Rheo354-355 - Pharma - Thixotropy

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s • c o n t r a ct t e s t i n g •
s tru ment indus t
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Thixotropy For
m e t c a e n t s • c o n t r a ct t e s i d s t
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Rheology Solutions for the

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How To Measure
& s e l a b l a c k e c i f i s u
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i r s o n s o n b e n t s • o p t i c a l Q C s y s t e m c s e r f a or
pa ti rb trum s for po min ce
t s • re p p l i c a r y • c al t e s t i n g i n s i c a l Q C s y s t e m s lyme a r sc
n i a o p t fo r

Cosmetic Industries
o ater r p o l ysm• p an ie

Pharmaceutical And
ume a r a tm
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g ti i n g
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Pharmaceutical and Cosmetic Industries

s t esm p • o p t i c
al QC systems f o e x t a t w o r a r b o n g • i m u m
roo

ru f m risa
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s a nu re i n s c re n c e o c t e ers orato
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r v t r a i n i n g c o u s c o met l a b p e c • s•
rav

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Rheo354
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Tim’s Top Tips - How To Measure Thixotropy For Pharmaceutical And Cosmetice rmpIndustries

• n ir

Page 1
s t c e e w t i o a
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Tim’s Top Tips - How To Measure Thixotropy For Pharmaceutical And Cosmetic Industries

Company Profile Contact Details


Rheology Solutions Pty Ltd is a specialist sales and service Rheology Solutions Pty Ltd
organisation dedicated to the science of materials Address: 15 -19 Hillside Street, Bacchus Marsh, Victoria, 3340
characterisation and are the exclusive Australian distributor for PO Box 754, Bacchus Marsh, Victoria, 3340
the brand names HAAKE, NESLAB, PRISM and CAHN from Phone: 03 5367 7477
Thermo Fisher Scientific, Optical Control Systems, Schleibinger Fax: 03 5367 6477
Gerate and Marimex Industries Corporation range of equipment Email: info@rheologysolutions.com
and instruments, and they also distribute the Shimadzu range of Website: www.rheologysolutions.com
tensile testers and texture analysers.

Rheology Solutions recognises the importance of specialisation Disclaimer


and dedication to a specification science and as such provides
full technical support and service throughout Australia. The The information contained in this report is not intended for direct
company goal is to integrate industry experience and materials use as a tool for process development. It is a guide only. This
characterisation techniques to provide practical solutions for document remains the property of Rheology Solutions Pty Ltd,
customers. and may not be reproduced or altered in any way without the
written permission of the owners.
Rheology Solutions has an established applications laboratory
equipped with a comprehensive range of instruments to meet the Written by Dr. T. Kealy
requirements of material characterisation. Specialist contract Technical Manager
testing services are also available and contracts can be tailored Rheology Solutions Pty Ltd
to suit discrete tests or protracted testing requirements involving
a series of tests over a period of weeks or months. © Rheology Solutions Pty Ltd 2007

A range of seminars and application specific workshops as well


as product launches and demonstrations are provided
throughout Australia. The seminars and workshops are designed
to meet the needs of specific customer and industry applications.
Rheology Solutions has its head office in Victoria and works with
a team of specialist sales and factory trained service personnel
throughout Australia. The combined experience of this team
ensures that Rheology Solutions are able to provide their
customers with access to the products to ensure that the right
technical support and service is provided.

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Tim’s Top Tips - How To Measure Thixotropy For Pharmaceutical And CosmeticrmpIndustries

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Tim's Top Tips - Rheology Solutions for the Pharmaceutical

e cif
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s
and Cosmetic Industries.

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How To Measure Thixotropy For

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Pharmaceutical And Cosmetic Industries

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Key Words: Rheology, rotational, liquid, viscosity, thixotropy, yield stress.

ical QC systems
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About The Author Introduction

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strume
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s
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t e
bber & on blac

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Tim has a background in


Often the cosmetics and pharmaceutical industries must

k
o

n
s

c
t

t
engineering and specifically in overcome problems related to (and often dominated by) the flow

a
s

n
a

b l
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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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t
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s
Chemical Engineering and has held these properties and production related issues are not always

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• carb
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s
postdoctoral research positions in immediately apparent. It is the purpose of this series of articles,

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k
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t
a
engineering rheology. Tim's

s
g
r
“Rheology Solutions for the Pharmaceutical and Cosmetic

bl
o

e
p l i o r y •r i a l t e s t i n
r

atory
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research has continued for the last

a

Industries”, to help illuminate the issues faced by the industry,

l
r

a
o
o
s

i
seven years and recent interests

ter
r
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

o
view to better processing.

n • a bpos r•a m a t

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t i

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a
and surface coatings systems. His current position encompasses

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the managment of customer contract testing and also includes

ica
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e

s
Definitions

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customer focussed education and training. Additionally he is

appl
a toi or kns hl o
i

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v

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available to provide technical input for existing or proposed
s e


materials characterisation systems for both laboratory and Thixotropy is a form of time dependent behaviour describing a
s&

t i

n
wa

eter

io
s
aertaepr sp l i c
production. material whose viscosity decreases over time while it is subjected
r

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i

ris at
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to shearing forces. After some time the material recovers


t

m
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vi iaslcs n • a

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completely to its original state.
isc
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Table Of Contents
c
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Thixotropy should not be confused with rheopexy, a rare
m erisa

ers
m

Introduction..........................................................3
stru

phenomenon, (rheopexy is also time dependent, but the viscosity


trud
t

teria
tw i n s c s cie nc e ha ract
a
s

Definitions ............................................................3 increases with time). The following techniques and discussions
r
g in

x
d
re w e o f

for measuring thixotropy apply for rheopectic measurements


a

Background and discussion ..................................3


u

m
n

re w
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ls c
i

xt

also.
t

Measurement techniques and pitfalls - CS or CR? 4


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in sc
t

r i

Experimental procedure
e
r

c
lyme

mat

Rheodestruction is also a time related phenomenon, but


n
w
the

1. The thixotropy loop test ....................................5


i
t

rheodestroyed materials do not recover their initial state. The


c
f
o

s
o
o

2. The constant shear test ....................................7


p

dedicated to the

following techniques and discussions for measuring thixotropy


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 •

3. The shear and recovery test ..............................8 apply for rheodestructive measurements also.
scien

t e
e

s
ion dedica
e
m

Summary ............................................................11
s
y

e
u
tical QC syst ems for po l

Other information for pharmaceutical


h

Background and Discussion


o

t
rvice • trai ning c

and cosmetic industries ......................................12


organis at

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
o l

orga

flow curves, or constant shear rate or shear stress


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

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r v i caen
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cri atr u•m e n

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sup
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Tim’s Top Tips - How To Measure Thixotropy For Pharmaceutical And Cosmetic Industries

measurements. A more complicated, but perhaps more Measurement Techniques


intuitively understood method is the shear and recovery method.
and Pitfalls
In order to attain repeatability the most appropriate technique
should be selected and the sample handling and experimental CS or CR?
procedures defined fully. These should be unchanged for all Thixotropy can be collected either in Controlled Rate, CR,
tests, so that thixotropy for different materials can be properly (impose a shear rate and measure the shear stress) or in
compared. Controlled Stress, CS, (impose a shear stress and measure the
resultant shear rate). In theory, for materials with no time
Thixotropy is a relative measure of the extent and speed of dependent properties both CS and CR flow curves should yield
recovery of the internal structure of a material during and after identical results. For thixotropic materials one should choose a
shear. It is useful because it allows an estimate of the effects of technique and stick to it, so that results will be comparable from
agitation, pumping etc for prolonged periods, and also the one test to the next. The main difference lies in the sensitivity of
effects of ceasing the agitation etc (i.e. how quickly the structure the instrument at low shear rates. CS instruments generally
will rebuild, and how difficult it will be to restart the process as combine an air bearing with a high-end motor to provide good
a result). control and measurement of very small deflections, and also of
high rpm measurements. CR instruments generally do not have
Note: Working definitions are provided at the end of the paper. the same level of control and detection at low rpm.

To make a CR or CS measurement you will need:

• 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.

• A suitable sensor system


Viscometric geometries should be used to make
measurements to generate flow and viscosity curves.
Viscometric geometries include cone and plate, cup and bob,
plate and plate (all for rotational instruments) and capillaries
(for a flow-through device such as a capillary viscometer).
Typically rotational devices are used and the viscometric
geometries that apply are shown in Figure 1.

Page 4 (4) info@rheologysolutions.com


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Tim’s Top Tips - How To Measure Thixotropy For Pharmaceutical And CosmeticrmpIndustries

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maximum shear rate back to zero shear again (called the down-

e cif
r
c

g
t
a

n
stry s

urf
curve). The rate of change of shear rate for the up- and down-

i negs t i

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m i
s
curves and the time at maximum shear rate are user defined and

t
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ustr
ruments • contract testing • indu

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t
g

s
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the number of data points is usually high so that a continuous

i fi c

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m
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• ind
test

moelry
curve is generated. Plotting the results as shear rate vs. shear

p e c

r s •l y p
stress or viscosity (Figure 3), if the up-curve lies above the down-

s
s
d

g
p o l y m•ep o
y
curve and the measurement can be repeated after some rest

n
r
o l
t

i
s

t
s
time, then the material is thixotropic.

ing instruments • contract tes


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ical QC systems
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Figure 2: Input for ramp test

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1.1 Experimental procedure

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C

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• carb
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The experimental layout can be one shown in Figure 1.

s
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n
k
n
Figure 1: Standard viscometric geometries (L to R) Cup & Bob,

i
i

t
a

s
g
r
u

bl
o

e
Cone & Plate, Plate & Plate

p l i o r y •r i a l t e s t i n
r

atory
• The material is loaded and the measuring geometry closed.

t
a t

l
r

a
o
o
s

i
b

ter
r

b
e

r
• Theory

r
a

o
a
t
• A lower and an upper shear rate (CR) or shear stress (CS) is

a
e

b
s

m
The theory for this type of measurement is that the flow m

s la
n
e
chosen, as is the number of measurement points between heo

n • a bpos r•a m a t

s•
behaviour is defined for a range of shear rates and shear
t i

n
them.
a

o
p
r

c
t
stresses so that its reaction to different processing conditions

i
o

t

ica
h
e

(pumping, mixing, storage etc) can be predicted. The range p

s
• The material is subjected to a shear rate profile, like in Figure

k
c

appl
a toi or kns hl o
i

r
v

of shear rates or shear stresses tested is usually defined by

o
r

2.

s•w
s e

those present in the process. The viscosity of a material is


o


s&

t i

n
w

calculated as follows:
a

eter

io
s
aertaepr sp l i c
r

i

i

ris at
a

e
p

m
c
e

(1)
vi iaslcs n • a

o
r

e
isc
ts •

c t
mh

a
v
c
o
o

ar
η = viscosity, mPa.s or cP (1mPa.s = 1cP)
n


t i
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ls ch
m erisa

ers
m

τ = shear stress, Pa or mPa


r
stru

•e

trud
t

γ = shear rate, s-1


teria
tw i n s c s cie nc e ha ract
r a
s
g in

x
d
re w e o f

a
u

m
n

re w

1.0 The thixotropy loop test


r

ls c
i

xt
t

f
s

o
e

in sc
t

r i

e
e
r

The following discussion is based on a CR ramp test, but the


lyme

mat

n
w
the

arguments hold equally for CS ramp tests. Similarly, step tests


i
t

c
f
o

s
o

could be used rather than ramp tests (see “How to measure flow
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 •

and viscosity curves for the pharmaceutical and cosmetics


scien

t e
e

industries” for further discussion on these subjects). As


ion dedica
e
m

mentioned before, once a technique is settled upon, it should be


y

e
u
tical QC syst ems for po l

h
o

used for every test. Figure 3: Thixotropy loop.


t
rvice • trai ning c
organis at

This thixotropy loop technique involves a transition from zero


nisa tion

shear rate to a maximum designated shear rate (called the up-


curve), holding the shear rate constant for a time (this step is
o l

orga

sometimes left out), and then ramping smoothly from the


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

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r v i caen
st ort •
cri atr u•m e n

p
sup
st
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.

• Other data • Temperature control


Since viscosity data can also be generated when viscometric At high shear rates, shear heating can be an issue. Shear
geometries are used, other interesting and useful data is heating is caused by internal frictional heat generated as the
available to the user. lamina of fluid move over each other. When the measuring
gap is small this can usually be successfully controlled, but
prolonged exposure to high shear rates can still be a
1.3 Potential problems with the thixotropy loop test problem.

• Understanding the meaning of the data • Settling materials


Sometimes, the real physical meaning of the changes in the If a material tends to settle, long test times tend to reduce
thixotropy loop area, are not apparent. The areas do the likelihood of successful test outcomes. The longer the
however offer a good comparison technique for different test takes, the more likely the solid fraction is to have settled
materials, or to gauge the effects of different rheology out of the measurement space, or at least created a
modifiers on the system. concentration gradient through it. Sometimes it is possible
to ramp from high to low shear rates first, rather than the
• Relative data other way around, allowing the material to be kept in
The results generated are relative only, and not absolute. suspension longer, and if possible to reduce ramp times as
Changing experimental procedure or handling could change much as practicable. Alternatively using a modified step test
the results significantly. A single loop does not fully describe with high shear steps to resuspend materials between
whether or not the sample is thixotropic, or if descending 'measurement' steps can also be successful. The
rheodestruction has taken place. Consecutive curves after key is to keep the technique consistent once it has been
fixed rest times are necessary to assess the recovery of the decided upon, so that all data is comparable. Often settling
material. materials will appear to be thixotropic as the shear stress
generally drops while the material settles.
• Solid fraction size
For multi-phase systems, often there is a solid fraction, which • Chaotic flow
has particles of considerable size. If this size is close to the One of the key assumptions for rheological measurements is
size of the measuring gap, then one or more particles may that the flow in the measuring gap is laminar. Too high shear
'bridge' the gap and cause an artificially high shear stress. rates can cause the flow regime to become turbulent and the
The problem can be solved by using particles no more than measurements are unreliable. The onset of chaotic flow can
1/3 of the gap size (1/10 for concentrated pastes). Also, be overcome or delayed by changing the measuring
often larger particles contribute little to the overall flow geometry or the measurement gap.
behaviour of the material and can be removed without large
penalties for the applicability of the measurement.

Page 6 (4) info@rheologysolutions.com


s m e n to p r h e

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mi t y vic

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v r

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p epa
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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
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c

g
t
a

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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

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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

e
n

m
t
i

• ind
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
y
reduce or remove the slip phenomenon. and shear stress curves, as illustrated in Figure 5.

n
r
o l
t

i
s

t
s

ing instruments • contract tes


u

s
ars •

e r
• Time dependent materials

n
The thixotropy of different materials can be compared by

olym
esting • i
Sample handling and experimental technique can be crucial comparing the times taken to reach a certain % of the initial

semin

o r
p
for repeatably measuring time dependent (eg thixotropic) shear stress, or some fixed value of the shear stress, or an

s f
r
m
o
materials. The same handling procedure (pouring, mixing, equilibrium value (see Figure 5).

n gi npsrto d u c t s •

f
e
t

ical QC systems
t
resting, loading into the test equipment etc) and

s
c

y
a

s
experimental procedure (rest time, ramp time and upper and

t r

C
n
lower limits) is critical for repeatable measurements, and it

Q
c o

l
must be remembered that for time dependent materials the

a

c
mke rt etsetsitnig

i
s

t
results are relative only - they depend on the technique used

p
n

o
strume
to generate them.

t

t
p

s
o
ts

t e
bber & on blac

rumen

k
o
2.0 The constant shear test

n
s

c
t

t
i

a
s

n
a

b l
e
l

n
e

g inst

n
i
b
t
The following discussion is based on a CR test, but the

u
r

o
s
a
e
r

• carb
c

t
t
arguments hold equally for CS tests, where the shear rate is

s
y•

n
k
n
c

i
i
monitored as a function of time.

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
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
heo

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
h
Figure 5: Results from a constant shear test
e

s
initial or final value, or by the time taken to achieve an

k
c

appl
a toi or kns hl o
i

r
v

o
equilibrium value
r

s•w
s e

2.2 Benefits of the constant shear test


o


s&

t i

n
wa

eter

io
s
aertaepr sp l i c
r

i

i

ris at
a

• Steady shear rates


p

m
c
e

vi iaslcs n • a

o
r

Tests can be chosen to cope better with shear heating.


e
isc
ts •

c t
mh

a
v
c
o
o

ar
n


t i
e

• Sensor inertia
ls ch
m erisa

ers
m

Because the shear rate is unchanged for the duration of the


stru

•e

trud
t

teria
tw i n s c s cie nc e ha ract
a
s

test, the controller has time to adjust the speed of rotation


r
g in

x
d
re w e o f

of the sensor so that it is exactly as specified.


e

a
u

m
n

re w
r

ls c
i

xt
t

f
s

o
e

Figure 4: Input for constant shear test


in sc

• Intuitive interpretation of the data


t

r i

e
e
r

c
lyme

The meaning of the data is easily understood and applied


mat

n
w
the

i e

once the appropriate process shear rates or shear stresses


t

2.1 Experimental procedure


c
f
o

s
o
o
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
t
ce
rs •

The experimental layout can be one shown in Figure 1.


scien

t e
e

• Time
ion dedica
e
m

s
y

Appropriate shear rates and % of original values can be


e

• The material is loaded and the measuring geometry closed.


u
tical QC syst ems for po l

h
o

chosen to enable the testing to be relatively quick.


rvice • trai ning c

• A constant shear rate (CR) or shear stress (CS) is chosen, as


organis at

• Simple measurement and simple analysis


nisa tion

is the number of measurement points.


The measurement is quite simple to execute and the data is
• The material is subjected to a shear rate profile, like in Figure straightforward to process.
o l

orga
r

4.
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

www.rheologysolutions.com (5) Page 7


r v i caen
st ort •
cri atr u•m e n

p
sup
st
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

Page 8 (4) info@rheologysolutions.com


s m e n to p r h e

rk
qs u&i p he •

wo
s e
mi t y vic

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v r

ir
a se
ggr

or
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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

d
e

• s•

an
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op

t
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en m en

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em

r
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i
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fic s

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u
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c i

s
m
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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

ing instruments • contract tes


u

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

the measuring gap and slip at the measurement geometry


o
o

ar
n


t i
e

ls ch
m erisa

walls. Data from a single shear rate test may not reveal this
ers
m

Figure 7: Results from a shear and recovery test


r
stru

information readily. Often in these cases settling material


trud
t

teria
tw i n s c s cie nc e ha ract
r a
s

will appear to be thixotropic as the shear stress generally


g in

3.2 Benefits of the shear and recovery test


x
d
re w e o f

drops while the material settles.


u

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

Of the tests mentioned this is the only one that immediately


c
lyme

mat

If a material tends to settle, long test times tend to reduce


n
w
the

informs about recovery.


i

the likelihood of successful test outcomes. The longer the


t

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

• Intuitive interpretation of the data


rs •

out of the measurement space, or at least created a


scien

e

The meaning of the data is easily understood and applied


t
e

concentration gradient through it. Settling materials will


ion dedica
e
m

once the appropriate process shear rates or shear stresses


s
y

appear to be thixotropic as the shear stress generally drops


e
u
tical QC syst ems for po l

are known.
o

while the material settles.


rvice • trai ning c

• Time
organis at

nisa tion

Appropriate shear rates and % of original values can be


chosen to enable the testing to be relatively quick.
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

www.rheologysolutions.com (5) Page 9


r v i caen
st ort •
cri atr u•m e n

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.

• Time dependent materials


Sample handling and experimental technique can be crucial
for repeatably measuring time dependent (eg thixotropic)
materials. The same handling procedure (pouring, mixing,
resting, loading into the test equipment etc) and
experimental procedure is critical for repeatable
measurements, and it must be remembered that for time
dependent materials the results are relative only - they
depend on the technique used to generate them.

Page 10 (4) info@rheologysolutions.com


s m e n to p r h e

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

ing instruments • contract tes


u
5 = Excellent 4 = Good 3 = Adequate

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

Measures materials with large particles & agglomerates 1 1 1


o


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

Direct determination of recovery from measurement No No Yes


e

vi iaslcs n • a

o
r

e
isc
ts •

c t
m

Shear heating reduced 5 4 5


h

a
v
c
o
o

ar
n


t i
e

Detection of slip, turbulence, shear heating etc 4 5 1


ls ch
m erisa

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

* Depending on the test, these parameters may be viewed


w
the

i e
t

alternatively as either a strength or as a weakness


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

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

www.rheologysolutions.com (5) Page 11


r v i caen
st ort •
cri atr u•m e n

p
sup
st
Tim’s Top Tips - How To Measure Thixotropy For Pharmaceutical And Cosmetic Industries

Contact Details Other Notes Available in the Tim's


Tips - Rheology Solutions for the
Pharmaceutical and Cosmetic
Industries Series are:
• How To Measure Yield Stress (Rheo356)

• How To Measure Flow and Viscosity Curves (Rheo352)

Other Information Available


for the Pharmaceutical and
Cosmetic Industries include:

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

Managing Director – Pat Griffin


Email: patgriffin@rheologysolutions.com

Technical Manager – Dr Tim Kealy


Email: timkealy@rheologysolutions.com

Service Engineer – Richard Donaldson


Email: richardd@rheologysolutions.com
service@rheologysolutions.com

Focused on providing our customers with materials characterisation


solutions through knowledge, experience and support.

Page 12 (4) info@rheologysolutions.com


s m e n to p r h e

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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
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• s•

an
th

ina

op

t
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en m en

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em

r
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w oce

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fic s

sem
u
nd en

t r
c i

s
m
nar s

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a

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Pharmaceutical & Cosmetic Dictionary

e cif
r
c

g
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a

n
stry s

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t
e

ustr
ruments • contract testing • indu

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t
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i

• ind
test

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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

ing instruments • contract tes


u

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

Industry Term: Linear Viscoelastic Envelope (LVE).


d
re w e o f

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

the imposed stress or deformation is gradually increased.


e

in sc
t

r i

e
e
r

Governing Properties: Measured on a CS rheometer using a stress sweep or a strain sweep.


c
lyme

mat

n
w
the

Rheology Solutions Instrument: HAAKE RheoStress, HAAKE MARS.


i
t

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

Industry Term: Rheodestruction.


s
ion dedica
e
m

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

Governing Properties: It can be measured using a thixotropy loop on a CS rheometer or a CR viscometer.


organis at

Rheology Solutions Instrument: HAAKE ViscoTester 550, HAAKE RotoVisco, HAAKE RheoStress, HAAKE MARS.
nisa tion
o l

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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

www.rheologysolutions.com (5) Page 13


r v i caen
st ort •
cri atr u•m e n

p
sup
st
Tim’s Top Tips - How To Measure Thixotropy For Pharmaceutical And Cosmetic Industries

Industry Term: Rheology.


Definition: The flow and deformation of matter.
Governing Properties: N/A
Rheology Solutions Instrument: HAAKE ViscoTester 550, HAAKE RotoVisco, HAAKE RheoStress, HAAKE MARS.

Industry Term: Rheometer (Controlled Stress).


Definition: An instrument designed for the measurement of viscous and viscoelastic flow properties
at specified temperature and atmospheric conditions, by measuring the force required to
move one layer over another without turbulence.
Governing Properties: Rheometers often have air bearings, making them highly sensitive to small variations in
load or displacement and can operate in rotation or oscillation for Controlled Rate or
Controlled Stress modes. Some rheometers have mechanical bearings, but in general they
do not have the required sensitivity to make good use of CS mode in these cases and can
not run oscillatory measurements well (or at all).
Rheology Solutions Instrument: HAAKE RheoStress, HAAKE MARS.

Industry Term: Rheometer.


Definition: An instrument designed for the measurement of viscous and viscoelastic flow properties
at specified temperature and atmospheric conditions, by measuring the force required to
move one layer over another without turbulence.
Governing Properties: Rheometers often have air bearings, making them highly sensitive to small variations in
load or displacement and can operate in rotation or oscillation for Controlled Rate or
Controlled Stress modes. Some rheometers have mechanical bearings, but in general they
do not have the required sensitivity to make good use of CS mode in these cases and can
not run oscillatory measurements well (or at all).
Rheology Solutions Instrument: HAAKE RheoStress, HAAKE MARS.

Industry Term: Rheopexy.


Definition: Rheopectic fluids show shear thinning behaviour combined with a time dependency. The
viscosity of a rheopectic fluid increases when subjected to a constant shear rate for a
period of time. The viscosity of rheopectic fluids often recovers substantially over a period
of time after the shearing forces have been removed.
Governing Properties: Rheopexy depends on the rate of structural recovery in the material. It can be measured
using a flow curve on a CR or CS instrument, or by measuring the recovery of the moduli
after shearing on a CS rheometer.
Rheology Solutions Instrument: HAAKE ViscoTester 550, HAAKE RotoVisco, HAAKE RheoStress, HAAKE MARS.

Industry Term: Shear Rate.


Definition: The rate of change of displacement resulting from an imposed shear stress.
Governing Properties: N/A
Rheology Solutions Instrument: HAAKE ViscoTester 550, HAAKE RotoVisco, HAAKE RheoStress, HAAKE MARS.

Industry Term: Shear Stress.


Definition: This is the force per unit area imposed on an element of fluid.
Governing Properties: The shear stress is dependent on the geometry of the fluid element and can be measured
by a CR viscometer and may be imposed by a CS rheometer.
Rheology Solutions Instrument: HAAKE ViscoTester 550, HAAKE RotoVisco, HAAKE RheoStress, HAAKE MARS.

Page 14 (4) info@rheologysolutions.com


s m e n to p r h e

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.

ing instruments • contract tes


u

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

Industry Term: Viscometer.


i

i

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

without turbulence; also referred to as viscometer.


o
o

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

rotational mode only.


trud
t

teria
tw i n s c s cie nc e ha ract
a
s

Rheology Solutions Instrument: HAAKE ViscoTester 550, HAAKE RotoVisco.


r
g in

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

Industry Term: Viscosity Curve.


t

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

derived from a flow curve on a CS rheometer or CR viscometer.


c
f
o

s
o
o
p

Governing Properties: Viscosity is the shear stress divided by the shear rate. These are measured on a CR
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 •

viscometer or CS rheometer using a flow curve.


scien

t e
e

s
ion dedica

Rheology Solutions Instrument: HAAKE ViscoTester VT550, HAAKE RotoVisco, HAAKE RheoStress, HAAKE MARS.
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

www.rheologysolutions.com (5) Page 15


r v i caen
st ort •
cri atr u•m e n

p
sup
st
Tim’s Top Tips - How To Measure Thixotropy For Pharmaceutical And Cosmetic Industries

Industry Term: Viscosity.


Definition: The resistance to flow of a fluid.
Governing Properties: Viscosity is the shear stress divided by the shear rate. These are measured on a CR
viscometer or CS rheometer using a flow curve.
Rheology Solutions Instrument: HAAKE ViscoTester VT550, HAAKE RotoVisco, HAAKE RheoStress, HAAKE MARS.

Industry Term: Yield Stress.


Definition: The minimum shear stress required to initiate flow in a fluid.
Governing Properties: Governed by the structural properties of the material at rest, measured by extrapolation
using a flow curve, or using the vane technique, both on a CR or CS instrument. It can
also be measured using a CS rheometer by a stress ramp.
Rheology Solutions Instrument: HAAKE ViscoTester 550, HAAKE RotoVisco, HAAKE RheoStress, HAAKE MARS.

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.

© Rheology Solutions Pty Ltd 2007

Page 16 (4) info@rheologysolutions.com


s m e n to p r h e

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
Information Request Form

e cif
r
c

g
t
a

n
stry s

urf

i negs t i

y sp
m i
s

t
e

Tim's Top Tips - Rheology Solutions for the

ustr
ruments • contract testing • indu

r
t
g

s
e
i fi c

e
n

m
t
i
Pharmaceutical and Cosmetic Industries

• ind
test

moelry
p e c

r s •l y p
s
s
d

g
p o l y m•ep o
y
i
How To Measure Thixotropy For Pharmaceuticals

n
r
o l
t

i
s

t
s

ing instruments • contract tes


u

s
ars •

r
And Cosmetic Industries

e
n

olym
esting • i
semin

o r
p
f
To ensure a speedy response to your enquiry, please take the time to ensure you complete

s
r
m
o
n gi npsrto d u c t s •

f
accurately all the relevant sections below.

e
t

ical QC systems
t
t

s
c

y
a

s
t r

C
Contact Details:

Q
c o

a l

c
Name ............................................................... Position ......................................

mke rt etsetsitnig

i
s

t
t

p
n

o
Company ............................................................... Department ......................................

strume
t

t
p

s
o
ts

e
Address .............................................................................................................................

t
bber & on blac

rumen

k
o

n
s

c
Suburb ............................................................... State ............ Postcode .................

t
i

a
s

n
a

b l
e
l

n
e

g inst
Telephone ....................................................... Fax ............................................................

n
i
b
t
u
r

o
s
a
e
r

• carb
c

t
Email .............................................................................................................................

t
s
y•

n
k
n
c

i
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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
t
Please provide me more information on the following:

a

l
r

a
o
o
s

i
b

ter
r

b
e
HAAKE VT550 - Controlled Rate Viscometer HAAKE Temperature Control Range - Refrigerated Circulators

r
r
a

o
a
t

a
e

b
s
HAAKE RotoVisco - Controlled Rate Viscometer HAAKE Temperature Control Range - Heating Circulators

m
m

s la
n
e
heo

n • a bpos r•a m a t

s•
HAAKE RheoStress - Controlled Stress Rheometer HAAKE RheoStress RS600 - Modular Controlled Stress Rheometer
t i

n
a

o
p
r

c
t
HAAKE RheoCap - Capillary Rheometer HAAKE MARS - Modular R&D Controlled Stress Rheometer

i
o

t

ica
h
Contract Testing Rheology Solutions for Pharmaceutical, Cosmetics and Allied
e

k s
c

appl
a toi or kns hl o
i

r
Industries Kit
v

o
r

s•w
e

Technical Literature for Pharmaceutical and Cosmetic Industries


s


s&

t i

n
Training & Seminars (Please specify) Other (Please specify)
wa

eter

io
s
aertaepr sp l i c
r

i

i

ris at
a

............................................................................... ...............................................................................
p

m
c
e

vi iaslcs n • a

o
r

e
isc
ts •

c t
mh

Comments: ...........................................................................................................................
a
v
c
o
o

ar
n


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

Please return your completed form to Rheology Solutions Pty Ltd by fax to 03 5367 6477
g in

x
d
re w e o f

a
u

or post to Rheology Solutions Pty Ltd. PO Box 754 Bacchus Marsh, Victoria 3340
m
n

re w
r

ls c
i

xt
t

or send an email to info@rheologysolutions.com


f
s

o
e

in sc
t

r i

e
e
r

c
lyme

mat

n
w
the

Focused on providing our customers with materials characterisation


i
t

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

solutions through knowledge, experience and support.


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

For all your rheology and service needs please contact:


organis at

Tel: 03 5368 7477 Fax: 03 5367 6477


nisa tion

Email: info@rheologysolutions.com
Website: www.rheologysolutions.com
o l

orga
r
n d es c o n t

ratur

Rheo355
ice
e

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e s aa t u r

erv
l i s tt e mt s • o p
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st

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