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Journal of Non-Newtonian Fluid Mechanics 214 (2014) 18–27

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Measurement of yield stress of cement pastes using the direct shear test
Joseph J. Assaad a,⇑, Jacques Harb b, Yara Maalouf c
Holderchem Building Chemicals, PO Box 40206, Lebanon
Civil Engineering Department, Notre Dame University, PO Box 72, Lebanon
Notre Dame University, PO Box 72, Lebanon

a r t i c l e i n f o a b s t r a c t

Article history: The direct shear test is widely used in soil mechanics to determine the cohesion (C) and angle of internal
Received 8 April 2014 friction (/). This paper aims to assess the suitability of this test to evaluate yield stress (s0) of cement
Received in revised form 19 October 2014 pastes having different flowability levels. Special emphasis was taken to eliminate friction between shear
Accepted 21 October 2014
boxes, thus allowing the measurement of C ranging from several kPa to just a few Pa. Tests have shown
Available online 30 October 2014
that the maximum shearing stress prior to failure is not a material constant, but rather varies with the
normal stress as per the Mohr–Coulomb law. Good correlations between C and s0 determined using
the vane method were established. Nevertheless, the vane method was found to over-estimate s0 when
Cement paste
the blades are positioned inside the specimen, particularly for cohesive materials.
Direct shear Ó 2014 Elsevier B.V. All rights reserved.
Yield stress

1. Overview on yield stress measurements Over the last decades, various techniques have been more or
less successfully developed to overcome the complications related
The yield stress (s0) is of interest for various industries; it is to wall slip and enable reliable measurement of s0 [9–13]. The
regarded as the transition stress between elastic solid-like behav- most popular techniques were those realized under quasi-static
ior and viscous liquid-like behavior [1]. The measurement of s0 is conditions and whose basic principle requires that shearing takes
generally performed using direct rheometric techniques that con- place within the material itself, i.e. not between the material and
sist of slowly shearing the material and recording the peak shear an object. Hence, ideally, this requires that a virtual plane of mate-
stress required to initiate flow. However, such measurements are rial should move inside the suspension, and the material–material
not easy to implement, given the need to accurately monitor vari- shearing stresses recorded at low shear rates [9,10,14]. The peak
ations of shear stresses at low shear rates [2–4]. Most importantly, shear stress needed to initiate flow can thus be considered as the
the wall-sample interactions can result in slip effects associated ‘‘true’’ s0 of tested material.
with displacement of the dispersed phase(s) away from the bound- The vane method is probably the most popular for measuring
aries, resulting in a low-viscosity particle-depleted layer near the s0, since slip is physically impossible and shearing completely
wall and under-estimation of s0 [5,6]. The probability of wall slip occurs within the material [6,9,15]. Its concept originated from soil
increases when dealing with smooth walls, relatively small gaps, mechanics, where vanes are used to determine shear strength of
low flow rates, and concentrated suspensions of large and floccu- soils as described in ASTM D2573 [16]. Hence, a four, six, or
lated particles. A common way to reduce the extent of slip is to eight-bladed vane of diameter D and height H, connected to a
roughen the wall’s surface in order to increase friction with the stress-controlled rheometer is fully immersed in the material and
suspension [7,8]. It is to be noted that s0 can also be determined rotated at sufficiently low shear rate to determine the maximum
using indirect techniques that consist of extrapolating to zero torque required to initiate flow. Nguyen and Boger [9] suggested
shear rate a series of shear stress vs. shear rate rheological data. a series of criteria for satisfactory s0 measurements of various con-
Nevertheless, such measurements are very sensitive to the centrated suspensions including H/D < 3.5, DT/D > 2, Z1/D > 1, and
assumed constitutive model as well as the accuracy and range of Z2/D > 0.5 (see Fig. 1 for notations). Elsewhere, Nguyen and Boger
experimental flow data especially at low shear rates [2,4]. [3] reported that Z1 + H + Z2 > 2H. Alderman et al. [17] utilized a
set-up where Z2 = H, Z1 = ½ H, and DT = 3D.
⇑ Corresponding author. To calculate s0, the maximum torque (Tm) is taken as the alge-
E-mail addresses: (J.J. Assaad), (J. Harb), braic sum of shear stress exercised by the lateral area (Ts) and (Y. Maalouf). the vane’s upper and lower areas (Te), such that:
0377-0257/Ó 2014 Elsevier B.V. All rights reserved.
J.J. Assaad et al. / Journal of Non-Newtonian Fluid Mechanics 214 (2014) 18–27 19

T m ¼ T s þ 2T e : (i.e., material in slot shearing against material in bulk). Zhang

et al. [14] considered that, unlike the vane method, the plate tech-
In terms of shear stress, the torque can be written in Eq. (1) as:
nique does not rely on an assumed yield surface area. The s0 was
p  Z D=2 calculated as Fnet = (F  Fi) divided by the slotted plate area; where
Tm ¼ D 2 ss H þ 4p se r2 dr ð1Þ F refers to the force recorded by the balance, and Fi is the initial
2 0
force reading calculated as the gravitational force due to plate and
where r is a radial coordinate, se is the shear stress on the upper and wire mass minus the buoyant force in suspension.
lower circular ends of the cylinder, and ss is the stress on the curved The plate technique was found adequate to determine s0 of var-
cylindrical surface. Assuming that yielding occurs at the cylindrical ious non-Newtonian fluids such as bentonite and TiO2 suspen-
surface defined by the tips of the blade, and that se and ss are uni- sions; however, several difficulties were encountered when
form and equal to s0 at maximum torque, Tm becomes equal to: testing cement pastes [14]. For example, s0 could be over-esti-
!  mated if the plate is not in a fully vertical position during testing,
pD 3 H 1 given that the force measured would be higher than that for a ver-
Tm ¼ þ s0 ð2Þ
2 D 3 tical plate. Another difficulty in determining s0 occurs in cases
when it is important to use a correction factor for edge effects
During s0 evaluation of various emulsions, Yoshimura et al. [18]
[14]. The determination of this factor is time-consuming, as it
considered positioning the top edges of the blades vane aligned
requires the use of various plate sizes and batching of cement
with the upper material’s surface, so as to eliminate the stress con-
pastes with different water-to-cement ratios (w/c).
tribution from emulsion located above the blades on torque mea-
Assaad and Harb [19] proposed using the triaxial and uncon-
surements. Consequently, Tm becomes equal to Ts + Te and the
fined compression tests to overcome the complications related to
factor (1/3) in Eq. (2) is replaced by (1/6), as follows:
slip effects, secondary flow, or confinement conditions encoun-
pD 3 H 1 tered in rheometric techniques. These tests are widely used in geo-
Tm ¼ þ s0 ð3Þ technical applications to analyze the soil’s shear strength
2 D 6
properties, including cohesion (C) and angle of internal friction
To measure s0 at very low shear rates, Zhu et al. [10] and Zhang (/), and are standardized by ASTM D2166, D2850, and D4767
et al. [14] developed the plate technique in which a slotted plate [20–22]. Two main drawbacks were however attributed to these
submerged in a test material is pulled out slowly while measuring tests, including a considerable time needed for specimen prepara-
the required load that comes from the material’s resistance to this tion (i.e., around 15–20 min) and inadequacy of testing flowable
motion. The plate was hung to a balance through very thin stainless mixtures having a flow exceeding around 140 mm, as per ASTM
steel wires and its velocity precisely controlled from 0.003 to C1437 [23]. A cohesion threshold of around 4 kPa was determined
60 mm/min [10,14]. The height of slots was at least 100 times larger on tested mortars, below which the specimens are no longer capa-
than the maximum particle size in the suspension. This strengthens ble to self-stand in a vertical position for testing [19]. Tests realized
the assumptions that the suspension remains static in the slots with under drained conditions displayed higher C values than those per-
no secondary flow, and that shearing occurs only at the slot edges formed under undrained ones, given the resulting increase in fric-
tion generated between solid particles within the matrix.

2. Use of direct shear to measure s0

The direct shear test is the oldest and simplest method used in
soil mechanics to determine the C and / parameters, and analyze
failure mechanisms occurring along interfaces [24–26]. The proce-
dure for specimen preparation is quite simple, and drawback
related to verticality encountered in triaxial and unconfined com-
pression tests is not present [19]. In this test, two portions of a spec-
imen are made to slide along each other by the action of steadily
increasing horizontal shearing force while a constant load is applied
normal to the plane of relative movement. The direct shear test is
realized under quasi-static conditions, and shearing takes place
within the material itself along a pre-defined interface represented
by the horizontal surface area of the shearing box. This physically
enables the determination of ‘‘true’’ s0, since all problems related
to wall slip and secondary flow are eliminated. The direct shear is
standardized equipment documented in ASTM D3080 [27] and
available in most research centers.
Besides its use in geotechnical applications, the direct shear test
has been popular when studying rheology of extrudable materials
like plastics, fiber composites, rubbers, clays, and asbestos [28,29].
In fact, conventional shear-driven rheometers such as parallel plates,
rotors, and concentric cylinders are not adapted to measure rheology
of highly cohesive pastes due to the difficulty of sample preparation,
wall slip, and plug flow. Alfani and Guerrini [29] reported that the
direct shear is among the most promising and suitable methods for
rheological characterization of cement-based extrudable materials
including the interfacial flow behavior between the bulk materials
and equipment forming wall systems. For adequate extrusion, Toutou
Fig. 1. Notations used for vane configuration. et al. [30] found that s0 has to be high enough to allow the material to
20 J.J. Assaad et al. / Journal of Non-Newtonian Fluid Mechanics 214 (2014) 18–27

retain its shape when leaving the extruder; the common minimum cement were 4050 cm2/g and 3.14, respectively. The cement had
usable s0 is evaluated at around 20 kPa. C3S, C3A, and Na2Oeq. values of 63.5%, 6.1%, and 0.71%, respectively.
Limited studies exist in literature pertaining to the suitability of A naphthalene sulphonate based high-range water reducer
direct shear to assess s0 of cementitious materials possessing flow- (HRWR), complying with ASTM C494 Type F, having a specific
able nature. L’Hermite and Tournon [31] were among the few gravity of 1.18 and solid content of 35% was used. A liquid cellu-
researchers who considered this test to study shear resistance of losic-type viscosity-modifying admixture (VMA) was also
normal-consistency fresh concrete. Keeping the displacement rate employed. Its specific gravity and solid content were 1.11 and
constant, the authors found that shear stress increases linearly 25%, respectively. A sodium gluconate based set-retarder was
with the degree of distortion up to a maximum value, then incorporated in all pastes at a rate of 0.2% of cement mass, to avoid
decreases towards a steady state region. A linear relationship hydration effects on test results.
between normal and shear stresses was established following the Ten cement pastes exhibiting different flowability levels were
Mohr–Coulomb law: tested. The flow was evaluated by determining the material’s aver-
age diameter after spreading on a horizontal surface. An ASTM
s ¼ C þ r0 tan / ð4Þ C1437 [23] mini-slump cone having top diameter, bottom diame-
The s and r0 in Eq. (4) refer to shear resistance and normal effec- ter, and height equal to 70, 100, and 50 mm, respectively, was used.
tive stress resulting from the solid grains, respectively. As summarized in Table 1, the flowability varied from highly cohe-
Hendrickx et al. [32] reported that s0 of relatively stiff mortars sive (i.e., flow of 100 mm) to highly flowable (i.e., flow of 250 mm).
intended for masonry and brick-laying applications are difficult to The required flowability was secured by selecting the appropriate
measure using traditional rheometric techniques; geotechnical w/c and, if necessary, adjusting the HRWR. Depending on w/c
methods such as the vane and direct shear should instead be used and targeted flowability, the VMA was added at different rates to
to quantify shear strength. The authors reported that the maxi- minimize bleeding and sedimentation. Such phenomena may
mum stress in an undrained mortar is not a material constant, directly affect stability of cement pastes with direct influence on
but rather depends on the rate of stress increase and normal load C and s0 measurements [37]. All cement pastes were batched with
applied. Tested mortars exhibited C values ranging from 1 to a laboratory mixer using water cooled to constant temperature of
3 kPa, whereas the / values varied from 25° to 47° [32]. Girish 20 ± 3 °C. Water was first introduced in the mixer followed gradu-
and Santhosh [33] developed a 150-mm cubic direct shear appara- ally by the cement and HRWR over 1 min. After a rest period of
tus to evaluate the Bingham rheological properties of fresh con- 30 s, the VMA and set-retarder were added and mixing resumed
crete. Excessively high s0 values varying from 13 to 80 kPa were, for 2 additional minutes. The bulk fresh unit weight of cement
however, reported depending on w/c and coarse aggregate concen- pastes was determined using a calibrated container having a vol-
tration. The authors attributed the high s0 values to the quasi-sta- ume of 0.5–l (Table 1).
tic nature of direct shear along with the high aggregate friction Five grades of poly-vinyl acetate (PVA) emulsions commonly
encountered during shearing at low rates [33]. used as adhesives for wood, furniture, paint, and paper industries
Lu and Wang [34,35] considered the direct shear to measure were tested [38]. These smooth white colored emulsions are pro-
‘‘true’’ s0 and validate a constitutive model developed for predict- duced by polymerisation of vinyl acetate and subsequent alcohol-
ing the yield behavior of cementitious materials. The model is prin- ysis of the polyvinyl acetate that is formed. Such materials display
cipally based on the concept of excess cement pastes and shear exceptional stability with no time-dependent behavior, thus mak-
stresses developed between two cement particles that arise from ing them ideal systems for rheological characterization and valida-
the combined effect of Van der Waal’s and electrostatic forces. tion purposes [18]. The PVAs were selected to exhibit different
The s0 determined at zero normal stress was found to decrease yield stresses; their physical properties including flowability deter-
from 1673 to 474, 202, and 142 Pa for cement pastes having w/c mined using the mini-slump cone are listed in Table 2. The solid
of 0.3, 0.35, 0.4, and 0.48, respectively [34]. The corresponding / content and maximum particle size were determined using mois-
values decreased from 6°, to 5°, 2.2°, and 2°, respectively. No ture analyzer and laser particle-size instruments, respectively.
attempts were made, however, to test cement pastes and mortars The viscosity was measured using Anton Paar coaxial cylinder rhe-
with higher w/c or to quantify the effect of friction between shear ometer (RheolabQC) using a sandblasted internal rotating cylinder
boxes on test results. to minimize slippage. The testing procedure consisted of pre-
This paper seeks to evaluate the suitability of direct shear test shearing the PVA at 100 s1 over 1 min to break down the suspen-
for assessing s0 of cement pastes possessing cohesive to flowable sion’s structure and ensure a reference state. Subsequently, the
nature. Special care was placed to reduce friction emanating from material is subjected to a hysteresis loop varying from 0 to
the shear boxes and allow measurements of C values in the order of 100 s1 and back to 0 s1. The elapsed time for each ascending
few Pa. Also, various emulsions displaying no time-dependent and descending part is 1 min. The download curve of the data
behavior were tested, and C responses are validated using s0 deter- recorded using a computer was used to determine the viscosity.
mined by the vane method. The paper also emphasis relevant phe-
nomena related to the friction angles that can be deduced from 3.2. Determination of C using the direct shear test
direct shear testing as well as effect of vane positioning on s0 mea-
surement and its computation using either Eq. (2) or Eq. (3). Data An ELE Direct Shear apparatus complying with ASTM D3080
presented in this paper can be of interest to researchers in various [27] requirements was used in this study. It comprises a metal
industries to facilitate inter-laboratory comparison and unify shearing box divided into two halves horizontally, and measuring
quantification of ‘‘true’’ s0 using standardized testing protocols. 100 mm diameter and 58 mm height. The lower section of the
box can move forward at different constant velocities varying from
0.001 to 9 mm/min, while the upper section remains stationary
3. Experimental program (Fig. 2). The apparatus is constructed to ensure minimum frame
distortion during testing. The normal load applied on the upper
3.1. Materials and mix proportions section of the shearing box is provided by a dead weight connected
to a horizontal beam, which in its turn, is connected to a loading
Portland cement conforming to ASTM C150 Type I was used in yoke that applies the normal load on the loading platen of speci-
this project. The Blaine surface area [36] and specific gravity of the men container [24]. The horizontal beam produces a loading ratio
J.J. Assaad et al. / Journal of Non-Newtonian Fluid Mechanics 214 (2014) 18–27 21

Table 1
Cement paste composition for different flowability levels.

w/c HRWR, % of cement VMA, % of cement Flow, mm Fresh unit weight, kg/m3
Paste #1 0.29 0 0 100 2060
Paste #2 0.31 0.1 0 110 2005
Paste #3 0.36 0 0 135 1960
Paste #4 0.4 0 0 160 1910
Paste #5 0.43 0 0 170 1870
Paste #6 0.45 0 0 195 1830
Paste #7 0.48 0 0.15 200 1815
Paste #8 0.5 0.1 0.25 225 1810
Paste #9 0.52 0.15 0.4 235 1785
Paste #10 0.55 0.2 0.6 250 1760

Notes: All pastes contained a fixed amount of set-retarder, i.e. 0.2% of cement.
The flow and unit weight are given within ±10 mm and ±25 kg/m3, respectively.

Table 2
Physical properties of tested PVAs.

Flow, mm Solid content, % Viscosity, Pa s Maximum particle size, lm Specific gravity pH

PVA #1 110 55 1.65 2.5 1.09 4.5
PVA #2 140 53.5 1.13 2.4 1.08 4.5
PVA #3 155 40 0.84 2.75 1.04 4.3
PVA #4 170 34 0.61 2.4 1.05 4.7
PVA #5 200 28 0.37 2.35 1.03 4.6

of 10:1 between the weight hanger and loading platen. The system aligned 10-mm long channels were laser-grooved in the bottom
is fully automated through high precision load cell and LVDT trans- part of the shear box (Fig. 3a). A steel ball having 2.5-mm diameter
ducers to provide real-time control of all loadings and strains tak- was then placed in each channel, thus allowing the lower plate of
ing place during shearing. The maximum load cell capacity is 50 N the shear box to behave like a roller with respect to the upper
having a resolution of 0.01 N. The resulting shear and normal stres- plate. Additionally, the upper plate of the shear box was very
ses were calculated by dividing the horizontal and vertical loads by slightly laser-grooved (Fig. 3b), in order to avoid eventual twisting
the specimen’s cross-sectional area, i.e. 7850 mm2. during movement. The resulting gap between the upper and lower
Several experiments were performed to determine the ‘‘net’’ plates was 10 ± 1 lm. Using this set-up, the ‘‘net’’ shearing force
forces required to overcome friction between the upper and bot- required to overcome friction was reduced to 180 mN (i.e.,
tom plates during shearing. A low-viscosity lubricant oil was 22.9 Pa), and most importantly, its fluctuation reduced to ±40 mN
applied between the plates, and tests were run without any mate- (i.e., 5.1 Pa). The value of 180 mN was systematically removed to
rial being filled in the shear boxes. Shearing forces were relatively obtain the ‘‘net’’ shearing stresses when calculating C. During test-
high and fluctuating within 1.4 ± 0.8 N (i.e., shear stresses of ing, the 10-lm clear opening between the upper and bottom plates
178.3 ± 101.9 Pa), which may lead to erroneous responses espe- was greased, so as to avoid leakage of cement pastes or PVAs
cially when testing materials displaying low yield stresses in the through the gap.
order of a few Pa. The problem of friction between plates is well The C and / parameters are considered being determined under
known when large-size direct shear boxes are used in geotechnical drained conditions, given the non-waterproof design of the shear
investigations, and improvements have been suggested with the box container and poor control of expelled interstitial liquid
use of Teflon rods, rollers, or needle linear bearings [39,40]. [24,19,41]. Two bronze porous stones were used to encase radially
In order to minimize friction and adapt the shearing box to test- the specimen (Fig. 2). Special fiberglass filters capable of retaining
ing flowable materials with relatively low C values, four perfectly all particles greater than 1 lm were provided between the cement
paste or PVA and contact faces of the porous disks. It is to be noted
that the upper porous stone was not placed when tests are realized
without normal load; rather all materials that protruded above the
top surface of the upper shear box plate were cut off to a plane
using a straight edge trowel.
Given that the shear box is divided into two horizontal halves,
the specimen was placed in three approximately equal layers, thus
reducing the risks of void formation within the interfacial region
where failure is expected to occur. The compaction of each layer
was realized by tamping the material depending on its flowability.
Hence, 10 gentle tamps were performed for PVA #1, PVA #2, and
cement pastes possessing flowability lower than around 175 mm.
The shear box was slightly tamped on its exterior surfaces for other
PVAs and cement pastes having more than 175 mm flow. The
cement paste specimens were allowed to rest for 30 s in the shear-
ing box prior to beginning of testing at given displacement rate. At
end of test, the total horizontal displacement of the bottom shear
box varied from 1 to around 3 mm, depending on flowability of
Fig. 2. Set-up for the direct shear test.
tested materials.
22 J.J. Assaad et al. / Journal of Non-Newtonian Fluid Mechanics 214 (2014) 18–27

Fig. 3. Photos for (left) direct shear box, and (right) grooving details in the upper and bottom plates.

3.3. Determination of s0 using the vane method

Anton Paar (RheolabQC) rheometer was used to evaluate s0 of

cement pastes and PVAs. The rheometer’s torque maximum capac-
ity and resolution are 75 and 0.01 mN m, respectively; while its
rotational speed can vary from 0.01 to 1200 rpm. The vane used
consisted of four blades arranged at equal angles around the main
shaft; its height (H) and diameter (D) were 24 and 12 mm, respec-
tively. A cylindrical recipient having 120 mm height and 100 mm
diameter was used for s0 measurements of cement paste and
PVA materials.
Two types of s0 measurements were realized, depending on the
position of the four-bladed vane with respect to tested material. In
the first measurement, the vane was inserted and centered in the
recipient, thus making Z1 = 40 mm (see Fig. 1). In case of cohesive
Fig. 4. Typical torque variations with time for Paste #3 and PVA #2 for different
materials possessing flow less than around 175 mm, special care vane positioning (Z1 = 40 mm or Z1 = 0 mm).
was placed to distribute and level uniformly the specimen above
the vane inserted inside the recipient. In the second measurement,
the top edges of the vane were aligned with the upper material’s materials, the profiles resemble to a large extent those obtained
surface, thus making Z1 = 0 mm. The cement pastes or PVAs were when determining s0 using the vane method. Initially, the shear
stirred manually between both measurements in order to mitigate stress varies almost linearly until reaching a maximum peak value
the formation of preferential shear planes due to particle orienta- indicating failure of bonds. Further horizontal displacement causes
tion. The cement pastes were allowed to rest for 30 s prior to each the stresses to decrease towards a steady state region. As men-
test, given their thixotropic nature that may affect s0 responses tioned earlier, the calculation of C was realized using the net shear
[37]. The total time duration for s0 measurements in both positions stress obtained by subtracting the peak value from 180 mN (due to
did not exceed 10 min after the initial mixing of cement with friction), and dividing by 7850 mm2.
water. Two photos taken right after completion of tests for Paste #1
Shearing was applied at low rotational speed of 0.1 rpm, a value and Paste #2 having flow of 100 and 110 mm, respectively, are
typically recommended in literature [3,4,6,18] and also found ade- given in Fig. 6. As can be seen, the yielding plane is clearly demar-
quate by experimentation for direct s0 measurements. The changes cated horizontally within the suspension, thus reflecting the ‘‘true’’
in rheometer’s torque for various cement pastes and PVAs are nature of the stress that is being measured. It is to be noted that it
recorded as a function of time. As can be seen in Fig. 4, all profiles was difficult to take photos for other tested materials, given that
exhibited an elastic linear region whereby the material resists
shearing, until reaching a maximum torque (Tm) indicating break-
age of majority of bonds and yielding of structure. The magnitude
of Tm decreased when the vane is positioned on the upper mate-
rial’s surface (Z1 = 0 mm), due to reduced stress contribution
resulting from the specimen self-weight. The s0 was calculated
using Tm following Eq. (2) or Eq. (3), depending on the vane’s posi-
tion. Detailed discussion on s0 determination using the vane
method can be seen in other references [such as 1–3,15,17], and
is beyond the scope of this article.

4. Test results and discussion

4.1. Shear stress profiles determined from direct shear test

Typical shear stress vs. horizontal displacement profiles deter-

mined at 0.5 mm/min without normal load for different cement
pastes and PVA #2 are illustrated in Fig. 5. For both types of Fig. 5. Typical shear stress variations with horizontal displacement.
J.J. Assaad et al. / Journal of Non-Newtonian Fluid Mechanics 214 (2014) 18–27 23

the specimen flows along the sides right after removal of the shear-
ing box.

4.2. Determination of appropriate displacement rate

4.2.1. Data obtained from cement pastes

The logarithmic variations of C vs. displacement rate for differ-
ent cement pastes tested without normal load are plotted in Fig. 7.
Regardless of consistency, the data obtained show a minimum in C
responses at displacement rates varying in the range from 0.3 to
0.7 mm/min. For example, when the displacement rate decreases
down to 0.05 mm/min, the C value increases up to 38.5 and
397 Pa for Paste #8 and #3, respectively. The material’s capability
to withstand higher shear stresses at low displacement rates can
Fig. 7. Effect of displacement rate on C values for tested cement pastes.
be related to the fact that the cement paste has enough time to
rebuild its structure and re-orient its particles within the shearing
plane. Hence, for example, a considerable elapsed time of 20–
40 min is required to displace the shear box by 1–2 mm, respec-
tively, at a rate of 0.05 mm/min, whereby cement hydration cou-
pled with significant loss in consistency may occur. Conversely,
speeds higher than around 2 mm/min would rip apart the struc-
tural network bonds and lead to an increase in C values. Such
trends are in complete agreement with those determined using
the vane method by other researchers [6,15]. Thus, at the mini-
mum of C vs. displacement rate curves (Fig. 7), the stress applied
by the direct shear box is just great enough to overcome the restor-
ing forces due to reorientation of particles, thixotropic recovery of
broken bonds, and structural development due to cement hydra-
tion reactions.

4.2.2. Data obtained from PVAs

Fig. 8. Effect of displacement rate on C values for tested PVAs.
The C vs. displacement rate curves obtained for various PVAs
are illustrated in Fig. 8. Unlike cement pastes whose properties
are time-dependent, the C values of PVAs remained almost con- assuming that flow takes place between two parallel planes, one
stant for displacement rates less than around 1 mm/min and vary- moving at constant speed and the other remaining stationary.
ing within the accuracy of testing (see next paragraph). However, Hence, c (in s1) becomes equal to the displacement rate (in
higher speeds led to gradual increases in C as a result of the mate- mm/s) divided by the distance between parallel planes (assumed
rial’s viscous resistance to shearing. to be 0.01 mm). Nevertheless, the over-estimation of viscosity
Based on Figs. 7 and 8, displacement rates varying from 0.3 to determined by direct shearing could mostly be related to the low
0.7 mm/min shall be considered appropriate for determining C of range of shear rates applied that varied up to 14 s1 (Fig. 9). Thus,
cement pastes and PVAs. The entire duration that extends from the use of higher shear rates as well as adequate control of the gap
the filling and compacting the material in the shear box till per- opening between the upper and bottom plates would be needed to
forming the test would not exceed around 10 min. make the direct shear test a reliable viscosity measurement tool.

4.2.3. Determination of PVA viscosity by direct shear 4.3. Evaluation of repeatability of C and s0 responses
It is interesting to note that the PVA viscosity values determined
by coaxial cylinders could be reproduced, to a certain extent, by the In order to evaluate repeatability of testing, the C and s0 mea-
direct shear test. As can be seen in Fig. 9, linear regressions follow- surements were realized 3–5 times (a new cement paste was bat-
ing the Bingham behavior are obtained between the various C val- ched for each test). The coefficient of variation (COV) is calculated
ues and corresponding shear rates (c). The c was determined by as the ratio between standard deviation of responses and their

Fig. 6. Photos of Paste #1 (left) and Paste #3 (right) taken after the materials have been taken out from the direct shear box.
24 J.J. Assaad et al. / Journal of Non-Newtonian Fluid Mechanics 214 (2014) 18–27

250 than around 6% for cement pastes having flow higher than
200 mm and PVA #4 and #5. The COV tended to increase gradually
200 Viscosity, Pa.sec for cohesive materials; the maximum COV of 13.3% corresponded
PVA #1: Coaxial cylinder Direct shear
y = 3.76x + 192.92 PVA #1 1.65 3.76
to Paste #1 having a flow of 100 mm. In fact, homogeneity of cohe-
Shear stress, Pa

R² = 0.95 PVA #2 1.13 1.49 sive materials adjacent to the vane’s blades was remarkably dis-
150 PVA #4 0.61 0.78
turbed when the vane was inserted inside the recipient prior to
shearing. This was visually noticed and believed to create some
PVA #2:
100 y = 1.49x + 112.48 air pockets around and above the vane that can alter shear stresses
R² = 0.89 PVA #4: required to breakdown the structure. The improvement in repeat-
y = 0.78x + 22.82 ability of s0 when the vane is positioned at Z1 = 0 confirms the ear-
50 R² = 0.88
lier statement, as this action reduces disturbance of material prior
to shearing. Hence, for example, the COV decreased from 13.3% at
0 Z1 = 40 mm to 10.4% when the vane was positioned at the upper
0 2 4 6 8 10 12 14 16
Shear rate, sec-1 material’s surface (Z1 = 0 mm).

Fig. 9. Relationships between shear stress vs. shear rate determined on PVAs using
the direct shear test. 4.4. Determination of angle of internal friction, /
mean values, multiplied by 100. Table 3 summarizes all C and s0
A minimum of three tests realized at different normal loads are
along with their COV values (the / values are also reported in
performed to obtain the / values of tested materials (a new batch
Table 3, but will be discussed in Section 4). The relationship
of cement paste was prepared and used for each test). Special
between C and flow is given as: C, Pa = 6277.1  exp[0.026  (flow, mm)]
emphasis was placed to avoid rotation of cover plate that can influ-
with coefficient of correlation (R2) equal to 0.73.
ence the distribution of normal load on top of specimen. In fact, the
contact point of this plate acts like a ball-and-socket around which
4.3.1. Data obtained from direct shear test it can freely rotates, particularly when testing flowable materials.
In general, materials having relatively cohesive nature exhibited This problem is well known in soil mechanics and improvements
adequate repeatability of C responses. Hence, the COV remained have been proposed in literature [42]. In the case of this study,
less than around 6% for cement pastes having flow less than the loading yoke assembly was detached from the system to allow
170 mm and for PVA #1 and #2. The COV increased up to 9% and better control of the squeezing pressure. Light dead weights (i.e., in
14.3% for cement pastes having 225 and 250 mm flow, respec- the order of 200 and 400 g) were used to apply concentrically the
tively. The PVA #4 and #5 resulted in COVs of 11.5% and 15.8%, normal stress on top of specimen. The use of light weights to create
respectively. The adequate repeatability resulting from cohesive the normal loads was found essential to maintain good homogene-
materials could be related to a more uniform distribution of shear ity and reduce bleeding of cement pastes, particularly those pos-
stresses along the failure plane, as can typically be seen in Fig. 6 for sessing flow larger than around 200 mm.
Paste #1 and #2. Conversely, the C responses of relatively flowable Typical shear stress vs. horizontal displacement profiles deter-
materials may become quite sensitive to the distribution of stres- mined at 0.5 mm/min at different normal loads for various materi-
ses as well as various steps implemented during testing including als are illustrated in Fig. 10. For all loadings, the shear stresses vary
the eventual leaking of materials between the upper and lower almost linearly until reaching a maximum peak value indicating
plates. failure of bonds. The increase in peak values with increasing nor-
mal load is caused by higher friction and interlocking of solid par-
4.3.2. Data obtained from vane test ticles during shearing. An approximately linear relationship
Unlike repeatability of C responses, materials possessing flow- following the Mohr–Coulomb theory exists between the maximum
able nature resulted in the lowest COV for s0 that remained less shear resistance and normal stress, as shown in Fig. 11. The C and /

Table 3
Direct shear and vane results – repeatability evaluation.

Flow, mm Direct shear test Vane method

C, Pa COV,a % /, degree Vane position: Z1 = 40 mm Vane position: Z1 = 0 mm
s0 from Eq. (2), Pa COV, % s0 from Eq. (3), Pa COV, %
Paste #1 100 559.5 5.1 7.4 762 13.3 657.2 10.4
Paste #2 110 467.2 4.3 7.2 611.3 n/a 522 n/a
Paste #3 135 326.8 4.4 6.4 466.2 10.7 388.3 n/a
Paste #4 160 197 6.2 6.5 242.7 8 211 6.3
Paste #5 170 168.3 5.8 4.9 183.5 n/a 149.6 n/a
Paste #6 195 91.2 8.3 4.3 133.2 8.1 88.6 7
Paste #7 210 43.5 7.7 4 55 n/a 47.2 n/a
Paste #8 225 26.6 9 3.1 31.9 5.3 23.5 n/a
Paste #9 235 10.1 11.8 2.5 18 3.8 13.9 5.4
Paste #10 250 9.3 14.3 2.4 10.2 5.7 8.6 5.9
PVA #1 110 195.5 4.6 5.5 341.7 9.7 264 7.5
PVA #2 140 111.4 6.2 3.8 172 6 122.1 n/a
PVA #3 155 41.7 8 3.3 62.6 n/a 43 n/a
PVA #4 170 24.2 11.5 2 40.2 6.3 22.6 6
PVA #5 200 6.7 15.8 1.4 11.4 5.5 7 5.8

The reported C and s0 values are averages of 3–5 measurements.

n/a refers to ‘‘not available’’.
COV of direct shear is determined on materials tested without normal load at 0.5 mm/min displacement rate.
J.J. Assaad et al. / Journal of Non-Newtonian Fluid Mechanics 214 (2014) 18–27 25

values are taken as the intercept on shear stress axis and slope of
linear fitting line, respectively.
The relationship between / and flow for all tested materials is
plotted in Fig. 12 (the correlation with C is also plotted). As can
be seen, the amplitude of / increases with decreased flowability;
the maximum value of 7.4° corresponded to the flow of 100 mm.
As concluded by other researchers [32,34], this indicates that the
maximum shear stress is not a material constant, but rather varies
depending on the normal stress applied. It is to be noted that the
range of / values that varied from 2° to 7.4° for cement pastes
(Table 3) is in complete agreement with that found by Lu and
Wang [34]. This reflects the standardized nature of the direct shear
test that could be used to unify characterization of cementitious
Fig. 11. Mohr–Coulomb failure curves for fresh cement pastes.

4.5. Analysis and interpretation of absolute C and s0 values

Given that repeatability of C and s0 responses is differently

affected by flowability, the cement pastes and PVAs were grouped
for analysis purposes into three categories including cohesive,
flowable, and highly flowable (Table 4). For each category, the lin-
ear regression model linking s0 with C values along with resulting
R2 is given. The developed model was forced to intercept the origin
of axis, thus taking the form s0 = A C, where A is the coefficient of
proportionality. Also, the root-mean square error (RMSE) that is
an indicator of the residual size or spread around the regression
model is given in Table 4. The normalized RMSE (NRMSE), in per-
cent, calculated as the ratio between RMSE and range of s0 values
(i.e., maximum minus minimum value) can be used as an index to
reflect the accuracy of the relationship. A NRMSE value of 0% indi-
cates a perfect model, whereas a value of 100% indicates that the
model is inaccurate. Fig. 12. Relationships between / with respect to flow and C values for all tested

4.5.1. Effect of vane positioning on s0 measurements

High R2 values greater than 0.95 are obtained for all categories;
To better interpret such variations, a series of s0 measurements
albeit the A-coefficients are affected by the vane positioning and
determined on cement pastes and PVAs were realized while posi-
flow level. For example, when the vane was positioned at
tioning the vane at Z1 = 20 mm and then Z1 = 60 mm (Fig. 13).
Z1 = 40 mm, the s0 determined on materials possessing cohesive
The s0 computed using Eq. (2) clearly shows that yield stress
nature was considerably higher than C (i.e., the A-coefficient is
increases with increasing Z1. This concludes that positioning the
1.38). The A decreased to 1.21 and 1.27 for materials possessing
vane at Z1 = 0 mm has the advantage of substantially reducing
flowable and highly flowable nature, respectively, at Z1 = 40 mm.
the contribution of normal stresses on torque measurements, thus
Conversely, the effect of positioning the top edges of the blades
resulting in closer absolute values between s0 and C. In other
vane aligned with the upper material’s surface (Z1 = 0 mm)
words, this indicates that the common approach that consists on
resulted in a net decrease in A-coefficients (Table 4). For example,
inserting the vane inside the material tends to over-estimate s0,
such decrease was equal to 0.99 and 1.04 for flowable and highly
particularly for cohesive cement pastes possessing the highest bulk
flowable materials, respectively.
unit weights (Table 1). The variations of / values with flow plotted
in Fig. 12 corroborate this statement; the lower the flow, the higher
is the influence of normal stresses on the shear stresses. Such
results are in complete agreement with Fall et al. [43] who
reported that yield stress can be ascribed to the frictional behavior
of the granular matrix under normal stresses due to gravity, and
depends on the difference between densities of solid particles
and surrounding liquid. Lu and Wang [34] reported that the stres-
ses potentially affecting measurements conducted by the vane
method may be due to the specimen self-weight located above
the shearing zone or any confining stress created from the vane
boundaries in the rheometer device.
The relationships between s0 and normal stress measured from
top surface of specimen to mid-point of the 24-mm high vane for
Paste #3, #5, #8, and PVA #2 are shown in Fig. 14. The normal
stress was calculated as the ratio between the load (i.e., volume
of cylindrical-shaped material located from top surface to mid-
Fig. 10. Effect of normal stress on variations of shear stresses determined using the
height of vane  density  gravity acceleration) divided by the cir-
direct shear test. cular surface area defined by the tips of the vane blade. Clearly, s0
26 J.J. Assaad et al. / Journal of Non-Newtonian Fluid Mechanics 214 (2014) 18–27

Table 4
Comparison between C and s0 absolute values.

Materials included in comparison Vane position: Z1 = 40 mm Vane position: Z1 = 0 mm

Cohesive materials: flow of 100–150 mm Paste #1 A-coefficient 1.38 1.17
Paste #2 R2 0.97 0.98
Paste #3 RMSE, Pa 31.92 23.76
PVA #1 Range of s0, Pa 590 535.1
PVA #2 NRMSE, % 5.4 4.4
Flowable materials: flow of 150–200 mm Paste #4 A-coefficient 1.21 0.99
Paste #5 R2 0.95 0.98
Paste #6 RMSE, Pa 15.13 13.46
PVA #3 Range of s0, Pa 202.5 188.4
PVA #4 NRMSE, % 7.47 7.14
Highly flowable materials: flow of 200–250 mm Paste #7 A-coefficient 1.27 1.04
Paste #8 R2 0.97 0.97
Paste #9 RMSE, Pa 3.15 3.36
Paste #10 Range of s0, Pa 43.6 40.2
PVA #5 NRMSE, % 7.23 8.35

between the rate of change of s0 with normal stress with respect

to / for the various cement pastes is given in Eq. (5).
¼ 2:99/  9:15 R2 ¼ 0:93 ð5Þ
dNormal stress

4.5.2. Evaluation of accuracy of relationships

The effect of vane positioning (Z1 = 40 mm vs. 0 mm) did not
considerably influence the RMSE values calculated for flowable
and highly flowable materials (Table 4), reflecting limited spread
of responses around the regression model. Nevertheless, the RMSE
varied remarkably from 31.92 to 23.76 Pa for cohesive materials
tested when the vane was positioned at Z1 = 40 or 0 mm, respec-
tively. Physically, this indicates that the vane insertion inside cohe-
Fig. 13. Effect of vane positioning, or Z1, on s0 calculated using Eq. (2).
sive material leads to higher spread of data.
The NRMSE of all tested categories was less than around 8%,
increases linearly with normal stress following the Mohr–Coulomb reflecting high accuracy of relationships established between s0
empirical equation; y = ax + b where ‘‘a’’ represents the slope of and C. However, in general, the NRMSE tended to increase when
relationship and ‘‘b’’ the yield stress that intersects the y-axis at evaluating responses of materials exhibiting higher flowability lev-
zero normal stress. It is interesting to note that the slope of rela- els. For example, the NRMSE increased from 4.4% to 7.14% and
tionships roughly coincides with the / values determined from 8.35% for cohesive, flowable, and highly flowable materials, respec-
direct shear test. For example, the slopes varied from 10.8° to 4° tively, when Z1 = 0 mm. This can numerically be explained by the
and 0.8° for Paste #3, #5, and #8, respectively; while the corre- relatively increased range of s0 values of cohesive materials,
sponding / was found equal to 6.4°, 4.9°, and 3.1°, respectively. thereby reducing the NRMSE ratio.
The wider range of values obtained from the vane test may reflect
increased sensitivity to the effective hydrostatic stress in the 5. Summary and conclusions
matrix of solid particles that depends on the difference between
densities of particles and surrounding liquid [43]. The correlation This paper does not aim at substituting the vane method by
direct shear test, especially knowing that the vane method is
widely used, simple, and versatile. Rather, the paper seeks to eval-
uate the suitability of direct shear to determine s0 which could
possibly makes it a referee test to, for instance, unify quantification
of yield stress or validate constitutive models intended for yield
behavior of materials. Other potential applications of the direct
shear may include the evaluation/validation of the vane shapes
(such as four, six, or eight blades, slotted or not) and dimensions
(H, D, and ratio H/D) on s0 responses. Special emphasis was placed
throughout the paper to eliminate friction between shear boxes,
thus allowing the measurement of the full flowability spectrum
with C values ranging from kPa to just a few Pa.
Test results showed that the shear stress vs. horizontal displace-
ment profiles required for determining C resemble to a large extent
those obtained when determining s0 using the vane method. Dis-
placement rates varying from 0.3 to 0.7 mm/min were found ade-
quate during testing. The maximum shear stress, however, is not a
Fig. 14. Relationships between s0 and normal stress calculated from top of material constant but rather varies depending on the rate of nor-
specimen to mid-height of vane. mal stress applied. Adequate repeatability of C responses was
J.J. Assaad et al. / Journal of Non-Newtonian Fluid Mechanics 214 (2014) 18–27 27

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