Materials and Structures (2017) 50:235

https://doi.org/10.1617/s11527-017-1103-x

ORIGINAL ARTICLE

Reproducible mini-slump test procedure for measuring

the yield stress of cementitious pastes
Zhijun Tan . Susan A. Bernal . John L. Provis

Received: 15 March 2017 / Accepted: 16 October 2017 / Published online: 19 October 2017
Ó The Author(s) 2017. This article is an open access publication

Abstract The mini-slump test is a fast, inexpensive Keywords Mini-slump test  Yield stress 
and widely adopted method for evaluating the work- Workability  Viscometry  Alkali-activated cements
ability of fresh cementitious pastes. However, this
method lacks a standardised procedure for its exper-
imental implementation, which is crucial to guarantee
reproducibility and reliability of the test results. This 1 Introduction
study investigates and proposes a guideline procedure
for mini-slump testing, focusing on the influence of For a given cementitious material in the fresh state, the
key experimental (mixing and testing) parameters on yield stress (denoted sy) and the plastic viscosity are
the statistical performance of the results. The impor- generally considered the two most important rheolog-
tance of preparation of always testing at the same time ical properties in terms of workability. The yield stress
after mixing, testing each batch once rather than of a cementitious material denotes the critical stress
conducting multiple tests on a single batch of material, value at which the material will begin to, or cease to,
is highlighted. A set of alkali-activated fly ash-slag flow, which is an important property when placing the
pastes, spanning from 1 to 75 Pa yield stresses, were material. Concrete with high yield stress is difficult to
used to validate the test method, by comparison of pump, and the associated poor workability results in
calculated yield stresses with the results obtained quality control issues in the hardened material [1].
using a conventional vane viscometer. The proposed Therefore, the determination of the yield stress of
experimental procedure for mini-slump testing pro- cementitious materials is of great importance in
duces highly reproducible results, and the yield stress enabling the design of mix formulations with desired
calculated from mini-slump values correlate very well workability.
with those measured by viscometer, in the case of Rheometers are increasingly adopted to determine
fresh paste of pure shear flow. Mini-slump testing is a the yield stress of cement paste or concrete, and there
reliable method that can be utilised for the assessment are two methods commonly applied using such
of workability of cements. instruments to measure yield stress [2]. The first is
by ramping the shear rate generated by the rheometer
and recording the resultant shear stress, or vice versa.
Z. Tan  S. A. Bernal  J. L. Provis (&) Using rheological models such as the Bingham,
Department of Materials Science and Engineering, The
University of Sheffield, Sir Robert Hadfield Building,
Herschel-Bulkley or Casson models [3], the yield
Mappin St, Sheffield S1 3JD, UK stress can be extrapolated from the relationship
e-mail: j.provis@sheffield.ac.uk
235 Page 2 of 12 Materials and Structures (2017) 50:235

between the shear rate and shear stress; where the ‘‘slump’’ and/or the ‘‘spread’’. The former is the
downwards ramp is used in the determination, as is the difference between the height of the mould at the
case here, the quantity measured is the dynamic yield beginning of the test and the remaining pat of material
stress. Alternatively, in a ‘direct measurement’ of when the flow stops (and is a more useful measure for
yield stress, a constant low shear rate (e.g. less-fluid pastes), while the latter is the final diameter
0.1–0.001 s-1) is applied to the material starting from of the pat of material when flow stops (or after a
rest, and the (static) yield stress is identified as the specified time), and is used to characterise more fluid
maximum in the stress-time profile [4, 5]. Other pastes. The result of the slump test result is at least
methods such as creep recovery can also be used to capable of qualitatively predicting the workability of
measure yield stress characteristics [6]. concrete flow for the purpose of quality control.
However, measuring yield stress using a rheometer However, it is often far from convenient to produce
is sometimes difficult due to challenges in the inherent and manipulate the large quantities of material
nature of the yield stress material and the proper required for a full-scale concrete slump test in a
selection of a rheological model. Problems such as slip laboratory context, as much research work is con-
flow [7], fracture, and expulsion of the material are ducted with paste or mortar specimens. In order to
commonly encountered when using conventional resolve this issue, the so-called mini-slump test, which
rheometers in the low shear rate range [3]. Extrapo- is essentially a down-scaled slump test [15], is here
lating yield stress from rheological models relies on examined in detail as a method by which the
the validity of the model, which would be a challenge workability of cementitious pastes may be
for a material without an appropriately validated investigated.
model to describe its rheological behaviour, as is The mini-slump method is a simple, inexpensive
usually the case for non-Portland cements. In addition, and fast test to study the rheology of cement paste, if it
yield stress values lower than 10 Pa directly measured can be shown to be applicable and reproducible. Mini-
by conventional viscometers are commonly less slump test results have previously been quantitatively
reliable [8] due to the limited sensitivity of most linked with yield stress values obtained from theory
instruments. This range is typical of self-compacting and numerical modelling [16–19], showing the poten-
concretes and pastes. Furthermore, from a practical tial for the mini-slump test method to provide valuable
viewpoint, a rheometer is neither inexpensive nor information regarding the yield stress of cementitious
particularly convenient for on-site measurement by pastes. However, there is not yet a standard protocol
field personnel. Conversely, the traditional slump test describing the appropriate procedure for performing
is still an easy and simple method to study the mini-slump tests on cementitious materials. Inappro-
workability of concretes. It has long been widely used priate practical operation of this method could lead to
on construction sites because of its simplicity, appli- either less reliable or very scattered mini-slump test
cability and very low cost, in spite of the known results, making it difficult to estimate reliable values
limitations of repeatability and precision associated of the yield stress of the paste. To fill this gap, this
with the standard forms of this test [9–11]. paper aims to present a practical procedure for
In a typical slump test, a mould of a given conical performing mini-slump testing. The study also con-
shape is filled with the material to be tested [12]; tributes to the evaluation of workability of cementi-
various different cone geometries and sizes are used in tious paste especially with very low yield stress, which
different applications, but in the field of construction may be outside the normal measurement range of a
materials science the most common is the ‘‘Abrams conventional viscometer. This is of significant impor-
Cone’’ geometry of ASTM C143 [13], a truncated tance in the case of non-Portland cement pastes, such
cone with height:base diameter:top diameter ratios of as alkali activated cement paste, as their workability
3:2:1. Neglecting any inertial effects [14] (when can be very sensitive to factors such as mix formula-
inertia stress is typically * 3 Pa), the material flows tion (e.g. type and concentration of activator), reaction
after the mould is lifted, and then stops when the shear kinetics, time-dependent behaviour of fresh paste [20]
stress due to flow under gravity decreases to the value and mixing procedure [21], and the correlation
of the yield stress of the flowing material. Two between flow table and rheological test results for
geometrical quantities are commonly measured: the these materials has been shown in the past to be
Materials and Structures (2017) 50:235 Page 3 of 12 235

problematic [22]. So, a series of alkali-activated pastes

are used here as a test case for the proposed protocols.

2 Experimental programme

2.1 Materials characterisation and mix designs

Ground granulated blast-furnace slag (ECOCEM,

France) and fly ash (BauMineral GmbH, Germany)
were used as precursors to prepare the alkali activated
cement pastes. Table 1 lists the chemical composi-
tions of the two materials used as determined by X-ray
fluorescence (XRF). Figure 1 shows the particle size
distributions of the two materials characterised by Fig. 1 Particle size distribution of slag and fly ash as
determined by laser diffractometry, The Dv(90) values of the
laser diffraction (Malvern Mastersizer 2000). slag and fly ash are 28.6 and 80.1 lm, respectively
A total of 27 paste formulations were studied. The
total water to binder (where ‘binder’ is defined as allowed to cool to ambient temperature, after addition
precursor ? solid component of the activator) ratios of the NaOH pellets. The solution was used on the
were 0.40, 0.44 and 0.48, with activator doses of 4, 8 same day as prepared, to avoid precipitation of solid
and 12% relative to the mass of precursor (dry solids sodium metasilicate hydrates. The complete 27 for-
basis). As solid precursors, slag and fly ash were mulations are summarised in Table 2.
blended at different levels (100:0, 75:25 and 50:50
ratios of slag:fly ash by mass) to yield pastes with 2.2 Mixing procedure and testing methodology
diverse rheological properties. The alkaline activator
was based on a commercial sodium silicate solution For blended pastes containing both slag and fly ash,
(PQ Silicates, UK), composed of 14.7 wt% Na2O, 30 min of pre-mixing of the dry powders was
29.4 wt% SiO2 and 55.9 wt% H2O; the modulus of the performed prior to mixing with the activating solution.
activating solution (Ms = SiO2/Na2O molar ratio) For each mini-slump test, 60 g of precursor powder
was adjusted by mixing the commercial solution with was combined with the specified amount of distilled
analytical grade solid NaOH (Sigma Aldrich, UK) to water and activator in a plastic cylindrical container
obtain a sodium metasilicate (Ms = 1) solution. The (diameter 5 cm and height 10 cm). The paste was then
adjusted metasilicate solution was stirred for 2 h, and mixed using a high shear mixer as shown in Fig. 2, at
400 rpm and ambient temperature (20 °C) for 2 min,
Table 1 Chemical compositions of the slag and fly ash on an unless specified otherwise in the description of the
oxide basis, as determined by XRF influence of testing parameters in Sect. 3 below. The
Oxide Slag (wt%) Fly ash (wt%) homogeneously mixed paste was immediately used for

CaO 43.0 5.8

Table 2 The 27 paste formulations studied; each cell contains
Al2 O3 10.1 22.7 the activator doses (in wt% relative to the mass of precursor)
SiO2 37.5 54.5 used for the specified w/b and slag:FA ratios
MgO 6.50 2.5 Slag:FA w/b
Na2O 0.1 0.9
0.40 0.44 0.48
K2O 0.3 1.8
Fe2O3 0.4 7.3 100:0 4, 8, 12% 4, 8, 12% 4, 8, 12%
TiO2 0.5 0.9 75:25 4, 8, 12% 4, 8, 12% 4, 8, 12%
Mn3O4 0.2 \ 0.05 50:50 4, 8, 12% 4, 8, 12% 4, 8, 12%
235 Page 4 of 12 Materials and Structures (2017) 50:235

mini-slump testing, unless specified otherwise in

Sect. 3.
The mini-slump test setup used in this study is a
downscaled Abrams cone geometry [15]: 19 mm top
diameter, 38 mm bottom diameter, 57 mm height as
shown in Fig. 3. Each test was performed using a
poly(tetrafluoroethene) mini-slump cone on a flat
sheet of poly(methyl methacrylate) marked with grid
squares of 2 9 2 cm2. Freshly mixed paste was
immediately poured into the cone, and then the cone
was lifted as slowly as possible (\ 0.005 m/s [23]) to
minimise inertial effects. After 1 min, a digital
photograph was taken from directly above the resul-
tant pat of material, from which the slump area was
calculated using the ImageJ software, calibrated using
the scaled grid. The diameter of the spread was then
calculated from the slump area. Each paste was tested
in triplicate, using three separately mixed batches of
paste to obtain good statistical reproducibility of the
data obtained, and to ensure that all tests were
conducted on pastes of directly comparable shear
history.
To compare the yield stress values calculated from
mini-slump testing with that determined using a
viscometer, a HAAKE Viscotester 550 instrument Fig. 3 Schematic diagram of mini-slump test cone geometry.
was employed to directly measure the yield stress of Note that the top and bottom diameters are inner sizes of the
fresh pastes, using a six-blade vane-in-cup geometry. cone
During the test, the shear rate was linearly ramped up
from 0 to 100 s-1 over 60 s, then held for 5 s, then
linearly ramped down from 100 s-1 to 0 over another
60 s, as illustrated in Fig. 4. The decreasing shear rate-
shear stress profile was chosen for analysis, and the
yield stress value was obtained by extrapolating the

Fig. 4 The applied shear rate as a function of time during the

viscometric testing

shear rate-shear stress curve to zero shear stress using

the Herschel–Bulkley model (Eq. 1), ensuring non-
negativity of all parameters during fitting, to obtain the
Fig. 2 The high shear mixer blade used in this study (dynamic) yield stress s0.
Materials and Structures (2017) 50:235 Page 5 of 12 235

s ¼ s0 þ kc_n ð1Þ activator. Sodium silicate is known to act as a

dispersant in particulate suspensions [24, 25], lower-
In Eq. 1, k and n are fitting constants determined by ing the yield stress of the paste [26] which resulted in a
regression of the shear rate-shear stress curve; the greater spread in the mini-slump test. This dispersion
Bingham model is a special case of the Herschel– effect is particularly remarkable in the relatively sticky
Bulkley model with n = 1. slag-based pastes; the spread diameter is only
This method was found to be more reliable and 72.5 mm in the pure slag paste with 4 wt% activator
reproducible than the direct measurement of yield dose at w/b 0.40, while a 12 wt% activator dose in the
stress using a constant low shear rate, particularly for equivalent paste increased the spread diameter to
pastes of low yield stress, considering the sensitivity 120.9 mm.
and capabilities of the viscometer used here.
Due to the somewhat larger volume of paste 3.2 The correlation of yield stress calculated
required for the viscometer to achieve pseudo-infinite from mini-slump spread size and measured
medium conditions, the pastes to be tested by this using a viscometer
method needed to be prepared in a slightly different
manner from those used in the mini-slump testing. For Based on the work of Kokado et al. [17] and of Roussel
each batch to be tested using the viscometer, 270 g of and Coussot [16], the yield stress of pastes can be
precursor powder was combined with the required calculated from the mini-slump spread diameter (or
amount of distilled water and activator in a 500 mL radius) when a set of conditions are fulfilled [14]:
plastic beaker. The paste was then mixed using the
high shear mixer (Fig. 2) at 800 rpm for 2 min, and 1. The tested volume must be representative of the
immediately analysed. The selection of the rotational mixture.
speed of 800 rpm for the larger batch (270 g precursor 2. The thickness of the sample must be at least five
cf. 60 g for mini-slump testing) is based on the times the size of the largest particle.
observation that this mixing protocol was found in 3. The surface tension and inertial effects must be
preliminary testing to result in equivalent performance negligible.
(comparable spread sizes of mini-slump test) com- With the exception of the paste made with 100%
pared with mixing the 60 g batch at 400 rpm for the slag, at w/b 0.40 and 4% activator dose, the alkali-
same time period (2 min). This indicates that each unit activated paste formulations studied here appeared to
of paste received comparable shear energy from the behave as pure shear flow pastes (i.e. the thickness of
two mixing strategies. spread is far less than the diameter of the spread) [16].
So, the yield stress (s0) of each paste was calculated
according to Eq. 2 [14, 16, 17], describing the yield
3 Results and discussion stress as a function of the density of the paste q,
volume of the mini-slump cone X, and the mini-slump
3.1 The influences of mix design parameters spread diameter R.
on the workability of alkali-activated pastes
225qgX2
Table 3 presents the spread diameters of the 27 alkali- s0 ¼ ð2Þ
128p2 R5
activated pastes measured by mini-slump testing,
which range from 72.5 to 139.5 mm across the pastes The density of each fresh paste was calculated
assessed. None of the pastes showed noticeable based on the mix formulation and density of each
bleeding or segregation during the mini-slump test. component, i.e. slag, fly ash, activator solution and
Increasing the water to binder ratio raised the spread water; g is the acceleration due to gravity (9.81 m/s2).
diameters of all pastes, as expected. Under otherwise To determine the accuracy of the yield stress values
comparable conditions, i.e. the same water/binder calculated from mini-slump testing of these alkali-
ratio and same slag/fly ash ratio, a higher activator activated pastes, the yield stress was also measured
dose also increased the spread diameter due to the using a viscometer, as described in Sect. 2.2. Figure 5
dispersion effect of the sodium metasilicate added as shows the yield stress values obtained according to the
235 Page 6 of 12 Materials and Structures (2017) 50:235

Table 3 The mini-slump spread diameters (reported in mm) of alkali-activated slag/fly ash blended pastes
Content of slag in the binder (wt%) Concentration of activator (wt%) Water/binder ratio
0.40 0.44 0.48

100 4 72.5 ± 1.2 92.7 ± 2.0 105.6 ± 0.5

8 105.0 ± 0.4 113.7 ± 1.2 118.4 ± 0.7
12 120.9 ± 1.6 124.8 ± 1.3 134.3 ± 2.4
75 4 95.7 ± 2.3 109.4 ± 1.2 117.7 ± 0.8
8 109.4 ± 0.9 119.1 ± 0.6 125.7 ± 0.4
12 135.0 ± 1.7 135.9 ± 1.6 136.2 ± 0.7
50 4 107.2 ± 1.1 117.2 ± 0.5 121.9 ± 0.2
8 117.9 ± 1.0 124.3 ± 0.5 128.1 ± 0.7
12 139.5 ± 1.6 137.8 ± 2.9 137.6 ± 0.6
Error values correspond to one standard deviation of three independent measurements

two methods. The yield stresses of all pastes range with the conditions noted above for Eq. 2 to be valid),
from 1.05 to 74.6 Pa, decreasing as the fly ash content, when using the proposed mixing procedure.
water to binder ratio and activator dose increase, However, it is worth noting that yield stress values
consistent with the discussion above. Comparison of measured via the mini-slump test are systematically
the results in Fig. 5 shows that low yield stresses slightly higher than those obtained from the viscome-
(below 10 Pa) determined from the mini-slump test ter. This could be attributed to the fact that the effect of
generally correlate very well with viscometer mea- the surface tension of the paste was not included in
surements, while there is quite a degree of scatter in Eq. 2; this would normally be of the same order as the
the values for yield stresses above 10 Pa, which will be yield stress (1–2 Pa) for low concentration suspen-
discussed in more detail below. The good agreement sions [27]. The neglect of surface tension effects in the
between the two methods for low yield stress values calculation of yield stress using Eq. 2 could system-
demonstrates the applicability and reliability of the atically overestimate the results compared with those
mini-slump test for measuring the yield stress of pastes measured by the viscometer. However, Roussel et al.
which slump in pure shear flow (i.e. which comply [27] reported that the surface tension effect in the
mini-slump test is negligible in pastes with yield
stresses larger than about 1 Pa, which is the case for all
pastes studied here.
At higher yield stress values ([ 10 Pa for the pastes
in this study), the determination of yield stress by
mini-slump testing via Eq. 2 seems less reliable. For
example, the yield stress of paste made of 100% slag,
w/b 0.40 and 4% activator dose is 74.6 Pa, which is
much higher than that determined by viscometry for
the same paste, 36.4 Pa. The latter value is expected to
be more accurate and reliable as the viscometer
performs very well in this range, and the shear rate-
shear stress curve measured by the viscometer (Fig. 6)
shows that the rheological model of the paste is well
approximated by the Bingham model, giving a rela-
tively reliable determination of the yield stress. The
Fig. 5 Yield stress values measured by mini-slump test and most likely reason for the inaccuracy of the evaluation
viscometer of yield stress based on mini-slump testing for this
Materials and Structures (2017) 50:235 Page 7 of 12 235

slumped, which is not consistent with the uniform pat

shape resulting from pure shear flow.

3.3 Reproducibility of the proposed procedure

for mini-slump testing

Figure 8 shows the coefficients of variation of spread

diameter in three replicates of each of the 27 pastes in
the mini-slump test; all values are lower than 2.4%,
with 24 of the 27 values lower than 2.0%. The average
coefficient of variation of all samples is less than 1%.
This demonstrates remarkably good repeatability of
the mini-slump testing procedure proposed in this
study.
Fig. 6 The shear stress-shear rate profile of a paste with 100% The reproducible measurement of paste spread size
slag, w/b = 0.40 and activator dose 4%, measured by viscom-
in the mini-slump test can also lead to relatively low
etry in a descending ramp (the shear rate linearly decreased from
100 s-1 to 0 during 60 s), showing Bingham-type paste scatter in the yield stress calculated by Eq. 2. Because
behaviour and a yield stress of 36.4 Pa this equation involves an inverse 5th-power relation-
ship between yield stress and spread diameter, a 2%
paste is that Eq. 2 is derived for pastes undergoing coefficient of variation in the spread size can lead to
pure shear flow, while the shape of the pat of the paste the calculated yield stress varying by approximately
(Fig. 7) indicates that the paste has undergone neither 10%, or about 5% when the coefficient of variation in
pure shear flow nor pure elongational flow, which spread is 1%. Considering the low yield stresses
agrees with the conclusion of Pierre et al. [18] that a associated with pure shear flow of a paste, which is the
material is mainly in a spread regime below yield regime in which Eq. 2 is valid, even a 10% uncertainty
stress values of 18 Pa. Figure 7 shows a visible raised in the calculated yield stress would still be a valuable
ring of material which has retained the circular form of result in terms of a rapid and inexpensive test for the
the cone at the centre of the pat as the material has determination of the shear stress of cementitious
pastes. However, the ability to achieve such a high
reproducibility is contingent on correct use of the test
methodology, and so the influence of various test

Fig. 7 The shape of the pat of a paste with 100% slag, w/

b = 0.40 and activator dose 4% after mini-slump testing,
showing evident deviation from uniform shear flow via the Fig. 8 The coefficients of variation (relative standard devia-
raised ring of material in the position of the original cone tion) of the spread size of all samples
235 Page 8 of 12 Materials and Structures (2017) 50:235

parameters on the ability to obtain correct results will times to measure three spread sizes for the same paste,
be explored in more detail in the following sections. to produce results with optimal reproducibility.
It is also worthwhile to note that the rapid removal
3.4 Influence of testing procedure on the results of the mould from the paste may introduce additional
of mini-slump test inertial effects to the final spread. The stress which can
be caused by inertial effects is in the range of several
Although many aspects of the experimental protocol Pa, which becomes significant in the case of pastes
may affect the statistical performance of mini-slump with very low yield stresses [29], e.g. \ 10 Pa. Rapid
test results, Pashias et al. [28] reported that no removal of the mould may also disturb the nature and
measurable difference was observed in their tests on shape of the paste when performing mini-slump
mini-slump of red mud due to factors such as the speed testing, particularly if there is some degree of adhesion
of removing the mould, the time at which the between the paste and the mould material, although
measurement of the test outcome was taken, the this was minimised in the current work through the use
surface on which the mini-slump testing was per- of a poly(tetrafluoroethene) mould. For the sake of
formed, and the aspect ratio of the mini-slump test practical experimental operation, the speed of removal
mould. of the mould should be slow enough to minimise the
However, the time taken to measure the outcome of inertial effects.
the test does have an influence for the study of In this study, the aspect ratio of the mini-slump test
cementitious materials. The paste studied in the work cone is 1.5, which is in accordance with the Abrams
of Pashias et al. [28] was red mud, which does not cone geometry widely used in the field of construction
show the same time-dependent rheology as do materials, but is higher than the aspect ratio recom-
cementitious materials. Cementitious pastes undergo mended by Pashias et al. [28], which was approxi-
chemical reactions leading to the build-up of a mately 1.0. Those authors explained that an aspect
complex microstructure, particles can also aggregate value too much larger than 1.0 may lead to the collapse
or flocculate, and these factors may all influence the of a cylindrical paste specimen, rather than the
spread size measured during mini-slump testing. Each material flowing. However, no collapse of the pastes
mini-slump test in this study was carried out in was observed here, which means that the geometry of
triplicate on individually mixed batches to obtain an the cone was satisfactory for all of the pastes in this
average value of the spread size, rather than the study.
common practice in the literature of measuring three
data points in succession from a single batch of paste. 3.5 The influence of mixing protocol on the results
This removes the possibility of introducing errors of mini-slump testing
through the time dependence (known as ‘slump loss’
in concrete practice) of the yield stress of the reacting To investigate the influence of the mixing protocol on
paste. the results of mini-slump testing, different possible
To illustrate the importance of the use of separate mixing schemes were studied. The first comparison is
paste batches in obtaining reproducible measurements the difference between hand mixing and high shear
in the current study, Fig. 9 presents the spread shapes mixing applied to the paste. Figure 10 shows the mini-
of the same mixed paste (100% slag, w/b = 0.40 and slump results for a paste with 100% slag, w/b = 0.40,
4% activator dose) measured immediately after mix- and activator dose 12%, mixed by hand (2 min) and
ing, and with 5 and 10 min delays before measure- using a high shear mixer (400 rpm for 2 min). The
ment. The dramatic change in the pat shape during this spread diameter after hand mixing is
short timeframe demonstrates the importance of the 126.1 ± 4.2 mm, while high shear mixing gave
structural evolution of the paste even in the first 120.9 ± 1.6 mm, showing that both the spread value
minutes after mixing, which may also include some and reproducibility of the tests were influenced by the
loss of water from the surface due to drying effects. choice of mixing method.
The images in Fig. 9 highlight the importance of These experimental results demonstrate that mixing
accurate timing of the mini-slump test. This is why it is by hand was not sufficient to disperse the precursor
proposed in this study to mix the paste separately three particles in the aqueous environment
Materials and Structures (2017) 50:235 Page 9 of 12 235

Fig. 9 The spread shapes of a paste with 100% slag, w/b = 0.40, and 4% activator dose, at different times, a tested immediately after
mixing, b 5 min after mixing, c 10 min after mixing

the two identical pastes (100% slag, w/b 0.40 and

activator dose 12%) after mini-slump testing, where
the pastes were mixed by hand and by the high shear
mixer, respectively. The shape obtained following
hand mixing appeared obviously less circular than the
one mixed at high shear, demonstrating the particles in
the paste mixed by hand was not evenly dispersed due
to the insufficient mixing intensity. This loss of pat
circularity for hand-mixed pastes was observed con-
sistently across multiple tests.
Experimental work by Han and Ferron [30]
demonstrated that all mixtures containing superplas-
ticisers prepared using the ASTM C1738 protocol for
high-shear mixing [31] displayed higher yield stresses
Fig. 10 Spread diameter of a paste with 100% slag, w/ than their counterpart pastes prepared according to the
b = 0.40, and activator dose 12%, mixed by hand
(* 150 rpm for 2 min) and using the high shear mixer
normal-shear ASTM C305 protocol [32]. The results
(400 rpm for 2 min) obtained here agree well with these previous observa-
tions, in that a smaller mini-slump spread size was
observed for the paste mixed by high shear mixing in
(water ? activator solution) used here. The speed of this study, and higher yield stress corresponds to
(vigorous) hand mixing in this study was approxi- smaller spread size [30, 33]. However, Roy and Asaga
mately 150 rpm, which is much lower than the [34] reported that increasing intensity of mixing
400 rpm generated by the high shear mixer. Apart caused a breakdown of particulate aggregates and
from the lower speed, the paddle used in hand mixing thus substantially decreased yield stress; the results
was also much less efficient than the dedicated shear obtained here were not consistent with that
blade of the high shear mixer. The larger spread interpretation.
diameter resulting from hand mixing could be The coefficient of variation of spread size of this
attributed to the insufficient mixing that is not strong paste mixed by hand (3.3%) is also much higher than
enough to evenly disperse particles in the paste, that achieved with the high shear mixer (1.3%),
allowing the liquid activator and water to flow indicating that high shear mixing produces more
unevenly (i.e. reach a larger spread diameter in the reproducible mini-slump test results than hand mixing,
longest dimension) when performing mini-slump as the energy and mode of mixing energy input are
testing. The pictures in Fig. 11 depict the shapes of better controlled using a mechanical mixer.
235 Page 10 of 12 Materials and Structures (2017) 50:235

Fig. 11 The outline of the paste (100% slag, w/b 0.40 and activator dose 12%) mixed by hand (a) and using the high shear mixer
(b) after mini-slump testing

Table 4 The spread diameter (mm) of pastes with 75% slag ? 25% fly ash, w/b = 0.40 and activator dose 8%, produced at different
mixing speeds, durations and batch sizes
400 rpm, 60 g precursor, 2 min 400 rpm, 270 g precursor, 2 min 800 rpm, 270 g precursor, 4 min
109.4 (set 1); 110.2 (set 2) 109.0 110.3

Table 4 shows the spread size of a paste with 75% paste with this formulation in the larger batch size.
slag ? 25% fly ash, w/b = 0.40 and activator dose Doubling both the speed and mixing duration (final
8%, mixed by a high shear mixer at different speeds, entry in Table 4) for the 270 g batch size again gave a
for different durations and with different batch sizes. mini-slump result matching the results obtained at
The combination of these factors generated different lower mixing energy density to within 1%. These
mixing energy densities. results indicate that once a satisfactory mixing condi-
The first (109.4 mm) value in Table 4 was mea- tion is determined for a particular paste (i.e. resulting
sured for a paste mixed by the mixing protocol which in a well-mixed condition), the test method presented
is adopted for all 27 samples in this study, i.e. 60 g here is satisfactorily robust to variability in mixing
precursor, 400 rpm for 2 min. It is interesting to note parameters to enable it to be a useful and reliable
that in re-testing using the same materials and mixing protocol in practice.
scheme 12 months after the initial tests (denoted ‘set
2’, where the initial test is ‘set 1’), a very similar value
(110.2 mm) was measured. This agreement shows that 4 Conclusions
the single-operator reproducibility of the measure-
ment procedure is high. The study investigated the measurement of yield stress
When the paste was mixed in a 270 g batch at of cementitious pastes based on a reproducible mini-
400 rpm for 2 min, a spread diameter of 109.0 mm slump testing method using a well-defined mixing
was obtained. Since the mixing speed and time procedure. The relationship between the spread
duration were as same as the baseline mixing scheme, diameter in mini-slump testing and yield stress was
each unit of paste in this larger batch received verified with results obtained using a rotational
approximately 22% of the mixing energy of the 60 g viscometer; the correlation between the two methods
batch size. However, the spread sizes of the two pastes is good for low yield stress values, but shows
are comparable, which means that a mixing speed of deviations at higher yield stresses when the flow
400 rpm is also adequate to disperse particles in the patterns and resultant pat shape in the mini-slump test
Materials and Structures (2017) 50:235 Page 11 of 12 235

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