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Rheo354-355 - Pharma - Thixotropy
Rheo354-355 - Pharma - Thixotropy
Rheo354-355 - Pharma - Thixotropy
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Tim’s Top Tips - How To Measure Thixotropy For Pharmaceutical And Cosmetice rmpIndustries
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Tim’s Top Tips - How To Measure Thixotropy For Pharmaceutical And Cosmetic Industries
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Tim's Top Tips - Rheology Solutions for the Pharmaceutical
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Pharmaceutical And Cosmetic Industries
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Key Words: Rheology, rotational, liquid, viscosity, thixotropy, yield stress.
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About The Author Introduction
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Tim has a background in
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Often the cosmetics and pharmaceutical industries must
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engineering and specifically in overcome problems related to (and often dominated by) the flow
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rheology, with a B.Eng and Ph.D. in properties of their product, though the relationships between
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Chemical Engineering and has held these properties and production related issues are not always
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postdoctoral research positions in immediately apparent. It is the purpose of this series of articles,
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engineering rheology. Tim's
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“Rheology Solutions for the Pharmaceutical and Cosmetic
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research has continued for the last
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Industries”, to help illuminate the issues faced by the industry,
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seven years and recent interests
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how they relate to the flow properties of problem materials and
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and publications include the
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how they can be successfully measured and controlled with a
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application of rheology and rheometry to mineral, food, polymer heo
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and surface coatings systems. His current position encompasses
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customer focussed education and training. Additionally he is
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available to provide technical input for existing or proposed
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materials characterisation systems for both laboratory and Thixotropy is a form of time dependent behaviour describing a
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production. material whose viscosity decreases over time while it is subjected
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Table Of Contents
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Thixotropy should not be confused with rheopexy, a rare
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Introduction..........................................................3
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Definitions ............................................................3 increases with time). The following techniques and discussions
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Experimental procedure
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3. The shear and recovery test ..............................8 apply for rheodestructive measurements also.
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Summary ............................................................11
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Pharmaceutical and cosmetic dictionary ..............13 Thixotropy is a relative measurement and as such depends on
nisa tion
Information request form ....................................17 the experimental conditions and technique used to measure it.
There are several such techniques, the simplest being modified
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Tim’s Top Tips - How To Measure Thixotropy For Pharmaceutical And Cosmetic Industries
• A viscometer or rheometer
In general a viscometer can make only CR measurements - in
other words flow and viscosity curves are the main purpose
of the instruments. As a result thixotropy loops, and steady
shear measurements can also be made with these
instruments. A rheometer is capable of much more, including
viscoelastic measurements, creep and recovery
measurements and so on. CS instruments have an air
bearing so that these extra measurements can be made. The
air bearing also allows shear and recovery measurements to
be made because they can probe the structure of the
material without influencing the rate at which it rebuilds.
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maximum shear rate back to zero shear again (called the down-
e cif
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g
t
a
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stry s
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curve). The rate of change of shear rate for the up- and down-
i negs t i
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m i
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curves and the time at maximum shear rate are user defined and
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the number of data points is usually high so that a continuous
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test
moelry
curve is generated. Plotting the results as shear rate vs. shear
p e c
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stress or viscosity (Figure 3), if the up-curve lies above the down-
s
s
d
g
p o l y m•ep o
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curve and the measurement can be repeated after some rest
n
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time, then the material is thixotropic.
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Figure 2: Input for ramp test
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1.1 Experimental procedure
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The experimental layout can be one shown in Figure 1.
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Figure 1: Standard viscometric geometries (L to R) Cup & Bob,
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Cone & Plate, Plate & Plate
p l i o r y •r i a l t e s t i n
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• The material is loaded and the measuring geometry closed.
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• Theory
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• A lower and an upper shear rate (CR) or shear stress (CS) is
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The theory for this type of measurement is that the flow m
s la
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chosen, as is the number of measurement points between heo
n • a bpos r•a m a t
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behaviour is defined for a range of shear rates and shear
t i
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them.
a
o
p
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stresses so that its reaction to different processing conditions
i
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ica
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• The material is subjected to a shear rate profile, like in Figure
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calculated as follows:
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(1)
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η = viscosity, mPa.s or cP (1mPa.s = 1cP)
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could be used rather than ramp tests (see “How to measure flow
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Tim’s Top Tips - How To Measure Thixotropy For Pharmaceutical And Cosmetic Industries
• The reaction of the material to the imposed shear rate • Sensor inertia
(reaction = shear stress) or shear stress (reaction = shear Sensors, in particular concentric cylinders and large diameter
rate) is measured and the viscosity calculated according to cones or plates may be quite heavy. As the rate of rotation
equation (1). changes through the ramp test, this weight causes the
sensors to accelerate to a higher speed than expected by the
• The result of the experiment is a thixotropy loop, as control software in the viscometer or rheometer and so the
illustrated in Figure 3. shear rate experienced by the material is higher than that
'imposed' by the controller. This results in a shift in shear
• The thixotropy of different materials can be compared by stresses and viscosities for the flow curve from the actual
comparing the area bounded by the thixotropy loop, as ones. This effect can be reduced or removed by allowing
illustrated in Figure 3. sufficient time for the ramp. A general rule of thumb is to
allow at least 1s of test time for every 1s-1 of shear rate in the
1.2 Benefits of the thixotropy loop test ramp. So, a ramp from 0-100s-1 should take at least 100s to
complete.
• The complete picture
A ramp test can provide a complete picture of how the • Time
material will behave between the set experimental limits. Because of the potential problems with inertia, ramp tests
covering very wide ranges of shear rate can take
• Simple measurement and simple analysis considerable time to complete. On the other hand, because
The measurement is quite simple to execute and the data is the test is a relative one, the maximum shear rate can be
straightforward to process. defined to shorten the duration of all tests if necessary.
rk
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Tim’s Top Tips - How To Measure Thixotropy For Pharmaceutical And CosmeticrmpIndustries
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• Slip • The reaction of the material to the imposed shear rate
e cif
r
c
g
t
a
n
stry s
urf
Multi-phase systems, tend to slip at the boundary of the (reaction = shear stress) or shear stress (reaction = shear
i negs t i
y sp
m i
s
measuring geometry. A major assumption for rheological rate) is measured and the viscosity calculated according to
t
e
•
ustr
ruments • contract testing • indu
r
t
g
s
e
measurements is that the first layer of material 'sticks' to the equation (1).
i fi c
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n
m
t
i
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test
moelry
walls of the measuring geometry. Plate & plate or concentric
p e c
r s •l y p
cylinder geometry walls can be roughened or serrated to • The results of the steady shear rate experiment are viscosity
s
s
d
g
p o l y m•ep o
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reduce or remove the slip phenomenon. and shear stress curves, as illustrated in Figure 5.
n
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t
i
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s
s
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• Time dependent materials
n
The thixotropy of different materials can be compared by
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esting • i
Sample handling and experimental technique can be crucial comparing the times taken to reach a certain % of the initial
semin
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p
for repeatably measuring time dependent (eg thixotropic) shear stress, or some fixed value of the shear stress, or an
s f
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o
materials. The same handling procedure (pouring, mixing, equilibrium value (see Figure 5).
n gi npsrto d u c t s •
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ical QC systems
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resting, loading into the test equipment etc) and
s
c
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a
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experimental procedure (rest time, ramp time and upper and
t r
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lower limits) is critical for repeatable measurements, and it
Q
c o
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must be remembered that for time dependent materials the
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results are relative only - they depend on the technique used
p
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to generate them.
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2.0 The constant shear test
n
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b l
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The following discussion is based on a CR test, but the
u
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c
t
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arguments hold equally for CS tests, where the shear rate is
s
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monitored as a function of time.
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p l i o r y •r i a l t e s t i n
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atory
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The constant shear technique involves imposing a single,
o
s
i
b
ter
r
b
e
r
r
a
constant shear rate (of shear stress) on the material and
o
a
t
a
e
b
s
m
m
s la
n
monitoring the response. The results are usually compared by an
e
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n • a bpos r•a m a t
s•
i
assessment of the time taken to reach a certain predetermined
t
n
a
o
p
r
c
t
i
o
shear stress or viscosity, or to achieve a predetermined % of the
t
•
ica
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Figure 5: Results from a constant shear test
e
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initial or final value, or by the time taken to achieve an
k
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equilibrium value
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•
t i
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• Sensor inertia
ls ch
m erisa
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m
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trud
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tw i n s c s cie nc e ha ract
a
s
x
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re w e o f
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re w
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t
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r i
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lyme
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w
the
i e
s
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p
are known.
dedicated to the
do rsg a n i s a t i oencdoendt ri coal t•e dt r taoi n i n g c o u r s e s
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• Time
ion dedica
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m
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4.
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Tim’s Top Tips - How To Measure Thixotropy For Pharmaceutical And Cosmetic Industries
2.3 Potential problems with the constant shear test • Chaotic flow
One of the key assumptions for rheological measurements is
A single test does not fully describe whether or not the sample that the flow in the measuring gap is laminar. Too high shear
is thixotropic, or if rheodestruction has taken place. Consecutive rates can cause the flow regime to become turbulent and the
curves after fixed rest times are necessary to assess the recovery measurements are unreliable. The onset of chaotic flow can
of the material. be overcome or delayed by changing the measuring
geometry or the measurement gap.
• Solid fraction size
For multiphase systems, often there is a solid fraction, which • Slip
has particles of considerable size. If this size is close to the Multi-phase systems tend to slip at the boundary of the
size of the measuring gap, then one or more particles may measuring geometry. A major assumption for rheological
'bridge' the gap and cause an artificially high shear stress. measurements is that the first layer of material 'sticks' to the
The problem can be solved by choosing a measurement walls of the measuring geometry. Plate & plate or concentric
geometry so that maximum particle size is no more than 1/3 cylinder geometry walls can be roughened or serrated to
of the gap size (1/10 for concentrated pastes). Sometimes reduce or remove the slip phenomenon.
larger particles contribute little to the overall flow behaviour
of the material and can be removed without large penalties • Time dependent materials
for the applicability of the measurement. Sample handling and experimental technique can be crucial
for repeatably measuring time dependent (eg thixotropic)
• Early warning of problems with technique or materials. The same handling procedure (pouring, mixing,
measurement resting, loading into the test equipment etc) and
Having data for the complete range of shear rates allows the experimental procedure (rest time, ramp time and upper and
user to investigate the possibility of settling, chaotic flow in lower limits) is critical for repeatable measurements, and it
the measuring gap and slip at the measurement geometry must be remembered that for time dependent materials the
walls. Data from a single shear rate test may not reveal this results are relative only - they depend on the technique used
information readily, especially if only a few data points are to generate them.
taken. Often in these cases settling materials will appear to
be thixotropic as the shear stress generally drops while the 3.0 The shear and recovery test
material settles.
The following discussion is based on a CS/CR/CS test, but the
• Temperature control arguments hold equally for CS/CS/CS tests, where the viscosity of
At high shear rates, shear heating can be an issue. Shear the middle segment is dictated by the imposition of a high shear
heating is caused by internal frictional heat generated as the stress for a short time.
lamina of fluid move over each other. When the measuring
gap is small this can usually be successfully controlled, but The shear and recover technique involves non-destructive
prolonged exposure to high shear rates can still be a evaluation of the initial structure, using an oscillatory
problem. To reduce this, the steady shear chosen for the test measurement, followed by a highly destructive rotation segment
can be reduced to reduce or remove the likelihood of shear at high shear rate or shear stress. These two are immediately
heating. followed by a non-destructive oscillatory measurement identical
in its settings to the first segment, observing structure rebuild.
• Settling materials The results are usually compared by an assessment of the time
If a material tends to settle, long test times tend to reduce taken to finally regain a certain predetermined viscosity, or to
the likelihood of successful test outcomes. The longer the achieve a predetermined % of the initial value, or by the time
test takes, the more likely the solid fraction is to have settled taken to achieve an equilibrium value.
out of the measurement space, or at least created a
concentration gradient through it. Sometimes it is possible
to step from high to low shear rates, rather than the other
way around, allowing the material to be kept in suspension
longer, and if possible to reduce step times as much as
practicable. Alternatively using a modified step test with
high shear steps to resuspend materials between descending
'measurement' steps can also be successful. A settling
material will appear to be thixotropic as the shear stress
generally drops while the material settles. Figure 6: Input for shear and recovery test
rk
qs u&i p he •
wo
s e
mi t y vic
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v r
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a se
ggr
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p epa
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Tim’s Top Tips - How To Measure Thixotropy For Pharmaceutical And CosmeticrmpIndustries
ra
s
r
r
ai
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e
• s•
an
th
ina
op
t
sh
e
en m en
ar
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em
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w oce
i
ts
fic s
sem
u
nd en
t r
c i
s
m
nar s
ins in
peci
c
u
e
a
i
3.1 Experimental procedure • Shear heating
e cif
r
c
g
t
a
n
stry s
urf
These tests, including the high shear segment can be set up
i negs t i
y sp
m i
s
The experimental layout can be one shown in Figure 1. to reduce the likelihood of shear heating.
t
e
•
ustr
ruments • contract testing • indu
r
t
g
s
e
i fi c
e
n
m
t
i
• ind
• Simple analysis
test
• The material is loaded and the measuring geometry closed.
moelry
e c
The data is straightforward to process.
r s •l y p
s
s
d
g
• The parameters (determined before) for the oscillatory and
p o l y m•ep o
y
i
n
r
o l
t
i
high shear segments are chosen.
t
s
3.3 Potential problems with the shear and recovery
s
ars •
e r
n
test
olym
esting • i
• The material is subjected to a shear rate profile, like in Figure
semin
o r
6.
p
f
• More complicated measurement
s
r
m
o
The measurement is not as straightforward to set up, as
n gi npsrto d u c t s •
f
e
• The reaction of the material to the imposed deformation (for
ical QC systems
t
t
s
some preliminary work needs to be done to find the Linear
y
oscillatory measurements it is convenient to use the complex
s
r
Viscoelastic Envelope (LVE) for the oscillatory segments.
C
viscosity), shear rate (reaction = shear stress) or shear stress
Q
o
(reaction = shear rate) is measured and the viscosity Experienced operators can quickly achieve this.
a l
•
c
calculated according to equation (1).
mke rt etsetsitnig
i
s
t
• Instrument
p
n
o
strume
A CS instrument is required for this type of measurement,
t
• The results of the steady shear rate experiment are viscosity
t
p
s
o
ts
which is usually more costly, and also involves the need for
e
vs. time curves, as illustrated in Figure 7.
t
bber & on blac
rumen
•
k
a supply of clean, oil-free compressed air.
n
s
c
t
t
i
a
s
n
a
l
The thixotropy of different materials can be compared by
b
e
l
n
e
g inst
• Solid fraction size
n
i
b
comparing the times taken to reach a certain % of the initial
t
u
r
o
s
a
e
r
For multiphase systems, often there is a solid fraction, which
• carb
c
t
shear stress, or some fixed value of the shear stress, or an
t
s
y•
n
k
n
has particles of considerable size. If this size is close to the
i
equilibrium value (see Figure 5).
t
a
s
g
r
u
size of the measuring gap, then one or more particles may
bl
o
e
p l i o r y •r i a l t e s t i n
r
atory
t
a t
•
n
'bridge' the gap and cause an artificially high shear stress.
l
r
a
o
o
s
i
b
ter
r
b
The problem can be solved by choosing a measuring
e
r
r
a
o
a
t
a
e
b
geometry so that maximum particle size is no more than 1/3
m
m
s la
n
e
heo
n • a bpos r•a m a t
of the gap size (1/10 for concentrated pastes). Sometimes
s•
t i
n
a
o
p
larger particles contribute little to the overall flow behaviour
r
c
t
i
o
t
•
ica
h
of the material and can be removed without large penalties
e
k s
c
appl
a toi or kns hl o
i
r
for the applicability of the measurement.
v
o
r
s•w
s e
•
s&
i
• Early warning of problems with technique or
t
n
wa
eter
io
s
aertaepr sp l i c
r
measurement
i
•
i
ris at
a
e
p
Having data for the complete range of shear rates allows the m
c
e
vi iaslcs n • a
o
r
e
isc
user to investigate the possibility of settling, chaotic flow in
ts •
c t
mh
a
v
c
ar
n
•
t i
e
ls ch
m erisa
walls. Data from a single shear rate test may not reveal this
ers
m
trud
t
teria
tw i n s c s cie nc e ha ract
r a
s
m
n
re w
r
ls c
i
xt
t
f
s
• Monitors recovery
e
in sc
• Settling materials
t
r i
e
e
r
mat
c
f
o
s
o
o
p
test takes, the more likely the solid fraction is to have settled
dedicated to the
do rsg a n i s a t i oencdoendt ri coal t•e dt r taoi n i n g c o u r s e s
t
ce
are known.
o
• Time
organis at
nisa tion
orga
r
n d es c o n t
ratur
ice
e
d ssael e s t e m p e
e s aa t u r
erv
l i s tt e mt s • o p
s a lp e r
p
sup
st
Tim’s Top Tips - How To Measure Thixotropy For Pharmaceutical And Cosmetic Industries
• Chaotic flow
One of the key assumptions for rheological measurements is
that the flow in the measuring gap is laminar. Too high shear
rates can cause the flow regime to become turbulent and the
measurements are unreliable. The onset of chaotic flow can
be overcome or delayed by changing the measuring
geometry or the measurement gap.
• Slip
Multi-phase systems tend to slip at the boundary of the
measuring geometry. A major assumption for rheological
measurements is that the first layer of material 'sticks' to the
walls of the measuring geometry. Plate & plate or concentric
cylinder geometry walls can be roughened or serrated to
reduce or remove the slip phenomenon.
rk
qs u&i p he •
wo
s e
mi t y vic
ks
v r
ir
a se
ggr
or
nd
p epa
roo &
w
Tim’s Top Tips - How To Measure Thixotropy For Pharmaceutical And CosmeticrmpIndustries
ra
s
r
r
ai
d
e
• s•
an
th
ina
op
t
sh
e
en m en
ar
rk&
em
r
n
w oce
i
ts
fic s
sem
u
nd en
t r
c i
s
m
nar s
ins in
peci
c
u
e
a
i
Summary
e cif
r
c
g
t
a
n
stry s
urf
Determining the most suitable type of measurement or
i negs t i
y sp
m i
s
instrument is not simply a matter of adding up the ranking for
t
e
•
Table 1 summarises the possibilities for measuring a flow or
ustr
ruments • contract testing • indu
r
t
g
each. Rather, identify which measurement technique, variable etc
s
e
i fi c
e
n
m
viscosity curve using the techniques discussed. Each of the
t
i
• ind
test
is most relevant and appropriate for your application/product.
moelry
c
techniques is ranked between 0 and 5 for each of the potential
p e
Often, more than one technique is required to ensure
r s •l y p
issues and solutions, where:
s
s
d
g
p o l y m•ep o
y
consistency, reproducibility and accuracy is achieved.
n
r
o l
t
i
s
t
s
s
ars •
e r
n
2 = Possible 1 = Difficult 0 = Not Possible
olym
esting • i
semin
o r
p
f
Table 1: Assessment of strengths/weaknesses for each technique
s
r
m
o
n gi npsrto d u c t s •
f
e
t
ical QC systems
t
t
s
c
Technique: Thixotropy Loop Constant Shear Shear & Recovery
y
a
s
t r
C
n
Measurement
Q
c o
a l
Rapid 3 4 4
c
mke rt etsetsitnig
i
s
t
t
p
Easy 4 4 3
o
strume
t
•
t
p
Accurate 4 4 5
s
o
ts
t e
bber & on blac
rumen
•
Small sample volume 4 4 4
k
o
n
s
c
t
t
i
a
s
n
a
l
Temperature control 4 5 5
b
e
l
n
e
g inst
n
i
b
t
u
r
o
s
Measuring system
a
e
r
• carb
c
t
t
s
y•
n
k
n
Rheometer or viscometer Both Both Rheometer
i
i
t
a
s
g
r
u
bl
o
e
p l i o r y •r i a l t e s t i n
r
Large variety of sensors 5 5 5
atory
t
a t
•
l
r
a
o
o
s
i
Structural disruption on loading avoidable 2 2 2
ter
r
b
e
r
r
a
o
a
t
a
e
b
Slip avoidable 4 4 4
m
m
s la
n
e
heo
n • a bpos r•a m a t
s•
i
Number of Participants
t
n
a
o
p
r
c
t
i
o
t
•
Single operator 5 5 5
ica
h
e
k s
c
appl
a toi or kns hl o
i
r
Experimental
v
o
r
s•w
s e
•
s&
t i
n
wa
eter
io
s
aertaepr sp l i c
Settling suspension measurements 2 2 1
r
i
•
i
ris at
a
e
p
m
c
vi iaslcs n • a
o
r
e
isc
ts •
c t
m
a
v
c
o
o
ar
n
•
t i
e
ers
m
r
stru
•e
trud
Inertia avoidable 4 4 4
t
teria
tw i n s c s cie nc e ha ract
r a
s
g in
Results
d
re w e o f
a
u
m
n
re w
r
ls c
Intuitively comprehended 4 5
i
5
xt
t
f
s
o
e
in sc
t
r i
e
e
r
c
lyme
mat
i e
t
s
o
o
p
dedicated to the
do rsg a n i s a t i oencdoendt ri coal t•e dt r taoi n i n g c o u r s e s
t
ce
rs •
scien
•
t e
e
s
ion dedica
e
m
s
y
e
u
tical QC syst ems for po l
h
o
t
rvice • trai ning c
organis at
nisa tion
o l
orga
r
n d es c o n t
ratur
ice
e
d ssael e s t e m p e
e s aa t u r
erv
l i s tt e mt s • o p
s a lp e r
p
sup
st
Tim’s Top Tips - How To Measure Thixotropy For Pharmaceutical And Cosmetic Industries
Head Office Rheology Solutions Pty Ltd • Rheology Solutions for Pharmaceutical, Cosmetics and Allied
Industries Information Kit
Address: 15 -19 Hillside Street, Bacchus Marsh, Victoria, 3340
PO Box 754, Bacchus Marsh, Victoria, 3340 • Applications Laboratory and Contract Testing Capabilities
Phone: 03 5367 7477 Statement for General Manufacturing Industries
Fax: 03 5367 6477
Email: info@rheologysolutions.com • Technical Literature for Pharmaceutical and Cosmetic
Website: www.rheologysolutions.com Industries
rk
qs u&i p he •
wo
s e
mi t y vic
ks
v r
ir
a se
ggr
or
nd
p epa
roo &
w
Tim’s Top Tips - How To Measure Thixotropy For Pharmaceutical And CosmeticrmpIndustries
ra
s
r
r
ai
d
e
• s•
an
th
ina
op
t
sh
e
en m en
ar
rk&
em
r
n
w oce
i
ts
fic s
sem
u
nd en
t r
c i
s
m
nar s
ins in
peci
c
u
e
a
i
Pharmaceutical & Cosmetic Dictionary
e cif
r
c
g
t
a
n
stry s
urf
i negs t i
y sp
m i
s
t
e
•
ustr
ruments • contract testing • indu
r
t
g
s
e
i fi c
e
n
m
t
i
• ind
test
moelry
e c
Industry Term: Capillary Rheometer.
r s •l y p
s
s
Definition: A rheometer which measures flow properties through a capillary.
g
p o l y m•ep o
y
i
n
r
o l
t
Governing Properties: The pressure on the liquid and the pressure drop of the liquid through the capillary. The
i
s
t
s
s
ars •
d
capillary geometry dictates the shear forces experienced by the liquid as if flows.
e r
n
olym
esting • i
Rheology Solutions Instrument: HAAKE RheoCap.
semin
o r
p
s f
r
m
o
n gi npsrto d u c t s •
f
e
t
Industry Term: Complex Viscosity.
ical QC systems
t
t
s
c
y
Definition: The viscosity measured by dynamic rheometry, related to both the viscous and elastic
s
t r
C
portions of flow for a viscoelastic fluid.
Q
c o
Governing Properties: This is a property governed by the viscoelastic properties of the material - elastic and
a l
•
c
mke rt etsetsitnig
viscous moduli (G' and G''). It is measured on a CS rheometer using a frequency sweep.
i
s
t
t
p
n
Rheology Solutions Instrument: HAAKE RheoStress, HAAKE MARS.
o
strume
t
•
t
p
s
o
ts
t e
bber & on blac
rumen
•
k
o
n
s
c
t
t
i
a
Industry Term: Controlled Rate.
n
a
b l
e
l
n
e
m
Definition: Mode of operation for a rheometer or viscometer. Controls the shear rate imposed on the
g inst
n
i
b
t
u
r
o
s
a
sample.
e
r
• carb
c
t
t
s
y•
n
k
n
Governing Properties: CR mode is usually available using a CS rheometer or a CR viscometer.
i
i
t
a
s
g
r
u
Rheology Solutions Instrument: HAAKE ViscoTester 550, HAAKE RotoVisco, HAAKE RheoStress, HAAKE MARS.
bl
o
e
p l i o r y •r i a l t e s t i n
r
atory
t
a t
•
l
r
a
o
o
s
i
b
ter
r
b
e
r
r
a
o
a
t
a
e
b
Industry Term: Controlled Stress.
m
m
s la
n
e
heo
n • a bpos r•a m a t
s•
Definition: Mode of operation for a rheometer or viscometer. Controls the shear stress imposed on
t i
n
a
o
p
r
the sample.
c
t
i
o
t
•
ica
h
Governing Properties: CS mode is usually available using a CS rheometer but not on a CR viscometer.
e
k s
c
appl
a toi or kns hl o
i
r
Rheology Solutions Instrument: HAAKE RheoStress, HAAKE MARS.
v
o
r
s•w
s e
•
s&
t i
n
wa
eter
io
s
aertaepr sp l i c
r
i
•
i
ris at
Industry Term: Flow Curve.
a
e
p
m
c
e
Definition: A flow curve is a plot showing the relationship between shear rate and shear stress.
vi iaslcs n • a
o
r
e
isc
ts •
t
Governing Properties: It can be measured using a CS rheometer or a CR viscometer.
c
mh
a
v
c
o
o
ar
n
Rheology Solutions Instrument: HAAKE ViscoTester 550, HAAKE RotoVisco, HAAKE RheoStress, HAAKE MARS.
•
t i
e
ls ch
m erisa
ers
m
r
stru
•e
trud
t
teria
tw i n s c s cie nc e ha ract
r a
s
g in
a
u
m
n
re w
r
ls c
Definition: The LVE is the region in which the internal structure of a material remains unchanged as
i
xt
t
f
s
in sc
t
r i
e
e
r
mat
n
w
the
c
f
o
s
o
o
p
dedicated to the
do rsg a n i s a t i oencdoendt ri coal t•e dt r taoi n i n g c o u r s e s
t
ce
rs •
scien
•
t e
e
Definition: The irrecoverable changes in the structure of a material due to the action of shearing
y
e
u
tical QC syst ems for po l
h
o
forces.
t
rvice • trai ning c
Rheology Solutions Instrument: HAAKE ViscoTester 550, HAAKE RotoVisco, HAAKE RheoStress, HAAKE MARS.
nisa tion
o l
orga
r
n d es c o n t
ratur
ice
e
d ssael e s t e m p e
e s aa t u r
erv
l i s tt e mt s • o p
s a lp e r
p
sup
st
Tim’s Top Tips - How To Measure Thixotropy For Pharmaceutical And Cosmetic Industries
rk
qs u&i p he •
wo
s e
mi t y vic
ks
v r
ir
a se
ggr
or
nd
p epa
roo &
w
Tim’s Top Tips - How To Measure Thixotropy For Pharmaceutical And CosmeticrmpIndustries
ra
s
r
r
ai
d
e
• s•
an
th
ina
op
t
sh
e
en m en
ar
rk&
em
r
n
w oce
i
ts
fic s
sem
u
nd en
t r
c i
s
m
nar s
ins in
peci
c
u
e
a
i
Industry Term: Slip.
e cif
r
c
g
t
a
n
stry s
urf
Definition: The liquid does not adhere to the wall of the measuring geometry.
i negs t i
y sp
m i
s
Governing Properties: N/A
t
e
•
ustr
ruments • contract testing • indu
r
t
g
s
e
Rheology Solutions Instrument: HAAKE ViscoTester 550, HAAKE RotoVisco, HAAKE RheoStress, HAAKE MARS. (Serrated
i fi c
e
n
m
t
i
• ind
test
moelry
sensors should be used.)
p e c
r s •l y p
s
s
d
g
p o l y m•ep o
y
i
n
r
o l
t
i
s
t
s
Industry Term: Thixotropy Loop.
s
ars •
e r
Definition: Thixotropy loop is a technique to measure the thixotropy of a liquid and consists of two
olym
esting • i
consecutive flow curves. The difference in the areas below the flow curve is a measure of
semin
o r
the thixotropy fluid and the loop is called a thixotropy loop.
p
s f
r
m
o
Governing Properties: Measuring using flow curves on a CS rheometer or CR viscometer.
n gi npsrto d u c t s •
f
e
t
ical QC systems
Rheology Solutions Instrument: HAAKE ViscoTester VT550, HAAKE RotoVisco, HAAKE RheoStress, HAAKE MARS.
t
t
s
c
y
a
s
t r
C
n
Q
c o
l
Industry Term: Thixotropy.
a
•
c
mke rt etsetsitnig
i
Definition: Thixotropic fluids show shear thinning behaviour combined with a time dependency. The
t
t
p
n
o
viscosity of a thixotropic fluid drops when subjected to a constant shear rate for a period
strume
t
•
t
p
s
of time. The viscosity of thixotropic fluids often recovers substantially over a period of time
o
ts
t e
bber & on blac
rumen
•
after the shearing forces have been removed.
k
o
n
s
c
t
t
i
a
Governing Properties: Thixotropy depends on the rate of structural recovery in the material. It can be measured
n
a
b l
e
l
n
e
m
using a flow curve on a CR or CS instrument, or by measuring the recovery of the moduli
g inst
n
i
b
t
u
r
o
s
a
after shearing on a CS rheometer.
e
r
• carb
c
t
t
s
y•
n
k
n
Rheology Solutions Instrument: HAAKE ViscoTester 550, HAAKE RotoVisco, HAAKE RheoStress, HAAKE MARS.
i
i
t
a
s
g
r
u
bl
o
e
p l i o r y •r i a l t e s t i n
r
atory
t
a t
•
l
r
a
o
o
s
i
b
ter
r
b
Industry Term: Viscoelastic Measurements.
e
r
r
a
o
a
t
a
e
c
Definition: Materials, which are partly elastic (i.e. solid) and partly viscous (i.e. fluid). When they are
b
s
m
m
s la
n
e
heo
o
deformed some of the energy is stored (solid) while the remainder is lost through flow
n • a bpos r•a m a t
s•
t i
n
a
(fluid).
o
p
r
c
t
i
o
t
•
ica
h
Governing Properties: N/A.
e
k s
c
appl
Rheology Solutions Instrument: N/A. a toi or kns hl o
i
r
v
o
r
s•w
s e
•
s&
t i
n
wa
eter
io
s
aertaepr sp l i c
r
ris at
a
e
p
Definition: An instrument for measuring the viscosity of a liquid at specified temperature and m
c
e
vi iaslcs n • a
o
r
e
isc
atmospheric conditions, by measuring the force required to move one layer over another
ts •
c t
mh
a
v
c
ar
n
•
t i
e
ls ch
m erisa
Governing Properties: Viscometers usually have mechanical bearings in their motor and generally operate in
ers
m
r
stru
trud
t
teria
tw i n s c s cie nc e ha ract
a
s
x
d
re w e o f
a
u
m
n
re w
r
ls c
i
xt
t
f
s
o
e
in sc
r i
e
e
r
c
lyme
mat
Definition: A viscosity curve is the (usually non-linear) relationship between viscosity and shear rate
n
w
the
i e
t
s
o
o
p
Governing Properties: Viscosity is the shear stress divided by the shear rate. These are measured on a CR
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Rheology Solutions Instrument: HAAKE ViscoTester VT550, HAAKE RotoVisco, HAAKE RheoStress, HAAKE MARS.
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Tim’s Top Tips - How To Measure Thixotropy For Pharmaceutical And Cosmetic Industries
Notes:
• o ViscoTester 550 and RotoVisco are controlled rate viscometers, RheoStress is a controlled stress rheometer, MARS is a modular
R&D Controlled Stress Rheometer, all of which are HAAKE brand names of Thermo Fisher Scientific (Karlsruhe, Germany) GmbH.
Disclaimer
The information contained in this report is not intended for direct use as a tool for process development. It is a guide only. This
document remains the property of Rheology Solutions Pty Ltd, and may not be reproduced or altered in any way without the written
permission of the owners.
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