes (~550 mixtures) with a wide range of consistency have been used for the
evaluation.
The mortar rheology was measured using a Bohlin CVO200 rheometer with concentric
setup, and the slump flow spread was measured using a mini-cone. For the concrete a
ConTec Visco5 rheometer was used together with a traditional Abram´s cone.
The results showed a large scatter and poor correlation, but a clear tendency was found.
The results indicate that the slump flow spread and T50 time are not a unique function of
yield stress or viscosity, respectively, but rather a more complex function of both. The
spread proved to be more closely connected with the yield stress than with the viscosity,
especially at high viscosity, whereas the T50 time was more dependent on both viscosity and
yield stress.
1. INTRODUCTION
To quantify the workability of fresh concrete, numerous tests of different types, more or
less empirical, have been developed. The oldest and most frequently used test today is the
slump cone test, which, associated with the Abram’s cone, has its origin in the USA around
1910 [1]. For high-flowable concrete, such as self-compacting concrete (SCC), the slump
cone is used to measure the spread of the concrete (slump flow) and the time for the concrete
to reach a spread of 500 mm (T50). For a more scientific approach, a rheometer/viscometer
can be used. The most established parameters used to define the concrete rheology are the
yield stress and plastic viscosity by the Bingham equation [2]. These rheological parameters,
unlike the measures of qualitative tests (e.g. the slump), are fundamental physical quantities,
mutually independent and not dependent on operator or equipment. But
rheometer/viscometer tests are often expensive, immobile, and mainly for laboratory use. In
the field, e.g. at concrete plant or construction site, fast, simple and cheap tests are preferred;
thus slump/slump flow and other empirical tests can hardly be replaced by a rheological test,
but should rather be a complement. To describe the flow properties of concrete, especially
for types with high flowability, a minimum of two independent parameters is required [2]-
[7]. Concrete mixtures with identical measures from an empirical test (e.g. slump flow) can
be very different in their flow behaviour. These differences can be detected by a rheological
test. However, in order to determine the properties of a non-Newtonian fluid, as all
1
cementitious materials are, a multipoint flow curve has to be measured. A single point
measurement does not describe these materials correctly (see Figure 1).
Shear stress, σ
Shear stress, σ
Shear stress, σ
Viscosity
(plastic), ηpl Yield stress, σ0
Shear rate, γ· Shear rate, γ· Shear rate, γ·

(a) (b) (c)
Figure 1: Illustration of concrete with: (a) same viscosity but different yield stress, (b)
same yield stress but different viscosity, and (c) same empirical measure but
different viscosity and yield stress (from [31]).
It has been shown by many that the empirical tests to some extent provide information
about the concrete rheology. Slump has for a long time [3][6]-[22] been considered to be a
function of yield stress, without influence by plastic viscosity. When analysed, the density of
the concrete is often incorporated as well as the geometry of the cone. More recently the
horizontal flow spread rather than the vertical slump has been used to calculate the yield
stress [2][23]-[25]. Usually these correlations concern concretes in a small range of
flowability (e.g. HPC, SCC, etc.), and are not valid for other or wider ranges. The increased
usage of high-flowable concretes has also raised the interest in more dynamic measures such
as flow time and viscosity. The flow time can be measured by e.g. a V-funnel or L-box, but
also by measuring the time for the concrete to spread 500 mm (T50). For SCC, the slump
flow spread is generally considered to correlate with the yield stress and T50 or V-funnel
with the viscosity [26]-[28]. Often the correlation is purely empirical, but there are also some
physical models proposed to explain this relationship. Examples of physical models linking
yield stress (σ0) to slump flow spread diameter (D) are:
2 ⋅ ρ ⋅ g ⋅V
σ0 = = a / D2 (Eq. 1) [14]
π ⋅D 2
4 ⋅ ρ ⋅ g ⋅V
σ0 = = b / D2 (Eq. 2) [29]
3 ⋅π ⋅ D 2
225 ⋅ ρ ⋅ g ⋅ V 2
σ0 = = c / D 5 (Eq. 3) [30]
4 ⋅π ⋅ D
2 5
where ρ is the material density, V the sample volume and g the gravity, while a, b and c are
constants for a given sample volume and density.
The objective of this paper is not to find a physical relationship between slump flow
values and Bingham parameters, but merely to present experimental results addressing the
interaction between the slump flow spread, flow time (T50), yield stress and plastic
viscosity.
2. TEST METHODS
2.2 Slump flow test

The slump flow measurement was carried out using a traditional slump cone (see Figure
1), for concrete the Abram’s cone (EN 12350-2 or ASTM C143) and for mortar the mini-
slump cone (EN 1015-3 or ASTM C230), but without compaction. The slump flow spread
diameter was measured in two perpendicular directions, presented as a mean value in
2
millimetre. In addition to the slump flow, the time from lifting the cone to when the flow
spread reaches a 500 mm circle was recorded; referred to as T50 and stated in seconds.
Slump cone (Abram) Concrete sample

Mortar sample ØD=100/200 mm Flow table
Mini-slump cone H=300 mm (non-adsorbent)
ØD=70/100 mm Flow table
H=60 mm
Spread Spread
T50 time
diameter diameter
Figure 2: Illustration of slump flow test used for mortar and for concrete (from [31]).
2.2 Rheology
For mortar a Bohlin CVO200 rheometer was used and for concrete a ConTec Visco5, both
using a rotating concentric setup at a controlled shear rate ( γ& ) at 20ºC. The experimental
geometry and measuring sequence is illustrated in Figure 3. The two rheological parameters
plastic viscosity (ηpl) and yield stress (σ0) were evaluated in accordance with the Bingham
model: σ = σ 0 + γ& ⋅ η pl (Eq. 4).
60 Mortar sample
Shear rate [1/s]
No logging
40
Logging H=37.5 mm
Rotating and
20 measuring
inner cylinder
0 Ri=10 mm Fixed outer
0 10 20 30 40 50 60 Ro=15 mm cylinder
Time [s]
8 Ro=145 mm
Concrete
Ri=100 mm sample
Shear rate [1/s]
4
No logging H=140 mm
2 Logging Measuring
inner cylinder
0 Rotating
0 10 20 30 40 50 60 outer cylinder
Time [s]
Figure 3: The measuring sequence for the Bingham evaluation (followed by segregation
estimation) and schematic illustration of the rheometers. For mortar the Bohlin
CVO200 and for concrete the ConTec Visco5 (from [31]).
The mixes and their constituents, as used in this study, comprise typical materials for self-
compacting concrete (SCC) in Sweden. For mortar the maximum grain size was 1.0 mm, and
for concrete 16 mm.
The consistency in some cases was very stiff, but as all mixtures incorporated both filler
and superplastisizer they were considered to be self-compacting. All mixtures have their
origin in other projects whose primary purpose was to examine the effect of different
constituent properties and proportions on the rheology. Examples of this are the effect of:
w/c, cement, silica, fly ash, different limestone fillers, coarse and fine aggregate content,
superplasticizer, air entrainer, viscosity modifier, etc.
3
The mortar samples were prepared in batches of 0.5-1.0 litres, using a 4.73 litre Hobart
laboratory paddle mixer. The mixing sequence was based on ASTM C305 standard. The
concretes were prepared in batches of 30-60 litres, mixed in a BHS60 twin-shaft paddle
mixer for 4 minutes after water was added to the premixed dry materials. The admixtures
were added directly after the water.
4. RESULTS AND DISCUSSION

The presented results are based on a large number of more or less self-compacting
mortars (~200 mixtures) and concretes (~550 mixtures) with a wide range of consistency.
The density is also considered to influence the slump and slump flow (see Eq. 1-3), but as
the difference in density of the mixes was relatively small, it was not taken into account.
Concretes and mortars with high tendency of visual segregation were excluded, as these are
considered to give misleading measures and thus a poor correlation between the slump flow
and rheology. For concrete slump flow spread (D) and time to 500 mm (T50) were recorded
and correlated with the Bingham parameters (yield stress and plastic viscosity). For mortar
only the spread was recorded and correlated with the Bingham parameters. The presented
correlations are not intended as a “true connection” of slump flow values and Bingham
parameters, but merely to show the more complex connection between the slump flow
spread, flow time, yield stress and plastic viscosity.
4.1 Rheology vs. slump flow spread

The experimental results of slump flow spread diameter and Bingham rheology
parameters (yield stress and plastic viscosity) for the mortar and concrete samples are
presented in Figure 4. The spread flow is grouped into intervals of 50 mm for mortar and 100
mm for concrete, starting with spread equal to the cone bottom diameter (D0=100 mm
respectively 200 mm). For each spread interval, a logarithmic trend-line is plotted, as this
was the tendency that was best fitted over a wide range of spreads. It can be noted that there
is a large scatter and rather poor correlation (R2=0.1-0.9) but still a clear tendency can be
observed that the slump flow is affected by both yield stress and viscosity. At high viscosity
or low yield stress, where the slope of the curve is lower, the effect of yield stress is more
pronounced. If slump flow were to be independent of viscosity the curve would be
horizontal. The slump flow can seem to be independent of viscosity for the higher flowable
mortars and concretes (with slump flow >250 respectively >500 mm), as the curve looks
horizontal. When excluding mixtures with lower spread flow it can be observed that also
here the spread is affected by both yield stress and viscosity.
4
70 600
>350 mm >700 mm
60 300-350 mm 600-700 mm
500
250-300 mm 500-600 mm
200-250 mm 200-300 mm 400-500 mm
50
150-200 mm
400 300-400 mm
Yield stress [Pa]
Yield stress [Pa]

100-150 mm
40 200-300 mm
100-150 mm 300
30 300-400 mm
150-200 mm
200
20
200-250 mm 400-500 mm
10 250-300 mm 100
500-600 mm
300-350 mm
>350 mm 600-700 mm
0 >700 mm
0
0 2 4 6 8 0 50 100 150 200
Viscosity [Pa s] Viscosity [Pa s]
Figure 4: The slump flow spread (in intervals of 50 resp. 100 mm) and Bingham rheology
parameters (yield stress and plastic viscosity) for the mortar and concrete.
Based on all the investigated mixes (> 750 mixes), the following approximate model for
calculating the relative slump flow area (Rp) for both mortar and concrete is proposed:
( H / 6 )2
Rp ≈ (Eq. 5) R p = ( D / D0 ) 2 − 1 (Eq. 6)
ln( η pl + 2 ) ⋅ σ 0
where ηpl is the plastic viscosity, σ0 the yield stress, H the cone height (60 resp 300 mm), D
the measured spread diameter in millimetre and D0 the flow cone bottom diameter (100 resp
200 mm). The model is purely empirical and is deficient in its units. In Figure 5 the model is
plotted for mortar and concrete.
70 600
60 Mortar Concrete
50
Yield stress [Pa]
Yield stress [Pa]
400
40 200-300 mm
100-150 mm
30
200 300-400 mm
20
150-200 mm
200-250 mm 400-500 mm
10 250-300 mm 500-600 mm
300-350 mm 600-700 mm
>350 mm >700 mm
0 0
0 2 4 6 8 0 50 100 150 200
Viscosity [Pa s] Viscosity [Pa s]
Figure 5: Calculated slump flow spread diameter as a function of Bingham rheology

parameters for mortar and concrete.
In Eq.5 the yield stress is predominant, where the effect of a change in yield stress
corresponds to ~3 times larger change in viscosity on the slump flow. These differences are
smaller at low viscosity, and are independent of the magnitude of yield stress.
In the literature, not all studies agree that slump flow spread is a measure of concrete
yield stress. For example, Nielssen & Wallevik [32] explain how a low viscosity will increase
the downward speed, overcome the yield stress and thereby generate a large slump flow
5
spread. For high viscosity the effect will be the opposite. Cauberg et al [33] state that the
relation between yield stress and slump flow, without taking viscosity into account, does not
show a satisfactory fit, and that these relations usually are formed for a certain range of
fluidity. Furthermore, a variable Z0, comprising both yield stress (σ0) and viscosity (ηpl), is
proposed for a better fit to the slump flow spread (D) in millimetres.
Z 0 = a ⋅ σ 0 + b / η pl (Eq. 7) Z 0 = 381 − 0.586 ⋅ D (Eq. 8)
where a and b are constants. In the region of spread D=400-600 mm, and with a=1 and
b=1000, Eq. 7 and Eq. 8 generate similar results as Eq. 5 and Eq. 6. For spread D>650 mm
Eq. 8 is not valid. Furthermore, the shape of the curve in a ηpl-σ0 diagram is independent of
the spread. Smeplass [34] has noted that the slump is more related to the yield stress than to
the viscosity of concrete, while the flow table spread is more related to the viscosity than the
yield stress. If the viscosity varies, at constant yield stress, so will the flow measures.
4.2 Rheology vs. slump flow time T50

The experimental results of slump flow spread time T50 and Bingham rheology
parameters for the concrete samples are presented in Figure 6. Concretes with slump flow
spread <500 mm have been excluded as they have no T50 measure (~380 mixtures with
slump spread >500mm). The T50 times are grouped into intervals of 2 seconds. For each T50
time interval a trend-line is plotted. It can be noted that there is a large scatter and poor
correlation (R2=0.1-0.4). Still the tendency can be observed that the T50 time is affected by
both yield stress and viscosity. If the flow time were independent of yield stress the curve
would be vertical.
120
>10 s
8-10 s
6-8 s
4-6 s
Yield stress [Pa]
80
2-4 s
<2
>10 s
8-10 s
40
4-6 s 6-8 s
2-4 s
<2 s
0
0 50 100 150
Viscosity [Pa s]
Figure 6: The experimental results of slump flow spread time T50 (in intervals of 2 s) and
Bingham rheology parameters (yield stress and plastic viscosity) for the
concrete.
Based on the results, the following empirical model for calculating the slump flow spread
time T50 in seconds is proposed:
T 50 ≈ 0.002 ⋅ σ 0 ⋅ η pl (Eq. 9)
In the literature, there is no general agreement that T50 is a measure of concrete plastic
viscosity (ηpl). For example, Tedaka et al [35] state that the slump flow spread corresponds
well to the yield stress (σ0), whereas the T50 flow time does not alone represent the viscosity
since slump flow also contributes. Thus, T50 can be used to evaluate the viscosity only when
the slump flow is constant. Furthermore, Ferraris et al [36] show that the slump flow spread
times of cement pastes with a wide range of yield stress have no correlation at all with the
viscosity. Emborg [37] has also noted a weak correlation, but then for the T50 vs. viscosity
6
of SCC. Utsi et al [38] have observed that T50 correlates not only to the viscosity but also to
the yield stress, and proposes that both the yield stress and viscosity influences the T50 and
slump flow respectively. By dividing the slump flow into different intervals the correlation
between T50 and viscosity was shown to be acceptable, which further fortified this theory.
5. CONCLUSIONS
It has been shown by many investigators that the results of empirical tests are strongly
related to the concrete rheology. For SCC, the slump flow spread is generally considered to
be a function of yield stress and T50 or V-funnel of viscosity. Often this correlation is purely
empirical, but there are also different physical models explaining this relationship. In the
presented work, the influence of Bingham rheology parameters on the slump flow values of
a large number of more or less self-compacting concrete and mortar has been evaluated.
Experimental results addressing the connection between the slump flow spread, flow time
(T50), yield stress and plastic viscosity are presented. The results clearly indicate that the
slump flow spread and T50 time are not a unique function of yield stress and viscosity
respectively, but rather a more complex function of both where neither yield stress nor
viscosity can be neglected. The spread proved to be more closely connected with the yield
stress than the viscosity (~3 times), especially at high viscosity, whereas the T50 time was
connected more equally with yield stress and viscosity. Consequently, T50 can only be used
to estimate the viscosity for mixture with constant yield stress, and slump flow can only be
used to estimate the yield stress with constant viscosity.
ACKNOWLEDGEMENTS
Financial support from Thomas Concrete Group and Färdig Betong is greatly appreciated.
REFERENCES
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Compendium of tests”, RILEM, France.
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[3] Domone P. (1998): ”The slump flow test for high-workability concrete”, Cement and Concrete
Research, vol 28(2), pp 177-182.
[4] Domone P.L.J., Xu Y., Banfill P.F.G. (1999): “Developments of the two-point workabiliy test
for high-performance concrete,” Magazine of Concrete Research, Vol 51(3), pp 171-179, 1999.
[5] Ferraris C.F., “Measurement of the rheological properties of high performance concrete: State
of art report”, Journal of NIST, vol 104(5), pp 461-478.
[6] Tattersall G.H. (1973): “The rationale of a two-point workability test,” Magazine of Concrete
Research, vol 25 (84), pp 169-172.
[7] Tattersall G.H., Banfill P.F.G. (1983): “Rheology of fresh concrete”, Pitman, London.
[8] Chidiac S.E., Madaani O., Razaqpur A.G., Mailvaganam, N.P. (2000): “Controlling the quality
of fresh concrete - A new approach”, Magazine of Concrete Research, vol 52 (5), pp 353-364.
[9] Clayton S., Grice T.G., and Boger D.V. (2003): “Analysis of the slump test for on-site yield
stress measurement of mineral suspensions”, Journal of Mineral Processing, Vol 70, pp 3-21.
[10] de Larrard F. (1999): “Concrete mixture proportioning, a scientific approach”, F&FN Spon,
New York.
[11] de Larrard F., Hu C., Sedran T., Szitkar J.C., Joly M., Claux F., Derkx F. (1997): “A new
rheometer for soft-to-fluid fresh concrete”, ACI Materials Journal, vol 94(3), pp 234-243.
[12] Ferraris C.F., de Larrard F. (1998): “Testing and modelling of fresh concrete rheology”,
NISTIR 6094, NIST, USA.
[13] Hu C., de Larrard F., Sedran T., Boulay C., Bosc F., Deflorenne F. (1996): “Validation of
BTRHEOM, the new rheometer for soft-to-fluid concrete”, Materials and Structures, vol
29(194), pp 620-631.
7
[14] Murata J. (1984): “Flow and deformation of fresh concrete”, Materials and Structures, vol
17(98), pp 117-129.
[15] Murata J., Kikukawa H. (1992): “Viscosity Equation for Fresh Concrete”, ACI Materials
Journal, vol 89(3), pp 230-237.
[16] Norberg J., Peterson O., Billberg P. (1997): “Effects of a new generation of superplasticizers on
the properties of fresh concrete”, CANMET/ACI International Conference, pp. 583-598, Italy.
[17] Pashias N., Boger D.V., Sumers J., Glenister D.J. (1996): “A Fifty Cent Rheometer for Yield
Stress Measurements”, Journal of Rheolgy, vol 40(6).
[18] Saak A.W., Jennings H.M., Shah, S.P. (2004): “A generalized approach for the determination of
yield stress by slump and slump flow”, Cement and Concrete Research, Vol 34, pp. 363-371.
[19] Schowalter W.R., Christensen G. (1998): “Toward a rationalization of the slump test for fresh
concrete -Comparisons of calculations and experiments”, J. of Rheology, vol 42(4), pp 865-870.
[20] Tanigawa Y., Mori H. (1989): Analytical study on deformation of fresh concrete”, Journal of
Engineering Mechanics, vol 115(3), pp 493-508.
[21] Tanigawa, Y., Mori, H., Watanabe, K. (1990): “Computer simulation of consistency and
rheology tests of fresh concrete by viscoplastic”, RILEM symposium on properties of fresh
concrete, pp 301-308, Hanover.
[22] Wallevik J. E. (2006): “Relationship between the Bingham parameters and slump”, Cement and
Concrete Research, vol 36, pp 1214-1221.
[23] Flatt R.J., Domenico L., Roussel N. (2006): “Linking yield stress measurements: Spread test
versus Viscomat”, Cement and Concrete Research, vol 36(11), pp 99-109.
[24] Rossel N., N’Guyen H.T.L., Coussot P. (2005): “Yield measurements using stoppage tests”,
RILEM symposium on SCC, pp 575-582, Chicago.
[25] Saak A.W., Jennings H.M., Shah S.P. (2004): “A generalized approach for the determination of
yield stress by slump and slump flow”, Cement and Concrete Research, vol 34(3), pp 363-371.
[26] Domone P.L. and Jin J. (1999): “Properties of mortar for self-compacting concrete” RILEM
symposium on SCC, pp 109-120, Stockholm.
[27] Grünewald S., Walraven J.C. (2003): “Rheological measurements on self-compacting fibre
reinforced concrete”, RILEM Symposium on SCC, PRO 33, pp 49-58, Reykjavik.
[28] Jin J., Domone P.L. (2002): “Relationships between the fresh properties of SCC and its mortar
component”, North American Conference on the Design and Use of Self-Consolidating
Concrete, pp 33-38, Chicago.
[29] Chidiac S.E., Maadani O., Razaqpur A.G., Mailvaganam N.P.(2000): ”Controlling the quality
of fresh concrete - a new approach”, Magazine of Concrete Research, vol 52(5), pp 353-363.
[30] Roussel N., Stefani C., Leroy R.,” From mini-cone test to Abrams cone test: measurement of
cement-based materials yield stress using slump tests”, Cement and Concrete Research, vol
35(5), pp 817-822.
[31] Esping, O. (2004): “Rheology of cementitious materials: effects of geometrical properties of
filler and fine aggregate”, Report 04:3, Chalmers University of Technology, Göteborg.
[32] Nielsen I., Wallevik O.H. (2003): “Rheological evaluation of some empirical test methods –
Preliminary result”, RILEM symposium on SCC, pp 55-68, Reykjavik.
[33] Cauberg N., Desmyter J., Dieryck V. (2005): “Rheology of Self-Compacting Concrete -
Validation of Empirical Test Methods”, RILEM symposium on SCC, pp 765-773, Chicago.
[34] Smeplass S. (1993): “Applicability of the Bingham model to high strength concrete”, RILEM
workshop on special concretes – Workability and mixing, pp 145-151, Paisley.
[35] Takada K., Tangtermsirikul S. (2000): “Testing of Fresh Concrete”, Self-compacting concrete:
State-of-the-art report, RILEM Technical Committee 174-SCC, Report 23, pp 25-39, France.
[36] Ferraris C., Obla K., Hill R. (2001): “The influence of mineral admixtures on the rheology of
cement paste and concrete”, Cement and Concrete Research, Vol 31(2), pp 245-255.
[37] Emborg M. (1999): “Rheology tests for self-compacting concrete - How useful are they for the
design of concrete mix for full scale production?”, RILEM symposium on SCC, pp 95-105,
Stockholm.
[38] Utsi S., Emborg M., Carlswärd J. (2003): “Relation between workability and rheological
parameters”, RILEM Symposium on SCC, PRO 33, pp 154-164, Reykjavik.
8
Paper II - Methods for characterisation
of fillers and fines for SCC
PAPER II: METHODS FOR CHARACTERISATION OF

FILLERS AND FINES FOR SCC
Esping O., “Methods for characterisation of fillers and fines for self-compacting
concrete”, 3rd International RILEM Symposium on Self-Compacting Concrete, PRO 33,
17–20 August, pp 208-219, Reykjavik, Iceland, 2003.
METHODS FOR CHARACTERISATION OF FILLERS AND FINES

FOR SELF-COMPACTING CONCRETE
Oskar ESPING
Chalmers University of Technology, Sweden
ABSTRACT: Due to the large surface area, quantification of fillers and the fine part of
aggregates is essential for the ability to control physical properties, such as workability of
self-compacting concrete. A new simple method for measuring the surface area has been
investigated and compared with other traditional methods.
The properties of eight different fillers (seven limestone and one glass filler) and their
influence on the rheology of self-compacting mortar have been evaluated.
KEYWORDS: self-compacting concrete, mortar, filler, rheology, specific surface.
1. INTRODUCTION
The rheology of a particle suspension is a function of the suspending media. For concrete,
optimized size distribution influence the workability positively since the suspension consists
of a matrix where the suspension of smaller particles fills the hollow spaces between the
coarser. To decrease the internal friction of fresh concrete, the particle surface is to be
covered with water and voids in the system to be filled. More water will reduce the volume
fraction of particles and thereby eases the particle motion. Consequently, when the contact
zone between the particles decreases there will be a significant reduction of plastic viscosity
and yield stress [1,2,4]. Besides particle concentration and size distribution, other important
properties affecting the workability are particle shape, porosity and surface texture [3].
Since surface area/volume ratio is inversely proportional to linear dimension, as size

decreases surface properties become more important. This effect can be exemplified by
studying how the surface area changes for a cube with the edge length 10 mm when it is
gradually divided into cubes with half the edge length (see Figure 1). This dividing process
(showed in Table 1) leads to a drastically enlarged surface area.
Table 1. How the surface area
increases with the dividing process
1 of the exemplified cube.
½ dividings edge length area [m2]
0 10 mm 0.0006
Figure 1. By dividing a cube to 8 cubes with half the 10 9.8 µm 0.6
edge length, the surface area will be doubled. 25 1.19 nm 20000
During real conditions, the surface area also comprises an enlarging effect from the shape,
porosity and surface texture. An irregular and porous particle can provide a considerable
larger surface area, accessible to water, than a spherical.
So, due to the large surface area, quantification of geometrical properties of fillers and the
fine part of the aggregates is essential for the ability to control physical properties, such as
workability, in the production of self-compacting concrete (SCC).
1
In this study, the properties of eight different fillers (seven limestone and one glass filler)
and their influence on the rheology of self-compacting mortar have been evaluated.
Traditional methods for measuring the surface area has been investigated and compared with
a new simple method, called BET (H2O).
2. THE BET (H2O) METHOD

2.1 Introduction
The cement and filler particles fineness is traditionally quantified with Blain measure. Due
to the methodology where the specific surface area is determined from air permeability,
based on packed spherical particles, information of the shape, texture and surface porosity is
neglected. The Blaine measure is mainly an indication of particle concentration and size
distribution. Other possibly more correct methods, such as the BET (Nitrogen) and image
analysis is more seldom used due to its complexity and costly equipment.
Concrete and mortar fluidity strongly depends on the size of the internal surface area that has
to be covered with water to create mobility. A true value of this area, especially concerning
the fines, is probably one of the quantification methods necessary for predicting the
rheological properties. A methodology for this quantification is the BET (H2O).
2.2 Methodology
The BET (H2O) is based on BET theory (named after Brunauer, Emmett and Teller) [8]
where the specific external surface area is estimated from determining the quantity of a
specific gas that adsorbs as a single layer of molecules, a so-called monomolecular layer,
under controlled conditions. But instead, as normally, of using nitrogen gas at controlled
temperature and pressure, moisture at two ore more relative humidity (RH) levels are used.
The technique by using the BET-relation with moisture instead of nitrogen gas has been
applied by Fuglsang Nielsen [6] and Ahlgren [7], but the focus was on internal porosity and
not on external particle surface.
It ought to be noted that moisture adsorption is not the same as for nitrogen gas. The water
molecule is slightly smaller than the nitrogen molecule, and the water molecule has larger
affinity forces (attraction) due to its two-polar covalent bonds (see Figure 2 and Figure 3).
However, using water (moisture) is probably closer to real condition in concrete production
than using nitrogen gas.
To be able to use the BET theory with moisture as an adsorbent restricted to a
monomolecular layer, the vapour pressure must be low. Therefore the RH is limited to
approximately 30% (at 20ºC).
Adsorbed +
H
molecules
+ N N
H O
-
Mono-layer
(~3.5Å for water) H 2O N2
Figure 3. The polar water (H2O) molecule

Figure 2. Molecules adsorbed to a surface versus the nonpolar nitrogen (N2)
When evaluating the BET (H2O)-method, a "two pressure" humidity generator (Thunder
2500, see Figure 4) where the specimens were conditioned in air vaporized at several levels
2
(6, 12, 16, 20, 25, 30 and 50% RH) with high accuracy. This was then compared with a
method where the specimens were conditioned in two separate climate boxes (11.3 and
33.1% RH with LiCl and MgCl2 salt, see Figure 5). The climate box (salt) method showed
adequate results, and are due to its simplicity a recommended method.
Figure 4. The Thunder 2500, a Figure 5. Two climate boxes with RH 11% (LiCl) and
"two pressure" principle humidity 33% (MgCl2) For stable atmospheres, the box must be
generator, producing tight and a mechanical fan are to be rotate the air
atmospheres with high accuracy. inside. The temperature must be kept constant at 20ºC.
By plotting the adsorption isotherm STP (see Eq.1 and Eq.2)
STP [kg/kg]
as a function of the relative humidity RH, the variables a and
b can be calculated by a linear relationship (see Figure 6).
The specific area S is then calculated according to Eq.3. [7] b
RH a
STP = [kg/kg] (RH {0;1}) (Eq.1)
(u ⋅ (1 − RH )) RH [-]
(m − mdry ) Figure 6. The intersection

Moisture content u = [kg/kg] (Eq.2) point (a) and slope (b) calcu-
mdry
lated from the linear relation-
3.54 ⋅ 106 ship between STP and RH.
S= [m2/kg] (Eq.3)
( a + b)
Recommended equipment for the BET (H2O)-analyse is:

2 salt boxes (11% RH with LiCl and 33% with MgCl2), see Figure 5.
105ºC oven
Scale (1/1000 g)
3. EXPERIMENTAL SETUP
3.1 Quantification methods
3.3.1 Surface area from size distribution
The surface area of the fillers was calculated from the particle size distribution, both from
the laser diffraction analyze (given in Figure 12) and from the image analysis (see section
3.3.5.), assuming spherical particles. The size distribution from the image analyze was
determined according to the Nordtest method NT BUILD 486.
3.3.2 BET (N)
3
The method is described in chapter 2.2. The test was performed both by Norkalk AB (lime-
stone filler producer) using a Micromeritics BET analyzer and by SP (Swedish National
Testing and Research Institute) also using a Micromeritics.
3.3.3 BET (H2O)

The method is described in chapter 2.2. The sample size was approximately 100 g. The test
was performed both with humidity generator and climate boxes (11% and 33% RH).
3.3.4 Blaine
The method determines fineness of powders in terms of specific surface. The test was made
according to ASTM C204 standard, with a Tonindustrie instrument. Norkalk AB also
performed this test, using a ToniPerm instrument.
3.3.5 Image analysis

The image analysis was made with the "UTHSCSA Image Tool" on pictures (2016·2016
pixels) taken on epoxy-molded and polished specimens in a low vacuum scanning electron
microscope (SEM).
Following factors was measured and calculated:
F-shape: the ratio of the length of the minor axis (Dmin) to a) Dmin
the length of the major axis (Dmax). If the elongation is 1, Dmax
the object is roughly circular or square (see Figure 7). The
F-shape is computed as:
Dmin / Dmax [-] (Eq.4)
b) Area p. Perimeter
F-circle: the ratio of measured area and area of a circle with
Area c.
the same perimeter as measured. At 1, the object is circular
(see Figure 7). The F-circle is computed as:
4 ⋅ π ⋅ Area
[-] (Eq.5)
Perimeter 2 c)
Dmax
Compactness: the ratio between the diameter of a circle
with the same area as measured (Dcircle) and the maximum Dcircle
elongation (Dmax) of measured area and. At 1, the object is
circular (see Figure 7). The Compactness is computed as:
Figure 7. a) F-shape; b)
2 ⋅ Area / π F-circle; c) Compactness.
[-] (= Dcircle / Dmax) (Eq.6)
Dmax
3.3.6 Retained water and water sensitivity

The retained water ratio βp and the deformation coefficient (sensitivity) Ep, was measured,
according to a method presented by Okamura et al. [9]. The method, using mini-slump test
(see 3.4.1), is based on the linear relationship between the relative flow area Rp (see Eq.4)
and the water by powder ratio by volume Vw/Vp (see Figure 8).
4
( D 2 − D02 )
Rp = 2
[m2/m2] (Eq.7)
D0
Vw/Vp [-]
70 mm
D is the average spread diameter, calculated in
four directions and D0 is the base diameter of Ep
60 mm
cone (Figure 8).
βp
D0 = 100 mm
The measure of retained water ratio βp can be Rp [-] D D 3 4
considered as the amount of water, adsorbed D
1
D 2
on the particle surfaces and filling the voids in

Figure 8. βp is represented by the
the particle system, needed to initiate flow. The
interception point and the Ep the slope,
deformation coefficient Ep is a measure of the
calculated from the linear relationship
sensitivity of increased water content [10].
between Vw/Vp and Rp.
3.2 Rheological test

3.4.1 Mortar flow test (mini-slump)
70 mm
A traditional slump flow
measure was carried out
60 mm
using a mini-slump cone

(see Figure 9), mea-suring
the spread flow diameter 100 mm
D (average value from two D 1
directions) The slump was D 2
measured 7 minutes after

adding water to cement. Figure 9. Mini slump flow test.
3.4.2 Rheology
A Bohlin CVO200 rheometer with rotating coaxial
cylinder was used to measure plastic viscosity (ηpl),
yield stress (σ0) and thixotropy at controlled shear
rate ( γ& ). The measuring device consisted an outer
cylinder (cup) with diameter Do=30 mm and a
grooved inner cylinder (bob) with diameter Di=20
mm, providing a gap of 5 mm (see Figure 10). The
temperature was controlled and kept constant at
20±0.1°C. The evaluation of viscosity and yield
stress was made according to the Bingham model
(see Eq.8) and the thixotropy was evaluated from a
linear up/down loop where the area in the flow
curve represented the thixotropic measure.
σ = σ 0 + γ& ⋅ η pl (Eq.8)
The measuring sequence setup was made after Figure 10. Bohlin CVO200 rheometer
consultation with Dr O. Wallevik [11] and is shown with a grooved inner cylinder (bob).
in Figure 11.
5
50 Logging
No logging 1
40
2
Shear rate [1/s]
Yield stress, σ0 [Pa]

30 3
20 1 2 3 Thixotropy [Pa/s]
10 Viscosity,ηpl [Pa s]
Shear rate, γ· [1/s]

0
0 10 20 30 40 50 60 70 80 90
Time [s]
Figure 11. The measuring sequence setup with a first loop (1) measuring the thixotropy, a
second (2) for the Bingham evaluation and a third (3) for segregation estimation.
3.3 Materials and mix design

The materials used in the experiments, are listed in Table 2. All have particles smaller than
0.5 mm. One coarse and one fine limestone filler, from three different time epochs, were
selected. The idea with the differences in age is to get variations in shape, surface porosity
and texture. Two additional fillers were selected, the Limus 40 (limestone) and the
Mikrofiller (glass), representing "standard" (in Sweden) fillers for SCC. The fillers size
distributions are presented in Figure 12 and SEM-photos as illustration shown in Figure 13.
Baskarpsand 15, an industrial washed and sieved natural sand smaller than 0.5 mm, are
selected to represent the fine part of concrete aggregate. All of the materials, except the
L180X-limestone filler, are commercial Swedish products.
The density was measured with pycnometer and the size distribution with a Malvern laser
diffraction instrument, both performed by Nordkalk AB (limestone filler producer).
Table 2. Materials.
Material Type Name Supplier Age Density
[milj years] [kg/m3]
Cement: CEMII/A-LL42,5R Byggcement (Bygg) Cementa 2980
Aggregate: Sand Baskarpsand 15 (B15) Baskarpsand 2650
Filler: Limestone Limus 10 (L10) Nordkalk 500 2680
Limestone Limus 15 (L15) Nordkalk 80 2710
Limestone L180X Nordkalk 1900 2730
Returned glass MicroFiller SGÅ 2510
Plasticizer: Polucarboxylate Sikament-56 Sika 1100
The mortar recipe is based on a "normal" (in Sweden) SCC, where the proportions were
scaled down due to the maximum grain size 0.5 mm.
The volume of aggregate, cement and plasticizer were kept constant, while the w/c was
varied in tree levels 0.45, 0.50 and 0.55. The volume distribution of the recipes is shown in
Figure 14. Due to different filler density, totally 24 recipes were produced. Each mortar mix
was prepared according to the ASTM Standard C 305 at 20˚C.
6
L10 Size distribution

100 L15
L10
L25 L15
L25
L40
80
L180
L180X Bygg L180
L190
60
Passing [%]
MF
L40
Bygg MF Figure 12.
B15
40
L190
Size distribution
of the seven
20
L180X
limestone fillers
and the glass
B15
filler measured
0 with a Malvern
0,002 0,004 0,008 0,016 0,031 0,063 0,125 0,250 0,500 laser diffraction
Size [mm]
instrument.
L10 L15 L25 L40
L180 L180X L190 MF
Figure 13. Pictures of the fillers, taken with scanning electron microscope (SEM). The edge
length of each picture responds to 0.5 mm. The specimens are epoxy-mould and polished.
Plasticizer Plasticizer Plasticizer

0,3% 0,3% 0,3%
Cement Cement
Water Cement
25,0% Water Water 25,0%
33,5% 25,0%
37,2% 41,0%
Aggregate Aggregate
Aggregate
Filler 25,0%
25,0% 25,0%
Filler
16,1% Filler
12,4%
8,7%
w/c 0.55
w/c 0.45 w/c 0.5
Figure 14. Mix proportion by volume.
7

4.1 Quantification methods
The results from the geometrical quantifications are presented in Figure 15, Figure 16,
Figure 17 and Figure 18. The quantifications incorporates the methods:
Specific surface area calculated from size distribution (laser diffraction) and from
image analysis (SEM)
Blaine
BET (N) and BET (H2O)
Image analysis (F-shape, F-circle, Compactness)
The retained water ratio βp and the deformation coefficient (sensitivity) Ep
700 10000
Calculated (Size distr)
600
Specific surface area [m2/kg]

Specific surface area [m2/kg]
BET (N)
Calculated (SEM) 8000
500 BET (H2O)
Blaine
400 6000
300 4000
200
2000
100
0 0
X
X
80
90
F
0
80
90
80
80
L1
L1
L2
L4
L1
L1
L2
L4
M
M
L1
L1
L1
L1
L1
L1
Figure 15. Specific area calculated from size Figure 16. Specific area measured with
distribution and measured with Blaine. BET (N) and BET (H2O).
Vw/Vp
Geometry Retained water and sensitivity
F-shape
0,9
F-circle Ep
0,06 1,00
Compactness βp
R
0,05
0,8
retained water ratio βp [-]
F -s hape, F -c irc le and
Deformation coeff Ep [-]
Ep 0,80
Com pac tnes s [-]
0,05
Bp
0,04
0,7
0,60
0,04
0,6 0,03
0,40
0,03
0,5 0,02 0,20

X
0
80
90
F
0
F
X
80
90
80
L1
L1
L2
L4
M
L1
L1
L2
L4
M
80
L1
L1
L1
L1
L1
L1
Figure 17. Roundness factors as F-shape, F- Figure 18. Retained water and sensitivity.
circle and Compactness, measured and Note that a high deformation coefficient
calculated from Image analysis (SEM). indicates a sensitive material.
8
4.2 Rheological test

The results, listed in Figure 19, Figure 20, Figure 21 and Figure 22, are based on a large
number oft test (~120 for the rheometer test and ~60 for the slump). Each test is presented as
a mean value.
Rheology Rheology
1000 10
w/c 0,45 w/c 0,45
Plastic viscosity ηpl [Pa s]

w/c 0,50 w/c 0,50
w/c 0,55
Yield stress σ0 [Pa]
w/c 0,55
100
10
1 0
X
0
0
X
F
80
90
0
F
80
90
80
L1
L1
L2
L4
L1
L1
L2
L4
80
M
M
L1
L1
L1
L1
L1
L1
Figure 19. Yield stress σ0 for the w/c 0.45, 0.50 Figure 20. Plastic viscosity ηpl for the w/c
and 0.55 mortar mix. 0.45, 0.50 and 0.55 mortar mix.
Rheology Rheology
10000 400
w/c 0,45 w/c 0,45
w/c 0,50 350 w/c 0,50
1000 w/c 0,55 w/c 0,55
Slump flow D [mm]
Thixotropy [Pa/s]
300
100 250
200
10
150
1 100
X
X
0
0
F
F
80
90
80
90
L1
L1
L2
L4
80
80
L1
L1
L2
L4
M
M
L1
L1
L1
L1
L1
L1
Figure 21. Thixotropy for the w/c 0.45, 0.50 Figure 22. Slump flow diameter D for the w/c
and 0.55 mortar mix. 0.45, 0.50 and 0.55 mortar mix.
4.3 Correlation
A correlation analyze was performed with the software tool AXUM 6.0. The results are
listed in Table 3, The correlation coefficient is represented by the Pearson product moment
corre-lation r, calculated as:
n ⋅ ∑ ( x ⋅ y ) − ∑ x ⋅∑ y
r= [-] (Eq.9)
(
n ⋅ ∑ x 2 −( ∑ x ) 2 ⋅ n ⋅ ∑ y 2 − ( ∑ y ) 2 )( )
x and y are the variables and n is the number of pairs that are to be compared.
The greater value of r the stronger correlation, as follows:
0.8 - 1.0 very strong
0.6 - 0.8 strong
0.4 - 0.6 moderate
< 0.4 weak
9
There are also negative relations, but the important quality of correlation coefficients is not
their sign, but their absolute value.
Table 3. Correlation matrix within geometry and between geometry and rheology. Results
with "very strong" (>0.8) correlation are typed bold and the strong (0.6 - 0.8) are
underlined.
Asize ASEM BETN BETH2O Blaine F-shape F-circle Comp. Ep βp
Asize 1.00
ASEM 0.84 1.00
BETN 0.49 0.21 1.00
BETH2O 0.32 0.08 0.98 1.00
Blaine 0.94 0.77 0.47 0.30 1.00
F-shape 0.23 -0.12 0.62 0.58 0.43 1.00
F-circle 0.25 -0.22 0.68 0.65 0.34 0.87 1.00
Comp. 0.49 0.02 0.79 0.72 0.54 0.85 0.95 1.00
Ep 0.88 0.60 0.76 0.62 0.90 0.57 0.54 0.75 1.00
βp 0.44 0.35 0.73 0.75 0.54 0.47 0.41 0.45 0.61 1.00
Thixotr. 0.13 0.00 0.81 0.89 0.15 0.41 0.49 0.47 0.38 0.86
w/c 0.45
σ0 0.35 0.07 0.86 0.84 0.42 0.54 0.66 0.70 0.67 0.76
ηpl 0.34 0.17 0.80 0.82 0.40 0.43 0.55 0.55 0.56 0.90
D -0.26 -0.19 -0.70 -0.75 -0.33 -0.38 -0.44 -0.40 -0.42 -0.94
Thixotr. 0.08 -0.02 0.65 0.71 0.18 0.33 0.43 0.37 0.34 0.83
w/c 0.50
σ0 0.37 0.08 0.95 0.93 0.41 0.60 0.69 0.75 0.71 0.75
ηpl 0.33 0.19 0.81 0.83 0.41 0.45 0.50 0.52 0.58 0.92
D -0.30 -0.19 -0.80 -0.84 -0.37 -0.47 -0.50 -0.50 -0.52 -0.94
Thixotr. 0.35 0.30 0.52 0.55 0.41 0.12 0.20 0.22 0.43 0.88
w/c 0.55
σ0 0.42 0.24 0.87 0.84 0.47 0.41 0.49 0.58 0.69 0.82
ηpl 0.46 0.37 0.62 0.64 0.48 0.18 0.28 0.32 0.52 0.92
D -0.41 -0.37 -0.74 -0.75 -0.44 -0.23 -0.27 -0.34 -0.56 -0.93
The analyze shows on strong Correlation

correlation between retained water 1,0
Retained water E p [-]
ratio βp and mortar slump flow D 0,9
(see Figure 23). This can be 0,8

w/c 0,45
explained by the fact that the 0,7
w/c 0,50
methods are based on the same 0,6 w/c 0,55
methodology and equipment. 0,5
100 150 200 250 300 350 400
Slump D [mm]
The correlations between the
roundness factors (F-shape, F-circle Figure 23. Correlation between retained water ratio
and Compactness) are good, as βp and mortar slump flow D for the w/c 0.45, 0.50
expected. and 0.55 mix.
But it ought to be pointed out that F-shape is more a measure of shape, F-circle more a
measure of texture and Compactness is somewhere between. This is exemplified in Figure
24 with four different geometrical shapes (ellipse, rectangle, triangle and hexagon) and their
impact on the roundness factor by changed size ratio (d/D).
10
The quantification by image analysis was problematic. The method is strongly dependent of
a large numbers of factors, such as: sample preparing, microscope performance, photo
quality (sharpness), resolution, number of particles, analyzing software, threshold technique,
etc. The method might be better if a larger part of the procedure were automatized and
standardized.
1,0 1,0 Ellipse 1,0

Rectangle
0,8 0,8 Triangle 0,8
Ellipse
Compactness [-]
Hexagone
Rectangle
0,6 0,6
Fcircle [-]
0,6
Fshape [-]
Triangle
Hexagone 0,4
0,4 0,4 Ellipse
Rectangle
0,2 0,2 0,2 Triangle
Hexagone
0,0
0,0 0,0
1:1 1:2 d/D 1:3 1:4 1:1 1:2 d/D 1:3 1:4 1:1 1:2 d/D 1:3 1:4
a) b) c) d)
d d d d
D D D D
Figure 24. The roundness factors F-shape, F-circle and Compactness and their geometrical
dependency exemplified by a) ellipse, b) rectangle, c) triangle and d) hexagon.
Another very strong correlation was found Correlation

500
between the calculated specific area (from size
Asize (size ditr.) [m2/kg]
distribution) and the measured with Blaine (see 400
Figure 25). This indicates that Blaine mainly is 300
a measure of size and size distribution, based on 200
theoretical spherical particles. Thus, it should be 100
noted that great variation was noted between 0

values measured on the same specimen, 0 200 400 600
Sarea (Blaine) [m2/kg]
800
especially between those performed by different

persons (and equipment). Figure 25. The linear relationship
between the calculated area and Blaine.
The highest single correlation is to be found Correlation
between the BET (N) and BET (H2O) measures 8000
(specific area). Although the measured value is
BET (H2O) [m 2/kg]
6000
not equal, the linear relationship is good (see
4000
Figure 26). One has to be aware of the
differences in size and polarity of the water and 2000
nitrogen molecule. This test has also been made 0
on fines (<1.0mm) sieved from different 0 2000 4000 6000 8000 10000 12000
aggregates, with the same good results. For BET (Nitrogen) [m2/kg]
binders, type cement, the BET (H2O) method has Figure 26. The linear correlation
not supplied reliable measures, and therefore not between the BET (N) and BET (H O)
2
recommended. measures.
Both BET (N) and BET (H2O) show strong correlation to the rheological measures. Why the
BET-method is better connected with rheological properties than the other surface area
quantifications could be explained by importance of shape, surface texture and porosity. If
11
the spread flow diameter D is recalculated into flow area (see Eq.4), the correlation with
BET gets even better. This is probably due to an exponential relation.
5. CONCLUSIONS
Due to the importance of the large surface area, quantification of fillers and the fine part of
aggregates properties is essential for the ability to control physical properties, such as
workability in the production of self-compacting concrete.
This study has proven the importance of particle size and geometry (shape, surface porosity
and texture).
The BET (H2O), a simple characterisation method for fillers and fines for self-compacting
concrete, has been introduced. The BET (H2O) has proven high potential. It is simple, low
cost, and has provided stable and reliable values. It has also shown on a strong correlation
with rheological properties and with the traditional BET (Nitrogen).
Other quantification methods have been carried out, but the specific area, quantified with
BET-technique, has shown to be the single most important measure concerning the mortar
rheology.
REFERENCES
1. Barnes H. A., Hutton J. F., Walters K., (1989), "An introduction to rheology", Elsevier,
Amsterdam.
2. Bartos P., (1992), "Fresh concrete: Properties and tests", Elsevier, Amsterdam.
3. Tattersall G. H., (1991), "Workability and quality control of concrete", E&FN Spon,
London.
4. Billberg P., (1999), "Self-compacting concrete for civil engineering structures - the
Swedish experience", Swedish Cement and Concrete Research Institute, CBI report 2:99,
Stockholm.
5. Persson A-L., (1996), "Image analysis of fine aggregates: Characterisation of shape and
grain-size parameters", Licentiate thesis, Royal Institute of Technology, Stockholm.
6. Fuglsang Nielsen L., (1993) "Moisture sorption in porous material - A modified BET-
description", 3rd Symposium on building physics in norden contries, pp 719-724, Vol 2,
Copenhagen.
7. Ahlgren L., (1972), "Moisture fixation in porous building materials", Devision of
building technology the Lund institute of technology, Report 36, Sweden (in Swedish)
8. Brunauer S., Emmet H. P., Teller., (1938) "Adsorption of gasses in multimolecular
layers", American Chemical Society.
9. Okamura H., Ozawa K., (1995), "Mix design for self-compacting concrete", Concrete
Library of the JSCE, No 25, pp 107-120, June, (Translation from Proc. of ISCE, No
496/V-24, 1994.8).
10. Domone P. L., Chai H., (1997), "Testing of binders for high performance concrete",
Cement and Concrete Research, Vol 27 (8), pp 1141-1147.
11. Personal communication with Dr O. Wallevik (Head of Concrete Division at the
Icelandic Building Research Institute), 2001.
12
Paper III - SCC flowability: Effect of changes in particle
surface area, and how to compensate for this
PAPER III: SCC FLOWABILITY: EFFECT OF CHANGES IN

PARTICLE SURFACE AREA, AND HOW TO
COMPENSATE FOR THIS
Esping O., “SCC flowability: Effect of changes in particle surface area, and how to
compensate for this”, Accepted for publication at 5th International RILEM Symposium
on Self-Compacting Concrete, 3-5 September, Ghent, Belgium, 2007.
SCC FLOWABILITY: EFFECT OF CHANGES IN PARTICLE

SURFACE AREA, AND HOW TO COMPENSATE FOR THIS
Oskar Esping
Dep. of Civil and Environmental Engineering, Chalmers University of Technology, Sweden.
Abstract
Due to the large particle surface area, quantification of fillers and the fine part of aggregates
is essential for the ability to control physical properties, such as workability of self-
compacting concrete. In the presented work, the effect of the specific surface area of gravel
and limestone filler on the rheology of self-compacting concrete has been evaluated. The
surface area was measured with a simplified BET-method, using water as adsorbate. A
model is presented, where a change in specific area by BET(H2O) is translated to a change in
water demand for the concrete mix. The model is based on an assumption that 30 full
molecular layers of water, covering the particle surface is required to decrease interactions
and provide lubrication, sufficient to create flowability. The results indicated that a change in
BET(H2O)-area of 1000 m2/kg corresponds to approximately 0.8% moisture content of the
gravel. E.g. a SCC with 1000 kg gravel (0-8 mm) that increases by 1000 m2/kg in area will
need 8.5 litre extra water, in order to retain its consistency. In cases where traditional
methods for geometrical characterization (size distribution, water absorption, modulus of
fineness, etc.) is kept within acceptance a normal gravel for concrete can vary by up to 7000
m2/kg in surface area.
1. INTRODUCTION
For concrete, particle concentration and size distribution strongly influences the workability
since its matrix consist a suspension of smaller particles filling the hollow spaces between
the coarser. To decrease the internal friction and generate mobility, the particle surfaces are
to be covered with water and the voids in the system to be filled. More water will reduce the
volume fraction of particles and thereby eases the matrix motion. Consequently, when the
contact zone between the particles decreases there will be a significant reduction of plastic
viscosity and yield stress. Other important properties affecting the workability are the
particle shape, porosity and surface texture. Since the ratio of surface area to volume
increases exponentially by particle irregularity (shape, surface texture and porosity) and
decreased size, quantification of geometrical properties of fillers and the fine part of the
aggregates is essential for the ability to control physical properties, such as workability.
A common problem at the job site or plant is that fresh concrete, of a given mix design, can
vary in workability from batch to batch and can have a large variation in consistency over
time (i.e. consistency loss). This is especially problematic for the self-compacting concrete
(SCC), due to its great complexity and because of its sensitivity to variation in the
constituents’ properties (gravel moisture content, aggregate grading, etc.). Contrary to
ordinary concrete with insufficient flowability on site, SCC is not to be adjusted with extra
water or plasticizer, or given extra energy by vibrating.
1
As the aggregate represents 60-80% of the total volume of concrete, it is obvious that its
influence on the fresh and hardened concrete is substantial. It is well known that two
aggregates, with apparently similar grading, can provide significant differences in concrete
workability (see e.g. [6] and [9]). These differences can be referred to the aggregate fineness,
surface texture, shape, porosity, mineralogy, etc. Properties of fine particles (<63 µm) and
their influence are often neglected because traditional standard methods for characterizing
aggregates are deficient or too complicated. Even though the content by volume or weight is
often small, the number of particles and their total surface area are large. A content of up to 3
vol-% of particles finer than 63 µm (EN 933-1, or 75 µm according to ASTM C33) is
normally considered harmful, but these particles and their surface properties have a
considerable influence on the quality of the concrete, either fresh or in hardened state [8].
The gravel fineness is traditionally quantified by modulus of fineness from the size
distribution, a method underestimating the contribution of the fines. The cement and filler
particles fineness is traditionally quantified with Blain measure. Due to the methodology
where the specific surface area is determined from air permeability, based on packed
spherical particles, information of the shape, texture and surface porosity is neglected. Other
possibly more correct methods, such as the BET with Nitrogen gas and image analysis is
more seldom used due to its complexity and costs.
The aim of this experimental study was to investigate the possibility to detect variations in
raw material properties that are deleterious for the fresh concrete quality, and how to
compensate for these.
2. TEST METHODS
2.1 BET(H2O)
By using BET theory, the specific surface area (S) can be determined by deducing the area
from the adsorbed volume of gas molecules required to cover and form a monolayer on the
surface of the sample [3]. The filler and fine part of aggregate specific surface area was
determined gravimetrically by the BET multipoint method, using water (moisture) as
adsorbate at different relative humidity (RH). The test was performed at 20ºC with climate
boxes with 11.3% and 33.1% RH, achieved with LiCl and MgCl2 saturated salt solutions (see
Figure 1a). The sample size was approximately 100 g, the weight (m) was measured by a
precision balance with 0.001 g readability and the sample was dried by oven at 105ºC. The
samples were conditioned in each climate for 4 days.
Box with tight lid Sample
y [kg/kg]
b
Fan
a
Net
0.113 RH [-] 0.331
Figure 1: Schematic illustration of climate box, and the BET-plot with adsorption isotherm
as a linear function of RH (from [6]).
By plotting the adsorption isotherm (y, see Eq.1) as a function of the RH, the variables a
(interception) and b (slope) were determined by the linear relationship in a BET-plot (see
Figure 1). The specific surface area (SBETH2O) was then calculated according to Eq.2 [1]-[6].
2
RH ⋅ mdry
y= [kg/kg] (RH {0;1}) (Eq.1)
( m − mdry ) ⋅ ( 1 − RH )
3.54 ⋅ 10 6
S BETH 2 O = [m2/kg] (Eq.2)
a+b
2.2 Slump flow test

A traditional slump flow measurement was carried out by using a slump cone) and
measuring the average spread flow diameter D (in two perpendicular directions). The test
was performed at 7 and 60 minutes after adding water to cement. No compaction was needed
(as in the vertical slump test EN 12350-2 or ASTM C143 standard for concrete).
2.3 Rheology
The rheology was evaluated from the measurements, carried out at 7 and 60 minutes after
adding mixing water, where the sample was let to stand between the runs. The mortar test
measurement was performed using a Bohlin CVO200 rheometer and the concrete a ConTec
Visco5, both using rotating coaxial cylinder at a controlled shear rate ( γ& ) at 20ºC. The
experimental geometry is illustrated in Figure 2. The rheological evaluation of plastic
viscosity (ηpl) and yield stress (σ0) was made according to the Bingham model:
σ = σ 0 + γ& ⋅ η pl [Pa] (Eq. 3).
8 Ro=145 mm Concrete
Ri=100 mm sample
Shear rate [1/s]
4
No logging H=140 mm
2
Logging Rotating
0 outer cylinder
0 10 20 30 40 50 60 Measuring
Time [s] inner cylinder
Figure 2: The experimental setup, and the schematic illustration of the ConTec Visco5
rheometer for concrete (from [6]).
3. BET(H2O)-MODEL
When there is a change in the dry material specific surface area, and as this area has to be
covered with water in order to create mobility, the concrete water demand will change. One
way to compensate for these variations in filler or fine aggregate, is to consider the specific
area by BET(H2O) and translate this to a change in water demand of the concrete mix. With
the assumption that 1 litre of water in one molecule layer covers 3 546 000 m2, the change in
mixing water (∆W) due to a change in specific surface area (∆SBETH2O) can be calculated as:
nH 2O
∆W = ∆S BETH 20 ⋅ ⋅ m mtr [liter/m3] (Eq. 4)
3.546 ⋅ 10 6
where mmtr is the mass of the dry material of the mix, and nH2O is the number of full water
molecular layers covering the particle surfaces required to providing sufficient dispersion for
flowability. Based on numerous experiments, a suitable value was found to be nH2O=30
layers. This can be compared to the proposed, in literature, 5-20 molecular layers of water
adsorbed at high relative humidity [1][4][7][9] or as much as 60 molecular thickness [5].
3
4. MATERIAL AND MIX DESIGN

The mix design and its constituents, as used in this study, comprise typical materials and
compositions for self-compacting concrete in Sweden. The properties of the materials are
listed in Table 1. Five limestone fillers with different geological origin and five natural 0-8
mm gravel named “Hol” (sample F to J) were used. The “Hol” gravel was collected at five
different occasions over a two month period at a concrete production plant. The size
distribution and specific surface area by BET(H2O) for the limestone fillers are presented in
Figure 3, and for the “Hol” gravel in Figure 4.
Table 1: Properties of dry materials (cement, fillers, aggregates and admixture).
ID Type Name Supplier Density [kg/m3]
C CEM II/A-LL 42.5R Byggcement, Skövde Cementa 3 080
F Ground limestone L40, L15, L70, G100 & G200 NordKalk & Karbonater 2 700
A 0-8 Natural aggregate Hol, E and F to J Färdig Betong 2 650
A 8-16 Crushed aggregate Kungälv Färdig Betong 2 700
SP Super plasticizer (PCE) Sikament 56 SIKA 1 100
100 8 000
L15
80 G100 SBETH2O [m /kg] 6148
6 000
Passing [%]
L40(ref)
2
60 L40
G200 L15
40 4 000
L70 L70
2308
20 G100 1808 1894 1822
2 000
G200
0
0.002 0.004 0.008 0.016 0.032 0.063 0.125 0.25 0.5 0
Size [mm] L40 L15 L70 G100 G200
Figure 3: Size distribution and spec.surface area by BET(H2O) for the five limestone
fillers.
100 4 000
3348
80 3019
2808
SBETH2O [m /kg]
F(ref) 3 000
Passing [%]
2570
G 2341
2
60
H 2 000
40
I
20 J
1 000
Average
0
0.063 0.125 0.25 0.5 1 2 4 8 0
Size [mm] F(ref) G H I J
Figure 4: Size distribution and specific surface area by BET(H2O) for the five “Hol”
gravel.
The concretes were prepared in batches of 40 litres, mixed in a BHS60 twin-shaft paddle
mixer for 4 minutes after water was added to the premixed dry materials.
Two self-compacting mixes were investigated (see Table 2): (1) with the five different
limestone fillers and (2) with the five 0-8 mm natural gravels named “Hol”.
4
Table 2: Recipe of the w/c 0.55 SCC mixes, in kg/m3.

ID Product name 1. 2.
W Mixing water 187 187
C Byggcement 340 340
F L40 220
L40/L15/L70/G100/G200 220
A 0-8 Hol E 873
Hol F to J 873
A 8-16 Kungälv 728 728
SP Sikament 56 4.08 4.08
In order to retain the consistency, relative the mix with the reference material,
complimentary mixes were made with extra water (see Table 3) compensating for the
difference in specific area by BET(H2O). This was made according to Eq. 4.
Table 3: Changes mixing water (∆mw) due to the differences in specific surface area for the
limestone filler and “Hol” gravel.
“Hol”
Limestone ∆SBETH2O ∆mw ∆SBETH2O ∆mw
gravel
filler ID [m2/kg] [kg/m3] [m2/kg] [kg/m3]
ID
L40 (ref) - - F (ref) - -
L15 +499 +0.68 G +229 +1.69
L70 +4 340 +5.89 H +468 +3.45
G100 +86 +0.12 I +679 +5.01
G200 +13 +0.02 J +1007 +7.44

All test results are represented by a mean value based on two or more tests. The slump flow
and rheology (plastic viscosity and yield stress) were measured at two timings (7 and 60
minutes from water addition). The results from the flowability measures for the mix with the
five different limestone fillers are presented in Figure 5. Both slump flow and rheological
evaluation (yield stress and plastic viscosity), show significant differences between the
samples, which is reflected by the differences BET(H2O)-area (see Figure 3). It can be noted,
that thus the “L70” filler was the coarsest it generated the largest surface area and in the SCC
mix it reduced the flowability most. All mixes with extra water achieved nearly the same
consistence as the reference mix with limestone filler “L40”.
5
800
7 min 60 min
600
Spread [mm]
400
200
L40 (ref)
L15 (+0.68)
L70 (+5.89)
G100 (+0.12)
G200 (+0.02)
L15
L70
G100
G200
400 60
507 Pa 7 min 60 min
300
Yield stress [Pa]
Viscosity [Pa s]
7 min 60 min 40
200
20
100
0
0 L40 (ref)
L15 (+0.68)
L70 (+5.89)
G100 (+0.12)
G200 (+0.02)
L15
L70
G100
G200
G100
G200
G100 (+0.12)
G200 (+0.02)
L15
L70
L40 (ref)
L15 (+0.68)
L70 (+5.89)
Figure 5: Flowability measures for the SCC mix with the limestone fillers, both without
and with the extra water added to compensating the BET-surface.
The results from the flowability measures for the mix with the five “Hol” gravel are
presented in Figure 6. Similar to the results for the limestone filler (see Figure 5), the
flowability with the “Hol” gravels shows significant differences between the mixes, which
can be addressed to the differences in BET(H2O)-area. All mixes with extra water achieved
nearly the same consistence as the reference mix with gravel “F”, which indicates that the
differences in surface area can be compensated with water according to the proposed
BET(H2O)-model, see Eq. 4. It can be noted, that thus the gravel size distributions is similar
(see Figure 4), there is up to ~1000 m2/kg difference in BET(H2O)-area. This is ~¼ of the
differences for the limestone filler, but then the content of gravel in the mix is ~4 times
larger then the limestone filler (see Table 2). In [6] it was found that a natural gravel
collected at different spots in a gravel pit, with small differences in grading, can vary in
BET(H2O)-area by ~7000 m2/kg.
6
800
7 min 60 min
600
Spread [mm]
400
200
I
H (+3.45)
I (+5.01)
H
G
F (ref)
G (+1.69)
J (+7.44)
J
150 80
60 min 7 min 60 min
60
Yield stress [Pa]
Viscosity [Pa s]
100 7 min
40
50
20
0 0
I
H (+3.45)
I (+5.01)
I
H (+3.45)
I (+5.01)
H
G
F (ref)
G (+1.69)
J (+7.44)
H
G
J
F (ref)
G (+1.69)
J (+7.44)
J
Figure 6: Flowability measures for the SCC mix with the “Hol” gravels, both without and
with the extra water added to compensating the BET-surface.
Question arises whether this extra water added for constant flowability, based on an
increased BET-area, is fixed to the aggregates or fillers and does not contributes to the
concrete hydration. Is it possible to add this extra water without affecting the w/c, in the
same approach made when using the particle water absorption (EN 1097-6 standard)? To
compensate for an increased BET-area by adding extra superplasticizer (SP) to the mix will
not have the same effect as extra water, as the SP (PCE based) normally only reduces the
yield stress and not the viscosity [10]. In Figure 7 the results of the measured compressive
strength for the SCC mix with the different limestone fillers, both without and with the extra
water added to compensating the BET-area, is given. The result shows that the strength is
promoted by increased area, whereas with additional water for constant flowability the effect
is in reverse ratio. This indicates that approx. 50% of this water can be added without
affecting the w/c.
Comp. Strenght, 28d [MPa]
48
No compensation Additional water
47
46
45
L40 L15 L70 G100 G200
Figure 7: Compressive strength (28 days) for the SCC mix with the limestone fillers, both
without and with the extra water added to compensating the BET-area
7
6. CONCLUSIONS
An experimental investigation of the effect of the specific surface area of different gravels
and limestone fillers and their influence on the rheology of SCC was carried out. The area
was measured with a simplified BET-method, using water (as moisture) as adsorbate. A
model was presented, where the effect of change in specific area by BET(H2O) is translated
to a change in water demand for constant flowability of the concrete mix. The following
observations and conclusions were made:
Due to the importance of their large surface area, quantification of fillers and the fine
part of aggregates’ properties is essential for the ability to control physical properties,
such as workability, in the production of SCC.
For better quality control and prediction of fresh concrete behaviour, the specific
surface area by BET is proposed as a potential means of geometrical characterization
for fillers and aggregates containing fines.
A coarser material can provide larger surface area than a finer, due to differences in
surface texture and porosity, and thereby negatively influence the flowability.
Addressing to the changes in BET(H2O)-area, a gravel with apparently consistent
grading over time can provide significant differences to the concrete workability.
The proposed model showed that it was possible to calculate the extra water needed to
compensate for changes in filler and fine aggregates BET(H2O)-area, in order to control
and produce SCC with small variations in flowability.
Approximately 30 molecular layers of water, covering the particle surface, are required
to decrease interactions and provide lubrication, sufficient to create flowability.
It was shown that the free water content, available to provide flowability, in 1 m3 SCC
mix can vary by several litres due to differences in apparently equivalent fine
aggregates. A change in BET(H2O)-area of 1000 m2/kg corresponds to approximately
0.8% moisture content of the gravel. E.g. a SCC with 1000 kg gravel (0-8 mm) that
increases by 1 m2/g in area will need 8.5 litre extra water, in order to retain its
consistency.
ACKNOWLEDGEMENTS
Financial support from Färdig Betong and Thomas Concrete Group is greatly appreciated.
REFERENCES
[1] Ahlgren L. (1972): “Moisture fixation in porous building materials”, Division of building
technology the Lund institute of technology, Report 36, Sweden (in Swedish).
[2] Allen T. (1997): “Particle size measurement – Surface area and pore size determination”,
London.
[3] Brunauer S., Emmet H.P., Teller E. (1938): “Adsorption of gasses in multimolecular layers”,
American Chemical Society.
[4] Brunauer S. (1944): “The adsorption of gases and vapours”, vol 1, Oxford.
[5] Eirich F. R. (1960): “Rheology – Theory and applications”, vol 3, New York.
[6] Esping, O. (2004): “Rheology of cementitious materials: effects of geometrical properties of
filler and fine aggregate”, Chalmers University of Technology, Göteborg.
[7] Gregg S. J., Sing K. S. W. (1967): “Adsorption, surface area and porosity”, New York.
[8] Neville A. M. (1963): “Properties of concrete”, London.
[9] Powers T. C. (1968): “The properties of fresh concrete”, New York.
[10] Wallevik O. (2003): “Rheology – A scientific approach to develop self-compacting concrete”,
3rd International Symposium on SCC, Reykjavik.
8
Paper IV - Investigation of autogenous deformation in SCC
PAPER IV: INVESTIGATION OF AUTOGENOUS

DEFORMATION IN SCC
Esping O., “Investigation of autogenous deformation in self-compacting concrete”,

International RILEM Conference on Volume Changes of Hardening Concrete, 20-23
August, pp 273-282, Lyngby, Denmark, 2006.
INVESTIGATION OF AUTOGENOUS DEFORMATION IN SELF-

COMPACTING CONCRETE
O. Esping
Chalmers University of Technology, Göteborg, Sweden
Abstract
For modern concretes, such as high-strength and self-compacting concrete (SCC),
increased amount of fines and binder content are a common explanation for the large
autogenous shrinkage and early-age cracking. In order to investigate the influence of
fineness of concrete constituents on autogenous shrinkage, tests with SCC, incorporating
limestone fillers with different specific surface area (by BET), were conducted. A
dilatometer was used, generating measures of linear autogenous (sealed) deformation of the
concrete cast in vapour-proof flexible tube mould. Temperature and pore pressure were
simultaneously measured with the deformation. Tests were conducted on mixes both with
and without cement, i.e. with and without chemical shrinkage. The results indicated that
increased surface area generated an increased magnitude and rate of autogenous shrinkage,
without influencing the times to initial and final set. The mixes without cement appeared to
generate a large “autogenous” shrinkage, without the presence of chemical reaction of
cement and water (hydration). The shrinkage was approximately 0.8 mm/m at 24 hours, after
an initial swelling up to 4 hours. This is the same magnitude as for the mixes with cement,
but then these mixes generated no swelling and almost all shrinkage before final set (at ~11.5
hours from mixing). Increased particle surface area also decreased the rate and magnitude of
evaporation, and consequently reduced the plastic crack tendency, despite increased
autogenous shrinkage. Adding extra water to the mix, compensating for the loss of
flowability due to increased particle surface area, increased the crack tendency significantly.
INTRODUCTION
Early-age shrinkage and cracking have become a recurrent problem in concrete
construction. Conditions such as reduced maximum aggregate size, increased amount of
fines, presence of retarding admixtures, increased binder content, and deficient covering and
curing all contribute to this problem.
At early age, when the cement paste is young and has poorly developed mechanical
properties, autogenous and drying shrinkage, both incorporated in the plastic shrinkage, are
the two main driving forces for cracking. When the concrete dries out due to evaporation, the
loss of water from the paste generates negative capillary pressure, causing the paste to
contract (see Wittmann [1]), which in turn can lead to cracks. These contracting capillary
forces are in reverse ratio to the meniscus radius, and hence the capillary tension stresses
increase with decreasing pore sizes and interparticle spaces. Care has to be taken to protect
the surface against drying, although experience in the use of concretes with low w/b has
revealed that severe cracking may occur in spite of proper protection (curing membrane,
1
etc.); see Bjøntegaard et al. [2]. For a concrete where evaporation is prevented, a contracting
negative capillary pressure will also develop, but only once the hydration commences and
the concrete sets (see Holt [3]). As long as the concrete is fluid, autogenous shrinkage is
considered to be equal to the chemical shrinkage; but once the self-supporting skeleton starts
to form, the autogenous will diverge from the chemical (e.g. Hammer [4], Jensen & Hansen
[5]). The pattern of autogenous deformation, exemplified in Figure 1, comprises three
distinct stages which can be defined as (I) plastic, (II) semiplastic and (III) rigid, separated
by the time to initial and final set; see Esping & Löfgren [6]. It has been suggested (e.g. by
Barcelo [7]) that, when measuring the autogenous deformation, the setting will be
manifested as a change of the slope of the deformation. Furthermore, once the internal voids
are created, it leads to the development of a capillary pore underpressure in the skeletal
structure (see Figure 1), which causes an external deformation of the hardening concrete (see
Radocea [8]).
Plastic Plastic Semiplastic Rigid
Water
Self-supporting skeleton starts to form

Cement grains
Initial set
Semiplastic
Final set
Solid grains
(aggregate/filler) Pore pressure (measured)
Autogenous deformation (measured)

Rigid Temperature (measured)
Solid hydrates
Chemical shrinkage (assumed)
Gas voids/pores 0 ~6 ~12 ~18 ~24
Figure 1: Schematic representation of the early-age linear autogenous deformation of

concrete and the corresponding development of temperature, capillary pore
pressure and microstructure (based on measures of SCC with w/c 0.45, from
Esping & Löfgren [6]).
It can be argued that the deformation occurring when the concrete is plastic mainly causes
setting and has little consequence for the risk of cracking, while the shrinkage taking place
when the concrete is semiplastic is considerably more detrimental as the concrete at this
stage has poorly developed tensile strain capacity; see Kasai et al. [9].
This paper aims at demonstrating how changes in particle specific surface area affect the
early-age deformations, primarily the autogenous.
In this study, the change in area is represented by limestone fillers with different specific
surface area quantified with the BET(H2O) method. Furthermore, early age is considered as
the time from mixing up to 24 hours after mixing. The term ‘deformation’ is preferably used,
since expansion also may occur. Autogenous deformation is considered to be the bulk
deformation under sealed conditions, and is referred to the full period of hardening from the
time when water was added to the mix. Linear displacement was used for measuring
autogenous deformation. No corrections were made for the differences between linear and
volumetric changes during the fluid state (before initial set). Moreover, ideal isothermal
conditions are attributed to autogenous deformation, and this was not strictly the case. No
compensation for thermal changes was made.
2
TEST METHODS
Autogenous shrinkage test method

In this study, autogenous linear deformation was monitored by a concrete digital
dilatometer (CDD), developed in order to start measurement before setting, when concrete is
fresh. The method is a modification of the CT1 digital dilatometer for pastes and mortars;
see Jensen & Hansen [10]. The CDD sample consists of a concrete specimen, cast in a steel
coil-reinforced vapour-proof flexible polyurethane tube with inner diameter of 82 mm and
specimen length ~400 mm, sealed with hose clamps and O-ring-equipped PVC end-caps.
The unrestrained linear deformation was recorded with a digital gauge (0.003 mm accuracy).
The test, containing three complete CDD setups, was performed in a thermostable room at
20ºC, where the recording was started at 30 minutes from water addition. In order to
elucidate the mechanism of autogenous deformation, and as it is highest up to an age of 12
hours, it is necessary to measure the deformation immediately after mixing (see Aïtcin [11]).
The equipment and apparatus for a typical test are shown in Figure 2. Due to greater stiffness
in the radial than in the longitudinal direction of the mould, when the concrete is in the fluid
state, the flexible mould transforms most of the volumetric deformation into a linear
deformation. As the concrete undergoes transition from a fluid to a rigid state, the
deformation becomes isotropic. The ratio between linear and volumetric deformation is
shown in Figure 2. No correction for this was made, as the setting point is not a well-defined
physical state but rather a continuous transformation from a liquid to a solid state (see Jensen
& Hansen [5]). The experiments were supplemented with measurements of temperature and
pore pressure placed in the centre of the core. The pressure transducers were connected to a
de-aired water-filled system with a needle (internal diameter of 0.4 mm and 50 mm length).
0%
Length change (deformation)
y = 0,338x
Specimen length 400 mm -1%
Adjustable Digital gauge
fixture Mould diameter 82 mm (1/1000 mm)
-2% y = 0,796x
2
y=x R = 0,9999
0 001
-3%
-4% Fluid (measured)
-5%
0% -1% -2% -3% -4% -5%
Volume change
Figure 2: To the left, illustration of the Concrete Digital Dilatometer (CDD) for linear
autogenous deformation measurement (from Esping & Löfgren [6]). To the right,
the ratio between linear and volumetric deformation for the mould. Filled with a
Newtonian fluid the ratio follows the measured ratio, but once rigid the ratio will
follow the calculated 3-D deformation (from [12]).
Plastic shrinkage cracking test method

To evaluate the plastic crack tendency of concrete at early ages exposed to drying, a
modified ring-test method, originally developed by Johansen & Dahl [13], was used. The
crack tendency was represented by a mean value of total crack area (crack length × crack
width) on the concrete surface of each of three specimens. The setup was equipped with
measurements of evaporation (by a scale), temperature and pore pressure (at depth 20 and 60
mm). Further description of the method can be found in Esping & Löfgren [6] and [14].
3
MATERIALS AND MIX DESIGN

The mix design and constituents used comprise typical materials and composition for
self-compacting concrete (SCC) in Sweden, listed in Table 1. Previous tests have shown that
at a w/c of about 0.55 the plastic crack tendency is at a minimum point, and that the interplay
between evaporation and autogenous deformation is at equilibrium (Esping & Löfgren [6]).
The limestone fillers’ size distribution and specific surface area by BET(H2O) are given in
Figure 3. It can be noted that, despite L70 being the coarsest limestone filler, it showed the
largest surface area. Normally, increased fineness generates a larger surface, but L70 is
probably more porous due to differences in geological origin and thereby larger in area.
The concretes were prepared in batches of approximately 40 litres, and mixed in a twin-
shaft paddle mixer for 4 minutes after water was added to the premixed dry materials. The
admixtures were added directly after the water.
Table 1: Properties of constituents and SCC composition (w/c 0.55).
ID Type
Product name Supplier Density Mass content
C CEM II/A-LL 42.5R
Byggcement, Skövde Cementa 3 080 kg/dm3 340 kg/m3
W Tap water - - 1 000 187
L40, L15 & L70 NordKalk
F Ground limestone ~2 700 160
G100 & G200 SMA Karbonater
A 0-8 Natural aggregate Hol NCC Ballast 2 650 875
A 8-16 Crushed aggregate Kungälv NCC Ballast 2 700 730
SP Superplasticizer (PCE) Sikament 56 SIKA 1 100 4.08
100 8 000
Specific surface area, BET(H2O) [m /kg]
2
6150
80
6 000
Passing [%
60
4 000
L40
40
L15
2310
L70 1810 1890 1820
2 000
20 G100
G200
0 0
0.002 0.004 0.008 0.016 0.031 0.063 0.125 0.25 0.5 L40 L15 L70 G100 G200
Size [mm]
Figure 3: The five limestone fillers. To the left is the size distribution, and to the right the
specific surface area measured with the BET(H2O) method.
Mixes were also made without presence of cement, in order to evaluate the effect (if any)
of particle surface area on the autogenous deformation without influence of chemical
shrinkage. The cement was replaced with an equal volume of limestone filler, i.e. the filler
content was increased from 160 to 458 kg/m3. Concrete flowability strongly depends on the
size of the particle surface area which has to be covered with water to create mobility. When
the specific surface area increases, so will the water demand of the mix for the same
consistency. Using L40 as reference, extra water was added to the mixes, compensating for
the differences in surface area by BET(H2O) and regaining constant flowability. A model
was used where 30 molecular layers of water covering the particle surface are required to
decrease interactions and provide lubrication sufficient to create flowability; see Esping [15].
4
In Table 2 the changes in recipe, due to differences in specific area of limestone filler, are
given. This was only applied to the plastic shrinkage ring test, as the effect of water content
on autogenous deformation has previously been demonstrated by Esping & Löfgren [12].
Table 2: Mixing water with compensations for the differences in specific surface area of
limestone fillers. L40 is used as reference (smallest surface area).
ID L40 (ref) L15 L70 G100 G200
3 187.02 (+0.02)
W 187 liter/m 187.68 (+0.68) 192.89 (+5.89) 187.12 (+0.12)
RESULTS
Autogenous deformation (with cement)

The results of the autogenous deformation measurements for the SCC incorporating the
five limestone fillers with different specific surface area are presented in Figure 4(a), while
Figure 4(b) and Figure 5(a) show the rate of the deformation. As can be observed, increased
surface area (by BET method) increased both the magnitude and rate of shrinkage, primarily
in the plastic region. The time to initial and final set, evaluated from the pattern of
autogenous deformation when the rate is close to zero, was 6.1 respective 11.6 hours from
mix; see Figure 5(b). The differences in surface area had almost no effect on times to set
(shorter than ±0.1 hours). This is confirmed by the measured temperature development; see
Figure 7(a-e).
Previous tests show that increased water content decreases the rate and magnitude of
autogenous deformation, primarily as plastic, without affecting the time to set, which is
equivalent to the effect that decreased surface area has (see Esping & Löfgren [12]).
0 100
L40
Rate of deformation [10 /h]
-6
G200 0
-300
G100
-6
L15 -100
L40
-600
G200
-200
G100
-900 L15
-300
L70 L70
-1200 -400
0 6 12 18 24 0 6 12 18 24
(a) (b)
Figure 4: SCC w/c 0.55 containing limestone filler with different specific area: (a) the
autogenous deformation and (b) the rate of deformation.
5
-400 15
Rate of deformation [10 /hour]
Time to set (from mix) [hour]

Plastic
-6
-300
Semiplastic 10
-200
5
-100 Initial set
Final set
0 0
L40
L15
L70
G100
G200
L40
L15
L70
G100
G200
(a) (b)
Figure 5: Evaluated values from autogenous deformation in the plastic and semiplastic
period: (a) the rate of autogenous deformation and (b) the rate of deformation.
Furthermore, Figure 6(a) shows the development of pore pressure, and Figure 6(b) the
evaluated maximum rate of pore pressure which occurred at approximately 7-8 hours from
mixing. The time to and magnitude of maximum underpressure could not be evaluated due
to the loss of pressure at random times. This effect is usually referred to as the breakthrough
pressure; see Wittman [1].
0 -60
G200
-20
Pore pressure [kPa]
dP/dt [kPa/hour]
-40
-40
L40
-60
L70
-20
-80 G100
L15
-100
0 3 6 9 12 0
Time (from mix) [hour] L40 L15 L70 G100 G200
(a) (b)
Figure 6: SCC w/c 0.55 containing limestone filler with different specific area: (a) the
development of capillary pore pressure during the first 12 hours from mix, and
(b) the maximum rate of pore pressure (at approximately 7-8 hours from mix).
Finally, the relationship between the development of autogenous deformation,

temperature, and pore pressure for the concretes with the five limestone fillers is shown in
Figure 7. As can be seen, as long as the concrete is plastic the deformation develops rapidly
with an almost linear relationship, while during this period the temperature and capillary
pore pressure undergo only small changes. However, at one point (at ~5 hours) the rate of
deformation is slowed down, indicating ‘setting’ of the matrix. At the following knee point
(at ~6 hours), indicating the initial set, both the capillary pore pressure and the temperature
reach an accelerating phase, which indicates that the cement hydration accelerates (see
Esping & Löfgren [6]). The final set (at ~12 hours) is manifested by a plateau in
deformation, slightly ahead of the temperature peak.
6
Max L40 L15 L70
Temp. Temp.
Temp.
Pore
Pore Pore
pressure
pressure pressure
Autogenous Autogenous
Autogenous
deformation deformation
deformation
Min
0 5 10 15 20 0 5 10 15 20 0 5 10 15 20
Time (from mix) [hour] Time (from mix) [hour] Time (from mix) [hour]
Max G100 G200

Temp. Temp.
Pore Pore
pressure pressure
Autogenous
Autogenous
deformation
deformation
Min
0 5 10 15 20 0 5 10 15 20
Figure 7: Development of temperature, pore pressure, and autogenous deformation

(normalized against maximum values), for SCC with respective filler.
“Autogenous” deformation (without cement)

The driving force of autogenous deformation is generally considered to be the hydration
process (generating chemical shrinkage); hence the term “autogenous” in the case of mixes
without cement is incorrect. The results of the “autogenous” deformation measurements for
the mixes without cement (same composition as SCC w/c 0.55, but cement is replaced with
equal-volume limestone filler) are presented in Figure 8. Even though no cement is present,
the mixes generated an “autogenous” shrinkage of approximately 0.8 mm/m at 24 hours,
counted after an initial swelling up to 4 hours. This is the same magnitude as for the mixes
with cement, but those generated no swelling and almost all shrinkage before final set. The
results indicate that larger surface area increases the deformation (both swelling and
shrinkage). The expansion can be explained by water being absorbed by the filler (and
aggregate) and by the disjoining pressure, i.e. the adsorption of water molecules in locations
where the distance between two surfaces is restricted, inducing pressure and expansion (see
Nawa & Horita [16]). Once lack of water occurs, this causes a restraining matrix of particles,
and there will be pores with meniscus-generated capillary tension and thereby a contraction
(see Hammer [17]).
7
800 600
L15
Rate of deformation [10-6/h]

L70
400 400
L70 L40
-6
L15
0 L40 200 G100
G100 G200
G200
0
-400
-200
-800 0 6 12 18 24
0 6 12 18 24 Time (from mix) [hour]
(a) (b)
Figure 8: The mix without cement (same composition as SCC w/c 0.55, but cement is
replaced with equal-volume limestone filler): (a) the “autogenous” deformation
and (b) the rate of deformation.
Plastic shrinkage cracking

A representative measure showing the relationship between the development of strain,
temperature, and pore pressure (at 20 and 60 mm depth) for one of the concretes exposed to
drying is shown in Figure 9(a). As can be seen, the pore pressure develops more rapidly in
comparison to sealed samples (autogenous). Here the maximum underpressure is reached at
5-6 hours from mix, with approximately 30 minutes between the two depths, whereas the
development of temperature is similar to the sealed samples. The measured strain indicated
that cracking was initiated at 3-4 hours from mixing. The average crack area (from three
samples) is presented in Figure 9(b), where it can be seen that the crack tendency is lower for
concrete incorporating filler with a high specific surface area.
Max 80
No compensation
Average crack area [mm ]
2
60 Extra water
Pore pressure (low)
Pore pressure (high)
40
Evaporation
Temperature
Strain 20
Initial crack
Min
0
0 5 10 15 20
L40(ref) L15 L70 G100 G200
(a) (b)
Figure 9: In (a) is the development of pore pressure, evaporation, temperature and strain
(normalized against maximum values), exemplified by the concrete with
limestone filler L40. In (b) is the crack tendency for the respective filler without,
and with, extra water compensating for the differences in surface area.
When adding extra water to compensate for the loss in flowability, the crack tendency
increased significantly. The differences in crack tendency are most likely a consequence
mainly of evaporation, which is verified by the measured evaporation in Figure 10(a) and its
8
initial rate (up to 4 hours from mix, before initial setting) in Figure 10(b). A large particle
surface area lowers the evaporation, whereas extra water increases the evaporation.
3 0,5
L70(+5,87)
No compensation
Rate of evaporation [kg/(m ·h)]

L15(+0.68)
Evaporation [kg/m ]
Extra water
2
2
2
L15
L70
L40(ref) 0,4
G100
1 G100(+0.12)
G200
G200(+0.02)
0
0,3
0 5 10 15 20
L40(ref) L15 L70 G100 G200
(a) (b)
Figure 10: SCC w/c 0.55 containing limestone filler with different surface area and extra
water compensating for this: (a) the measured evaporation and (b) the evaluated
initial rate (<4 hours from mix).
CONCLUSIONS
An experimental investigation of early-age (<24 hours) deformation was made on a series
of self-compacting concretes with w/c 0.55 containing limestone filler with different specific
surface area measured with BET(H2O). Autogenous linear deformations were measured and
additional investigation of plastic crack tendency was carried out, both complemented by
simultaneous measurements of pore pressure and temperature development.
The results show that:

• Increased particle surface area (by BET method) increased the rate and magnitude of
autogenous shrinkage, primarily in the plastic region, without affecting the
temperature development and the times to initial and final set.
• The relationship between autogenous deformation, temperature, and pore pressure
shows that, as long as the concrete is plastic, the deformation develops rapidly and
almost linearly while, during this period, the temperature and capillary pore pressure
undergo only small changes. However, at one point (at ~5 hours) the rate of
deformation is slowed down, indicating ‘setting’ of the matrix. At the following knee
point (at ~6 hours), indicating the initial set, both the capillary pore pressure and the
temperature reach an accelerating phase, which indicates that the cement hydration
accelerates. The final set (at ~12 hours) is manifested by a plateau in deformation,
slightly ahead of the temperature peak.
• The mixes without cement appeared to generate a large “autogenous” shrinkage,
despite absence of chemical reaction of cement and water (hydration). The shrinkage
was approximately 0.8 mm/m at 24 hours, after an initial swelling up to 4 hours. This
is the same magnitude as for the mixes with cement, but then these mixes generated no
swelling and almost all shrinkage before final set (at ~11.5 hours from mixing).
• Increased particle surface area decreased the rate and magnitude of evaporation and
consequently reduced the plastic crack tendency, despite increased autogenous
shrinkage. Adding extra water to the mix, compensating for the loss of flowability due
to increased particle surface area, increased the crack tendency significantly.
9
ACKNOWLEDGEMENTS
Financial support from AB Färdig Betong is greatly appreciated.
REFERENCES
[1] Wittmann, F.H., ‘On the Action of Capillary Pressure in Fresh Concrete’, Cement and Concrete
Research, Vol. 6, pp. 49-56, 1976.
[2] Bjøntegaard Ø., Hammer T. A., Sellevold E. J., ‘Cracking in High Performance Concrete before
Setting’, Symposium on High-Performance and Reactive Powder Concretes, Sherbrooke, 1998.
[3] Holt, E. E., ‘Early age autogenous shrinkage of concrete’. Technical Research Centre of Finland,
VTT Publication 446, Finland, 2001.
[4] Hammer T. A., ‘Test method for linear measurements of autogenous shrinkage before setting’, in
Autogenous shrinkage of concrete (ed. Tazawa E.), E & FN Spon, London, pp. 143-154, 1998.
[5] Jensen O. M., Hansen F., ‘Autogenous deformation and RH-change in perspective’, Cement and
[6] Esping, O., Löfgren, I., ‘Cracking due to plastic and autogenous shrinkage – Investigation of
early age deformation of self-compacting concrete’, Publication 05:11, Chalmers, Sweden, 2005.
[7] Barcelo, L., Moranville, M., and Clavaud, B., ‘Autogenous shrinkage of concrete: a balance
between autogenous swelling and self-desiccation’, Cement and Concrete Research, Vol. 35, pp.
177-183, 2005.
[8] Radocea A., ‘A Study on the Mechanisms of Plastic Shrinkage of Cement-Based Materials’,
Doctoral dissertation, Chalmers, Sweden, 1992.
[9] Kasai, Y., Yokoyama, K., and Matsui, I., ‘Tensile Properties of Early Age Concrete’,
Mechanical Behavior of Materials, Society of Materials Science, Vol. 4, pp. 288-299, Japan,
1972.
[10] Jensen O. M., Hansen F., ‘A dilatometer for measuring autogenous deformation in hardening
Portland cement paste’, Materials and Structures, Vol. 28 (181), pp. 406-409, 1995.
[11] Aïctin, P.C., ‘Autogenous shrinkage measurement’, in Autogenous shrinkage of concrete (ed.
Tazawa E.), E & FN Spon, pp. 257-268, 1999.
[12] Esping, O., Löfgren, I., ‘Investigation of early age deformation in self-compacting concrete’,
Conference advanced cement-based materials, DTU, Denmark, 2005.
[13] Johansen, R., Dahl, P.A., ‘Control of plastic shrinkage of cement’. 18th Conference on Our
World in Concrete and Structures, Singapore, 1993.
[14] Löfgren, I., Esping, O., ‘Early age cracking of self-compacting concrete’, RILEM Conference of
Volume Changes of Hardening Concrete, Denmark, August 2006.
[15] Esping O., ‘Rheology of cementitious materials – Effects of geometrical properties of filler and
fine aggregate’, Licentiate thesis, Publication No. P-04:3, Chalmers, Sweden, 2004.
[16] Nawa T., Horita T., ‘Autogenous shrinkage of high-performance concrete’, Proceedings on
microstructure and durability to predict service life of concrete structures, Japan, 2004.
[17] Hammer T. A., ‘Is there a relationship between pore water pressure and autogenous shrinkage.
Before and During Setting?’, in Self-desiccation and its importance in concrete technology,
Lund University of Technology, TVBM-3104, pp. 27-38, 2002.
10
Paper V - Investigation of early age deformation in SCC
PAPER V: INVESTIGATION OF EARLY AGE

DEFORMATION IN SCC
Esping O., Löfgren I., “Investigation of early age deformation in self-compacting

concrete”, 2nd International Symposium on Advances in Concrete Science, 11-15
September, Quebec, Canada, 2006.
INVESTIGATION OF EARLY AGE DEFORMATION IN SELF-

COMPACTING CONCRETE
Oskar Esping (1) and Ingemar Löfgren (2)
(1) Dept. of Civil and Environmental Engineering, Chalmers University of Technology,

Sweden, and AB Färdig Betong.
(2) Thomas Concrete Group AB, Sweden
Abstract
In the presented work, early age (< 24 h) autogenous deformation was measured and
crack tendency due to plastic shrinkage was evaluated; see Esping and Löfgren [1]. For the
autogenous deformation, a specially developed digital dilatometer was used which generated
accurate measurements of the linear displacements of the concrete, which was cast in a
vapour-proof flexible tube mould. The plastic shrinkage cracking tendency was evaluated by
exposing concrete specimens to early drying conditions while these were restrained by an
inner steel ring. A large number of different SCC constituents and mix compositions have
been investigated: e.g. w/c-ratio from 0.38 to 0.67, silica fume, and different admixtures. For
comparison, tests with standard concrete were also made. The influence of different
constituents and mixes on the autogenous deformation and plastic shrinkage crack tendency
was observed. The results indicated that a high crack tendency arose when there was: large
autogenous shrinkage (silica addition, low w/c, high fineness); high water evaporation (high
w/c, low fineness); retardation (retarder or high superplasticizer dosage); low content of
coarse aggregate. Minimum crack tendency was found at w/c 0.55.
1. INTRODUCTION
At early age, when the cement paste is young and has poorly developed mechanical
properties, autogenous and drying shrinkage – both incorporated in the plastic shrinkage –
are the two main driving forces for cracking. Generally, plastic shrinkage is usually defined
as the shrinkage of fresh concrete, exposed to drying, that takes place during the time when
the concrete is ‘plastic’, the duration is usually short (< 8 to 12 hours) and ends when the
concrete has reached its final set. In traditional concretes plastic shrinkage cracking is mainly
caused by the loss of water from the fresh concrete, e.g. by evaporation of water, which
generates negative capillary pressures; this cause the paste to contract (see Wittmann [2]),
which in turn can lead to cracks. These contracting capillary forces are in reverse ratio to the
meniscus radius, and hence the capillary tension stresses increase with decreasing
interparticle spaces. For a concrete where evaporation is prevented, a negative capillary
pressure will also develop, but only once the hydration commences and the concrete sets. To
avoid this type of cracks, care has to be taken to protect the surface against drying. However,
experience in the use of concretes with low w/b has revealed that severe cracking may occur
in spite of proper protection (curing membrane, etc). Conditions such as reduced maximum
aggregate size, presence of retarding admixtures, increased binder content, and deficient
curing all contribute to this problem. Early cracking is usually observed in the period soon
1
after casting up to 6-8 hours later, depending on the concrete temperature, material
composition, weather conditions and the degree of retardation. In this early phase, the
rheology of concrete changes dramatically as the concrete sets, i.e. it changes from a liquid
to a solid behaviour within some hours. At the same time the tensile strain capacity goes
through a minimum. The cause of this change in rheology is the hydration of Portland
cement, which is a complex sequence of chemical reactions leading to setting and hardening.
Immediately after mixing cement and water, reactions start to occur and these generate an
outburst of heat (Stages I in Figure 1). After these initial stages an induction period, or
dormant period, is entered (Stage II). During the induction period not much hydration takes
place, but this does not mean that the paste is ‘dormant’ with respect to volume changes.
Setting (during Stage III) is defined as the onset of rigidity in fresh concrete, and the
period of fluidity, preceding setting, corresponds to the induction period (Stage II); see
Figure 1(a). As long as the concrete is fluid, there will be a linear relationship between the
linear shrinkage and the volumetric chemical shrinkage. However, once the self-supporting
skeleton starts to form, the chemical shrinkage will mainly result in internal voids and the
linear deformation diverges from the chemical shrinkage. It has been suggested (e.g. by
Barcelo [4]) that, when measuring the linear deformation, the setting will be manifested as a
change of the slope of the deformation; see Figure 1(b). Furthermore, once the internal voids
are created it leads to the development of a capillary underpressure in the skeletal structure,
see Figure 1(b), which causes an external deformation of the hardening concrete. It can be
argued that the deformation occurring when the concrete is plastic may have little
consequence for the risk of cracking, while the shrinkage taking place when the concrete is
semiplastic is considerably more detrimental as the concrete at this stage has poorly
developed mechanical properties (low tensile strength and strain capacity).
Dissolution: Plastic Semiplastic Rigid
Deformation, Pressure & Temperature
Final set Diffusion-controlled

ettringite formation
Rate of heat evolution
reactions Temperature
Rapid formation Pressure
of C-S-H and CH
Formation of
Induction period: monosulfate
increase in Ca2+
concentration Final set
Initial set
Initial set Deformation
I II III IV V
0 ~6 ~12 ~18 ~24
~10 m ~4 h ~12 h ~24 h Time (from mixing) [hour]
Time of hydration I & II III & IV V
(a) (b)
Figure 1: (a) Heat evolution during hydration (based on [3]) and (b) early-age linear
autogenous deformation of concrete and the corresponding development of
temperature and capillary pore pressure (from [1]).
2. TEST METHODS
2.1 Autogenous shrinkage test method

In this study, autogenous linear deformation was monitored by a new test method, the
concrete digital dilatometer (CDD), developed in order to start measurement before setting,
when concrete is fresh, as well as for the hardening concrete. The method is a modification
of the CT1 digital dilatometer for pastes and mortars [5]. The CDD sample consists of a
concrete specimen, cast in a steel coil reinforced 0.4 mm thick vapour-proof flexible
polyurethene (PU) tube with inner diameter of 82 mm and specimen length ~400 mm, sealed
2
with a pair of hose clamps and 30 mm thick PVC end-caps equipped with O-ring sealing.
The mould was placed in a mechanical stable measuring rig, where a digital gauge recorded
the unrestrained linear deformation with an accuracy of 0.003 mm. The test was performed
in a thermostable room at 20ºC, where the measurement recording was started at 30 minutes
from water addition. The equipment and apparatus for a typical test are shown in Figure 2,
and for each test three complete CDD set-ups were used. The experiments have also been
supplemented with measurements of temperature and pore pressure in sealed specimens.
Specimen length 400 mm Didital gauge
Adjustable Mould diameter 82 mm 1/1000 mm
fixture
0 001
0 001
Figure 2: Test arrangement of the Concrete Digital Dilatometer (CDD) for linear
autogenous deformation measurement (from [1]).
2.2 Plastic shrinkage cracking test method

The method used is intended for determination of the cracking tendency of concrete at
early ages (developed by Johansen and Dahl; see [6] and [7]) but does not separate between
cracks formed before or after final setting. The variability (or scatter) of the test method is
relatively high; for one test series (three samples) the coefficient of variation is in the range
of 20 % to 50 % and the repeatability is in the same order (for three repeated series). In the
test, the fresh concrete is cast between two concentric steel rings and the specimen is then
placed under an air funnel, creating an air velocity of 4.5 m/s over a fresh concrete surface;
see Figure 3. The crack sensitivity is expressed as a crack index, see Figure 3, and both the
temperature and the weight loss of the specimens is continuously recorded. The
measurements started 60 minutes after mixing. After 20 hours of drying, the rings were taken
out of the rig and the crack index was measured as the average total crack area (crack length
× crack width) on the concrete surface of each of the three specimens. The crack width was
measured with a crack microscope (to an accuracy of 0.05 mm) and the crack length was
measured with a digital measuring wheel (to an accuracy of ±1 mm).
Fan
Climat conditions:
Average crack area =
∑ (crack length × crack width )
23±2 ºC
3
35±5% RH
Air funnel
Air velocity Steel rings
4.5 m/s
(Ø300/600)
Sample
10 Sample
80
Stress raisers
Scale Base plate
Ø 300
(steel)
Ø 600
Figure 3: Test arrangement for the determination of the cracking tendency (from [1]).
3
3. EXPERIMENTAL PROGRAM
3.1 Materials
The mix design and its constituents, as used in this study, comprise typical materials and
compositions for self-compacting concrete (SCC) in Sweden. The properties of the dry
materials and admixtures are listed in Table 1 and Table 2. The concretes were prepared in
batches of 40 or 60 liters, mixed in a twin-shaft paddle mixer for 4 minutes after water was
added to the premixed dry materials. The admixtures were added directly after the water.
Table 1: Properties of dry materials (cement, silica, filler and aggregate).

Density
ID Type Product name Supplier
[kg/dm3]
C CEM II/A-LL 42.5R Byggcement, Skövde Cementa 3 080
SF Silica fume Microsilica ELKEM 2 250
F Ground limestone Limus 40 NordKalk 2 670
A 0-8 Natural aggregate Hol Färdig Betong 2 650
A 8-16 Crushed aggregate Kungälv Färdig Betong 2 700
Table 2: Properties of admixtures.

Density Dry content
ID Type Product name Supplier
[kg/dm3] [weight%]
SP Super plasticizer (polycarboxylate ether) Sikament 56 SIKA 1 100 37 %
ACC Accelerator (sodium) SikaRapid-1 SIKA 1 200 37 %
RE Retarder (polyalkyl ether) SikaRetarder SIKA 1 200 27 %
SRA Shrinkage-reducer (polymeric glycol) SikaControl-40 SIKA 1 000 –
In order to evaluate the effect of constituent type and dosage, a number of different mixes
were investigated. The following mixes are presented in this paper (for the full experimental
study see [1]):
1. Reference concretes: w/c 0.38, 0.45, 0.55 and 0.67 (see Table 3).
2. Silica fume: 5% and 10% SF by cement weight (SF replaced equal C volume).
3. Coarse aggregate content: 20%, 30%, 40% (REF) and 50% A 8-16 of total volume of
aggregate. The changes were replaced by equal volume of A 0-8.
4. Superplasticizer dosage: 0.6%, 0.8% (REF) and 1.0% SP dosage of C weight.
5. Accelerator and retarder: 1.5% ACC and 0.2% RE by C weight.
6. Shrinkage-reducing admixture: 1.0% and 2.0% SRA by C weight.
7. Conventional concrete: w/c 0.55 with 345 kg cement and 60/40% (0-8 mm/8-16 mm)
aggregate; and w/c 0.67 with 330 kg cement and 60/40% (0-8 mm/8-16 mm) aggregate.
Table 3: Recipe of SCC reference mixes in kg/m3.

ID w/c 0.38 w/c 0.45 w/c 0.55 w/c 0.67
C 420 380 340 300
W 160 171 187 200
A 0-8 1021 998 960 926
A 8-16 694 678 651 628
F 40 100 160 220
SP 7.6 (1.8%C) 5.7 (1.5%C) 4.1 (1.2%C) 2.4 (0.8%C)
4
4. RESULTS
4.1 Autogenous deformation

The results of the autogenous deformation measurements for the reference concretes and
one conventional concrete are presented in Figure 4(a), while Figure 4(b) shows the rate of
the deformation. As can be observed, increased cement content (lower w/c) increased both
the total chemical shrinkage and its rate, and thereby the total autogenous deformation.
Increased cement content (lower w/c) also increased the autogenous deformation and its rate
in the semiplastic period (between initial and final set). Finally, increased superplasticizer
addition had a delaying and retarding effect on the hydration and thereby extends all the time
to the initial and final set.
Furthermore, Figure 5 shows the relationship between the development of deformation,

temperature, and pore pressure for the concretes with w/c 0.45 (a) and w/c 0.67 (b). As can
be seen, as long as the concrete is plastic the deformation develops with almost a linear
relationship and, during this period, the temperature and capillary pore pressure undergo
only small changes, which are linear. However, at one stage (at about five hours for w/c 0.67
and seven hours for w/c 0.45) the rate of the deformation is slowed down, indicating
‘setting’ of the concrete, and a knee point is reached. At this point in time, it can be seen that
both the capillary pore pressure and the temperature reach an accelerating phase, which
indicates that the dormant period is ended and that the cement hydration accelerates. Final
set is reached at about 10 hours for w/c 0.67 and 13 hours for w/c 0.45, which for the
deformation is manifested in a plateau slightly ahead of the temperature peak.
0 6 12 18 24 0 6 12 18 24
0 25
Rate of deformation [10 m/m/hour]
conventional w/c 0.55

conventional w/c 0.55
-200 0
-6
-400 -25
-6
SCC w/c 0.67

-600 SCC w/c 0.67 -50
SCC w/c
-800 SCC w/c 0.55 -75
SCC w/c 0.45 SCC w/c 0.45
-1 000 -100
SCC w/c 0.38 SCC w/c 0.38
-1 200 -125
Time [hours] Time [hours]
(a) (b)
Figure 4: Autogenous deformation of self-compacting concrete with w/c from 0.38 to 0.67
(a) and (b) rate of deformation (from [1]).
5
Pressure & Deformation [-] Pressure w/c 0.45 Pressure w/c 0.67
Pressure & Deformation [-]

Initial set
Temperature [-]
Temperature [-]
Temp.
Temp.
Final set
Final set
Deformation
Initial set
Deformation
0 5 10 15 20 0 5 10 15 20
(a) (b)
Figure 5: Development of temperature, capillary pore pressure, and autogenous
deformation (the axes have been normalized against maximum values): (a) for
concrete with w/c 0.45; and (b) for concrete with w/c 0.67 (from [1]).
It is well known that silica fume increases the autogenous shrinkage, as well as
accelerating the early hydratation and initiating the stiffness at earlier age. The results of the
autogenous deformation measurements for the concretes with silica fume are presented in
Figure 6. These results indicate that addition of silica fume increased the magnitude and rate
of autogenous shrinkage in all periods (in the plastic, semiplastic, and rigid periods), and the
effect increased with increased silica dosage. Silica fume decreased the plastic time period,
and the effect increased with increased silica dosage. No changes in semiplastic time could
be observed.
0 6 12 18 24 0 6 12 18 24
0 25
-200 0
w/c 0.55 (ref)

-6
-400 -25
-6
-600 -50
w/c 0.55 (ref)
-800 w/c 0.55 Si 5% -75
w/c 0.55 Si 5%
w/c 0.55 Si 10%
-1 000 -100
w/c 0.55 Si 10%
-1 200 -125
(a) (b)
Figure 6: Effects of silica fume (Si) on: (a) the autogenous deformation of self-compacting
concrete with w/c from 0.55 and (b) the rate of deformation (from [1]).
The results for the concrete with varying coarse aggregate content are presented in Figure
7. It should be noted that the content of coarse aggregate had a large impact on the rheology,
which can be deduced from the aggregate packing. Good packing improves the flowability
as more water is made available for dispersing the particles. The results indicate that
increased coarse aggregate content decreased both the magnitude and rate of autogenous
6
deformation. The effect was more apparent at higher content of coarse aggregate, which
might be explained by the coarser particles’ ability to create a restraining matrix. No
significant changes in times for the plastic and semiplastic periods could be observed, but an
increased content of coarse aggregate tended to delay the rigid period.
0 6 12 18 24 0 6 12 18 24
0

25
w/c 0.55 50% (8-16)
0
w/c 0.55 (ref) 40% (8-16)
-6
-200
-6
-25
w/c 0.55 30% (8-16)
-50
w/c 0.55 20% (8-16)
w/c 0.55 50% (8-16)
-400 -75
w/c 0.55 (ref) 40% (8-16)
-100 w/c 0.55 30% (8-16)
w/c 0.55 20% (8-16)
-600 -125
Time [hours] (w/c 0.55) Time [hours]
(a) (b)
Figure 7: Effects of coarse aggregate content (8-16) on: (a) the autogenous deformation
and (b) the rate of deformation (from [1]).
The results of the autogenous deformation measurements for the concrete with shrinkage
reducing admixture (SRA) are presented in Figure 8. The results indicate that addition of
SRA decreased the magnitude and rate of autogenous shrinkage for all concretes, and the
effect increased with increased SRA dosage. In the semiplastic period the effect of SRA was
not as pronounced as in the plastic and rigid periods. SRA showed no effect on the times of
the plastic and semiplastic periods.
0 6 12 18 24 0 6 12 18 24 0 6 12 18 24
0
w/c 0.55 SRA 2%

w/c 0.45 SRA 2%
-200 w/c 0.45 SRA 1% w/c 0.55 SRA 1%

-6
w/c 0.45 (ref)

-400
w/c 0.67 SRA 2%
w/c 0.67 SRA 1%
-600 w/c 0.55 (ref) w/c 0.67 (ref)
-800
(a) (b) (c)

Figure 8: Effect of the addition of shrinkage-reducing admixture (SRA) on autogenous
deformation: (a) for w/c 0.45, (b) for w/c 0.55, and (c) for w/c 0.67 (from [1]).
It is well known that SP retards the concrete, as it delays the early hydration and initiates
the stiffness at higher age. The results of the autogenous deformation measurements clearly
7
verify these phenomena, as can be seen in Figure 9(a). The results indicate that with
increased SP dosage the magnitude of autogenous shrinkage increased, which can be
explained by improved cement dispersion; see Holt [8]. An increased SP dosage also
increased the rate of shrinkage in the plastic and semiplastic periods. After setting, the effect
was the opposite, where the rate of shrinkage decreased with SP dosage. Moreover, an
increased SP dosage prolonged the plastic time period, while no changes in the semiplastic
time could be observed.
The results of the autogenous deformation measurements for the concrete with accelerator
(ACC) and retarder (RE) are presented in Figure 9(b). The results indicate that in the plastic
period (before initial setting), the accelerator increased the magnitude and rate of shrinkage
while the retarder hade the opposite effect, which could be expected. In the semiplastic
period, the accelerator and retarder showed no significant effect on magnitude and rate of
shrinkage. In the rigid period, both the accelerator and retarder increased the rate of
shrinkage. The accelerator tended to shorten the time to initial setting while the retarder
tended to delay it. According to the supplier (SIKA), RE will have a small delaying effect at
early hydration (to initial setting), and ACC will have no effect in the same period. The
results in this study showed the same tendency.
0 6 12 18 24 0 6 12 18 24
0 0
w/c 0.67 SP 0.6%
w/c 0.67 ACC (1.5%)
-200 w/c 0.67 (ref) SP 0.8% -200

w/c 0.67 (ref)
-6
-6
-400 -400
-600 w/c 0.67 SP 1.0% -600

w/c 0.67 RE (0.2%)
-800 -800
(a) (b)
Figure 9: Autogenous deformation of concrete with w/c 0.67: (a) effect of superplasticizer
dosage (SP) 0.6%, 0.8%, and 1.0%; and (b) effect of accelerator (ACC) and
retarder (RE) (from [1]).
4.2 Plastic shrinkage cracking

The results for the average crack area for the reference concretes are presented in Figure
10(a). As can be seen, it is evident that the concrete with the high w/c-ratio (0.67) had the
highest crack area and that the concrete with w/c 0.55 had the smallest crack area.
Furthermore, there seems to exist an optimum w/c-ratio for the investigated reference mixes,
which indicates that the w/c-ratio should be in the region of 0.55. The conventional concrete
had a higher crack area for both the tested w/c values. Evaporation curves for the concretes
are presented in Figure 10(b) where it can be seen that the evaporation is higher for a
concrete with high w/c and lower for low w/c. Moreover, the conventional concrete had
significantly higher evaporation, which could explain the increased cracking tendency. The
initial rate of evaporation (before initial set) for the investigated concretes varied between
8
0.37 and 0.44 kg/m2/h (the low values for w/c ≤ 0.45); this can be compared with the
evaporation from a free water surface of 0.50 kg/m2/h under same conditions.
150 4
conv. w/c 0.67
conv. w/c 0.55
2
Conventional Water
3
Evaporation [kg/m ]
2
100
SCC SCC w/c 0.67
2
50 SCC w/c 0.55

1
SCC w/c 0.45
SCC w/c 0.38
0 0
0.35 0.45 0.55 0.65 0.75 0 6 12 18 24
w/c Time [hours]
(a) (b)
Figure 10: Influence of w/c on: (a) the crack tendency and (b) the evaporation (from [1]).
When silica fume replaced 5% and 10% of the cement in the concrete with w/c 0.55, the
average crack area, which can be seen in Figure 11(a), increased dramatically. The effect
that silica fume had on the evaporation can be seen in Figure 11(b). Silica reduced the
evaporation. A possible explanation for the increased crack area is an increased amount of
small particles, which increased the autogenous shrinkage, as could be seen in the CDD
experiments.
150 4
2
w/c 0.55 (ref)

Evaporation [kg/m ]
3
2
100
2
w/c 0.55 Si 5%
50
w/c 0.55 1 w/c 0.55 Si 10%
0 0
0% 5% 10% 0 6 12 18 24
Silica [weight% of Cement] Time [hours]
(a) (b)
Figure 11: Influence of silica fume (Si) on: (a) the crack susceptibility and (b) the
evaporation (from [1]).
That the aggregates are important is well known, and it is beneficial to have large
aggregates and a high aggregate content. The effect of the coarse aggregate content (8-16 in
relation to total aggregate content) on crack area can be seen in Figure 12(a). As the coarse
aggregate was reduced, the crack area increased. Interestingly, however, an increased
amount of fine aggregate content also reduced the evaporation, as can be seen in Figure
12(b). This indicates that it is not only the evaporation which determines the cracking
behaviour; also the autogenous deformation plays an important role.
9
50 4
w/c 0.55 (ref) 40% 8-16

2
40
3
Evaporation [kg/m ]
2
w/c 0.55
30
2
20
w/c 0.55 30% 8-16
10 1
0 0
30% 40% (ref) 0 6 12 18 24
Coarse agg. content [vol% of total] Time [hours]
(a) (b)
Figure 12: Influence of coarse aggregate content (8-16) on: (a) the crack susceptibility and
(b) the evaporation (from [1]).
The shrinkage-reducing admixture (SRA) had a positive effect on the crack area. As can be
seen in Figure 13(a), for both the investigated concretes (w/c 0.55 and 0.67) the crack area
was reduced with SRA. The effect of SRA on the evaporation can be seen in Figure 13(b).
This effect starts to be notable at about three hours, after which point the evaporation and its
rate were significantly lower for the concretes containing SRA. The main effect of the SRA
is that it reduces the surface tension of the water (or pore solution), which has a positive
effect on shrinkage as it reduces the capillary tension caused by a reduction in pore radius.
However, the SRA also influences the rate of drying; the concretes containing SRA had a
significantly lower weight reduction than the reference concretes, and the mechanism is
notable as soon as the hydration starts.
100 4
w/c 0.67 (ref)
2
80 w/c 0.55 (ref)

Evaporation [kg/m ]
3
2
w/c 0.67
60
2
40
w/c 0.55 SRA 2%
w/c 0.55
1 w/c 0.67 SRA 1%
20
w/c 0.67 SRA 2%
0 0
0% 1% 2% 0 6 12 18 24
Shrinkage reducer [weight% of Cement] Time [hour]
(a) (b)
Figure 13: Influence of shrinkage-reducing admixture (SRA) on: (a) the crack susceptibility
and (b) the evaporation (from [1]).
The superplasticizer dosage seemed to have a large influence on the average crack area.
As can be seen in Figure 14(a), when the SP-dosage was reduced to 0.6% the crack area was
significantly reduced, and with the high SP-dosage (1.0%) the crack area increased. For the
case with a delayed additional SP-dosage (0.2% after 30 min) the crack area increased even
10
more. The effect that the superplasticizer (SP) dosage had on the evaporation is presented in
Figure 14(b). An increased dosage, as in the case with 1.0% and with a delayed dosage of
0.2%, resulted in an increased evaporation. With a reduced SP-dosage, 0.6%, the evaporation
was reduced. That the evaporation increases is probably a result of the prolonged setting
time.
200 4
w/c 0.67 SP 0.8% + w/c 0.67 SP 0.8+0.2%
2
0.2% delayed addition (30min) w/c 0.67 SP 1.0%
Evaporation [kg/m ]
150 3
2
100 2
w/c 0.67 (ref)
SP 0.8%
50 1
w/c 0.67 w/c 0.67 SP 0.6%
0 0
0,6% 0.8% (ref) 1,0% 0 6 12 18 24
SP dosage [weight% of Cement] Time [hours]
(a) (b)
Figure 14: Influence of superplasticizer (SP) dosage on: (a) the crack susceptibility and (b)
the evaporation (from [1]).
Similarly to the effect of the SP-dosage, accelerating and retarding the concrete had a
considerable effect on the crack area, as can be seen in Figure 15(a). For the concrete with
accelerator the crack area was reduced, while for the concrete with retarder the crack area
increased. The effect that the accelerator and the retarder had on the evaporation can be seen
in Figure 15(b), and is comparable to the effect that the SP-dosage had. For the concrete with
accelerator the evaporation was reduced, and for the concrete with retarder the evaporation
increased.
150 4
w/c 0.67 RE (0.2%)
2
w/c 0.67
Evaporation [kg/m ]
3
2
100
2
w/c 0.67 (ref)
50
w/c 0.67 ACC (1.5%)
1
0 0
ACC (1.5%) Reference RE (0.2%) 0 6 12 18 24
SP dosage [weight% of Cement] Time [hours]
(a) (b)
Figure 15: Influence of accelerator (ACC) and retarder (RE) on: (a) the crack susceptibility
and (b) the evaporation (from [1]).
11
5. DISCUSSION
Based on the results of this study, the following paragraph contains a general discussion
of the mechanisms leading to the formation of plastic shrinkage cracks, and a brief
description of possible actions to counteract them is presented. The formation of plastic
shrinkage cracks is governed by the development of capillary pore pressure. However,
depending on the characteristics of the concrete, different mechanisms are responsible. For
concrete with a high w/c-ratio, evaporation is the governing mechanism, while for concrete
with a low w/c-ratio (or with the addition of silica) the autogenous deformation is the driving
force. This is presented in Figure 16, which also indicates that the optimum concrete has a
w/c-ratio of 0.55. These observations also suggest that, in order to avoid plastic shrinkage
cracking, different actions need to be taken depending on the type of mechanism. A concrete
with a high w/c needs to be protected against early evaporation (e.g. by a curing membrane:
see [1]). For a concrete with a low w/c-ratio, protection against evaporation may not help, as
experience shows (see [9]), and the autogenous deformation needs to be reduced. This can be
achieved for example with a shrinkage-reducing admixture (which also reduces evaporation)
or by an increased coarse aggregate content.
6
Relative crack area [-]
0 6 12 18 24 4
0 2 Water w/c 0.67
Evaporation [kg/m ]
2
w/c 0.67
3
w/c 0.55
-6
-400 0 2
0.38 0.45 0.55 0.61 0.67
w/c 0.55
w/c 1
-800 w/c 0.45
w/c 0.45 w/c 0.38
w/c 0.38 w/c < 0.55 w/c > 0.55 0
-1 200 Autogenous w/c 0.55 Evaporation 0 6 12 18 24
Time [hours] deformation optimal Time [hours]
Figure 16: Separation of mechanisms governing the formation of plastic shrinkage cracks.
6. CONCLUSIONS
An experimental investigation of early age deformation and cracking tendency was made
on a number of self-compacting concretes, having w/c-ratio between 0.38 and 0.67, and the
influence of various mix parameters was investigated. Autogenous deformations were
measured and the cracking tendencies were investigated in a restraint ring specimen.
The results from the measurements of linear autogenous deformation by the CDD show that:
− Increased cement content (lower w/c) increased the rate of and total chemical
shrinkage and thereby the autogenous deformation.
− Increased coarse aggregate content decreased the magnitude and rate of autogenous
deformation.
− Addition of silica fume increased the magnitude and rate of autogenous shrinkage and
the effect increased with increased silica dosage. Silica fume decreased the time of the
plastic period.
12
− Addition of shrinkage-reducing admixture (SRA) decreased the magnitude and rate of

autogenous shrinkage for all concretes, and the effect increased with increased SRA
dosage.
− Increased SP dosage increased the magnitude of autogenous shrinkage. SP dosage
increased the rate of shrinkage at the plastic and semiplastic periods. After setting, the
effect was the opposite, where the rate of shrinkage decreased with SP dosage.
− Accelerator (ACC) increased the magnitude and rate of shrinkage, and retarder (RE)
had the opposite effect, in the plastic period (before initial setting). ACC and RE
showed no significant effect on the time of the periods, but RE tended to delay the
time to initial setting.
The conclusions that can be drawn from the restraint ring tests are that:
− The rate of evaporation was not always the governing factor for the cracking tendency.
− Silica fume led to increased autogenous deformation (the CDD experiments) and
increased crack area in the ring test, though the evaporation was reduced.
− Reduced aggregate content increased autogenous deformation, while the evaporation
was reduced.
− A shrinkage-reducing admixture (SRA) proved to be very effective in reducing the
cracking tendency. SRA reduced the autogenous deformation as well as the
evaporation.
− Delaying/retarding the hydration, with increased SP-dosage or by adding a retarder,
increased both the autogenous deformation (the CDD experiments) and the crack area.
− Accelerating the hydration, e.g. by adding an accelerator, decreased both the
autogenous deformation (the CDD experiments) and the crack area.
− The concrete with the high w/c-ratio (0.67) had the highest crack area. Furthermore,
there seems to exist an optimum w/c-ratio for the investigated mixes, which indicates
that the w/c-ratio should be in the region of 0.55; see Figure 10(a).
− The conventional concrete showed a similar tendency as the SCC (minimum cracking
tendency at w/c 0.55) but, due to higher evaporation, it was found to be more
susceptibile to cracking.
ACKNOWLEDGEMENTS
Financial support from SBUF (the Swedish construction industry’s organisation for
research and development) and AB Färdig Betong is greatly appreciated.
REFERENCES
[1] Esping, O. and Löfgren, I., 'Cracking due to plastic and autogenous shrinkage – Investigation of
early age deformation of self-compacting concrete – Experimental study', Publication No 05:11,
Department of Building Technology, Chalmers University of Technology, Göteborg 2005, 95
pp.
[2] Wittmann, F.H., 'On the Action of Capillary Pressure in Fresh Concrete', Cement and Concrete
Research, Vol. 6 (1976), pp. 49–56.
[3] Gartner, E.M., Young, J.F., Damidot, D.A., and Jawed, I., 'Hydration of Portland cement'.
Chapter 3 in Structure and performance of cements (ed. Bensted and Barnes), Spoon Press,
London, 2002.
13
[4] Barcelo, L., Moranville, M., and Clavaud, B., 'Autogenous shrinkage of concrete: a balance
between autogenous swelling and self-desiccation', Cement and Concrete Research, Vol. 35
(2005), pp. 177–183.
[5] Jensen O. M., Hansen F., 'A dilatometer for measuring autogenous deformation in hardening
Portland cement paste', Materials and Structures, Vol. 28 (181), pp. 406-409, 1995.
[6] Johansen, R. and Dahl, P.A., 'Control of plastic shrinkage of cement'. Paper presented at the 18th
Conference on Our World in Concrete and Structures, Singapore, 1993.
[7] NORDTEST NT BUILD 433, 'Concrete: Cracking Tendency – Exposure to Drying During the
First 24 Hours'. NORDTEST (Espoo, Finland, 1995).
[8] Holt, E.E., 'Early age autogenous shrinkage of concrete'. Technical Research Centre of Finland,
VTT Publication 446 (2001), Espoo, 184 pp.
[9] Bjøntegaard Ø., Hammer T.A., and Sellevold E.J., 'Cracking in High Performance Concrete
before Setting', Proceedings of the Int. Symposium on High-Performance and Reactive Powder
Concretes, Sherbrooke, Aug. 1998.
14
Paper VI - Effect of limestone filler BET(H2O)-area on
the fresh and hardened properties of SCC
PAPER VI: EFFECT OF LIMESTONE FILLER BET(H2O)-

AREA ON THE FRESH AND HARDENED
PROPERTIES OF SCC
Esping O., “Effect of limestone filler BET(H2O)-area on the fresh and hardened
properties of self-compacting concrete”, Submitted for publication in Cement and
Concrete Research, 2007.
Effect of limestone filler BET(H2O)-area on the fresh and

hardened properties of self-compacting concrete
O. Esping*
Department of Civil and Environmental Engineering, Chalmers University of Technology, Sweden
Abstract
This paper presents a study on the use of limestone fillers with different specific surface area and their effect on
the fresh and hardened properties of self-compacting concrete (SCC). The surface area was determined by a
simplified BET method using water vapour as adsorbate. A rheometer and a slump flow test were used to measure
the flowability of fresh concrete. A concrete dilatometer was used to measure the autogenous shrinkage, and a ring-
test for the plastic cracking tendency. The compressive strength was determined at 28 days. It was found that the
measure of BET(H2O)-area can be used to evaluate the water requirement for constant workability of the SCC,
where a change in BET(H2O)-area of 1 000 m2/kg corresponds to approximately 0.8% in moisture content. The
results showed that filler with a large area will result in an increased autogenous shrinkage, decreased evaporation,
lower plastic cracking tendency, and a higher compressive strength. With additional water the results was the
opposite.
Keywords: Concrete; Filler; Surface Area; Rheology; Autogenous; Shrinkage
1. Introduction retarding effect of superplasticizer, the concrete may

Ground limestone has been used in concrete develop a large autogenous shrinkage and plastic
production for the last 25 years [1], for the main cracking tendency [4]. At early age, when the cement
purposes of lowering the costs and environmental paste is young and has poorly developed mechanical
load of cement production, but also to increase the properties, evaporation and autogenous shrinkage,
concrete durability. More recently ground limestone both incorporated in the plastic shrinkage, are the
is also used as a filler material to improve the two main driving forces for cracking. When the
workability and stability of fresh concrete. For a high concrete dries out, the loss of water from the paste
flowable concrete, such as self-compacting concrete generates negative capillary pressure, causing the
(SCC), limestone filler is added to increase the paste to contract, which in turn can lead to cracks [5].
packing of the granular skeleton, bind excess water These contracting capillary forces are in reverse
and increase the volume of the continuous phase of proportional to the meniscus radius, and hence the
lubricating paste. SCC has to possess two capillary tension stresses increase with decreasing
incompatible properties: high flowability and high pore sizes and interparticle spaces. For a concrete
segregation resistance. This balance is made possible where evaporation is prevented, a contracting
by the dispersing effect of high-range water-reducing negative capillary pressure will also develop, but
admixture (superplasticizer) combined with only when the hydration commences and the
cohesiveness of high concentration of fine particles concrete sets [6]. As long as the concrete is fluid,
in additional filler material [2]. The main autogenous shrinkage is generally considered to be
mechanisms controlling this fine balance are related equal to the chemical shrinkage; but once the self-
to surface physics and chemistry; hence SCC is supporting skeleton starts to form, the autogenous
strongly dependent on surface activity of the will diverge from the chemical [7,8]. The setting will
admixtures together with the high specific surface be manifested as a change of the slope of the
area generated by the fines [3]. A consequence of the autogenous deformation, and once the internal voids
high concentration of powder material and the are created the development of capillary pore
1
underpressure in the skeletal structure will cause an surface area by Blaine fineness. Due to the
external deformation [9]. The pattern of autogenous methodology where the specific surface area is
deformation, exampled in Fig. 1, comprises three determined from air permeability, based on packed
distinct stages which can be defined as plastic, spherical particles, information about the shape,
semiplastic and rigid, separated by the time to initial texture and surface porosity is neglected [28,32].
and final set [11,12]. Other possibly more correct methods, such as the
BET with nitrogen gas and image analysis, are more
Plastic Semiplastic Rigid Self-supporting seldom used due to their complexity and costs.
skeleton starts to form
In this work, the effect of the specific surface area
Initial set
of different limestone fillers on the fresh and
Final set hardened properties of self-compacting concrete
Pore pressure (SCC) has been experimentally evaluated. The
(measured)
investigated properties were rheology, autogenous
Autogenous defor-
mation (measured) deformation, plastic cracking tendency and
Temperature compressive strength. The surface area was
(measured) determined by a simplified BET method, using water
Chemical shrinkage vapour as adsorbate. The change in BET(H2O)-area
0 ~6 ~12 ~18 ~24 (assumed) was translated to a change in water demand for the
concrete mix to maintain a constant workability,
Fig. 1. Typical early-age linear autogenous deformation
and corresponding development of temperature and based on the assumption that 30 full molecular layers
capillary pore pressure (based on measures of a SCC w/c of water covering the particle surface are required to
0.45, from [12]). decrease interactions and provide sufficient
lubrication for flowability.
The physical nature of better packing, by addition
of filler material, will not only govern the concrete
flowability, but also the compressive strength due to 2. Materials and mix design
the denser matrix and the better dispersion of cement
grains [13-16]. Furthermore, the surfaces of the filler The mix design and its constituents, as used in this
material will act as nucleation sites for the early study, comprise typical materials and compositions
reaction products of CH and CSH, which will for self-compacting concrete with w/c 0.55 in
accelerate the hydration of cement clinkers Sweden. The cement was a type CEM II/A-LL
(especially C3S) and consequently increase the early 42.5R, the fine aggregate a 0-8 mm natural ground
age compressive strength [17-20]. The effect of gravel, the coarse aggregate a 8-16 mm crushed
nucleation on the strength is dependent on the filler’s granite stone and the superplasticizer a
affinity to cement hydrates, and it increases with polycarboxylate ether-based type. Five ground
fineness and specific surface area of the filler. limestone fillers, with similar chemical composition
Limestone filler is not pozzolan, but nor fully inert as but different size distributions and specific surface
it reacts with the alumina phases of the cement. If the areas, were used. The area was determined by
cement has a significant amount of tricalcium BET(H2O); A simplified method, based on the BET
aluminate (C3A), calcium carboaluminate will be theory [33], where the area was determined
produced from the reaction between calcium gravimetrically on conditioned samples at different
carbonate (CaCO3) from the limestone and the C3A relative humidities and deduced from the adsorbed
[21-27]. This reaction, accelerating the hydration and volume of water molecules required to cover and
increasing the compressive strength, increases with form a monolayer on the surface of the sample
the C3A content of the cement and the fineness and [28,34-37]. The measured BET(H2O)-area (SBETH2O),
specific surface area of the filler. the area by Blaine (SBlaine) and the calculated area
from size distribution (SSize) [34,37] for the five
Since the ratio of surface area to volume increases limestone fillers are given in Fig. 2. The size
exponentially with particle irregularity (shape, distribution, measured with a Malvern laser
texture and porosity) and decreased size, and as this diffraction instrument, is presented in Fig. 3. The
area has a predominating effect on fresh and limestone filler named L40 has the smallest BET-
hardened concrete [28-31], quantification of area, and is used as a reference. It can be noted that
geometrical properties of fillers and fines is essential. the filler named L70 is the coarsest, but has the
Powder material (filler, cement, etc.) is traditionally largest BET-area.
characterized by the size distribution and the specific
2
The BET(H2O)-area for the gravel is ~2800 m2/kg, flowability. In Table 1 the changes in mixing water
and the BET(N2)-area for the cement is ~2000 m2/kg. due to differences in specific area of limestone filler,
For cement the BET(H2O) method is not valid. Due using L40 as reference, are given.
to the differences in size and polarity of the water
and nitrogen molecule the area by BET(H2O) is Table 1. Mixing water, in litre/m3, with compensations for
larger than by BET(N2) [37]. With a linear the differences in specific surface area of limestone fillers.
relationship of 1.55 [12], the BET(H2O)-area for the The L40 with the smallest BET area is used as reference.
cement can be estimated to 3100 m2/kg. L40 (ref) L15 L70 G100 G200
187.00 187.68 192.89 187.12 187.02
8 000 800 (+0.68) (+5.89) (+0.12) (+0.02)
SBlaine & SSize[m /kg]

SBETH2O[m /kg]
6 000 600
2
The concrete was prepared in batches of 40 litres,
2
4 000 400 and mixed in a BHS-60 twin-shaft paddle mixer for 4

2 000 200
minutes after water was added to the premixed dry
materials. The admixtures were added directly after
0 0 the water.
L40 L15 L70 G100 G200
BET(H2O) 1808 2307 6148 1894 1821
Blaine 357 565 254 345 353 3. Experimental methods
Size 259 458 160 165 154
Fig. 2. The five limestone fillers’ specific surface area by 3.1. Flowability test methods
BET(H2O) and by Blaine, and calculated from size
distribution. A slump flow test was carried out by using a
100 traditional slump cone (EN 12350-2), measuring the
L15 spread flow diameter (average from two
80 G100 perpendicular directions).
L40(ref) Concrete rheology measurements were performed
Passing [%]
60 L40 using a ConTec Visco5 with a rotating concentric

G200
L15 setup at a controlled shear rate ( γ& ). The experimental
40 L70
L70 geometry and measuring sequence are illustrated in
20 G100 Fig. 4. The rheological parameters, plastic viscosity
G200 (ηpl) and yield stress (σ0), were evaluated in
0 accordance with the Bingham model:
0.002 0.004 0.008 0.016 0.032 0.063 0.125 0.25 0.5 σ = σ 0 + γ& ⋅η pl (Eq. 1).
Size [mm]
Both slump flow and the rheology test were
Fig. 3. Size distributions for the five limestone fillers’. performed at 7 and 60 minutes after adding water to
the mix.
Corresponding mixtures were made without
presence of cement, in order to evaluate the effect (if Ro=145 mm
any) of fillers’ surface area on the autogenous Ri=100 mm
Measuring
deformation without influence of chemical inner cylinder
shrinkage. The cement content (340 kg/m3) was Concrete sample
H=140 mm
replaced with an equal volume of limestone filler Rotating
(i.e. filler content increased from 160 to 458 kg/m3), 8
outer cylinder
whereas the other constituents was kept constant.

Shear rate [1/s]
Finally, mixtures were made with additional water, 6

compensating for the fillers’ differences in 4
No logging
BET(H2O)-area in order to regain constant
2 Logging
flowability. A model was used where 30 molecular
layers of water covering the particle surface are 0
required to decrease interactions and provide 0 10 20 30 40 50 60
Time [s]
lubrication sufficient to create flowability [28]. An
Fig. 4. The ConTec Visco5 geometry, and the measuring
increase in BET(H2O)-area of 1000 m2/kg
sequence for the Bingham evaluation and segregation
corresponds to a need for additional water of ~0.8% estimation (from [28]).
by mass of filler (or gravel) content for constant
3
3.2. Autogenous deformation test method addition, and the sample was exposed to an air
velocity of 4.5 m/s with 23±2ºC and 35±5% RH.
The autogenous linear deformation was monitored Temperature, pore pressure and weight loss
by a concrete digital dilatometer (CDD), able to (evaporation) in the concrete specimens, and the
measure before setting when concrete is fresh [12]. strain in the inner ring, were continuously recorded.
The method is a modification of the CT1 dilatometer After 20 hours of drying the crack index was
for pastes and mortars by Jensen & Hansen [38]. The measured as the average (of three specimens) total
CDD setup consists of a concrete specimen cast in a crack area (crack length × crack width) on the
steel coil-reinforced vapour-proof flexible PE-tube concrete surface.
with tight end-caps, a measuring rig in stainless steel,
and a digital gauge (3 µm accuracy) recording the Steel rings (Ø300/600) Sample Stress raisers
unrestrained linear deformation; see Fig. 5. The test, Fan Base plate (steel) Cracks
containing three complete CDD setups, was Air funnel

performed at 20±1ºC, and was started at 30 minutes Air velocity
(4.5 m/s)
from water addition.
Sample
10 mm
Specimen length ~400 mm
Adjustable Digital gauge 80 mm
fixture Mould diameter 82 mm (1/1000 mm)
Scale
Ø 300 mm
0 001
Ø 600 mm
Fig. 6. The ring-test method for evaluation of plastic

shrinkage crack tendency (from [12]).
Fig. 5. The Concrete Digital Dilatometer (CDD) for linear 3.4. Compressive strength test
autogenous deformation measurement (from [12]).
Compressive strength was measured on 150 mm
Due to greater stiffness in the radial than in the cubes after 28 days, in accordance with EN 12390-
longitudinal direction of the mould, in fluid state, the 1,-2 and -3. All presented values of compressive
flexible mould transforms a large part of the strength (fc) are normalized to a porosity of 4%. Due
volumetric deformation into a linear deformation. As to the differences in limestone fillers’ BET-area the
the concrete undergoes transition from a fluid to a flowability was not consistent between the mixtures;
rigid state, the deformation becomes isotropic. Based hence also the air content was not equal. A series of
on empirical evaluation, the ratio between linear and corresponding mixes with different air content, in the
volumetric deformation for a liquid is approximately range of 0-5%, were made in order to evaluate the
0.8 [39]. No correction for this was made as the effect of air content (porosity) on the compressive
setting point is not a well-defined physical state but strength. This was made in accordance with the
rather a continuous transformation from liquid to a general equation for ceramic materials [41]:
solid state. f c = f c 0 ⋅ e k ⋅ P (Eq. 2). The porosity, P, was
The experiments were supplemented with determined by the measured density in fresh and
measurements of temperature and pore pressure hardened states (according to EN 12350-6 and EN
placed in the centre of the core. The pressure 12390-7), together with the measured air content by
transducers were connected to a de-aired water-filled pressure test (EN 12350-7). The compressive
system with a needle (internal diameter of 0.4 mm strength “without” pores, fc0, was 55.0 MPa for the
and 50 mm length). concrete de-aired in a vacuum desiccator for 30
minutes before moulding. The constant k was
3.3. Ring- test method for plastic shrinkage cracking empirically evaluated to 6.5.
The plastic cracking tendency of concrete at early

ages exposed to drying was evaluated, using a
modified ring-test method [12], originally developed
by Johansen & Dahl [40]. In the test, the fresh
concrete is cast between two concentric steel rings
and then exposed to drying; see Fig. 6. The
measurement was started at 60 minutes after water
4
4. Results and discussion calculated change in water content in order to regain

constant flowability. All mixtures with additional
4.1. Flowability water showed nearly the same rheological measures
as the reference mix with “L40”. At 7 minutes the
The results from the concrete flowability slump flow for the reference SCC (L40) and the
measurements (slump flow, yield stress and plastic mixtures with additional water was 595±5 mm, the
viscosity) are presented in Fig. 7. All test results are yield stress 71±12 Pa, and the viscosity 35±2 Pa·s.
represented by a mean value based on two or more The deviations were similar for the measures at 60
tests. minutes. The results are presented in [42].
800 The specific area by Blaine and from size
distribution (see Fig. 2) showed a poor correlation
600
with the flowability, which can be explained by the
differences in size distribution (see Fig. 3). Thus,
Spread [mm]
7 min
despite the fact that “L70” is coarser, it generates a
400
larger specific area and thereby a stiffer consistency,
60 min and has a larger water demand. This might be
200
explained by the filler’s geological origin and age,
where “L70” has a rougher and more porous particle
0 surface.
600
4.2. Autogenous deformation
450
Yield stress [Pa]
60 min The results (from [43]) of the autogenous

300
deformation measurements are presented in Fig. 8,
and the evaluated rate of deformation in Fig. 9. As
can be observed, increased surface area by
150
7 min BET(H2O) increased both the magnitude and rate of
shrinkage, primarily in the plastic region. The time to
0 initial and final set, evaluated from the pattern of
60 autogenous deformation when the rate reaches a
minimum, was 6.1 and 11.6 hours from mix,
60 min respectively. The differences in BET-area had almost
Viscosity [Pa s]
50 no effect on times to set (shorter than ±0.1 hours).

This was confirmed by the measured temperature
7 min development, where the measures showed almost no
40 differences.
Previous tests show that increased water content
decreases the rate and magnitude of autogenous
30
deformation, without affecting the time to set, which
0 2000 4000 6000 8000
2
is equivalent to the effect decreased particle surface
SBETH2O [m /kg] area [12].
Fig. 7. Limestone fillers BET(H2O)-area vs. slump flow, 0
yield stress and plastic viscosity for the SCC mixtures (at 7 L40
and 60 minutes). G200

-300
G100
-6
The results shows that the limestone filler L15

BET(H2O)-area have a strong influence on the SCC -600
flowability. The larger area, the higher yield stress
and viscosity, and consequently the lower slump -900
flow. The loss in flowability by time is significant L70
regarding slump flow and yield stress, and increases
-1200
with BET(H2O)-area, whereas the change in
0 6 12 18 24
viscosity by time is small. Time (from mix) [hour]
Furthermore, results indicated that the differences
Fig. 8. Autogenous deformation for the SCC with different
in BET(H2O)-area can be compensated for with a
limestone fillers (from [43]).
5
0 2 000 4 000 6 000 8 000

0 The results of the measured “autogenous”
Rate of deform. [10 /hour]
deformation for the mixtures without cement (same

composition, but cement is replaced with equal-
-100
-6
volume limestone filler) are presented in Fig. 12.

Semiplastic There was no separation observed, thus no cement
-200 was present, and the consistencies were similar to the
Plastic corresponding SCC mixtures.
-300
800
L15

-400 L70
2 400
SBETH2O [m /kg]
-6
Fig. 9. The limestone filler’s BET(H2O)-area and the L40
0
evaluated rate of autogenous deformation from autogenous G100
deformation in the plastic and semiplastic period. G200
-400
Furthermore, Fig. 10 shows the development of the
measured pore pressure, and Fig. 11 the evaluated -800
maximum rate of pore pressure which occurred at 7- 0 6 12 18 24
8 hours from mixing [43]. The point of maximum Time (from mix) [hour]
underpressure could not be evaluated due to the loss Fig. 12. Sealed (“autogenous”) deformation for the
of pressure at random times. This effect is usually mixtures where the cement was replaced with equal
referred to as the breakthrough pressure [5]. It can be volume filler (from [43]).
noted that the rate of pore pressure, and rate and
magnitude of autogenous deformation, showed to The hydration process (generating chemical
correlate with the limestone fillers’ BET(H2O)-area. shrinkage) is generally considered to be the driving
0 force of autogenous deformation; hence the term
G200 “autogenous” in this case might be incorrect. Even
Pore pressure [kPa]
-20 though no cement is present, the mixes generated an

“autogenous” shrinkage of approximately 0.8 mm/m
-40 at 24 hours, counted after an initial swelling up to 4
L40 hours. This is the same magnitude as for the mixes
-60
L70 with cement, but those generated no swelling and
-80 G100 almost all shrinkage before final set. At 48 hours, the
development of shrinkage levels out. It ought to be
L15
-100 noted that the effect of differences in surface area is
0 3 6 9 12 augmented, as the content of limestone filler is larger
Time (from mix) [hour] relative the SCC mixtures (i.e. 458 instead of 160
Fig. 10. Development of capillary pore pressure during the kg/m3). The results indicate that larger BET(H2O)-
first 12 hours from water addition (from [43]). area increases the deformation (both swelling and
shrinkage). The expansion can be explained by water
0 2 000 4 000 6 000 8 000
being absorbed by the filler (and aggregate) and by
0
Rate of pore pres. [kPa/hour]
the disjoining pressure, i.e. the adsorption of water

L40 & G200 molecules in locations where the distance between
two surfaces is restricted, inducing pressure and
-20
G100 expansion [44]. Once lack of water occurs, this
causes a restraining matrix of particles, and there will
L15 L70 be pores with meniscus-generated capillary tension
-40
and thereby a contraction [45].
-60
2
SBETH2O [m /kg]
Fig. 11. The limestone filler’s BET(H2O)-area and the
evaluated maximum rate of pore pressure (at 7-8 hours
from mixing).
6
4.3. Plastic shrinkage cracking The differences in crack tendency are most likely a
consequence mainly of evaporation, which is verified
A representative measure (from [43]) showing the by the initial rate of measured evaporation (up to 4
relationship between the development of strain, hours from mix, before initial setting) in Fig. 15. A
temperature, and pore pressure (at 20 and 60 mm large particle surface area lowers the evaporation,
depth) for one of the concretes exposed to drying is whereas extra water increases the
shown in Fig. 13. As can be seen, the pore pressure evaporation.
develops more rapidly in comparison with the sealed 0.44
samples, in Fig. 10. The maximum underpressure is
Rate of evapor. [kg/(m ·h)]

reached at 5-6 hours from mix, with approximately
2
Additional water
30 minutes between the two depths. The measured 0.42
strains indicate that cracking was initiated at 3-4
No compensation
hours from mixing [43]. The average crack area is
presented in Fig. 14, where it can be seen that the 0.40
crack tendency is lower for concrete incorporating
filler with a high BET(H2O)-area, and that, when
adding extra water to compensate for the loss in 0.38
flowability, the crack tendency increased 0 2000 4000 6000 8000
2
significantly. An increase in filler’s BET(H2O)-area SBETH2O [m /kg]
of 1000 m2/kg results in ~20% less cracking Fig. 15. Initial rate (<4 hours from mix) of evaporation,
tendency. without and with extra water added to compensate for the
Max BET(H2O)-area.
4.4. Compressive strength

Pore pressure (low)
Pore pressure (high) The results (from [42]) of the measured
Evaporation compressive strength are presented in Fig. 16. Due to
Temperature the differences in air content, the presented values
Strain are adjusted to an equal porosity of 4%, in
Initial crack
accordance with Eq. 2. All test results are
Min represented by a mean value based on two or more
0 5 10 15 20 mixtures.
Time (from mix) [hour] As can be observed, the compressive strength
Fig. 13. Development of pore pressure, evaporation, increased with BET(H2O)-area of the filler. And for
temperature and strain (normalized against maximum the mixtures with additional water, compensating for
values), for the SCC with limestone filler L40 (from [43]). the loss in flowability, the effect was the opposite.
80 The increased strength with particle surface area can
be attributed to the filler effect (denser packing and

2
Additional water
60
accelerated hydration due to nucleation). But as the
filler with the largest area (“L70”) also was the
coarsest, the increased strength can also be attributed
40
No compensation to the filler’s porosity increasing its absorption of
water and consequently reducing the effective
20 water/cement ratio. A change in BET(H2O)-area by
1000 m2/kg proved to correspond to ~0.15 MPa in
0 compressive strength for a SCC with 160 kg
0 2 000 4 000 6 000 8 000 limestone fillers (i.e. ~1 kPa/kg filler).
2
SBETH2O [m /kg] That the porosity (accessible to water absorption) is
incorporated in the BET-area is confirmed by the
Fig. 14. The limestone filler’s BET(H2O)-area and the
plastic shrinkage crack area, without and with extra water measured “autogenous” deformation on the mixtures
compensating for the differences in BET-area (“L40” as without cement (Fig. 12), where the mixture with
reference). “L70” generated the largest shrinkage (and swelling).
7
48 water, are in reverse ratio to the effect without

Comp. Strenght, 28d [MPa]
compensation.
No compensation o The mixtures where the cement was replaced
47 with limestone filler generated an “autogenous”
shrinkage of ~0.8 mm/m at 24 hours, counted
after an initial swelling up to 4 hours. The
46 magnitude of deformation (both swelling and
shrinkage) corresponded to the limestone filler’s
Additional water
BET(H2O)-area.
45
0 2000 4000 6000 8000
2
SBETH2O [m /kg] References
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SCC compressive strength (28d), both without and with the limestone in concrete – A new look, Build. Res. J. 43
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5. Conclusions Symp. on SCC, Stockholm, 1999, pp. 3-14.
[3] Rilem Technical Committee, Final report of Rilem
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Early Age Properties of Self-Compacting Concrete - Effects of Fine Aggregate and Limestone Filler - Thesis

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Early Age Properties of Self-Compacting Concrete - Effects of Fine Aggregate and Limestone Filler - Thesis

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Early age properties of

Department of Civil and Environmental Engineering

Early age properties of self-compacting

Department of Civil and Environmental Engineering

© Oskar Esping, 2007

Doktorsavhandlingar vid Chalmers tekniska högskola

Department of Civil and Environmental Engineering

II CHALMERS, Civil and Environmental Engineering

Key words: self-compacting concrete, rheology, autogenous deformation, plastic

CHALMERS, Civil and Environmental Engineering III

IV. Investigation of autogenous deformation in self-compacting concrete

V. Investigation of early age deformation in self-compacting concrete

VI. Effect of limestone filler BET(H2O)-area on the fresh and hardened

IV CHALMERS, Civil and Environmental Engineering

CHALMERS, Civil and Environmental Engineering V

APPENDIX B: CONCRETE DIGITAL DILATOMETER 99

APPENDIX C: CONCRETE CRACKING RING TEST 105

APPENDIX D: GLOSSARY 111

PAPER I: SLUMP FLOW VALUES VS. BINGHAM PARAMETERS

PAPER II: METHODS FOR CHARACTERISATION OF FILLERS AND

PAPER III: SCC FLOWABILITY: EFFECT OF CHANGES IN PARTICLE

PAPER IV: INVESTIGATION OF AUTOGENOUS DEFORMATION IN

PAPER V: INVESTIGATION OF EARLY AGE DEFORMATION IN SCC

PAPER VI: EFFECT OF LIMESTONE FILLER BET(H2O)-AREA ON THE

VI CHALMERS, Civil and Environmental Engineering

Göteborg, February 2007

CHALMERS, Civil and Environmental Engineering VII

Symbol Description Unit

VIII CHALMERS, Civil and Environmental Engineering

α angle [rad] or [º]

CHALMERS, Civil and Environmental Engineering IX

X CHALMERS, Civil and Environmental Engineering

CHALMERS, Civil and Environmental Engineering 1

1.2 Objective and limitations

2 CHALMERS, Civil and Environmental Engineering

1.3 Disposition of the thesis

1.4 Original features

CHALMERS, Civil and Environmental Engineering 3

4 CHALMERS, Civil and Environmental Engineering

Elasticity, G [Pa] Viscosity, η [Pa s]

CHALMERS, Civil and Environmental Engineering 5

6 CHALMERS, Civil and Environmental Engineering

2.2 Particle suspensions

CHALMERS, Civil and Environmental Engineering 7

2.2.1 Interparticle forces

Size [mm]: 30 1 0.1 2·10-4 10-6 10-7

8 CHALMERS, Civil and Environmental Engineering

function of interparticle distance (r), is illustrated in Figure 4. At a small separation

Cementitious materials are highly

suspension [4][18][19][28]. For cement-based Primary minimum

CHALMERS, Civil and Environmental Engineering 9

Interacting forces of composite particle systems

Size [mm]: 30 1 0.1 2·10-4 10-6 10-7

To increase a fresh cementitious material’s flowability, regarding the interparticle forces,

10 CHALMERS, Civil and Environmental Engineering

2.2.2 Flow characteristics

range of shear rates. Additionally, some σ0 3a)

1. Newtonian: Viscosity is constant with shear rate changes.

CHALMERS, Civil and Environmental Engineering 11

General non-Newtonian Fluids

2.2.3 Rheological models

12 CHALMERS, Civil and Environmental Engineering

Power-law (or Ostwald-de Waele)