Rheol Acta (2012) 51:603–607
DOI 10.1007/s00397-012-0627-9
ORIGINAL CONTRIBUTION
Experimental study on yield behavior of Daqing crude oil
Lei Hou
Received: 4 October 2011 / Revised: 27 January 2012 / Accepted: 16 March 2012 / Published online: 1 April 2012
© Springer-Verlag 2012
Abstract The yield behavior of Daqing crude oil was
studied by means of multi-mode controlled-stress tests
with a high-precision stress controlled rheometer. Two
experiments of creep and constant stress loading rate
were performed. The yield stress of gelled crude oil
was dependent on the test conditions such as the stress
loading time and the stress loading rate, but the yield
strain did not change with test conditions. The yield
strain did exist objectively and it can be used as the
criterion for the yielding of the structure of gelled crude
oil. The yield strain of gelled oil was studied through
experiments of creep, constant stress loading rate, os-
cillatory shear stress increase, and constant shear rate.
The yield strain of gelled crude oil decreased with the
increasing gel strength. The experiment of constant
speed increase of stress showed the strain softening
phenomena for low gel strength oil.
Keywords Waxy crude oil · Yield behavior · Creep ·
Stress increase · Constant shear rate
Introduction
When the waxy crude temperature is below the wax
appearance temperature (WAT), wax crystals separate
out from oil solution. If being continually cooled, more
and more waxy crystals appear and interlock to form a
network, which entraps the liquid oil, resulting in the
gelation of crude oil. The wax contained in crude oil
L. Hou (B)
College of Mechanical and Transportation Engineering,
China University of Petroleum, Beijing 102249, China
e-mail: houleicup@126.com
imparts various complex non-Newtonian and nonlinear
characteristics to the flow properties, including yield
stress, viscoelasticity, and thixotropy. Yield behavior,
as one of the most important rheological behaviors of
non-Newtonian fluid, can characterize the gel strength
of waxy crude oil. The study of yield behavior of waxy
crude oil contributes to the comprehensive and system-
atical understanding of rheological behavior of crude
oil, meanwhile, has practical significance for the flow
assurance of oil transportation (Barnes 1999; Hénaut
et al. 1999; Yang 2006; Zhang and Ma 2004). In 1919,
Bingham and Green proposed the yield stress concept
for the viscoplastic fluid (Bingham and Green 1919).
After that, many models describing the relation of
shear stress and shear rate for viscoplastic materials
were proposed, in which the yield stress was defined
as the minimum shear stress for the occurrence of flow
portent. It is actually the dynamic yield stress being
commonly used now. In 1958, Houwink et al. proposed
that there are two kinds of yield stress, corresponding
to the end of elasticity and the appearance of viscosity.
With the progress of experimental techniques, there
is growing recognition that although the material is
subjected to the shear stress below the so-called yield
stress, it still undergoes slow, continuous and steady
deformation. Therefore, some scholars believed that
yield stress does not exist as the real material prop-
erty and even asserted that the yield stress itself is a
myth. In 1990, Kraynik proposed three yield stresses
to characterize rheological behavior of electrorheolog-
ical fluid, which are elastic limit yield stress, static
yield stress and dynamic yield stress. In 1998, Chang
et al. studied the yield behavior of waxy crude oil at
low temperature with the controlled-stress rheometer
Carri-Med CSL 100, and divided the yielding process
604
into three stages: initial elastic response, viscoelastic
creep, and final fracture (Chang et al. 1998). In 1999,
the yield behavior of Xinjiang crude oil was studied
by creep and stress increase test with the controlled-
stress rheometer RS75, and proposed that the gelled
oil began to yield as long as the strain increased to
the critical yield strain under any shear stress loading
conditions (Li and Shi 2001). However, this conclusion
is only based on the experiment of Xinjiang crude oil,
needing further verification of other crude oils. To sum
up, no systematic studies on the strain change under
various kinds of shear stress loading conditions have
been conducted. The problem for critical yield strain
is still obscure and there is no research for the rela-
tionship between the critical yield stress and structural
strength of waxy crude (Wardhaugh and Boger 1991;
Moussa et al. 2004; Chang et al. 2000). In this paper,
the yield behavior for waxy crude oil was systematically
investigated through experiments of several controlled-
stress modes including creep, constant speed increase
of stress, oscillatory shear stress increase, and constant
shear rate.
Experimental section
A crude oil is essentially a very complex mixture
formed by hydrocarbons of paraffinic, naphthenic, and
aromatic type, but there are also other organic com-
pounds containing sulfur, oxygen, nickel, iron, and cop-
per. Nowadays it is impossible to exactly know the
composition and the fraction of each component. How-
ever, a consensus had been reached that a network of
plate, needle or malformed crystals is responsible for
the non-Newtonian behavior including the yielding and
recovery after yielding. This study was performed by
phenomenological method.
Oil specimen and apparatus
The oil specimens were sampled from Daqing oil field.
It had a wax content of 24.37% and a WAT of 42.13◦ C.
Its gel point was 32◦ C at the heat treatment tempera-
ture of 45◦ C.
The rheological properties of waxy crude oil are
influenced by many factors. To ensure the repeatability
and comparability of test data, the experiment condi-
tion must be controlled strictly. The oil specimens were
pretreated to eliminate the memory effect for the ther-
mal and shear history. First, the oil samples in sealed
bottles were heated quiescently to 80◦ C in water bath.
After having been kept at this temperature for 2 h to
become homogeneous due to thermal diffusion, the oil
Rheol Acta (2012) 51:603–607
samples were statically held at the room temperature
for 48 h (Luo 1991).
The yield experiments were conducted by a
controlled-stress rheometer RSH150 with a coaxial
cylinder test system Z41Ti (HAAKE Corporation,
Karlsruhe, Germany). This controlled-stress rheometer
was equipped with a program-controlled water bath
C35 (HAAKE Corporation, Karlsruhe, Germany) with
a temperature resolution of 0.1◦ C.
Experimental method
(1) Creep. The oil specimens were loaded to the
rheometer at 45◦ C, being higher than the WAT.
After having been held undisturbed for 15 min to
make the inside temperature fully uniform, the oil
specimens were cooled to different test tempera-
tures at a cooling rate of 0.5◦ C/min. Then the oil
specimens were statically kept at the test temper-
ature for 30 min to make the oil gel adequately.
For an oil specimen at a definite temperature, the
different shear stresses were loaded in a definite
time. The curves of the strain with the loading
time were measured, being called the creep curve.
(2) Constant stress loading rate. The oil specimens
were loaded to the rheometer at 50◦ C, being
higher than the WAT. After having been held
undisturbed for 15 min to make the inside temper-
ature fully uniform, the oil specimens were cooled
to different test temperatures at a cooling rate of
0.5◦ C/min. Then the oil specimens were statically
kept at the test temperature for 30 min to make
the oil gel adequately. For an oil specimen at a
definite temperature, the shear stress was loaded
at a constant stress loading rate. The curves of the
strain with the loading time were measured.
(3) Oscillatory shear stress increase. The oil spec-
imens were loaded to the rheometer at 45◦ C,
being higher than the WAT. After having been
held undisturbed for 15 min to make the inside
temperature fully uniform, the oil specimens were
cooled to different test temperatures at a cooling
rate of 0.5◦ C/min. Then, the oil specimens were
statically kept at the test temperature for 30 min to
make the oil gel adequately. The specimens were
tested in oscillation amplitude sweep mode; the
changes of viscoelastic parameters and strain with
the stress loading time were measured.
(4) Constant shear rate. The oil specimens were
loaded to the rheometer at 45◦ C, being higher
than the WAT. After having been held undis-
turbed for 15 min to make the inside temperature
fully uniform, the oil specimens were cooled to
Rheol Acta (2012) 51:603–607 605

different test temperatures at a cooling rate of 10000

2Pa/min
0.5◦ C/min. Then, the oil specimens were statically 1000
100 5Pa/min
kept at the test temperature for 30 min. The spec-
imens were sheared at a constant shear rate of 10 15Pa/min
0.3 s−1 and the curves of strain with time were 1

strain
40Pa/min
measured. 0.1
0.01
0.001

Results and analyses 0.0001

0.00001
0 10 20 30 40 50 60 70 80
Yield behavior for creep test stress (Pa)

Different shear stresses were applied to the oil spec-
imens within 10 min at 28◦ C, 29◦ C, 30◦ C, and 31◦ C,
respectively. The creep curves of crude oil at 29◦ C are
shown in Fig. 1. The results showed are as follows:
(1) The yield stress of crude oil not only has direct
relation with gel strength but also depends on
the test condition, such as the creep time. This is
owing to the fact that the creep of crude oil is a
time process. Even under a small shear stress, as
long as loading time is long enough, the crude oil
can still reach the critical yield strain. For the oil
specimen at 28◦ C, the yield stresses are 100 Pa and
97 Pa corresponding to the loading time of 90 s
and 876 s, respectively.
(2) The yield strain changes a little with the shear
stress for the gelled crude of same gel strength.
For example, the yield strain is somewhere around
0.085 under shear stresses of 97 Pa and 100 Pa
at 28◦ C. While for the oil specimen at 29◦ C, the
yield strain is near 0.095 under shear stresses of
45 Pa, 50 Pa and 60 Pa, respectively. Then, the
yield strain is thought the same for the same gel
Fig. 2 Variation of yield strain with shear stress for Daqing
crude oil at 31◦ C
strength of gelled crude oil and can be used as a
criterion for the occurrence of yielding.
(3) The lower the temperature, the higher the gel
strength and the smaller the yield strain is. This
shows that the flexibility of crude oil decreases
with the increase of gel strength. The yield strains
are 0.086, 0.095, 0.148 and 0.172 at the tempera-
ture of 28◦ C, 29◦ C, 30◦ C and 31◦ C, respectively.
Yield behavior for constant stress loading rate test
The curves of strain with shear stress at 30◦ C, 31◦ C,
and 35◦ C were measured at different increasing speeds
of shear stress. Figures 2 and 3 respectively show the
change of strain with shear stress at 31◦ C and 35◦ C.
Figure 4 shows the variation of yield stress with stress
loading rate at 30◦ C, 31◦ C, 35◦ C. The results showed
are as follows:
(1) The yield stress increases with the increasing
gel strength. The gel strength increases as the

100000
10000
10000
1000
1000
100
100
10
strain

strain

10 60Pa
50Pa 1
1 45Pa
0.1
2Pa/min
0.1 0.01 5Pa/min
0.01 0.001 10Pa/min
0.001 0.0001
0 20 40 60 80 100 120 0 1 2 3 4 5 6 7
loading time (s) stress (Pa)

Fig. 1 Creep curves of Daqing crude oil at 29◦ C under different Fig. 3 Variation of strain with shear stress for Daqing crude oil
shear stresses at 35◦ C
606 Rheol Acta (2012) 51:603–607

100 0.2 90
80
yield stress (Pa)
80 30 ºC 70

Loss angle (˚ )
0.15
31 ºC Strain 60

Strain
60 35 ºC Loss angle 50
0.1
40
40 30
0.05 20
20 10
0 0
0 0.1 1 10 100
0 5 10 15 20 25 30 35 40 45
Stress (Pa)
stress loading rate (Pa/min)
Fig. 6 Variation of strain and loss angle of Daqing crude oil at
Fig. 4 Variation of yield stress with stress loading rate 30◦ C with oscillatory shear stress amplitude

temperature decreases, while the yield stress at

Yield behavior for oscillatory shear stress increase test
30◦ C, 31◦ C and 35◦ C is 70.54 Pa, 40.44 Pa, 5.36 Pa,
respectively.
Figure 5 shows the change of viscoelastic parameters
(2) The yield stress depends on the stress loading rate.
with the amplitude of oscillatory shear stress for Daqing
For the same crude oil, the yield stress increases
crude oil at 30◦ C. When the amplitude is between 0.1
with the increasing speed of shear stress. The yield
and 10 Pa, the viscoelastic parameters are almost the
stress at 30◦ C increases from 65.42 Pa to 95.13 Pa
same. The storage modulus, loss modulus, and loss an-
as the stress loading rate is increased from 2 to
gle are about 2050 Pa, 430 Pa, 11◦ respectively, showing
40 Pa/min.
the waxy structure is not destroyed by the shear stress
(3) When the gel strength of gelled crude oil is rel-
and the viscous property exceeds the elastic property.
atively low, the strain increases with the increas-
When the amplitude is between 10 and 18.5 Pa, the
ing shear stress until the oil begins to yield. Af-
storage modulus and loss modulus decrease with the
ter that, the stress decreases with the increased
increase of the stress amplitude, while the loss angle
strain which is being called as the strain softening
increases with the increase of the stress amplitude,
(Ma et al. 1995). As the strain softening reaches
showing the creep property. As the stress amplitude
to a certain level, the stress begins to increase
increases beyond 18.5 Pa, the storage modulus and loss
again with the strain, which being called the strain
modulus sharply decreases, with the storage modulus
strengthening. This phenomenon occurred for the
more sharply than the storage modulus, resulting in the
oil at 35◦ C.
sharp increase of loss angle, which shows that the vis-
(4) The yield strains are the same for the gelled crudes
cous property progressively excel the elastic property
with the same gel strength, regardless of the stress
and the crude oil yields.
loading rate. As can be seen from Fig. 2, the yield
Figure 6 shows the variation of strain and loss angle
strains of crude oils at 31◦ C are always near 0.1
with the amplitude of oscillatory shear stress for Daqing
at the stress loading rates of 2, 5, 15, 40 Pa/min.
crude oil at 30◦ C. The amplitudes of oscillation shear
The yield strain decreases with the increase of
stress are the same corresponding to the sharp increase
gel strength of crude oil. For the oil specimens
of strain and loss angle. It can be concluded that the
at 30◦ C, 31◦ C, and 35◦ C, the yield strains are
yield stress can be determined by the loss angle varia-
respectively 0.06, 0.1, and 1.
tion with the amplitude of oscillatory shear stress.

10000 90
80
120 1.4
70
Loss angle (˚ )

1000
Modulus (Pa)

1.2
yield stress (Pa)

60 100
yield strain

50 80 1
100 Storage modulus 0.8
40 60
loss modulus 0.6
Loss angle 30
10 40 yield stress
0.4
20 yield strain
10 20 0.2
1 0 0 0
0.1 1 10 100 26 28 30 32 34 36
Stress (Pa) temperature (ºC)

Fig. 5 Variation of viscoelasic parameters of Daqing crude oil at Fig. 7 Yield stress and yield strain tested by constant shear rate
30◦ C with oscillatory shear stress amplitude method
Rheol Acta (2012) 51:603–607
Yield behavior for constant shear rate test
Figure 7 shows the yield strain and yield stress of gelled
crude oil at different temperatures. The results show
that the yield strain decreases with the increasing yield
stress. For example, the yield stress and yield strain are
56.41 Pa and 0.172 at 29◦ C, while the yield stress and
yield strain are 9.70 Pa and 0.589 at 32◦ C.
Conclusion
1. The yielding property of gelled crude oil was stud-
ied by the tests of creep and constant stress load-
ing rate. It can be concluded that the yield stress
depends on the measuring conditions, such as the
stress loading time and the stress loading rate, but
the yield strain does not change with the measuring
conditions, which further verifies the existence of
yield strain. Therefore, the yield strain can be used
as a criterion for the crude oil yielding.
2. The yield strain was studied through experiments
of creep, constant stress loading rate, oscillatory
shear stress increase, and constant shear rate. The
yield strain of gelled crude oil decreased with the
increasing gel strength.
3. The experiments of constant stress loading rate
showed that for the crude oil with low gel strength,
the stress decreases with the increased strain after
yielding and increases with the increased strain as
the strain reaches a certain level.
607
Acknowledgement Support from general program of the
National Natural Science Foundation of China (No. 51174218)
is greatly acknowledged.
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