Journal of Petroleum Science and Engineering 77 (2011) 286–304

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Journal of Petroleum Science and Engineering

j o u r n a l h o m e p a g e : w w w. e l s ev i e r. c o m / l o c a t e / p e t r o l

Novel approaches to waxy crude restart: Part 2: An investigation of flow events

following shut down
David A. Phillips a,⁎, Ivor N. Forsdyke a, Ian R. McCracken b, Paul D. Ravenscroft b
a
Kernow Analytical Technology Ltd, North Petherwin, Cornwall PL15 8TE, United Kingdom
b
BP Exploration Operating Company Ltd, Sunbury on Thames, Middlesex TW16 7LN, United Kingdom

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

Article history: This paper describes cooling-induced flow events following the shut-in of waxy fluids in a transparent model
Received 19 August 2009 pipeline. Flow, indicated by entrained marker spheres, and gel fracture and fragmentation, are recorded by
Accepted 6 April 2011 digital photography. Pressure changes during cooling were also recorded. The observed flow events and
Available online 13 April 2011
pressure changes are consistent with numerical simulations of shrinkage flow. The test results show
comparability with previously reported observations obtained with steel model pipelines. Numerical
Keywords:
waxy crude oil
simulations of shrinkage in pipes are presented as comparative examples. The paper also reports predicted
pipeline restart and experimental results for shrinkage of a wax-free high viscosity Newtonian standard fluid in a steel model
shrinkage flow pipeline, which indicate that gradients of reducing pressure are a general phenomenon associated with high
pressure gradients flow resistance during cooling in pipes. The findings reported in this paper represent part of an ongoing
void formation investigation into aspects of waxy crude restart that may lead to predictive inaccuracy.
numerical simulation © 2011 Elsevier B.V. All rights reserved.

1. Introduction
Gradients of reducing pressure that develop during cooling of
waxy crude oil and condensates in steel model pipelines were
reported in Part 1 in this series (Phillips et al., in press). Such gradients
were postulated to be the result of fluid resistance to true (non-affine)
flow, in response to reducing specific volume engendered by
molecular cohesion. In addition, it was suggested that such shrinkage
flow might be interrupted by the formation of vapour-filled voidspace
at any location where the pressure reduced to the level of the liquid/
gel saturation vapour pressure (SVP). The accepted relationship of
changing specific volume with cooling (net of the change in pipe
volume) during a given time step, formed the basis of numerical
calculation of shrinkage flow. It was assumed that in most all field
pipelines, that gravity will direct such flow and ensure that the fluid/
gel remains in contact with the pipewall. It was further assumed that
this flow is laminar and that widely used descriptions of flow (such as
Hagen–Poiseuille) could thus relate the flow rate, the ratio of pipe
length to diameter (L/D ratio) and the fluid flow resistance (apparent
viscosity), so as to derive a proportional induced pressure gradient.
Shrinkage flow was deemed to differ from normal pipeflow in that:
1. Flow is induced by the fluid itself (molecular cohesion) rather than
by an externally impressed pressure gradient; (the action of gravity
supports and directs the flow but does not induce it).
DOI of original article: 10.1016/j.petrol.2010.11.009.
⁎ Corresponding author at: Kernow Analytical Technology Ltd, Rural Workshops,
North Petherwin, Cornwall PL15 8TE, United Kingdom. Tel.: + 44 1566 785778.
2. Flow rate in a given line section, varies from a maximum (usually at
the line high point) to zero at a shrinkage null.
3. In lines of complex topography, shrinkage flow may occur in
opposing axial directions with multiple shrinkage nulls.
The implications of this shrinkage flow were discussed, particu-
larly with respect to shear-induced changes in the liquid/gel state and
it was suggested that such changes, together with any voidspace
formation, were in accord with the gel auto-destruction process
postulated by Gill and Russell, 1954. An example calculation for a field
pipeline was presented, indicating a marked variation in liquid/gel
state along the line length. Emphasis was given to the conclusion, that
for a given fluid and cooling regime, the sample aspect ratio (L/D ratio
for a pipe) dictates the rate of flow and hence the extent of the shear-
induced disruption. Shrinkage shearing will therefore be minimal in
samples used for rotational rheometry but significant in model
pipeline tests; while the greatest effect is likely in field pipelines.
Similarly, void creation within the liquid/gel body is unlikely in
rotational rheometry samples but may well occur in pipelines.
The possibility of interstitial flow of liquid continuous phase as
permeation through a more or less static solid wax matrix was
considered, as was the likelihood of some form of slip at or near the
pipewall. These and other issues, such as change in gel compressibil-
ity, are further discussed below in relation to the experimental
observations presented in this paper.
Experimental evidence previously presented in support of these
postulates was mainly indirect, in the form of pressure measurements
obtained with two steel model pipelines, one of 5.9 mm ID and the
other of 12.7 mm ID. Each line is 15.24 m long and fitted with

0920-4105/$ – see front matter © 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.petrol.2011.04.003
 D.A. Phillips et al. / Journal of Petroleum Science and Engineering 77 (2011) 286–304
differential pressure transducers at 1.9 m intervals from inlet to outlet
valves. Test results were described showing pressure change during
the ‘static’ cooling of waxy fluids in various configurations of pipeline
valve closure and when a modest elevation head was added by way of
a 3.3 m vertical extension. It was particularly noted that gradients of
reducing pressure (as partial vacua) could be sustained even though
one or both ends of the pipe were open to atmosphere.
In this paper, we report similar tests performed in a transparent
model pipeline that allows visualization of test fluids. Cooling-
induced flow is demonstrated by means of marker spheres entrained
within the fluid column and this flow can be related to pressure
gradients recorded during the cooling tests. These tests were intended
to challenge the validity of the shrinkage flow postulates, including
the fracturing of highly viscous oil/gels and the resultant formation of
voidspace.
As a further test of validity, a high viscosity, wax-free Newtonian
standard fluid (N5100) was cooled in the 5.9 mm ID multiport steel
pipeline with the valve at one end closed and the other end open to
atmosphere and a 0.1 m elevation head. The flow at the open end was
recorded, as were the pressure gradients. These observations were
then compared with the flow rate and pressure changes predicted by
numerical simulation. The purpose of this test was to provide a key
baseline demonstration in support of the following propositions for
the stated pipe configuration:
1. The development of gradients of reducing pressure are a general
property of flowable media, dependent upon the rate and extent of
cooling, the pipe L/D ratio and the apparent resistance to flow.
2. Given a simple, single-phase Newtonian liquid where viscosity
varies only with temperature and a consequent absence of shear-
rate dependent variation or wall depletion effects, then the axial
distribution of reducing pressure takes a characteristic, numerically
predictable form that provides a reference for comparison with
more complex fluids such as waxy oils.
That temperature dependent flow in pipes is a reality is evident in
any liquid-in-glass thermometer. If the high viscosity Newtonian fluid
demonstrates viscosity dependent pressure gradients during cooling,
then this provides strong support for the premise that such gradients
observed during cooling of waxy fluids are also the consequence of
high flow resistance and thus provide an indication of the flow
characteristics of that fluid.
2. Materials and methods
2.1. The glass model pipeline
A transparent model pipeline of 10 m overall length was
constructed. Five lengths of borosilicate glass tube, each 1.5 m long
by 6 mm ID and one length of 0.5 m were supported at their ends in
machined acetal blocks. These blocks also supported 0.1 m OD clear
extruded acrylic tubes surrounding each length of glass, to create
cooling jackets. The respective tubes were sealed into the end blocks
with O-rings and seven blocks were machined with ports for pressure
transducers. These six glass tube sections were connected by flexible
Tygon high pressure tube of 6.4 mm ID and 4.8 mm wall thickness.
The outer coolant chambers were each coupled with three parallel
lengths of flexible reinforced PVC tube to minimise restriction of
coolant flow. The flexible couplings were of variable length to allow a
compact overall layout, and also allow the raising of individual
sections to enable gravity assisted flow. These couplings were
insulated with flexible padding but the rest of the rig length was
uninsulated. A schematic of the rig layout in raised-end configuration
is shown in Fig. 1.
The 10 m line length was chosen as a compromise between
complexity of construction and the need for sufficiently high L/D ratio
to attain acceptable shrinkage flow rate and pressure change. The
287
Valve
P1
P2
Pressure
transducer Acetal cap
P7 P6
P3
P4 P5
Tygon coupling tube Glass tube Acrylic tube
Fig. 1. Schematic of glass pipeline showing two sections raised to give a total 2.33 m
head. The other four sections (from P3 to P7) are horizontal.
flexible couplings between the pipe sections were successful in
allowing easy re-configuration but we suspect that this flexibility and
the overall asymmetry of the rig, may have contributed an undesirable
distortion of the test results.
The need for visibility required that the coolant jackets remain
uninsulated. By using a high throughput centrifugal coolant pump, the
in–out temperature drop was limited to b1 °C, but despite using an
8 kW chiller, the maximum attainable cooling rate was limited to ca.
20 °C/h and was non-linear as indicated in Table 1. Numerical
simulation indicates that faster cooling causes more pronounced
pressure gradients, however, the much slower rate of cooling (mean
7.8 °C/h) used in the third example, proved sufficient to induce
measurable gradients.
Four primary tests were planned so as to approximately repeat the
test configurations previously reported using the steel model
pipelines:
1. In Test 1, the line is horizontal with one end closed and the other
open to atmosphere. In the equivalent test reported for the steel
model pipeline, the pressure falls toward the closed end creating a
gradient of partial vacuum. Flow is postulated in a single direction
toward a shrinkage null close to the closed valve. This configuration
is common to many model pipeline test protocols.
2. In the glass pipeline Test 2, both ends are closed but a significant
elevation head is created by a riser configuration as indicated in
Fig. 1. The postulate, based on the equivalent reported steel
pipeline test, is that the action of gravity will direct and support
shrinkage flow in a single direction toward the lower closed valve,
where the lowest pressure will develop. The highest pressure is
expected at the base of the riser. This combination of closed valves
and a significant elevation head represents the usual field pipeline
case.
3. In the glass line Test 3, both valves are open to atmosphere and the
line is in horizontal configuration. The corresponding reported test
in the steel model pipeline recorded a pressure minimum close to
the axial centre, thus creating two opposing gradients from this
minimum toward each open end. Shrinkage flow is postulated in
two opposed directions; from each open end toward a null point
close to the longitudinal centre.
4. For Test 4, the glass line was horizontal with both valves closed.
The equivalent reported test in the steel line indicated reduced
pressure with cooling but little longitudinal variation — no
significant pressure gradients. Our numerical simulation method
288 D.A. Phillips et al. / Journal of Petroleum Science and Engineering 77 (2011) 286–304

Table 1 very low. A further problem with this fluid was the very rapid onset of
The calculated cooling rates, the movement of the entrained Sphere A and the high flow resistance within a very narrow temperature range (b2 °C
calculated maximum liquid/gel velocity in the glass pipeline.
below the gelation point). While this property was helpful in
Time Temperature Step interval Mean rate of encouraging the formation of voids, the resultant disruption of
(min) (°C) temperature cooling shrinkage flow limited the opportunity for observation of flow events
(°C) (°C min−1)
below the gel point when cooled at the highest rate. In attempting to
0 54 ameliorate these difficulties, it was found that by loading this fluid at
57 29 25 0.4386
38 °C and cooling more slowly, that useful observations were possible,
75 24 5 0.0667
90 20.5 3.5 0.0389 as in Test 3.
110 18 2.5 0.0227 The proposed numerical simulation method clearly indicates the
likely formation of voids at sites of low pressure and also allows
Time Mean step Sphere Sphere velocity Maximum
calculation of the resultant changes in shrinkage flow. However, in
(min) temperature movement (10−6 m s−1) velocity
(°C) (mm) (10−6 m s−1) addition to visualizing void formation, the glass line test program was
also intended to approximately emulate the previously reported tests
0
57 41.5 141 41.13 46.85
using black oils (Fluid 1 and Fluid 2 in Appendix A) loaded at
75 26.5 6 1.333 1.515 temperatures well above their respective wax appearance tempera-
90 22.25 3 0.555 0.631 tures and cooled to below the corresponding observable gelation
110 19.25 2 0.303 0.344 points. We therefore attempted to modify the behaviour of the
condensate by preparing an artificial variant of this fluid, adding 20%
vol/vol of high viscosity Newtonian standard oil (N190000 —
requires that an axially directed asymmetry exists so as to establish Appendix A) to the condensate to create a model fluid (Fluid 8). The
a flow direction — the result of gravity-induced elevation head in resultant viscosity increase effectively eliminated sphere flow by-pass
the case of field pipelines and some model pipeline tests, or at higher temperatures such that adequately accurate sphere
exposure to atmospheric pressure in other model pipeline tests. In placement was possible. While the wax appearance temperature
the case of a strictly horizontal line that is sealed by end valves and was unchanged, the viscosity increase raised the visible gelation
has insignificant asymmetry with respect to bends, couplings or temperature to ca. 28 °C. The rapidity of gel strength development
other discontinuities, then for a homogeneous substance, the was apparently reduced such that void onset was delayed until 18 °C
isotropic tensile forces of molecular cohesion that cause shrinkage in Test 1 and apparently absent in Test 2 (at the lowest test
will tend to produce uniform proportional dimensional stresses temperature of 25 °C). This model fluid was also used in Test 4.
with respect to the radial and longitudinal axes. Such stresses The primary purposes of these glass line tests were:
would tend to induce isometric change as in an equivalent, isolated
solid cylinder for example. In the case of flowable media initially 1. To establish whether or not that, despite the differences in fluid/gel
filling and sealed within a rigid pipe of lower thermal expansivity, behaviour, line dimensions and cooling regime, the general
then voidspace must develop, with a consequent reduction in patterns of pressure change during cooling are similar to those
internal pressure. The primary parameters that affect the devel- obtained in the previously reported tests for similar configurations
opment of such voidspace are the asymmetric action of gravity as a of steel model pipelines.
vector force normal to the pipe axis and the balance between the 2. To show whether or not that cooling-induced, variable-rate flow
inter-molecular cohesive forces and the adhesive bond to the develops in directions consistent with recorded pressure gradients.
pipewall and end valves. Additionally, in the case of crude oil for 3. To show whether or not that voids can form within the body of the
example, void formation may be affected by compositional and liquid/gel column (and thus contribute a significant increase in
‘structural’ non-homogeneity caused by discrete solid entities such compressibility prior to restart).
as wax, asphaltenes or mineral inclusions or in the form of
entrained gas bubbles. We have not as yet attempted a numerical 2.2. The steel model pipeline
simulation of this complex situation but have included the test so
as to visualize such events in the glass pipe. We further consider The layout of the two steel model pipelines referred to in the
such a test configuration in the Discussion section, with respect to Introduction is described in Phillips et al. The 5.9 mm ID multiport line
the significance of shrinkage and void formation. was modified with the addition of a 1.2 m inclined glass tube of 6 mm
ID. One end of this glass tube was raised by 0.1 m and remained open
When loading the glass line with test fluids, spherical plastic balls to atmosphere during the test, while the opposite, lower end was
were inserted into the liquid column during sample loading, to attached to the multiport line inlet. A metric ruler was positioned
provide visual indication of flow events. This loading process proved alongside this glass tube so that fluid movement in the tube could be
to be difficult. A sphere injection system, similar to a syringe, was recorded during cooling by digital time-lapse photography. Prior to
attached at the pipe inlet but precise axial location of the spheres was loading, both the line and the test fluid were pre-heated to ca. 40 °C,
not possible. The main reason for this was a tendency for very low and the line was evacuated to b0.01 MPa to minimise trapped air.
viscosity liquid to flow around the sphere which consequently tended The warm test fluid (Newtonian standard oil N5100 —Appendix A)
to ‘stick’ and move more slowly than the fluid. was slowly loaded into the evacuated line by applying a modest
Fluid 4 (Appendix A), a waxy condensate, had initially been chosen pressure differential until approximately 1 l of fluid had emerged
because of its translucency which allowed sphere visualization and from the multiport line outlet. The outlet valve was then closed and
because it formed a robust gelled state at relatively high temperature the loaded line subjected to a conditioning pressure of 1 barg
(visible gelation at ca. 27 °C). However, this fluid proved problemat- (recorded by a separate reference gauge) until pressure equilibrium
ical in having very low viscosity (b0.01 Pa s) at the preferred loading was confirmed on all line pressure transducers. An equilibrium
temperature of ca. 50 °C (well above the wax appearance temperature atmospheric pressure condition was then established — at which
of 40 °C). At high temperature, this fluid tended to flow around the point all 8 differential pressure transducers recorded zero gauge
sphere periphery such that accurate sphere placement was effectively pressure (0 psig) and the cooling test was started.
impossible. This flow by-pass also limited the accuracy of the spheres As explained in the Introduction, the purpose of this test was to
as indicators of flow at higher temperatures when the viscosity was establish the interdependence between shrinkage flow, viscosity and
 D.A. Phillips et al. / Journal of Petroleum Science and Engineering 77 (2011) 286–304
pressure gradient for a simple single-phase fluid of known viscosity
where shear-rate induced viscous variation and wall depletion effects
are insignificant. The test thus challenges the postulate that the
development of pressure gradients during cooling in pipes of
significant L/D ratio is a fundamental and numerically predictable
phenomenon exhibited by all highly viscous flowable media. It
follows that, in the absence of an experimentally supported
alternative postulate, such pressure gradients demonstrated by
waxy fluids under similar conditions are probably similarly depen-
dent upon shrinkage flow and the fluid/gel resistance to that flow
(apparent viscosity).
2.3. Numerical simulation
In the first paper of this series, Phillips et al. present a sequence of
calculations that enable numerical description of cooling-induced
shrinkage in pipes and also suggested that a finite element (FE)
approach could be used to include the effect of topographical variation
in elevation or temperature variation along the line.
This numerical approach was applied to simulate the test
described above for the Newtonian standard oil in the steel multiport
line. The calculated result can thus be compared with the experi-
mental observations.
In the case of waxy oils or other complex fluids, cooling-induced
shrinkage is also inevitable, though the trend of decreasing specific
volume is likely to be somewhat reduced in proportion to the increase
in solid phase wax. The molecular cohesive forces responsible for
reducing the volume of both liquids and solids are essentially
isotropic, acting as uniform tensile forces in both the axial and radial
directions. It follows therefore, that if the observed change in volume
is predominantly axial, such that radial shrinkage exactly matches the
pipe shrinkage and the liquid/gel remains in contact with the
pipewall, then a true shearing flow deformation must occur so as to
compensate the sample radial shrinkage. Conversely, if the material
behaves as a rigid gelled solid, then it will inevitably undergo radial
shrinkage such that its diameter becomes less than that of the pipe. In
consequence, a more or less axially-continuous voidspace will form,
either as an annular gap close to the pipewall (adhesive failure) or as
single or multiple voids within the diametric section (cohesive
failure). In such case, while the pressure in a sealed line will fall
(with reducing gel volume), the pressure change will be more or less
uniform along the line and no gradients will form because there is no
flow.
For numerical calculation, we have assumed that the liquid/gel
remains in contact with pipewall and that the most usual situation is
that true flow occurs such that all of the volumetric change is
accommodated entirely by an axial dimensional change. We have also
assumed that, while voids are likely to form if the local pressure falls
to the liquid/gel SVP, the resultant pattern of voidspace is discontin-
uous. Thus the shrinking gel column becomes subdivided so that each
section continues under shrinkage flow, though at a slower rate
(because of the lower L/D ratio of each sub-section) and possibly in a
reversed direction depending on the local topography.
As described in the first paper, we have as yet found no single
rheological model that adequately describes the range of waxy oil
behaviour that we have recorded during concentric cylinder rota-
tional viscometry. Our historical collection of routine measurement of
viscous increase with cooling at different rates of shear indicates that
each of the widely used rheological models can be fitted to some
fluids, for some pretreatments over at least a limited temperature
range, but no model adequately describes all the fluid and pretreat-
ment variants. Hence, we do not suggest that existing rheological
models are likely to offer an accurate representation of shrinkage
flow. Our preferred approach is to build a matrix of measured data
that includes the range of temperature and shrinkage flow rates for
the given field pipeline.
289
However, despite the inevitable differences between shrinkage
flow and ‘normal’ flow — that the flow rate varies continuously at
different axial locations and that the flow is dependent upon internal
molecular cohesion rather than being driven by an externally
impressed pressure gradient — we have calculated simple-case
examples using two common rheological models to serve as reference
illustrations for comparison with the Newtonian calculation and with
some historical examples of cooling-induced pressure gradients. The
first of these is the Ostwald-de Waele or power-law model in which
viscosity has a non-linear relationship to the rate of shear according to
an experimentally derived exponent but ignores the near certainty
that, if cooled statically to below the pour point, then the liquid/gel
will develop a level of solid structural strength that requires a
minimum level of applied force to fracture it (usually referred to as a
‘yield stress’). The second model is the widely used Bingham model
that includes a fixed yield stress term and adds a viscous resistance
that varies as a simple multiple with the rate of shear.
In addition, a third example has been presented based on the
premise that shrinkage flow is accommodated by the permeation of
low viscosity wax-depleted continuous phase through a more or less
static waxy solids matrix. Such interstitial flow of ‘base oil’ was
postulated by Verschuur et al., 1971a as demonstrating a flow rate and
pressure relationship in accord with the Darcy equation but that if the
resultant wall stress exceeded the yield value of the waxy structure,
then this structure was broken. The resultant suspension of broken
waxy particulates in continuous phase was assumed to display low
apparent viscosity so that ‘normal’ flow was restored in the pipe
section leading up to the point of rupture with Darcy flow continuing
in the unruptured section. Simulations of the effect of progressive
rupture are shown.
The expressions used in calculation of these example simulations
are listed in Appendix B.
3. Results
Results are presented for laboratory tests in both the glass and the
steel pipelines. Laboratory test results for the glass line are evaluated
in Section 3.1 with respect to the basic assumptions of the numerical
model. Example calculation based upon different rheological flow
models are presented in Section 3.2. Some results from steel pipeline
tests for waxy black oils are shown for comparison in Section 3.3. In
Section 3.4, the results of tests using a Newtonian standard oil are
presented together with the numerical simulation for each test.
3.1. Glass pipeline results
Despite the limitations of the glass pipeline, the fundamental
model predictions were confirmed in all test conducted so far. The
following essential general observations were found:
1. Movement of the spheres clearly shows significant flow with
cooling and in flow directions consistent with predictions.
2. As flow resistance increased with cooling, pressure gradients were
recorded and became more pronounced with further cooling.
3. Flow continued with cooling even at temperatures below the static
fluid gelation point (static pour point).
4. However, fracture and/or bubble voids formed when the local
pressure fell below a fixed value at a given temperature.
5. When one end of the line is open to atmospheric pressure, flow is
uni-directed toward the closed end. If both ends are open, flow
tended to be directed from each end toward the line mid- length.
6. Closing both ends of the line in horizontal layout, nearly eliminated
pressure gradients, though pressures decreased with reducing
temperature. Flow tended to be directed from each end toward the
line midpoint, but was disrupted and limited. Sphere movement
290 D.A. Phillips et al. / Journal of Petroleum Science and Engineering 77 (2011) 286–304

12.7 mm ID steel line linear pressure distribution

was reduced by approximately ten-fold compared with the double
0
open-ended test with the same fluid.
7. Raising one end of the closed line to create a gravity-induced
elevation head (2.33 m), restored flow to a level closely similar to
the observed movement in the comparable single open-end test
(allowing for the different sphere location and temperature range). -1

P (psig)
The first example is that of the horizontal configuration with one
end closed and the other open to atmosphere. This approximates the
situation frequently used in laboratory restart test protocols. For this -2
10°C
test, the model fluid described above was cooled from 54 °C to 18 °C in 7.5°C

110 min. Three entrained spheres were observed and their movement 5°C
2.5°C
recorded. The total movement of each sphere, represented by Fig. 2,
0.5°C
clearly indicates a pattern of fastest flow at the open inlet with an
-3
approximately linear decrease in flow toward a shrinkage null at the 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16
closed end.
Distance from open end (m)
Pressure profiles along the line are shown in Fig. 3. These are less
smooth than those reported by Phillips et al., for a comparable test
Glass line test 1 linear pressure distribution
with less viscous oil (Fluid 1) in the 12.7 mm ID multiport steel tube 1
rig (also shown in Fig. 3 for comparison), but nonetheless display
gradients consistent with the flow direction. 0
By measuring the incremental movement of sphere A during each
-1
of four temperature steps, the sphere velocity can be calculated. If the
gel velocity is maximal at the open end (locus 0) and decreases -2

P (psig)
linearly to zero at locus 10, then the sphere velocity at its 1.2 m locus
is assumed to be 0.88 of the maximum. Hence the maximum velocity -3
can be estimated for each temperature step as shown in Table 1.
-4 29°C
Fig. 4 displays the log values of cooling rates and velocity maxima
27°C
for the experimental temperature range. -5
24°C
Although, the recorded pressure profiles are ragged, the overall
21°C
line pressure drop during each of these temperature steps can be -6
18°C
extracted. An estimate of mean resistance to flow is then possible as -7
shown in Table 2. 0 1 2 3 4 5 6 7 8 9 10
By assuming that the average flow velocity in the full 10 m length, Distance from open end (m)
during each step, is approximately half the maximum, as indicated by
the movement of sphere B in Fig. 2, an approximate flow resistance Fig. 3. Pressures recorded at temperature intervals during cooling. Comparison of a
can be determined — represented as a mean apparent viscosity moderate-wax black oil in a steel multiport line with the model fluid in the glass model
consistent with the average flow and the measured pressure drop for pipeline. Both lines were in the single open-ended, horizontal configuration.
each of the four temperature steps. The calculated results are shown
in Table 2 and are presented in the chart of Fig. 5. consistent with a plausible increase in apparent viscosity with
It must be emphasised that these calculations are necessarily reducing temperature (Fig. 5).
approximate. The results are presented so as to show that the In this first test, voids developed in the section adjacent to the
postulated relationships between cooling, shrinkage flow and flow closed end when the pressure had reached approximately minus
resistance are consistent with the measurements recorded. In 5 psig toward the end of the test. These bubble voids are indicated by
particular that the flow velocity is broadly in line with the rate of the overlay arrows on the image in Fig. 6. While such void formation is
cooling (Fig. 4) and that the observed increase in pressure gradient is expected to disrupt flow and the consequent pressure gradients, this
test appears to demonstrate flow (indicated by sphere displacement)
and increasing pressure gradient, at temperatures well below the ca.
Glass-line test 1 shrinkage flow 28 °C (static) gelation temperature.
180 In Test 2, the movement of sphere A, shown in Fig. 7, is far less than
160 in the first example, partly because it is positioned at 3 m (so as to lie
Sphere A within the horizontal section) compared to 1.2 m as in the first
Total movement (mm)

140
example; and partly because of the reduced cooling range (to prevent
120 void formation during the subsequent ‘aging’ period).
100 The pressure profiles (Fig. 8) in the second test are assumed to be
Sphere B
80 the combined effect of the gravity head and shrinkage of the fluid with
cooling.
60
The lowest pressure initially is at the highest point where a void
40 Sphere C
quickly forms. The pressure increases towards the base of the raised
20 section because of the hydrostatic head. This pressure is initially near
0 constant along the horizontal section, and the pressure difference of
0 1 2 3 4 5 6 7 8 9 10 approximately 2.7 psid is consistent with the vertical rise and a
Sphere initial locus from open end (m) density of approximately 800 kg m−3. When significant wax structure
forms below about 28 °C, a gradient begins to develop from the riser
Fig. 2. Movement of spheres entrained in the liquid/gel when cooled through 36 °C. The base. The flow (indicated by sphere displacement) continues and the
pipe-end at 10 m was closed and the other end was open to atmospheric pressure. pressure gradient increases as the temperature is reduced toward
 D.A. Phillips et al. / Journal of Petroleum Science and Engineering 77 (2011) 286–304 291

Glass-line test 1 estimated cooling rate Glass-line test 1 estimated mean apparent viscosity
1.0E+00 1.0E+05
Log scale cooling rate (°C min-1)

Log scale viscosity (Pa·s)

1.0E+04

1.0E-01 1.0E+03

1.0E+02

1.0E-02 1.0E+01
15 20 25 30 35 40 45 15 20 25 30 35 40 45
Step mean temperature (°C) Step mean temperature (°C)

Glass-line test 1 estimated shrinkage-flow velocity Fig. 5. Estimated increase of apparent viscosity determined from the observed pressure
1.0E-04 drops and calculated mean flow velocities.
Log scale velocity (m s-1)

1.0E-05
1.0E-06
1.0E-07
15 20 25 30 35
Step mean temperature (°C)
Fig. 4. Cooling rates and flow velocity maxima estimated at each of four temperature
steps. Gelation onset was observed at approximately 28 °C.
25 °C. Given that the flow resistance increases with further cooling,
then the increase in pressure gradient from the riser base to the end of
the horizontal section is consistent with expectation. However, the
cooling rate was much slower from 28 to 25 °C as was the observed
rate of shrinkage flow and in consequence, although the mean overall
line pressure is lower at 25 °C than at 28 °C, the pressure in the riser
has risen slightly (note that the pressure transducer P1 recorded the
pressure in the adjacent liquid/gel and not that in the voidspace above
the fluid). The only void that formed was that at the highest end.
At 64 min cooling was stopped and the temperature held at 25 °C.
Pressures initially continued to decrease and then began to rise so that
at 2 h elapsed the lowest pressure (at 10 m) had risen to − 2.5 psig
(from −2.86 psig at 64 min) and the pressure at the base of the riser,
close to sphere A, had risen from −0.72 psig at 64 min to −0.15 psig
at 2 h. The position of the sphere C was unchanged at 2 h but sphere A
had moved an additional 3 mm and sphere B an additional 2 mm. No
voids formed within the gel column.
Example three is not relevant to any field-case, but serves to confirm
the expected flow pattern when both ends of a horizontal line are open
to atmosphere. In this test, the unmodified condensate (Fluid 4) was
cooled from 38 °C to 25 °C in 100 min. The lower start temperature and
slower cooling rate were adopted so as to minimise flow by-pass and
delay fracture void onset. In this way valid observation was possible so
40 45 as to demonstrate patterns of shrinkage flow and pressure gradient
development in the unmodified condensate rather than the model fluid
used in the other tests.
Fig. 9 shows movement of sphere A that indicates flow away from
its adjacent open end, but in this case, sphere C also indicates flow
away from its adjacent open end (shown as a negative distance). Thus
there is bi-directional opposed flow toward a shrinkage null near the
mid-length, as also indicated by the limited movement of sphere B.
The twin flow directions are postulated to induce characteristic
pressure profiles as shown in Fig. 10, with lowest pressures developed
near the mid-length. A closely similar pattern of pressure distribution
was reported in the first paper when Fluid 1 (a moderate-wax black
oil) was cooled in the 5.9 mm ID multiport steel line in this open-
ended configuration. In the glass line Test 3, the condensate was not
cooled much below the 27 °C gelation temperature, hence there was
limited pressure reduction and no voids were formed.

Table 2
Recorded pressure differentials (psid), calculated mean liquid/gel velocity and the
corresponding estimated mean apparent viscosity increase in glass pipeline Test 1.

Mean step Step mean Recorded Apparent

temperature velocity pressure viscosity
(°C) (10−6 m s−1) (psid) (Pa s)

41.5 23.43 0.35 11.2

26.5 0.7576 3.04 3,000
22.25 0.3157 4.39 10,500
Fig. 6. Void formation (indicated by yellow arrows) in the last section of the line where
19.25 0.1722 5.39 23,500
the lowest pressures developed.
292 D.A. Phillips et al. / Journal of Petroleum Science and Engineering 77 (2011) 286–304

Glass-line test 2 shrinkage flow Glass-line test 3 shrinkage flow

120 30

Sphere A 20
100
Total movement (mm)

Total movement (mm)

10
80 Sphere A
Sphere B 0 Sphere B
60
-10
40 Sphere C
Sphere C -20
20
-30

0 -40
0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 10
Sphere initial locus from raised end (m) Sphere initial locus from left-hand end (m)

Fig. 7. Model fluid was cooled through 25 °C. Both pipe-ends were closed and the first Fig. 9. Waxy condensate was cooled through 13 °C in a horizontal line configuration.
2.33 m were raised to vertical. Both pipe-ends were open to atmospheric pressure. Flow is indicated in opposing
directions from the pipeline ends toward the linear centre.

Example four is relevant to some laboratory test protocols. Both
ends of the line were closed when in horizontal configuration and the
model fluid cooled from 50 °C to 15 °C in 110 min. In this case
movement was also opposed bi-directional, but far less than in any
other test configuration. Fig. 11 shows that the flow pattern is markedly
asymmetric with an apparent shrinkage null well to the right of the
mid-length, probably because of the rig asymmetry. This very limited
movement for such a wide temperature range is only possible if the
flow is disrupted by fracturing to compensate for the shrinkage.
Low pressures (Fig. 12) and fractures (Fig. 13), developed at an
early stage during cooling. Pressure gradients were extremely limited.
As described in Section 2.1, the calculation of the effect of
shrinkage in a sealed horizontal symmetrical configuration is likely
to be primarily influenced by the compositional non-homogeneity of
the oil/gel. We have not tried to model this situation but have
considered some of the possibilities in the discussion. While such a
scenario is unlikely ever to occur in field lines (which are almost
always subject to an axially directed gravity vector component,
Phillips et al., in press), it is a common configuration for laboratory
testing. Thus understanding the effects of shrinkage in such tests is
important, particularly in contrast to the probably very different
situation in the field line that the test is intended to mimic. Inclusion
of such a configuration among these glass line tests was intended
simply as an exploratory investigation rather than as a challenge to
prediction.
Our postulate forecasts that in such a test, the pressure will fall
rapidly in a more or less uniform manner and that a calculable void
volume will form. However, prediction of the distribution of such
voidspace is likely to be influenced by any non-uniformity in the
system such as the variation in adhesive bonding to pipewall and end
valves or sample non-homogeneity with respect to void nucleation
sites. Multiple fracturing is likely below the vapour pressure so as to
produce many short discrete lengths. Example four supports such a
conclusion to some extent, but even less flow and more fracturing
might have been expected. However, as stated already, the glass rig is
imperfect, being somewhat flexible, asymmetrical and not truly
horizontal. It is worth noting that in this test, as in the other tests,
minus 5 psig represented the approximate low pressure limit at 18 °C
below which fracture-voids formed. However, with additional cool-
ing, the vapour pressure decreases further, and lower pressures may
be sustained, as shown in this example.
A selection of fracture void images from other tests is displayed in
Fig. 14. Two such voids formed adjacent to entrained beads which
represent significant discontinuities. The spherical beads appear
elliptical in the images as a result of the lens-effect of the transparent
tubes and the coolant.
3.2. Numerical simulation examples
Prediction of void formation represents a very valuable feature of
numerical simulation because of the consequent modification of gel
compressibility. However the usefulness of numerical modelling is
also related to the prediction of shrinkage flow rate and the variation

Glass-line test 2 linear pressure distribution Glass-line test 3 linear pressure distribution
1 0

-1
-1
P (psig)
P (psig)

-2
-2
50C 28C
-3
28C 26C
25C 25C
-4 -3
0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 10
Distance from raised end (m) Distance from left-hand end (m)

Fig. 8. Pressures recorded at three temperature intervals during cooling in sealed and Fig. 10. Pressures recorded at three temperature intervals during cooling in a test with
raised-end configuration. open-ended horizontal pipe configuration.
 D.A. Phillips et al. / Journal of Petroleum Science and Engineering 77 (2011) 286–304 293

Glass-line test 4 shrinkage flow

12

10
Total movement (mm).

8
Sphere A Sphere B
6

0 Sphere C

-2

-4
0 1 2 3 4 5 6 7 8 9 10
Sphere initial locus from left-hand end (m)

Fig. 11. Model fluid was cooled through 35 °C in a horizontal line configuration when
pipe-ends were closed. Arrows indicate opposing flow directions.

of that flow along the pipeline and depends upon the assumption that
waxy fluids are subjected to shear during cooling-induced shrinkage
flow such that waxy solid structural development is limited to some
extent (shear thinning). Numerous citations in support of this
assumption were listed in the first paper, including Chang et al.,
1998 who state that “even the smallest shear rate in steady flow could
lead to deformations large enough to damage the wax structure”.
Thus, even if the fluid demonstrates a significant yield stress when
cooled under static (zero-flow) conditions, as would be expected at Fig. 13. Fracture void images from the glass line Test 4.
temperatures below the pour point, if shrinkage flow continues below
the pour point or gelation temperature, then there must be sufficient
disruption of the waxy solids development to reduce the effective
yield stress to a level below that of the shrinkage-induced wall stress. each example and that voids do not form within the liquid/gel body.
The possible exception to this assumption is the interstitial or The flow rate corresponds to that calculated for a black oil (Fluid 1)
permeation flow model at flow rates and consequent wall stresses cooled through 5 °C at 0.02 °C/min. The resultant profiles of axial
that are less than the ‘rupture stress’ value of the static waxy pressure distribution and wall shear stress are derived from
structure. calculation at each of 12 equidistant loci.
As in Section 2.3, we believe that existing rheological models are The upper chart of Fig. 15 displays calculated pressure profiles
unlikely to provide an adequate representation of shrinkage flow and based on the assumption that flow resistance (apparent viscosity)
we explore this in the Discussion section. However, in order to varies with changing wall shear rate according to a power-law
provide a reference for interpretation and discussion, example relationship such that values of the power index n less than unity
simulations based on different rheological flow models are shown indicate shear thinning. When n = 1 there is no shear thinning and the
below. In each case the same cooling regime and consequent fluid is Newtonian. Three lower values for n were chosen (0.6, 0.3 and
shrinkage is assumed, such that the volume flow rate Q declines 0.1) to represent increasing levels of shear-induced degradation of
linearly from a maximum (ca. 1.27 × 10−10 m3 s−1) at one end of a waxy structure. The corresponding values of intrinsic viscosity (K)
6 mm ID pipe to zero at the opposite end. The calculation also assumes were 1100 for the Newtonian example and 105.3, 17.8 and 5.6
the same total pressure drop of 5 psid over the full 15 m line length in respectively for the others. These values were chosen so as to attain
the same overall pressure drop for the specified shrinkage flow rate.
The lower chart of Fig. 15 shows the corresponding distribution of
Glass-line test 4 linear pressure distribution
2 calculated wall stress based on the pressure drop across each 1.25 m
1 element.
0 The Bingham model was selected to represent the effect of
-1 inclusion of a yield stress. While this model does not allow for shear
-2 thinning, the assumption that the fluid is undergoing shrinkage-
P (psig)

-3 induced flow at temperatures below the static pour point, must mean
-4 that this flow has, in some manner, limited the development of the
-5 yield stress (compared to that for a static cooled sample) to a level
50C below that of the wall stress induced by molecular cohesion. Two
-6
-7
25C possible Bingham fluids were modelled for illustration. The Bingham 1
24C
-8 example in Fig. 16 has a Bingham yield level of 2.25 Pa and the
15C
-9 Bingham 2 fluid has a yield stress of 3.125 Pa. The corresponding
0 1 2 3 4 5 6 7 8 9 10 Bingham viscosity levels are 220 and 20 respectively. These values
Distance from left-hand end (m) also accord with the specified shrinkage flow and overall line pressure
drop. The most shear thinning power-law example and the Newto-
Fig. 12. Pressures recorded during a test at four temperature intervals during cooling in nian example are both included in Fig. 16 for comparison. As an
sealed horizontal configuration. additional illustrative comparison, the calculated radial velocity
294 D.A. Phillips et al. / Journal of Petroleum Science and Engineering 77 (2011) 286–304

Simulated axial pressure distribution

0

-1

-2

P (psig)
-3

-4 n = 1 Newtonian
n = 0.6
-5 n = 0.3
n = 0.1

-6
0 5 10 15
Locus (m)

Simulated axial wall stress distribution

7

Wall stress (Pa)

5

3
n = 1 Newtonian
2 n = 0.6
n = 0.3
1 n = 0.1

0
0 5 10 15
Locus (m)

Fig. 15. A comparison of the effect of shear thinning according to a power-law

relationship. The predicted pressure variation during shrinkage flow is shown in the
upper chart and corresponding distribution of wall shear stress in the lower chart.

profiles that are more or less intermediate to those shown in Figs. 15

Fig. 14. Fracture void images from other tests at lower temperatures.
profiles for the most shear thinning fluid (n = 0.1) and the Bingham 2
example are shown in Fig. 17. The profiles selected are for the 1.25 m
locus (high shrinkage flow rate) and for the median flow rate at the
axial midpoint.
The Ostwald-de Waele (power-law) and Bingham models could be
described as the opposed extremes of rheological interpretation. Most
other models might be considered as representing both shear
thinning and the existence of a yield stress (or a rate based
equivalent). In consequence, the application of these models to the
description of shrinkage flow produces pressure and wall stress
and 16.
However, there is a further possible interpretation of shrinkage
flow based upon the permeation or interstitial flow postulated by
Verschuur et al., 1971a. This model assumes that the waxy solid
structure is effectively static and exhibits a yield stress. Volumetric
change with cooling (shrinkage) is accommodated by flow of wax-
depleted ‘base oil’ through the porous wax structure in accord with
the Darcy relationship. If the resultant wall stress increases to the level
of the waxy structural yield point, then a rupture occurs, the flow
resistance falls to a low residual level and flow of this degraded
material accords with the Hagen–Poiseuille relationship (between the
‘inlet’ end and the point of rupture). In the unruptured region, flow
resistance and the consequent pressure and wall stress profiles are
dictated by the viscosity of the wax-depleted liquid continuous phase
and the permeability of the waxy matrix.
While it is possible to apply this model to the specified shrinkage
flow selected for the previous examples, the specified overall pressure
drop can only be fitted to a single assumption in respect to the degree
of waxy rupture. Thus while the initial pressure drop in the example
shown in Fig. 18 is 5 psid for entirely Darcy flow (with a wall stress
lower than the yield stress of 6.7 Pa), this pressure drop inevitably
decreases (the pressure thus rises) once the waxy matrix exhibits
significant rupture. Three profiles indicating the progression of waxy
structural breakdown are also shown. The numerical assumptions in
this simulation are that the viscosity of the continuous phase liquid
increases (from an initial level of 10 Pa s to 14.5 Pa s) and the
permeability of the intact wax structure decreases (from an initial
level of 1.023 × 10−8 m2 to 7.0 × 10−9 m2) during the cooling period.
The post-rupture apparent viscosity (of the suspension of broken
down waxy particles) is assumed to be 10% higher than that of the
 D.A. Phillips et al. / Journal of Petroleum Science and Engineering 77 (2011) 286–304 295

Simulated axial pressure distribution Simulated radial velocity distribution

0 6.E-06

-1 5.E-06

-2
4.E-06

Velocity (m s-1)
P (psig)

-3
3.E-06

-4
n = 1 Newtonian
2.E-06
Bingham 1
Power-law at 1.25 m
Bingham 2
-5 Power Law n = 0.1
Bingham 2 at 1.25 m
Power-law at 7.5 m
1.E-06
Bingham 2 at 7.5 m

-6
0 5 10 15
Locus (m) 0.E+00
0.0 0.2 0.4 0.6 0.8 1.0
Proportionate radius
Simulated axial wall stress distribution
7
Fig. 17. Calculated radial velocity variation for a power-law fluid (n = 0.1) compared
with a Bingham fluid (Bingham viscosity = 20, Bingham yield stress = 3.125). Velocity
profiles are shown for 2 axial locations; at 1.25 m, where the shrinkage flow is near
6 maximum and at the axial midpoint.

Simulated axial pressure distribution

5 1
Wall stress (Pa)

0
4
-1
P (psig)

-2
3
-3
n = 1 Newtonian Darcy
2 Bingham 1 -4 1/6 ruptured
Bingham 2 1/3 ruptured
Power Law n = 0.1
-5
1/2 ruptured
1 -6
0 5 10 15
Locus (m)
0
0 5 10 15
Simulated axial wall stress distribution
Locus (m) 10
Darcy
9 1/6 ruptured
Fig. 16. The predicted behaviour of two Bingham fluids during shrinkage flow. Bingham 8 1/3 ruptured
1 has a Bingham viscosity of 220 and a yield stress of 2.25. Bingham 2 has a Bingham
Wall stress (Pa)

7 1/2 ruptured
viscosity of 20 and a yield stress of 3.125. The Newtonian and power-law (n = 0.1)
profiles are included for comparison. 6
5
4
continuous phase (base oil) for each simulation. The permeation flow 3
is assumed uniform such that the flow velocity is the same at all radial 2
locations. The levels of viscosity increase and permeability decrease 1
were chosen for illustration of the progression of rupture. It would be
0
unusual that such rapid change would occur within the 5 °C cooling 0 5 10 15
increment assumed for these examples. Locus (m)
The relationships between flow, pressure gradient, wall stress and
radial velocity used in the above example simulations are given in
Fig. 18. A simulation of the interstitial flow model assuming progressive rupture of the
Appendix B. waxy matrix as ‘base oil’ viscosity increases and waxy structural permeability decreases.

3.3. Experimental comparison

below in Fig. 19. These results of tests in the steel multiport rig (with
In addition to the experimentally determined profiles shown for one end open to atmospheric pressure) for three waxy, shear thinning
the steel and glass lines in Fig. 3, some further examples are shown fluids (Appendix A) were selected on the basis of demonstrating a
296 D.A. Phillips et al. / Journal of Petroleum Science and Engineering 77 (2011) 286–304

Measured coolant temperature change

significant pressure gradient during cooling under the required test 60
conditions. The Fluids 5 to 7 demonstrated pour points under test
pretreatment of 15, 18 and 30 °C respectively. Similar cooling regimes 50 Fluid 5

Temperature (oC)
were used in these three tests as indicated in Fig. 20. 40 Fluid 6
Fluid 7
The example cooling-induced pressure profiles of Figs. 3 and 19 are
30
broadly representative of the profiles recorded during some 140
restart tests using multiport steel model pipelines. The fluids tested 20
include black oils, condensates and water-in-oil emulsions with 10
widely differing waxy character but which all exhibited at least
0
moderately high apparent viscosity under test conditions. Cooling
regimes were selected on the basis of the field line conditions rather -10
0 1 2 3 4 5 6 7 8 9 10
than for the purpose of demonstrating cooling-induced pressure
change and thus the resultant recorded profiles indicate a significant Time (hours)
range in terms of overall pressure drop, degree of profile curvature or
linearity and the uniformity of profile. However, two general Fig. 20. Temperatures recorded during the cooling of the three waxy black oils shown in
observations may be applied to all test data collected to date (from Fig. 19.

multiport line tests with one end open to atmosphere). Firstly, the
effect of cooling invariably induced a partial vacuum with the lowest
pressures in the sections adjacent to the closed end such that a

pressure gradient is formed. Secondly, the pressure tended to

decrease with cooling and no pressure rise has so far been recorded
until cooling ceases or the rate of cooling is significantly reduced.
Fluid 5 measured linear pressure distribution
1
0 3.4. A Newtonian validation
-1
-2 The assumptive basis of the numerical simulation of shrinkage
-3 flow is that pressure decrease and formation of pressure gradients
P (psig)

-4 with cooling is a fundamental property of highly viscous flowable

-5
media. It is further assumed that the presence of ‘flow-modifiers’ such
-6 11.9C
-7 as waxy solids are likely to not only increase the overall flow
8.5C
-8 5.7C
resistance and consequent pressure drop, but also to introduce axially
-9 0.2C variable non-uniformity of flow resistance such as to alter the shape of
-10 the induced pressure gradient. Hence it was deemed essential to
0 1 2 3 4 5 6 7 8
demonstrate experimentally the fundamental premise that the extent
Port number
and axial distribution of pressure decrease was consistent with
prediction in the case of a wax-free simple liquid of known viscosity.
Fluid 6 measured linear pressure distribution
0 The results of such a demonstration might then serve as a comparative
-1 reference for complex fluids such as waxy oils.
For these reasons, the shrinkage flow and resultant pressure
-2
gradients were calculated for a Newtonian fluid (N5100), when
-3
P (psig)

cooled through consecutive temperature decrements during 30 min

-4 intervals defined by a laboratory test in the 5.9 mm ID multiport line
12.1C
-5 using this standard fluid. Pressure minima recorded during the 34 h
9.6C
-6 7.2C test are shown in Fig. 21 together with the experimental cooling and
4.8C shrinkage profiles. The numerical simulation assumed a closed valve
-7
-0.5C adjacent to port 8 and the other line end open to atmosphere. This was
-8 the configuration in the multiport line during the experiment.
0 1 2 3 4 5 6 7 8
Port number The shrinkage determined from photographic records for the first
four 30 min intervals was linked to the temperature record during
Fluid 7 measured linear pressure distribution those time steps and these temperature and time intervals were used
0 for numerical simulation. Table 3 shows a comparison of the
-1 measured and simulated shrinkage movement.
-2 Fig. 22 shows the pressure gradient recorded during the test
-3 (upper chart) and the corresponding simulated gradients (lower
P (psig)

-4 chart) while Table 4 presents the numerical data for comparison.

-5 While a pressure minimum of minus 3.86 psig was reached after ca.
-6
12.5C 2.5 h at approximately minus 7.5 °C, significant cooling extended to
-7
9.2C minus 10.62 °C, at 5 h elapsed. Slight further cooling to minus 10.99 °C
-8 4C during the next 4.5 h was contemporaneous with additional shrink-
-9 -4C
age of 23 mm and a pressure rise from minus 3.09 to minus 0.97 psig.
-10
0 1 2 3 4 5 6 7 8 Despite the efforts taken to eliminate entrapped air, a void formed
Port number in the last section of the line. This bubble of approximately 2 mm
diameter, was evident when the line was unloaded. In consequence,
Fig. 19. Pressures recorded at several temperature intervals during cooling of three the pressure reduction at ports 7 and 8 was limited and the profiles
waxy black oils. thus distorted.
 D.A. Phillips et al. / Journal of Petroleum Science and Engineering 77 (2011) 286–304 297

Shrinkage of Newtonian standard oil N5100 Measured linear pressure distribution

900 25 0

800 Oil level

20 -1
Temperature
700 15

T (oC) & P (psig)

Pressure minima

P (psig)
Oil level (mm)

600 -2
10
500
5 -3
30 mins
400
0 60 mins
300 -4 90 mins

200 -5 2 hours
-5
100 -10 0 1 2 3 4 5 6 7 8

0 -15 Port number

1 4 7 10 13 16 19 22 25 28 31 34
Time (hours) Simulated linear pressure distribution
0

Fig. 21. Shrinkage was recorded as a changing oil level with temperature. Both -1
temperature (T) and gauge pressure (P) are plotted to the secondary axis.

P (psig)
-2

-3
30 mins
4. Discussion 60 mins
-4 90 mins

4.1. Shrinkage flow 2 hours

Despite the limitations of the glass pipeline, the results so far
compare well with those previously reported by Phillips et al. for
similar tests in steel lines. The glass line tests clearly show flow caused
by thermal shrinkage and the consequent flow-induced pressure
gradients, entirely consistent with the patterns predicted. The effect of
gravity in directing flow and supporting pressure gradients has also
been well demonstrated. The results also indicate a low pressure limit,
below which void formation is likely within the fluid/gel column.
While there is a high degree of approximation in the calculation,
the estimated viscosity values of Table 2 are surprisingly close to
expected values for the model fluid, based on extrapolation from
rheometer measurement and the values expected for a fluid at and
below its measured gel point. The viscosity at 40 °C arises mainly from
the 20% volume content of N190000 (at 40 °C N190000 viscosity is
146.5 Pa s), while below the gelation temperature, the effect of wax
formation in Fluid 4 predominates. Therefore, below ca. 28 °C, we
might expect viscosities of ca. 1.0 × 103 Pa s, and much higher as the
temperature falls. The estimated shrinkage velocities and consequent
shear rates in this test are far lower than those assumed in the
previous estimation of viscosity at the pour point (Phillips et al.).
The cooling-induced pressure gradients demonstrated for a
Newtonian fluid (Fig. 22 and Table 4) show a fair correspondence
with model predicted values, except at locus 1 and near the closed end
of the pipe where a void had formed. Void formation was not
anticipated at such sub-pressures and may have been the result of a
bubble entrained during loading. If void formation is included in the
model prediction by setting a vapour pressure limit at minus 3.5 psig,
then a similar flattening of the pressure profile occurs. The wall shear
stress profiles derived from this experiment are effectively linear, as
Table 3
Comparison of shrinkage derived from experiment and model prediction.
Temperature range Shrinkage movement
Time T1 T2 Measured
(min) (°C) (°C) (mm)
30 18.6 8.5 73
60 8.5 1.7 62
90 1.7 −2.6 39
120 −2.6 −5.5 27
-5
0 1 2 3 4 5 6 7 8
Port number
Fig. 22. Pressures recorded during cooling of Newtonian oil N5100 are shown in the
upper chart. The lower chart shows the corresponding pressures obtained by numerical
simulation.
predicted for a Newtonian fluid. Thus the shrinkage-induced pressure
profiles for a Newtonian fluid (free of voids and other discontinuities)
in a tube that is open to atmospheric pressure at one end, are
confirmed experimentally as exhibiting a generalised quadratic form:
2
Px = P0 −ax + bx
where P0 is ambient pressure and x is the proportional line distance
from the open end (a and b are fluid-specific constants). This accords
with the theoretical deduction where during a given time increment
with uniform cooling of a Newtonian liquid, the mean viscous
resistance can be assumed constant. The slope of the axial change in
mean shrinkage velocity dV / dL can also be assumed constant (for the
single mean step temperature). Consequently, the rate of axial change
in pressure gradient is constant. Therefore given an axially linear
increase in flow rate there is a corresponding linear increase in
pressure gradient. Hence the progressive sum (to obtain actual
pressure) of this arithmetic sequence of increasing pressure drop, has
a quadratic form — in the same manner that the linear change in shear
stress and shear strain rate with respect to the pipe radius, produces a
quadratic (paraboloid) form in the radial velocity profile during
laminar flow of a Newtonian liquid.
It follows therefore, that any non-linearity in the relationship
between flow resistance (apparent viscosity) and shrinkage flow will
induce a change in this quadratic Newtonian form of axial pressure
distribution and the corresponding linear decrease in wall stress from
Simulated a maximum to zero (at the shrinkage null). The predicted change in
(mm) pressure gradients and consequent wall stress profiles for shear
90 thinning fluids is indicated by the model predictions of Fig. 15 and
61 those for Bingham fluids in Fig. 16. Such predicted behaviour appears
38 similar to the experimental results shown in Figs. 3 and 19. With more
26
pronounced shear thinning or increasing yield stress, the predicted
298 D.A. Phillips et al. / Journal of Petroleum Science and Engineering 77 (2011) 286–304
Table 4
Comparison of pressures derived from experiment and model prediction.
Pressure (psig) Pressure (psig)
Time 30 min Time 60 min
Locus Measured Simulated Measured
1 −0.78 −0.43 −0.99
2 −1.26 −0.91 −1.67
3 −1.65 −1.32 −2.22
4 −1.97 −1.65 −2.67
5 −2.21 −1.91 −3.02
6 −2.37 −2.10 −3.26
7 −2.45 −2.21 −3.37
8 −2.47 −2.24 −3.33
pressure gradients become more linear in shape and the wall stress
profiles become less steep. The radial change in flow velocity for the
shear thinning and Bingham assumptions also depart from the
Newtonian parabolic velocity distribution and develop a more plug-
like flow form as shown in Fig. 17.
By contrast, numerical simulation of the effect of permeation flow
of wax-depleted oil through a static wax matrix (as suggested by
Verschuur et al., 1971a) produces a Newtonian-like quadratic form of
axial pressure distribution as shown by the Darcy profile in Fig. 18.
Like Newtonian flow, the Darcy expression indicates a linear
relationship between volume flow rate and dP / dL. However, the
postulate of Verschuur et al. that the waxy matrix can be progressively
ruptured, results in a distinctive step change in pressure profile such
as to produce significant increases in pressure, particularly in the pipe
sections containing the degraded material. The effect of such
progressive rupture is also indicated in Fig. 18. As stated in Section 3.3,
measurement of pressure change during cooling of a wide range of
fluids has, as yet, not provided an example of pressure rise until
cooling ceases or the rate of cooling is significantly reduced.
The shrinkage flow postulate assumes that displacement of
material during cooling represents true shearing flow rather than
the isometric (affine) dimensional change that characterises a
shrinking solid. This assumption is supported by the observations of
the glass pipe tests. While both cohesive and adhesive failures are
clearly evident in the formation of diameter-spanning voids (Fig. 14),
there is no evidence that shrinkage isometry produces a more or less
continuous core void formation or radial contraction away from the
pipewall. The co-existence of pressure gradients and significant
apparent flow (indicated by sphere movement) also lends support
to the flow postulate. Such gradients would not be induced by
isometric shrinkage. In the case of a near continuous core void
formation, there would be little or no axial displacement because
shrinkage would be accommodated mainly by growth of the core
void. In the case of radial contraction away from the wall, the resultant
annular fracture would create a gap and any subsequent shrinkage
displacement would no longer affect the pressure transducers
(mounted on the upper pipe surface). Recorded pressures would
subsequently remain constant or, more likely, tend to rise and
equalise.
4.2. Waxy structural development
The ongoing study of the kinetics and morphology of waxy solid
formation presents significant insight into a complex and variable
combination of thermal and shear influenced processes that are likely
to affect both the deposition of robust waxy layers on pipewalls
during full production flow and the onset of more diffuse cooling-
induced waxy structure following shut-in. It is this latter process that
can lead to a gel state throughout the oil body that is associated with
the pour point and with restart problems.
Pressure (psig) Pressure (psig)
Time 90 min Time 2 h
Simulated Measured Simulated Measured Simulated
−0.80 −1.12 −0.98 −1.16 −1.01
−1.60 −1.93 −1.93 −2.03 −1.99
−2.28 −2.56 −2.74 −2.72 −2.82
−2.83 −3.09 −3.40 −3.28 −3.50
−3.26 −3.49 −3.92 −3.72 −4.03
−3.57 −3.80 −4.29 −4.08 −4.41
−3.76 −3.88 −4.51 −4.16 −4.64
−3.82 −3.83 −4.58 −4.11 −4.71
The process of waxy solid formation is considered to be a
continuum of events beginning with the association of wax molecules
(generally regarded as C17 and higher) to produce multicomponent
mixtures of saturated hydrocarbons (Srivastava et al., 1993).
Molecular size ranges in length from over 2 nm for C17 to over
11 nm for C100 (Dirand et al., 2002) and nucleation events result in
single or multispecies associations (binary to quinary). Using
transmission electron microscopy, Kané et al., 2003 indicate primary
crystallite size of ca. 50 nm under quiescent conditions and 20–30 nm
under shear. Subsequent aggregation results in size increase to
150 nm (100 nm under shear). Other studies of suspensions of
colloidal size particles also indicate that shear can affect the formation
process (Drabarek et al., 2008; Hanley et al., 1999) at temperatures
above the cloud point. Such events are well below the resolution
limits of techniques usually deployed for determination of cloud point
or wax appearance temperature (Coutinho and Daridon, 2005), with
cross polar microscopy for example having a detection-limit of ca.
0.5 μm. Further cooling encourages both growth of existing crystals
and additional nucleation (Chang et al., 2000; Lopes-da-Silva and
Coutinho, 2007), while the resultant morphology and gel structure is
also significantly influenced by shear (Kané et al., 2004; Lorge et al.,
1997; Singh et al., 1999; Venkatesan et al., 2005; Visintin et al., 2005).
Above the cloud point, waxy oils are typically Newtonian but with
increasing quantities of suspended waxy particulates, non-Newtonian
behaviour becomes increasingly evident. The solid phase composition
and quantity both change as the temperature decreases, though the
solid phase proportion remains low (≤ 6%) even at the pour point
(Rønningsen et al., 1991). Compositional polydispersity of alkanes is
indicated as an important factor influencing the crystallization (Senra
et al., 2008) and affecting gel strength (Paso et al., 2005). Other
common constituents of crude oil such as asphaltenes and resins are
also known to affect wax crystallization (Kriz and Andersen, 2005;
Tinsley et al., 2009; Venkatesan et al., 2003). While there has been
much progress in understanding wax crystallization processes, the
compositional diversity of crude oil presents a significant challenge to
any experimental or theoretical analysis (Espada et al., 2010; Kané
et al., 2003; Zougari and Sopkow, 2007).
As the fluid cools below the wax appearance temperature (WAT),
crystal size tends to increase (in some cases to 100 μm and larger with
slow cooling for example) and crystal aggregation is usual, particu-
larly under quiescent and low shear conditions, such that the solid-
like behaviour of the waxy suspension increases. Thus at some point
between the WAT and the pour point, a transition can be determined
by small-deformation oscillatory rheometry, when the increasing
elastic response G′ (solid behaviour) becomes equal to the viscous
response G″. The transition is dependent upon wax development and
is thus strongly affected by thermal and shear conditions. This
instrumental criterion of gelation onset is considered to indicate the
initial development of an interlocking structure that, at lower
temperature, results in a (partially) self-supporting structural
 D.A. Phillips et al. / Journal of Petroleum Science and Engineering 77 (2011) 286–304
network (Lopes-da-Silva and Coutinho, 2004; Venkatesan et al.,
2002). This subsequent gel state is visually evident by slump
resistance and pour resistance and represents the gelation point
referred to in this paper. The existence of yield stress behaviour
depends upon the degree of interlocking (jammed structure) that
develops and the network fragility.
The complexities of waxy solids formation result in similar
complexity of flow behaviour in pipes and in the mechanism whereby
flow can be re-established in a developed static structural gel
(Rønningsen, 1992). Hence studies of waxy crude flow and static gel
strength have commonly focused on rotational rheometric techniques
rather than pipe or capillary based methods (Wardhaugh et al., 1988;
Wardhaugh and Boger, 1987; Wardhaugh and Boger, 1991). By
directly applying a shearing force to a sample contained within a
defined geometry, such rotational techniques enable greater precision
in terms of both measurement and theoretical interpretation.
Rotational methods have been extended to allow increasing sophis-
tication (Dimitriou et al., 2010; Ovarlez et al., 2009) leading to a better
understanding of the complex flow behaviour of yield stress fluids
particularly with respect to flow discontinuities such as shear banding
and slip. However, capillary based studies have also advanced (Isa
et al., 2007), allowing the visualization and measurement of
anomalous flow patterns in yield stress fluids. Comparable advances
in visualization techniques have also been developed for pipeflow (El-
Gendy et al., 2011). Waxy oils pose particular problems of measure-
ment and interpretation compared with simple colloidal systems,
because of a tendency to exhibit time-dependent waxy structural
change under constant temperature conditions (Chang et al., 2000;
Lopes-da-Silva and Coutinho, 2004). Such issues are especially
relevant to the evaluation of the effects of shrinkage which are
entirely thermally driven. In terms of the conditions necessary for
restart, it is important to recognise that fluids containing typically
large aggregated waxy structures can behave quite differently from
colloidal yield stress fluids (Nguyen and Boger, 1992; Wardhaugh and
Boger, 1991) and a more complex theoretical treatment of the solid-
like yielding behaviour of quiescently cooled waxy gels has been
devised (Chang et al., 1998).
4.3. Flow-induced change
To what extent the shearing effect of shrinkage flow modifies the
oil/gel behaviour is as yet not clear. Using a controlled stress
rheometer, Venkatesan et al., 2005 indicate that applying modest
levels of shear (≤5 Pa) to a model wax/oil system during cooling
markedly alters the development of gel strength in a complex manner
depending on the rate of cooling and the level of applied shear stress.
Under fast cooling of 10 °F min−1 (ca. 5.6 °C min−1), an applied
steady shear stress of 5 Pa approximately halved the gel strength
while conversely, under a stress of 2 Pa, gel strength increased to a
peak ca. 50% higher than that under quiescent (unstressed) cooling. At
lower cooling rates, the level of stress that enhanced gel strength was
also lower so that at 1 °F min−1 (ca. 0.6 °C min−1) cooling rate, a peak
yield stress, approaching double that of the quiescently cooled
sample, was induced by an applied shear stress of ca. 0.25 Pa. At
1 Pa applied stress, the yield strength of this slow cooled sample was
more than halved and at 5 Pa, was reduced to ca. 2% of the level
attained under quiescent cooling.
The contrasting effects of applied shear were attributed to a shear-
induced increase in aggregation and entanglement of waxy entities at
low stress levels but disruption of structural development as the
applied stress increases. Such stress levels are similar to or less than
those wall stresses that correspond to measured pressure gradients
during cooling in our multiport rig (Appendix B 10), though the
cooling rates were typically variable (Fig. 20) and rarely faster than
0.25 °C min−1 (0.45 °F min−1). In field lines with typically much
higher L/D ratios, equivalent cooling would induce higher wall
299
stresses. However, given that shrinkage flow is induced by internal
cohesion acting in tension rather than by an externally impressed
shear or compressive force, then the usual assumptions as to the wall
stress levels (Appendix B 10) may need modification. Note that the
deformation behaviour (creep) of static gels under applied stresses
lower than that required to fully fracture the gel and re-establish flow
cannot be considered as equivalent to similar stress levels during
shrinkage flow where such flow has continued since cooling began
and thus a full static yield stress has not yet developed. It is also
important to recognise that while the rate of deformation during
shrinkage may be very low, the accumulated strain can still be large
when compared with the sub millimetre scale of discrete aggregated
waxy structures. In field lines for example, linear displacements in
excess of 1 m would be usual in over 90% of the line length with 10 °C
cooling, even in lines as short as 3 km.
Based on the evidence presented in the foregoing citations and
assuming that the linear movement and concomitant development of
pressure gradients observed during cooling indicate flow, then the most
likely pattern of flow appears to be plug-like (Fig. 17). If so, then
shearing action will be concentrated within the near-wall annulus
where the radial velocity gradient is consequently steep. In small pipes
like the glass line (6 mm ID), the radial distance across this sheared
annulus can be much less than 1 mm and thus smaller than the potential
maximum size of discrete waxy aggregations. In consequence, there is
an increased likelihood of jamming events that can cause stick/slip.
Other factors such as depletion (where suspended solids migrate from
the high shear annulus into the core region) or the shear-induced phase
separation demonstrated by Singh et al. are also likely to result in
a significant change in flow resistance that can be regarded as slip
(Phillips et al.). However, if the adhesive fracture between the gel and
the pipewall described by Venkatesan and Fogler, 2002 and Lee et al.,
2008 were assumed to occur along the full length of the gelled column,
then no pressure gradient would be recorded because resistance to axial
shrinkage movement would be primarily the result of friction and thus
constant irrespective of the rate of movement.
However, for a plug-flow assumption during shrinkage flow, the
radial width of the sheared annulus varies continuously along the pipe
axis (as does the flow velocity) from a maximum in the fastest flow
region to a minimum near the shrinkage null. Thus the conditions that
encourage flow discontinuity (such as flow velocity, flow resistance and
width of the sheared annulus) all vary along the length of the shrinking
column. Hence, any induced flow instability is likely to be localized with
respect to the pipe axis and thus indicated by pronounced variation of
the pressure gradient profile near the affected region. The glass line
profile shown in Fig. 3 may well exemplify such a situation in the region
between the transducers at 2.3 and 4.3 m.
In the much greater diameter field lines, shrinkage flow may also
have a plug-like form but the sheared near-wall annulus would
typically have a much larger radial width compared with the
dimension of waxy aggregates. Shrinkage flow velocity is likely to
be significantly increased in accordance with the higher L/D ratios
typical of field lines. Production of waxy fluids will result in deposition
of an aged, wax-enhanced robust layer on the pipewall (Singh et al.,
2000; Singh et al., 2001) which is not wholly removed by remediation
methods such as pigging. Thus the jamming mechanism and the
adhesive fracture events that may occur in small-scale, clean, smooth-
walled pipes are far less likely in field lines but particle depletion
within the sheared zone is still possible.
Given the likelihood of plug flow during shrinkage in both laboratory
and field lines and the likely disruption of waxy structure within a
narrow near-wall annulus, then there is a consequent likelihood of
a significant radial variation in waxy structural morphology and
mechanical strength, between the largely undisturbed core region and
the high shear near-wall zone. In addition, given the continuous axial
decrease in shrinkage flow velocity toward zero at a shrinkage null, then
there is also likely to be an axial variation in waxy structure within the
300 D.A. Phillips et al. / Journal of Petroleum Science and Engineering 77 (2011) 286–304
sheared annulus. The resultant variation in oil/gel flow resistance may
be further accentuated by topographical factors in field lines such that
there may be multiple flow directions (away from high points for
example) each with its own velocity profile.
4.4. Void formation
The shrinkage flow postulate assumes that with reducing pressure
there is a tendency for void formation once that pressure approaches
the liquid/gel SVP. Thus, where a pressure gradient exists, void
formation is likely to be localized within the line sections where the
lowest pressures develop. While the most probable first event is the
formation of a vapour bubble, this may lead to full diametric fracture if
the thermally induced imperative for shrinkage requires additional
shrinkage flow because the bubble inevitably reduces the overall
cohesive limit in the adjacent liquid/gel. This sequence is illustrated in
Fig. 23.
Bubble voids and full diametric fractures were observed during the
glass line tests (Figs. 6, 13 and 14). In all cases the void formation
appeared to coincide with a reduction in pressure to approximately
−5 psig (assumed to be the effective SVP at 18 °C) and thus tended to
form at the sites of lowest pressure near the respective shrinkage null-
points. Nearly all the voids that formed in the glass line tests resulted
in diametric fracture and axial separation.
Under essentially static conditions (as for example at the
shrinkage nulls or in sealed horizontal configuration laboratory test
lines), the flow-induced tendency for void expansion by diametric
fracture is limited or absent and the pattern of void growth might then
resemble the forms illustrated by Hénaut et al., 1999— a voided
segment at the top of the pipe section with slow cooling, or a more or
less radially central voidspace and discrete radially directed fractures
under fast cooling. However, as stated by Hénaut et al., field pipelines
typically undergo slow cooling and are thus subject to a gravity-
induced topographical influence. Given that topographical gradients
of field lines (terrestrial or sub-sea continental shelf) are rarely less
than 1:500, then an axially directed vector component of gravity is
present with a consequent tendency for axially directed flow from
high points to low points. Such asymmetry also arises if one or both
ends of the line are exposed to atmospheric pressure as in the case of
most of the tests reported in this paper. Hence, with cooling and
shrinkage, voidspace initially forms at high points in the line.
If a cooling-induced pressure gradient subsequently develops so as
to reduce the pressure within the liquid/gel column towards the SVP,
then voidspace may be created at the sites of low pressure.
Conversely, if the hydrostatic pressure is high, then although a
Fig. 23. Micrograph illustrating the development of a shrinkage-induced fracture from
an initial bubble-void. The outline of the original bubble is indicated by the yellow
arrow.
cooling-induced pressure gradient may develop, the absolute pres-
sure may never approach the SVP within the oil/gel and all voidspace
will be confined to the high points. Thus in the case of a line where the
high points are located at one or both line ends and hydrostatic
pressure in the main body of the liquid/gel prevents pressure
reduction below the SVP, then little or no voidspace is entrained
within the gel and there will be no significant void-induced change in
gel compressibility. Where line high points occur at intermediate
distances along the length (forming vertices) or where hydrostatic
pressure is modest such that shrinkage flow can reduce the line
pressure below the SVP in some localities, then voidspace will be
entrained at discrete sites within the gel column and thus alter the
overall compressibility.
Therefore, in field lines or in laboratory rigs that are exposed to
atmosphere or provided with some form of gravity head, the
distribution of voidspace will never be homogenous along the full
length of the gel and the effect of such discretized axial distribution of
voidspace is likely to engender discontinuity in the progression of gel
breakdown during restart. Such a situation has been modeled for live,
multiphase flowlines where the high SVP and large quantities of gas
phase encourage the development of discrete plugs of oil/gel
separated by gas-filled voidspace (Davidson et al., 2007; Nossen et
al., 2003). Thus the assumption that the voidspace is uniformly
distributed along the gel column and in consequence exhibits axially
uniform compressibility (Cawkwell and Charles, 1987; Lee et al.,
2008) is not appropriate in the case of discontinuous void distribution.
4.5. Compressibility
The inclusion of voidspace within the oil/gel column has long been
regarded as likely to assist the restart process (Cawkwell and Charles,
1987; Davidson et al., 2007; Gill and Russell, 1954; Hénaut et al., 1999;
Lee, 2008; Nossen et al., 2003; Perkins and Turner, 1971; Thomason,
2000; Verschuur et al., 1971b; Vinay et al., 2007; Wachs et al., 2009;
Williams et al., 1996).
However, the effect of compressibility with respect to restart
resistance is difficult to measure. Perkins and Turner used a flexible
walled pipe to mimic the effect of increasing compressibility. Hénaut
et al. induced voidspace in an oil/gel sample by cooling in test cell
fitted with an axially movable piston to allow gel compression. The
pressures recorded during tests at two temperatures which were
reported in Fig. 3 of that paper, indicated high initial compressibility
as the voidspace is compressed to a small volume, followed by
markedly lower compressibility which reflects the compression
response of the void-free oil/gel.
If the fugacity of the adjacent gel is low then re-dissolution of
vapour from the void under increased pressure may be very low
during the test timeframe and thus an approximation of isothermal
void compression may be represented as obeying gas laws. By
applying published compressibility for dodecane (from the NIST
Chemistry WebBook), an approximation of volume change for the
(void-free) oil/gel may be calculated. Dodecane was selected to
represent the oil/gel on the basis that while the higher alkanes (and
the waxy solids) display somewhat lower compressibility, there will
be a small proportion of lower alkanes present that display
significantly greater compressibility. If the remaining measured
volume change is assumed to be compressed voidspace (ca. 97%
compressed at the highest experimental pressure of 3000 kPa), then a
corresponding gas-law compression can be calculated for the entire
experimental pressure range. The two calculated volume changes (for
the oil/gel represented by dodecane and for the vapour void) are then
added together to provide an estimate of the compressive behaviour
of the voided oil/gel over the experimental pressure range. The results
of such calculation are shown in Fig. 24 where the composite of the
gas-law void compression and the dodecane compression is shown
together with the experimental results at 23 °C presented by Hénaut
 D.A. Phillips et al. / Journal of Petroleum Science and Engineering 77 (2011) 286–304
Experimental and calculated compression
of an oil/gel and vapour void
0.10
0.08
0.06
ΔV/V0
0.04
Gas law + dodecane
Hénaut
Dodecane
0.02
0.00
0 1000 2000 3000
Pressure kPa
Fig. 24. Comparison of the Hénaut et al. experimental results for compression of a
voided oil/gel at 23 °C with void-free dodecane and calculated values based on the
combined compression for dodecane and a void that obeys gas-law behaviour.
et al. The much lower volume change of the void-free dodecane is also
shown for comparison. Given that the sample demonstrated a yield
stress, then the process of fracturing the waxy framework may also
contribute a resistance to compression particularly at the initial stage
where displacement (and consequent strain) is large for modest
pressure increase. This may account for the discrepancy between the
calculated and experimental values at low measured pressures. The
results of this calculation contrast with those of Lee, 2008 and Lee et
al., 2008, where application of a Tait expression provides a reasonable
fit for the Hénaut et al. experimental values of ≤200 kPa but less well
at higher pressures that are more relevant to field restart.
4.6. Pressure propagation
The efficiency of hydraulic actuation systems relies upon the near
instantaneous transmission of applied pressure. However, our
experience of recording pressure rise during restart tests in the
multiport lines indicates significant delay in the rate of pressure
propagation along the line. This observation accords with similar
reported experience (Borghi et al., 2003; Davenport and Somper,
1971; Rønningsen, 1992; Smith and Ramsden, 1978; Thomason, 2000;
Uhde and Kopp, 1971). Investigation of this phenomenon indicated
that the rate of pressure propagation can be directly related to a
change in the fluid viscosity for a simple Newtonian fluid but is
independent of the amount of applied pressure, assuming a rigid,
void-free pipeline and constant fluid compressibility. This is logically
consistent in that the fluid must be progressively compressed in order
to transmit the pressure along the line and the rate at which this
compression occurs is dictated by the flow resistance of the fluid. Thus
assuming the same fluid compressibility and flow resistance, then a
301
doubling of applied pressure requires twice the axial displacement to
attain an equilibrium compressed volume, but at double the pressure,
the flow rate is also doubled such that the compression time remains
constant.
However, we also discovered experimentally, that a modest (b1%)
volume of entrained voidspace dramatically slowed the rate of
pressure propagation for a high viscosity Newtonian liquid. Such a
result is consistent with long established experience of the deleterious
delaying effect of void inclusion in hydraulic actuators such as motor
vehicle braking systems for example.
In the light of these observations and the likelihood that entrained
voidspace will be axially discontinuous (Section 4.3) rather than
uniformly distributed through the oil/gel column, we have assumed
that each discrete void will only assist restart if there is a rapid and
significant additional breakdown of waxy structure as the material
surges into each voidspace. Our attempts at modeling such transient
events indicate that while the inclusion of voids delays the pressure
propagation, the effect of enhanced transient breakdown of apparent
viscosity markedly reduces the time taken to clear the line once the
pressure wave reaches the line end. Note that, unlike the Newtonian
case, the non-Newtonian simulations proved sensitive to the level of
applied pressure. The rate of pressure propagation increased with
increasing applied pressure in accordance with the assumed degree
and rate of breakdown of the gel to lower apparent viscosity.
However, the inclusion of voids invariably slowed the progress of
pressure rise along the line (compared with the void-free case)
because the initial pressure rise was insufficient to produce significant
gel breakdown. These numerical simulations also indicate that the
axial distribution and the size (length) of each void are critical factors.
However, experimental support for these conclusions remains as a
target for ongoing study.
5. Conclusions
Experimental evidence is presented in support of the postulate
that pressure gradients which develop during cooling of flowable
media in pipes, indicate that the media exhibits high resistance to the
flow that occurs in response to thermal shrinkage. A direct
relationship is demonstrated between the extent and rate of
shrinkage flow and the extent and rate of cooling in a manner
comparable to the function of liquid-in-glass thermometers. A similar
direct relationship is shown between the known viscous resistance of
a shrinking liquid and the concurrent development of pressure
gradients. It is also shown that some form of axially directed
asymmetry must be present such as to direct the shrinkage flow
that is engendered by molecular cohesion. The presence of such
asymmetry in the form of an axially directed vector component of
gravity or by exposure of one or both pipe-ends to atmospheric
pressure is suggested as responsible for inducing an axial flow
direction. The same external forces are deemed responsible for
sufficient radial flow so as to compensate the radial shrinkage of the
deformable media. Thus shrinkage flow may be regarded as a non-
affine translation producing true shearing deformation flow without
which pressure transducers cannot be actuated.
Example numerical simulations are presented for two widely
familiar rheological models of non-Newtonian fluid flow for a given
shrinkage flow rate and a given overall line pressure drop. The
resultant calculated pressure profiles are shown to significantly differ
from the equivalent profile for a Newtonian fluid. Experimental
determination of a cooling-induced pressure profile for a shear-
insensitive liquid supports the theoretical analysis that such Newto-
nian profiles exhibit a quadratic format. We conclude that if a fluid
exhibits significant non-linearity of flow behaviour (non-Newtonian),
then the pressure profile during cooling is likely to differ from the
Newtonian quadratic form such as to display increasing linearity of
pressure profile with increasing non-linearity of flow behaviour.
302 D.A. Phillips et al. / Journal of Petroleum Science and Engineering 77 (2011) 286–304

Contrasting simulations are also shown on the basis of assumed Appendix A (continued)
permeation flow and an advancing series of flow-induced rupture Fluid 7 — Black medium/high viscosity oil.
events. We conclude that on the basis of observations, that the Wax appearance temperature by CPM 49 °C
Upper pour point 30 °C
permeation flow model has yet to be demonstrated.
Lower pour point 3 °C
From cited evidence of the effect of shear-induced disruption of Fluid 8 — Model fluid is a blend comprising 80% Fluid 4 and 20% Newtonian
waxy solid structural development, it is deemed likely that shrinkage standard N190000.
flow will induce similar effects, such as to alter the flow resistance of Lower pour point 30 °C
the oil/gel. Given the inherent axial variation in shrinkage flow Newtonian standard N190000 — added to Model Fluid 8.
Certified viscosity 33.78 Pa s at 60 °C
velocity, then a concomitant variation of modified gel state along the
146.5 Pa s at 40 °C
pipeline is indicated. Similarly, given the likely plug-like flow form of 532.2 Pa s at 25 °C
non-Newtonian fluids at low flow rates, then a corresponding radial 860.3 Pa s at 20 °C
variation of induced gel state is also indicated. Uniform fluid-temperature pour point was determined at 18 °C
Newtonian standard N5100
Hence, numerical simulation of cooling-induced flow on the basis of
Certified viscosity 0.1435 Pa s at 100 °C
measured sample flow behaviour and line topography is likely to yield a 0.3588 Pa s at 80 °C
more realistic estimate of oil/gel state prior to restart than the currently 1.107 Pa s at 60 °C
common assumption of cooling under quiescent (no shear) conditions. 2.141 Pa s at 50 °C
Further evidence is provided to support the postulate that pressure 4.45 Pa s at 40 °C
15.58 Pa s at 25 °C
reduction induced by shrinkage flow can result in cohesive failure and
24.76 Pa s at 20 °C
the formation of voids at sites of low pressure.
The implications of void formation processes are discussed with
respect to the distribution of such voids and the effect that they might Appendix B
have upon the progression of line restart. We conclude that
application of numerical simulation to determine the likelihood and In laminar flow of a simple Newtonian liquid, volume flow rate Q is
location of voids within the oil/gel column also offers potential described by the Hagen–Poiseuille equation:
improvement in the accuracy of restart prediction.
4
Q = πR ΔP = ð8LηÞ ðB:1Þ
Acknowledgements
where R is the pipe radius at the wall, ΔP is the pressure drop along a
The authors would like to thank the management of BP given pipe length L and η is the liquid flow resistance (viscosity).
Exploration Operating Company and Kernow Analytical Technology The equivalent relationship for a power-law liquid is given by the
for their permission to publish this paper. The authors also wish to Weissenberg–Rabinowitsch expression:
thank Adrian Johnson of Whitewood Ltd for information and guidance
relating to current field practice.  
3 ð1 = nÞ
Q = πR n = ð3n + 1Þ ðΔPR = ð2KLÞÞ ðB:2Þ
Appendix A
where K is the liquid consistency (intrinsic viscosity) and n is the
Fluids used for tests and modeling example exercises described in power-law index derived from the relationship between shear stress
this paper and in Phillips et al., in press. Note that the pour points are and shear strain rate for that fluid.
in accord with ASTM test protocols D97 and D5853. Thus the cited For a Bingham fluid the Buckingham–Reiner equation applies:
pour point temperatures may be up to 3 °C above the actual gelation
temperature. Wherever possible we have modified the ASTM pro-   
4 4
tocols to allow a record of the gelation point to within ±1 °C as cited Q = πR ΔP = ð8LηB Þ 1−4 = 3ðrB = RÞ + 1 = 3ðrB =RÞ ðB:3Þ
in the Materials and methods section.

where ηB is the Bingham viscosity and rB is the Bingham radius which

Fluid 1 — Black moderate viscosity oil. is described by:
Wax content by BP237 8%
Wax appearance temperature 34 °C by crossed-polar-microscopy (CPM)
rB = 2LτB = ΔP ðB:4Þ
Upper pour point 19 °C
Lower pour point 2 °C
Fluid 2 — Black moderate viscosity oil.
where τB is the Bingham yield stress.
Wax content by BP237 7.2%
Wax appearance temperature by CPM 32.5 °C The velocity Vr in any annulus of radius r during laminar flow of a
Upper pour point 8 °C simple Newtonian liquid may be calculated from:
Lower pour point −6 °C
Fluid 3 — Translucent condensate of low viscosity above the pour point.   
2 2
Upper pour point 17 °C Vr = 4Q = 2πR 1−ðr= RÞ ðB:5Þ
Lower pour point 14 °C
Fluid 4 — Translucent condensate of low viscosity above the pour point.
Wax content by BP237 14% For a power-law fluid the equivalent expression becomes:
Wax appearance temperature by CPM 40 °C
Upper pour point 27 °C   
2 ðn + 1 Þ = n
Lower pour point 24 °C Vr = ð3n + 1ÞQ = ðn + 1ÞπR 1−ðr=RÞ ðB:6Þ
Fluid 5 — Black medium/high viscosity oil.
Wax appearance temperature by CPM 42 °C
Upper pour point 15 °C For a Bingham fluid the velocity of the plug region (r ≤ rB) is given
Lower pour point −3 °C by:
Fluid 6 — Black medium/high viscosity oil.
Wax appearance temperature by CPM 45 °C
Upper pour point 18 °C 2 2
Vr = ΔPR = ð4ηB LÞ ð1−ðrB =RÞÞ ðB:7Þ
 D.A. Phillips et al. / Journal of Petroleum Science and Engineering 77 (2011) 286–304
Outside of the plug region, the velocity Vr in any annulus of radius
r (r ≥ rB) is given by:
   
2 2 2
Vr = ΔPR = ð4ηB LÞ 1− r = R −2ðrB = RÞ ð1−r = RÞ ðB:8Þ
Flow through porous media is described by the Darcy equation:
Q = ðkA = ηÞ ðΔP = LÞ ðB:9Þ
where k is the permeability of the porous medium (wax matrix), A is
the cross sectional area of the pipe and η is the viscosity (of the wax-
depleted continuous phase oil in the examples shown in Fig. 18).
In all cases, the shear stress at the pipewall τW is given by:
τW = 0:5RðΔP = LÞ ðB:10Þ
SI units
Units of pressure used in this paper are the units recorded by the
transducers and gauges used during laboratory experimentation. The
same units were used in numerical modelling exercises to allow
immediate comparison with laboratory measurement.
The pressure transducers deployed for test measurement were of
differential construction and recorded pressures represent the
difference between the test measure and the level of atmospheric
pressure in the laboratory at the time of measurement. Hence the
units, pound force per square inch gauge (psig) and bar gauge (barg)
can only be represented in terms of absolute pressure if related to the
exact atmospheric pressure at the time of measurement.
Atmospheric pressure was not recorded during laboratory testing
and exact conversion into absolute pressure equivalent is not possible.
However, an approximate conversion may be achieved by assuming
atmospheric pressure equal to the standard atmospheric pressure
(atm) and an accepted approximation of the SI equivalent of the unit
pound force per square inch (psi):
1atm = 101325Pa
−2 3
1lbfin ðpsiÞ≈6:894757 × 10 Pa
1atm≈14:696 psi absolute ðpsiaÞ
Thus a given pressure PPSIG may be approximately converted to an
absolute pressure equivalent (PSI) in kilo Pascals (kPa) by:
PSI kPa ðabsÞ≈6:894757 ðPPSIG + 14:696Þ
Gauge pressure in bar units PBARG may be similarly converted
where:
1bar = 100 000 Pa
PSI kPa ðabsÞ = 100 ðPBARG + 101:325Þ
Temperature values have been given in centigrade units (°C) and
are the units recorded by the thermometers used during laboratory
experimentation. The absolute temperature equivalent of a given
temperature TTEST °C can be converted to an absolute temperature in
units Kelvin ( TABS °K) by:
TABS°K = TTEST°C + 273:15
The SI unit for the rate of shear strain is the reciprocal second (s−1)
where a shear rate of 1 s−1 is obtained in a Newtonian fluid flowing at
1 m s−1 between two parallel plates 1 m apart.
303
The widely used centiPoise unit of viscosity (cP) is related to the SI
unit, the Pascal second (Pa s) as:
−3
1cP = 1 × 10 Pa·s
Some measurement units have been given for convenience in
multiples or sub−multiples of SI units such as the linear units
kilometres (km) and millimetres (mm) where:
1 km = 1000 m
1 mm = 0:001 m
and the mega-Pascal (MPa) pressure unit where:
6
1 MPa = 1 × 10 Pa
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