9/26/2016

“Rubber Process Analyzer – RPA.

Bridging the gap between polymer and
compound rheological properties and true
material processing on the shop floor”.

Henri G. Burhin
www.polymer-process-consult.be
TA Rubber testing Seminar
Greenville SC, September 2016

Copyright TA Instruments, USA

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Rubber Process Analyser, presentation outline

• Instrument design and history

• Testing scope
• Elastomers (pure gum).
• Rubber compounds
• Polymer case studies
• AMW, MWD and LCB
• Compound case studies
• Mixing
• Extrusion (surface aspect, output and green-strength).
• Thixotropy
• Silica mixing
• Advance curemeter
• Cure fundamental parameter and cure simulation
• Sponge compounds.

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Rubber Process Analyser

• History and market position

• Development: late 80ies early 90ies
• Commercialization: 1992
• Aim: address rubber processing problems
• Original design: Moving Die Rheometer
• Retain MDR curemeter capability
• Isothermal and non isothermal cure
• Monitoring of sponge compound blowing
• Became soon popular at large rubber factories (tire
manufacturers)
• Much less popular at small to medium size companies who
found it:
• Far too complex to operate and to understand
• Expensive

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Limitation of Standard Tests (Mooney viscosity)

SCARABAEUS
Mooneyprüfung
Entwicklung

80.0

1
64.0
η
viscosity
Mooney-Viskosität [MU]

48.0 Polymer C1
Polymer C1
Polymer B1
Polymer B1
Polymer A1
0,1
Polymer A1
32.0

ML1+4
16.0

0,01
0.0
0.0 1.6 3.2 4.8 6.4 8.0
Zeit [min]
0,01 0,1 1 10 100
.
SCARABAEUSGMBH- info@scarabaeus-gmbh.de- Tel.:+49(0) 6403/9034-0
shear rate,γ

Mooney Viscosity ML1+4: Conversion factors for MU to

Nm and RPM to true shear
Shear rate 1.6 s-1 (2 rpm) rate in s-1.
But a torque rather than a viscosity. 1 MU = 0.083 Nm
2 RPM = 1.58 s-1 (
 )

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Curemeters design and limitations.

Moving Die Rheometer “MDR”

Improperly called rheometer
Scarabaeus GmbH Amplitude 2.79%
Meß- undProduktionstechnik Frequenz 1.67Hz
SISV50 Abbruchkriterium

5.0 2.00

1.80

4.0 1.60

1.40

• Rheometer
Elastischer Anteil [dNm]

3.0 1.20

• Biconic dies

Tan Delta
1.00

2.0 0.80

0.60
• closed die system
1.0 0.40
• 100cpm /1.67 Hz
0.20 • 0.5° / 7% strain
0.0 0.00
0.0 2.0 4.1 6.1 8.2 10.2
Zeit [min]

SCARABAEUSGMBH- info@scarabaeus-gmbh.de- Tel.:+49(0) 6403/9034-0 one point method

•Standard test It is important to get

•Isotherm more information to help
•Anisotherm the developer
•S‘ and S‘‘ -> TanDelta
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TA Instruments – RPA, a true rheometer

0
0 5 10 15 20 25 30 35 40

γ1 γ2
Viscosity is measured with various -1

-2

types of viscometers and rheometers. A -3

Z e it
rheometer is used for those fluids which
cannot be defined by a single value of γ
1 .5
ω1
1

viscosity and therefore require more 0 .5

parameters to be set and measured than

0
0 5 10 15 20 25 30 35 40

-0 .5

is the case for a viscometer -1 .5

-1

ω2
Z e it

https://en.wikipedia.org/wiki/Rheometer

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RPA Rheometer (Closed boundary DMA)

γ
1.5
ω1 Frequency:
1
RPA 0.001…50.0 Hz
0.5
Step 0.001Hz
0
0 5 10 15 20 25 30 35 40

-0.5

-1

-1.5
ω2
Zeit

Ω,ϕ θ
Open boundary DMA
α ARES – ARES G2

R
M
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Dynamic testing typical output from

frequency sweep

In a single test,
frequency sweep
provides several
outputs
• Dynamic viscosity
(η*)
• Dynamic modulus
(G’ and G”)
• Tangent δ

One single test

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Effect of Molecular Weight Distribution (MWD)

on compound extrusion behavior

Surface defect as
« shark skin »on
extrusion

Tentative conclusion
Shark skin effect in extrusion is due to
MWD effect and not LCB effect.

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Effect of Molecular Weight Distribution (MWD) on

compound extrusion behavior
1

0.9

0.8
Crossing 1 Ligne 1 Ligne 2

0.7 LCB Index LCB Index

4.39 5.47
0.6
Tangent δ (-)

0.5

0.4 50°(EPDM3)

0.3 125°EPDM3)

Crossing 2
50°(EPDM1)
0.2

125°(EPDM1)
0.1

0
0.1 1 10 100 1000 10000 100000
Frequency (Rad/s)
1

0.9
• LCB contend of both polymers was Production line 1

0.8
very similar 0.7
Production line 2

• The extrudability problem (shark skin) 0.6

dwt/d(logM)

was found in the large reduction of 0.5

small molecules in the problem 0.4

polymer 0.3 Maximum extrusion speed for no surface

defect
• Very small molecules act in compound 0.2 Production line 1: 25 m/min
Production line 2: 2 m/min
as excellent processing aid 0.1

• The higher tangent δ value at high 0

3.5 4.5 5.5 6.5

frequency for the good processing Log MW (Daltons)

polymer confirmed this result.

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RPA Rheometer Strain sweep

From small strain to large strain (SAOS to LAOS)

3
Strain:
2 RPA 0.005…360.0 °
1
Step 0.01°
0
0 5 10 15 20 25 30 35 40

-1
γ1 γ2
-2

-3
Zeit

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Comparison of Butyl IIR (RPA)

Technical information

Instrument: RPA flex

Company: TA Instruments
Sample A) : Synthetic Butyl
Edbrisic - BK
B) : Synthetic Butyl
Exxon
Film: Dartek - polyamid film

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Comparison of Butyl (RPA)

Test Program

Temperature Frequency Strain

Method
[°C] [Hz] [°of arc]

Frequency-Sweep 150 0.05 - 50 0.5

Strain-Sweep 150 0.2 0.5 - 90

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Comparison of Butyl (RPA)

Frequency - Sweep, 150°C, 0.5°of arc, G’, G”

Crossover Point at different Frequencies

=> Different Molecular Weight

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Comparison of Butyl (RPA)

Frequency - Sweep, 150°C, 0.5°of arc, tan δ

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Comparison of Butyl (RPA)

Frequency - Sweep, 150°C, 0.5°of arc, η” (Log-Scale)

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Comparison of Butyl (RPA)

Frequency - Sweep, 150°C, 0.5°of arc, η” (Lin-Scale)

15.4%

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Comparison of Butyl (RPA)

Strain - Sweep, 150°C, 0.1 Hz, G’, Tan δ

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Comparison of Butyl (RPA)

Strain - Sweep, 150°C, 0.1 Hz, Long Chain Branching

LCB index typical repeatability

95% confidence
Different Branching Index ±0.09

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Rubber compound process troubleshooting

Rubber compound extrusion.

Serious processing problem in production
Summary of observations:
• All batches passed standard QC tests.
• QC test involves rheometer only (MDR).
• One batch gave higher extrusion head pressure and temperature,
higher swell and surface defect (“Orange skin”) suggesting possible
scorch in the extruder.
• The faulty batch was compared to a trouble free batch.

Good
Bad
Good
Bad
Both compounds have identical or almost identical ML and
160° C
MH.
The faulty compound exhibits a lower cure rate (?)
The faulty compound exhibits a significantly LONGER
scorch time (??????)

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Rubber compound process troubleshooting

Non isothermal cure test (80° C – 180° C)

Non isothermal cure test confirms

identical ML and MH and longer
cure time for the faulty batch
Some differences are observed on
Good G’ and Tangent δ before cure
Bad
suggesting that viscoelastic
Some differences in
the uncured state properties of uncured compounds
being different.

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Rubber compound process troubleshooting

RPA testing “Payne” diagram – 100° C

Bad compound shows higher

modulus at both low and high
strain.
Good This suggest that filler
Bad
dispersion is not the cause of
the problem.
The problem therefore stays
in either polymer quality of
filler content.

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Rubber compound process troubleshooting

Frequency sweep at 100° C Strain sweep at 100° C

Bad and good batches show almost

identical viscoelastic properties in both
frequency and strain sweep.
Only some significant difference is
observed at very low shear rate
(frequency) on Tangent δ.

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Rubber compound process troubleshooting

LAOS test 100° C, 90° arc, 0.2 Hz

The bad compound has
been found to dissipate
almost 10% higher energy
W disp.
per cycle in non-linear
(J) conditions.
Good 168.94 Premature scorch for this
Bad 177.11 compound is produced by
large heat generation in the
extruder.

ISO Standard method 4664-1

Where ε is the ellipse area or the energy lost per
oscillation
γ0 is the maximum strain
ε = π.γ .σ .sin δ
0 0
σ0 is the maximum stress

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Practical example, linear and branched Polymer

Keltan 6950 Nordel 5565

Mooney ML 1+4 [MU] 65 65

Ethylen [%] 48 50

ENB content [%] 9 7.5

Distribution medium medium

Degree of branching Branched Linear

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Practical example, linear and branched Polymer

Frequency Sweep

Shear - thinning

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Practical example, linear and branched Polymer

Frequency Sweep

Mooney
Low
Frequency

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Physical description of Polymers

Strain Sweep - LAOS

High Strain

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Physical description of Polymers

Strain Sweep - LAOS

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Recipe of Compounds

Keltan Nordel
compound compound
phr phr
EPDM (LCB) 100
EPDM, linear 100
Fast Extrusion Furnace (FEF)
carbon black 95 95
Chalk 50 50
Paraffinic Oil 65 65
ZnO 6 6
Stearic acid 1 1
Drying agent 9 9
Antiaging agent 0,5 0,5

Sulfur and accelerator 4,5 4,5

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Physical description of filled Polymers

Strain Sweep - PAYNE

A. R. Payne, Rubber Plast. Age 42, 963 (1961)

Pic. 2.2.: schematic representation of the composition of the dynamic modulus
of various proportions by Payne [16]

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Payne diagram, increasing filler content

G* (kPa)
500
10 phr Variation of G* of
400 20 phr reinforced rubber
40 phr compound in the strain
300 60 phr domain

200

100

0
0.1 1 10 100 1000
Strain (%)

Henri Buhrin, "Visco-elasticity Properties of Polymers and Compounds. From Linear

to Non Linear Visco-elasticity, Benefit and Potential”

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Compound, Reinforcing fillers

Scarabaeus GmbH Prüftemperatur 100 °C

Meß- und Produktionstechnik

SIS-V50

1500

1400
Delay time before start test
1300

0.5, 1.0, 2.0, 4.0, 8.0 min

1200

1100

1000
Schubmodul G* [kPa]

900
10357
800 10359
10361
700 10363
10365
600

500

400

300

200

100

0
0.01 0.1 1

RPA Rheometer Amplitude [Grad]

SCARABAEUS GMBH - info@scarabaeus-gmbh.de - Tel.:+49 (0) 6403/9034-0

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Uncured compound thixotropy in

DMA measurements.

Instrument closure

Compound property
change after instrument
CLOSURE!

1800
1600
1400
1200
G' (kPa)

1000
800
600
400
200

Non stationary conditions 0

0.01 0.1 1 10 100
Strain (%)
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Uncured compound thixotropy in DMA

measurements.
What is thixotropy ? – Viscosity time dependence

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Compound, Reinforcing fillers

Scarabaeus GmbH
Meß- und Produktionstechnik
SIS V50

8 00.0

7 00.0

6 00.0

5 00.0
Schubmodul G' [kPa]

0.05° 5744
4 00.0 0.05° 5747

3 00.0

2 00.0

1 00.0

0.0
0 .0 6.0 12 .0 18.0 2 4.0 30 .0
Zeit [m in]

SCA RA BA EUS GMBH - info@s carabaeus -gmbh.de - Tel.:+49 (0) 6403/9034-0

xx:yy

Heinrich, dN/dt=kN2 ,1995

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Physical description of filled Polymers

Strain Sweep - PAYNE

Tensile Strength [Mpa]

Keltan cmp. 9.25

Nordel cmp. 8.32

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Kinetic description of filled Polymers

Vulcanisation

Keltan Nordel
compound compound

S' Min [dNm] 1.21 1.4

S' Max [dNm] 20.44 23.17

ENB content [%] 9 7.5

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Physical description of filled Polymers

Frequency Sweep

5% Shear thinning

15%

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Extrusion – Machine parameters

Extrusion Keltan compound Nordel compound

70 70
Temp. extruder [°C]

91.3 102
Pressure die [bar]
111.5 124
Current [A]
10.5 10.5
Speed [m/min]

114 114-125
Temp. Mass [°C]

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Additional use of Payne diagram

Tread compound formulation
Silica compound
Ingredient PHR
Buna VSL 4020-1 103.1
Buna CB 10 25.0
Ultrasil 3370GR 80.0
Silane X50S 12.5
High aromatic oil 5.0
ZnO 2.5
Stearic acid 1.0
6 PPD 2.0
Wax 1.5

Patent Application EP 0501 227, Michelin, R. Rauline, February 25th, 1991

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Silica silane chemistry

TESPT (Si69 DEGUSSA) Silica "silanisation"
Bifunctional organosilanes

Mixing from 140°C to 160°C

Oligosulfane Group
C2H5O OC2H5
C2H5O OC2H5 C2H5O Si-(CH2)3-S-S-S-S-(CH2)3-Si OC2H5
C2H5O Si-(CH2)3-S-S-S-S-(CH2)3-Si OC2H5 C2H5O OC2H5
C2H5O OC2H5
OH OH OH OH
(Varying from 2 to 7 sulphur atoms)
-O-Si-O-Si-O- SILICA -O-Si-O-Si-O-
Alkoxy Groups
G*0

Filler/Filler weak interactions

Van Der Waals Interactions (Carbon
Log (G*)

Black)
Hydrogen bonding (Silica) given by
Hydroxi group

G*∞
Polymer/Filler strong interactions Bond rubber
Occluded rubber
Hydrodynamic effect (Filler loading)
Polymer AMW

0.01 0.1 1 10 100 1000

Strain (%)

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Masterbatch mixing procedure

MASTERBATCH MIXING PROCEDURE

Internal mixer: 3 L Tangential

Time (mins) Addition Temp (°C) Energy
(W.h)
0 Add polymers 65 0

½ Add ZnO, ¾ silica, ¾ X50S and stearic ? 20

acid

Add rest of silica, rest X50S, wax, ? 550

6PPD and oil

Sweep ? 700
Dump at 750 W.h ? 750

Remill
0 Add masterbatch 65 0

Dump at 650 W.h ? 650

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Mixing conditions and Payne diagram

Mixer Mixer Dump temp Dump temp Total
speed step speed step step 1 step 2 mixing
1 2 energy
CPD 1 65 65 155 180 4.123
CPD 2 55 55 145 161 4.076
CPD 3 MIXING
45 CYCLE
45 IMPROVEMENT
146 (Payne
146 Diagram)
4.067
CPD 4 65 45 153 155 4.133
G' (KPa)
1,000

Increasing reaction
SiO 2 > Silane increased silane
degradation
100

No 1 (65 RPM)
No 2 (55 RPM)
No 3 (45 RPM)
No 4 (65&45 RPM)

10
0.10 10.00 1000.00
1.00 100.00

Strain (% SSA)
100° C, 0.1 Hz
Uncured

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Mooney viscosity versus visco-elasticity

At first, Mooney viscometer was used for QC of silica

compounds

MS(1+4) G’@1% S’@450%

100°C strain (kPa) strain
(dNm)
CPD 1 68.7 448 27.69
CPD2 65.4 568 23.75
CPD3 68.1 754 19.75
CPD4 60.5 448 19.04

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TESPT versus TESPD

Silica silane reaction can essentially be measured

after mixing second G' vs. Strain
stage
TESPT vs. TESPD (Masterbatch & Remill)
G', KPa
10,000

Masterbatch

1,000

Remil

100

6.00 phr TESPD Optimised mixing (65-45 RPM)

6.25 phr TESPT Optimised mixing (65-45 RPM)
6.00 phr TESPD High speed mixing (65 RPM)
6.25 phr TESPT High speed mixing (65RPM)
10
0.10 10.00 TAINSTRUMENTS.COM
1000.00
1.00 100.00

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Silica mixing test conclusion

Careful visco-elasticity measurements on masterbatch can rapidly and
easily:
• Fully characterize Payne diagram
• Payne diagram low strain elastic modulus provides essential
information of silica/silane chemical reaction
• Payne diagram high strain elastic modulus or better elastic
torque provides information on the uncured compound
processability

2 industrial uncured compounds

• Compound 1 can be processed
but won’t provide adequate
cured properties
• Compound 2 will provide
adequate cured properties but
cannot be processed.

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Physical description of filled Polymers

Strain Sweep – Injection molding compounds

Highly variable mixing

Large difference in
Carbon Black
dispersion.

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Physical description of filled Polymers

Strain Sweep
Energy dissipation in process
LAOS – 90° Arc – 100°C, 0.1 Hz
ε = π.γ0.σ0.sin δ

UNCONTROLLED
MIXING PROCESS

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Instrument repeatability, Compound

homogeneity and production variation

Relevant QC Irrelevant QC
•Instrument repeatability Poor material homogeneity
•Additional mixing compound More variation within one batch than between
•Sample number: 15 batches

•CV (Std Dev/Mean) ≈ 0.75% Complex modulus (G*)

@ low frequency
•Production compound homogeneity Mean 1232.5 Within
•Batch number: 1 Std Dev 166.1 batch
•Sample number: 12 CV (%) 13.5
•CV ≈ 0.75%

•Production variability
•Batch number: 18 Mean 940.0 Between
•CV from 15.43% to 4.72% Std Dev 50.7 batch
CV (%) 5.4

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Enhanced Calculation MDR: Cure Kinetic

SCARABAEUS GMBH Prüfdatum 12.12.2003 Prüftemperatur 180 °C

Postfach 200 163 Amplitude 0.50° Frequenz 1.67Hz

D-35399 Langgöns

24.0

22.0

20.0

18.0

16.0
Elastischer Anteil [dNm]

180°C
14.0 170°C
160°C
12.0 150°C
140°C
10.0

8.0

6.0

4.0

2.0

0.0
0.0 5.0 10.0 15.0 20.0 25.0 30.0
Zeit [min]

Copyright SCARABAEUS GMBH, Germany

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Enhanced Calculation MDR: Cure Kinetic

PEX B, crosslink of silane modified PE with water (H2O)

kj/mole
Ea 63.7751

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Enhanced Calculation MDR: Cure Kinetic

SCARABAEUS GMBH Teilenummer ISOTHERM

Reaktionskinetik Datum 18.12.2003
SIS V50
ln (ti) [min] ln Uk(n) [1/min]
2.50 Ea (ti) [kJ/mol] 93.16
1.50 Ea (Uk) [kJ/mol] 97.29
a (ti) [min] -25.04
a (Uk) [1/min] 27.04
b (ti) 11.204
1.92
0.90 b (Uk) -11.702
R² (ti) 0.999
R² (Uk) 1.000
Anzahl Werte 5
1.34 Reaktionsordnung 1.00
0.30

0.76
-0.30

0.18 -0.90

-0.40 -1.50
2.180 2.205 2.230 2.255 2.280 2.305 2.330 2.355 2.380 2.405 2.430
1/T *1000 [K]

Copyright SCARABAEUS GMBH, Germany

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Cure simulation based on kinetics. verification

SCARABAEUS GMBH Prüfdatum 12.12.2003 Prüftemperatur 180 °C

Postfach 200 163 Amplitude 0.50° Frequenz 1.67Hz
SCARABAEUS
D-35399 Langgöns Datum 18.12.2003
Heizzeitrechnung
20.0 Temperaturprogramm
192.00
Temperatur [°C] Reaktions umsatz [%]
18.0 200.0 176.00 100

16.0 190.0 160.00 90

180.0
144.00
14.0 80
170.0
128.00
Elastischer Anteil [dNm]

Ist-Temperatur [°C]

12.0 70
160.0
112.00

10.0 150.0
96.00 60

140.0 Soll-Temperatur
8.0 80.00 berechnete Umsatz
50
gemessene Umsatz
130.0
64.00
6.0
40
120.0
48.00
4.0 110.0 30
32.00

2.0 100.0
16.00 20
90.0
0.0 0.00
0.0 6.0 12.0 18.0 24.0 30.0 10
80.0
Zeit [min]
70.0 0
0.0 10.0 20.0 30.0
Copyright SCARABAEUS GMBH, Germany Zeit [min]

Copyright SCARABAEUS GMBH, Germany

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Cure simulation based on kinetic parameters

Edge

Rubber slab: 10 mm thick Mid-point

10 mm Center
155° C cure temperature
Compound initial temperature: 30° C
Arbitrary heat conductivity values
Cure
simulation

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Cure simulation – Cure time optimization

Rubber slab: 10 mm thick

155° C cure temperature
Compound initial temperature: 30° C

Taking into account both heating

and cooling, cure time can safely be
reduced from 8 min. to 5 min., 35%
reduction

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MDR - Application on sponge rubber

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Use of kinetic analysis on different MDR curves

Conversion rate constant on pressure curve

Boyle Law:  ∙    ∙  ∙
Pressure is linearly proportional to n so P can be used to calculate
conversion rate constant of gas formation in the compound.
Detection of dual decomposition reaction in silica compound based on
filler level TAINSTRUMENTS.COM

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Activation energy of blowing agent decomposition

Insulation foam Car door seal

NBR-PVC blend with Cellogen AZ EPDM compound with Cellogen OT

TA Instruments TAINSTRUMENTS.COM

Confidential

Results – Different sample weight, same shape

Accurate cure and blowing agent decomposition testing prerequisite:

• Identical material quantity
• Identical shape with minimizing material flow in the test chamber.

Increasing compound sample size

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Effect different sample shape, same weight

Different sample high and different Diameter

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Results – Same sample weight, same shape

Optimum repeatability and accuracy can only be archieved on cure and

pressure with sample weight ±0.01 g and sample diameter ±1 mm

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RPA summary and conclusion

• Since its commercialization, the RPA has found a growing importance in rubber testing.
• At first, at big rubber manufacturers such as tire companies
• But these were the most reluctant to share useful information on how to use this novel
instrument.
• The level of complex physical properties of rubber compound and even pure polymers
have hindered wide and fast distribution
• Available literature may present some of RPA useful technique in showing how things
are different but often failed to explain why.
• In this presentation I tried to present some of critical RPA tests in connection to material
fundamental properties.
• These properties include processing related characteristics such as viscosity, green-
strength (sagging resistance), surface aspect, mixing etc.
• We have also seen precise relationship between RPA measurements and polymer
characteristics (AMW, MWD, LCB etc.) affecting compound processing.
• The RPA effective testing power remains essentially within it high and flexible
programmability thus offering a unique testing versatility.
• So the RPA is capable to replace a large amount of conventional techniques.
• It can as well considerably deepen rubber behavior understanding.

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Thank You

The World Leader in Thermal Analysis,

Rheology, and Microcalorimetry

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