INTERNATIONAL ISO

STANDARD 11443

Second edition
2005-03-01

Plastics — Determination of the fluidity

of plastics using capillary and slit-die
rheometers

Plastiques — Determination de Ja fluidité au moyen de rhéométres

équipés d'une filiére capillaire ou plate

== Reference number
ISO 11443:2005(E)

8/50 2005
ISO 11443:2005(E)

Contents Page

Foreword

4 Geer Al. PING PlOS sav

enisitisssisaissceseseceneeessseresuctcscaesaentiaiassbeasswiaaiesiase dacesouean
dane bes tauuiactaaclaaeani TEAL 4

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bakanee AUIS Ge eco nace Ta eee 4

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as 11

f POC Rr ia aaa seannca es ciscabacaeaectecaesczaccct tees nav named a STE ES Se

toe reer an 11

& Exprnassiom. of nesultaiicicetes cocci ea lia ee es 14

9 PRR RECRS DE: sccisstasscscaticicei tesa seciccts cea accra cee Sea ae vadncn bk
ccdabeaa eaar 22

10 West Papo Mb wiiceresccasce eae er anal es eon en 23

Annex A (informative) Method of correcting for the influence of 4/8 on the apparent
shear rate........... 26

Annex B (informative) Measurement

Orrors..............csessccesssssensssersssssesecsrstsansescerstsaenseseusnienssssn
uasntessaceracncers 28

Annex C (informative) Uncertainties in the determination of shear viscosity by

capillary extrusion
PRIGOMMetry NOSE Gs sass caresses iicvisentersaeteasunns
seedtduceasdtcaclecopeacteb se ose aps uat yp voit sated
uastvagecereeneeeuenmeeeeeps 29

REG ibcnd neta gyre pa a yi iS SEES RST UE aes 34

©1SO 2005 — All rights reserved uo

INTERNATIONAL STANDARD ISO 11443:2005(E)

Plastics — Determination of the fluidity of plastics using

capillary and slit-die rheometers

1 Scope

This International Standard specifies methods for determining the fluidity of

plastics melts subjected to shear
stresses at rates and temperatures approximating to those arising in plastics
processing. Testing plastics
melts in accordance with these methods is necessary since the fluidity of plastics
melts is generally not
dependent solely on temperature, but also on other parameters, in particular shear
rate and shear stress.

The methods described in this International Standard are useful for determining
melt viscosities from 10 Pa-s
to 10’ Pas, depending on the measurement range of the pressure and/or force
transducer and the
mechanical and physical characteristics of the rheometer. The shear rates occurring
in extrusion rheometers
range from 1s-1 to 108 5-1,

Elongational effects at the die entrance cause extrudate swelling at the die exit.
Methods for assessing
extrudate swelling have also been included.

The rheological techniques described are not limited to the characterization of

wall-adhering thermoplastics
melts only: for example, thermoplastics exhibiting “slip” effects "| [2] and
thermosetting plastics can be
included. However, the methods used for determining the shear rate and shear
viscosity are invalid for
materials which are not wall-adhering. Nevertheless, the standard can be used to
characterize the rheological
behaviour of such fluids for a given geometry.

2 Normative references

The following referenced documents are indispensable for the application of this
document. For dated
references, only the edition cited applies. For undated references, the latest
edition of the referenced
document (including any amendments) applies.

ISO 4287, Geometrical Product Specifications (GPS) — Surface texture: Profile

method — Terms, definitions
and surface texture parameters

ISO 6507-1, Metallic materials — Vickers hardness test — Part 1: Test method

ISO 11403-2, Plastics — Acquisition and presentation of comparable multipoint data

— Part 2: Thermal and
processing properties
ISO 1133, Plastics — Determination of the melt mass-flow rate (MFR) and the melt
volume-flow rate (MVR) of
thermoplastics

3 Terms and definitions

For the purposes of this document, the following terms and definitions apply.

3.1
Newtonian fluid
fluid for which the viscosity is independent of the shear rate and of time

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ISO 11443:2005(E)

3.2
non-Newtonian fluid
fluid for which the viscosity varies with the shear rate and/or with time

NOTE For the purposes of this Intemational Standard, this definition refers to
fluids for which the viscosity varies only
with the shear rate.

3.3

apparent shear stress

Tap

fictive shear stress to which the melt in contact with the die wall is subjected,
expressed in pascals (Pa)

NOTE It is calculated as the product of test pressure and the ratio of die cross-
sectional area to die-wall area.
3.4

apparent shear rate

Yap

fictive shear rate that the melt at the wall would experience at the observed
volume flow rate if its behaviour
were Newtonian, expressed in reciprocal seconds (s~').

3.5

true shear stress

=.

actual shear stress to which the melt in contact with the die wall is subjected,
expressed in pascals (Pa)

NOTE 1 It is estimated from the test pressure p by applying corrections for

entrance and exit pressure losses, or is
directly determined from the melt-pressure gradient in the channel.

NOTE 2 For the purposes of notation, the absence of a subscript is used to denote
true values.

3.6
true shear rate

¥
shear rate obtained from the apparent shear rate 3, by taking into account the
deviations from Newtonian
behaviour by appropriate correction algorithms (see Note to 8.2.2), expressed in
reciprocal seconds (s-')

NOTE For the purposes of notation, the absence of a subscript is used to denote
true values.

3.7
viscosity

i
viscosity in steady shear, defined as the ratio r/; of true shear stress rto true
shear rate +, expressed in
pascal seconds (Pas)

3.8

apparent viscosity

Tap

ratio 7! ’ap of apparent shear stress ;,, to apparent shear rate j, , expressed in
pascal seconds (Pa‘s)

3.9
Bagley corrected apparent viscosity

TlapB
ratio r/ 7?) of true shear stress rto apparent shear rate 7.) , expressed in pascal
seconds (Pa's)

3.10
Rabinowitsch corrected apparent viscosity

TapR
ratio r,,/ 7 of apparent shear stress r,, to true shear rate » , expressed in
pascal seconds (Pa's)

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1SO 11443:2005(E)

NOTE This term is appropriate for use when testing with a single die of large
length to diameter aspect ratio for which
entrance effects are negligible.

3.11

volume flow rate

QO

volume of melt flowing through the die per unit time, expressed in cubic
millimetres per second (mm/s)

3.12
swell ratio at room temperature
5,

a
ratio of the diameter of the extrudate to the diameter of the capillary die, both
measured at room temperature

3.13

swell ratio at the test temperature

ST

ratio of the diameter of the extrudate to the diameter of the capillary die, both
measured at the test
temperature

3.14

percent swell at room temperature

“a

difference between the diameter of the extruded strand and the diameter of the
capillary die, expressed as a
percentage of the diameter of the capillary die, both measured at room temperature

3.15

percent swell at the test temperature

ST

difference between the diameter of the extruded strand and the diameter of the
capillary die, expressed as a
percentage of the diameter of the capillary die, both measured at the test
temperature

NOTE Equivalent slit-die extrudate swell terms can be derived, based on the
thickness of slit-die extrudate with
reference to the slit-die thickness.
3.16
preheating time
time interval between completion of charging of the barrel and the beginning of
measurement

3.17
dwell time
time interval between the completion of charging of the barrel and the end of
measurements

NOTE In certain special cases, it may be necessary to nate the dwell time at the
end of each measurement where
more than oné measurement per barrel filling is made.

3.18

extrusion time

time corresponding to the period of measurement for a given shear rate

3.19

critical shear stress

value of the shear stresses at the die wall at which any of the following occur:

— a discontinuity in the curve plotting shear stress against flow rate or shear
rate:

— roughness (or waving) of the extrudate as it leaves the die

NOTE lt is expressed in pascals (Pa).

© 150 2005 — All rights reserved 3

ISO 11443:2005(E)

3.20
critical shear rate
shear rate corresponding to the critical shear stress, expressed in reciprocal
seconds (s~')

4 General principles

The plastics melt is forced through a capillary or slit die of known dimensions.
Two principal methods can be
used: for a specified constant test pressure p the volume flow rate Q@ is measured
(method 1), or for a
specified constant volume flow rate Q the test pressure p is measured (method 2).
These methods can be
used with capillary dies (method A) and slit dies (method B). For full designation
of the test-method options,
see Table 1.

Table 1 — Designation of test methods

Preset parameter
Die cross-section flow
Test pressure, p venient
Circular
(capillary die) Al Aa
Rectangular
(slit die} Bf 62

Measurements can be made using a range of values of the preset parameter (either
applied test pressure in
method 1, or volume flow rate in method 2).

if a slit die with pressure transducers positioned along its length and also
upstream of the die entry is used,
then entrance and exit pressure-drop values can be determined. If capillary dies of
the same radius but of
varying length are used, then the sum of the entrance and exit pressure drops can
be determined.

A slit die with pressure transducers positioned along its length is particularly
suited for automated
measurements using on-liné computer evaluation.

Recommended values for capillary die dimensions and for flow rates and temperatures
to be used in testing
are presented either in the relevant clauses below or in |SO 11403-2.

NOTE In using a slit die, either the aspect ratio A/8 between the thickness A and
the width 2 of the slit is small or
else a correction for H/8 (see Annex A) is necessary. In the latter case, the
calculated quantities are dependent on
assumptions made in deriving the correction equations used, notably that elastic
effects are irrelevant.

5 Apparatus
5.1 Test device

5.1.1 General

The test device shall consist of a heatable barrel, the bore of which is closed at
the bottom end by an
interchangeable capillary or slit die. The test pressure shall be exerted on the
melt contained in this barrel by a
piston, screw or by the use of gas pressure. Figures 1 and 2 show typical examples;
other dimensions are
permitted.

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1SO 11443:2005(E)

5.1.2 Rheometer barrel

The barrel shall consist of a material resistant to wear and corrosion up to the
maximum temperature of the
heating system.

The barrel may have a lateral bore for the insertion of a melt-pressure transducer
close to the die entrance.

The permissible deviations in the mean bore diameter throughout the length of the
barrel shall be less than
+0,007 mm.

The barrel shall be manufactured using techniques and materials that produce a
Vickers hardness preferably
of at least 800 HV 30 (see ISO 6507-1 and Note 1) and a surface roughness of less
than R= 0,25 um
(average arithmetic discrepancy, see ISO 4287).

NOTE 1 For temperatures up to 400 °C, nitrided steel has been found suitable.
Materials of hardness values lower than
that specified but of sufficient corrosion and abrasion resistance have been found
to be acceptable for construction of the
barrel and dies.

NOTE 2 An increase in barrel-bore diameter increases the number of measurements

that can be made with a single
barrel filling and increases the shear-rate range of the instrument, Disadvantages
of using a larger barrel-bore diameter
are that larger sample masses are required, and that the time necessary to reach
temperature equilibrium throughout the
sample is greater. The barrel-bore diameters of commercially available rheometers
lie in the range between 6,35 mm and
25 mm.

5.1.3 Capillary dies (method A)

5.1.3.1 The entire length of the capillary die wall shall be machined to an
accuracy of + 0,007 mm for the
diameter (2) and + 0,025 mm for the length (L) (see Figure 1).

The capillary shall be manufactured using techniques and materials that produce a
Vickers hardness
preferably of at least 800 HV 30 (see ISO 6507-1 and Note 1 to 5.1.2) and a surface
roughness of less than
R, = 0,25 um (average arithmetic discrepancy, see [SO 4287).

The capillary opening shall show no visible machining marks nor perceptible
eccentricity.

NOTE 1 Diameters of capillary dies typically used lie in the range between 0,5 mm
and 2 mm, with various lengths to
obtain the desired L/D ratios. For testing of filled materials, larger diameters
might be required.

NOTE 2 Hardened steel, tungsten carbide, stellite and hardened stainless steel are
the most common die materials.
NOTE 3 The precision with which capillary dimensions can be measured is dependent
upon both the capillary radius
and the capillary length. With capillaries of diameter smaller than 1,25 mm, the
specified precision (+ 0,007 mm) is difficult
to obtain. Due to the extreme sensitivity of flaw data to capillary dimensions, it
is important that the capillary dimensions,
and the precision with which the dimensions are measured, are known and reported.
This also applies to the dimensions
(thickness, width and length) of slit dies (see 5.1.4),

© 180 2005 — All rights reserved 5

ISO 11443:2005(E)

Dimensions in millimetres.

+0,01
e120

200
Key

1 applied force or constant velocity 5 heating coil 9 optical sensor

2 thermal insulation 6 pressure transducer 10 temperature-controlled air chamber

3. sopiston * capillary die 11. thermometer

4 barrel 8 die-retaining nut 12. inlet angle

Figure 1 — Typical example of an extrusion rheometer used with a capillary die

6 © 150 2005 — All rights reserved

6 |
ay
|
|
JG
Al WZ
|
|
|
2 | x
| +0,01
| A #12 0
|

L= 12,4

1
2
3
4
5
6
P.

T
ISO 11443:2005(E)

Dimensions in millimetres

piston

barre

die

exchangeable part
channel

electrical heater

| = pressure transducers
; = thermometers

Figure 2 — Typical example of an extrusion rheometer used with a slit die

©1350 2005 — All rights reserved

ISO 11443:2005(E)

§.1.3.2 To determine the apparent shear rate 7',, and the apparent shear stress r,,
with one capillary
die, the ratio L/D of the length £ to the diameter D of the capillary die shall be
at least 16 and its inlet angle
shall be 180°, unless otherwise specified by the referring standard. Only data
obtained with capillaries of the
same inlet angle (+ 1°), length (+ 0,025 mm) and diameter (+ 0,007 mm) shall be
compared. The inlet angle is
defined in Figure 1.

It is recommended that a die of length either 16 mm or 20 mm, diameter of 1 mm and

entry angle of 180° be
used (see Note 1). Options for the die diameter of 0.5mm, 2mm or 4mm are permitted
when the
recommended value is not appropriate, for example for heavily filled materials. For
dies of diameter other than
1mm, the recommended ratio of length to diameter (L/D) shall be the same, where
possible, as that of the
1 mm diameter die used in that instrument.

NOTE 1 ~~ Die lengths of 16 mm and 20 mm are most commonly used, the choice often
being dependent on, and limited
by, the design of the instrument.

NOTE2 For a given value of the apparent shear rate, the effect of shear heating of
the melt is reduced by use of
smaller-diameter capillary dies.

5.1.3.3 To determine the true shear rate 7 and the true shear stress +, capillary
dies of the same
diameter (+ 0,007 mm) and inlet angle (+ 1°) and having at least two different L/D
ratios selected from the
recommended series 1/D = 0,25 to 1, 5, 10, 16, 20, 30, 40 (see also 8.4.2) are
required, provided the following
conditions are met.

The use of only two dies, of the same diameter {+ 0,007 mm) and inlet angle (+ 1°),
of L/D < 5 and L/D = 16 is
permitted where the test conditions are such that the resultant Bagley plot is not
significantly non-linear, i.e.
these conditions having been established in advance for each class of sample, by
using additional dies (see
8.4). When using only two dies the difference in the L/D ratios of the two dies
shall be at least 15.

It is recommended that, when using only two dies to determine shear viscosity
corrected for entrance pressure
drop effects, a short die of length to diameter (//D) ratio in the range 0,25 to 1,
and a long die of length to
diameter (PP) ratio in the range 16 to 20, both dies having a diameter of 1 mm and
an entry angle of 180°, be
used. Options for the die diameter, of 0,5 mm, 2mm or 4mm, shall be permitted when
the recommended
value of 1 mm is not appropriate, for example for heavily filled materials. For
dies of diameter other than 1mm
the recommended ratios of length to diameter (//P) shall be the same as that
specified for the 1mm diameter
dies.

NOTE The procedure for correction for entrance pressure drop effects (see 8.4) is
based on an extrapolation of data
to a die length of zero, rather than by making the approximation that the short die
yields the entrance pressure drop value.

5.1.4 Slit dies (method B)

5.1.4.1 The entire length of the slit die shall be machined to an accuracy of +
0,007 mm for the thickness,
+0,01 mm for the width and + 0,025 mm for the length. As applicable, the distance
between the centres of the
pressure transducers and the exit plane shall be determined to + 0,05 mm. (See Note
3 to $.1.3.1.)

The die shall be manufactured using techniques and materials that produce a Vickers
hardness preferably of
at least 800 HV 30 (see ISO 6507-1 and Note 1 to 5.1.2) and a surface roughness of
less than &, = 0,25 um
(average arithmetic discrepancy, see ISO 4287.)

NOTE For slit-die materials, see Note 1 to 5.1.2 and Note 2 to 5.1.3.1.

5.1.4.2 To determine the apparent shear rate 7, and the apparent shear stress :,,,
unless otherwise
specified by the referring standard, the slit die shall have a ratio H/8 of the
thickness H to the width # of at
most 0,1 and shall have an inlet angle of 180°. Only data obtained with slit dies
of the same inlet angle (+ 1°),
thickness (+ 0,007 mm), width (+ 0,01 mm) and length (+ 0,025 mm) shall be
compared.

§.1.4.3 To determine the true values of shear rate » and shear stress ;, slit dies
conforming to the
specification given in 5.1.4.1 and 5.1.4.2 may be used in exactly the same way as
capillary dies, i.e. using the
Bagley correction method modified accordingly (see 8.4). Alternatively, a slit die
with pressure transducers
positioned along the length of its channel can be used to determine true shear
stress values.

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6

ISO 11443:2005(E)

5.1.5 Piston

If a piston is used, its diameter shall be 0,040 mm + 0,005 mm smaller than the
barrel-bore diameter. It may
be equipped with split or whole sealing rings in order to reduce melt backflow past
the land of the piston. The
hardness of the piston shall be less than that of the barrel, but not less than 375
HV 30 (see ISO 6507-1).

5.2. Temperature control

For all temperatures that can be set, the barrel-temperature control shall be
designed such that, within the
range of the capillary die or slit die, as applicable, and the permissible filling
height of the barrel, the
temperature differences and variations measured at the wall do not exceed those
given in Table 2 for the
duration of the test.

Table 2— Maximum allowable temperature differences as a function of

distance and as a function of time

Temperature difference —_
Test temperature, 7 from the set temperature bade eet ae ae
as a function of distance * epee Orne
7 3G 7S
< 200 +1,0 +05
200 < ¢= 300 21,5 +1,0
> 300 +2,0 +1,5
4 For all positions within the range of the capillary die or slit die, as
applicable, and the
permissible filling height of the barrel, for the duration of the test.

The test device shall be designed so that the test temperature can be set in steps
of 1 °C or less.
5.3 Measurement of temperature and calibration
5.3.1 Test temperature

5.3.1.1. Method A: Capillary dies

When capillary dies are used, the test temperature shall be either the temperature
of the melt in the barrel
near the capillary inlet or, if this is not possible, the temperature of the barrel
wall near the capillary inlet, It is
preferable that the test temperature is measured at a position not more than 10 mrn
above the capillary inlet.
(See also 5.3.2.)

5.3.1.2 Method B: Slit dies

When slit dies are used, the die-wall temperature shall be measured and taken as
the test temperature. This
temperature shall be equal to the test temperature measured in the barrel to within
the distance-related and
time-related temperature tolerances given in Table 2. (See also 5.3.1.1 and 5.3.2.)

5.3.2 Measurement of test temperature

The tip of the temperature-measuring device shall be either in contact with the
melt or, if this is not possible, in
contact with the metal of the barrel or die wall not more than 1,5 mm from the melt
channel. Thermally
conductive fluids may be used in the thermometer well to improve conduction.
Thermometers, preferably
thermocouples or platinum resistance sensors, may be placed as shown in Figure 1
and Figure 2.

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ISO 11443:2005(E)

5.3.3 Temperature calibration

The temperature-measuring device used during the test shall read to within 0,1 °C
and be calibrated by
means of a standard thermometer, with error limits of + 0,1 °C, whilst complying
with the depth of immersion
prescribed for the thermometer concermed. For this purpose, the barrel may be
filled to the top with a low-
viscosity melt.

No liquids that may contaminate the die or barrel or influence the ensuing
measurements, e.g. silicone oil,
shall be used as heat-transfer media during calibration.

5.4 Measurement of pressure and calibration

5.4.1 Test pressure

The test pressure shall be the pressure drop in the melt, measured as the
difference between the pressure in
the melt before the capillary-die or slit-die inlet and the pressure at the die
exit, as applicable. If possible, the
test pressure shall be measured by a melt-pressure transducer located near the
entrance of the die, in which
case the distance from the pressure transducer to the die entry face shall be kept
constant for all tests and
should preferably be not more than 20 mm (see Note). Otherwise, the test pressure
shall be determined by
the force exerted on the melt, e.g. by the piston, that force being measured by a
load cell above the piston
{see Annex B, Clause B.1).

NOTE [tis important that the distance from the die entry face to the pressure
transducer is kept constant for all tests
as this will otherwise affect the pressure drop measured. The use of pressure
transducers at a distance equivalent to that
of the barrel diameter from the die entry face may reduce fluctuations in the
pressure being measured that may arise due
to recirculating flow above the die entry.

lf testing is to be carried out by extruding to a channel or vessel pressurized to

a pressure above atmospheric
pressure, then the pressure at the die exit shall also be measured, preferably
using a pressure transducer
located immediately below the exit of the die.

The force- or pressure-measuring devices shall be operated in the range between 1%

and 95% of their
nominal capacity.

3.4.2 Pressure drop along the length of the slit die

When using slit dies, the pressure profile along the length of the die shall be
measured by flush-mounted melt-
pressure transducers positioned along the die wall.

Alternatively, when slit dies not equipped with melt-pressure transducers are used,
the sum of entrance and
exit pressure losses can be taken into account by employing the Bagley correction
modified for slit dies
(see 8.4.3).

5.4.3 Calibration

External hydraulic test equipment may be used for the calibration of melt-pressure
transducers. Load cells
shall be calibrated in accordance with manufacturer's specifications. The maximum
permissible error in the
reading of the melt-pressure transducers or load cells shall be both less than or
equal to 1% of the full-scale
value and less than or equal to 5 % of the absolute value. The calibration of melt-
pressure transducers should
preferably be performed at the test temperature.

5.5 Measurement of the volume flow rate of the sample

The volume flow rate shall be determined either from the feed rate of the piston or
by weighing the mass of
the sample extruded during a measured period of time.

If weighing is performed, the conversion to the volume flow rate shall be made by
using the density of the melt
at the prevailing test temperature, the influence of the hydrostatic pressure on
the density being ignored.

10 © 150 2005 — All rights reserved

ISO 11443:2005(E)

The volume flow rate shall be determined to within 1%.

It is recommended that, for purposes of providing comparable data, the apparent

shear rates and hence flow
rates used for testing are such that data at the true shear rates specified in ISO
11403-2 can be determined
by interpolation. The apparent shear rates should be set at equispaced intervals,
when plotted logarithmically,
and there should be at least two data points per decade of apparent shear rate.

NOTE The specified maximum permissible error for determining the volume flow rate
via the feed rate of the piston
can only be conformed to if, inter alia, the leakage rate between the piston and
barrel is sufficiently small. Experience
indicates thal this can be achieved if the clearance between piston and barrel does
not exceed 0,045 mm (see 5.1.5),

6 Sampling

From the material to be tested, a representative sample shall be taken for use as
the test sample. The number
of determinations per single barrel filling depends on the moulding material under
test and shall therefore be
agreed upon between the interested parties. The temperature during test-sample
preparation shall be less
than that during the subsequent test.

7 Procedure

7.1 Cleaning the test device

Before each measurement, ensure that the barrel, transducer bores, where
applicable, piston and capillary or
slit die are free of adherent foreign matter. Make a visual examination to check
for cleanliness.

If solvents are used for cleaning, ensure that no contamination of the barrel,
piston and capillary or slit die has
occurred that might influence the test result.

NOTE For the purpose of cleaning, circular brushes made of a copper/zine alloy
(brass) and linen cloths have proved
satisfactory. However, the use of copper-containing materials may accelerate
degradation of the polymer when testing
palyethylene and polypropylene. Cleaning can also be performed by cautious burning
out. Using graphite on threads
facilitates unlocking after the test.

WARNING — The operating conditions chosen may entail partial decomposition of the
material under
test, or cause it to release dangerous volatile substances. The users of this
International Standard
shall make themselves aware of possible risks, shall prevent or minimize such risks
as appropriate,
and shall provide appropriate means of protection.

7.2 Selection of test temperatures

It is recommended that, for the purpose of providing data for comparison or for
modelling, data at three
temperatures be obtained (see ISO 11403-2). For any given material type, one of the
temperatures used
should preferably be the same as that specified in the appropriate material
designation or specification
standard for use in melt flow rate testing (see ISO 1133). Far the other two
temperatures, it is recommended
that a temperature interval of 20 °C be used (see Notes 1 and 2). Both of the
additional temperatures may be
either higher or lower than the recommended temperature as used for the melt flow
rate test (see ISO 1133),
or one higher and one lower. However, other values may be used and may be
preferable to use, dependent
on the specific grade of material and the application for which the data are
required.

NOTE 1 From an analysis of CAMPUS databases, the average interval in temperature

used to measure shear viscosity
ranged from 10 °C to 30 °C and was dependent on the material grade.

NOTE 2 Typical test temperatures for several materials are given in Table 3. These
are listed for information only. The
most useful data are generally obtained at the temperatures used for processing the
material. The shear stresses and
shear rates applied should also closely approximate those observed in the actual
processing.

ISO 20065 — All rights reserved 11

ISO 11443:2005(E)

Table 3 — Typical test temperatures

Material Temperature, °C

Polyacetal 190 to 220

Polyacrylate 140 to 300
Acrylonitrile-butadiene-styrene (ABS) 200 to 280
Cellulose esters 190
Polyamide PA66 250 to 300
Polyamide (not PAG6) 130 to 300
Poly(chloratrifluoroethylene) 265

Polyethylene and ethylene copolymers and terpolymers 150 to 250

Polycarbonate 260 to 300
Polypropylene 190 to 260
Polystyrene and styrene copolymers 180 to 280
Poly(vinyl chloride) 170 to 210
Poly(butylene terephthalate) 245 to 270
Poly(ethylene terephthalate) 275 ta 300
PMMA and copolymers 180 to 300
Poly(vinylidene fluoride) 195 to 240
Poly(vinylidene chloride) 150 to 170
Ethylene-vinyl alcohol copolymer 190 to 230
Palyetheretherketone 340 to 380
Palyethersulfone 360

7.3 Preparation of samples

In cases where the fluidity of the melt depends on one or more factors, such as the
residual monomer content,
gas inclusions and/or moisture, apply pretreatment or conditioning procedures in
accordance with the referring
standard and/or the relevant material standard, as applicable.

NOTE Examples of materials that may require special preparation regimes include
poly(ethylene terephthalate),
poly(butylene terephthalate) and polycarbonate.

Allow the assembled apparatus to reach thermal equilibrium at the test temperature
before applying the final
torque on the die (where applicable), then start charging (see Warning in 7.1).

To avoid air inclusions, introduce the sample into the barrel in separate small
quantities, performing
intermediate compactions by means of a piston. Fill the barrel to within
approximately 12,5 mm of the top.
Accomplish charging in not more than 2 min.

7.4. Preheating

Immediately after charging the barrel, start the preheat timer. Either extrude a
small portion of the barrel
charge at a constant pressure (method 1) or apply a constant volume flow rate until
a positive load or pressure
is obtained (method 2). Then stop the extrusion or volume flow until a preheat time
of at least 5 min, unless
otherwise specified by the referring standard, is completed. Check that the preheat
time used is sufficient to
obtain thermal equilibrium of the test sample throughout the volume of the barrel,
for each material to be
tested, either by ensuring that on increasing the preheat time the measured
quantity (volume flow rate or test

12 © 180 2005 — All rights reserved

ISO 11443:2005(E)

pressure, as applicable) at constant test conditions does not change by more than
+5 %, or by inserting a
thermometer into the sample in the barrel and ensuring that, within the specified
preheat time, the sample
temperature is equal to the specified test temperature within the tolerance for the
distance-related temperature
difference given in Table 2. Then extrude a small quantity of the substance under
test, stop the piston, wait for
1 min and perform the measurement.

7.5 Determination of the maximum permissible test duration

To check that degradation or other processes are not affecting measurements, carry
out a repeat
measurement towards the end of the test on the same barrel charge, using the same
conditions as were used
at the beginning of the test. Compare values obtained at the start and end of the
test. A difference in values is
indicative of degradation or other processes affecting measurements.

Alternatively, for each sample and each test temperature, determine by testing,
employing several different
preheating times prior to the actual tests, the maximum permissible test duration
which corresponds to the
time span, from the end of charging of the barrel, within which the measured
quantity (volume flow rate or test
pressure, as applicable) at constant test conditions does not change by more than
+5 % (see also 7.4.)

If determination at all of the required values of test pressure or volume flow rate
is not possible within the
maximum permissible test duration of a single test, then make measurements stage by
stage, using several
barrel fillings of the same sample (see Note 1 to 7.8).

NOTE For materials that are unstable, in order to minimize the effect of changes on
the measurements it is
recommended that testing be carried out using a decreasing speed profile. The
degree of compaction of the sample may
also influence its stability.

7.6 Determination of test pressure at constant volume flow rate: Method 2

lf the test pressure necessary to maintain a given volume flow rate is to be

determined (see also 5.4.1 and
7.8), use either of the following methods (see Table 1):

method A2, using capillary dies;

method B2, using slit dies.

7.7 Determination of volume flow rate at constant test pressure: Method 1

lf, as an alternative to 7.6, the volume flow rate for a given test pressure drop
is required (see also 7.8), use
either of the following methods (see Table 1):
method A1, using capillary dies;

method B1, using slit dies.

7.8 Waiting periods during measurement

At each measurement, wait until the test pressure (method A2 or B2) or the volume
flow rate (method At
or B1) has become constant (e.g. to+ 3%) over a given time period (e.g. 15s).

NOTE 1 With a single barrel filling it is generally possible to determine several

pairs of values for volume flow rate and
fest pressure.

NOTE 2 Itis recommended that selected measurements are repeated to check the
repeatability.

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ISO 11443:2005(E)

7.9 Measurement of extrudate swelling

7.9.1 General

Measure the degree of extrudate swelling either at the test temperature during the
extrusion process, or after
cooling of the extruded strand to roam temperature.

NOTE The diameter of the extrudate is dependent on the flow rate, the test
temperature, the time since extrusion, the
manner of cooling (for the ratio at room temperature), the length of the extrudate,
the capillary die length, diameter and
entry geometry and the barrel diameter. The results obtained can be very sensitive
to the details of the measurement
technique. Comparable results can only be obtained when all testing conditions are
identical.

The following procedures give a measure of the degree of extrudate swelling. Other
methods can be used.
Although the procedures described are written for capillary dies, they also apply
by analogy to slit dies.

7.9.2 Measurement at room temperature

The diarneter of the extruded strand is measured with a micrometer. In order to

minimize the effects of gravity,
use the following procedure:

— remove any extrudate attached to the capillary die by cutting it off as close as
possible to the die;

— extrude a length of extrudate not longer than 5cm and cut off the length of
extrudate, marking the end
that was extruded first;

— when cutting off the length of extrudate, hold it with tweezers and subsequently
allow it to cool,
suspended in air, to room temperature:

— measure the diameter of the strand as close as possible to the marked end
(outside the area deformed by
cutting and marking).

7.9.3 Measurement at the test temperature

Use a photographic or optical method that involves no mechanical contact with the
extruded strand. In order to
minimize the effect of gravity, use the following procedure:

— remove any extrudate attached to the capillary die by cutting it off as close as
possible to the die;
— extrude a length of extrudate not longer than 5 cm;

— measure the diameter of the extruded strand at a fixed point below the die outlet
by photographic or
optical techniques.
NOTE In order to minimize cooling of the extruded strand during the measurement of
extrudate swelling, the strand

may be extruded into a temperature-controlled air chamber, such as that shown

schematically in Figure 1.

8 Expression of results

8.1 Volume flow rate

Calculate the volume flow rate ©, in cubic millimetres per second, by means of one
of the following equations:

O=Av (1)

tS
i
|

(2)

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—
ISO 11443:2005(E)

where
A is the piston cross-sectional area, in square millimetres;
vis the velocity of the piston, in millimetres per second:
m is the mass flow rate of the sample, in grams per second:

pe is the density of the sample at the test temperature, in grams per cubic
millimetre.
8.2 Apparent shear rate

8.2.1 General

Calculate the apparent shear rate ;,, , in reciprocal seconds, at the die wall,
using the equation given in 8.2.2
or 8.2.3, a5 applicable.

8.2.2 Method A: Capillary dies

320

— (3)

Yap
where
) is the diameter of the capillary die bore, in millimetres;

0 is the volume flow rate, in cubic millimetres per second (see 8.1).

NOTE In the case of Newtonian fluids, Equation (3) gives the true shear rate ¥ at
the capillary wall. As plastics melts
do not generally exhibit Newtonian behaviour, the quantity calculated using this
equation is termed the apparent shear rate
Pap The true shear rate j can be determined from the apparent one 73, by a
correction procedure (see 8.5.1).

8.2.3 Method B: Slit dies

, __60
* ap RH

where
5 is the width of the die, in millimetres;

A is the thickness of the die, in millimetres:

© is the volume flow rate, in cubic millimetres per second (see 8.1).
See Note to 8.2.2.

NOTE Equation (4) is strictly true only for infinitesimally small thickness-to-
width (4/8) ratios. The use of Equation (4)
overestimates the apparent shear rate Yap by less than 3%, however, if 4/8 < 0,1. A
detailed analysis of the correctness
of the approximation involved in using Equation (4), together with a correction
procedure, is given in Annex A.
8.3 Apparent shear stress

8.3.1 General

Calculate the apparent shear stress Zap: in pascals, at the die wall, using the
equation given in 8.3.2 or 8.3.3,
as applicable.

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ISO 11443:2005(E)

8.3.2. Method A: Capillary dies

Ey
rap ar (5)

p is the test pressure, in pascals;

£ is the length of the die, in millimetres;

) is the diameter of the die, in millimetres.

8.3.3 Method B: Slit dies

t=)" a
where

p isthe test pressure above the die inlet, in pascals;

£ is the length of the die, in millimetres;

8 is the width of the die, in millimetres:

H is the thickness of the die, in millimetres.

NOTE The shear stresses calculated using Equations (5) and (6) are apparent
quantities because the pressure drop

along the length of the die is smaller than the test pressure » which is the sum of
the pressure losses at the die entrance,
in the die and at the die exit. True shear stresses can be determined by applying
appropriate corrections either to the test
pressure p or to the die length £ (see 8.4).

8.4 True shear stress

8.4.1 General

The true shear stress can be obtained by using the Bagley correction method ©! (see
8.4.2 or 8.4.3, as
applicable), or can be determined directly if slit dies (methods B1 and B2)
equipped with pressure transducers
are used (see 8.4.4).

If non-linear Bagley or slit-die pressure-drop versus distance plots are obtained,

a statement shall be made to
that effect in the test report. In such cases, shorter dies shall be used, unless
otherwise specified by
agreement, in which case the procedure used shall be stated in the test report.

NOTE In using capillary-die or slit-die extrusion rheometers for measuring the

shear viscosity of plastics, viscous
dissipation and the pressure dependence of the viscosity can affect the results.
Non-linear plots may result.

8.4.2 Bagley correction for capillary dies (method A)

Determine the sum of the entrance and exit pressure losses using the following
procedure:
a) For method Aj, using at least two, but preferably more, capillary dies of the
same inlet angle and
diameter but with different 1/D ratios such that (L/D), < (L/D), determine the
apparent shear rate Fap at
the die wall as a function of the test pressure p (see Figure 3).

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ISO 11443:2005(E)

b) For method A2, using at least two, but preferably more, capillary dies of the
same inlet angle and
diameter but with different L/D ratios such that (L/D), < (L/D)., measure the test
pressure p as a function
of the apparent shear rate Yap atthe die wall.

c) From the data obtained in a) or b), as applicable, plot the test pressure p as a
function of L/D for different
values of the apparent shear rate 73) (see Figure 4). The so-called Bagley lines
which result have a
slope that is four times the true shear stress.

lf, when using long capillary dies, deviations from the straight line arise due to
the influence of pressure on the
melt viscosity or due to viscous-dissipation effects, make the measurements using
shorter capillary dies,
unless otherwise specified by agreement, in which case the procedure used shall be
stated in the test report
(see Note to 8.4.1).

NOTE The Bagley correction may be performed using suitable computer programs. It is
then not necessary to follow
the data-plotting procedure described above. However, if computers are used to
apply corrections to measured data, a
graphic printout of the Bagley plots can enable the operator to assess the validity
of the assumptions made (i.e. to check
that the Bagley lines are straight).

Extrapolate the Bagley line for each apparent shear rate 73, to zero pressure (see
Figure 4). The ordinate
distance p, corresponds to the sum of the die-entrance and die-exit pressure losses
at the apparent shear rate
Yap Concerned.

logy,

(LID, (LID), (LID),

¥ ap2

Fapt

loge

Figure 3 — Application of the Bagley correction method |°) — Plot of the apparent
shear rate 7,
versus the test pressure p for different values of L/D

® ISO 2005 — All rights reserved 17

ISO 11443:2005(E)

Poo

(LID) c4
(LID ex

(LID), LID

Key
1 slope=4r

Figure 4 — Schematic Bagley plot for capillary dies

{the melt pressure p is plotted as a function of L/D for dies of the same diameter
for different values of the apparent shear rate 7g, )

Calculate the true shear stress + for the apparent shear rate +, of interest using
either Equation (7) or
Equation (8):

t=(p~ Pe)o~ (7)

where
pis the test pressure, in pascals;
p, is the pressure correction, in pascals;
Dis the diameter of the capillary die, in millimetres;
fis the length of the capillary die, in millimetres.
Because the diameter 2 of the die is constant, the abscissa distances (//D),.
represent die-length corrections.

Thus, as an alternative to Equation (7), the true shear stress rfor the apparent
shear rate »,, of interest may
be calculated using Equation (8):

p
4{(L/D)+(LID), |

[=

(8)

where (/D),. is the die-length correction (dimensionless).

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ISO 11443:2005(E)

8.4.3 Bagley correction for slit dies (method B)

Determine the sum of the entrance and exit pressure losses using the following
procedure:

a) For method B1, using at least two, but preferably more, slit dies of the same
inlet angle, width and
thickness, but of different lengths £ such that 1, is less than Ls, determine the
apparent shear rate Yap at
the die wall as a function of the test pressure p.

b) For method B2, using at least two, but preferably more, slit dies of the same
inlet angle, width and
thickness, but of different lengths Z such that Z, is less than /, measure the test
pressure p as a function
of the apparent shear rate jg) at the die wall.

¢) From the data obtained in a) or b), as applicable, plot the test pressure p as a
function of LU + 8VHB for
different values of the apparent shear rate Yap- The Bagley lines which result have
a slope that is twice
the true shear stress (see Figure 5).

LAH + BAB L(H + BVHE

Key
1 slope =2r

Figure 5 — Schematic Bagley plot for slit dies

(the test pressure p is plotted as a function of L(H + 8)/A8 for dies of the same
width & and thickness H
for a single value of the apparent shear rate jap )

If, when using long slit dies, deviations from the straight line arise due to the
influence of pressure on melt
viscosity or due to viscous-dissipation effects, make the measurements using
shorter slit dies, unless
otherwise specified by agreement, in which case the procedure used shall be stated
in the test report (see
Notes to 8.4.1 and 8.4.2),

Extrapolate the Bagley line for each apparent shear rate Yap to zero pressure. The
ordinate distance p,

corresponds to the sum of the die-entrance and die-exit pressure losses at the
apparent shear rate j-4,
cancemed,

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ISO 11443:2005(E)

Calculate the true shear stress 7 for the apparent shear rate Yap of interest using
either Equation (9) or
Equation (10):

HB (p=pc)
a

"“2(#+B) OL

(9)

where
Al is the thickness of the slit die, in millimetres;
8B is the width of the slit die, in millimetres;
p — is the test pressure, in pascals;
p. is the pressure correction, in pascals;
Lis the length of the slit die, in millimetres.
Because the die dimensions 1 and # are constant, the abscissa distances L.(H + #\
WHB represent die-ength

corrections. Thus, as an alternative to Equation (9), the true shear stress rfor
the apparent shear rate 7,, of
interest may be calculated using Equation (10):

pH
2(L+L,) (H+B)

(10)

where L(A + 8\HB is the die-length correction (dimensionless).

8.4.4 Direct determination using slit dies (method B)

From the longitudinal pressure gradient do/d/i, measured using pressure transducers
placed along the length
of the slit die, calculate the true shear stress rat the die wall using the
following equation:

HB dp
2(H+B) dL

r=

(11)

where

a is the longitudinal pressure gradient, in pascals per millimetre;

8 — js the width of the slit die, in millimetres;

is the thickness of the slit die, in millimetres.

6.5 True shear rate

8.5.1 General
Calculate the true shear rate » at the capillary-die or slit-die wall from the
apparent shear rate by applying the
Weissenberg-Rabinowitsch correction method |], using Equation(12) for method A (see
8.5.2) and
Equation (13) for method B (see 8.5.3).

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ISO 11443:2005(E)

8.5.2 Method A: Capillary dies

.# .
_ *F dio
pie OO ey OF ap (12)
4\ dlogr |
dlogy,
where ——-=P js the slope of the curve log;'a, =/(loga.
diogr Pp Od ¥ap =/(logz)
NOTE It is noted that the method by which this correction is applied, specifically
either the choice of the function used

to fit the log Yap versus logz data from which the slope is determined or the use
of an altemative method of determination
of the slope of the data, can result in significant errors in the corrected (true)
values of shear rate, and consequently true
shear viscosity. This is particularly the case when the slope of the curve is large
or where the selected curve does not fit
the data well, for example at the highest and lowest shear rate data points.

8.5.3 Method B: Slit dies

; dlogy
j- 2s [2, Searen (13)

3 dlogr
dlogy
where —-272P. is as defined in 8.5.2.
dlogz

See Note to 8.5.2.

8.6 Viscosity
Calculate the viscosity as the ratio of the shear stress to the shear rate.

If the ratio is not derived exclusively from true quantities of shear stress and
shear rate, then one of several
apparent viscosities will result. These shall be named and identified by subscripts
as defined in 3.8 to 3.10.

8.7 Determination of extrudate swelling

8.7.1 Measurement at room temperature

Calculate the extrudate swell ratio at room temperature 5, and the percent swell at
room temperature s,, using
Equations (14) and (15):

54> =a (14)
59 = 72? 100 % (15)
where

D, is the extrudate diameter, in millimetres, measured at room temperature;

Dis the capillary-die diameter, in millimetres, measured at room temperature.

8.7.2 Measurement at the test temperature

Calculate the swell ratio at the test temperature S$; and the percent swell at the
test temperature sy, using
Equations (16) and (17):

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ISO 11443:2005(E)

= 16
iD (16)
a = 2m—OT «100 % (17)

where
DOD, is the extrudate diameter, in millimetres, measured at the test temperature;
Dy is the capillary-die diameter, in millimetres, measured at the test temperature.

NOTE In the case of slit dies, these calculations can be made using the thickness
(or width) of the extrudate instead
of the extrudate diameter and the die thickness (or die width) instead of the die
diameter in Equations (14) to (17). Since
swelling may be different in the width and thickness directions, it should
preferably be determined in both of these
directions.

9 Precision

Two interlaboratory test programmes have been carried out. The first
interlaboratory test programme was
completed in 1990, involving seven laboratories and two materials (PP and PVC).

In the first interlaboratory comparison, two types of apparatus and two measurement
procedures were used:

— a rheometer measuring the extrusion pressure at the capillary inlet (four

laboratories) and a rheometer
measuring the force applied to the piston (two laboratories);

— the shear rates applied during the tests were imposed successively in decreasing
order of magnitude (two
laboratories) or increasing order (four laboratories).

Repeatability was examined by two laboratories, and was found to be improved if the
pressure was measured
at the inlet to the capillary rather than determined from the force applied to the
piston, and to be less good at
low shear rates (< 100 s~’) than at high shear rates (> 100 s-'). Estimated
repeatability was + 10 % and +5 %,
respectively. If long dies are used (L/D > 20), the effect of the geometry of the
capillary inlet can be
disregarded if the inlet angle is = 90°.

The reproducibility of the method was estimated by measuring, in seven

laboratories, the viscosity of PVC at
180 °C and 190 °C and that of PP at 210 °C and 240 °C. Reproducibility was found to
be poorer at low shear
rates (< 100 s~1) than at high shear rates (> 100 s-1), being + 20 % and + 10 %,
respectively.

From an examination of the results, it can be seen that reproducibility is affected

by

— the order in which the various shear rates are examined during a single test;

— the sensitivity of the pressure-sensor or force-sensor used: measurements cannot

be carried out with the
same precision at high pressures (high shear rates) and at low pressures (low shear
rates) using the
same sensor;

— the method used to determine the shear stress: measurement of pressure at the
capillary inlet is
preferred since it is more accurate.

The effect of the cleanliness of the capillary on the results was not investigated
in these tests.
In the second interlaboratory test programme, completed in 1996, 20 laboratories
took part in total, using
polyethylene (PE) and glass-fibre-filled polypropylene (GFPP) samples |l. The
precision data presented in

Table 4 on the measurement and determination of extrusion pressure, entrance

pressure drop and shear
viscosity corrected for both entrance effects and non-Newtonian velocity profile
were determined.

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ISO 11443:2005(E)

Values presented are for 95 % confidence levels, these values having been
determined using a factor of
2,8 times the calculated standard deviation values.

NOTE 1

NOTE 2
in accordance with Reference [7].

The contraction ratio is defined as the ratio of the barrel diameter to the die
diameter.

NOTES Seealso Annexes Ato C.

Table 4 — Precision data for extrusion rheometry
Extrusion pressure measurement
Material Polyethylene Glass-fibre-filled
polypropylene
Test temperature, °C 190 230
Repeatability (95 % confidence) 20% 38 %

(Weissenberg-Rabinowitsch correction)]

Shear viscosity measurement [corrected for entrance pressure drop and non-Newtonian
velocity profile
Material Polyethylene oho
Test temperature, °C 190 230
Repeatability (95 % confidence) 20 % 24 %
Reproducibility (95 % confidence) 28 % 34 %

Entrance pressure drop measurement

Material Polyethylene Polyethylene ee

Test temperature, °C 190 190 230
Contraction ratio 15 9,55 to 15,5 15
Reproducibility (95 % confidence) 42% 50 Yo 56 %

10 Test report

10.1 General

The test report shall include the following information, as applicable:

a) areference to this International Standard and any referring standards;

6) the information specified in 10.2, 10.3 and 10.4, as applicable;

c) the date of the test.

© 150 2005 — All rights reserved

The standard deviations and repeatability and reproducibility limits (95 %

confidence values) were determined

23
ISO 11443:2005(E)

10.2 Test conditions

a)
b)

c)

f)

g)
h)

i)

a description of the material under test;

details of any conditioning or preparation of the material or sample, e.g. drying
or compounding;
the method used (A1, A2, B1 or B2);

a description of the rheometer used and its barrel diameter D,;

the diameter D, length / and ratio of length to diameter L/D of the straight
section of the capillary die used,

and the degree of precision of these measurements, if applicable;

the thickness H, width # and length £ of the slit die used, and the degree of
precision of these
measurements, if applicable;

a description of the capillary-die or slit-die inlet angle profile;

a description of the technique used to measure the extrudate swelling;

the temperature at which the measurements were made:

the pressure below the die exit when extruding to pressures other than atmospheric
pressure, a
description of the method used to obtain and measure this pressure, and the
precision of measurement of
the pressure, if applicable;

the sample-preheating time;

the dwell time;

the dwell time corresponding to the appearance of an alteration in the material, if

applicable;

the maximum permissible test duration, if applicable;

the extrusion time;

details of any deviations from the requirements of this International Standard and
any incidents likely
to have influenced the results.
10.3 Flow characteristics

10.3.1 General

Report whether the shear rate, the shear stress and the viscosity are “apparent” or
“true” values.

Report the method of viscosity determination if the Bagley or pressure drop versus
distance plots are non-
linear.

For plastics which are not wall-adhering, present the results in the form of
apparent shear stress plotted as a
function of flow rate Q, or vice versa.

10.3.2 Graphical representation

The following plots may be included, as necessary:

24

log shear stress versus log shear rate, or vice versa;

log viscosity versus log shear stress or log shear rate;

© 150 2005 — All rights reserved

————
ISO 11443:2005(E)

— log viscosity versus the reciprocal of absolute temperature at constant shear

stress or shear rate;
— log viscosity versus temperature in degrees Celsius at constant shear stress or
shear rate;

— log critical shear stress or log critical shear rate for each of the observed
effects (see 3.19 and 3.20)
versus the reciprocal of absolute temperature;

log critical shear stress or log critical shear rate for each of the observed
effects (see 3.19 and 3.20)
versus temperature in degrees Celsius;

— log volume flow rate versus log shear stress, or vice versa;

— pressure versus die length;

— pressure versus distance of pressure transducer from die exit (slit dies);

— log pressure correction versus log shear stress or log shear rate or log volume
flow rate;

— capillary-die or slit-die inlet and exit pressure loss versus shear stress or
shear rate or volume flow rate;
— swell ratio at room temperature or at the test temperature versus shear rate or
volume flow rate:

— percent swell at room temperature or at the test temperature versus shear rate or
volume flow-rate.
Apparent and/or true values of shear rate, shear stress and viscosity may also be
presented.

10.3.3 Individual values

These may be given for a given series of test conditions, as necessary:

— shear stress, in pascals;

— shear rate, in reciprocal seconds;

— viscosity, in pascal seconds;

— swell ratio at room temperature;

— percent swell at room temperature;

— swell ratio at the test temperature;

— percent swell at the test temperature.

Apparent and/or true values of shear rate, shear stress and viscosity may also be
presented.

10.4 Visual examination

If visual examination is possible, report any change in the surface appearance of

the extrudate (e.g. break in
flow, distortion of extrudate), noting the test conditions at which the change
occurs.

Such changes may correspond to the critical shear stresses. In this case, note the
values individually in the
test report as “visual” critical shear stresses.

In addition, if the material changes colour, report the corresponding dwell time.

© 150 2005 — All nghts reserved 25

ISO 11443:2005(E)

Annex A
(informative)

Method of correcting for the influence of H/B on the apparent shear rate

Equation (4) given in 8.2.3 for the apparent shear rate is valid only for an
infinitely wide slit. Equation (4)
therefore gives the apparent shear rate which will exist when the volume flow rate
in the die-length direction is
Q over a distance 8 in the die-width direction and assuming that no flow takes
place in the width direction or in
the thickness direction. At finite ratios of A/8, Equation (4) is still a good
approximation, as shown in
Figure A.1. This shows the ratio of the apparent shear rates obtained, at identical
volume flow rates ©, from
Equation (4) and from Equation (A.1), a corrected equation given in reference [5].

y= 7 og Sf 1 xB) is
BH el ci

where # is an odd integer.

x
1,06

je

1,02

0 0,1 02 03 X
Key
x thickness-to-width ratio H/8
Y° shear rate ratio ¥-4p/7'ap

Figure A.1 — Shear-rate ratio ;,,/ iy versus thickness-to-width ratio H/8

26 ® 180 2005 — All rights reserved

ISO 11443:2005(E)

Dividing Equation (4) by Equation (A.1) gives Equation (A.2):

amb ) |
2H }|

im =| ; =| '4- near 45 Os tanh

se ' fn

(A.2)

which expresses the ratio of the apparent shear rates as a function of the
thickness-to-width ratio /8.

The summation term in Equation (A.2) is 1,004 4 when 4/8 = 0,3. Thus the corrected
apparent wall shear rate
is given (using Equation 4) by

WT < :

PS, - $2, [1+ |[1-0,6302 ] (A.3)

BHE|\ B}\, By}

The error introduced by using Equation (4) instead of Equation (A.3) is less than
3% for thickness-to-width
ratios less than 0,1.

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ISO 11443:2005(E)

Annex B
(informative)

Measurement errors

B.1 Error due to piston friction

Friction is caused by contact between the piston and the barrel, Usually, the
effect of the frictional farce thus
produced is negligible compared with the pressure drop through the capillary or
slit die. It should, however, be
confirmed that the frictional force is negligible by carrying out a dry run at the
test temperature.

This precaution may be disregarded if measurements are made at constant velocity,

and pressure is
measured using a pressure sensor placed in the immediate vicinity of the die inlet.

B.2 Error due to back-flow of material

The clearance between the piston head and barrel may allow a small quantity of the
sample to flow back past
the piston instead of through the capillary or slit die. This results in a measured
shear rate lower than that
calculated from the piston velocity. Usually, this error is negligible. In certain
cases, however, particularly
when the piston is operating at low speed and with a sizeable load, a correction
may be necessary. Material
which has flowed back past the piston head is collected and weighed, and its mass
compared with that of the
extrudate produced during the same time interval, in order to determine the
percentage error due to back-flow.

B.3 Error due to melt compressibility

Some liquids exhibit very high compressibility. Given that the shear rate at the
die wall is calculated fram the
piston travel speed, an error is therefore introduced owing to the drop in
hydrostatic pressure (and hence the

decrease in density) along the length of the die. With the decrease in density of
the liquid, the flow velocity
increases, resulting in an increase in shear rate towards the exit of the die.

B.4 Error due to non-zero liquid velocity at the die wall

The calculations relating to flow in the die are based on the assumption that the
velocity of the liquid is zero at
the die wall. For high-viscosity polymer melts, slippage may occur between the
polymer and die wall.

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ISO 11443:2005(E)

Annex C
(informative)

Uncertainties in the determination of shear viscosity by capillary

extrusion rheometry testing

C.1 Analysis of uncertainties

The combined uncertainty u(y) of the measurand » (the quantity to be measured) can
be determined from the
partial derivatives of the function y = /(x,) and the uncertainties u(x,) in the
parameters x, of that function.
Assuming that individual uncertainty sources are uncorrelated, the combined
uncertainty w,(v) can be
computed using the root sum squares:

welv) =f fewulx,)I? (C.1)

i=1

where

c:

, is the sensitivity coefficient (partial derivative) associated with the quantity

x;

u(x,) is the uncertainty in that quantity.

The combined uncertainty u.(v) corresponds to one standard deviation and therefore
has an associated
confidence level of approximately 68 %. Assuming a normal distribution, then an
expanded uncertainty LU’,
equivalent to a 95 % confidence level, can be determined using a coverage factor of
2, i.e. twice the combined
uncertainty value. The relative uncertainty is the ratio of the uncertainty in the
parameter to the value of the
parameter.

To determine the uncertainties, an expression relating the shear viscosity to the

measurement parameters
must first be derived. From Equations (3), (7) and (12), Subclause 3.7 and the
equations

. , [ant]
Y=Yap|—a, | (C.2)
dloga,]
n= =P (C.3)
dlogr
320
Fen = (C.4)
ap np?
and
2
D
o-— (C.5)

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ISO 11443:2005(E)

the shear viscosity corrected for entrance pressure drop and non-Newtonian velocity
profile (Weissenberg-
Rabinowitsch correction) is given by

pb’ 4n
where
Pap is the apparent shear rate;
OQ is the volume flow rate;
is the barrel diameter;
v is the piston speed;
p is the extrusion pressure;
Pe is the entrance pressure drop correction;
D is the capillary-die diameter;
L is the capillary-die length.

Thus, using Equations (C.1), (C.2) and (C.6), it can be shown that the combined
uncertainty in the measurement
of shear viscosity (17) is given by

2
= | (4e2d¥ 4 (lea? x) 2u(Dp) > ,{ u(pP+ulpe)? | {__uln)
ucl4)=1 ( D +| L +| . 2 Db - (p—pele n(3n #1) (C.7)

and the combined uncertainty in the shear rate u.() by

ere (222) (o] (2a) ae)

The ratio of the uncertainty in the quantity u(x;) to the value of the quantity x,
is the relative uncertainty for that
parameter, e.g. u(D)/D is the relative uncertainty in D.

(C.8)

The effects of the temperature dependence of viscosity and degradation can be

incorporated into Equation (C.7)
as additional terms, thus:

2
=, | (42) any (sy. 249) u(p)? + up.) u(r) oye?
uel) = > el Pa ml Gas | eee)
(C.9)

where /{d) is the relative uncertainty due to degradation and /(4 is the relative
uncertainty due to the combined
effect of the temperature dependence of viscosity and errors in the test
temperature. The latter, (@, may be
expressed as

£(0)= Zuo) (C10)

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ISO 11443:2005(E)

Thus Equation (C.9) can be used to estimate the uncertainty in the measurement of
shear viscosity given the
uncertainties in, and magnitude of, each term. Equations (C.7) and (C.9) are for
true shear viscosity corrected
for both entrance effects and the non-Newtonian velocity profile (Weissenberg-
Rabinowitsch). Equation (C.8)
is for true shear rates. Equivalent expressions can be deduced for apparent shear
viscosity and apparent
shear rate by removing the terms involving » and u(n) from these equations
[effectively setting u(n) to zero]
and replacing the true shear viscosity term iin Equation (C.7) by the apparent
shear viscosity term 17,,, and
the true shear rate term » in Equation (C.8) by the apparent shear rate term 7, .
Similarly, an expression for
apparent shear viscosity that has not been corrected for entrance effects can be
obtained by removing the
terms u(p,) and p,, in Equation (C.7) [effectively equating u(p,) and p, to zero.

C.2 Worked example

AS a specific example, uncertainty values for the various components in the

measurement of shear viscosity
have been calculated and presented in Table C.1, based on the tolerance values and
assumptions stated in
this International Standard. To avoid excessive over-complexity of the uncertainty
analysis, the calculations
have been based on the measurement of shear viscosity using two dies: a long die of
20 mm length and a
short die of negligible length that is used to determine the entrance pressure
drop.

In carrying out an uncertainty analysis on a specific instrument, it would be

preferable to utilize the calibration
data to determine actual quantity ranges and, if appropriate, assume normal
probability distributions for those
ranges rather than rectangular distributions as assumed here.

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ISO 11443:2005(E)

Table C.1 — Uncertainty terms and estimates for shear viscosity measurement

: a Standard Relative
Quantity, symbol a| Probability -~.. ¢| Quantity | Quantity ‘
and units Type distribution © Divisor value, x range ® pee uncertamty
ute) ular
Capillary-die length £, mm B R va 20 + 0,025 0,014 0,000 7
eo ems] R 43 1 + 0,007 0,004 0,004 0
Barrel diameter Dy, mm B R 3 15 = 0,007 0,004 0,000 27
SER ICRNCIN | R 13 variable | =!% i 0,005 8!
Pa of range
/ variable 1%
Pressure correction p,, Pa B R V3 (assume aera _ 0,005 8 f
Po = 0,2p) :
oo rate measurement OQ, B R \3 _ £1% _ _
mm/s
Piston speed v, mmis B R V3 — +1% 9 — 0,005 89
Gradient of log'r versus’ | 4 N 1 0.4 0,03" 0,03 0,075
log Pap plot, »
Temperature @ °C ? _ 245? Ti
(for @ < 200 °C) B R v3 £1,5°C 0,87 0,008
Temperature @ °C \ es a96° j
(for 200 °C < @< 300°C) B R va 22,5°C 14 0,014
Temperature 4, °C | — + 2 j
(for @> 300 °C) B R V3 +3,5°C 20 0,020
Variation in extrusion
pressure with time due to B R N3 — +5% a 0,029 *
degradation effects
3. The uncertainties in type A quantities are estimated by statistical means. They
are based on experimental observations of the
variation in the values and are assumed to have a normal distribution (N). The
uncertainties in type 8 quantities are estimated from the
specification of tolerances given in this International Standard. In all type B
cases, the quantities are assumed to have a rectangular
distribution (R)}, i.e. the actual value has an equal probability of lying anywhere
in the quoted tolerance range.

ed, @ The standard uncertainty is obtained by dividing the quantity range (d) by
the divisor (c) that is based on the assumed
probability distribution (b} of that quantity’s range.

f The values quoted are for using the pressure traneducer at its full range. When
using the transducer in a lower part of its range, this
value must be factored accordingly, e.g. at 50% of range the relative uncertainties
are doubled to 0,012. The uncertainties in the
measurement of extrusion pressure p and pressure correction », were taken to be the
same, specifically 1% of the full-scale range of
the pressure transducer. Also it was assumed that the magnitude of the pressure
correction », was one-fifth of that of the extrusion
pressure for the long die, thus p, = 0,2 x p.

The assumptions stated here imply that different transducers, of appropriate range,
were used for each of the long and short dies.
Where the same transducer is used in both cases, the uncertainties in », could be
greater, estimated to be by a factor of
approximately 5.

9 The uncertainty in the piston speed is approximately the same as that in the flow
rate as the contribution due to the relative
uncertainty in the barrel diameter is negligible.

h The quantity range estimated for » is for one standard deviation.

id The uncertainty in the measurement of shear viscosity is related to the

temperature dependence of the test sample. For the high-
density polyethylene and glass-fibre-fillad polypropyene samples used in the
intercomparison (Sl it was estimated, based on
Measurements made at different temperatures, that the temperature dependence of
shear viscosity was of the order of 1 %5/°C. For
polymers having temperature dependence factors different from this, the value of
the relative uncertainty must be factored accordingly,
6.9. for a material having a temperature dependence of 2 %/°C then the relative
uncertainty is 0.028 for ¢ = 200 °C. It also assumes that
the quantity range is equal to the sum of the permitted spatial and temporal
variations in temperature.

Kin determining the values of the uncertainty in the measurement of shear viscosity
where degradation may occur, it was alsa
assumed, in accordance with this International Standard, that testing is carnied
out over a period during which the extrusion pressure
(and hence viscosity) does not change by more than 5%.

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ISO 11443:2005(E)

Given these assumptions, and the values presented in Table C.1, expanded
uncertainty values for shear
viscosity have been calculated for various temperature errors and temperature
dependencies, for utilization of
only part of the pressure transducer range, and with and without a contribution due
to degradation effects, as
shown in Table C.2. The values calculated assuming a 5 % effect of degradation are
presented in brackets.

Table C.2 — Expanded uncertainties in measurement of true shear viscosity

All values expressed as percentages (%)

Temperature | Temperature | Expanded uncertainties (95 % confidence level) in

viscosity measurement due to
dependence error use of only part of the range of the pressure transducer,
excluding degradation
of viscosity effects [values in brackets include 5 % effect due to degradation,
/{d) = 0,05]
i +°C using 100 % of using 50 % of using 20 % of using 10 % of range
range of pressure | range of pressure | range of pressure of pressure
transducer transducer transducer transducer

0 _— 7,9 (9,7) 8,7 (10,4) 11,1 (12,6) 21,8 (22,5)

1 15 8,1 (9,9) 7 8,8 (10,6) 11,3 (12,7) 21,9 (22,6)

1 2,5 8,4 (10,2) 9.1 (10,8) 11,5 (12,9) 22,0 (22,7)

3 1,5 9,5 (11,1) 10,0 (11,6) 12,3 (13,6) 22,4 (23,1)

NOTE Values quoted are to one decimal place to show the trends in values, and not
as an indication of the
accuracy of such values.

2 Corresponds to the case for the relative uncertainties presented in Table C.1,
using a relative uncertainty in the temperature
of 0,008 7.

The expanded uncertainty (95 % confidence level) in the apparent shear rate is
calculated to be approximately
2,7 % and in true shear rate approximately 7 %, the difference being due to the
Weissenberg-Rabinowitsch
correction for the non-Newtonian velocity profile and the uncertainty associated
with it (via the uncertainty in
the gradient n of the log rversus log 7, plot). This correction is also a
significant factor contributing to the
overall uncertainty in the Weissenberg-Rabinowitsch-corrected true shear viscosity.
In the above example,
this factor alone gives an expanded uncertainty in true shear viscosity of 6,8 %.

The significant effect of using the pressure transducer in only the lower part of
its range is clearly apparent in

Table C.2. Using a transducer at only 10 % of its range can increase the
uncertainty by a factor of up to
about =3.

These uncertainty values do not take into account errors due to viscous heating and
the pressure dependence
of viscosity. Both these factors will increase the level of uncertainty of the
measurements and the
reproducibility of the results, particularly when different test conditions are
used to obtain viscosities at similar
shear rates, for example by using different die dimensions.

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ISO 11443:2005(E)

[1]
[2]
[3]
[4]

[5]
[8]

Bibliography

CHUNG, B., AND COHEN, C.: Polym. Eng. Sci., 25 (1985), pp. 1001-1007
LuPTON, J.M., AND REGISTER, J.W.: Polym. Eng. Sci., 5 (1985), pp. 235-245
BAGLEY, E.B.: J. Appl. Physics, 28 (1957), p. 624

EISENSCHITZ, R., RABINOWITSCH, B., and WEISSENBERG, K.: Mitt Dtsch. Mat.-Prf.-Anst.
(Bulletin of
German Materials-Testing Institution), Sonderheft 9 (1929), p. 91

McxeELvey, J.M., Polymer Processing, John Wiley and Sons, New York/London (1962)

Ripes, M., AND ALLEN, C.R.G.: Capillary extrusion rheometry intercomparison using
polyethylene and
glass-fibre filled polypropylene melts: measurement of shear viscosity and entrance
pressure drop,
NPL Repert CMMT(A)25, May 1996, National Physical Laboratory, Teddington,
Middlesex,
United Kingdom, TW11 OLW

ISO document TC 61/SC 5WG 21 N18 E 14, Determination of the precision of a test
method —
Practical guide

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