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'Packing density of cementitious materials: Part 1-Measurement using a wet


packing method'

Article  in  Materials and Structures · May 2008


DOI: 10.1617/s11527-007-9274-5

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Packing density of cementitious materials: part 1 -


measurement using a wet packing method

H.H.C. Wong and A.K.H. Kwan*


Department of Civil Engineering,
The University of Hong Kong, Hong Kong, China

Abstract: The packing characteristics of the cementitious materials have great


influence on the performance of a concrete mix, but there is so far no generally
accepted method of measurement. Herein, a new method, called the wet packing
method, is developed. It mixes the cementitious materials with water and then
measures the apparent density and voids content of the resulting mixture at varying
water/cementitious materials ratio to characterise the packing behaviour of the
cementitious materials. Trial mixing and testing revealed that the mixing procedure is
crucial to the success of the test method. To ensure thorough mixing within a
reasonable time, a special mixing procedure is adopted. Using this method, the
packing characteristics of pure cement and blended cementitious materials under
different conditions have been measured. Based on the results so obtained, it is
advocated that the packing density and water demand should be measured directly
using a wet packing method rather than indirectly by any consistence test because the
water content at any preset consistence is not necessarily the same as the minimum
water content needed to fill up the voids. Some useful applications of the new method
are illustrated in Part 2 of this paper.

Keywords: Cementitious materials; Consistence; Packing density; Water demand

*
Corresponding author. Tel.: +852-2859-2647; fax: +852-2559-5337
Email addresses: hhcwong@graduate.hku.hk (H.H.C. Wong); khkwan@hku.hk (A.K.H. Kwan).
Mail address: Dept. of Civil Engg., The University of Hong Kong, Pokfulam Road, HKSAR, China.

1
1 Introduction

Early in the 1960s, Powers [1] had suggested that we could imagine a concrete
mixture to be composed of aggregate and cement paste. As conceived by Powers, the
cement paste has to first fill up the voids between aggregate particles and the “excess”
paste will then disperse the aggregate particles to produce a thin coating of paste
surrounding each aggregate particle for lubricating the concrete mix. In general, the
higher the packing density of the aggregate is, the smaller will be the volume of voids
to be filled and the larger will be the amount of excess paste for lubrication. Hence, a
higher packing density could at a fixed paste volume, lead to a better workability and
for a given workability, lead to a reduced paste demand. Following the geometric
similarity principle, the packing density of the cementitious materials should have a
similar effect; an increase in packing density of the cementitious materials should
improve the flowability of the paste and/or reduce the water demand.

In 1994, by maximising the packing density of the cementitious materials


using a packing model, DeLarrard and Sedran [2] had reduced the water/cementitious
materials (W/CM) ratio to as low as 0.14 by weight and thereby achieved concrete
strengths of 165 to 236 MPa. One year later in 1995, by maximising the packing of all
granular materials in the concrete mix using the same packing model and also
applying other advanced production techniques, Richard and Cheyrezy [3] had
achieved concrete strengths in the order of 200 to 800 MPa. Besides reducing the
W/CM ratio to increase strength, such strategy may also be employed without
reducing the W/CM ratio to increase workability. In 1996, Sedran et al. [4] had
applied the packing theory to the design of self-consolidating concrete and based on
the successful outcome concluded that the performance optimisation of concrete is
mainly a matter of improving the packing density of its granular skeleton.

Subsequently, Lange et al. [5] showed that improving the packing density of
the cementitious materials by blending ordinary cement with a finer blast furnace slag
based cement could significantly reduce the water demand and enhance the overall
properties of the mortar produced. More recently, Jones et al. [6] studied both
theoretically and experimentally the effectiveness of different types of fillers in

2
minimizing the voids content of the cementitious materials. It was found that the
effectiveness of the fillers is dependent on whether a superplasticiser is present and
that in general finer fillers are more effective especially when a superplasticiser has
been added to disperse the particles and reduce agglomeration.

The concept of particle packing is useful also in other fields of engineering [7]
and throughout the years has advanced to a high degree of sophistication. However,
although a number of theoretical packing models have been developed, accurate
measurement of the packing density of very fine materials, such as the cementitious
materials used in concrete, has remained a difficult task. The packing density of
cementitious materials has been measured in terms of the water demand arbitrarily
taken as the water content required for a certain consistence, but such water content is
not really the same as that needed for filling up the voids. Moreover, since there may
be air entrapped, the packing density evaluated just from the water demand may not
be accurate. A review of the existing methods of packing density measurement is
given in the next section. Apart from the review, the present study aims to develop a
new method that could overcome the afore-mentioned problems.

2 Existing methods of packing density measurement

The existing methods may be broadly classified into direct methods that
determine the packing density directly from the bulk density of the packed particles
and indirect methods that determine the packing density indirectly by consistence
tests. They do not yield the same results and in fact are measuring different
parameters. Details of these methods are reviewed in the following.

2.1 Direct methods

The British Standard BS 812: Part 2: 1995 [8] has specified a dry packing
method for measuring the bulk density of aggregate, from which the voids content and
packing density may be determined. There are two versions, one for coarse aggregate
under uncompacted or compacted conditions and the other for filler under compacted

3
condition. This methodology is widely used also in the field of powder technology.
However, Svarovsky [9] warned that the bulk density of a powder is very much
dependent on the state of compaction and it must be explicitly stated whether the bulk
density measured is the aerated, poured, tapped or compacted bulk density. Moreover,
the exact treatment to be applied to the powder sample has to be standardized as this
could affect the test results and their interpretation.

Another major problem with dry packing is that with decreasing particle size,
the adhesion phenomena arising from Van der Waals and electrostatic forces between
the particles become more and more important, causing agglomeration that increases
the voids content [10]. According to Pietsch [11], the critical size is approximately
100 µm. At a smaller size, the ratio of inter-particle force to gravity is greater than
unity and agglomeration is likely to be significant. That is why the packing behaviour
of fine particles is different from that of coarse particles. In general, the dry packing
method would tend to overestimate the voids content and underestimate the packing
density of fine particles.

The authors have actually applied the dry packing method to cementitious
materials and found that the measured packing density results were unreasonably low
compared to those obtained using the proposed wet packing method (the comparison
will be presented later in this paper). Serious agglomeration was observed during dry
packing and thus unless this problem has been completely resolved, the dry packing
method is not suitable for measuring the packing density of cementitious materials, of
which the grain sizes are generally smaller than 100 µm.

2.2 Indirect methods

Virtually all the indirect methods measure the voids content of a sample of
cementitious materials in terms of the water demand taken as the minimum water
content needed for the cementitious materials to form a paste and achieve a certain
consistence. Such practice is based on the faith that for any cementitious materials,
there is a minimum water content for the formation of a paste and at this minimum
water content, the voids content is also minimum. In many cases, it is further assumed

4
that there is no air entrapped in the paste and so the volume occupied by this
minimum water content may be taken as the minimum voids content of the
cementitious materials from which the packing density may be evaluated.

The simplest way of measuring the water demand is to follow the standard
consistence test, as specified in BS EN 196: Part 3: 1995 [12] or other recognized
standards. In the standard consistence test, the Vicat apparatus is used and the
consistence of the paste is measured in terms of the penetration depth of the plunger.
To further simplify the test, the change of penetration depth with water content is not
fully explored and only the water content at which the penetration depth is equal to
34±1 mm is arbitrarily taken as the water content for standard consistence. It is
assumed that this water content for standard consistence is the same as the water
demand of the cementitious materials.

Different researchers measured the water demand in different ways. Lange et


al. [5] used the standard consistence test method without adding any plasticiser or
superplasticiser. Jones et al. [6] carried out standard consistence tests both with and
without superplasticiser added and obtained for each mixture of cementitious
materials, two water demand values, one without any superplasticiser added and the
other with a certain dosage of superplasticiser added. Their results revealed that the
water demand was dependent on the presence of superplasticiser and that the water
demand measured with a superplasticiser added generally agreed better with the
theoretical packing model.

Whilst adopting the standard consistence test as specified in BS EN 196 for


determining the water demand, Dewar [13] suggested to allow for an air content of
say 1.5% in the paste when evaluating the voids content of the cementitious materials.
Bigas and Gallias [14] also followed the standard consistence test method of BS EN
196 but instead of assuming an arbitrary value of air content in the paste actually
measured the apparent density of the paste to allow for the presence of air. Since the
effect of the air content on the bulk volume of the paste has been taken into account,
their method of determining the voids content and packing density should be more
accurate than the other methods.

5
On the other hand, DeLarrard [15] suggested to measure the water demand
without going through the standard consistence test. He took the water demand as the
minimum water content for producing a thick paste and assumed that any water
content lower than this minimum will only yield a humid soil. He also advised that if
any admixture with plasticising properties is to be used in the concrete mix, then the
water demand should be measured with the same dosage of admixture added. In his
method, the water demand is simply measured by mixing the cementitious materials
with different amounts of water and finding the water content that gives a consistence
intermediate between a humid soil and a thick paste. Without any mechanical and
quantitative measure, the consistence of the paste has to be determined by manual
judgment. After the water demand is measured, the voids content and packing density
are evaluated with the air content in the paste assumed to be zero.

Experience with the water demand tests indicated that the mixing process
during preparation of the paste is more efficient for compacting the fine particles than
the normal combination of vibration and pressure applied during dry packing and that
as a result the packing density achieved in a paste is generally higher than that in a dry
packed form. Moreover, with the addition of a superplasticiser, which disperses the
particles and reduces agglomeration, the packing density would be even higher.
Overall, the wet mixing method should yield higher and more reliable packing density
results than the dry packing method.

However, the indirect methods are not without problems. Firstly, the water
demand has been taken as the water content at a certain arbitrarily chosen level of
consistence but there is so far no evidence to prove that at such consistence level, the
water content is just enough to fill up the voids. Secondly, as pointed out by Iveson et
al. [16], liquid-bound granules can exist in different states of liquid saturation. In the
pendular state, the particles are held together by liquid bridges at their contact points.
In the capillary state, the granules are saturated with surface liquid drawn back into
the voids under capillary action. Between these, there is a transitional funicular state
in which the voids are not fully saturated. Since the transition from pendular to
capillary state (in the present context, this corresponds to transition from a humid soil
to a thick paste) is gradual and not clear-cut, it is difficult to judge whether the

6
capillary state, at which the liquid is just enough to fill up the voids, has been reached.
Thirdly, the air content in the paste is often neglected, resulting in underestimation of
the voids content and overestimation of the packing density.

Having considered the above, it may be concluded that the water content at a
certain fixed consistence is not a good measure of the voids content of cementitious
materials. It is an important parameter in its own right but should not be used to
evaluate the packing performance of cementitious materials. To measure the voids
content and packing density of cementitious materials, a new method not relying on
consistence measurement is needed, as presented in the next section.

3 Proposed method of packing density measurement

3.1 Definitions of terms

At the outset, the terms used to describe the packing behaviour of cementitious
materials are defined to avoid misunderstanding, as different researchers are using
different terms with different definitions causing a lot of confusion.

In a bulk volume of granular material, the voids are the interstitial space
between the solid particles. The voids content (denoted by ε) is defined as the ratio of
the volume of voids to the bulk volume of the granular material, while the voids ratio
(denoted by u) is defined as the ratio of the volume of voids to the solid volume of the
granular material. They are inter-related by the following equation:

u
ε = (1)
1+ u

The voids may be filled with water or air or both. The water content (denoted by εw) is
defined as the ratio of the volume of water to the bulk volume of the granular material
and the water ratio (denoted by uw) is defined as the ratio of the volume of water to
the solid volume of the granular material. On the other hand, the air content (denoted

7
by εa) is defined as the ratio of the volume of air to the bulk volume of the granular
material and the air ratio (denoted by ua) is defined as the ratio of the volume of air to
the solid volume of the granular material. They are related to each other by:

uw
εw = (2)
1 + u w + ua
ua
εa = (3)
1 + u w + ua

The solid concentration of the granular material (denoted by φ) is defined as the ratio
of the solid volume of the granular material to the bulk volume of the granular
material. It may be evaluated using the following equation:

1
φ = 1− ε = (4)
1+ u

3.2 Development of the proposed wet packing method

The proposed method has the following characteristics:


(1) It is a wet packing method. In other words, it mixes the given cementitious
materials with water to form water-bound granules, from which the voids
content and solid concentration are measured.
(2) It does not rely on any consistence observation or measurement. Instead, the
W/CM ratio is varied and the resulting voids content and solid concentration
are determined by measuring the apparent density of the granules.
(3) Since the voids content and solid concentration are evaluated from the
apparent density, the air content is automatically taken into account. In fact,
the air content may also be evaluated for analysis.
(4) The mixing procedure, which has been found during trials to be crucial to the
success of the method, is specially designed. Conventional mixing procedure
requires a long time to achieve thorough mixing when the water content is low
and/or very fine materials are dealt with. The mixing procedure adopted herein
would allow thorough mixing to be achieved within a much shorter time.

8
During the development of the proposed method, several mixing procedures
had been tried. At the beginning, the mixing procedure in BS EN 196 was followed.
As per BS EN 196, the cement and water were added in a single batch into the mixing
bowl and then the mixture was stirred for 3 minutes. However, it was found that this
mixing procedure worked well only when the water ratio was higher than 0.6. At a
lower water ratio, the mixing time of 3 minutes was found to be insufficient. With the
mixing time extended, it was revealed that the consistence would improve with time
up to a certain limit. Very often, the mixture remained for a long time in the form of
discrete water-bound granules with dry surfaces and it was only when the mixing time
was considerably prolonged then the granules eventually coalesced together to form a
thick paste. When the cement was blended with very fine materials such as condensed
silica fume, the required mixing time was even longer and could be as long as 60
minutes. Hand mixing had also been tried but the situation was no better.

As explained by Iveson et al. [16], when mixing a powder and water together,
the following processes take place: “wetting and nucleation”, and “consolidation and
growth”. During wetting and nucleation, the water distribution is initially very poor
and only discrete water-bound granules are formed. The pores inside the granules are
saturated but the surfaces remain dry. Later on, consolidation and growth occur, as the
“excess” water in the mixture, if any, wets the surfaces of the granules or the water
inside the granules are squeezed to the surfaces to facilitate coalescence of the
granules together. When the water content is high such that there is excess water to
wet the surfaces of the granules, the consolidation and growth process is quite fast
resulting in the formation of a slurry or paste within minutes. However, when the
water content is low, the coalescence will be dependent mainly on the water-
squeezing process, which is in general very slow [17], leading to a much longer
mixing time required for forming a paste. The reason why the mixing of finer
materials and water together takes a longer time is that the squeezing of water through
finer pores requires more energy and time.

To overcome the above problem, the authors have adopted the strategy of
avoiding the slow water-squeezing process by keeping the mixture saturated most of
the time. When under-saturated, the granules are not easy to be deformed or

9
intermixed with each other because of the capillary forces that give them strength
[16]. However, when saturated or over-saturated, such strength is lost [18] and
thorough mixing can be achieved quite easily and quickly. To keep the mixture
saturated as far as possible, the powder is added bit by bit instead of in a single batch
to the water during mixing. By so doing, at the beginning, a slurry is formed. Then, as
more powder is added, the slurry is turned into an over-saturated paste. When further
powder is added by spreading it evenly to the paste, the powder is very soon wetted
and intermixed with the paste. As the degree of saturation gradually drops, the mixing
becomes more difficult but the total time needed is still much shorter than that
required when the conventional mixing method of adding all the powder in a single
batch is used. The authors have tried different ways of adding the powder to the water
and arrived at the conclusion that the best way is to first add one half of the powder to
the water to form a slurry and then add the remaining half in four equal portions. The
testing procedure so developed is presented in the following.

3.3 Testing procedures

The packing density is not the same as the solid concentration, which varies
with the W/CM ratio. When the W/CM ratio is relatively high, the solid particles are
dispersed in the water, resulting in a solid concentration that decreases as the W/CM
ratio increases. On the other hand, when the W/CM ratio is relatively low, the water
content is not sufficient to thoroughly mix with the solid particles to form a paste,
resulting in a solid concentration that decreases as the W/CM ratio decreases. There is
an optimum W/CM ratio at which maximum solid concentration is achieved. The
maximum solid concentration, which occurs when the particles are tightly packed
against each other, is taken as the packing density of the granular material. Therefore,
to determine the packing density, it is necessary to carry out the wet packing tests at
different W/CM ratios over a range wide enough to cover the optimum W/CM ratio.
With no previous test data to help decide on an appropriate range, it is suggested to
start at a W/CM ratio by volume of 1.0 for the first test and then successively reduce
the W/CM ratio for further tests until the solid concentration has reached a maximum
value and then dropped. It should be noted that the W/CM ratio by volume is the same
as the water ratio uw. All W/CM ratios referred to hereafter are by volume.

10
The procedures of the proposed test method are described below (note: all
equipment used are the same as those specified in BS EN 196: Parts 1-3):
(1) Set the W/CM ratio at which the wet packing test is to be carried out. Weigh
the required quantities of water, cementitious materials and superplasticiser (if
any) and dose each ingredient into a separate container.
(2) If the cementitious materials consist of several different materials blended
together, pre-mix the materials in dry for 2 minutes.
(3) Add all the water into the mixing bowl.
(4) Add half of the cementitious materials and superplasticiser into the mixing
bowl and run the mixer at low speed for 3 minutes.
(5) Divide the remaining cementitious materials and superplasticiser into four
equal portions. Add the remaining cementitious materials and superplasticiser
into the mixing bowl one portion at a time and after each addition run the
mixer at low speed for 3 minutes.
(6) Transfer the mixture to a cylindrical mould and fill the mould to excess. If
compaction is to be applied, apply compaction at this stage. Remove the
excess with a straight edge and weigh the amount of paste in the mould.
(7) If so desired, the consistence of the paste may be measured at this stage using
the Vicat apparatus. It should be noted however that the consistence results
will not be used to calculate the packing density.
(8) Repeat steps (1) to (7) at successively lower W/CM ratios until the maximum
solid concentration, i.e. the packing density, has been found.

From the test results so obtained, the voids ratio, air ratio and solid
concentration may be determined as depicted in the following. Let the mass and
volume of paste in the mould be M and V, respectively (the mould used by the authors
is of 62 mm diameter × 60 mm height but any other mould of similar size may also be
used). If the cementitious materials consist of several different materials denoted by
α, β, γ and so forth, the solid volume of the cementitious materials Vc and the volume
of the water Vw in the mould may be worked out from the following equations:

M
Vc = (5)
ρ w u w + ρ α Rα + ρ β Rβ + ρ γ Rγ

11
Vw = uw Vc (6)

in which ρw is the density of water, ρα, ρβ and ργ are the solid densities of α, β and γ,
and Rα, Rβ and Rγ are the volumetric ratios of α, β and γ to the total cementitious
materials. Having obtained Vc and Vw, the voids ratio u, air ratio ua and solid
concentration φ may be determined as:

u = (V − Vc ) Vc (7)

ua = (V − Vc − Vw ) Vc (8)

φ = Vc V (9)

4 Results and discussions

4.1 Materials

Three types of cementitious materials, namely, ordinary Portland cement


(OPC), pulverised fuel ash (PFA) and condensed silica fume (CSF), were used in the
experiments. The OPC was a commonly used cement, which had been tested to
comply with BS 12: 1996. The PFA was a classified ash, which had been tested to
comply with BS 3892: Part 1: 1982. The CSF was imported from Norway and
according to the supplier, it complied with ASTM C 1240-03. Their particle densities
had been measured in accordance with BS 812: Part 2: 1995 as 3110 kg/m3, 2329
kg/m3 and 2202 kg/m3, respectively. The particle size distributions of the OPC and
PFA had been measured by the laser diffraction method, as depicted in Fig. 1. The
particle size distribution of the CSF had not been measured but according to the
supplier, the mean particle size of the CSF was about 0.15 µm.

Where required, a superplasticiser (SP) was added during the tests. The SP
used was a polycarboxylate-based admixture. It has a solid mass content of 20% and a
relative density of 1.03. According to the supplier, the normal dosage of this SP,
measured in terms of liquid mass, should be 0.5 to 3.0 % by mass of cement, but a

12
higher dosage may also be used if proven to be satisfactory by trial mixing. As the
OPC, PFA and CSF have different densities and it is the solid volume rather than the
mass that is more important, the SP dosage is expressed in terms of the liquid mass of
SP per unit solid volume of the cementitious material. The standard dosage of SP
(denoted by 1×SP) used in this study was 93.3 kg/m3 (corresponding to the upper limit
of the normal dosage recommended by the supplier). Double dosage (denoted by
2×SP) and triple dosage (denoted by 3×SP) were also used in some of the tests to
investigate the effects of SP dosage.

4.2 Presentation and interpretation of test results

During the tests, the apparent density (for voids ratio and solid concentration
evaluation) and the penetration depth (for consistence evaluation) of the paste were
measured. The results are presented in Fig. 2 by plotting the voids ratio and
penetration depth against the W/CM ratio. In the voids ratio graph, a straight line
entitled “εa = 0” is drawn. This line is an equality line because εa = 0 when u = uw.
The actual air ratio ua (given by ua = u – uw) may be obtained as the vertical distance
between the voids ratio curve and the “εa = 0” line. Several important parameters can
be obtained from the curves plotted. From the lowest point of the voids ratio curve,
the minimum voids ratio umin and the basic water ratio uwb (the water ratio yielding
minimum voids ratio) can be determined. From the penetration depth curve, the water
ratio at standard consistence uws can be obtained. For many years, umin, uwb and uws
have been treated by many researchers as equivalent. However, it will be shown from
the test results that they are not the same and should not be mixed up.

4.3 Packing of OPC

The test results for OPC with no SP or 1×SP added are presented in Fig. 3.
From the results for OPC with no SP added, it can be seen that at high W/CM ratio,
the voids ratio curve followed closely the “εa = 0” line indicating that the air content
was then negligibly small. As the W/CM ratio was reduced to lower than 0.900, the
voids ratio curve started deviating from the “εa = 0” line because the air ratio had
began to increase. When the W/CM ratio reached 0.846, the air ratio increased to

13
around 2%. Further reduction of the W/CM ratio to the basic water ratio of 0.750
yielded a minimum voids ratio of 0.831 and a maximum solid concentration of 0.546.
At a W/CM ratio lower than the basic water ratio, no paste could be formed and as a
result the voids ratio became very large. On the other hand, the penetration depth
results revealed that the water ratio at standard consistence was 0.958.

The corresponding results for OPC with 1×SP added are similar in general
trend to those for OPC with no SP added. The major differences are that with SP
added, the basic water ratio changed from 0.750 to 0.525, the minimum voids ratio
decreased from 0.831 to 0.607, the maximum solid concentration increased from
0.546 to 0.622, while the water ratio at standard consistence decreased from 0.958 to
0.554. These changes demonstrated the effectiveness of the SP in dispersing the
cement particles. However, it should be noted that regardless of whether SP has been
added, the basic water ratio is substantially lower than the minimum voids ratio. In
fact, at the basic water ratio, the air content is quite large and the water content is not
sufficient to fill up the voids. Furthermore, the water ratio at standard consistence is
quite different from the basic water ratio or the minimum voids ratio. In other words,
the water ratio at standard consistence, which has long been used to determine the
water demand, is not really the same as the minimum water ratio at which the water
content is just sufficient to fill up the voids.

4.4 Effects of SP dosage

Fig. 4 shows the test results for OPC with different dosages of SP added. It
can be seen from these results that when the dosage was increased from 1×SP to
2×SP, the basic water ratio changed from 0.525 to 0.480, the minimum voids ratio
decreased from 0.607 to 0.567 and the maximum solid concentration (i.e. the packing
density) increased from 0.622 to 0.638, but when the dosage was further increased to
3×SP, the packing behaviour of the paste remained more or less the same. From these
values, it may be worked out that the packing density increased only by 3% when the
dosage of SP was doubled or even tripled. Hence, the addition of a higher dosage of
SP than the standard dosage (1×SP) provided little further improvement in packing
performance and the standard dosage was already quite close to the saturation dosage.

14
It can also be seen from these results that regardless of the SP dosage, the basic water
ratio is always substantially lower than the minimum voids ratio whereas the water
ratio at standard consistence is neither equal to the basic water ratio nor equal to the
minimum voids ratio.

4.5 Effects of compaction

In order to investigate the effects of compaction, a series of tests was carried


out with each cement-water mixture compacted by vibration before its apparent
density and penetration depth were measured. The compaction was applied by filling
the cement-water mixture into the mould of the Vicat apparatus in four equal layers
and vibrating the mould after adding each layer. The vibration was carried out by
mounting the mould onto the vibration machine, which was normally used for
compacting mortar cubes in compliance with BS 4550: Part 3: 1978 [19], and running
the motor of the machine each time for exactly 30 seconds.

The test results so obtained for OPC with 1×SP added and with or without
compaction applied are compared in Fig. 5. At W/CM ratio higher than 0.700, the
effect of compaction was insignificant because even without compaction the paste
was saturated with little air inside. When the W/CM ratio was decreased to around
0.600 or lower, the compaction started to take effect as more air tended to be
entrapped in the paste during mixing. After the compaction was applied, the apparent
density of the paste was increased and the voids ratio decreased. It had also been
observed that at W/CM ratio lower than 0.500, the cement-water mixture appeared
more like a non-cohesive soil before compaction and was turned into a cohesive paste
after compaction. At the end, the compaction demonstrated its effectiveness by
reducing the basic water ratio from 0.525 to 0.450 and the minimum voids ratio from
0.607 to 0.508, and increasing the packing density from 0.622 to 0.663.

From Fig. 5, it can also be seen that along with the reduction in voids ratio,
there was also a reduction in penetration depth after compaction. This was due to
densification of the solid particles, which increased the penetration resistance. As a
result, the water ratio at standard consistence was increased from 0.554 to 0.589.

15
4.6 Effects of blending with PFA or CSF

To demonstrate the usefulness of the new test method, another series of tests
was carried out to evaluate the effects of blending OPC with PFA or CSF. Two
cementitious materials mixtures have been prepared, one containing 75% OPC plus
25% PFA and the other containing 85% OPC plus 15% CSF (all percentages are by
volume). The SP dosage was fixed at 1×SP, while the W/CM ratio by volume was
varied from 0.800 to lower than the basic water ratio. The test results so obtained are
compared to those for pure OPC with the same SP dosage in Fig. 6.

It is evident from the comparison that blending OPC with either PFA or CSF
could at all W/CM ratios significantly decrease the voids ratio. With 25% of the OPC
replaced by an equal volume of PFA, the minimum voids ratio decreased from 0.607
to 0.558 (8% decrease) and the packing density increased from 0.622 to 0.642 (3%
increase). On the other hand, with 15% of the OPC replaced by an equal volume of
CSF, the minimum voids ratio decreased from 0.607 to 0.422 (30% decrease) and the
packing density increased from 0.622 to 0.703 (13% increase). The improvement in
packing density may be attributed partly to the filling effect of PFA and CSF, which
reduces the voids volume by filling up the gaps between the OPC particles, and partly
to the spherical shape of the PFA and CSF particles, which allows better packing to be
achieved [20,21]. CSF is more effective than PFA in improving the packing density
because of the greater filling effect arising from its ultra-high fineness.

However, the improvement in packing density would not be apparent if the


dry packing method was used to determine the packing density. The packing densities
of pure OPC and the (75% OPC + 25% PFA) and (85% OPC + 15% CSF) mixtures
have also been measured by the dry packing method. During dry packing, the
specified proportions of OPC, PFA and CSF were pre-mixed and then filled into a 45
mm diameter × 45 mm height cylindrical mould in five successive layers, each tapped
40 times by a 10 mm diameter rod. After tapping, the mixture inside the mould was
weighed for determination of packing density. The results so obtained are compared
to those by the proposed wet packing method in Table 1, from which it can be seen
that the packing densities measured by the dry packing method are far too low and

16
that the increase in packing density by blending OPC with CSF would not be revealed
by the dry packing method. Aggregation, coating and caking, which are signs of
strong inter-particle force and agglomeration [11], were observed during dry packing.
It may thus be inferred that agglomeration was the main reason for the low packing
densities obtained by the dry packing method.

4.7 Significance of umin, uwb and uws

Table 2 summaries the various values of umin, uwb and uws obtained in the
present study. It is evident that these three ratios are not the same. The minimum
voids ratio umin is of importance because it may be used to evaluate the packing
density of the given mixture of cementitious materials. The basic water ratio uwb is the
optimum W/CM ratio at which the voids ratio is minimum. Since the corresponding
air ratio ua is not equal to zero, the basic water ratio must not be taken as the
minimum water ratio at which the water is just sufficient to fill up the voids.

From Figs. 3 to 6, it can be seen that, in general, at a W/CM ratio lower than
the minimum voids ratio umin, there would be a significant amount of air voids inside
the paste but at a W/CM ratio just slightly higher than the minimum voids ratio umin,
the amount of air voids inside the paste would become insignificant (as revealed by
the variation of the air ratio ua with the W/CM ratio). Hence, the minimum voids ratio
umin may also be taken as the minimum water ratio at which the water content is just
sufficient to fill up the voids. In fact, the minimum voids ratio umin should be regarded
as the absolute minimum W/CM ratio to be used in concrete mix design because a
W/CM ratio lower than this would lead to an unacceptably large air content.

The water ratio at standard consistence uws has long been used to determine the
water demand. However, it is quite different from both the basic water ratio and the
minimum voids ratio. Furthermore, in the case of OPC with 1×SP added, the
compaction applied reduced the basic water ratio and the minimum voids ratio but at
the same time increased the water ratio at standard consistence. Hence, the water ratio
at standard consistence cannot be a physically true measure of the minimum voids
ratio or the minimum water ratio.

17
5 Conclusions

The existing methods of measuring the packing density of cementitious


materials have been reviewed and their problems identified. It was found that the dry
packing methods are afflicted by agglomeration while the common practice in the wet
mixing methods of determining the water demand as the water content at a certain
preset consistence is not really appropriate. To resolve these and other problems, a
new method, which is a wet packing method not relying on consistence measurement,
has been developed. It mixes the cementitious materials with water at different
water/cementitious materials ratios, determines the voids ratio and solid concentration
of each resulting mixture by measuring its apparent density rather than consistence,
and takes the maximum solid concentration achieved as the packing density of the
cementitious materials. A special mixing procedure of adding the cementitious
materials bit by bit to the water so as to keep the mixture saturated as far as possible is
adopted to ensure thorough mixing within a reasonable time.

The new method has been applied to study the basic packing behaviour of a
common cement, the effects of superplasticiser dosage, the effects of compaction and
the effects of blending cement with pulverised fuel ash or condensed silica fume.
From the test results, the basic water ratios, the minimum voids ratios and the water
ratios at standard consistence of the various cementitious materials under different
conditions have been obtained. These revealed that the basic water ratio, the minimum
voids ratio and the water ratio at standard consistence are not the same. Generally, the
basic water ratio is substantially lower than the minimum voids ratio. This is because
at the basic water ratio, there is always some air in the paste (i.e. the paste is not
saturated). More importantly, the minimum voids ratio may be taken as the minimum
water ratio at which the water is just sufficient to fill up the voids. Lastly, since there
is no logical relation between the water ratio at standard consistence and the minimum
voids ratio, the traditional practice of determining the water demand from the water
ratio at standard consistence is incorrect and should be abandoned.

The wet packing tests conducted herein have shown quantitatively in a correct
manner for the first time (to the best of the authors’ knowledge) the actual increase in

18
packing density that could be achieved by blending cement with either pulverised fuel
ash or condensed silica fume. Further studies on triple blending of cement, pulverised
fuel ash and condensed silica fume, and on how the flow of the cement paste could be
improved by maximising the packing density of the cementitious materials have also
been carried out, as reported in Part 2 of the paper.

Acknowledgement

The work described in this paper was fully supported by a grant from the
Research Grants Council of the Hong Kong Special Administrative Region, China
(Project No. HKU 7139/05E).

References

[1] Powers TC (1968) The properties of fresh concrete. John Wiley & Sons, New
York
[2] DeLarrard F, Sedran T (1994) Optimization of ultra-high-performance concrete
by the use of a packing model. Cem Concr Res 24(6):997-1009
[3] Richard P, Cheyrezy M (1995) Composition of reactive powder concretes. Cem
Concr Res 25(7):1501-1511
[4] Sedran T, DeLarrard F, Hourst F, Contamines C (1996) Mix design of self-
compacting concrete. In: Bartos PJM et al (eds) Proceedings of the
international RILEM conference on production methods and workability of
concrete, Paisley, Scotland, pp 439-450
[5] Lange F, Mörtel H, Rudert V (1997) Dense packing of cement pastes and
resulting consequences on mortar properties. Cem Concr Res 27(10):1481-
1488
[6] Jones MR, Zheng L, Newlands MD (2003) Estimation of the filler content
required to minimize voids ratio in concrete. Mag Concr Res 55(2):193-202
[7] Reed JS (1995) Principles of ceramics processing. John Wiley & Sons, New
York

19
[8] British Standards Institution (1995) BS 812 Testing of aggregates part 2:
method of determination of density. BSI, London
[9] Svarovsky L (1987) Powder testing guide: methods of measuring the physical
properties of bulk powders. Elsevier Applied Science Publishers Ltd, England
[10] Yu AB, Bridgwater J, Burbidge A (1997) On the modeling of the packing of
fine particles. Powder Technol 92(3):185-194
[11] Pietsch W (1997) Size enlargement by agglomeration. In: Fayed ME, Otten L
(eds) Handbook of powder science and technology, 2nd edn. Chapman & Hall,
New York
[12] British Standards Institution (1995) BS EN 196 Methods of testing cement part
3: determination of setting time and soundness. BSI, London
[13] Dewar JD (1999) Computer modelling of concrete mixtures. E & FN Spon,
London
[14] Bigas JP, Gallias JL (2002) Effect of fine mineral additions on granular
packing of cement mixtures. Mag Concr Res 54(3):155-164
[15] DeLarrard F (1999) Concrete mixture proportioning: a scientific approach. E &
FN Spon, London
[16] Iveson SM, Litster JD, Hapgood K, Ennis BJ (2001) Nucleation, growth and
breakage phenomena in agitated wet granulation processes: a review. Powder
Technol 117(1-2):3-39
[17] Schaafsma SH, Vonk P, Segers P, Kossen NWF (1998) Description of
agglomerate growth. Powder Technol 97(3):189-190
[18] Iveson SM, Wauters PAL, Forrest S, Lister JD, Meesters GMH, Scarlett B
(2001) Growth regime map for liquid-bound granules: further development and
experimental validation. Powder Technol 117(1-2):83-97
[19] British Standards Institution (1978) BS 4550 Methods of testing cement part 3:
physical tests. BSI, London
[20] Zou RP, Yu AB (1996) Evaluation of the packing characteristics of mono-sized
non-spherical particles. Powder Technol 88(1):71-79
[21] Kwan AKH, Mora CF (2001) Effects of various shape parameters on packing
of aggregate particles. Mag Concr Res 53(2):91-100

20
Tables

Table 1 Packing densities measured by dry and wet packing methods


Wet packing method
Dry packing method
Mix proportions (with 1×SP added but no
(with tapping applied)
compaction applied)
Pure OPC 0.514 0.622
75% OPC+25% PFA 0.539 0.642
85% OPC+15% CSF 0.480 0.703

Table 2 Summary of voids ratio and water ratio results

Cementitious mixture umin uwb uws

OPC (no SP) 0.831 0.750 0.958


OPC (1×SP) 0.607 0.525 0.554
OPC (2×SP) 0.567 0.480 0.505
OPC (3×SP) 0.574 0.480 0.483
OPC (1×SP and compaction) 0.508 0.450 0.589
75% OPC+25% PFA (1×SP) 0.558 0.458 0.473
85% OPC+15% CSF (1×SP) 0.422 0.358 0.401

21
Figures

Figure 1 Particle size distributions of OPC and PFA

Figure 2 Presentation and interpretation of test results

Figure 3 Test results for OPC with no SP or 1×SP added

Figure 4 Test results for OPC with different dosages of SP added

Figure 5 Test results for OPC with or without compaction applied

Figure 6 Test results for blended cementitious materials

22
100
.

80
Cumulative volume (%)

60
PFA

40 OPC

20

0
1 10 100
Particle size (µm)

Figure 1 Particle size distributions of OPC and PFA

23
.

εa= 0
Voids ratio

u min ua

uw

u wb
W/CM ratio by volume

34 mm
.
Penetration depth (mm)

u ws
W/CM ratio by volume

Figure 2 Presentation and interpretation of test results

24
1.2

1.0
.
Voids ratio

0.8 εa =0

0.6
OPC (no SP)
OPC (1xSP)
0.4
0.4 0.6 0.8 1.0 1.2
W/CM ratio by volume
40
.

30
Penetration depth (mm)

20

10
OPC (no SP)
OPC (1xSP)
0
0.4 0.6 0.8 1.0 1.2
W/CM ratio by volume

Figure 3 Test results for OPC with no SP or 1×SP added

25
0.8

0.7
εa =0
.
Voids ratio

0.6

0.5
OPC (1xSP)
OPC (2xSP)
OPC (3xSP)
0.4
0.4 0.5 0.6 0.7 0.8
W/CM ratio by volume
40
.

30
Penetration depth (mm)

20

10
OPC (1xSP)
OPC (2xSP)
OPC (3xSP)
0
0.4 0.5 0.6 0.7 0.8
W/CM ratio by volume

Figure 4 Test results for OPC with different dosages of SP added

26
0.8

0.7
.

εa =0
Voids ratio

0.6

0.5

OPC (no compaction)


OPC (compaction)
0.4
0.4 0.5 0.6 0.7 0.8
W/CM ratio by volume
40
.

30
Penetration depth (mm)

20

10

OPC (no compaction)


OPC (compaction)
0
0.4 0.5 0.6 0.7 0.8
W/CM ratio by volume

Figure 5 Test results for OPC with or without compaction applied

27
0.8

0.7
.

0.6
Voids ratio

εa =0
0.5

0.4 Pure OPC


75%OPC+25%PFA
85%OPC+15%CSF
0.3
0.3 0.4 0.5 0.6 0.7 0.8
W/CM ratio by volume
40
.

30
Penetration depth (mm)

20

10
Pure OPC
75%OPC+25%PFA
85%OPC+15%CSF
0
0.3 0.4 0.5 0.6 0.7 0.8
W/CM ratio by volume

Figure 6 Test results for blended cementitious materials

28

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