(TA, 2008) AR-G2, AR 2000ex and AR 1500ex Rheometers - Operator's Manual

AR-G2
AR 2000ex AR 1500ex
Rheometers
Operator's Manual
RevisionK
IssuedJune2008
2000-2008 by TA Instruments
109 Lukens Drive
New Castle, DE 19720
Notice
The material contained in this manual, and in the online help for the software used to support this instrument,
is believed adequate for the intended use of the instrument. If the instrument or procedures are used for purposes
other than those specified herein, confirmation of their suitability must be obtained from TA Instruments.
Otherwise, TA Instruments does not guarantee any results and assumes no obligation or liability. TA Instruments
also reserves the right to revise this document and to make changes without notice.
TA Instruments may have patents, patent applications, trademarks, copyrights, or other intellectual property
covering subject matter in this document. Except as expressly provided in written license agreement from TA
Instruments, the furnishing of this document does not give you any license to these patents, trademarks,
copyrights, or other intellectual property.
TA Instruments Operating Software, as well as Module, Data Analysis, and Utility Software and their associated
manuals and online help, are proprietary and copyrighted by TA Instruments. Purchasers are granted a license
to use these software programs on the module and controller with which they were purchased. These programs
may not be duplicated by the purchaser without the prior written consent of TA Instruments. Each licensed
program shall remain the exclusive property of TA Instruments, and no rights or licenses are granted to the
purchaser other than as specified above.
2
AR-G2/AR 2000ex Operators Manual
Important: TA Instruments Manual Supplement
Please click on the links below to access important information supplemental to this
Getting Started Guide:
TA Instruments Trademarks
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Other Trademarks
TA Instruments End-User License Agreement
TA Instruments Offices
3
Table of Contents
Important: TA Instruments Manual Supplement. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
Table of Contents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
Notes, Cautions, and Warnings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
Safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
Instrument Symbols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
Chapter 1: Introducing the AR-G2,AR 2000ex, and AR1500ex . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
Warnings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
Attention . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
Safety and EMC Conformity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
Safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
EMC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
La sret et EMC Conformit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
Spcifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
Sret . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
EMC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
Lifting and Carrying Instructions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
Electrical Safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
Liquid Nitrogen Safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
Handling Liquid Nitrogen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24

If a Person is Burned by Liquid Nitrogen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
Chemical Safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
Usage Instructions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
Maintenance and Repair . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
Chapter 2: Description of the Instruments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
A Brief History of Rheology and the Development of CMT Rheometers . . . . . . . . . . . . . . . . . . . . . 27
The AR-G2, AR 2000ex and AR 1500ex . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29

Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
Components of the Measuring System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
Chapter 3: Unpacking, Installation, and Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
Removing the Packaging and Preparing for Installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
4
Installation Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
Connecting the System Together . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33

Connecting the Rheometer to the Electronics Control Box . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33
Connecting the Computer to the Electronics Control Box Using Serial Communications . . . . . . 33
Connecting the Computer to the Electronics Control Box Using Ethernet Communications . . . . 34
Connecting Air and Water to the Rheometer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
Start-Up and Shut-Down Procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35

Starting Up the Rheometer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
Shutting Down the Rheometer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
Chapter 4: Key Rheometer Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
Casting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
Ball Slide . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
Magnetically-Levitated Bearing (AR-G2) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38
Air Bearing (AR 2000ex/AR 1500ex) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
Radial Air Bearings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40

Rotational Mapping . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40
Motor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
Optical Encoder . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
Normal Force Transducer (AR-G2 and AR 2000ex Only) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
Front Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43
Smart Swap . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
Auto GapSet Mechanism . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44

Zeroing of the Gap . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
Closing the Gap . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
Thermal Compensation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
Chapter 5: Smart Swap Temperature Systems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
Temperature Systems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
Using the Smart Swap . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46

Installing the Lower Stage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46
Removing the Lower Stage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47
5
Chapter 6: The Peltier Plate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
Introducing the Peltier Plate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
Chapter 7: The Upper Heated Plate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51
Introduction to the Upper Heated Plate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51
Attaching the Upper Heated Plate to the Rheometer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52

Installing the (Optional) Vortex Air Cooler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54
Configurations for the Cooling Water . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56
Connecting the Cooling Control Unit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
Using Circulating Fluids Other Than Water . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58
Connecting and Disconnecting the Geometry Holder . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60
Connecting the Geometry and Holder . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60
Removing the Geometry and Holder . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60
Configuring the Upper Heated Plate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61
Calibration of the Upper Heated Plate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62
Clamping the Bearing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65
Using an Inert Gas Atmosphere . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 66
Using the Sample Cover . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 67
Using the UHP for Asphalt Testing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 67
Chapter 8: The Peltier Concentric Cylinders . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69
Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69
Setting Up the Concentric Cylinder System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69
Attaching the Bob and Finding the Zero Position . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 70
Changing the Cup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 70
Solid Sample Submersion Clamps . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 71
Chapter 9: The Pressure Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73
Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73
Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 74
Operating Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 74
Safety Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 74
Operational Limits . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 74
Pressure Cell Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 75

The Pressure Cell Cup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 76
The Inlet Port . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 76
The Pressure Gauge Port . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 76
Safety Relief Port . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 77
6
Rotor Assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 77
Magnet Assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 78
Pressure Manifold . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 79
Requirements for External Pressure Source . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80
Installing and Using the Pressure Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 81

Step 1: Install High-Pressure Piping Manifold . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 82
Step 2: Install and Configure Pressure Cell Cup and Rotor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 83
Step 3: Positioning Gap and Pressure Cell Calibrations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85
Step 4: Loading a Sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 86
Step 5: Align Manifold and Make Manifold Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 88
Step 6: Pressurizing/Depressurizing the Cell and Running Experiments . . . . . . . . . . . . . . . . . . . . 89
Running Experiments in Self-Pressurization Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 90
Running Experiments in External Pressurization Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 92
Maintaining the Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94

Cleaning the Pressure Cell Cup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94
Cleaning the Rotor Assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94
Disassembling the Rotor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 95
Reassembling the Rotor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 96
Replacement Parts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 98
Chapter 10: The Starch Pasting Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 99
Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 99
System Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 100

Starch Pasting Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 100
Temperature Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 101
Connecting the CCU . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 102

Setting the Cooling Water Parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 103
Assembling the Starch Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 104
Calibration of the Measuring Sytem Factor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 105

Operating Parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 105
Performing the Calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 105
Sample Type . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 105
Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 105
Conical Rotor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 107
Chapter 11: The Interfacial Accessory and Du Noy Ring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 109
Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 109
Interfacial Rheology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 109
Setting up the Geometry Details . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 110
Bicone Interfacial Accessory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 112

Dimensions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 112
Experimental Procedure and Data Treatment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 113
7
Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 114
Setting up the Interfacial Bicone Accessory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 114
Zeroing the Gap . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 114
Mapping and Other Calibrations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 114
Determining Each Fluid's Contribution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 115
Finding the Interface Position . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 115
Analyzing Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 117

Calculation of the Interfacial Contribution to the Torque . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 117
Calculation of the Interfacial Linear Viscoelastic Properties . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 118
The Du Noy Ring (AR-G2 Only) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 119

Du Noy Ring Dimensions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 119
Setting Up the Du Noy Ring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 120
Zeroing the Gap . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 120
Mounting the Ring on the AR-G2 Spindle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 120
Mapping . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 121
Loading the Sample & Locating the Interface . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 121
Calculation of Interfacial Linear Viscoelastic Properties . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 122
Cleaning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 122
Cleaning the Ring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 122
Cleaning the Sample Dish . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 122
Chapter 12: The Environmental Test Chamber . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 123
Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 123
ETC Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 123
Using the ETC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 125

Installing the Low Temperature Accessory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 128
Operating Hints . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 130
Controlling Cooling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 130
Low Temperature System Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 130
Chapter 13: The ETC Viewer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 131
Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 131
Installing the ETC Viewer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 131
Schematics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 134
Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 136
Rheology Advantage Instrument Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 136
Image Controls . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 137
Storing Images . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 138
Data Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 138
Image Playback . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 140
Chapter 14: The Electrically Heated Plates (EHP) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 141
Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 141
8
Components of the Electrically Heated Plates . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 141
Installing the Electrically Heated Plates . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 143

Mounting and Connecting the Manifold . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 143
Mounting and Connecting the Upper and Lower Fixtures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 145
Attaching the Geometry Holder . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 147
Removing the Geometry Holder . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 147
Attaching and Removing the Purge Gas Cover . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 148
Running Experiments Using the Purge Gas Cover . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 149
Removing the Purge Gas Cover . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 149
The View Cover . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 149
Setting the Gas Flow Rates . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 150
EHP Temperature Calibration Factors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 151

AR-G2 with Standard Plates . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 151
AR-G2 with Disposable Plates/AR2000/AR2000ex/AR 1500ex . . . . . . . . . . . . . . . . . . . . . . . . . . . . 151
Chapter 15: Asphalt Submersion Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 153
Chapter 16: Curing Accessory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 155
Chapter 17: Small Angle Light Scattering Accessory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 157
Chapter 18: The Measuring Systems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 159
Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 159
General Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 159

Measuring System Factors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 159
Geometry Materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 160

Stainless Steel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 160
Hard Anodized Aluminium . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 160
Titanium . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 160
Acrylic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 160
Cone and Plate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 161

Temperature Systems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 161
Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 161
Filling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 162
Parallel Plate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 163

Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 163
Filling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 163
Concentric Cylinders . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 165

Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 165
Filling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 165
9
Double Gap Concentric Cylinders . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 166
Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 166
Filling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 166
Solid Sample (Rectangular) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 167

Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 167
Loading . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 167
Working Equations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 167
Choosing the Best Measuring System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 169

Cone and Plate and Parallel Plate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 169
Angles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 170
Diameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 170
Curing Systems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 170
Concentric Cylinders . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 170
Solid Sample Rectangular . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 171
Attaching a Geometry . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 172
Chapter 19: Extensional Fixture . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 173
Chapter 20: AR-G2 Smart Swap Geometries . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 175
Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 175
Using the Smart Swap Geometries . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 176

Reprogramming the Serial Number . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 178
Using the Geometry Wizard . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 179
Chapter 21 : Sources of Error . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 181
Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 181
Using Fluid Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 181

Loading . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 181
Gap Closure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 181
Sample Filling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 181
Cone and Plate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 181
Parallel Plate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 182
Reducing Evaporation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 182
Preventing Slippage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 183
Parallel Plate Measuring System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 183
Concentric Cylinder Measuring System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 183
Particulate Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 183
Temperature Compensation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 183
Normal Force Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 183
Using Solids and Rubbery Materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 184
10
Appendix A: Technical Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 185
Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 185
AR-G2/AR 2000ex/AR 1500ex Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 185
Power On Messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 191

Initialising ... . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 191
Bearing overspeed . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 191
Appendix B: Error & LCD Display Messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 191

Bearing pressure too low . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 192
Encoder index not found . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 192
Nf gauge fault . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 192
Nf temp sensor fault . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 192
Operator stop event . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 192
Power cable fault . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 192
Signal cable fault . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 192
Temp sys element fault . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 192
Temp system environment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 192
Temp system sensor fault . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 193
Other Messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 193
Appendix C: Symbols and Units . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 195

Cone and Plate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 197
Appendix D: Measuring System Factors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 197

Parallel Plate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 198
Concentric Cylinders . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 198
Standard Size Double-Gap Concentric Cylinders . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 199
Interfacial Measuring Systems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 199
Solid Sample (Rectangular): Exact . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 200
Solid Sample (Rectangular): Approximation 1 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 200
Solid Sample (Rectangular): Approximation 2 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 201
*Conversion of System Factors From S.I. to c.g.s. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 201
Appendix E: Materials List . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 203
Materials Used in TA Instruments AR Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 203

Peltier Plate Materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 203
Geometries . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 203
Plate 2 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 03
Concentric Cylinder Materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 203
Interfacial Accessory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 204
Pressure Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 204
Starch Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 204
Environmental Testing Chamber (ETC) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 204
Shield . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 204
Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 205
11
Notes, Cautions, and Warnings
The following conventions are used throughout this guide to point out items of importance to you as you read
through the instructions.
A NOTE highlights important information about equipment or procedures.
A CAUTION emphasizes a procedure that may damage equipment or cause loss of data
if not followed correctly.
A WARNING indicates a procedure that may be hazardous to the operator or to the

environment if not followed correctly.
12
Safety
Instrument Symbols
The following labels are displayed on the AR-G2/AR 2000 ex/AR 1500ex instrument for your protection:
Symbol Explanation
= Mains switch OFF
= Mains switch ON
The exclamation point within the triangle is a warning sign alerting you of
important instructions accompanying the product.
This symbol indicates that a hot surface may be present. Take care not to touch
these areas or allow any material that may melt or burn to come in contact with
these hot surfaces.
This symbol indicates that you are advised to consult the rheometer operating
manual (this manual) for instructions.
Please heed the warning labels and take the necessary precautions when dealing with those parts of the
instrument. This manual contains cautions and warnings that must be followed for your own safety.
13
14
Chapter 1
Introducing the AR-G2,AR 2000ex, and AR1500ex
Overview
The TA Instruments AR-G2/AR 2000ex/AR 1500ex Rheometers are controlled stress/controlled strain/controlled
rate rheometers capable of handling many different types of samples, using a range of geometry sizes and types.
This manual relates to all hardware aspects of the AR-G2/AR 2000ex/AR 1500ex Rheometers. For complete
information on the operation of the instrument, you may also have to refer to the software manuals supplied
with the instrument.
This chapter describes some important safety information. Please read this information thoroughly before
proceeding.
Warnings
Please make sure that you read the following warnings BEFORE using this equipment. This section contains
information that is vital to the safe operation of the AR-G2/AR 2000ex/AR 1500ex.
WARNING: This equipment must not be mounted on a flammable surface if low flashpoint
material is being analyzed.
WARNING: An extraction system may be required if the heating of materials could lead
to liberation of hazardous gasses.
WARNING: It is recommended that this instrument be serviced by trained and skilled

TA Instruments personnel at least once a year.
WARNING: The material used on the top surface of the Peltier plate is hard, chrome-
plated copper and the material used for the 'skirt' of the Peltier is stainless steel.
Therefore, use an appropriate cleaning material when cleaning the Peltier plate.
WARNING: The internal components of the ETC are all constructed from chemically
resistant materials, and can therefore be cleaned with standard laboratory solvents. The
only exception is the cladding for the thermocouples, which should not be immersed in
a solvent for long periods. Use a small amount of solvent on a soft cloth and wipe the
soiled area gently. This procedure should never be conducted at any temperature other
than ambient.
15
AR-G2/AR 2000ex/AR 1500ex Operators Manual
WARNING: During the installation or reinstallation of the instrument, ensure that the
external connecting cables (i.e., data, RS232 etc.) are placed separate from the mains
power cables. Also, ensure that the external connecting cables and the mains power
cables are placed away from any hot external parts of the instrument.
Note: Ensure that the mains power cable is selected such that it is suitable for the
instrument that is being installed or reinstalled, paying particular attention to the current
rating of both the cable and the instrument.
WARNING: Before switching the instrument on, apply the air to the instrument and
switch on the water supply to the Peltier system (if used).
WARNING: During operation, extreme hot or cold surfaces may be exposed. Take
adequate precautions. Wear safety gloves before removing hot or cold geometries.
WARNING: Liquid nitrogen can cause rapid suffocation without warning. Store and use
in an area with adequate ventilation. Do not vent liquid nitrogen in confined spaces. Do
not enter confined spaces where nitrogen gas may be present unless the area is well
ventilated. The warning above applies to the use of liquid nitrogen. Oxygen depletion
sensors are sometimes utilized where liquid nitrogen is in use.
WARNING: The various surfaces and pipes of the ETC and the supply Dewar can get
cold during use. These cold surfaces cause condensation and, in some cases, frost to
build up. This condensation may drip to the floor. Provisions to keep the floor dry should
be made. If any moisture does drip to the floor, be sure to clean it up promptly to prevent
a slipping hazard.
WARNING: Always unplug the instrument before performing any maintenance.
WARNING: No user serviceable parts are contained in the rheometer. Maintenance and
repair must be performed by TA Instruments or other qualified service personnel only.
WARNING: This instrument must be connected to an earthed (grounded) power supply.

If this instrument is used with an extension lead, the earth (ground) continuity must be
maintained.
16
WARNING: Take adequate precautions prior to heating of materials if it can lead to
explosion, implosion or the release of toxic or flammable gases.
WARNING: The impeller is constructed from a rigid polymer composite material of

density about 1.6 g cm-3. It is intended to be operated only with the impeller blades fully
immersed in the cup provided. The usual operating angular speed is 160 revolutions per
minute, rpm, (16.76 radians per second). Under these conditions the unit is unlikely to
provide a significant hazard to the user, and only the normal precautions observed when
operating the rheometer need be taken.
The instrument software does permit operation of the rheometer at its maximum angular
speed, without immersion of the impeller.
Take reasonable precautions to avoid contact with the impeller when it is rotating at high
angular speed. Ensure that clothing, jewelry, etc. does not become entangled in the
impeller.
ATTENTION: Le rotor est construit partir d'un matriau en polymre composite rigide,
de densit proche de 1.6 g.cm-3. Il est impratif que le rotor soit pleinement immerg
l'intrieur de son cylindre. La vitesse angulaire habituelle d'utilisation est de 160 tours
par minute, tr/m, (16,76 radians par seconde). Dans ces conditions, il est improbable que
l'utilisateur puisse faire encourir un risque sa cellule. Seules les prcautions d'usage
lies la bonne marche du rheometer doivent tre respectes.
Le logiciel de pilotage permet au rhomtre de tourner sa vitesse angulaire maximale

sans immersion du rotor.
Il est en outre recommand l'utilisateur de prendre toutes les prcautions ncessaires

pour ne pas rentrer en contact avec le rotor tournant haute vitesse et de s'assurer
qu'aucun vtement, bijou ou autre ne vienne son contact.
17
Attention
Cet instrument ne doit tre en aucun cas install sur une surface inflammable lors de
l'analyse d'chantillons ayant un faible point d'clair.
Une bouche d'extraction est ncessaire lors de la combustion de matriaux librant des
gaz toxiques.
Il est recommend que cet appareil soit rvis au moins une fois par an par un ingnieur
TA Instruments.
La surface suprieure en cuivre de la plaque Peltier est recouverte de chrome. Et la

surface latrale est recouverte d'acier. Il est important d'utiliser des produits adquats,
lors du nettoyage du Peltier, qui n'altrerons pas ces deux matriaux.
Les composants internes du four (ETC) mont sur l'AR2000 sont conus pour rsister
toute attaque chimique. Ils peuvent donc tre tous nettoys, l'aide de solvants
quelconques, l'exception du revtement des thermocouples, qui ne doivent pas, quant
eux, baigner dans un solvant pendant une longue priode. Ceux-ci doivent tre nettoys
a temprature ambiante en frottant lgrement avec un chiffon imbib de solvant.
Les cables externes doivent tre toujours separs du cable d'alimentation. S'en assurer
chaque installation. De mme, tout cable doit tre loign de toute source de chaleur
(Peltier).
Avant toute mise en marche, s'assurer que l'arrive d'eau pour le Peltier (si utilis) ainsi
que l'arrive d'air pour le moteur sont connectes et que l'eau et l'air circulent.
Les diffrentes surfaces, tuyaux de lETC ainsi que le reservoir dazote liquide peuvent
tre exposs de trs basses tempratures pendant l utilisation. Ces surfaces froides
provoquent de la condensation et peuvent mme tre lorigine dune formation de
glace. Cette condensation risque de goutter par terre. Afin dviter tout accident d un
sol glissant, il serait prfrable de garder le sol aussi sec que possible.
Lors de toute maintenance, couper l'alimentation.
Toute maintenance ou rparation doivent tre effectues par TA Instruments ou un

personnel de service qualifi.
18
Cet appareil doit tre connect la terre. Toute rallonge utilise avec cet appareil doit
comporter une masse de securit.
Utiliser l'azote liquide avec prcautions car une utilisation inadquate peut provoquer
des suffocations. Stocker et utiliser dans une pice suffisament ventile. Ne pas pntrer
dans une pice remplie d'azote avant d'en avoir evacu le gaz.
19
Safety and EMC Conformity
Specifications
In order to comply with the European Council Directives, 73/23/EEC (LVD) and 89/336/EEC (EMC Directive),
as amended by 93/68/EEC; the AR-G2/AR 2000ex/AR 1500ex has been tested to the following specifications:
Safety
This equipment has been designed to comply with the following standards on safety:
IEC & EN 61010-1: 2001
IEC & EN 61010-2-010: 2003
UL 61010-1 issued: 2004/07/12 Ed: 2
CAN/CSA C22.2 No. 61010-1 issued: 2004/07/12 Ed: 2
CAN/CSA C22.2 No. 61010-2-010-04
EMC
EN61326: 1997 +A1: 1998 + A2: 2001 incorporating:
EN55011: 1991 Conducted Emissions Group 1 Class 1

EN55011: 1991 Radiated Emissions Group 1 Class 1
EN61000-3-2: 2000 Harmonics
EN61000-3-3: 1995 + A1: 2001 Voltage Flicker
EN61000-4-2: 1995 Electrostatic Discharge
EN61000-4-3: 1996 Radiated Immunity
EN61000-4-4: 1995 Fast Burst Transients
EN61000-4-5: 1995 Surge Immunity
EN61000-4-6: 1996 Conducted RF Immunity
EN61000-4-11: 1994 Voltage Dips
20
La sret et EMC Conformit
Spcifications
Afin de se conformer aux directives du Conseil europen, 73/23/EEC (LVD) et 89/336/EEC (directive d'cEmc),
comme modifi par 93/68/EEC; l'AR-G2/AR 2000ex/AR 1500ex a t test selon les caractristiques suivantes:
Sret
Ce matriel a t conu pour tre conforme aux normes de scurit suivantes:
IEC & EN 61010-1: 2001
IEC & EN 61010-2-010: 2003
UL 61010-1 issued: 2004/07/12 Ed: 2
CAN/CSA C22.2 No. 61010-1 issued: 2004/07/12 Ed: 2
CAN/CSA C22.2 No. 61010-2-010-04
EMC
EN61326: 1997 +A1: 1998 + A2: 2001 incorporating:
EN55011: 1991 Conducted Emissions Group 1 Class 1

EN55011: 1991 Radiated Emissions Group 1 Class 1
EN61000-3-2: 2000 Harmonics
EN61000-3-3: 1995 + A1: 2001 Voltage Flicker
EN61000-4-2: 1995 Electrostatic Discharge
EN61000-4-3: 1996 Radiated Immunity
EN61000-4-4: 1995 Fast Burst Transients
EN61000-4-5: 1995 Surge Immunity
EN61000-4-6: 1996 Conducted RF Immunity
EN61000-4-11: 1994 Voltage Dips
21
Lifting and Carrying Instructions
Please follow these recommendations when you move or lift the instrument and its accessories:
Before moving the rheometer, you should remove any temperature attachments from the Smart Swap
holder. See Chapter 5 for more information.
When moving the rheometer, the air-bearing clamp should always be in place, ensuring that the bearing
cannot be moved. See Chapter 6 for information on the air-bearing clamp and how it is attached.
Use two hands to lift the instrument, keeping your back straight as you lift, to avoid possible strain on your
back. You should always use two people to lift the instrument.
Treat the AR-G2/AR 2000ex/AR 1500ex with the same degree of care you would take with any scientific
laboratory instrument.
Electrical Safety
Always unplug the instrument before performing any maintenance.
Supply Voltage 110 - 230 Vac

Fuse type 2 x T15A H250V
Mains Frequency 50 to 60 Hz
Power 1.4 kW
WARNING: Because of the high voltages in this instrument, maintenance and repair of
internal parts must be performed by TA Instruments or other qualified service personnel
only.
Cet instrument etant sous hautes tensions, l'entretien et la rparation des pices internes
doivent tre effectues exclusivement par TA instruments ou tout autre personnel de
service qualifi.
22
Liquid Nitrogen Safety
Potential Asphyxiant
WARNING: Liquid nitrogen can cause rapid suffocation without warning. Store and use
in an area with adequate ventilation. Do not vent liquid nitrogen in confined spaces. Do
not enter confined spaces where nitrogen gas may be present unless the area is well
ventilated. The warning above applies to the use of liquid nitrogen. Oxygen depletion
sensors are sometimes utilized where liquid nitrogen is in use.
Potentiel Agent asphxyiant

L'azote liquide peut causer des suffocations rapides. Stocker et utiliser dans une zone
dote d'une ventilation adquate. Ne pas ventiler d'azote liquide dans des espaces
confins. Ne pas pntrer dans des espaces confins o le gaz d'azote peut tre prsent
moins de bien arer la zone. L'avertissement ci-dessus s'applique l'utilisation de
l'azote liquide. Des capteurs d'puisement d'oxygne sont parfois utiliss.
Extremes of temperature
During operation, extreme hot or cold surfaces may be exposed. Take adequate precau-
tions. Wear safety gloves before removing hot or cold geometries.
Tempratures extremes.
Lors du fonctionnement, des surfaces extrmement chaudes ou froides peuvent tre
exposes. Prendre toutes prcautions necessaires telles que l'utilisation de gants de
protection avant d'enlever les gomtries chaudes ou froides.
23
Handling Liquid Nitrogen
The ETC uses the cryogenic (low-temperature) agent, liquid nitrogen, for cooling. Because of its low temperature
[-195C (-319F)], liquid nitrogen will burn the skin. When you work with liquid nitrogen, use the following
precautions:
Liquid nitrogen evaporates rapidly at room temperature. Be certain that areas where liquid nitrogen is used are
well ventilated to prevent displacement of oxygen in the air.
1. Wear goggles or a face shield, gloves large enough to be removed easily, and a rubber apron. For extra
protection, wear high-topped, sturdy shoes, and leave your trouser legs outside the tops.
2. Transfer the liquid slowly to prevent thermal shock to the equipment. Use containers that have satisfactory
low-temperature properties. Ensure that closed containers have vents to relieve pressure.
3. The purity of liquid nitrogen decreases as the nitrogen evaporates. If much of the liquid in a container has
evaporated, analyze the remaining liquid before using it for any purpose where high oxygen content could
be dangerous.
The oven inner doors have a trough around the bottom of the element assembly for collection of excess liquid
nitrogen. Any excess fluid collected will drain out from the oven at the lower outer edge.
If a Person is Burned by Liquid Nitrogen

1. IMMEDIATELY flood the area (skin or eyes) with large quantities
of cool water, then apply cold compresses.
2. If the skin is blistered or if there is a chance of eye infection, take

the person to a doctor IMMEDIATELY.
Chemical Safety
Do not use hydrogen or any other explosive gas with the ETC.
Use of chlorine gas will damage the instrument.
If you are using samples that may emit harmful gases, vent the gases by placing the instrument near an exhaust.
24
Usage Instructions
Before connecting the rheometer to auxiliary equipment, you must ensure that you have read the relevant
installation information. Safety of the rheometer may be impaired if the instrument:
Shows visible damage

Fails to perform the intended measurements
Has been badly stored
Has been flooded with water
Has been subjected to severe transport stresses.
Maintenance and Repair

CAUTION: Adjustment, replacement of parts, maintenance and repair should be carried
out by trained and skilled TA personnel only. The instrument should be disconnected
from the mains before removal of the cover.
Le rglage, le remplacement des pices, l'entretien et la rparation devraient tre

effectus exclusivement par le personnel qualifi de TA Instruments. Avant l'ouverture
du chssis, dbrancher l'instrument.
WARNING: The cover should only be removed by authorized personnel. Once the cover
has been removed, live parts are accessible. Both live and neutral supplies are fused
and therefore a failure of a single fuse could still leave some parts live. The instrument
contains capacitors that may remain charged even after being disconnected from the
supply.
Le chssis doit tre retir exclusivement par le personnel autoris. Une fois le chassis
retir, les pices connectes l'alimentation sont accessibles. L'instrument contient
plusieurs fusibles. L'instrument contient des condensateurs qui peuvent rester chargs
mme aprs avoir t dbranchs.
25
26
Chapter 2
Description of the Instruments
Overview
This chapter reviews the history of rheology, and traces the development of combined motor and transducer
(CMT) rheometers. The AR-G2, AR 2000ex, and AR 1500ex are introduced, and brief descriptions of their main
components and accessories are given. Please read this chapter carefully to familiarize yourself with the
terminology used throughout this manual.
A Brief History of Rheology and the Development of CMT

Rheometers
In 1929, Professor Eugene Bingham, a physical chemist working at Lafayette College in Pennsylvania, decided
that the study of the deformation and flow of matter was important enough to merit its own title. On the advice
of a Professor of Classics, he coined the term "rheology", from the Greek (rheo) meaning flow. But the
discipline of rheology is much older than the word. The first formal scientific description of a rheological
phenomenon appeared in Isaac Newton's Principia Mathematica, published in 1687, where he suggested that
"the resistance which arises from the lack of slipperiness of the parts of [a] liquid, other things being equal, is
proportional to the velocity with which the parts of the liquid are separated from one another." Today we would
say that the shear stress is proportional to the shear rate, and we would call the constant of proportionality the
viscosity of the liquid. As we now know, Newton's postulate applies only to a limited class of low molecular weight
liquids, over finite ranges of shear rate or stress. Rheology is usually more concerned with materials whose
behavior is non-Newtonian, in that their viscosity is a function of shear rate or stress. Such materials include
polymers, paints, inks, creams, gels, shampoos, drilling fluids, adhesives, and many foodstuffs.
It seems that Newton conducted no experimental work on the viscosity of liquids, and it was not until the middle
of the nineteenth century that work in that area was led by Poiseuille. The operating principle of most of the
early viscometers, including Poiseuille's, was that the fluid was driven by pressure or gravity through a capillary
or other constriction, and the rate of flow measured. Devices of this design are still in use today, but, although
they may have the advantage of simplicity of construction and operation, they have the drawback that the sample
can only be subjected to a finite strain.
However, a great step forward was made in the 1880's when the rotational viscometer was introduced by Couette
and others. In this type of device, the sample is situated either in the annular gap between two concentric
cylinders, as in Couette's original design, or in the gap between two concentric, horizontally mounted, parallel
platens. One of the cylinders or platens (the stator) is fixed, the other (the rotor) is rotated, and provided that
the rotation can be permanently maintained, there is no limit to the strain that the sample can be subjected to.
In Couette's design, the outer cylinder was fixed, the inner was driven by a weight connected to it through a
series of pulleys. The angular velocity of the rotating cylinder was calculated from the time taken for the weight
to fall. This design is interesting for two reasons, one being that it was the stress that was controlled (through
the weight) rather than the strain or strain rate, the other being that actuator and detector were mounted on the
same axis. It happens that the first of these gave rise to the term used to describe the successors to this type of
viscometer: "controlled stress". They might alternatively have been described by the second as "combined motor
and transducer" (CMT). This term is now preferred, since modern rheometers can operate in both controlled
stress and controlled rate modes.
27
It was many years before an electrically driven version of Couette's CMT apparatus was developed. The next
major advance in rheological instrumentation was introduced by Weissenberg in the 1940's. Weissenberg's
intention was to investigate the viscoelasticity of polymer melts and solutions, but the viscometers that existed
at the time were not suitable for this study. This led to the next advance in instrumentation.
The study of elasticity parallels closely the study of viscosity. The first scientific reference to elasticity was made
by Robert Hooke, a correspondent and rival of Newton's, who published his famous anagram "CEIINOSSITTUU"
in 1676, revealed as "ut tensio sic uis" (as the extension, so the force) in 1679. Hooke's Law, as it came to be called,
was supported by experimental observation, but it was not until the work of Young in the early nineteenth
century that it was realized that the law could be applied to material properties, rather than simply to extensive
sample properties. In modern terminology, we would summarize Young's findings by saying that the strain is
proportional to the stress, and we would refer to the "constant of proportionality" as the "modulus of the material."
Later in the nineteenth century, the work of Maxwell, Voigt, Kelvin, Boltzmann and others showed that the
distinction between viscous liquids and elastic solids was not as clear as had previously been thought. Most of
the materials listed above as non-Newtonian, are also viscoelastic, in that they exhibit aspects of both types of
behavior. (The names of the scientists who contributed to the development of rheology reveal its importance:
Einstein was also involved, and rheologists like to say that in their discipline Newton, Maxwell and Einstein
did the easy bits.)
To conduct his investigation into polymer viscoelasticity, Weissenberg developed the first modern, electrically
driven, rheometer during the early 1940s, the basis of which was a lathe turned on its end. As such it differed
in two very significant ways from the Couette viscometers, firstly in that it was what later became called a
controlled rate rheometer, and secondly in that the actuator and detector were mounted on separate axes. To
adopt the principle of naming used above, this can be called the "separate motor and transducer" (SMT) design.
The principle of operation was that one of the platens of the measuring system was rotated at a set angular
speed, the torque transmitted by the sample being measured at the other platen. Weissenberg called his
instrument a "Rheogoniometer", since both the torque and the axial force could be measured, the latter being
used to calculate the normal stress which results from the elasticity of the sample. In the late 1940s the
rheogoniometer was commercialized, but its price was beyond the range of most materials testing laboratories.
In 1970 Chris Macosko and Joe Starita formed the Rheometrics company (later renamed Rheometric Scientific)
to produce a lower cost alternative, and launched the first of a long line of high quality SMT rheometers that
led eventually to the modern ARES. Rheometric Scientific was acquired by TA Instruments in January 2003, and
its products continue to be manufactured and developed.
In the meantime, interest revived in CMT instruments, partly because of a desire to perform creep tests, and
partly because of the need to investigate the phenomenon of the yield stress in more detail, for which the available
SMT rheometers lacked the sensitivity. To these ends, Jack Deer, who was employed as a technician at the London
School of Pharmacy, designed a rotational rheometer based on the Couette viscometer, but with the weight
replaced, originally by an air-turbine drive, and later by a drag cup motor. To reduce the friction in the instrument,
an air bearing was introduced. Deer's first published description of the instrument appeared in 1968 [Davis,
Deer and Warburton, J. Sci. Instr. 2, 933-936, 1968]. He began to commercialize it shortly afterwards. In the early
1980's the design was taken up by the Carri-Med company, at Deer's instigation, and that company launched
its first rheometer, the CSR, in 1984.
Carri-Med acquired the rights to the Weissenberg rheogoniometer in 1990, but the mainstay of its business
remained the CMT successors to the Deer, which included the CSL and CSL2, until the company was purchased
by TA Instruments in 1994. From that time on, progress in CMT technology has been remarkable, with the AR
1000 launched in 1996 and the AR 2000 in the year 2000 by TA Instruments. Both these instruments used air
bearings, but the limits of that technology appear to have been reached, and for the AR-G2, launched in 2005, a
magnetically levitated bearing was used. This and other developments by TA Instruments have advanced the
instrumentation further. Developments, for example, in the drag cup motor and the electronics, have led to
substantial improvements in the low torque, controlled rate, and transient performances of the instrument. TA
Instruments' AR-G2 is now the world's most advanced CMT rheometer. Some of the improvements made in the
electronics and other components of the rheometer have also been incorporated into the AR 2000 to form the
AR 2000ex and AR 1500ex.
28
The AR-G2, AR 2000ex and AR 1500ex
The AR-G2, AR 2000ex, and AR 1500ex are the world's most advanced combined motor and transducer (CMT)
rheometers. The instruments consist of a main unit and a separate control box containing the electronics. The
interplay between the rheometer main unit and the electronics is described in Chapter 4.
A schematic of the AR-G2 rheometer is given in Figure 2.1. The AR 2000ex and AR 1500ex are similar.
Description
The body of the rheometer is a rigid, single metal Motor and
casting comprising a base and column. Head Bearing
The instrument head is attached to a ball-slide,

which is mounted within the column. The ver- Smart Swap
tical position of the head is controlled by driving Connection
Column
the screw of the ball-slide. The head contains the
following:
Coolant
The drag cup motor, with an armature that Connections
forms the rotating spindle of the rheometer.
An air or magnetic thrust bearing that Normal Force

supports the spindle. Transducer
Base
An optical encoder that determines its Front Panel

angular position.
Each of these components is described in more Figure 2.1

detail in Chapter 4. The AR-G2 Rheometer
(AR 2000ex and AR 1500ex are similar)
Components of the Measuring System

When using the instrument, the sample is positioned between a lower stage, mounted on the base of the casting,
and a removable upper stage or geometry, which attaches to the instrument's rotating spindle. The spindle is
hollow, with a detachable draw rod. The draw rod is threaded at the bottom end so that the geometry can be
securely attached.
Together, the lower stage and geometry form the measuring system, of which there are four main types, the cone
and plate, parallel plate, concentric cylinders and rectangular solid sample. Detailed descriptions of these, and
guidance on the correct choice of measuring system, are given in Chapter 16.
The lower stage is mounted on the rheometer by a Smart Swap magnetic connector, described in Chapter 5.
On the AR-G2, the Smart Swap geometry recognition system allows the instrument to automatically recognize
the geometry that is attached. See Chapter 16 for more information.
The lower stage forms part of the instrument temperature control system, and to compliment the outstanding
performance of the rheometers, TA Instruments has developed a range of these: Peltier Plate, Upper Heated
Plate (UHP), Peltier Concentric Cylinder system, Pressure Cell, Starch Cell, Interfacial Cell Environmental Test
Chamber (ETC) with integral ETC Viewer, and Electrically Heated Plate (EHP). These are described separately
in Chapters 6 to 14. Note: Not all temperature systems are available on every rheometer.
29
The lower stage on the AR-G2 and AR 2000ex mounts on a normal force transducer that detects the axial force.
This can be used for closed loop control of the head position to limit the stress imposed in the sample during
head closure, or to keep the sample under tension or compression during a measurement, or to determine the
normal stress produced by shearing the sample. The normal force transducer is described in Chapter 4. The AR
1500ex does not have a normal force transducer.
Connection of the lower stage to the normal force transducer is through a magnetic Smart Swap connector. This
enables very rapid exchange of temperature systems, and is described in Chapter 5.
TA Instruments hope that you enjoy using your rheometer, and are confident that you will be able to perform
better rheology than has ever been possible before now.
30
Chapter 3
Unpacking, Installation, and Operation
Overview
Normally the installation of your new system will be carried out by a member of the TA Instruments sales or
service staff, or their appointed agents, and it will be ready for you to use. However, should you need to install
or relocate the instrument, this chapter provides the necessary instructions.
Removing the Packaging

and Preparing for Installation
If needed, the first step is to carefully remove all items from any and all packaging. We recommend that you
retain all packaging materials in case the instrument has to be shipped back to TA Instruments at some point in
the future (for example, in the case of some upgrades).
Please follow these recommendations when you move or lift the instrument and its accessories:
Always remove the temperature control module from

the rheometer before attempting to move it. Details on
how to do this can be found later in this section (Smart
Swap).
When moving the rheometer, the bearing clamp

should always be in place, ensuring that the bearing
cannot be moved.
Bearing Clamp
Figure 3.1
Inserting the Draw Rod
1. Insert the draw rod into the top of the rheometer.
2. Push the bearing clamp up onto the draw rod. Hold it in place while
turning the knob at the top in a clockwise direction.
CAUTION: Always hold the clamp and turn the

knob never the other way round.
Toujours tenir la gomtrie et tourner la molette

jamais le contraire.
Treat the rheometer with the same degree of care you would take with
Figure 3.2 any scientific laboratory instrument.
Performing Step 2
31
Installation Requirements
It is important to select a location for the instrument using the following guidelines.
Choose a location that is...
In
An indoor area only (A clean environment).

Altitude up to 2000 m.
A temperature-controlled area (5C to 40C).
An area where the maximum relative humidity is 80% for temperatures up to 31C, decreasing linearly to
50% relative humidity at 40C.
An area where the mains lead is readily identifiable and easily reached by the operator. Use the mains lead
supplied with the instrument as the length of this cable is not more than 3 m.
An area with ample working and ventilation space around the instrument, approximately 2 meters in length,
with sufficient depth for a computer and its keyboard.
On
A stable, vibration-free work surface.
Near
A power outlet. (Mains supply voltage fluctuations not to exceed 10% of the nominal voltage, installation
category II.)
Your computer for direct connection of serial or ethernet cable or a network port.
Sources of compressed lab air and purge gas supply for use during cooling and sub-ambient experiments.
Air Bearing Gas Pressure (air or nitrogen) must be clean, dry, oil-free compressed air at 50100 psi. The dew
point should be -20C or better. Flow rate should be 25 L/min.
Away from
Dusty environment (pollution degree 2).

Exposure to direct sunlight.
Poorly ventilated areas.
After you have decided on the location for your instrument, refer to the following sections to unpack and install
the AR-G2/AR 2000ex/AR 1500ex Rheometer.
32
Connecting the System Together
Connecting the system together should present no problems, as long as you use instructions found in the
following sections.
Connecting the Rheometer

to the Electronics Control Box
The Electronics Control Box forms the link between the rheometer and the
computer. All the required processing is done within the control box. The
following steps should be followed to connect the two units together (refer
to Figure 3.3).
1. Push the female end of the power cable into the Power port on the back
of the rheometer and the other end in the Power port on the back of the
control box.
2. Push the D-type cable into the Signal port on the back of the rheometer
and connect the other end to the Signal port on the back of the control box.
The AR-G2/AR 2000ex/AR 1500ex rheometers are able to communicate with

the control computer via a serial or Ethernet link.
Connecting the Computer

to the Electronics Control Box Using Serial
Figure 3.3
Communications Cable Connections
The electronics control box and computer are connected via a single RS232 cable, which is supplied with the
system.
1. Push the 9-pin connector into the 9-pin socket marked 'Computer' on the back plate of the controller (Figure
3.3).
2. Push the 9-pin connector into the serial port socket on the back of the socket on the computer.
NOTE: You must configure the software for the appropriate communications portrefer to the
online help for instructions on how to do this.
Vous devez configurer le logiciel en fonction du port de transmissions utilisse rfrer l'aide
fournie dans le logiciel.
33
Connecting the Computer to the Electronics Control
Box Using Ethernet Communications
Ethernet communications can be setup in two ways. The electronics control box and computer can be connected
directly via a single Ethernet cable, or both can be connected using separate cables to a Local Area Network
[LAN]. Check with your TA Instruments representative for the appropriate cables needed.
Connecting Air and Water to the Rheometer

Refer to Figure 3.3 on the previous page for information on the location of the relevant connections in the
instructions below.
Cooling water is required for Peltier-based Smart Swap temperature systems. Connect a supply of cooling water
as follows, if Peltier temperature systems will be used.
1. Connect a supply of cooling water the flow and return connections at the rear of the rheometer
2. Connect the air supply (from the air regulator assembly) to the 'air in' connection. Set the regulator to 2 bar
(30 psi).
34
Start-Up and Shut-Down Procedures
Starting Up the Rheometer
Follow the steps below to start the rheometer:
NOTE: This assumes that the rheometer has already been correctly installed.
1. Check that the air supply is turned on
2. Remove bearing clamp if fitted.
3. Turn on fluid circulation, if required for correct operation of the installed temperature system.
4. Turn on power to the rheometer.
5. Connect to rheometer via the software.
Shutting Down the Rheometer

Follow the steps below to shut down the rheometer:
1. Turn off the power to the rheometer.
2. Turn off any fluid circulation.
3. Fit the air bearing clamp if it is likely that the bearing will be disturbed while the air is off. In the case of
the EHP, UHP, and ETC (doors closed), simply removing the draw rod should be sufficient to protect the
bearing unless the instrument is going to be moved.
NOTE: It is recommended that the air be left on and that the bearing remain unclamped.
4. Turn off the air supply.
It is possible for the motor/bearing assembly on an AR2000ex\AR1500ex to slowly drop under its own weight
when the power is off. This will not damage the rheometer, and will only result in the zero gap position being
lost. To maintain the zero reference in such cases, follow the alternative shut-down procedure below:
1. Remove any temperature systems from the Smart Swap connector.
2. Remove upper geometry if fitted.
3. Lower the bearing\motor assembly to the bottom of its travel.
4. Turn off power to the rheometer.
5. Fit the bearing clamp, if bearing is likely to be disturbed while the air is off.
6. Turn off the air supply.
35
36
Chapter 4
Key Rheometer Components
Overview
In this chapter, the main components of the rheometer are described. If you have a good understanding of the
design and function of each component, it will make efficient use of the rheometer easier. The chapter describes
in detail the design and functions of the:
Casting
Ball slide
Air thrust bearing (AR 2000ex/AR 1500ex)
Magnetically levitated thrust bearing (AR-G2)
Radial air bearings
Rotational mapping
Motor
Encoder
Normal force transducer (AR-G2/AR 2000ex)
Electronics
Front panel
Smart swap
Auto GapSet Mechanism
Casting
The body of the rheometer is a single-piece aluminium casting, consisting of a base and column. The casting is
an important component of the rheometer, as it needs to be rigid to axial and torsional stresses, robust, and
capable of being machined to high precision and accuracy to ensure correct alignment of the other components
of the instrument. Computer Numerical Control (CNC) machining is used to ensure concentricity, flatness and
parallelism in the measuring system when attached.
Ball Slide
The instrument head assembly containing the motor, bearing and optical encoder is mounted on a stiff, linear
motion, precision ball slide guide. The ball slide is mounted within the instrument column, and a motor and
optical encoder are located in the base of the casting to drive the ball slide screw, moving the instrument head
vertically, and to measure its position.
37
Magnetically-Levitated Bearing (AR-G2)
All CMT rheometers contain a bearing, and it is this component that largely controls the quality of data that can
be obtained on the instrument. The design of a bearing is a compromise involving several properties such as
friction, stiffness, air consumption and tolerance to contamination and misuse. To keep the friction low, non-
contact bearings have always been used in the better quality rheometers. A thrust disc is mounted horizontally
on the rotating spindle of the rheometer and, on traditional instruments, this disc is supported within a chamber
by air introduced from below at high pressure. To prevent the spindle moving upwards, air is also introduced
into the chamber from above, and to prevent it moving laterally, radial air-bearings are used.
On the AR-G2 rheometer, the thrust disc is retained, but it is levitated magnetically. The thrust disc is constructed
from a magnetically susceptible material. Electromagnetic actuators are positioned above and below the disc,
the strength of the magnetic field generated by each actuator is controlled through the current supplied to its
coils. The stronger the field, the greater the attraction between the actuator and the thrust disc. The axial position
and motion of the spindle are detected by sensors mounted above the upper actuator, and can be closely controlled
by varying the supplied current to each actuator coil.
This arrangement has advantages over the traditional air-bearing in many respects. The gap between the thrust
disc and the stationary components of the instrument can be much wider, of the order of millimeters rather than
micrometers. This results in both the friction of the bearing being substantially lower, and increases the
smoothness of rotation. The latter is particularly important, since it means that the variation in the bearing
characteristics with angular position, that are inevitable for any real bearing, can be more easily allowed for by
calibration ("mapping"). The axial stiffness of the bearing is increased, because of the tightness of the control
loop governing the axial position (to prevent lateral movement of the shaft, radial air-bearings are retained on
the AR-G2). The air consumption is reduced, and the wider gap and more durable materials used make the
bearing more robust and less susceptible to contamination.
38
Air Bearing (AR 2000ex/AR 1500ex)
As its name suggests, an air bearing uses air as the lubricating medium. This allows virtually friction-free
application of torque.
The design of an air bearing is a compro-

mise between several characteristics such Ultra Hi-Res Optical Encoder
as air consumption, friction, stiffness, and
tolerance to contamination and misuse.
Air Bearing (Radial)
The amount of air consumed is related to Air Bearing (Thrust)
the pressurized bearing clearance. To min-
imize air consumption, a small clearance
(<10 m) is needed. However, as air has a
Drag Cup
finite viscosity (0.0018 mPa.s), small gaps
give rise to high shear rates and, corre- Motor Windings
spondingly, the friction increases.
Air Bearing (Radial)
If large gaps are used, the shear rate is
lowered and friction is reduced, but the
stiffness of the air bearing is also reduced. Drive Shaft
Thus, a compromise in the design of an air

bearing is needed for optimal perfor- Figure 4.1
mance. AR 2000ex Rheometer Head
The air bearing uses a mixture of proven bearing techniques with novel materials. The surfaces can be easily
machined to tolerances of less than 1 m, providing an extremely smooth finish.
A schematic of the air bearing and the other main components of the rheometer head is shown in Figure 4.1 above.
The bearing is designed to be virtually friction- free, so that it moves under the smallest of forces. Even extremely
small manufacturing variations in the bearing can be sufficient to make it rotate. Therefore, to ensure that the
bearing rotation is steady throughout a full 360, a process called Rotational Mapping, which is explained in the
next section, is carried out.
39
Radial Air Bearings
Radial bearings provide stiffness and support in the radial direction. The AR-G2, AR 2000ex, and AR 1500ex are
designed with two porous carbon radial bearings, located above and below the motor.
Rotational Mapping
The characteristics of any real bearing will vary with angular position. By combining absolute angular position
data from the optical encoder with microprocessor control of the motor, these small variations can be mapped
automatically, and the results stored. Unless changes to the bearing characteristics occur, the variations are stable
over time.
The microprocessor can, therefore, allow for the variations by recovering the stored map and making the
appropriate baseline correction to the applied torque. This results in a very wide bearing operating range, without
operator intervention.
Instructions for performing the rotational mapping can be found in the Rheology Advantage online help. The
figures below show examples of the AR-G2 performance before and after mapping.
Figure 4.2
Rotational Mapping Examples
40
Motor
The requirement that the bearing used on the rheometer should be low in friction applies equally to the motor.
The AR rheometers use a non-contact "drag cup" motor. A thin-walled metal cup is mounted on the rotating
spindle of the rheometer. A magnetic field rotating at thousands of revolutions per minute is generated by
continuously varying the current supplied to stationary pole pieces surrounding the cup. This produces an
eddy current in the cup, which generates a second magnetic field. The two fields oppose each other, in accordance
with Lenz's law, and the cup field is forced to follow the rotating field. Hence, the cup is "dragged" round by
the rotating field, and a torque is generated whether the cup moves or not.
Drag cup motors have many desirable characteristics besides their low friction. Since they have no fixed magnets,
the torque produced is independent of the angular position. Futhermore, the torque is approximately propor-
tional to the square of the current, which means that a wide torque range is produced by a relatively narrow
current range. The rotating components of the motor can be very low in inertiathe limit is the thinness to
which the cup walls can be machined. Low inertia is important whenever the angular velocity of the moving
parts is changed, for example, during transient or dynamic experiments, or steady changes in torque.
The motor on the AR-G2 rheometer incorporates a patented drag cup temperature sensor. For the first time in
any rheometer design, the temperature of the drag cup is measured, ensuring the most accurate possible torque
output.
The low friction and inertia of the motor, together with sophisticated modern electronics allow close control of
the motor, both in its native, controlled torque, mode, and through feedback in controlled displacement or
angular velocity mode. Although designed according to the principles of traditional controlled-stress rheom-
eters, the AR rheometers are better regarded as both controlled-stress and controlled-strain rheometers.
Optical Encoder
The transducer used to determine the angular position of the rotating spindle should have high resolution, low
friction (i.e., non-contact), low inertia, and a rapid linear response. These criteria are met by the optical encoder
used on the AR rheometers. This consists of a non-contacting light source and photocell, arranged on either
side of a transparent disc mounted on the rheometer spindle. At the edge of this disc are extremely fine,
photographically etched radial lines, which form a diffraction grating. A stationary segment of a similar disc
is also mounted between the light source and the photocell, and the diffraction pattern formed by the light
transmitted through the gratings is detected by the photocell. As the spindle rotates, the diffraction pattern
changes. The associated electronic circuitry interpolates and digitizes the resulting signal, to produce digital
high resolution, angular position data.
The angular velocity of the rotating spindle is calculated from successive readings of the angular position, and
since this is done at electronic processor speed, the encoder effectively has two outputs, the angular position
and the angular velocity.
41
Normal Force Transducer (AR-G2 and AR 2000ex
Only)
Normal force is detected on the static lower measuring geometry assembly using high sensitivity load cell
technology. This results in a fast response, wide range signal, which is easy to calibrate, and has a genuine
normal force measurement capability.
Both the AR-G2 and AR 2000ex rheometers have the ability to control the amount of normal force during an
experiment, and make quantitative measurements of normal forces generated by a sample during a test.
CAUTION: During sample loading and measurement, the normal force transducer is
protected from overload. However, take care when cleaning or attaching accessories
to the lower plate that you do not exceed the maximum normal force.
Le capteur de force normale est protg contre toute surcharge. Cependant, prendre
soin de ne pas dpasser la force normale maximale lors de toute manipulation (nettoy-
age, changement de plaque).
When a viscoelastic liquid is sheared, a force can be generated along the axis of rotation of a cone or parallel
plate geometry. For this to happen, the structure responsible for the elasticity must not be completely disrupted
by steady shear.
For this reason, colloids, suspensions, etc., although elastic at rest, become effectively inelastic under steady
shear and can show negative normal forces due to inertial effects. However, polymer solutions and melts, and
products incorporating them, are typically elastic under shear because of the long lifetime of the molecular
entanglements.
Normal force measurements are made with cone and plate or parallel plate geometries; therefore, it is important
to use a method to detect the force that does not allow significant changes in the gap. This would result in the
actual shear rate varying with normal force, due to deflections of the force-detecting component.
42
Front Panel
Some of the operation of the rheometers can be controlled through buttons on the front panel, as shown in the
figure, as well as through the rheometer software
Head Up Head Down Zero Gap Release
On/Off Indicator Stop Start Bearing Lock
Figure 4.3
Front Panel
Explanation of the front panel from left to right:
On/Off Indicator (red): Lights up when power to the instrument is on.
Head Up: Used to raise the instrument head.
Head Down: Used to lower the instrument head.
Stop: Terminates whatever operation the instrument is performing, for example finding the gap zero,
mapping the bearing or running an experimental procedure.
Start: Used to start an experimental procedure. (AR-G2 only)
Bearing Lock: Applies a software lock to bearing to prevent the instruments shaft from rotating. This lock
will be over-ridden when the experimental procedure is started. (AR-G2 only)
Zero Gap: Starts the automatic gap zero position finder.
Release: Used as the SmartSwap release button. See Chapter 5 for more information.
SmartSwap indicator light (green).
43
Smart Swap
The AR rheometers feature "Smart Swap" technology that automatically senses the temperature control
system present and configures the rheometer operating software accordingly, loading all relevant calibration
data. The use of this feature is covered in this manual.
Also available for use with the AR-G2 only are the Smart Swap geometries, which are an extension of the
Smart Swap technology. These geometries can be automatically identifed when installed on the AR-G2
rheometer. The magnetic coating on the head of each geometry provides the read/write technology that will
uniquely identify it to the instrument.
Auto GapSet Mechanism

The auto gap set facility has three major functions, as follows:
Automatic setting of gaps via software

Programmed gap closure
Thermal gap compensation.
Zeroing of the Gap

It is important that you use a reproducible gap zeroing technique to reduce errors from such factors as operator-
to-operator techniques. The automation of gap zeroing on the rheometer minimizes these errors.
Closing the Gap

Once you have set the gap and loaded the sample, the head is lowered. The velocity and deceleration of the
head as it is lowered is controlled via the Automatic gap options set in the Rheology Advantage software.
There are four closure options availableStandard, Linear, Exponential, and Normal Force. The options
available are described in detail in the online help available in the rheology software.
CAUTION: Keep hands and fingers away from the plate during head movement.
S'assurer que les mains ou doigts ne soient pas entre le peltier et la gomtrie lors du
mouvement de la tte de l'instrument.
Thermal Compensation
When the temperature is varied during experiment, components of the rheometer will heat or cool, causing
a change in the measuring system gap. A typical expansion value for stainless steel is 0.5 m C-1. The auto-
gap set facility can be used to compensate for these changes. As the components expand or contract, the head
position will change so that the gap remains constant. In general, the default values provided for each geometry
are usually adequate, but for a more precise value, the measuring system can be calibrated using the Gap
temperature compensation Wizard under the Settings tab found under Geometry details.
44
Chapter 5
Smart Swap Temperature Systems
Overview
Each measuring system requires some form of temperature control. How this is provided will depend on the
type of measuring system and the temperature required. This chapter introduces those available and describes
the operation of Smart Swap system. Each temperature control system is described separately in the chapters
that follow.
Temperature Systems
The temperature systems available for each rheometer are:
Temperature System AR-G2 AR 2000ex AR 1500ex
Peltier Plate X X X
Upper Heated Plates (UHP) X X X
Peltier concentric Cylinders X X X
Starch Cell X X X
Interfacial Bi-cone System X X
Environmental Test Chamber (ETC) X X
Electrically Heated Plates (EHP) X X X
Asphalt Submersion Cell X X X
Each system has a fixed lower stage that is attaches to the rheometer body using the Smart Swap connection.
45
Using the Smart SwapTM
The following sections explain how to attach/detach temperature modules using Smart Swap. Note that the
installation and removal procedures are essentially the same for all modules.
The following modules can be used with the Smart Swap:
Peltier plate
Upper Heated Plate (UHP)
Peltier Concentric Cylinders
Starch Pasting Cell (SPC)
Interfacial Accessory
Environmental Test Chamber (ETC)
Electrically Heated Plates (EHP)
Asphalt Submersion Cell
Installing the Lower Stage

1. Press the Release button on the control panel as seen in
Figure 5.1. A continuous green light indicates that the
attachment can be fitted. Figure 5.1
Press the Release Button
NOTE: The release state will only stay
active for 10 seconds.
Le dvrouillage restera seulement actif
pendant 10 secondes.
2. Fit the attachment as shown in Figure 5.2 to the right,
ensuring it is aligned correctly. The alignment lug on
the lower stage should locate in the slot on the Smart
Swap base. On the Peltier Plate and Peltier Concentric
Cylinder systems, there is an additional alignment
mark, which should be align with the corresponding
Note the
mark on the instrument base.
alignment pin
Figure 5.2
Fitting the Attachment
3. Connect the power and, if necessary, the fluid cables. See Figure
5.3.
4. When the green status light goes out, the rheometer is ready for
use.
Figure 5.3
Connecting Power and Fluid Cables
46
Removing the Lower Stage
1. Press the 'Release button' on the control panel (see
Figure 5.4). A flashing green light indicates that the
attachment can be unplugged.
2. Press the Release button again. A continuous green

light indicates that you can remove the attachment.
3. Remove the attachment from the rheometer. See

Figure 5.5.
NOTE: The release state will stay active

for 10 seconds and then revert to locked.
Figure 5.4
Le dvrouillage restera actif pendant 10
Releasing the Attachment
secondes. A l'issue de ces 10 secondes
la plaque sera vrouille automatique-
ment.
Figure 5.5
Removing the Lower Stage
47
48
Chapter 6
The Peltier Plate
Overview
In this chapter the operating principles and use of the Peltier Plate temperature control system are described.
Introducing the Peltier Plate

The Peltier Plate (schematic shown in the figure below) is the standard temperature control system for the
rheometers. It uses the Peltier thermoelectric effect to control the temperature accurately, with rapid heating
and cooling. The plate consists of a copper disc, with hard chrome plating on the upper surface. A Pt100
temperature probe is embedded in the disc, in thermal contact with it and close to the surface. Copper is used
as the disc material for its very high thermal conductivity, ensuring negligible temperature gradients across the
surface of the plate. The hard chrome plating prevents mechanical or chemical damage to the plate.
The basis of the Peltier effect is this: When an electric current passes across the junction between two dissimilar
metals or semiconductors, a temperature gradient across the junction resultsthe temperature will rise on one
side and fall on the other. The direction of the current determines on which side the temperature rises.
On the AR rheometer plates, a set of Peltier elements is placed below and in thermal contact with the copper
disc. The desired level of active heating or cooling can be achieved by controlling the direction and magnitude
of the current supplied to these elements.
Hard Chrome Bath Pt100

Plate
Seal
Peltier Element
Blocks (x4)
Coolant Connections
Figure 6.1: Peltier Plate Top View Schematic

(With plate in place [left] and plate removed [right].)
Since a temperature gradient can only be maintained by the input of energy, the Peltier plate requires a heat
sink to remove any waste heat. This is provided by a coolant fluid, normally water, passing through a bath
situated below the Peltier elements. If the fluid circulating through the bath is from a closed reservoir, then its
temperature will rise unless it is actively cooled, particularly when the Peltier plate is operating at temperatures
far from ambient.
49
The Peltier plate works most efficiently when the temperature of the heat sink fluid is within 15C of that of the
plate. To work at temperatures in the range 20C below ambient to 60C above ambient, the fluid temperature
should be close to ambient. It may be raised for working at higher temperatures, and it might be necessary to
reduce it for working at lower temperatures. It is recommended that when the Peltier system is routinely used
at temperatures above 100C, the system is connected to a main water supply.
The flow rate of the fluid through the bath does not need to be high. A flow rate of at 0.5 liters per minute is
usually adequate, although this should be increased to 1 liter per minute when working at very low temperatures.
If this flow rate is not maintained, the Peltier will lose the ability to provide cooling.
Cooling fluids other than water may be used, and are essential to obtain temperatures below -20C.
Measuring systems available for use with the Peltier plate are the cone and plate and parallel plate. For detailed
information on geometry selection and the measuring system factors, see Chapter 16.
Table 6.1 Peltier Plate System Specifications
Temperature range
Tank and pump -5C to 100C
Pumped water supply -20C to 200C
Water at 60C 10C to 200C
Water at 40C 0C to 200C
Water at 1C -20C to 180C
Appropriate circulating fluid at -20C -40C to 160C
Typical ramp rate 30C min-1
Ramp rate (20C to 100C) 50C min-1

(100C to 150C) 25C min-1
Pt100 internal resolution 0.01C
CAUTION: The Peltier Plate may be damaged by operating the instrument without a flow
of water through the Peltier Plate. There is a Peltier overheat protection device that will
activate, if the device becomes too hot.
Sans coulement d'eau, le systme Peltier peut tre endommag. Un dispositif de

protection a t conu pour se dclencer en oas surchauffe.
50
Chapter 7
The Upper Heated Plate
Introduction to the Upper Heated Plate

At the Peltier plate's temperature range extremes, a vertical temperature gradient may be introduced across the
sample, the significance of which will depend on the samples thermomechanical properties. Although this
gradient can be reduced by the use of an upper geometry containing a thermal break, it can only be effectively
eliminated if the Peltier plate and upper geometry are constrained to the same temperature. The Upper Heated
Plate (or UHP) has been developed to allow this and is used in conjunction with the standard Smart Swap
Peltier plate.
On the AR-G2, the system can be configured. with the Upper Temperature Sensor (UTS) so that the temperature
of the upper platen is measured directly. The UTS consists of a special drawrod containing a Pt100 temperature
sensor. The information from this sensor is
transmitted to a remote reading device
The Upper Heated Plate consists of two

main components:
A fixture that attaches to the rheometer

head. This fixture contains electrical
heating elements and a coolant channel.
An upper geometry holder that attaches

to the rheometer rotating shaft. The
geometry holder contains a heat
spreader. Figure 7.1
Exploded View of the UHP and Upper Geometry Holder
There is no physical contact between the two
components (see Figure 7.1). Heating of the Upper Heated Plate is through the electrical elements. Cooling is
provided by vortex air, water, or other fluid carried in the coolant channel.
Control of the water flow is through a 3-way solenoid valve contained in a Cooling Control Unit (CCU) placed
upstream of the Upper Heated Plate. The CCU is also connected to an air supply, allowing purge air to displace
water from the coolant channel during heating or at elevated temperatures. If vortex air or fluids other than
water are used as coolants, purge air is not required, and the CCU is replaced by a 2-way solenoid.
A Pt100 probe placed within the Upper Heated Plate heat spreader reads the temperature of the Upper Heated
Plate. The offset between the read temperature and that of the upper geometry plate is obtained by prior
calibration.
An inert gas atmosphere can be produced using the inert gas inlet located between the inlet and outlet coolant
ports on the Upper Heated Plate. The inert gas jets are located on the underside of the heating element cover.
A protective sample cover and an instrument air bearing clamp are also provided.
51
Attaching the Upper Heated Plate to the Rheometer
FollowthestepsbelowtoattachtheUpperHeatedPlatetotherheometerhead.
1. Ensurethatairatthecorrectpressureissuppliedtotheairbearing,andremovethebearingcap.Turnon
therheometerandraisetheheadtothemaximum(usetheHeadUPbuttonlocatedontheinstrumentcontrol
panel).
2. AttachtheUpperHeatedPlatefixturetothemountingringontheundersideoftheinstrumenthead,using
thethreecaptivescrewsprovided.Notethatthepowercableshouldprojecttotherightoftheinstrument
whenviewedfromthefront,withtheportsforthecoolantandinertgastotheleft(seeFigure7.2).
Mounting Ring
Coolant Ports Power Cable
Heating Element Cover
Upper Geometry
Peltier Plate
Figure 7.2
The Upper Heated Plate Shown Mounted on a Rheometer
3. DisconnectthePeltierplatecable
fromtheSmartSwapsocket, Connector to
usingtheReleasebuttononthe Smart Swap
instrumentcontrolpanel. Socket
Peltier Connector UHP Connector

4. ConnectthePeltierplateand
UpperHeatedPlatecablestothe
leftandrightsocketsontheSmart
SwapUpperHeatedPlateadap Figure 7.3
torrespectively(seeFigure7.3to The Smart Swap UHP Adaptor
theright).Forpropersystem
indentification,itisimportantthatthisstepbecompletedbeforestep5.
52
5. Connect the Upper Heated Plate adap-
tor to the Smart Swap socket (see
Figure 7.4 to the right).
6. To return the temperature control to

Peltier plate only, remove the adaptor
from the Smart Swap socket using
the Release button on the instrument
control panel. Remove the Peltier con-
nector from the adaptor and plug the
connector directly into the Smart
Swap socket.
WARNING: Do not
remove the heating ele-
ment cover.
Figure 7.4
ATTENTION: Nenlevez Connection of the UHP Adaptor to the Smart Swap Socket
pas la couverture dl-
ment de chauffe.
53
Installing the (Optional) Vortex Air Cooler
Follow the steps below to attach and connect the vortex air cooler to the rheometer. Refer to the figures as
needed.
1. Use the two screws provided to mount the vortex air cooler bracket to the rear of the rheometer casting
as shown in Figure 7.5 to the right.
2. Clip the vortex air cooler into the spring clips with the brass
muffler extending upward as shown in Figure 7.6 below.
Exhaust
Vent Muffler
(STEP 6)
Vortex Tube
Mounting
Screws
White (STEP 1)
Tubing
(STEPS 7&8)
Air Inlet From Figure 7.5

Exhaust Air 2-Way Valve
Mounting the Bracket
From UHP
(STEP 5)
Cold Air
Oultet to
UHP
Black Insulated Tube

(STEP 4)
Swagelok
Figure 7.6 Adapter
Attaching the Vortex Air Cooler (STEP 3)
3. Remove the metal push-fit connector from

White Tubing
the inlet port on the UHP and fit the
(STEP 5)
Swagelok adapter supplied in the kit. See
Figure 7.7 to the right. (Note that once this
has been fitted, it cannot be removed. Insulated
Returning to the push-fit connector will Tube
require the supplied adapter.) (STEP 4)
Figure 7.7
UHP Swagelok Adapter
54
4. Connect the black insulated tube between the lower (vertical) outlet of the vortex air cooler and the Swagelok
fitting on the UHP inlet, and insulate the exposed metal connections.
5. Cut 800 mm of the white 6-mm O.D. tubing. Connect this tubing between the Upper Heated Plate outlet
and the lower bulkhead fitting on the vortex air cooler bracket.
6. Either use the short 6-mm fitting supplied or cut 150 mm of the white 6-mm O.D. tubing and connect to the
upper bulkhead fitting on the vortex air cooler bracket. The other end is left open to vent to the atmosphere.
7. Connect white 6-mm O.D. tubing between the outlet of the two-way valve from the CCU unit and the
middle (horizontal) inlet of the vortex air cooler.
8. Connect the opposite end of the white 6-mm O.D. tubing used in step 7 to a source of dry compressed air
(80 to 100 psi, 30C dew point or better). An 8-mm "Y"-piece and 8-mm to 6-mm reducer are supplied to
break into the rheometer air line before the filter regulator.
9. Connect the event socket on the valve bracket to the EVENT B socket on the rear of the rheometer using
the cable provided.
Table 7.1
Minimum Temperature Maximum Temperature
Vortex Air Cooler 5 C 150 C
NOTE: If you find a reduction in the expected cooling performance, check that there is exhaust
air flowing from the white 6-mm O.D. tubing. If there is limited or no air flow, this is an indication
that the cold end of the vortex tube is blocked with ice, formed by condensing moisture in the
air supply. The tube can be taken apart and ice removed, but the only long-term solution is to
supply drier air.
55
Configurations for the Cooling Water
The minimum temperature and the cooling rate attainable on the Upper Heated Plate will depend on the
temperature, flow rate and heat capacity of the circulating fluid. In general, provided that the flow rate is
adequate, the minimum temperature will be about 5C above that of the circulating fluid at the inlet, although
this will depend on the ambient conditions. The standard configuration is with water as the circulating fluid,
in which case mains water or a general laboratory circulator can be used.
It is recommended that separate sources should be used for the cooling water supplied to the Peltier plate and
the Upper Heated Plate, as the pulsing of the cooling water can influence the instrument normal force reading.
However, the same supply may be used for both units, provided that sufficient pressure is available to ensure
adequate flow through both (for example from an FP50-MS fluid circulator available from Julabo GmbH,
www.julabo.com; mains water supply is also normally suitable). Note that if a single supply is used, the Peltier
and Upper Heated Plate should always be connected in parallel, never in series. Some possible configurations
are shown below.
Important: For efficient operation, the Peltier plate and Upper Heated Plate should be
connected in parallel, NOT in series, if the same water supply is used for both.
Important: Pour une opration efficace, le plan de Peltier et lUpper Heated Plate devraient
tre relis en parallle, PAS en srie, si la mme source en eau est employ pour tous les deux.
Air Inlet
Drain
Mains Water Flow
Non-Return "Y"
Drain
Valve Piece
Figure 7.8
Cooling Water Configuration 1
Mains Water Supplying Both Peltier and Upper Heated Plate
Air Inlet
Reducer
Circulator Return
Water Flow
"Y"
"Y"
Piece
Piece
Figure 7.9
Fluid Circulator Supplying Both Peltier and Upper Heated Plate
56
Air Inlet
Drain
Mains Water Flow
Non-Return
Valve
Circulator
Return
Water Flow
Figure 7.10
Fluid Circulator Supplying Peltier, Mains Water Supplying Upper Heated Plate
Alternative configurations, not shown here, are for the Upper Heated Plate and Peltier to be supplied by separate
fluid circulators, and for the Upper Heated Plate to be supplied by a fluid circulator, the Peltier by mains water.
The non-return valve is not required for either of these configurations.
Connecting the Cooling Control Unit

This unit may be free standing, or wall mounted using the
clearance holes on top of the unit (see Figure 7.11 to the right
below).
1. Connect the air supply to the GAS IN port on the CCU

using the 8-mm outer diameter tubing (white). If it is
necessary to split the air line to provide a source for
both the instrument air bearing and the CCU, this
should be done upstream of the instrument filter regu-
lator system.
2. Connect the water supply to the LIQUID IN port on the

CCU using the 6-mm outer diameter tubing (blue). If
mains water is used as the supply, then the non-return
valve (see Figure 7.12 below) should be placed in the
line upstream of the CCU.
Figure 7.11
The Cooling Control Unit
Water IN
Water OUT Important: Note the direction of flow
through this valve.
Important: Notez la direction

Figure 7.12 dcoulement travers de la valve.
Non-Return Valve
(For use with mains water supply only.
Note the direction of flow through the valve.)
57
3. Connect the GAS / LIQ-
UID outlet port on the
CCU to the Coolant
Inlet port on the Upper
Heated Plate using the
4-mm outer diameter Coolant Inlet Port
tubing (blue) and the 4-
mm to 6-mm adaptor
provided.
Inert Gas Port
4. Connect the Coolant
Outlet port on the Coolant Outlet Port
Upper Heated Plate to
drain, if mains water is
the supply, or to return,
if a fluid circulator is
used. Use the 4-mm Figure 7.13
outer diameter tubing Coolant and Inert Gas Connections for the UHP
(blue) for this port. A 4-
mm to 6-mm adaptor and 6-mm "Y" piece are provided for the connection to the fluid circulator.
5. Connect the EVENT socket on the CCU to the EVENT B socket on the rear of the rheometer, using the cable
provided.
6. Set the purge air flow rate to 1 Liter per minute (L/min). Note that the reading is taken from the center of
the float. To set the flow rate, it may be necessary to raise the temperature of the Upper Heated Plate using
Rheology Advantage software, to ensure continuous air flow.
Using Circulating Fluids Other Than Water

For low temperatures, circulating fluids other than water must be used. These should be fluids of the silicone
type, as recommended by the supplier of the fluid circulator. A separate kit is available for use with these fluids.
WARNING: Flammable fluids such as ethanol or mineral oils should NOT be used with
the Upper Heated Plate. Circulating fluids should NOT be used outside the ranges given
by the supplier.
ATTENTION: Des fluides inflammables tels que lthanol ou les huiles minrales ne
devraient pas tre employs avec lUpper Heated Plate. Des fluides de circulation ne
devraient pas tre employs en dehors des gammes donnes par le fournisseur.
Silicone fluids are usually higher in viscosity than water, and the required flow rates cannot be achieved with
the standard CCU described above. The special low temperature kit should replace this. As when water is used
as the circulating fluid, it is suggested that separate sources should be used for the cooling fluid supplied to the
Peltier plate and the Upper Heated Plate. Then water may be used for the Peltier, and a silicone fluid for the
Upper Heated Plate, for example. However, the same supply may be used for both units, provided that sufficient
pressure is available to ensure adequate flow through both. Note that if a single supply is used, the Peltier and
Upper Heated Plate should always be connected in parallel, never in series.
58
1. Connect the flow port on the fluid circulator to the inlet of the 2-way CCU valve using the 6-mm outer
diameter (blue) tubing provided.
2. Connect the outlet from the valve to the Upper Heated Plate inlet, and the outlet from the Upper Heated
Plate to the circulator return port using the 6-mm outer diameter tubing (blue). Note that when silicone
fluids are used as coolants, the air purge on the Upper Heated Plate is not required.
3. Connect the EVENT socket on the CCU to the EVENT B socket on the rear of the rheometer, using the cable
provided.
Table 7.2 shows minimum and maximum temperatures for the Upper Heated Plate, using circulating fluids
available from Julabo GmbH, www.julabo.com, with an FP50-MS fluid circulator supplied by the same company.
Table 7.2
Circulating Fluid Minimum Temperature (C) Maximum Temperature (C)
Water 5 150
Thermal HY -30 55
Thermal H5S -20 105
Thermal H10S -10 150
59
Connecting and Disconnecting the Geometry Holder
WARNING: The Upper Heated Plate fixture, upper geometry holder, and the upper
geometry, may be hot. Ensure that these components are cool before attempting to
remove or replace the upper geometry holder.
ATTENTION: Le montage dUpper Heated Plate, le support suprieur de la gomtrie et

la gomtrie suprieure, peuvent tre chauds. Assurez-vous que ces composants sont
froid avant dessayer denlever ou remplacer le support de la gomtrie suprieure.
Connecting the Geometry and Holder

To connect the upper geometry and holder follow these steps:
1. Raise the instrument head fully, using either the Rheology

Advantage software or the Head UP button located on Heat Spreader
the instrument control panel.
2. Attach the geometry to the holder, using the attaching tool

25 mm Geometry
provided, if necessary. (This tool cannot be used with the
40-mm diameter geometry, which can attached to the
holder by hand.) If the Upper Temperature Sensor (UTS) Figure 7.14
is being used with the AR-G2, the geometry and upper Upper Geometry Holder
geometry are a single assembly. (Shows the cylindrical heat spreader with
a 25 mm diameter geometry in place.)
3. When the geometry is in place, carefully insert and posi-
tion the holder within the Upper Heated Plate, and connect to the instrument shaft by rotating the drawrod.
For Upper Heated Plate geometries, a backoff distance of 120,000 m is recommended.
4. Use 1.448 x 10-3 rad/Nm for the geometry compliance, unless other information is available.
Removing the Geometry and Holder

To remove the upper geometry and holder from the rheometer follow these steps:
1. Raise the instrument head fully, using either the Rheology Advantage software or the Head UP button
located on the instrument control panel. Grasp the holder firmly, and unscrew from the instrument shaft
by rotating the drawrod.
2. Lower the geometry holder carefully until it is clear of the Upper Heated Plate.
3. When the geometry holder is free of the instrument, the geometry can be removed from the holder using
the geometry attaching tool provided, if necessary. If the Upper Temperature Sensor (UTS) is being used
with the AR-G2, the geometry and upper geometry are a single assembly.
60
Configuring the Upper Heated Plate
The temperature of the upper Upper Heated
Plate is controlled through the instrument
firmware. For the best performance the con-
trol algorithm requires accurate information
concerning the thermal properties of the
Upper Heated Plate and the cooling fluid. In
the Rheology Advantage control module,
under the Options menu click Instrument
and then the Temperature tab. The window
box shown in the figure to the right will
appear.
A list of the features are described as follows:
Cooling Temperature: The temperature

of the circulating water, measured at the
inlet: should be entered manually. For
the vortex air cooler, use the value given
in Table 7.3
Cooling range: This is inversely

proportional to the flow rate. For the Figure 7.15
vortex air cooler, use the value in Table UHP Configuration Window
7.3. Typical values are given in the table
below.
Table 7.3
Feed Temperature Flow Rate Range
Mains Tap Water 15 C 0.75 Liter min-1 5 C

Fluid Circulator 5 C 0.25 Liter min-1 15 C
Vortex Air Cooler 15 C -- 100 C
For Configurations without UTS:
Thermal mass: The energy required to raise the temperature of the upper platen. It is suggested that the
value of 65 J/C, obtained by TA Instruments, be used unless other information is available.
Gradient calibration span: Arrived at by calibration (see below) although a manual entry may be made.
Gradient calibration offset: Arrived at by calibration (see below) although a manual entry may be made.
For Configurations with UTS:
Every UTS is uniquely calibrated with a traceable dry block temperature system during the manufacturing
process. These calibration values are stored within the component, and used automatically by the system
without operator involvement. The calibration described in the following section is not required when using a
UTS.
61
Calibration of the Upper Heated Plate
The temperature of the Upper Heated Plate is read from a probe positioned within the Upper Heated Plate heat
spreader as close to the upper geometry as possible, although not in physical contact with it. The temperature
of the Peltier plate is read from a probe positioned in thermal contact with the plate as close to the surface as
possible. The temperature reported by Rheology Advantage is that of the Peltier probe. For best performance
the Upper Heated Plate probe should be calibrated to the temperature of the upper geometry plate.
NOTE: Calibration should be performed on installation of the Upper Heated Plate, and at least
annually thereafter. The calibration routine may take several hours, and it is more efficient to
perform a single calibration with more points, rather than several calibrations with fewer points
NOTE: Le calibrage devrait tre effectu sur linstallation de lUpper Heated Plate, et au moins
annuellement ensuite. La routine de calibrage peut prendre plusieurs heures, et il est plus
efficace deffectuer un calibrage simple avec plus de points, plutt que plusieurs calibrages
avec peu de points.
During the automatic calibration routine a heat flow sensor is used to determine the temperature gradient
between the Peltier plate and the upper geometry. The gradient is reduced to within preset tolerances by
adjusting the temperature of the Upper Heated Plate while the temperature of the Peltier plate is held constant.
After each adjustment a user-defined stability criterion is applied and, once temperature stability is achieved,
comparison is made with the gradient tolerance. When the gradient tolerance condition is satisfied the
temperature value is accepted.
The procedure is repeated for a number of points over a range set by the user. When the calibration routine is
complete the temperature values for the upper geom-
etry determined by the calibration are compared with
those reported by the Upper Heated Plate probe to
obtain the appropriate offset and span values.
1. Under the Options menu click Instrument and

then the Temperature tab. The window, shown
in Figure 7.15 on the previous page, will be
displayed.
2. Ensure that the Cooling temperature and Cool-

ing range boxes contain the appropriate values.
3. Click Calibrate. The Calibrate Zero Heat Flow

window, shown in Figure 7.16 shown to the right,
will be displayed.
The parameters shown on the window are

described as follows:
Start Temperature: Temperature at which

calibration is to begin.
Figure 7.16
UHP Calibrate Zero Heat Flow Window
End Temperature: Temperature at which
calibration is to end.
Number of Points: Number of temperature points, which will be at equal intervals.
62
Initial Equilibration Time: Time at each set temperature, before readings are taken.
Adjust Equilibration Time: Time after each adjustment to the Upper Heated Plate temperature, before
readings are taken.
Average Time: Time after each adjustment, over which successive temperature readings are averaged
to provide a data point.
Average Stable Tolerance: Range within

which two successive data points must fall
for the temperature to be accepted as sta-
ble.
Gradient Zero Tolerance: Once stability

is achieved, the last data point is compared
with the set temperature. If the difference
is not more than the gradient zero toler-
ance, the set temperature is accepted as the
temperature value. If the difference is
greater than the gradient zero tolerance, a
further adjustment is made to the Upper
Heated Plate temperature.
Gradient Scale Factor: It is suggested that

the default value of 1.5 should be used
unless other information is available.
4. Click Next. A window similar to that shown in

Figure 7.17 is displayed. Follow the instruc- Figure 7.17
tions given. The Upper Heated Plate calibration Zero Value Determination Instructions
box and zero value plug are shown in Figure
7.18 below.
Figure 7.18
Upper Heated Plate Calibration Box (Left) and Zero Value Plug (Right)
63
5. When the zero value calibration has been completed
a window, similar to that shown in Figure 7.19, will
be displayed. Follow the instructions given. The zero
heat flow sensor is shown connected to the calibration
box in Figure 7.20 below.
Figure 7.20
Zero Heat Flow Sensor Connected to
Calibration Box (Note the T on the
Figure 7.19 upperside of the sensor.)
UHP Calibration Instructions
6. Use the instrument Head UP and Head DOWN buttons to position the heat flow sensor between the Peltier
plate and the geometry as shown in Figure 7.21.
7. Click Next to begin
calibrating as
instructed (see Fig-
ure 7.19, above
left). When the cal-
ibration is com-
plete the results
will be displayed as
shown in Figure
7.22 (to the left).
The graph shows

the temperature Figure 7.21
difference between Positioning the Heat Flow
the set temperature Sensor
and the tempera-
ture read by the Upper Heated Plate heat spreader
probe, plotted against set temperature. The Gradi-
ent calibration span is the slope of the best-fit
straight line through the data, and the Gradient
calibration offset is the intercept.
Figure 7.22
Results of UHP Calibration The average and peak errors are also reported. If the
average error is less than 0.1 C, and the peak error
less than 0.2 C, then the calibration should be considered acceptable. NOTE: Negative slopes are possible.
8. To accept the values click Next. The instrument firmware will automatically be updated with these values.
9. When the calibration is finished, raise the instrument head, and remove the calibration sensor. Remove
the connector from the electronics box.
64
NOTE: For safety reasons the temperature control is set to idle at the end of the calibration
routine, although the final temperature will still be displayed as the set temperature.
Clamping the Bearing

A bearing clamp is provided for use with the Upper Heated
Plate. Never attach or remove the clamp unless the air
supply is connected and switched on.
To attach the clamp
1. Remove the geometry holder from the instrument

shaft, and remove the geometry from the holder (see
Figure 7.23).
2. Replace the geometry holder
3. Push the clamp up onto the drawrod and attach it by

turning the drawrod counterclockwise (anticlock-
wise).
To remove the clamp hold it firmly and release it by turning Figure 7.23
the drawrod clockwise. Bearing Clamp
65
Using an Inert Gas Atmosphere
Many samples experience oxidation at elevated temperaturesan atmoshere of inert gas such as nitrogen or
argon can be used to prevent this. The gas supply should be regulated to less than 40 psi (2.8 bar) before
connection to the Upper Heated Plate. A gas flow meter (not supplied) should be used to set the gas flow rate.
1. Connect the gas supply to the inlet port on the gas flow meter.
2. Connect the outlet port on the flow meter to the inert gas inlet port on the Upper Heated Plate using 4-mm
outer diameter tubing (white) and the connector provided.
3. Set the inert gas flow rate at 1 Liter per minute (L/min). If the gas flow rate is set too high, temperature
control of the Upper Heated Plate may be affected.
66
Using the Sample Cover
Some samples are affected by drafts and general air flow, which can cause drying at the sample edge. To avoid
this, a protective sample cover is provided. The cover should be placed in the up position during sample loading
and trimming: the cover is held in this position by a bayonet fitting that attaches over the coolant connectors.
The cover should be used in the down position during the experimental run.
Figure 7.24
Sample Cover
Up Position (Left ) and Down Position (Right)
WARNING: The sample cover may be hot. Ensure that it is cool before attempting to
raise or remove it.
ATTENTION: Le couvercle chantillon peut tre chaud.

Assurez-vous quil est froid avant dessayer de lenlever.
Using the UHP for Asphalt Testing

The UHP, together with stepped Peltier plate, are the temperature systems used for the "Dry Asphalt System."
Information on running asphalt binder tests and performing additional system calibrations are covered in the
Asphalt Submersion Cell Manual.
Click here to open the manual for the Asphalt Submersion Cell.
67
Optional UHP/Peltier Manifold
TheUHP/Peltiermanifoldprovidesaneffective,tidy,solutionforthenetworkofinterconnectingtubingand
cableswhentheUHPistobeusedinthetemperaturerange5to90C.Usingwaterat2Casthecirculation
fluidmakesitanidealchoiceforcombiningwiththesteppedPeltierplateandUHPinthedryasphalt
configuration.
Fitting & Connecting the Optional UHP/Peltier Manifold

1. Attachthemanifoldtotherearoftherheometerusingthefourscrewsprovided.
2. Lookingattherearoftherheometer:
a. connectthefluidsupplyfromyourcirculatortothepushfittingsonthelefthandsideofthemanifold
usingtheclear6mmtubingprovided.
b. connectthetubesexitingthemanifoldonthetoprighthandsidetotheUHP.
c. connectthetubesexitingfromthemaincentralblocktothePeltierflowandreturnpushfittingsonthe
rheometer.
d. connecttheeventcabletoeventB.
NOTE: It maybe necessary to insulate long tubing runs with pipe wrap to achieve the minimum
temperature specification.
FluidSource MinimumTemperature MaximumTemperature
Polyscience612@2C 5C 90C
68
Chapter 8
The Peltier Concentric Cylinders
Overview
The operation of the Peltier Concentric Cylinder system is similar to that of the Peltier plate described in Chapter
6. The basis of the Peltier effect, and the conditions for efficient operation are described there.
The concentric cylinder system consists of a water jacket, an inner cylinder (or cup) and a rotor (or bob). As with
the Peltier plate, heating is through Peltier elements, and a circulating fluid is used as a heat sink.
The water jacket is fitted to the instrument through the Smart Swap connection described in Chapter 5.
Setting Up the
Concentric Cylinder
System
The concentric cylinder system consists of a water
jacket, an inner cylinder (the cup) and a rotor (or bob).
To set up the concentric cylinder system, follow these

steps:
1. Raise the rheometer head to the top most position.
2. Press the 'Release button' on the control panel as

seen in Figure 8.1. A continuous green light indi-
cates that the attachment can be fitted. Figure 8.1
Press the Release Button
NOTE: The release state

will only stay active for 10
seconds.
Le dvrouillage restera
actif pendant 10 secondes.
3. Fit the cylinder attachment, ensuring it

is aligned correctly. See Figure 8.2.
Figure 8.2
Fitting the Cylinder Attachment
69
4. Connect the power and fluid cables as shown in Figure 8.3 to the
right.
5. When the green status light goes out, the lower cup is correctly
installed.
6. Lift the rheometer head and attach the correct rotor (bob) to the
air bearing.
Attaching the Bob and Finding

the Zero Position
Finding the zero gap position for the rotor is slightly more difficult
than for the geometries used with the Peltier plate, as the gap between
the rotor and the bottom of the cup cannot be observed visually. It is Figure 8.3
a good idea to place the bob in the cup before attaching it to the draw Connecting Power and Fluid Cables
rod, to ascertain the approximate zero position. Look for the position
of the rotor shaft relative to the top of the cup. On most geometries, a
datum mark is machined on the shaft to help with finding the zero position.
Attach the rotor to the draw rod in the way described in Chapter 15.
To find the zero position, lower the instrument head until the datum
mark on the shaft of the rotor is level with the top of the cup as shown
in the figure, You can now set up the measuring geometry in the
rheometer software and set the gap as explained in the online Help
Changing the Cup

If you need to change the size of the cup you are using, follow these
steps:
1. Undo the two screws on the cup. Turn and lift it out as shown
in the figure below.
Figure 8.4
Lowering Rheometer Head
2. Replace with the required cup size and twist into

place. Tighten the two screws by hand.
Figure 8.5
Changing the Cup
70
The following rotors are available for use with the Peltier concentric cylinder system:
Standard Size DIN (conforms to DIN 53019)

Recessed End
Double Gap
Standard Vane
Wide Gap vane.
These are described in detail in Chapter 16.
Solid Sample Submersion Clamps

Some solid samples are required to be run while submerged in water. For this the Peltier concentric cylinder
system is used. The operation is similar to that of the solids samples used with the ETC. To facilitate sample
loading, Rheology Advantage includes a solid sample clamp Wizard.
Table 8.1 Peltier Concentric Cylinder System Specifications
Specification Value(s)
Temperature Range:
with tank and pump 0C to 100C
with plumbed water supply -10C to 150C
with fluid at -20C -40C to 100C
Ramp Rate:
Cooling 15C/min maximum
Heating 13C/min maximum
Pt100 Internal Resolution 0.01 C
CAUTION: The Peltier Plate may be damaged by operating the instrument without a flow
of water through the Peltier Plate. There is a Peltier overheat protection device that will
activate, if the device becomes too hot.
Sans coulement d'eau, le systme Peltier peut tre endommag. Un dispositif de

protection a t conu pour se dclencer en oas surchauffe.
71
72
Chapter 9
The Pressure Cell
Overview
WARNING: TA Instruments' Pressure Cell is designed for use at temperatures up to 150C
and pressures up to 138 bar (2000 psi). At all times during the use of the cell, wear safety
glasses and clothing that afford adequate protection against the sample under test, and
the temperature and pressure used. At other than ambient temperature, the outer
surfaces of the cell may become very hot or cold. When operating at these temperatures,
wear gloves that afford adequate protection against the surface temperature of the
pressure cell and its fittings.
The Pressure Cell is used with the standard concentric cylinder, Peltier-controlled, heating jacket on the AR-G2
and AR 2000ex. A copper sheath is fitted to the cell to ensure good heat transmission between the jacket and the
cell.
The Pressure Cell may be used either in self-pressuring mode, in which the pressure is produced by the volatility
of the sample, or in external pressurization mode, with an applied pressure of up to 138 bar (2000 psi). In this
chapter, the pressure cell assembly and operation for both modes are described.
NOTE: For external pressurization, the user of the cell is required to provide a high-pressure
source, and suitable pressure-rated connections to a 1/8-inch or 1/4-inch NPT female fitting.
AR-G2/AR 2000ex/AR 1500ex Operators Manual 73

Specifications
Operating Specifications
Thespecificationsforthestandardpressurecellconcentriccylindersare:
Statorinnerradius: 14.00mm
Rotorouterradius: 13.00mm
Cylinderimmersedheight: 44.00mm
Gap: 3500m(recommended)
Backoffdistance: 3500m
Geometryinertia: 67.00N.m.s2(approximate)
Samplevolume: 9.50.5ml
Temperaturerange: 10to150C
Maximumappliedpressure: 138bar(2000psi)
Maximumpressure(selfpressurizing): 5bar(72.5psi)
Torquerange about100N.mto0.2N.m
Maximumangularvelocity: 50rad/s
Sealconstruction: DuPontKalrez
Safety Specifications
Overpressurerupturedisk: 172bar(2500psi)
Hydraulicallytestedto: 414bar(6000psi)
Operational Limits
CAUTION: To prevent sample entering the upper part of the cell and contaminating the
bearings, the cell should not be used above the limits given below. Exceeding these limits
may also cause mechanical damage to the cell.
MaximumAngularVelocity: 50rad/s
MaximumSampleViscosity: Thegeometryshouldnotbeforcedintothesample.Lighthandpressure
shouldbeallthatisrequired.
MaximumFrequency: 50Hz(314rad/s)
NOTE: The quality of data obtained using the pressure cell cannot be expected to match that
obtained when conventional measuring systems are used with the rheometer. Some of the
normal calibration routines are not relevant to, or cannot be used with the Pressure Cell.
Alternative calibration routines are described in this chapter.

74 AR-G2/AR 2000ex/AR 1500ex Operators Manual
Pressure Cell Components
The Pressure Cell consists of four main Retaining Plate
component assemblies. These compo-
nents include the pressure cell cup, the Magnet
concentric cylinder rotor, the magnet Assembly Cover
assembly, and the pressure manifold. 4-Pole
Figure 9.1 shows a schematic cross sec- Magnet
tion of the pressure cell cup, rotor, and
magnet assemblies, and Figure 9.2
shows a fully configured Pressure Cell KalrezTM Seal Thumbscrew
installed on an AR Rheometer. The
following section will discuss these 4-Pole
four components individually. Sapphire
Magnet
Bearings
Rotor
Assembly Locking Nut
Kalrez Seal
Rotor
Gauge Port Inlet Port
Cup
Figure 9.1
Cross Section Schematic
Magnet
The Pressure Cell is shown assembled on the AR rheom-

Cup
eter, with the instrument head in the DOWN position, in
Peltier Figure 9.2 to the left.
Heating
Jacket
Manifold
Assembly
Figure 9.2
Pressure Cell on AR Rheometer

The Pressure Cell Cup
The Pressure Cell Cup contains
the sample fluid. It is inserted into
Rupture Disk
the Peltier jacket, which mounts Assembly in the Rotor
on the rheometer using the Smart SafetyRelief Assembly
SwapTM connection. A copper Port Cap
sheath ensures good heat trans-
mission between the jacket and the
cup. There are three ports on the
Snubber and
cup, which are identified by
Compression
engraved labels. Pressure Gauge
Fitting in the
in the Pressure
Inlet Port
NOTE: When Gauge Port
installing NPT fit-
tings use
Teflon thread
sealing tape. Figure 9.3
Pressure Cell Cup with Rotor Assembly
CAUTION: Do not attempt to attach or detach any fittings to or from the cell while it is
mounted on the rheometer. Doing so can cause damage to the instrument.
The Inlet Port

The Inlet Port, which is used in the external pressurization mode, is where the compressed gas is introduced
to the cup. A pressure manifold is supplied that attaches to the inlet port using a compression connector. A
pressure snubber is fitted between the port and the high-pressure line to slow the pressure build and prevent
sample from entering the line.
The Pressure Gauge Port

This port is fitted with a pressure gauge which indicates the pressure within the cell, and a relief valve. This
valve is only intended to be used when the pressure
from the cell cannot be relieved in the usual way (see
"Pressurizing and Depressurizing the Cell," found later
in this chapter). You will need a 5/8-inch open or box-
end wrench to hold the valve body and a 7/16-inch
wrench to open the valve.
Figure 9.4
Pressure Gauge Port
(Gauge and Valve Shown)

Safety Relief Port
The Safety Relief Port is equipped with a rupture disk assembly that is designed to relieve excessive cup pressure.
At excessive internal pressure, the rupture disk breaks and propels the internal atmosphere out of the cup.
WARNING: Do not operate the pressure cell without the safety relief fitting in place. Do
not remove the rupture disc from the safety valve fitting, as this may cause the pressure
cell to crack during an overpressure condition, resulting in damage and personal injury.
The rupture disc should only be replaced by a qualified TA Instruments Service Repre-
sentative.
CAUTION: You MUST install the Safety Relief Port with the Rupture Disk such that it is
pointed to rear of the AR-G2 and away from the operator. This will prevent sample material
from being ejected toward the operator in the event of an over-pressure situation.
Rotor Assembly
The rotor assembly contains the Concentric Cylinder rotor, which is mounted on a shaft that is radially supported
by two sapphire bearings located under the rotor assembly cap. Also attached to the shaft is a four-pole magnet.
The rotor assembly installs into the cup using a threaded mount, and seals with a Kalrez seal. A second Kalrez
seal is seated between the cap and the thumbscrew.
Thumbscrew
4-Pole
Magnet
Cap
Locking
Nut Kalrez
Seal
Rotor
Figure 9.5
Pressure Cell Rotor Assembly with Cap Off (Left) and On (Right)
CAUTION: Prior to use, ensure that the two Kalrez seals are installed and are in good
condition. Replace, if damaged, with seals provided by TA Instruments only.

Magnet Assembly
The magnet assembly attaches to the rheometer's rotating spindle,
and then lowers over the rotor assembly. The spindle collar of the
magnet assembly includes an insert adapter. The adapter insert
should remain in the collar for use with AR2000 or AR2000ex
rheometers. If using the pressure cell with an AR-G2 rheometer,
take the adapter insert out of the spindle collar by removing the Reference
two Phillips (or cross head) screws extending for the outer surface Mark
of the spindle collar. See the figure below. Like the rotor assembly,
the magnet assembly contains a 4-pole magnet. When the spindle
and magnet assembly are rotated, the attraction between the two
4-pole magnets produces a corresponding rotation of the rotor.
There is no physical contact between the two assemblies.
Figure 9.6
CAUTION: Do not place magnetic storage Magnet Assembly with
media near the magnet assembly, as it con- Cover
tains a powerful magnet capable of destroying
magnetically recorded material.
Adapter
Insert
(Used with
AR 2000/AR 2000ex.)
(Remove for AR-G2.)
Figure 9.7
Magnet Assembly with AR 2000/
AR 2000ex Adapter Insert

Pressure Manifold
The Pressure Cell includes a
high-pressure manifold
assembly that is connected to
the rheometer frame. The
rigid piping pressure mani-
Pressure Gauge
fold provides strain relief
between the pressure cell
and external high-pressure
connections. It also includes
necessary valves and gauges
for safely pressurizing and
depressurizing the cell. It is
a critical part of the pressure
cell assembly and the pres-
sure cell should not be oper-
ated without the manifold in
place. The pressure mani- Three-Way Valve
fold, shown in Figure 9.8 to
the right, includes the fol-
lowing:
Mounting Plate
Mounting plate and
Sorbothane block. The
Sorbathane block is a
flexible material that Sorbothane
Block
provides flex between
the rigid pressure cell
piping assembly and the
rheometer frame.
Figure 9.8
1/8-inch and 1/4- inch Pressure Manifold Assembly
female NPT fittings for
high-pressure connections.
Three way valve for pressurizing, maintaining cell pressure, and depressurizing the cell.
Pressure gauge for monitoring pressure in the cell.

Requirements for External Pressure Source
Fittings are provided for external pressurization up to 138 bar (2000 psi). A high-pressure source must be
supplied with 1/8-inch or 1/4-inch NPT male fittings for connection to the manifold supplied by TA
Instruments. In addition, a means of isolating the source from the manifold, and of relieving the pressure in
the line from the source to the manifold should be provided. Figure 9.9 below shows a typical set up for
external pressurization.
WARNING: Only use TA Instruments' high-pressure manifold when operating the

pressure cell. Ensure that the manifold can be isolated from the high-pressure source
provided by the user, and that there is a pressure vent valve in the line between the
source and the manifold.
Figure 9.9
Typical Setup for External Pressurization

Installing and Using the Pressure Cell
The AR Pressure Cell is shipped with the Rotor installed in the pressure cell cup, and the high-pressure piping
manifold fully assembled. Installing the AR Pressure Cell from it's initial shipped configuration requires some
disassembly. Disassembly instructions are as follows:
Step 1: Unpack the preassembled pressure cell cup and rotor. Using the spanner (Tommy bar) provided,
remove the rotor assembly from the pressure cell cup, and carefully place the rotor in a safe location. Remove
foam packing material from Cup.
NOTE: All the compression fittings that are used on the manifold assembly have a specific
tightening procedure for the first time the nut is tightened on the tubing during the manufacturing
process. Subsequent disassembly and remake of any fitting should be done by first putting a
reference mark on the nut and the body of the fitting before loosening the fitting. After
reassembly of the fitting to a finger tight condition, the nut should then be tightened with a
wrench so that the mark on the nut aligns with the mark on the body of the fitting. A second
wrench should be used to hold the body of the fitting in place while turning the nut.
Step 2: Unpack the preassembled piping manifold assembly. Using a wrench, remove the furthest extending
angled pipe from the Tee fitting joining the gas inlet and pressure gauge.
Figure 9.10 below shows the disassembled configuration.
The steps on the next several page provide the instructions needed to install and use the pressure cell.
Pressure Cell Cup

with Gauge Tommy Bar Manifold Assembly
Rotor Assembly Angled Pipe
Figure 9.10
Entire Pressure Cell Configuration Disassembled

Step 1: Install High-Pressure Piping Manifold
The pressure manifold attaches to the lower right
rear as viewed from front of rheometer or left lower
corner when facing rear of the AR rheometer, as
shown in Figure 9.11.
Attach the mounting plate and Sorbothane block to

the two M5 using the cap head screws provided, as
shown in Figure 9.12 below.
Attach
manifold
here
Manifold
Sorbothane Block
Cap Head Screws

Figure 9.11
Attach Manifold to Back of Rheometer
Manifold
Bracket
Figure 9.12
Manifold Installed

Step 2: Install and Configure Pressure Cell Cup and Rotor
Follow the instructions below to both install and configure the Pressure Cell Cup and Rotor:
1. Locate the Peltier Concentric Cylinder Jacket. Remove the Peltier Jacket, if it is installed on the AR Instrument.
2. Remove any Peltier Concentric Cyl- Safety Relief

Valve
inder cups and remove the two
knurled screws that fasten the stan- Angled
dard Peltier cups in place (Note the Pipe
standard knurled screws can not be
used with the Pressure Cell).
Peltier
3. Insert the Pressure Cell cup into the
Jacket
jacket, with the Safety Relief valve
facing to the rear of the cup. (Note
the "Hot" symbol and white Smart Hot Symbol
Swap alignment line are markings on
the front of the Peltier Jacket). Fix Smart Swap
the cup in position in the jacket using Alignment
Line
the two hex head screws and hex
keys provided with the Pressure Figure 9.13
Cell. See Figure 9.13 to the right. Pressure Cell Cup Installed in Peltier Jacket
4. Connect angled high-pressure pipe

to the cell inlet port, ensuring that the straight part of the pipe is vertical as shown in Figure 9.13. Tighten
the compression connector as directed in the NOTE on page 79.
5. Locate the rotor assembly. Place the small magnet onto the rotor
assembly, as shown in Figure 9.14, such that the small magnet is
vertically aligned with the scribe line etched on the collar on the rotor Small
assembly. Magnet
6. Hand-tighten the rotor assembly into the cup. Fully tighten the rotor
until flush with the cup using the wrench (also called a Tommy bar). Wrench
(Tommy
Bar) Hole
Small Scribe
Magnet Line
Figure 9.14
Rotor Assembly
with Small Magnet
7. Position the small magnet on the

rotor to face in the front center
of the Peltier Jacket as shown in
Figure 9.15 Figure 9.15 to the left.
Orientation of Small Magnet

8. Install Peltier Jacket on rheometer using Smart Swap Connectors.
9. Install the Magnet Assembly onto the shaft of the rheometer.
10. Rotate the draw rod so the magnet assembly refer-

ence mark is aligned with the small magnet on the
Rotor. Ensure that the reference mark on the upper
geometry remains aligned with the small magnet by
lightly holding the rheometer draw rod and begin
lowering the rheometer head as shown in Figure
9.16
11. At a gap of about 20 mm between the shoulder on Reference

the rotor assembly, and the underside of the upper Mark
magnet assembly, the magnets in the upper assem-
bly will engage with those in the rotor assembly as
shown in Figure 9.17. (A small noise will be heard
when this happens and a change of a few Newtons
will be seen in the normal force reading.). Immedi- Small
Magnet
ately stop moving the rotor assembly down and
remove the small magnet.
Figure 9.16
Aligning the Reference Mark
Figure 9.17
Magnets Engaging

Step 3: Positioning Gap and Pressure Cell Calibrations
Once the Pressure Cell cup and rotor have been installed, you will need to position the gap and perform the
calibrations as directed in this section.
CAUTION: The standard calibration routines used by Rheology Advantage for zero gap,
geometry inertia and bearing friction are not suitable for use with the pressure cell. When
the pressure cell is selected as the measuring geometry, these routines are either
disabled or are replaced by more appropriate routines. Do not attempt to use or calibrate
the pressure cell unless this geometry is selected.
1. Ensuring that the pressure cell geometry is selected in the software, find the gap zero position. Do not request
the instrument to raise the head to the backoff distance. Set a gap of 3500 m.
2. When the Pressure Cell is the selected geometry on an AR2000 or AR2000ex, the Gap Zero Mode of normal
force with a value of 5N will be used. This will override any other settings in Rheology Advantage software.
3. Conduct the Bearing Friction Calibration. The bearing friction routine used when the Pressure Cell is selected
as the geometry is slightly different from the standard routine. The calibration should be conducted at a
geometry gap of 3500 m. The bearing friction calibration must be done again when another measuring
system is used. A typical value for the Pressure Cell should be between 8 and 15 N.m / (rad/s). This is about
ten times higher than for other geometries.
4. Map the Air Bearing. Perform a rotational mapping at a gap of 3500 m using the Standard mapping routine.
NOTE: DO NOT USE PRECISION OR EXTENDED MAPPING ROUTINES WITH THE PRES-
SURE CELL.
CAUTION: It is important that the bearing is re-mapped before any other measuring
system is used.
NOTE: When changing to other geometries, Rheology Advantage does not restore the previous
settings. However, the mapping table is cleared and the bearing friction is reset to zero. Any
functions that were previously unavailable are reactivated and the gap zero mode settings are
restored, because the settings were not overwritten.
5. Check the Cell by running peak-hold test at 0.05 rad/s and a duration time of 126 sec. The peak-to-peak
residual torque should not be larger than 100 N.m.

Step 4: Loading a Sample
Samples are loaded in the pressure cell after the cell is set up and calibrated. The following steps will detail
the sample loading procedure.
1. Rotate the drawrod so the reference mark on the magnet assembly is facing the front of the instrument.
Raise the rheometer head high enough to place the small magnet on the rotor. Once the small magnet is
in place, raise the rheometer head to the maximum height.
NOTE: DO NOT REMOVE MAGNET ASSEMBLY FROM THE RHEOMETER HEAD. IF IT IS

REMOVED, THE MAPPING WILL NO LONGER BE AS EFFECTIVE, CAUSING AN
INCREASE IN RESIDUAL TORQUE.
2. Remove the Peltier jacket from rheometer.
3. Leaving the small magnet in place, gently remove the rotor from the cup.
4. Load the sample into the cup. For very viscous samples, you may find it easiest to weigh the sample in the
cup, if the sample density is known (this can be done after removing the cup from the jacket).
NOTE: Volume is 9.5 0.5 mL.
5. Ensure that the small magnet is still aligned with

the mark on the rotor assembly.
6. Replace the rotor assembly and fully tighten.
7. Replace the Peltier jacket onto the Smart Swap Base

of the rheometer.
8. Rotate the draw rod so the magnet assembly refer-

ence mark is aligned with the small magnet on the
Rotor. Ensure that the reference mark on the upper Reference
Mark
geometry remains aligned with the small magnet
by lightly holding the rheometer draw rod and
begin lowering the rheometer head as shown in
Figure 9.18.
Small
Magnet
Figure 9.18
Aligning the Reference Mark

9. At a gap of about 20 mm between the shoulder on the
rotor assembly and the underside of the upper magnet
assembly the magnets in the upper assembly will
engage with those in the rotor assembly as shown in
Figure 9.19. (A small noise will be heard when this
happens and a change of a few Newtons will be seen
in the normal force reading.). Immediately stop mov-
ing the rotor assembly down and remove the small
magnet.
10. Lower the instrument head to the geometry gap

(default 3500 m). Do not zero the gap.
Figure 9.19
Magnets Engaging

Step 5: Align Manifold and Make Manifold Connections
After the sample is loaded, you will need to align the manifold
as follows. The pressure manifold should only be connected
and disconnected from the cup assembly at the bottom of the
angled pipe connected to the cup as shown in Figure 9.20.
Please refer to the NOTE on page 79.
1. Prior to connecting the pressure manifold to the angled

pipe, slacken off to finger tight the compression connec-
tors on the manifold in order to easily align the manifold
with the pipe mounted on the cup. DO NOT USE EXCES-
SIVE FORCE TO POSITION THE PRESSURE MANI-
FOLD.
2. Finger-tighten ONLY the manifold to the angled pipe

mounted on the cup, using the connector indicated in
Figure 9.21.
Figure 9.20
Place to Connect/Disconnect Manifold
3. Once this fitting is finger tight, fully tighten all other

Finger compression fittings as directed in the NOTE on
Tighten page 79.
This
Connector
4. Finally, fully tighten the angled pipe to the manifold
as directed in the NOTE on page 79.
CAUTION: To avoid putting excessive

force on the pressure cell, make sure that
Figure 9.21 connection or disconnection between the
Connector Used to pressure cell and the manifold is made at
Connect/Disconnect Manifold
the breakage point compression connec-
tor only (see Figures 9.20 and 9.21. Con-
nection or disconnection should be made at no other point while the pressure cell is
mounted on the rheometer.
NOTE: To disconnect the pressure cell from the manifold, ensure that both the cell and the
manifold are depressurized. Then disconnect the compression connector indicated in Figures
9.20 and 9.21.
WARNING: Before disconnecting the pressure cell from the manifold, ensure that neither
the cell nor the manifold is pressurized, and that both are cool enough to touch.

Step 6: Pressurizing/Depressurizing the Cell and Running
Experiments
When the cell is fully installed, it can be operated in either self-pressurization mode, in which the pressure
is due to the volatility of the sample, or in external pressurization mode, in which the pressure is provided
by an external source. The pressure achieved when the cell is used in self-pressurizing mode will depend
on the sample and temperature. As a guide, the vapor pressure of water at 150C is about 4.76 bar (69 psi.).
When the cell has been assembled correctly as directed in this chapter, it can be pressurized. The manifold
contains a three-way valve. The three positions for the valve are shown in Figure 9.22.
Vertical UpPressure Vertical DownPressure HorizontalOff

Relief Build (external pressuriza-
tion mode) Isolation between the
Connection between the pressure cell and the con-
pressure cell and atmo- Connection between the nector block on the man-
sphere. pressure cell and the con- ifold.
nector block on the manifold.
Figure 9.22
Three-Way Valve Positions

Running Experiments in Self-Pressurization Mode
After the manifold is installed, all fittings have been tightened, and the sample has been loaded, follow these
steps to run an experiment in the self-pressurization mode.
1. Make sure the three-way valve on the manifold is set to the OFF position (horizontal).
NOTE: The secondary pressure relief valve on the Pressure Gauge Port should only be
opened if the primary pressure relief passage becomes clogged. If this valve was opened,
make sure it is closed.
2. Set the testing temperature from the software.
3. Program the test procedure.
4. Run the experiment.
5. After running the experiment, depressurize the cell by following these steps:
a. Ensure the the pressure cell is isolated from the high pressure source.
b. When the experiment is complete, the temperature should be set back to 25C (ambient temperature)
before attempting to relieve the pressure in the cell.
c. Once the cell has cooled, set the three-way valve on the manifold to the "Pressure Relief" position
(arrow pointing upward). Note that the pressure may reduce very slowly, due to the snubbers in the
manifold.
NOTE: There are two snubbers in the manifold, one of which is located on the cell itself and
the other in the vent line, as described earlier in this chapter. These are used to slow the
build and relief of pressure in or from the cell. The snubbers may become clogged with sample,
preventing the cell pressure from being properly relieved (this problem is more likely to occur
when external pressurization is being used). You must maintain the cleanliness of the
snubbers, ensuring that gas can pass through them. You can verify that they are operating
properly by pressurizing and depressurizing the cell without a sample. If there is any doubt
concerning the cleanliness or operation of the snubbers, they should be replaced.
NOTE: The pressure relief valve on the cells Pressure Gauge Port can also be used to relieve
the pressure in the cell. This should only be done if the three-way valve on the manifold
cannot be used, if, for example, the snubbers have become blocked. The cell should also be
at room temperature before using this valve, and appropriate gloves and safety glasses
should be worn.
The pressure gauge located on the Pressure Gauge Port and the pressure gauge on the manifold can be used
to help verify that the snubbers are not clogged. After relieving the pressure in the cell using the manifold
and three-way valve, the two gauges should read zero (0) pressure. If the snubbers are clogged, the pressure
gauge in the Pressure Gauge Port may still register pressure. If that condition occurs, use the relief valve on
the Pressure Gauge Port to release pressure from the cell.

CAUTION: Although the pressure gauge on the cell may to appear to register zero, the
level of pressure in the cell may still be above ambient.
Disconnect the pressure cell from the manifold at the designated disconnection point at bottom of the
angled pipe.
Raise the head and decouple the magnet assembly and the rotor, and remove the Peltier jacket from the
rheometer using the procedures outlined previously in "Step 4: Loading a Sample."
Remove the cup and rotor for cleaning. See "Maintaining the Cell" for details.

Running Experiments in External Pressurization
Mode
NOTE: If the maximum pressure of the external pressure source is greater than 138 bar (2,000
psi), (e.g. N2 tank), the source must be regulated to a maximum value of 138 bar (2000 psi).
After the manifold is installed, all fittings have been tightened, and the sample has been loaded, follow these
steps to run an experiment in the external pressurization mode.
1. Make sure the three-way valve on the manifold is set to the OFF position (horizontal).
NOTE: The secondary pressure relief valve on the Pressure Gauge Port should only be opened
if the primary pressure relief passage becomes clogged. If this valve was opened, make sure
it is closed.
WARNING: Before applying high pressure, check for leaks at low pressure. Raise the
pressure of the cell, gradually, making frequent leak checks.
2. Regulate the external pressure source to the pressure required for the experiment. THIS PRESSURE
CANNOT EXCEED 138 bar (2,000 psi).
3. Gently pressurize the cell by slowly opening the three-way valve on the manifold to the pressure build
position (arrow pointing vertically downwards). Check the pressure cell to make sure there are no leaks.
If it is free from leaks at low pressure, raise the pressure gradually, making frequent leak checks using a
liquid leak test material.
4. During operation, the pressure cell should be isolated from the high-pressure source. Set the three-way
valve on the manifold to OFF (arrow horizontal), and relieve the pressure in the line between the high-
pressure source and the connector block. If the cell is free from leaks, the pressure in the cell will be
maintained.
WARNING: During operation, isolate the pressure cell from the high-pressure source,
and relieve the pressure in the line between the source and the manifold.
5. Set the testing temperature from the software.
6. Program the test procedure.
7. Run the experiment.
8. After running the experiment, depressurize the cell by following these steps:
a. Ensure the the pressure cell is isolated from the high pressure source.
b. When the experiment is complete, the temperature should be set back to 25C (ambient temperature)
before attempting to relieve the pressure in the cell.

c. Once the cell has cooled, set the three-way valve on the manifold to the "Pressure Relief" position
(arrow pointing upward). Note that the pressure cell may reduce very slowly, due to the snubbers in
the manifold.
NOTE: There are two snubbers in the manifold, one of which is located on the cell itself and
the other in the vent line, as described earlier in this chapter. These are used to slow the
build and relief of pressure in or from the cell. The snubbers may become clogged with sample,
preventing the cell pressure from being properly relieved (this problem is more likely to occur
when external pressurization is being used). You must maintain the cleanliness of the
snubbers, ensuring that gas can pass through them. You can verify that they are operating
properly by pressurizing and depressurizing the cell without a sample. If there is any doubt
concerning the cleanliness or operation of the snubbers, they should be replaced.
NOTE: The pressure relief valve on the Pressure Gauge Port on the pressure cell can also
be used to relieve the pressure in the cell. This should only be done if the 3-way valve on the
manifold cannot be used, if, for example, the snubbers have become blocked. The cell should
also be at room temperature before using this valve, and appropriate gloves and safety
glasses should be worn.
The pressure gauge located on the Pressure Gauge Port and the pressure gauge on the manifold can be used
to help verify that the snubbers are not clogged. After relieving the pressure in the cell using the manifold
and three-way valve, the two gauges should read zero (0) pressure. If the snubbers are clogged, the pressure
gauge in the Pressure Gauge Port may still register pressure. If that condition occurs, use the relief valve on
the Pressure Gauge Port to release pressure from the cell.
CAUTION: Although the pressure gauge on the cell may to appear to register zero, the
level of pressure in the cell may still be above ambient.
Disconnect the pressure cell from the manifold at the designated disconnection point at bottom of the
angled pipe.
Raise the head and decouple the magnet assembly and the rotor, and remove the Peltier jacket from the
rheometer using the procedures outlined previously in "Step 4: Loading a Sample."
Remove the cup and rotor for cleaning. See "Maintaining the Cell" for details.

Maintaining the Cell
WARNING: Before removing the heating jacket from the rheometer or the cell from the
jacket, ensure that cell and manifold are not under pressure, and that the both are at
safe touching temperature. The pressure relief procedure is described above.
Cleaning the Pressure Cell Cup

The cup can be cleaned simply by washing it in solvent or other type of cleaner (water, etc.), depending on
the material being test, after removal from the heating jacket.
Cleaning the Rotor Assembly

CAUTION: When cleaning the rotor, observe the following precautions:
(1) Do not apply a sideways force to the rotor. Doing so can bend, break, or otherwise
damage it. If a bent rotor shaft is suspected (will not rotate freely), hold the rotor
assembly horizontally by the upper body (do not hold by the rotor), and spin the rotor
while observing the edge. No discernible wobble should be seen as the edge of the
rotor rotates.
(2) Do not allow sample or solvent to flow upward into the upper portion of the body
of the rotor assembly, as this may result in a change in the friction of the sapphire
bearings.
If sample fluid has flowed into the sapphire bearings and magnet of the rotor assembly, the rotor may become
"sticky" (not rotate freely). In this case, the rotor assembly must be dismantled and cleaned as follows:
1. Hold the rotor assembly by the upper portion only. Be careful not to bend the rotor shaftsee Caution #1
above.
2. Place the tips (bent at 90) of the supplied pliers into the holes of the locking nut and unscrew the nut by
rotating counterclockwise (anticlockwise).
3. Remove all inner components by gently pulling the rotor straight out of the assembly. Clean the inner
components using an appropriate solvent. Cellophane tape can be used to clean surfaces that have been
contaminated by solid particles, but be certain that no adhesive residue remains on the components.
4. If sample has flowed to the upper sapphire bearing, remove the thumbscrew and clean the inner
components using solvent.
5. Reassemble the pieces in the reverse order, being careful not to overtighten the locking nut (hand-tight is
sufficient).
NOTE: Typically, sapphire bearings are designed to work "dry." The Pressure Cell is therefore
supplied without lubricant. However, it has been found that a small amount of suitably
compatible grease applied to the bearings can reduce the risk of a "sticky" bearing following
contamination of the bearing by condensation or overflow of sample fluid.

Disassembling the Rotor
1. Insert the wrench (also called a Tommy bar)
provided into one of the six holes in the rotor
assembly cap and turn the rotor assembly Pliers
counterclockwise until the entire assembly
can be removed.
2. Place the rotor assembly upside down on a

flat surface (table or lab bench). Be careful not
to bend the rotor shaftsee Caution #1 on the
Locking
previous page.
Nut Holes
3. Place 90 pliers into the holes of the locking Locking

nut and unscrew the locking nut by rotating Nut
it counterclockwise (anticlockwise). See the
figure to the right. (You may find it easier to
holdthe locking nut steady with the pliers
and rotate the rotor cap clockwise.) Figure 9.23
Taking Apart the Rotor Cell Assembly
4. Remove the cap covering the magnet (see the
figure to the right for reference, if needed).
Scribe Line Scribe Line on Alignment Ring
5. Before disassembling the remaining parts, note the
scribe lines on the magnet and bob collar. This will allow
you to realign the magnet properly after cleaning. See
the figure to the right.
6. Continue to remove parts only if you have a torque

wrench to retighten the rotor setscrews again as directed
in step 13 on the next page.
Figure 9.24
7. Loosen the two setscrews on the rotor to remove the Marking Magnet to Line
rotor from the shaft. The locking nut and sapphire bear-
Up with Alignment Hole
ing holder can now be removed from the shaft. See the
figure below for reference.
Upper Sapphire Bearing
Thumbscrew Rotary Cap Magnet Shaft Sapphire Rotor

Locking Nut
Bearing Holder
Figure 9.25
Parts of the Rotary Assembly (In correct order of assembly)

8. Clean the inner components using an appropriate solvent (e.g., alcohol, acetone). Cellophane tape can be
used to clean magnet surfaces that have been contaminated by solid particles, but be certain that no adhesive
residue remains on the components.
9. If sample has flowed to the upper sapphire bearing, remove the thumbscrew and clean the inner
components using solvent. A pipe cleaner can be used to clean inside surfaces.
Reassembling the Rotor

Make sure all of the parts are dry after the cleaning process and follow the steps below to reassemble the pieces.
10. Slide the sapphire bearing holder onto the magnet shaft making sure the flat side is facing towards the
rotor (which will be on the bottom).
11. Slide the locking nut over the shaft with the plier holes facing toware the rotor.
12. Align the magnet's mark with the rotor alignment ring, insert the shaft into the rotor, and make sure the
shaft bottoms out in the rotor.
13. Tighten the two setscrews on the rotor, using a torque wrench to adjust the
setscrews to 8.5 lbf-in or .96 N-m.
14. Turn the rotary cap upside down and rest it on a flat surface (table or lab
bench).
15. Taking the parts already loosely assembled, insert the shaft into the rotary
cap until you feel it hit the bottom. You may need to move it around slightly
until it drops all the way through. The tip of the shaft should be visible at
the top of the rotor as seen in the figure to the right.
16. Using the 90pliers, screw down the lock-

ing nut by rotating it clockwise. See the
lower right-hand figure. (You may find it
easier to tighten the nut by rotating the
rotary cap counterclockwise and holding
the locking nut steady with the pliers.) Rotor
17. Watch the top surface of the locking nut as

it is tightened. Once the locking nut's top
surface is even with the cap, the shaft must
Locking Nut
be fully inserted in the sapphire bearing as
Top Surface
directed in step 15.
The rotor will rest on top of the 90 pliers Rotary

if the shaft is correctly located inside the Cap
sapphire bearing.
DO NOT CONTINUE TIGHTENING Figure 9.26

UNTIL THIS IS VERIFIED. THE BEAR- Reassembling the Rotary Assembly
INGS MAY BE DAMAGED IF THE
SHAFT IS NOT INSIDE BOTH BEAR-
INGS BEFORE TIGHTENING COMPLETELY.

18. Replace the thumbscrew at the top of the rotary cap.
19. Turn the entire assembly right-side up and place it back into the pressure cell cup.
20. Insert the wrench (also called a Tommy bar) provided into one of the six holes in the rotor assembly cap
and turn the rotor assembly clockwise threading it down and into the cup.

Replacement Parts
Replacement parts for the AR Pressure Cell are available from TA Instruments. See the table below when
ordering parts.
Part Number Description
200352.002 Pressure snubber used in manifold kit
200353.001 Three-way ball valve used in manifold kit
200380.001 Wrench Open-End 7/16 & 1/2
200380.002 Wrench Open-End 7/16 & 9/16
200380.003 Wrench Open-End 9/16 & 11/16
400.09199 Wrench (Tommy Bar) used to torque the Rotor Cap into the Pressure Cell
Cup
403001.901 Pressure Cell Assembly
403008.901 Upper Pressure Cell Assembly (with bob and magnet)
403029.901 Manifold Assembly
403032.901 Alignment Magnet used to hold the Rotor Assembly Magnet in place
403040.001 Sorbothane Pad used to mount the Tubing Manifold
403067.901 Safety Pressure Relief Port (with 2500 PSI Rupture Disc)
603.03519 Large Kalrez O-Ring 1.296 I.D. used between Rotor Cap and the Pressure
Cell Cup
603.03557 Kalrez O-Ring 0.208 I.D. used with Thumbscrew on top of Rotor Assembly
Cap
613.03378 Metric Hex Wrench Set (5, 4, 3, 2.5, 2, 1.5 mm sizes)
613.04701 90-degree Angle Pliers used on the Rotor Assembly Locking Nut

Chapter 10
The Starch Pasting Cell
Overview
Starch is used as a rheology modifier in many foodstuffs. As a raw material, it is normally supplied in the form
of approximately spherical granules, with diameters between about 1 m and 100 m. To be used as a rheology
modifier, starch must undergo gelatinization, which occurs when the granules are disrupted in aqueous
environments, to swell and eventually release the constituent molecules. The temperature at which this process
commences will depend on the nature of the starch, but it is usually approximately 60C. The process is thermally
irreversible, and when the temperature is reduced, the system remains gelatinized, although some slow de-
gelatinization (retrogradation) may occur.
The precise gelatinization temperature, the time taken for the process to go to completion, and the rheological
properties of the gelatinized starch, will depend on the source of the starch, any physical and chemical
modifications made, the pH of the aqueous phase, and so on. Test methods have been developed in the starch
industry allowing the rapid testing of starches. The general procedure is as follows:
Dispersal of a specified quantity of starch in water or buffer solution at low temperature

Raising the temperature rapidly to above the gelatinization temperature
Holding the temperature for a fixed period
Reducing the temperature to below the gelatinization temperature
Holding the temperature for a further fixed period.
Stirring is carried out during the entire process. The stirring is necessary in the pre-gelatinization stage to prevent
the starch particles from sedimenting. In the post-gelatinization stages, it is used to ensure good mixing.

System Components
Starch Pasting Cell
The SPC consists of a cell jacket, similar to that shown in Figure 10.1, mounted
on a Smart SwapTM connector for use with the AR-G2/AR 2000ex/AR 1500ex
Rheometers.
There are four components to the Starch Pasting Cell:
The jacket, which is mounted on the instrument base (see Figure 10.1)
The cup, which is removable and inserts into the jacket (see Figure 10.2)
The cap, which screws onto the jacket (see Figure 10.2)
The impeller, which attaches to the instrument spindle (see Figure 10.2).
Figure 10.1
Starch Pasting Cell Jacket
Mounted on the SPR Body
Figure 10.2
The SPR Cup (left), Cap (center) and Impeller (right)

Temperature Control
Heating is accomplished through the electrical elements placed
within the jacket, concentrically to the cup. The sample is
cooled using water carried in a helical conduit in close prox-
imity to the cup outer walls. The cooling water flow is con-
trolled through the Cooling Control Unit (CCU) (see the figure
to the right), which is placed upstream of the cup.
Purge air is used to displace the water from the conduit during
heating. The temperature is read by a Pt 100 probe in close
thermal contact with the cup bottom. The impeller shaft is
designed to prevent significant solvent evaporation.
NOTE: If the geometry gap is unreferenced

("unknown") or greater than 50,000 microns,
the temperature will be controlled to a probe
located in the jacket, rather than to the one in
contact with the cup, as it otherwise would.
Figure 10.3
Cooling Control Unit (CCU)

Connecting the CCU
The flow of the cooling water and purge air is controlled
through a Cooling Control Unit (see Figure 10.4). This
unit may be free standing, or wall mounted using the
clearance holes on top of the unit.
Connect the CCU as follows:
1. Connect the air supply to the GAS IN port using the

8-mm outer diameter tubing.
2. Connect the water supply to the LIQUID IN port

using the 6-mm outer diameter tubing. If mains water
is used as the supply, then the non-return valve
(shown in Figure 10.5) should be placed in the line
upstream of the CCU.
Important: Note the direction of flow

through this valve.
Figure 10.4
Important: Notez la direction Cooling Control Unit (CCU)
d'coulement travers de la valve.
Note the direction of flow through

the valve.
3. Connect the GAS/LIQUID outlet

port to the upper port on the
Water In Starch Cell jacket, using the 4-
Water Out
mm outer diameter tubing with
the 4-mm to 6-mm adapter pro-
vided.
Figure 10.5 4. Using the 4-mm outer diameter

Non-Return Valve tubing connect the lower port on
(For Use with Mains Water Supply Only) the Starch Cell jacket to the drain,
if the mains water is the supply,
or to the return, if a fluid circu-
lator is used.
5. Connect the EVENT B socket on the rear of the rheometer to the
EVENT socket on the CCU using only the cable.
6. Set the air flow rate to 1 L/min. Note that the reading is taken from
the center of the float. To set the flow rate, it may be necessary to raise
the temperature of the Starch Cell using the instrument software to
ensure continuous flow.
Figure 10.6
Adapter

Setting the Cooling Water
Parameters
For optimum temperature control, the parameters

for the cooling water can be set in the Rheology
Advantage Instrument Control program. Under
the Options menu, click Instrument, and select the
Temperature tab (see Figure 10.7 to the right).
The Cooling water temperature should be set to

the median temperature expected for the cooling
water during the operation of the Starch Cell.
The Cooling water range is inversely proportional

to the flow rate, measured at the exit of the drain
line. Typical values for these factors are given in
the table below. Figure 10.7
Temperature Tab
Feed Temperature Flow Rate Range
Mains tap water 15 C 0.75 L/min 5 C

Fluid circulator 5 C 0.25 L/min 15 C
NOTE: The other entries under this tab are not used by the SPC, and need not be changed
when the SPC is used.

Assembling the Starch Cell
Follow these instructions to assemble
the starch cell:
1. Raise the instrument head.
2. Insert the cup into the jacket (as

shown in Figure 10.8 to the right).
3. Screw the cap onto the jacket

(shown in Figure 10.9 to the far
right).
Figure 10.8 Figure 10.9

Inserting the Cup Into the Jacket Fitting the Cup Into the Jacket
CAUTION: To avoid damaging the threads, do not over tighten; the purpose of the cap
is to prevent rotation of the cup and to ensure good thermal contact between the base
of the cup and the temperature sensor. Light finger tightness should be sufficient to
achieve this.
Important: Afin de ne pas endommager le filetage, ne pas serrer trop fort ; le rle du
couvercle est d'empcher la rotation du cylindre externe et d'assurer un bon contact
thermique entre la base du cylindre et la sonde de temprature. Une pression lgre
exerce par le doigt est suffisante pour accomplir ceci.

Calibration of the Measuring Sytem Factor
Calibration of measuring system is required to obtain the factor used in the calculation of the sample
viscosity from instrument parameters. Typically the cell has already been calibrated by TA Instruments'
engineers and it is unlikely that the factor for any other unit will differ substantially from this. Therefore,
you should not find it necessary to recalibrate. However, a suggested procedure is provided here for
your convenience.
Operating Parameters
The operating parameters of rotational rheometers are the torque, M, which in the S.I. system has units
of newton meters, N.m, and the angular velocity, , which has S.I. units of radians per second, rad s-1,
although revolutions per minute, rpm, are also often used (1 rpm = / 30 rad s-1).
To obtain the sample viscosity, a measuring system factor, Fm is used, which depends on the form and
dimensions of the measuring geometry used. Then the viscosity, , is given by:
= Fm M /
The S.I. units of viscosity are pascal seconds, Pa.s, and those of Fm are therefore m-3.
For standard measuring systems, such as the cone and plate or concentric cylinders, which produce well
defined (viscometric) flow regimes, Fm can be derived analytically, and there is no need for calibration.
However, for measuring systems such as the Starch Cell impeller, which produce non-viscometric flow
regimes, Fm cannot be derived analytically, and calibration is required.
Performing the Calibration

Sample Type
For the calibration, at least one Newtonian liquid is required. Newtonian liquids are those for which the
viscosity is independent of the applied shear stress or shear rate. Certificated traceable standards can be
obtained from companies such as Poulten, Selfe and Lee, www.rheotek.com, or Cannon Instrument Co.,
www.cannoninstrument.com. A lower cost alternative is to use materials that are known to show
Newtonian behavior, such as sugar solutions or lubricating oils, the viscosity of which can be indepen-
dently determined.
Recommended are standard liquids that are close in viscosity to those expected for typical starch samples
(about 1 Pa.s), at a temperature close to ambient (for example 20C).
Procedure
1. Prepare the Starch Cell as described in this manual.
2. Remove the cup and add the volume of standard liquid as would be used for a starch sample (normally
about 28 cm3). It may be necessary to perform a preliminary inquiry to establish the appropriate
level in the cup.

3. Replace the cup and cap, and send the instrument to the required geometry gap.
4. Using the instrument status page, set the required angular velocity, which should be the same as the value
used for the starch testing, normally 160 rpm (16.76 rad s-1). Record the reading for the torque when this
reaches a steady value.
The measuring system factor is then given by:
Fm = / M
5. To enter the measuring system factor, ensure that the starch cell is selected as the current geometry, then
on the Geometry menu click View, and under the Dimensions tab enter the value obtained in the
Calibration factor box (see Figure 10.10 below).
Figure 10.10
Geometry Dimensions Tab
The default value of 10800 m-3 was obtained as the average of several runs for three standard liquids, by TA
Instruments' engineers. This can be replaced by the value you determine, if preferred.
NOTE: Starch pastes are non-Newtonian liquids and their viscosities will depend on the shear
rate or shear stress imposed. For non-viscometric flows, such as that produced by the Starch
Cell impeller, the shear stress and, therefore, the sample viscosity will not be uniform within
the sample. The value reported by the SPC will be the Newtonian equivalent viscosity, which
is often sufficient for practical purposes.

Conical Rotor
The SPC may also be used as a conventional concentric cylinder rheometer, with the conical hard anodized rotor,
part number 545761.001.
To set up this geometry, under the Geometry menu in the Rheology Advantage Instrument Control program,
click New and DIN or conical concentric cylinders. On the New Geometry/Dimensions page enter the
details as:
Stator inner radius (mm) 18.50

Rotor outer radius (mm) 15.55
Cylinder immersed height (mm) 37.00
Gap (mm) 5920

Chapter 11
The Interfacial Accessory and Du Noy Ring
Overview
In this chapter, the bicone and Du Noy ring measuring systems, used to measure the rheological properties of
interfaces, are described. The bicone is available only for both the AR 2000ex and the AR-G2, the Du Noy ring
is available only for the AR-G2.
Interfacial Rheology
At the interface between two immiscible liquids, or between a liquid and a gas, a two-dimensional phase exists
that has its own rheological properties, distinct from those of the two bulk phases [D.A. Edwards, H. Brenner
and D.T. Wasan "Interfacial Transport Processes and Rheology" Butterworth-Heinemann, Boston, 1991] (the
interface between a liquid and a gas is often referred to as the "surface." In this manual the general term "interface"
is used for both cases).
The interface can be deformed either by changing its area (the dilatational mode) or by keeping the area constant
but moving elements of the interface relative to each other (the shear mode). Schematics of each mode are shown
in Figure 11.1. Interfacial counterparts of the bulk rheological properties exist for both dilational and shear
deformation modes. Thus the interface will have a dilatational and a shear viscosity, complex modulus, and so
on. For each deformation mode, interfacial stresses and strains analogous to those of a bulk fluid can be defined.
If the interface is assumed to be two dimensional (i.e. to possess zero thickness), then the interfacial stress becomes
a force acting over a line, so has units of N.m-1. Like the bulk strain, the interfacial strain is dimensionless.
Unperturbed Interface Shear Deformation
Dilatational Deformation
Figure 11.1
Interface Schematic
The interface is represented by schematic surfactant molecules. The less dense bulk phase is assumed to be above
the interfacial plane, and the more dense bulk phase below it. The interface itself is assumed to be of zero
thickness. The interfacial stress acts along the red line in the direction of the arrow.

Likethebulkextensionalandshearproperties,theinterfacialshearanddilatationalpropertiesmustbemeasured
separately.Onesetofpropertiescannotbesecurelypredictedfromtheother.Forexample,themostcommonly
measuredpropertyoftheinterfaceistheinterfacialtension,whichcanbedefinedastheforceresistingachange
insurfaceareaforagivenlengthofsurfaceperpendiculartotheforce,andis,therefore,adilatationalproperty.
Sotheinterfacialshearpropertiescannotbeobtainedfromtheinterfacialtension.TAInstrumentsinterfacial
rheologyaccessoriesaredesignedtomeasuretheshearpropertiesoftheinterface,althoughtoavoidunnecessary
repetition,thedeformationmodeisnotalwaysreferredtointhismanualandinRheologyAdvantagesoftware.
Severalwaysofdeterminingtheinterfacialshearpropertieshavebeendeveloped,someofwhichcan,inprinciple,
beadaptedforusewithaconventionalrotationalrheometer[E.Shotton,K.Wibberley,B.Warburton,S.S.Davis
andP.L.Finlay,RheologicaActa,10,142152,1971].Butuntilrecently,rheometersdesignedtomeasurethebulk
propertiesofmaterialslackedthesensitivitytoperformmeaningfulinterfacialmeasurements,andonlytheAR
G2hasthesensitivityoftraditionalinterfacialrheometers.
Thebicone,whichconsistsofathinbiconicaldiscpositionedattheinterface,isusedtomeasuretheinterfacial
steadyshearviscosity,interfacial.Thesampleisheldinacircularcup,andthemeasuringsystemisthereforea
twodimensionalanalogueoftheconcentriccylindersystem.Buttherelativelyhighmomentofinertiaofthe
rotormakeitlessusefulformeasuringtheinterfaciallinearviscoelasticproperties,exceptwheretheseareis
exceptionallyhigh.TheoscillatingDuNoyringsystem,forwhichthegeometryisaplatinum/iridiumring
andthestatorisadish,isbettersuited,sincethemomentofinertiaoftherotorismuchlower.
TAInstrumentshavethereforedevelopedtwomeasuringsystemsusedfordeterminingtheinterfacialshear
properties:theBiconeInterfacialAccessory,designedprimarilytomeasuretheinterfacialviscosity,andtheDu
NoyRingsystem,availablefortheARG2only,usedinoscillationmodetodeterminetheinterfacialviscoelastic
properties.Usuallytheinterfacialviscosityisrequiredwhenbothphasesareliquids,andtheviscoselastic
propertiesarerequiredwhentheupperphaseisair.
Setting up the Geometry Details

BoththebiconeandtheDuNoyringcanbetreatedasinterfacialanaloguesoftheconcentriccylindersystem,
andanalogousfactorscanbeused.Theinterfacialmeasuringsystemfactorsare:
whereR1istheradiusofthebiconeorDuNoyring,andR2istheinnerradiusofthecupordish.Thefactors
fortheavailableinterfacialbiconeandDuNoyringaregiveninTable11.1
Cupordishinnerdiameter Biconeorringdiameter S.I.units c.g.s.units

F F F F
mm mm m2 cm2
80 68 6.207118.66.2070.01186
66 20 1.202868.81.2020.08688
Table 11.1:Bicone and Du Noy Ring Measuring Systems Factors

The geometry details can be set up using manual factors. On
the Geometry menu, click New and select Manual factor
input. On the Description window, name the geometry as
preferred, for example Interfacial bicone. On the Dimensions
window, shown in the figure to the right, for insert the
appropriate factors (the value for the fluid density factor
should be set to effective zero and that for the normal force
factor is set to unity, for convenience).
NOTE: The units for the interfacial shear

Figure 11.2
stress factor should be m-2 for S.I. units, and Manual Factors Input Window
cm-2 for cgs units, not as displayed.

Bicone Interfacial Accessory
The bicone interfacial accessory is mainly used to determine the viscosity of the interface between two liquid
phases. The stator is a circular cup with removable lid, the geometry is a thin, biconical disc (Figure 11.3). For
chemical inertness, and to reduce the meniscus effect, the cup and lid are constructed from poly(tetrafluoroet-
hene), PTFE, and the geometry from stainless steel. It is important that the cup and disc are aligned concentrically,
and the base with Smart SwapTM connector into which the cup sits has been designed to ensure this. Normally,
the cup should be exactly half filled with the more dense sample fluid, and filled to the top with the less dense
fluid. The disc is placed at the interface of the two fluids. A mark has been lightly inscribed on the inside of the
cup to indicate when it is half full.
Biconical Geometry
Lid
Fluid B
Interface
Cup
Fluid A
Figure 11.3
Interfacial Rheology Accessory Schematic
Liquid A is the more dense fluid, liquid B the less dense fluid, R1 is the disc radius, R2 is the cup inner radius,
H1 is the lower fluid depth, and H2 is the upper fluid depth. For correct operation H1 should equal H2.
Dimensions
Cup: Depth 45 mm
Inner diameter 80 mm
Volume 226 cm3 (approximately)
Material PTFE
Geometry: Disc diameter 68 mm

Bicone angle 10
Inertia 32.4 Nm s2 (approximately)
Material BS970-303 S31 grade stainless steel
Interfacial surface area: 1395 mm2
Geometry gap with disc edge level with the cup half full mark (22.5 mm): 19,500 m (approximately)
Temperature control: Ambient only

Experimental Procedure and Data Treatment
The calculation of the interfacial viscosity for the general case is complicated and can only be solved using
numerical procedures [S-G. Oh and J.C. Slattery, Journal of Colloid and Interface Science, 67, 516 - 525, 1978].
However, if the first order assumption is made that the contributions from the three phases are independent of
each other, then the calculation becomes relatively straightforward. The contributions from each of the two bulk
fluids can be determined separately, and the interfacial contribution can be obtained by subtraction of these
from the total contribution.
To do this, the cup is filled completely with one of the fluids, and the geometry is set to gap of 19,500 m, so
that the disc edge is level with the half full mark. The viscosity contribution is determined over the range of
shear rates of interest. The process is repeated for the other fluid, and for each shear rate the contributions for
the two fluids are added together. The total will be twice that of the upper and lower fluids combined when
they each occupy half the cup volume. This value can therefore be halved and subtracted from the total
contribution, obtained in the presence of the interface, to give the viscosity due to the interface. A two-dimensional
analog of the concentric cylinder geometry is used to calculate the interfacial rheological properties. Details of
the analysis are given below. A similar procedure can be used to obtain the dynamic properties of the interface.

Operation
Setting up the Interfacial Bicone Accessory
Follow the instructions below to set up the rheometer with
the interfacial accessory:
1 Raise the instrument head, and attach the cup holder to

the rheometer using the Smart SwapTM connector, as
shown in Figure 11.4.
2 Place the cup in the holder, without the lid. Insert the
geometry shaft through the hole in the cup lid, and attach
the geometry to the rheometer spindle. Lift the lid and fix
in the upper position, as shown in Figure 11.5 below, by
passing the slots in the lid over the lugs attached to the
geometry shaft, and rotating the lid. Use the knurled grips Figure 11.4
to handle the lid, to avoid touching the under surface; Interfacial Accessory Base Installed
these can either be gripped manually, or using a pair of
fine-nosed pliers.
Figure 11.5
Instrument Head and Lid in the UP Position (left) and DOWN Position (right)
Zeroing the Gap

Lower the instrument head until the bicone is within the cup, but is clear of the cup lower surface. Lower the
lid to sit in the groove on top of the cup. Zero the geometry gap in the usual way. Note that at the zero position
the lugs on the geometry shaft will be approximately 2 mm clear of the lid.
Mapping and Other Calibrations

Rotational and oscillatory mapping and other calibrations, for example of the geometry inertia and bearing
friction, are best carried out at this stage. Set a gap of 19500 mm, and perform the mapping and calibrations in
the usual way.

Determining Each Fluid's Contribution
Follow the steps below to determine the contribution from each bulk fluid.
1 With the gap set at 19500 mm fill the cup with sample Fluid A until the fluid is just above the lower edge of
the groove on top of the cup. Gently lower the lid. The fluid should overflow from the annular gap between
the lid and the geometry.
2 To obtain the sample viscosity, use a Flow procedure and apply the required shear rate (or angular velocity)
or range of shear rates. It is usually preferable to use a Steady State Flow procedure for this, but the details
will depend on the sample, and the reasons for conducting the experiment. This procedure gives the viscosity
contribution of fluid A, Acalibration( ), at shear rate .
3 To obtain the sample linear viscoelastic properties, use an oscillation procedure and apply the required strain
or range of strains, at the frequency of interest. This will give the storage and loss modulus contributions of
Fluid A, GAcalibration() and GAcalibration().
NOTE: When setting up the procedure, in the conditioning step on the Settings tab, uncheck
the Wait for correct temperature box. Any temperature settings in the procedure will be ignored.
4 After running the procedure, raise the instrument head, and remove, clean and replace the cup. Repeat the
procedure for the sample Fluid B, to obtain Bcalibration( ), GBcalibration() and GBcalibration(), then remove,
clean and replace the cup.
Finding the Interface Position

Use the following procedure to fill the cup and find the interface position:
1. Raise the instrument head to the backoff distance then lift and fix the lid.
2. Fill the cup to the half full mark with the more dense of the sample fluids.
3. Set a gap of 24000 m and lower the lid.
4. Ensure that the "Zero normal force before run" box is checked under Options/Experiment/Pre-experiment.
5. Use a squeeze test similar to that shown below in Figure 11.6. This can be set up using Procedure/New/Flow.
Figure 11.6
Procedure to Identify Interface Position

6. Plot the results as normal force against gap. When the geometry is at the interface, the normal force passes
through zero. To establish this point, the graph grid and cursors can be used, as shown in Figure 11.7.
Figure 11.7
Graph to Identify the Interface Position
7. Determine the point at which the normal force passes through zero. This is the position of the interface,
which should be at a gap of approximately 19500 m. Adjust the fluid volume to obtain this gap. Keep in
mind that 1 mL of fluid changes the level by about 0.275 mm.
8. When the interfacial position has been identified, manually set the gap to that position (in the example
shown on above, to 19527 m).
9. Lift and fix the lid. You may find it convenient at this stage to add any surfactants to be used.
10. After addition of surfactant, gently add the less dense fluid until the lower edge of the groove on the top of
the cup is just covered, then lower the lid gently. The upper fluid should overflow from the annular gap
between the lid and the geometry shaft. The viscosity of the total system including the interface can now be
measured.
11. Run the Flow or Oscillation procedure to determine the contributions of the two bulk fluids, described above,
to obtain the total viscosity contribution total( ), or modulus contributions Gtotal() and Gtotal() as
described.
12. Calculate the interfacial viscosity or dynamic properties as in the next section.

Analyzing Results
Calculation of the Interfacial Contribution to the Torque
The interfacial contribution to the torque, interfacial( ) at a particular shear rate is calculated by subtracting
the contributions of the two bulk fluids, A and B from the total viscosity contribution for the system at that shear
rate, i.e.:
interfacial( ) = total( ) + A( ) + B( )
A and B, are obtained from the calibration routine described above. Note that these are not the actual viscosities
of the two fluids, they are the contributions that their viscosities make to the total resistance to flow.
But A ( ) is half the viscosity contribution obtained at for fluid A from the calibration routine, and B is
half that obtained for fluid B, since for the calibration routines the cell is filled with the relevant fluid, whereas
for the interfacial measurement it is half filled with Fluid A and half with Fluid B, i.e.
A ( ) = Acalibration( ) / 2 and B ( ) = Bcalibration( )/2
Three data points are therefore needed for each shear rate used:
the calibration data point for Fluid A

the calibration data point for Fluid B
the data point for the total system
Then:
interfacial( ) = total( ) - [Acalibration( ) + Bcalibration( )] / 2
NOTE: The units for interfacial viscosity are Pa.s.m for S.I. units, and P.cm for cgs units, not
as reported by Rheology Advantage.
If the interfacial shear stress is required, it can now be calculated:
interfacial = interfacial x
NOTE: The units for interfacial shear stress are N m-1 for S.I. units, and dyne cm-1 for cgs
units, not as reported by Rheology Advantage.

Calculation of the Interfacial Linear Viscoelastic Properties
The calculation of Ginterfacial() and Ginterfacial() can be made in a similar way to the calculation of hinterfacial.
The properties of complex variables allow us to consider the in- and out-of -phase components of Fluids A and
B and the interface separately. Then:
Ginterfacial() = Gtotal() - [GACalibration() + GBCalibration()] / 2
Ginterfacial() = Gtotal() - [GACalibration() + GBCalibration()] / 2
Note: the units for the interfacial moduli are N m-1 for S.I. units, and dyne cm-1 for cgs units, not
as reported by Rheology Advantage.
Other variables can now be calculated if required, for example:
|G*interfacial()| = {[Ginterfacial())]2 + [Ginterfacial()]2}0.5
= atan [Ginterfacial()/Ginterfacial()]
interfacial = |G*interfacial()| x
NOTE: The units for the magnitude of the interfacial complex modulus, |G*interfacial()| are
N m-1 for S.I. units, and dyne cm-1 for cgs units, and the units of the interfacial shear stress are
are N m-1 for S.I. units, and dyne cm-1 for cgs units, not as reported by Rheology Advantage.
The phase angle, , is dimensionless.

The Du Noy Ring (AR-G2 Only)
The Du Noy ring measuring system is mainly used to determine the linear viscoelastic properties of the interface
between a liquid and air. It consists of a thin wire ring and a Duran glass dish (Figure 11.8). The ring is constructed
from a platinum / iridium (Pt/Ir) alloy, for chemical inertness, ease of cleaning, and wettability. It is important
that the ring and dish aligned concentrically, and a locating ring is provided that fits over the Peltier plate to
ensure this. Two dishes are available, the outer diameter of the standard dish is 70 mm, and of the small dish is
50 mm.
Du Nouy Ring
Interface
Dish Fluid
Figure 11.8
Du Noy Ring Measuring System Schematic
R1 is the ring radius, R2 is the dish inner radius.
Du Noy Ring Dimensions

Dish (standard): Depth 30 mm (approx)
Outer diameter 70 mm
Inner radius 66 mm (approx)
Dish (small) Depth 30 mm (approx)

Outer diameter 50 mm
Inner diameter 46 mm (approx)
Material Duran glass (Schott AG)
Geometry: Ring diameter 10 mm

Inertia 0.70 Nm s2 (approx), including holder
Material Platinum / iridium (Pt/Ir) alloy
Temperature control: Peltier plate

Setting Up the Du Noy Ring
Follow the instructions in this section to set up the ring.
CAUTION: Handle the Du Noy ring with care: it is delicate and can easily be deformed
or broken.
Zeroing the Gap

Follow these steps to zero the gap:
CAUTION: To avoid damaging the Du Noy ring, zeroing the gap should only be done
with the gap zero tool, not with the ring.
1. Ensure that the Peltier plate is fitted to the AR-G2.
2. Insert the zero gap tool into the geometry holder,

ensuring that the tool is fully seated in the centering
hole, and fix it in place by turning the collet.
3. Raise the head of the instrument and attach the geom-

etry holder to the draw rod (see Figure 11.9).
4. Zero the gap in the usual way.
5. Remove the holder from the spindle and the tool from
the holder.
Mounting the Ring on the AR-G2 Spindle

Follow these instructions to mount the ring:
Figure 11.9
1. Raise theinstrument head. Zero Gap Tool in the AR-G2 Geometry Holder
2. Attach the geometry holder to the draw rod, then

insert the Du Noy ring into the holder, ensuring that it is fully seated in the centering hole. Turn the
collet to secure. This is best done if the rheometer spindle is locked by pressing the button on the front
panel, or you may find it easier to install the ring into the holder before attaching the holder to the draw
rod. Tighten the collet finger tight, do not overtighten. (See Figure 11.10 on the next page).
3 Place the sample dish locating ring on the Peltier plate. Use the insert also, if the 50-mm diameter dish is
used.
4. Proceed to the next section to perform the mapping function.

Mapping
After the ring is mounted, perfrom the mapping function as follows:
1. Lower the instrument head until the ring is about 40-mm above the Peltier plate.
2. Use the oscillatory mapping function described in the Rheology Advantage Help System. Make sure that
you do not touch the instrument head or the Du
Noy ring after the mapping.
3. Load the sample as described in the next section.
Loading the Sample & Locating the

Interface
Follow the instructions below:
1. Load the sample into the dish. The depth of the

sample is not critical, but about 15 mm is reason-
able.
2. Place the dish on the Peltier plate within the locat-

ing ring.
3. Lower the head until the ring is in the plane of the

sample surface. This may be done by entering the
approximate height of the sample surface above
the Peltier plate, as the Gap Required Value then
click Send. Fine adjustment can be made manually.
The rate of head movement for manual control is Figure 11.10
set in Rheology Advantage under gap control Du Noy Ring at the Liquid Surface
Other Velocity.
4. Ensure that the ring is fully wetted by bringing it

completely through the surface the approach the
surface from below (See Figure 11.10)
5. Gently fit the draft shield in place, ensuring that the shield does not touch the Du Noy ring or instrument
head while fitting.
6. Begin the experiment.

Calculation of Interfacial Linear Viscoelastic Properties
The properties of the interface as measured using the TA Instruments Du Noy measuring system are absolute,
i.e., the contribution from bulk liquid is not subtracted. If the excess interfacial moduli are required, the properties
of the bulk fluid / air interface need to be accounted for. This is not normally necessary if water is the bulk liquid,
since the moduli of the water / air interface are very low.
NOTE: The units for the interfacial moduli are N m-1 for S.I. units, and dyne cm-1 for cgs units,
not as reported by Rheology Advantage. The units for the magnitude of the interfacial complex
modulus, |G*interfacial()| are N m-1 for S.I. units, and dyne cm-1 for cgs units, and the units of
the interfacial shear stress are are N m-1 for S.I. units, and dyne cm-1 for cgs units. The phase
angle, , is dimensionless.
Cleaning
The biggest source of error when making surface rheological measurements is contamination of the ring or dish.
Both the ring and dish should be thoroughly cleaned before and after use.
Cleaning the Ring

To clean the ring:
1. Remove the ring from the rheometer.
2. Rinse or soak the ring in an appropriate solvent.
3. Use a micro-jet gas burner to burn off any additional residue. Position the flame on the ring until it glows
red. Every part of the ring that will be in contact with the sample should be treated in this way.
WARNING: Do not attempt to flame the Du Noy ring while it is mounted on the rheometer
This could cause serious damage and may be dangerous. Take care when flaming the Du
Noy ring. It can be held by the holder, but do not grasp it directly. Ensure that no flammable
materials are nearby. Do not touch the ring or place it in contact with flammable materials
until it has cooled down.
Cleaning the Sample Dish

Clean the sample dish using a proprietary cleaning agent. Then rinse it thoroughly with distilled water. You can
also safely heat the dish to 500 C in an oven.

Chapter 12
The Environmental Test Chamber
Overview
The ETC is an add-on unit for the AR-G2/AR 2000ex that enables
it to characterize solid samples in torsion. To work on composites/
polymers in torsion requires a temperature-controlled chamber
for environmental control of the sample, plus specially designed
sample clamps. The ETC can also be used for conventional
rheology measurements with the appropriate geometries.
ETC Components
The ETC chamber is mounted onto a metal plate that is secured
to the back of the AR-G2/AR 2000ex using existing mountings.
ETC
The oven is made up of two halves (left and right as viewed from
the front see Figure 12.1), with each half containing a specially
designed heating element with a thermocouple welded to it (see
Figure 12.3 on the next page). Various interlock devices are fitted
for safety purposes. These devices detect the position of the doors
and whether the heat shield, which protects the rheometer from
being damaged, is fitted.
The left-hand door also incorporates the gas ring, which allows
stirring air and liquid nitrogen to be fed into the chamber. The
control electronics are contained within the main electronics of Figure 12.1
the ETC. ETC Mounted on AR-G2

Torsion/Rectangular Gas Ring Light or Optional Camera
Tool Thermocouple
Thermocouple
Insulation Thermocouple Heating Coil
Heating Coil
Figure 12.2
Heating Chamber Interior (LHS)

Using the ETC
This section provides information on how to install and set up the Environ-
mental Testing Chamber (ETC). For more information on the ETC, see the
Rheology Advantage online help.
1. Turn on the rheometer and move the rheometer head up to the maximum
height. (Use the 'Head UP' button, located on the instrument control
panel.)
2. Fit the air-bearing clamp to the rheometer.
3. Turn off the power to the rheometer control box.
4. Ensure that the two top screws (A and B in Figure 12.3) are fitted with
washers and are located in placebut make sure that they are almost
totally unscrewed (two turns in).
5. Open the ETC oven (see Figure 12.4) and then use the handles on the
oven doors to lift it onto the two top screws. Lightly tighten these screws.
Figure 12.3
Mounting Screws
Figure 12.4
The ETC Open
6. Insert the final two screws (C and D in Figure 12.5).
7. Adjust the position of the ETC on the screws and then tighten all four.
8. Check the adjustment and adjust if required by loosening the screws

and shifting the position of the ETC on the rheometer.
9. Connect the two cables on the ETC to the attachment connectors on

the rheometer as shown in Figure12.6.
10. Open the ETC oven doors to gain access to the Smart Swap mount-
ing.
Removal of the ETC is the reverse of the preceding steps. Note, however
that you can leave the oven in place when you wish to use the one of the
Peltier systems.
Figure 12.5
Connecting the Cables

g
e ETC
11. Press the Release button, , on the control panel. A continuous
green light indicates that the attachment can be fitted.
NOTE: The release state will only stay active for 10

seconds.
Le dvrouillage restera actif pendant 10 secondes.
12. Fit the lower attachment, ensuring it is aligned correctly. See Figure
12.7 below.
Figure 12.6
13. Connect the cable from the ETC with Open Oven Doors
lower attachment to the
rheometer as seen in
Figure 12.8.
14. Close the oven and

ensure that no part of
the doors touch any
part of the lower fix-
ture. Adjust the posi-
tion of the ETC again, if
Alignment Pin
required.
Figure 12.7
Fitting the Lower Attachment
15. Attach the upper geometry, again making sure that no parts are
touching the fixture, adjusting the ETC if necessary.
16. If you plan to use the liquid nitrogen option with the ETC, skip
the following steps and proceed to the next section for installation
instructions.
Figure 12.8
Connecting the Cable from the Lower
Attachment to the Rheometer

17. Connect the purge gas to the rheometer as seen
in Figure 12.9 to the right. If you have a suitable
supply of nitrogen gas (2 bar minimum pressure,
nominal 10 liters per minute flow rate) it is rec-
ommended that you connect the feed gases to the
ETC as shown in Figure 12.11. Otherwise, connect
as shown in Figure 12.10 below.
CAUTION: The reducing valve is

factory-set to 10 liters per minute
and should not be adjusted.
La valve rductrice est rgle 10

litres par minute et ne devrait pas
tre modifie.
Figure 12.9
Connecting the Purge Gas
Figure 12.10
ETC Connections Using Air as the Agitation Gas
Figure 12.11
ETC Connections Using Nitrogen as the Agitation Gas

Installing the Low Temperature Accessory
In order to operate the ETC at temperatures below ambient and also to facilitate rapid cooling, the (optional)
low temperature accessory can be used. This works by supplying a controlled flow of liquid nitrogen/cold
nitrogen that is fed down the inside of the oven and evaporates off the wire wool.
Follow the installation procedure in the previous section up to step 15. Then use
the following additional steps to complete the installation (see Figure 12.14 and
Figure 12.15).
1. Connect the Event cable from the CCU flow control assembly to the Event A
connection on the rheometer.
2. Ensure that the cryogenic system has been installed as directed in the instruc-
tions supplied by the manufacturer.
3. Connect the tap and solenoid valve unit to the liquid nitrogen outlet on the
Dewar, and the unit to the Liquid in port on the Flow Meter Assembly using
the long flexible hose provided. Connect the Gas/Liquid Out port on the Flow Meter Assembly to the purge
gas port on the ETC using the short flexible hose provided, as shown in Figure 12.12.
Figure 12.12
Connecting the Hose
The electrical and gas/ liquid connections for the ETC low temperature assembly are shown in Figure 12.13.
4. Connect a gas feed to the Gas In port on the Flow Meter Assembly using the 8-mm internal diameter white
nylon tubing provided. If the main air supply is used as the feed gas, the line should be split upstream of the
Flow Meter Assembly and Rheometer Filter/Regulator.
5. Connect the cable from the 'Liq' connector on the flow assembly to the solenoid valve on the cryogenic system.
6. Set a pressure of 15 to 20 PSI on the Dewar system.
7. Open the control valve approximately two full* turns.
8. Set a flow rate of 10 liters per minute (LPM) on the flow meter assembly. Make sure the oven is closed.
* The exact setting depends upon the required operating conditions for the ETC as well as the type of cryogenic
cooling system used. Additional information on this setting can be found in "Operating Hints" later in this chapter.

Figure 12.13
Electrical and Gas/Liquid Connections for the ETC Low Temperature
Assembly
(The electrical connections are shown as the narrow black lines.)
If the system has been set up according to the instructions, the rheometer should now be ready to use. However,
we recommend that you follow a few extra precautions, described on the next several pages.
If you are planning to start your experiment at a high temperature, preheat the system by lowering the head
to the measurement gap and allowing upper and lower geometries to rise to the set temperature.
When you use the cone and plate or parallel plate geometries, it is important to use the correct sample
volume. The Rheology Advantage software calculates the exact volume required based upon the gap size
and geometry diameter. If you know the density of the sample, you can weigh out the correct amount of
sample. If you underfill or overfill the gap, you can cause experimental errors in your data.
When you use the parallel plates, make sure that the oven thermocouple is not touching the plates.
When you use the parallel plates, if you find that the lower plate is difficult to remove, make sure that you
apply a twist to the lower mounting platedo not apply any force to the ceramic part of the geometry.
Clean the plates immediately after your experiment with the appropriate solvent. If you are measuring
highly viscous materials, or materials that are likely to cure, unscrew the draw rod from the geometry before
you raise the head. Stubborn materials can sometimes be removed by heating the plates to a high temperature.
The sample will bake and then crumble apart. You can also remove the plates and soak them in an appropriate
solvent. It is good practice to always unscrew the draw rod before raising the head. The two plates, together
with the sample, can then be removed as a sandwich unit.

Torsion rectangular tools only: You can gently move the thermocouple (inside the oven) closer to the sample
to increase performance; however, you should avoid making any sharp bends in the thermocouple sheath.
Repeatedly adjusting the positioning may damage the thermocouple and should be avoided.
Operating Hints
Although the response time of the temperature control system is rapid, many of the samples that are of interest
at high temperatures (e.g., bitumen, molten polymers, etc.) are very poor conductors of heat. Therefore, the
limiting factor in reaching the desired starting temperature is the time it takes for the heat to be conducted into
the sample and for the sample to reach thermal equilibrium. You can investigate a sample by carrying out an
experiment using no equilibrium time and doing a time sweep experiment (in oscillation mode). If you plot a
graph of how the properties of the sample vary with time, you can quickly establish the required equilibrium
time.
The tendency of polymers (which are measured while in their molten state) to oxidize can present an additional
complication. This problem is generally sample-dependent, but can be reduced by surrounding the sample
with an inert atmosphere. To do this, use nitrogen gas rather than air as the feed to the ETC. It also helps if
you optimize your test procedures to minimize the amount of time that the sample is held at high temperatures.
Make sure the upper geometry is in place and free to rotate when you perform procedure for mapping of the
bearing. For best results, perform the mapping procedure at ambient temperature and without purge gas
flowing. (Further information on the mapping procedure can be found in the Rheology Advantage Help
system.)
Controlling Cooling
When you set the control valve on the liquid nitrogen unit, you must compromise between the rate of cooling
(which is improved by having a large flow rate) and the fineness of control (which is optimized when there is
minimal flow rate from the needle valve.) When only a small amount of cooling is required, the solenoid valve
is able to open and shut frequently. However, if a large surge of coolant occurred every time the solenoid valve
opened, the system temperature would oscillate on either side of the set point.
The setting of the needle valve is affected by the desired set-temperature:
If cooling is needed at only a few degrees below ambient, then a very small opening is all that is necessary.
If you operate at -100 C, then a correspondingly higher flow rate of nitrogen is required.
As a general rule, the correct needle valve setting for the desired temperature is one that results in the opening
and closing of the solenoid valve for more or less equal periods. Start with a setting of "open two complete
turns" and experiment to find the optimum position for your work experiment procedures.
Low Temperature System Maintenance

For maintenance instructions of the cryogenic pressure vessel, please refer to the instructions supplied with the
unit. If you purchased the Dewar flask from TA Instruments, the document is titled "Guide to good
housekeeping, maintenance and periodic examination of cryogenic pressure vessels."

Chapter 13
The ETC Viewer
Overview
WARNING: After ETC use, do not turn off the cooling air to the ETC Viewer until the unit
has returned to room temperature. Doing so could damage the lens assembly and/or
camera chip.
AVERTISSEMENT : Aprs avoir utilis lETC, et jusqu ce que lunit soit revenue la
temprature ambiante, laissez larrive de lair de refroidissement ouvert dans lETC
Viewer (Systme de visualisation du four). Le fait de fermer cette arrive trop tt pourrait
endommager le systme optique et/ou la camra.
The ETC (Environmental Testing Chamber) Viewer is as an option that can be used with the rheometer for the
following purposes:
Viewing the edge of plates and cones and the torsion sample
Providing streaming video on Status page and during tests
Capturing images with data point (not fast sampling)
Viewing point image in Rheology Advantage Data Analysis and pseudo playback
The software provided with the ETC Viewer works with any USB camera so a web cam can be easily used for
Peltier tests. The viewer assembly is air cooled to allow it to perform over whole temperature range of the ETC
(-160 to 600 C). The primary and secondary illumination, as well as the focusing aspects of the viewer, are all
controlled from Rheology Advantage Instrument Control software for your convenience.
Installing the ETC Viewer

All AR-G2 ETCs are shipped in a state which is prepared to install the ETC Viewer. Insulated plugs fill the viewer
and secondary lighting cavities that are needed for the
viewer. The viewer will generally be fitted by a TA service
engineer, but if the unit needs to be removed for return to
a TA service shop for repair follow these instructions.
WARNING: Make sure ETC is at ambi-

ent temperature before attempting
this procedure. 3-mm
Hex Head
Screws
AVERTISSEMENT : Avant de raliser
cette procdure, assurez-vous que
lETC est la temprature ambiante.
1. Turn off power and air.
2. Remove the two 3-mm hex head screws shown in the

picture to the right.

3. Loosen the two 3-mm hex head screws
shown in the figure to the right. This will
allow the cover to be removed as seen below.
3-mm
Hex Head
Screws
Bulkhead
Screws
4. Remove the three 3-mm hex head bulkhead screws

holding the secondary lighting in place and remove
the unit. Fit the insulated plug in its place.
5. Remove the three 3-mm nuts holding the main

viewer module in place and remove the unit. Fit
the insulated plug in its place.
Location
NOTE: The location of the stand offs of Stand offs
is shown in the figure to the right.
The actual stand offs are not visible
in the picture.

6. Disconnect the signal/power connector and cooling air Signal/Power
supply from the inside of the back panel shown in the Connector
Cooling Air
figure to the right. Supply
The complete unit can now be removed and packed in its

original packing material.
7. Follow the instructions in reverse for fitting the viewer

module.
The picture below shows the viewer control box and connec-
tions.
8. Place a "T" connector in the main air line to the rheometer,

before the filter regulator, and then feed through the
supplied flow meter at 15 L/min. This is for the cooling
air supply.
9. Connect EXP-1 on the control box to EXP-1 on the rear of

the main electronics box. See the figure below.
EXP-1
Cooling Air Video Out EXP-1

Connection
Video Out USB Adapter
10. Connect the video out to a USB adapter, which is in turn

connected to a USB port on the control PC. Refer to the
installation instructions provided by the original equip-
ment manufacturer (OEM supplier) for installing the
driver needed for this device.

Schematics
The following figures provide schematics of the various components of the ETC Viewer.
Schematic of Cooling
Schematic of Primary Lighting
Sample View

Lighting Schematic

Software
The software for the ETC Viewer is compatible with the viewer and any other USB camera with appropriate
drivers.
Rheology Advantage Instrument Control

Icon toggles between showing/
hiding live image

Image Controls Main
Lighting
Peripheral
Lighting
Intensity Intensity
Adjust the controls (shown in the figure to the right) to illuminate Focus In
part of the sample of interest. The peripheral lighting is particularly
useful for illuminating the edge of the sample. These controls can Focus Out
be adjusted during the measurement.
Right clicking on the image allows access to the live image capture
setup (shown in the figure below).
Other USB cameras

(i.e., web cam) can
be selected here

Storing Images
To keep file sizes to acceptable limits an image is, in
most cases, captured at the same time as the data point.
Some fast sampling modes may restrict the frequency
of image capture. The settings are found under
Options/Experiment for each procedure type. The
setting for flow is shown to the right.
Data Analysis
If images have been stored with the data file, the
individual point images can be viewed in the data
analysis software by checking the point image under
Options/Settings.
The image for the current point [marked with '*' on

the gaph or highlighted in the table view] is shown
in a dockable window.

Tooltips also provide point information if the cursor
is positioned over the image. See the figure to the right.
Right clicking on the image displays a pop-up menu

(shown below) which allows images to be adjusted,
saved as jpegs, and played back in sequence.
Selecting Image sequence setup from

the pop-up menu displays the dialog
shown to the right. Use this dialog to
choose the way the picture will be dis-
played and to adjust the image bright-
ness and contrast.

Image Playback
The stored images can be played back in sequence by
selecting Show image sequence from the pop-up menu.
The dialog to the right is displayed. Choose the number
of frames to be shown per second and click OK.
You can also use the slider bar to play an image as shown
in the figure below.
WARNING: After ETC use, do not turn off the

cooling air to the ETC Viewer until the unit has
returned to room temperature. Doing so could
damage the lens assembly and/or camera chip.

Chapter 14
The Electrically Heated Plates (EHP)
Overview
The Electrically Heated Plates (EHP) consist of a high temperature parallel plate and a cone and plate Smart
Swap temperature system. It designed for use with the AR-G2, AR2000ex, and AR 1500ex rheometers. The EHP
is commonly used for the testing of polymer melts. On the AR-G2 the temperature of the upper platen is measured
directly using the Upper Temperature Sensor (UTS). This consists of a special drawrod containing a Pt100
temperature sensor, the information from which is transmitted to a remote reading device.
The Electrically Heated Plates are cooled by air passing through ducts. The air flow is controlled manually. The
EHP includes a heated purge. Operation can be either in air or under nitrogen or other inert gas. A gas purge
cover is provided for operation under inert gas.
An optional low temperature cooling accessory, the Gas Cooling Accessory (GCA), is also available for
temperature control down to -70 C. Click here to access the GCA manual.
Components of the Electrically Heated Plates

The EHP consists of three main Gas Purge Duct
components (see Figure 14.1)
Motor Cooling
An Upper Fixture that attaches Duct
to the rheometer head. This
fixture contains electrical
heating elements, cooling
ducts, and purge duct.
Upper Upper
A Lower Fixture that mounts Fixture Fixture
Cooling Duct
on the rheometer Smart Swap
connector. This fixture Geometry
contains electrical heating Upper Fixture Holder
Heating Element
elements and a cooling duct.
Sample
Geometry
A Geometry Holder that Holder
attaches to the rheometer Lower Fixture Heat Spreader
rotating shaft. The geometry Cooling Duct
holder contains a heat Lower Fixture
spreader. There is no physical Heating Element
contact between this Lower
component and the upper Fixture
Lower Fixture
fixture. For the AR-G2, the Smart Swap
geometry holder is supplied Connector
as a single unit, with a fixed
geometry. For the AR2000ex
and AR 1500ex, the geometry
can be removed from the Figure 14.1
holder. EHP Main Components Schematic

In addition to the three main components, a Manifold, containing flow meters that mounts on the rear of the
rheometer is supplied. The 6-mm outer diameter high temperature tubing required to connect this unit to
the cooling ducts of the upper and lower fixtures is supplied cut to length and with the appropriate connectors
attached.
WARNING: Do not use any tubing other than that provided by TA Instruments to
connect the bracket to the upper and lower fixtures. If replacement tubing is required,
please contact your local TA Instruments' representative or service engineer.
ATTENTION: Ne pas utiliser de tuyaux autrement que que fourni par TA Instruments
pour connecter le crochet aux accessoires suprieurs et plus bas. Si les tuyaux de
remplacement sont exigs, s'il vous plat contacter votre reprsentant des TA
Instruments local ou l'ingnieur de service.
Heating of the EHP is through the electrical elements in the upper and lower fixtures. Cooling is provided
by air carried in the coolant ducts. The air flow rate is manually controlled.
The temperature of the lower fixture is read by a Pt100 probe placed close to the surface of the lower plate,
and in close thermal contact with it.

Installing the Electrically Heated Plates
The steps needed to attach the EHP to the rheometer involve the following:
Mounting and connecting the manifold

Mounting and connecting the upper and lower fixture
Attaching the geometry holder
Attaching the purge gas cover
The following topics are also covered in this section:
Removing the geometry holder

Removing the purge gas cover
Mounting and Connecting the Manifold

Follow these instructions to install the EHP manifold:
1. Ensure that the main air supply is

turned off and depressurized.
Motor
Cooling Gas
2. Mount the manifold on the rear Outlet Purge
of the rheometer using the four Outlet
crosshead screws provided (see
Figure 14.2).
Crash Cool
A schematic of the main air and Upper
purge gas inlet connections to the Outlet
rheometer and manifold is shown
in Figure 14.3 on the next page.
Refer to the schematic for the
remaining instructions.
Crash Cool
3. Disconnect the main air supply Lower
Outlet
from the instrument filter regula-
tor system, and attach the 8-mm
'Y' piece provided to the main air
line.
Crash Cool Motor Gas Purge
4. Connect one branch of the 'Y' Inlet Cooling Inlet
piece to the filter regulator system Inlet
using the 8-mm outer diameter Figure 14.2
white/natural tubing provided.
Electrically Heated Plates Manifold
5. Insert the 8-mm to 6-mm reducer
into the second branch of the 'Y' piece. Then connect this to the 6-mm 'Y' piece using the 6-mm outer
diameter white/natural nylon tubing.
6. Connect one branch of the 6-mm 'Y' piece to the Crash Cool inlet port on the manifold using the 6-mm
outer diameter white/natural nylon tubing.

This is used to isolate the manifold
if you want to remove it.
"Y" Pieces
Crash Cool
On/Off (6 mm)
Valve Gas Purge
(6 mm)
Motor Cooling
Reducer (6 mm)
Main Air In
(8 mm)
Filter
Regulator
Instrument
Bearing
(8 mm)
Figure 14.3
Schematic of Air and Gas Purge from
the Manifold to the Rheometer
7. Connect the other branch of the 'Y' piece to the motor cooling inlet port on the manifold using the
6-mm outer diameter white/natural nylon tubing.
NOTE: The Motor Cooling inlet and outlet, and Gas Purge inlet connectors are Swagelok
fittings that you will need to install. Information on the correct procedure for this is given on
the Swagelok company website at www.swagelok.com.
8. If inert gas is required, connect the gas purge supply to the gas purge inlet on the manifold using the
6- mm outer diameter white/natural tubing. The purge gas should be nitrogen or other inert gas used
to prevent oxidation of the sample by contact with air. The maximum pressure for the purge gas is
100 psi (6.9 bar).

Mounting and Connecting the Upper and Lower Fixtures
Followtheinstructionsbelowtoinstalltheupperandlowerfixturesontherheometer.RefertoFigure14.4,
whichshowstheupperandlowerfixturesmounted,forreference.
1. Ensurethattherheometeristurnedon.Raisetheheadtothemaximum(usetheHeadUPbuttonlocated
ontheinstrumentcontrolpanel)
2. Attachtheupperfixturetothemountingringontheundersideoftheinstrumenthead,usingthethree
captivescrews
provided.Note
thatthepower
cableshouldproj
ecttotherightof
theinstrument
whenviewedfrom
thefront.
3. Mountthelower
fixtureontherhe
ometerusingthe
SmartConnection
asdescribedin
Chapter5ofthis
manual.
4. Connecttheupper
andlowerfixture
cablestotheright Figure 14.4
andleftsockets
Upper and Lower Fixtures Mounted
respectivelyonthe
SmartSwapEHP Gas Purge Cover Up (Left)
adaptor.For Gas Purge Cover Down (Right)
propersystem
identification,itisimportantthatthisstepbecompletedbeforestep5.
Connector to
Smart Swap
Socket 5. ConnecttheSmart
SwapEHPadaptorto
theSmartSwapsocket
Connector to
(seeFigure14.5).
Connector to Upper Fixture
Lower Fixture
Figure 14.5
Smart Swap Adaptor Connections

A schematic of the cooling air and gas purge
outlet connections from the manifold is shown
in Figure 14.6 to the right.
Motor Cooling Gas Purge
6. Remove the plugs from the connectors on

the cooling ducts. Crash Cool Upper
Crash Cool Lower
7. Connect the motor cooling and Crash Cool

upper and gas purge outlets on the mani-
fold to the appropriate inlets on the upper
fixture, using the fittings provided. (See
Figure 14.7 below.)
Figure 14.6
Schematic of Cooling Air and Gas Purge Outlets
from Upper and Lower Fixtures
Gas Purge Inlet 8. Connect the crash cool upper

Motor Cooling exhaust pipe (Figure 14.8) and lower
Exhaust exhaust pipe to the crash cool upper
Crash Cool
Upper Inlet and lower outlets respectively, using
the compression fittings provided.
Ensure that the pipes are pointing
away from the flexible tubing.
Motor Cooling
Crash Cool
Inlet
Upper Exhaust
Figure 14.8:
Crash Cool Crash Cool Upper Exhaust Pipe
Crash Cool
Lower Exhaust
Lower Inlet
Figure 14.7
Cooling Air and Purge Gas Connections
to the Upper and Lower Fixtures

Attaching the Geometry Holder
The geometry holder and geometry holder spanner are shown in Figure 14.9. The holder used with the
AR-G2 is a single piece, with fixed geometry. The holder used with the AR 2000ex and AR 1500ex has a
removable geometry.
Machined Flats
Geometry Heat Spreader
Figure 14.9
Geometry Holder (Left) and Geometry Holder Spanner (Right)
Follow the instructions below to install the geometry holder onto the rheometer:
1. Ensure that the rheometer is turned on. Raise the head to the maximum (use the Head UP button located
on the instrument control panel)
2. For the AR2000ex and AR 1500ex Only: Attach the geometry to the holder and tighten using the geometry
holder spanner.
3. Carefully insert and position the holder within the Upper Fixture, and connect it to the instrument shaft
by rotating the drawrod.
4. Tighten the geometry holder by grasping it on the machined flats at the base of the heat spreader with the
geometry holder spanner, and rotating the drawrod.
Removing the Geometry Holder

Follow the instructions below to remove the geometry holder:
1. Ensure that the rheometer is turned on. Raise the head to the maximum (use the Head UP button located
on the instrument control panel).
2. Grasp the geometry holder on the machined flats at the base, and unscrew from the instrument shaft by
rotating the drawrod.
3. Lower the geometry holder carefully until it is clear of the upper fixture, and remove from the rheometer.

Attaching and Removing the Purge Gas Cover
The purge gas cover is shown in Figure 14.10. The cover fixing tool is shown
in Figure 14.11. The fixing tool should always be used to handle the hot cover.
Follow the instructions below to install the purge gas cover:
Figure 14.11 Figure 14.10.

The Purge Gas Cover Fixing Tool The Purge Gas Cover
1. Raise the instrument head (use the Head UP button

located on the instrument control panel).
2. Use the tool to lift the cover, by engaging with the

slots on the lover cover rim as in Figure 14.12.
CAUTION: Gloves should be worn

when handling the tool as it can get
hot.
3. Slide the cover over the upper fixture, engaging the

bayonet fittings on the cover with the lugs on the
upper fixture.
Hold Here
Figure 14.12
Using the Purge Gas Cover Fixing Tool
4. Twist the cover to hold in place and remove the fixing

tool. The cover is now in the up position as shown in
Figure 14.13 to the left.
NOTE: The fitting tool may not fit if the

temperature difference between the cover
and the tool is too large. In that case, cool
the UHP before attempting to remove the
cover.
Figure 14.13
Purge Gas Cover in Up Position

Running Experiments Using the Purge Gas
Cover
While an experimental procedure is running, the cover should be
in the DOWN position as shown in Figure 14.14.
To lower the purge gas cover, twist the fitting tool, slightly to
disengage from the lugs on the upper fixture, and lowering. The
cover should sit squarely on the rim on the lower fixture.
Remove the fixing tool after loweing the cover.
Removing the Purge Gas Cover

Follow these instructions to remove the purge gas cover:
1. Raise the instrument head (use the Head UP button located Figure 14.14
on the instrument control panel). Gas Purge Cover in Down Position
2. Lower the cover using the fitting tool, and bring it clear of the
instrument upper and lower fixtures.
The View Cover

An optional extra for the EHP is the View Cover shown in
Figure 14.15. This is designed to allow the sample to be seen
by the user, and replaces the Purge Gas Cover. The View Cover
can also be used with nitrogen or other inert gas. To attach
and remove the View Cover, use the same procedure as that
used for Purge Gas Cover.
NOTE: The View Cover should not be used

above 300C
Figure 14.15
The View Cover
Shown in Place on the EHP

Setting the Gas Flow Rates
The Electrically Heated Plates cooling and purge gas flow rates are operated manually. The regulators and
flow metres are mounted on the sides of the manifold (Figure 14.16). The gas purge regulator and flow meter
are on the left of the manifold, the motor cooling regulator and flow meter, and the crash cool regulator are
mounted on the right of the manifold, when viewed from the front.
Gas Purge
Flow Meter Motor Cooling
Flow Meter
Crash Cool
Regulator
Gas Purge
Regulator
Motor Cooling
Regulator
Figure 14.16
Manifold Left and Right Side Views
Follow these guidelines when setting the gas flow rates:
If required, use the purge gas regulator to set the purge gas flow rate to a maximum of 5 liters per minute
(lpm).
It is only necessary to use the motor cooling when the temperature of the EHP is greater than 250C, in
which case the gas flow rate should be set to 10 lpm.
Use the crash cool regulator, if rapid cooling of the EHP is required.
NOTE: When using the EHP, avoid contaminating the mating surfaces of the cover and Upper
and Lower Fixtures with sample, since this may impede removal of the cover."

EHP Temperature Calibration Factors
Platinum Resistance Thermometers (PRT's) are located in the lower pedestal, upper jacket assembly, and Upper
Temperature Sensor (UTS) (This applies to the AR-G2 with standard plates only). Depending on your config-
uration, it may be necessary to enter calibration factors into the Rheology Advantage instrument control
software.
AR-G2 with Standard Plates

The PRT's in the EHP lower and UTS are uniquely calibrated with a traceable dry block temperature system
during the manufacturing process. These calibration values are stored within the component and are used
automatically by the system. You will not need to enter these values.
AR-G2 with Disposable Plates/AR2000/AR2000ex/AR

1500ex
Without the UTS, the temperature of the upper plate can only be inferred by calibration, using a zero heat flow
sensor that matches the calibrated PRT in the EHP lower with the PRT in the upper jacket assembly. This
calibration is carried out during the manufacturing process and the calibration factors are supplied on a certificate
with every EHP system. To enter these factors follow the instructions on the certificate.
NOTE: If you also have an AR-G2 with standard plates, the system will automatically configure
itself when you change between the two configurations.

Chapter 15
Asphalt Submersion Cell
This temperature control system is specifically for the measurement of asphalt binders. Its operation is covered
by the Asphalt Submersion Cell manual.
Click here to open the manual for the Asphalt Submersion Cell.

Chapter 16
Curing Accessory
TA Instruments has developed a Curing Accessory, designed to be used with the AR-G2 and AR2000ex
rheometers. The information needed for this accessory can be found in separate document.
Click here to open the manual for the AR Series Curing Accessory manual.

Chapter 17
Small Angle Light-Scattering Accessory
TA Instruments has developed a Small Angle Light-Scattering (SALS) Accessory, designed to be used with the
AR-G2 and AR2000ex rheometers. The information needed for this accessory can be found in separate document.
Click here to open the manual for the AR Series Small Angle Light Scattering
Accessory manual.

Chapter 18
The Measuring Systems
Overview
This chapter describes the measuring systems currently available from TA Instruments, and provides guidelines
for making the appropriate choice for each application. The advantages and disadvantages of each system are
discussed, and typical examples of its use are given. The working equations for each system are also provided.
General Description
A measuring system is defined as those components of the instrument that are in direct contact with the sample.
It consists of two parts:
A fixed member (or stator), for example the Peltier plate.
A geometry (or rotor), which is attached to the rheometer spindle, where it is locked in position using the
draw rod. The draw rod is detachable, and passes through a hole bored in the spindle. The geometry
constitutes the moving member of the measuring system.
There are four general types of measuring system:
cone and plate

parallel plate
concentric cylinders, either single or double gap
torsional rectangular.
For each, the dimensions can be chosen to provide the optimum working ranges of strain or strain rate, and stress.
Measuring System Factors

The rheometer operating variables are angular displacement, angular velocity, torque and normal force, and
factors are required to convert from these to the sample variables, shear strain, shear rate, shear stress and normal
stress respectively. The factors will depend on the type and dimensions of the measuring system used.

Thus: = F = F = F M and N = FN Fz
Where F is the shear strain factor, F is the shear rate factor, F is the shear stress factor and FN is the normal
force factor. Since F = F this factor is not reported in Rheology Advantage, and is not listed below. The
measuring system factor, Fm, reported in Rheology Advantage, is defined by Fm = F /F . For the derivation
of these factors, and the conditions assumed see R.W. Whorlow "Rheological Techniques", 2nd edition, Ellis
Horwood, 1992. The density factor, F, quoted in Rheology Advantage refers to a small correction made in the
software for sample inertia.

For non-standard measuring systems, the factors can be entered manually. If no information is available on
the density factor, set this to 10-18 m5, i.e. too low for the sample inertia correction to be effective.
Geometry Materials
Standard geometries for the rheometers are constructed from stainless steel, hard anodized aluminium,
titanium or acrylic (polymethyl methacrylate).
NOTE: This applies only to the face of the geometry in direct contact with the sample, the
shaft may be constructed from other materials.
Other materials may be available on request, at additional charge. The geometry should be as low in density
possible, to minimize its moment of inertia, it should be chemically resistant to the sample, and it should have
a surface texture that provides adhesion to the sample, to eliminate slippage.
Stainless Steel
The density of stainless steel is about 8000 kg m-3. The chemical resistance of stainless steel is very good to
most sample materials and it is very durable. This is usually the material of choice, if nothing is known about
the sample.
Hard Anodized Aluminium

The density of hard anodized aluminum is about 2700 kg m-3. The chemical resistance is good to most materials.
The anodizing increases the durability of the geometry, but aluminium is still less durable than stainless steel.
Titanium
Density about 4500 kg m-3. Chemical resistance good to most sample materials. Less durable than stainless
steel. Relatively expensive.
Acrylic
Density about 1200 kg m-3. Chemical resistance poor to many organic materials. Should not be used above
40C. Not available for use with the AR-G2.
For further information on the materials used, see Appendix E.

Cone and Plate
Temperature Systems
The cone and plate can be used with the Peltier Plate, Upper Heated Plate (UHP), Environmental Test Chamber
(ETC), and Electrically Heated Plates temperature systems.
Description
A schematic of the cone and plate measuring system is shown in Figure 16.1. The stator is a flat plate, the rotor
is an inverted cone with a conical angle, < 4. The cone and plate are arranged to be parallel, in principle with
the tip of the cone in the plane of the plate. However, to avoid contact between the cone and the plate, and to
prevent damage to either, the cone is truncated, i.e the tip is removed, and the gap should be set at the truncation
distance, that is with the virtual cone tip in the plane of the plate.
The conical angle and truncation of each cone are individually calibrated. These values and the serial number
are inscribed on the geometry stem, and a calibration certificate containing the values is also supplied with this
type of geometry.
Figure 18.1. Cone and Plate Measuring System Showing Correct Filling
The sample should form a section of a sphere with its centre at the virtual apex of the cone. The gap should be
set at the truncation distance, T.

Filling
Correct filling of the cone and plate is with the sample forming a section of a sphere with its center at the virtual
apex of the cone, and with radius equal to the slant edge of the cone. In practice, this filling is difficult to achieve,
but since the conical angle is small, the error produced by trimming the sample edge to be flush with the rim of
the cone will usually be insignificant. Other methods of filling are described later in this manual.
For the cone and plate geometry N corresponds to first normal stress difference, N1.

Parallel Plate
Temperature Systems
The parallel plate can be used with
the Peltier Plate, Upper Heated
Plate (UHP), Environmental Test
Chamber (ETC), and Electrically
Heater Plates temperature sys-
tems.
Description
A schematic of the parallel plate
measuring system is shown in Fig-
ure 16.2. The stator is a flat plate,
the rotor is a circular flat plate. The
two plates are arranged to be par-
allel. In principle the gap between
the plates can be any distance, but
in practice it is recommended that
the gap should not be less than 1% Figure 18.2.
of the plate diameter, nor too large Parallel Plate Measuring System Showing Correct Filling
to support the sample.
The sample edge should be flush with the rim of the plate
Filling
The correct filling of the parallel plate is with the sample forming a disc with its edge flush with the rim of the
plate. This filling is usually best achieved by preformed the sample into a correctly sized disc, or by overfilling
slightly and trimming.

For the parallel plate geometry, the shear rate (or shear strain) experienced by the sample varies with radial
position. The expressions given here, and used in Rheology Advantage, refer to the maximum shear rate (or
shear strain), which occurs at the geometry rim. The exact expression for the shear stress factor is:
It is this expression, which is used for the stress correction transformation function in Rheology Advantage Data
Module. It reduces to the uncorrected expression for F given above when d ln M / d ln = 1, i.e., in the case of
a Newtonian sample. The measuring system factor, Fm, given above, is likewise exact for a linear viscoelastic
sample.
For the parallel plate geometry N is the first normal stress function, N1, minus the second normal stress function,
N2. The expression given above is an approximation, which is exact in the case where the normal force Fz does
not change with shear rate. For the general case:
This factor is used for the stress correction transformation function in the Rheology Advantage Data Module.

Concentric Cylinders
Temperature Systems
Single gap concentric cylinders are with the Peltier
Concentric Cylinder and Pressure Cell temperature
systems.
Description
A schematic of the concentric cylinder system, or
cup and bob, is shown in Figure 16.3. The sample is
located in the annular gap between two coaxial
cylinders, the outer of which (the cup) is the stator,
the inner (the bob) being the rotor (the Couette
system). Several types of rotor are available, includ-
ing the vane in which the inner cylinder is taken as
the volume swept out by the vane during a complete
rotation.
Filling
The recommended filling according to DIN 53019
part 1 (1980), is with the distance of between the Figure 18.3
upper edge of the rotor and the sample surface equal Concentric Cylinder System Showing Correct Filling
to or greater than the radius of the rotor. This rec- For DIN 53019 Part 1, L1 = L2 = R1
ommendation can only be applied to the Peltier
concentric cylinder system. For details on filling the
Pressure Cell, see Chapter 9.
When concentric cylinders are used, information on normal stresses cannot be obtained.

Double Gap Concentric Cylinders
Temperature Systems
Double gap concentric cylinders can
only be used with the Peltier Concentric
Cylinder temperature system.
Description
A schematic of the double gap concen-
tric cylinder system is shown in Figure
16.4. The system differs from the stan-
dard single gap system in that the rotor
is uncapped and hollow, and the stator
has an inner and an outer wall. There
are thus two annular gaps, and the shear
stress factor is lower than that of the
single gap system, which means that
lower shear stresses can be achieved.
Filling
To enable filling to the correct depth, the
stator contains a well within the inner
wall. Correct filling is the top of the
inner wall, which is best achieved by
allowing the sample to overflow into
the well.
Measuring System
Figure18.4
Factors Double Gap Concentric Cylinder System Showing Correct Filling
When the double gap system is used, information on normal stresses cannot be obtained.

Solid Sample (Rectangular)
Temperature Systems
Rectangular solid samples can be used with the Environmental Test Chamber (ETC), or with the Peltier concentric
cylinder system submersion clamps.
Description
Solid or rubbery samples are preformed into rectangular bars and clamped with their long axis coaxial with the
rheometer spindle (Figure 14.5). The ETC is used for samples to be run in air or inert gas; for submersion in
water or aqueous solutions, a submersion cell is available for use with the Peltier concentric cylinder jacket.
Loading
For information on sample loading for the ETC, see the Rheology Advantage Help System. Although the samples
used with the submersion clamps have the same dimensional ranges as those used with the standard ETC solid
sample clamps, the same loading procedure canno t be used, because the clamping nuts cannot be tightened
when the sample is in place in the cup. For this reason, the sample must be mounted in the clamps before being
introduced to the cup. This means that, unlike those of the standard ETC, the upper and lower clamps of the
submersion cell need to be aligned as part of the sample loading procedure. To allow this, the base of the
submersion cup, which has the lower clamps integrally mounted, is removable and can be located centrally on
top of the submersion cup. For Gap setting and sample loading using the submersion clamps, follow the
instructions given in the Wizards. The sample loading Wizard is activated on the Geometry Dimensions
window.
Working Equations
Although samples of rectangular cross section under torsional deformation are commonly used in rheology, the
stress and strain analysis for this system is not straightforward. The solution depends on the sample end
conditions, and the degree of warping in the sample that these permit [S.P. Timoshenko and J.N. Goodier, Theory
of Elasticity, 3rd edition, McGraw-Hill, 1970]. Some analyses assume that the sample ends are constrained, and
that the sample is not free to warp [C.L.M.H. Navier, Rsum de Leons sur l'Application del la Mcanique, 3rd
edition, 1864]. An exact solution for these conditions is not available, although an approximation is included in
Rheology Advantage as Approximation 1.
Other analyses assume that the sample ends are unconstrained, and the exact solution for these conditions has
been derived [S.P. Timoshenko, Theory of Elasticity, McGraw-Hill, 1934]. This solution has terms in hyperbolic
cosines and tangents, which can be expressed as infinite series. The series converge sufficiently rapidly for the
exact solution to be derivable using modern computers, and it is therefore included in Rheology Advantage.
However, for computational ease various approximations have been used in the past, some of which have
acquired status through usage. One of these is included in Rheology Advantage as Approximation 2 [R.J. Roark,
Formulas for Stress and Strain 4th edition, McGraw-Hill, 1965]. This is the approximation used in TA Instruments
Orchestrator software
The three alternatives will give values for the sample modulus, |G*()|, which differ by no more than a few
percent, although differences in the values returned for the stress and strain may be greater. The phase angle,
, will not be affected.

The factors for rectangular solid samples all have the form of:
But the expressions for A and B are different for the three cases. For solid rectangular samples, information on
normal stresses cannot be obtained.
Exact Equation
Approximation 1 (RA versions 1 to 4)
Approximation 2

Choosing the Best Measuring System
Before selecting the measuring system to use, it is important to consider the purpose of the experiment, the
nature of the sample, and the conditions under which the experiment is to be performed. The AR-G2/AR 2000ex
is adaptable for many more operations than are likely to be needed. It is wise to have some ideaof the information
required from your experiments.
For example, consider the following items:
Choose the type of experiment do you wish to carry out: steady shear, oscillation, creep, or stress relaxation.
Consider the required stress, strain shear rate or frequency ranges, and temperature.
Determine the sample type: low or high viscosity, low or high modulus, possessing particulates, chemically
aggressive, likely to show slippage or solvent evaporation, etc.
Sometimes not all answers to these questions are known, although the guidelines given below should help. But
remember that the rheological properties of the sample are independent of the measuring system used. Good
selection is required to obtain the best possible quality data, and to eliminate errors such as slippage and solvent
evaporation. The standard geometries supplied by TA Instruments will cover almost all eventualities, although
other materials or dimensions can be provided on request.
Cone and Plate and Parallel Plate

These both use relatively small sample volumes, are low in inertia, easy to clean, and can potentially achieve
high shear rates. They can be used with most samples, are easy to set up and use, so are usually the choice to
obtain the best possible data. They are also available in various sizes, so it is important to know how to choose
the geometry with the correct dimensions.
The main advantage of the cone and plate is that the shear rate is uniform throughout the sample. This makes
the geometry suited to measuring the non-linear properties of samples, such as the viscosity of non-Newtonian
fluids. It is also favored because the first normal stress difference can be directly obtained from the measured
normal force, as there is no contribution from the second normal stress function, N2.
A disadvantage of the system is that the gap between the cone and plate cannot be varied, so the shear rate factor
for each geometry is fixed. The surface of the cone is difficult to texture by serration or grit blasting to eliminate
slippage between the sample and the geometry surface.
Cone and plate systems are generally used for low to medium viscosity homogenous samples, or samples with
sub-micron sized particles. They are not recommended for samples containing larger particles, since these may
migrate to the apex of the cone, and become jammed in the truncation area, producing misleading results. The
measuring system is only recommended for experiments conducted isothermally.
The parallel plate system has the advantage over the cone and plate that the gap between the plates can be
varied, and it can therefore be used with samples containing larger particles. A good rule of thumb is that the
gap size should be at least ten times as large as the maximum particle size.
The main disadvantage of the parallel plate is that the shear rate varies across the plate, from zero in the center
to a maximum at the rim. The strain and shear rate reported by Rheology Advantage software are those at the
rim. The reported stress assumes that the sample is Newtonian or linearly viscoelastic, so this measuring system

is also recommended for oscillatory experiments conducted within the sample's linear viscoelastic regime, for
which the reported material functions are exact. But to obtain exact values for the viscosity of non-Newtonian
samples, the correction described above must be used.
Although there is no theoretical minimum to the usable geometry gap, in practice any slight lack of parallelism
between the plates will result in a measurement error which increases as the gap is reduced. For this reason,
the minimum usable gap is often taken to be 1% of the geometry diameter. The maximum usable gap will
depend on the properties of the sample, but remember, if the Peltier plate is used at large gaps, temperature
gradients across the sample may result. This effect is eliminated if the UHP, EHP, or ETC are used.
To eliminate wall slippage, the geometry can be serrated or roughened by grit blasting (stainless steel only).
Usually a similarly textured cover plate is used in conjunction with geometries finished in this way.
To reduce solvent evaporation, cones and plates may be used with the solvent trap cover described inthis
manual.
Angles
Cones are provided in angles of 0.5, 1.0, 2.0 and 4.0. The 4.0 is the largest available because assumptions
in the theory used to calculate the materials properties do not hold for larger angles. The greater the angle (or
gap, if a parallel plate is used), the lower the shear rate factor, so the lower the shear rate for a particular
angular velocity. This means that a large angle (or gap) is better suited to low strain or shear rate measurements,
for example in creep or oscillate, whereas a larger angle or gap is better suited to high shear rate measurements.
The 2.0 cone is often the best starting point for an unknown sample
Diameters
The smaller the diameter of the cone or parallel plate, the larger the shear stress factor. This means that the
higher the modulus or viscosity of the sample, the smaller the diameter should be. For the plate, although not
the cone, the shear rate factor also depends on the diameter, and the larger the diameter, the higher the shear
rate. The 40- mm diameter cone or plate is suited to most purposes, and is a good starting choice for an unknown
sample.
Curing Systems
For curing systems, the ETC disposable plates should be used.
The concentric cylinder (or cup-and-bob) measuring system is normally used for low viscosity samples that
may not be held in the gap, if a cone or plate parallel plate were used. It is also used for samples that show
phase separation under gravity. Wall slippage can be eliminated using the standard vane, and for samples
containing large particles, the wide gap vane can be used. For some samples it is relatively easy to guard
against solvent loss when concentric cylinders are used.
The drawbacks of the concentric cylinders are the relatively large sample size, the difficulty of loading the
sample without excessively shearing it, and the presence of end-effects. The measuring system is not suited
to high viscosity samples.
Rotors available for use with the Peltier concentric cylinder system are the Standard Size DIN (conforms to
DIN 53019), Recessed End, Double Gap, Standard Vane and Wide Gap vane.

The DIN rotor is the standard for use with the concentric cylinder system, and is used with the standard
cup. The recessed end rotor has the same effective dimensions as the DIN, but is designed to reduce end
effects by trapping a bubble of air below the rotor.
The double gap rotor is designed to provide a larger surface area than the standard single gap. This reduces
the value of F, and lowers the minimum shear stress. The problem of sample loading is particularly
marked for the double gap system and, for some samples, it may be impossible to fill the annulus fully.
The double gap cylinder is used with a corresponding cup.
The standard vane rotor is used to eliminate wall slippage and the wide gap vane for samples containing
large particles. The grooved cup is recommended for use with the vane rotors.
To reduce solvent evaporation, the concentric cylinders may be used with the solvent trap cover.
For the concentric cylinder system, the shear stress and, hence, the shear rate, varies across the annulus.
The effect on the reported viscosity is small for all the concentric cylinder systems provided by TA
Instruments except the wide-gap vane.
Solid Sample Rectangular

Solid samples are usually formed as rectangular bars and are run using the ETC or, if the sample is required
to be immersed in water or aqueous solution, with the Peltier concentric cylinder submersion clamps. The
sample should be mechanically stable during the test procedure. For polymeric materials this means that
it should be in the glassy or rubbery phase.

Attaching a Geometry
Theprocedureforattachingageometrytotheinstrumentspindleissimilartothatdescribedforattaching
thebearingclamp:
1. Switchontheairandremovethebearingclampbyturningthedrawrodcounterclockwise(anticlockwise).
2. Pushthegeometryupthespindleandholditwhilelocatingthedrawrodinthescrewthreadofthe
geometry.
3 Screwthedrawrodupwards(clockwise).Itshouldbescrewedfingertightbutnotforced.
Toremovethegeometry,performthisoperationinreverse.
Correcting Geometry Visible Run-out ("Wobble")

AllgeometriespassaQualityControlcheckthatmeasurestheirtotalrunouttobelessthan2thou
(51microns).Visiblerunout,orwobble,ofgeometriesastheyareslowlyrotatedonthedriveshaftisgenerally
causedbydirtonthematingsurfaces,particularlythoseshowninFigure18.5thatcontroltheflatness.
Itisgoodpracticetovisibleinspecttheinteriorshankofthegeometryfordirt,andifnecessarycleanbefore
fitting.Ifyoubelievethereisaproblemwithrunoutthenremovethegeometryandcleanthesurfaces
indicated.
NOTE: The run-out of the knurled knob on the top of the drawrod is not a concern, as it has
no impact on the run-out of the geometry.
Figure 18.5 Areas to Inspect on Geometry

Chapter 19
Extensional Fixture
This section will be made available by TAUpdate as soon as it is complete.

Meanwhile, please contact your TA Instruments Rheology Support Specialist for
assistance in using this fixture.

Chapter 20
AR-G2 Smart Swap Geometries
Overview
This chapter describes the Smart Swap geometries, which are an extension
of the Smart Swap technology. These geometries can be automatically iden-
tified when installed on the AR-G2 rheometer. (Note: This option is not
available for the AR 2000ex or AR 1500ex.) The magnetic strip on the head
of each geometry provides the information that will uniquely identify it to
the instrument. These geometries are resistant to changes in temperature and
the use of solvents and do not interfere with your experiment in any way.
NOTE: If the magnetic strip becomes damaged during use

and can no longer be read, please contact TA Instruments
for service.
The Smart Swap geometries have a larger diameter than previous geometries,
which is required to record sufficient data (36 bits) around the circumference.
In addition, the geometries have a larger bore to allow a better location surface
and easier cleaning.
Each geometry has a unique six-digit serial number for identification pur-
poses. When the geometry is set up for the first time this number is encoded
into the magnetic strip and a link is established to a geometry file in the instrument control software. The geometry
then becomes "Smart."
When a Smart Swap Geometry is attached to the rheometer, a

sensor registers the attachment and slowly spins the shaft to read
the serial number from the magnetic strip. The geometry file
Sleeve with Magnetic Strip
associated with this serial number is then loaded by the software.
NOTE: Upper Heated Plate geometries cannot be

totally smart as the geometry screws into the heat
spreader. You will be given a list of all UHP
geometries in the database when a heat spreader
is identified.
Geometry Base
The Environmental Test Chamber (ETC) geometries, with the
exception of disposable plates, are available with the Smart Swap
technology.
Previous AR Peltier geometries (with a narrow bore) can be used

with a smart adapter. You will be given a list of all standard
geometries in the database when the adapter is identified.

Using the Smart Swap Geometries
NOTE: Smart Swap geometries can only be used with TA Instruments AR-G2 rheometers.
NOTE: If a Smart Swap geometry loses the ability to be read by the instrument for any reason,
it can still be used manually.
When the AR-G2 rheometer has been installed and configured with the software, the following message will be
displayed as Smart Swap geometry is attached and identified.
The message to the right is displayed if there is no change in

geometry.
The message above is displayed if you checked Options/Set-

tings/Rotational mapping as shown in the figure below.

If the geometry installed is a different
geometry, but one that has been previ-
ously set up, a message will be displayed
to inform you. See the figure to the right.
It will also prompt to invalidate the zero

reference.
The program will also prompt you to map the instrument,

if the option was checked in Options/Settings/Rotational
mapping.
Parallel Plates A Special Case:
Unlike cones, parallel plates do not have unique gaps

associated with them. It is therefore possible to have more
than one geometry file for a given measuring geometry.
To make selection easier, it is suggested that you include the gap in your geometry file name, i.e., 40-mm SST
plate 1000 microns.
If the serial number cannot be read for any reason the following message is displayed.

Reprogramming the Serial Number
An attempt to reprogram the serial number can be made by following these steps.
1. Select Options/Instrument/ID and

click on the Service button the dialog
shown to the right is displayed.
2. Select the Program button. The dia-

log shown below is displayed.
3. Select the Smart swap geometry radio button.

The instrument will attempt to read the existing serial
number and will return a value of 1000, if nothing
can be read.
4. Enter the serial number of the geometry (located on

the geometry shaft, storage box, and certificate) and
then click on Next.
The adapter and UHP shafts are special cases as these cannot be uniquely identified.

The geometry will now be programmed and verified as seen in the figures below.
If the serial number is not already associated with a geometry file in the controller database when the geometry
is read, this link must be established. This is done through the Geometry wizard.
Using the Geometry

Wizard
Based on the currently identified temper-
ature system, a list of new geometries is
presented (see the figure to the right).
NOTE: Check the box

at the bottom of the win-
dow to list all geometry
types.
Using the Geometry wizard will create

the geometry file and establish a link with
the serial number in the database.

Smart Swap geometry recognition can be disabled from Geometry on
the main menu shown in the figure to the right. Once it has been disabled,
geometry files will need to be manually selected.
NOTE: The Smart Swap database can also be main-

tained by selecting Geometry/Smart swap database
maintenance. The dialog shown below will be dis-
played.

Chapter 21
Sources of Error
Overview
In this chapter, some sources of error that may arise when making rheological measurements are described. But
remember that all samples are different, and that the solutions suggested here are for guidance only, and may
not be suitable for your material. If you are running an unknown sample, or one that differs substantially from
those that you are familiar with, it usually helps to try various ways of sample filling, loading and so on. The
key to obtaining good rheological data is to take care at every step: sampling, loading, filling, and running.
Using Fluid Samples

Loading
Avoid shearing the sample excessively during loading. Thixotropic samples may take a considerable time to
recover from shearing, and in some cases are irreversibly shear thinning; their original properties will never be
recovered. To prevent excessive shearing, the geometry gap can be closed at a fixed rate profile, or the gap
closure can be programmed so that a particular normal force is not exceeded.
Gap Closure
The gap closure rate should be as slow as is reasonably possible. Rapid closure can result in the sample
experiencing surprisingly high shear rates. It is usually best to use normal force control during closure; the force
used will depend on the sample. Typical would be about 1 N for a dispersion, about 5 to 10 N for a polymer melt.
Sample Filling
It is important that the sample is filled correctly. The measuring system factors given in this manual apply only
to the correctly filled sample. Either overfilling or underfilling will result in the wrong values for the sample
material properties being returned by Rheology Advantage.
Cone and Plate

The correct gap is at the truncation distance, T, which is inscribed on the shaft of each geometry. For the sample
filling, imagine a sphere centered on the virtual tip of the cone, with a radius equal to the slant length of the
geometry. The sample should be the segment of this sphere contained between the cone and the plate. This
filling can be difficult to achieve in practice, but there are several ways in which a good approximation can be
achieved:
1. Overfill the geometry slightly, send the gap to the truncation distance, then trim the sample flush with the
rim of the geometry. If you find that the sample is underfilled, do not try to add additional sample. It is
always better to raise the instrument head, remove the sample, and begin again.

2. Overfill the geometery slightly, send the gap to the trim gap, htrim, which is a few millimeters greater than
the truncation distance. Trim the sample flush with the rim of the geometry then send the gap to the truncation
distance. The trim gap is calculated from:
htrim = T + [D (tan3) / 3]
where D is the geometry diameter and is the cone angle. Calculated values for the standard geometries
are given in Appendix D.
3 For low viscosity samples only: set the gap to the truncation distance, then gently inject the sample using a
wide-nozzle syringe. It sometimes helps if a constant angular velocity is applied to the geometry during
filling, but beware of shearing the sample excessively: 0.1 rad s-1 is often suitable.
Parallel Plate
The correct fill is with the sample in the form of a disc, with its edge flush with the rim of the geometry. This is
usually easier to achieve than the cone and plate fill, and there are several ways of achieving an almost exact
filling. Methods 1 and 3 described above for the cone and plate can also be used for the parallel plate. If the
sample is underfilled slightly using the parallel plate, unlike cone and plate it may not be necessary to begin the
filling again. The gap can be reduced until the filling is correct.
In addition to the methods used for the cone and plate, some samples can be preformed into a disc of the correct
dimensions.
Reducing Evaporation
Samples containing volatile solvents
can if the solvent evaporates. Use the
solvent trap cover to reduce the rate of
evaporation. The moat on the top of the
geometry should be filled with the
appropriate solvent, and the two
halves of the cover placed such that the
Solvent
rim is partially immersed in the sol-
vent. Ensure that no part of the cover
is in contact with the geometry. If the
solvent trap cover is used with the ser-
rated cover plate, the spacer is required
to ensure that the cover is set at the
correct height.
Figure 21.1
Solvent Trap Cover in Place

Preventing Slippage
Slippage can take two forms. In one case, the lack of adhesion between the sample and the surfaces of the
measuring system produces a form of plug flow. In another type of slippage, a thin layer of depleted samples
occurs at the measuring system wall, resulting in a low apparent viscosity. Both forms of slippage can usually
be overcome by texturing the surfaces of the measuring system. This is normally only done for the parallel
plate stainless steel measuring system.
Parallel Plate Measuring System

When using the parallel plate measuring system, keep in mind the following guidelines to prevent slippage:
Use a rotor and stator with textured surfaces.

When using low viscosity samples, the textured surface should be grit blasted.
NOTE: Serrated (cross-hatched) surfaces are not recommended for low viscosity samples.
When used with the Peltier plate, the geometries described are best used with a similarly textured stainless
steel cover plate. This will affect the thermal characteristics of the Peltier plate so that the full temperature
range and temperature ramp rates may not be attainable.
Concentric Cylinder Measuring System

When using the concentric cylinder measuring system, use a vane rotor and grooved cup to prevent slippage.
Particulate Samples
The cone and plate system is not recommended for samples containing any particles with diameters greater
than ten percent of the cone truncation. Remember that the particle sizes quoted by suppliers are often average
values; there may be some much larger particles present. If in doubt, use a parallel plate, but again observe the
ten percent rule: the gap should be at least ten times the diameter of the largest particle.
Temperature Compensation
A change in temperature will produce a change in the dimensions of the components of the instrument, including
the geometry. The only significant effect of this will be to change the measuring system gap. This can be allowed
for, if the thermal expansion coefficient is known. A correction can be invoked when performing an experiment
under non-isothermal conditions, such as a temperature ramp or sweep.
To minimize the effect of thermal expansion, the geometry gap should be zeroed at the working temperature
for isothermal experiments, or at a temperature in the middle of the range for non-isothermal experiments. The
cone and plate measuring system is not recommended for non-isothermal experiments.
Normal Force Control

To allow for the change in sample dimensions during non-isothermal experiments, constant normal force,
rather than constant gap, conditions can be used. It is usually best to use a zero or slightly compressive (positive)
force.
NOTE: Normal force control cannot be used with the cone and plate measuring system.

Using Solids and Rubbery Materials
This type of sample is usually tested in dynamic mode, using a temperature ramp. As this sample softens,
it will tend to buckle or sag in the clamps. To prevent this a constant normal force should be applied.
The correct procedures for sample loading, and recommendations for normal force conditions are given in
the Rheology Advantage Help System.

Appendix A
Technical Specifications
Overview
This chapter contains the technical specifications for the AR-G2/AR 2000ex/AR 1500ex Rheometer. You can
obtain further information from your local Sales Representative.
AR-G2/AR 2000ex/AR 1500ex Specifications

The following specifications apply to the TA Instruments AR-G2/AR 2000ex/AR 1500ex rheometers.
Table A.1
AR-G2 Rheometer Dimensions
Accessory (Electronics Base)
Width 7.25 in.(18.5 cm)

Height 14.75 in.(37.5 cm)
Depth 17.75 in.(45 cm)
Weight 38.1 lbs(17.3 kg)
Module (Instrument Base)
Width 11.75 in.(30 cm)

Height 26.5 in.(67 cm)
Weight 63.8 lbs(29 kg)
Table A.2
AR-G2 Rheometer Specifications
Supply Voltage 110 230 Vac

Supply Frequency 50 to 60 Hz
Power 1.4 kW
Maximum Torque 200 mNm
Minimum Torque Oscillation CR 0.003 N.m
Minimum Torque Oscillation CS 0.003 N.m
(table continued)

Table A.2 (continued)
AR-G2 Rheometer Specifications
Minimum Torque Steady CR 0.01 N.m

Minimum Torque Steady Shear CR 0.01 N.m
Frequency Range 7.5 E-7 to 628 rad s-1
Angular Velocity Range Controlled Stress: 0 to 300 rad s-1
Controlled Strain: 1.4 E-9 to 300 rad s-1
Angular Displacement Resolution 25 nRad
Step Change in Velocity 7 ms
Step Change in Strain 30 ms
Normal Force Range 0.005 to 50 N
Air supply 2.1 bar (30 PSI)
Table A.3
AR 2000ex/AR 1500ex Rheometer Dimensions
Accessory (Electronics Base)
Width 7.25 in.(18.5 cm)

Height 14.75 in.(37.5 cm)
Module (Instrument Base)
Width 11.75 in.(30 cm)

Height 26.5 in.(67 cm)
Table A.4
AR 2000ex Rheometer Specifications

Power 1.4 kW
Torque Range 0.1 Nm to 200 mNm
Angular Velocity Range Controlled Stress: 0 to 300 Rad s-1
Controlled Strain: 10-8 to 300 Rad s-1
Angular Displacement 40 nRad
Resolution
Minimum Strain 0.00006
Normal Force Range 0.005 to 50 N

Table A.5
AR 1500ex Rheometer Specifications

Power 1.4 kW
Torque Range 0.1 Nm to 150 mNm
Angular Velocity Range Controlled Stress: 0 to 300 Rad s-1
Controlled Strain: 10-7 to 300 Rad s-1
Angular Displacement 40 nRad
Resolution
Minimum Strain 0.00006
Normal Force Range N/A
Table A.6
Peltier Plate System Specifications
Temperature Range
tank & pump -5C to 100C

pumped water supply (20C) -20C to 200C
water at 60C 10C to 200C
water at 40C 0C to 200C
water at 1C -30C to 180C
fluid at -20C -40C to 160C
Typical Ramp Rate 30 C min-1

Ramp Rate (20 to 100 C) 50 C min-1
(100 to 150 C) 25 C min-1
Pt100 Internal Resolution0.01 C
Table A.7
Optional Accessory Specifications for
Environmental Test Chamber Module (ETC)
Temperature Range
No cooling 50C to 600C
LN2 cooling -160C to 600C
Typical Ramp Rate maximum ramp rate up to 60C/min
Internal Resolution 0.02 C

Table A.8
Optional Accessory Specifications for
Peltier Concentric Cylinder System
Temperature range
with tank and pump 0C to 100C
with plumbed water supply -10C to 150C
with fluid at -20C -40C to 100C
Ramp Rate
Cooling 15C/min maximum
Heating 13C/min maximum
Pt100 Internal Resolution 0.01 C
Table A.9
Optional Accessory Specifications for Upper Heated Plate
Temperature range
plumbed water supply (11C) 20C to 150C
low viscosity silicone circulating fluid at -40C -30C to 55C
vortex air cooler -5C to 150C
Ramp rate 15C maximum
Maximum temperature difference between plates 0.1C
Table A.10
Optional Accessory Specifications for Electrically Heated Plate
Temperature Range Ambient to 400C
Maximum Heating Rate 30C/min (uncontrolled)

10C/min (controlled)
Crash Cooling Flow Rate No limits
Purge Gas Flow Rates 5 L/min recommended

(Set the lowest flow below 5 L/min that stops
oxidation. This will reduce noise and residuals
during sensitive creep tests.)

Table A.11
Optional Accessory Specifications for Electrically Heated Plate with GCA
Temperature Range -70 to 400 C
Maximum Heating Rate 30 C/min (uncontrolled)

10 C/min (controlled)
Maximum Cooling Rate -40 C/min (uncontrolled)

10 C/min (controlled)
Purge Gas Flow Rates 5 L/min recommended

(Set the lowest flow below 5 L/min that
stops oxidation. This will reduce noise and
residuals during sensitive creep tests.)

Appendix B
Error & LCD Display Messages
The LCD display on the front of the rheometer electronics box displays useful information and error messages.
Power On Messages
Immediately after power up of the rheometer, the display will show 'Initialising...' After a few seconds this
will change to 'AR-G2 8.xx xx/xx/xx' (x is version dependent). If it does not, there is a problem with the
rheometer.
After a few more seconds, the display will either show 'System test Ok' or 'System test failed Y,' where Y is
an error code as show below:
1 ROM checksum error Either bad firmware or Try reloading firmware, otherwise call
or hardware fault for service.
2 RAM error Hardware fault Call for service.
4 Dual port RAM error Hardware fault Call for service.
40 Battery failure Low battery Sometimes seen the first time the system
is restarted after a firmware upgrade.
Cycles power off then on.
80 Backup RAM error Hardware fault Call for service.
400 Parameter block Either corrupted Call for service.

checksum error internal system
parameters or
hardware fault
Initialising ...
During start up of the rheometer, the following items are shown as initializing:
Electronics
Power board
Instrument
Bearing overspeed
Shown when the rheometer bearing rotation exceeds the specified maximum speed.

Bearing pressure too low
This is displayed if the air supply has been inadvertently switched off while the rheometer was on or if the
supply pressure has dropped below the minimum operating pressure.
Encoder index not found

This message can be displayed if the air bearing is not free to move. This can occur if the air-bearing clamp is
still attached or if the air bearing lock is on. Failing this, there may be a fault on the position encoder.
Nf gauge fault
This message is displayed if an excessive normal force was detected when attempting to zero the normal force
reading. This could be caused by either an excessive force being applied by air bearing/sample/mechanical
interference with ETC or a gauge fault.
Nf temp sensor fault

This message is displayed if there are either faulty normal force temp sensors or, if you have for instance, frozen
the instrument with excessive liquid nitrogen.
Operator stop event

This message is displayed when the Stop button was pressed while the Rheology Advantage software had the
keypad locked. This usually indicates that a test run was in progress and the operator aborted it using the
rheometer stop button.
Power cable fault

This indicates that the Power cable may not be plugged in firmly. See Chapter 5 for connection information.
Signal cable fault

This message indicates that the signal cable may not be plugged in firmly. See Chapter 5 for connection
information.
Temp sys element fault

This message is displayed because the Peltier or heater element has developed a fault.
Temp system environment

There is a configuration problem with the installed temperature control module. I.e., no water to the Peltier,
etc. Re-read the manual to check you have set everything up correctly.

Temp system sensor fault
This message is likely caused by fault/damage to the Pt100 or thermocouple.
Other Messages
Other error messages may be displayed. These are usually indicative of problems with the rheometer that can
only be fixed by a qualified TA Instruments representative.

Appendix C
Symbols and Units
Tables of the variables referred to in this manual and used in Rheology Advantage software are given here,
along with the symbols and units for each variable.
Table C.1
Sample Variables
Variable Symbol Units Units Conversion

(S.I.) (c.g.s) S.I. to c.g.s
Viscosity (steady shear) Pa.s P (poise) x 10

Complex viscosity * Pa.s P (poise) x 10
Dynamic viscosity Pa.s P (poise) x 10
Out-of-phase component of * Pa.s P (poise) x 10
Modulus G Pa dyn cm-2 x 10
Complex modulus G* Pa dyn cm-2 x 10
Storage modulus G Pa dyn cm-2 x 10
Loss modulus G Pa dyn cm-2 x 10
Compliance J Pa-1 cm2 dyn-1 x 10-1
Complex compliance J* Pa-1 cm2 dyn-1 x 10-1
Storage compliance J Pa-1 cm2 dyn-1 x 10-1
Loss compliance J Pa-1 cm2 dyn-1 x 10-1
Phase angle (delta) -
Shear stress Pa dyn cm-2 x 10
Oscillatory stress 0 Pa dyn cm-2 x 10
Shear rate s-1 s-1 -
Shear strain - - -
Shear strain (oscillation) 0 - - -
Normal stress N Pa dyn cm-2 x 10
Normal stress coefficient Pa.s2 dyn sec2 cm-2 x 10
Sample density, fluid or solid kg.m-3 g cm-3 x 10-3

Table C.2
Instrument or Measuring System Variables
Variable Symbol Units Units Conversion

(S.I.) (c.g.s) S.I. to c.g.s
Torque M Nm dyn cm x 107

Oscillatory torque M0 Nm dyn cm x 107
Angular velocity rad s-1 rad s-1 -
Angular displacement rad rad -
Angular displacement
(oscillation) 0 rad rad -
Normal force Fz N gf (gram force) x ~ 102
Angular frequency rad s-1 rad s-1 -
Frequency f Hz Hz -
Raw phase or rad or rad -
Shear stress factor F m-3 cm-3 x 10-6
Shear strain factor F - - -
Shear rate factor F - - -
Measuring system factor Fm m-3 cm-3 x 10-6
Normal force factor FN m-2 cm-2 x 10-4
Fluid density factor F m5 cm5 x 1010
Moment of inertia I kg m2 g cm2 x 107
Geometry radius
(cone and parallel plate) R m cm x 102
Geometry conical angle (cone) -
Measuring system gap
(parallel plate) h m cm x 102
Rotor outer radius
(concentric cylinder) R1 m cm x 102
Stator inner radius
(concentric cylinder) R2 m cm x 102
Stator outer radius
(double concentric cylinder) R1 m cm x 102
Rotor inner radius
Rotor outer radius
Stator inner radius
Cylinder immersed height H m cm x 102
Solid sample length L m cm x 102
Solid sample width W m cm x 102
Solid sample thickness T m cm x 102

Appendix D
Measuring system factors are used to convert from the instrument variables: torque, angular displacement,
angular velocity and normal force, to the sample variables: stress, strain, shear rate and normal stress
respectively.
Thus = F M = F =F and N = FN .Fz
Where F is the shear stress factor, F is the shear strain factor, F is the shear rate factor, and FN is the normal
force factor. Since F = F this factor is not reported in Rheology Advantage, and is not listed below. The measuring
system factor, Fm, reported in Rheology Advantage, is defined by Fm = F / F
For information on the derivation of the factors see R.W. Whorlow, Rheological Techniques, 2nd edition, Ellis
Horwood, 1992.
Cone and Plate

Geometry Dimensions Measuring System Factors (S.I.)*
Diameter Angle Trim Sample Shear Shear Measuring Fluid Normal

Gap Volume Rate Stress System Density Force
mm m mL approx - m-3 m-3 m5 m-2
20 0.5 0 0.02 114.6 4.775E5 4167 3.655E-13 6366

20 1.0 0 0.04 57.29 4.775E5 8333 7.311E-13 6366
20 2.0 0 0.07 28.64 4.775E5 16670 1.462E-12 6366
20 4.0 2 0.15 14.30 4.775E5 33330 2.924E-12 6366
25 0.5 0 0.04 114.6 2.445E5 2133 1.116E-12 4074
25 1.0 0 0.07 57.29 2.445E5 4267 2.231E-12 4074
25 2.0 0 0.14 28.64 2.445E5 8533 4.462E-12 4074
25 4.0 3 0.29 14.30 2.445E5 17070 8.924E-12 4074
40 0.5 0 0.15 114.6 59680 520.8 1.170E-11 1592
40 1.0 0 0.29 57.29 59680 1042 2.339E-11 1592
40 2.0 1 0.59 28.64 59680 2083 4.679E-11 1592
40 4.0 5 1.17 14.30 59680 4167 9.358E-11 1592
60 0.5 0 0.49 114.6 17680 154.3 8.883E-11 707.4
60 1.0 0 0.99 57.29 17680 308.6 1.777E-10 707.4
60 2.0 1 1.97 28.64 17680 617.3 3.553E-10 707.4
60 4.0 7 3.95 14.30 17680 1235 7.106E-10 707.4

Parallel Plate
Geometry Dimensions Measuring System Factors (S.I.)*
Diameter Gap Sample Shear Shear Measuring Fluid Normal

Volume Rate Stress System Density Force
mm m mL approx - m-3 m-3 m5 m-2
8 500 0.03 8.000 9.947E6 1.243E6 6.702E-14 39790

8 1000 0.05 4.000 9.947E6 2.487E6 1.340E-13 39790
12 500 0.06 12.00 2.947E6 2.456E5 3.393E-13 17680
12 1000 0.11 6.000 2.947E6 4.912E5 6.786E-13 17680
20 500 0.16 20.00 6.366E5 31830 2.618E-13 6366
20 1000 0.31 10.00 6.366E5 63660 5.236E-12 6366
25 500 0.25 25.00 3.259E5 13040 6.392E-12 4074
25 1000 0.49 12.50 3.259E5 26080 1.278E-11 4074
40 500 0.63 40.00 79580 1989 4.189E-11 1592
40 1000 1.26 20.00 79580 3979 8.378E-11 1592
60 500 1.41 60.00 23580 393.0 2.121E-10 707.4
60 1000 2.83 30.00 23580 786.0 4.241E-10 707.4
Geometry Dimensions
Rotor type Stator inner Rotor outer Cylinder Gap Sample

radius radius immersed volume
height (approx)
mm m mm mm m mL
Standard size DIN

(conical) 15.00 14.00 42.00 5920 21.26
Recessed end 15.00 14.00 42.00 4000 6.65
Vane (narrow gap) 15.00 14.00 42.00 4000 28.72
Wide gap vane 15.00 7.50 38.00 4000 27.25
Pressure cell 14.00 12.75 44.00 - 10.00
Measuring System Factors (S.I.)*
Rotor type Shear Rate Shear Stress Measuring Fluid Normal

System Density Force
s-1 m-3 m-3 m5 -

Standard size
DIN (conical) 14.52 18090 1246 2.413E-10 -
Recessed end 14.52 18090 1246 2.413E-10 -
Standard size vane 14.52 18090 1246 2.413E-10 -
Wide gap vane 1.667 46540 27920 2.384E-10 -
Pressure cell 10.72 20350 1898 2.385E-10 -

Standard Size Double-Gap Concentric Cylinders
GeometryDimensions
Rotorouter Rotorinner Statorinner Cylinder Gap Sample

radius radius radius immersed volume
height (approx)
mm mm mm mm m mL
17.5 16 15.1 53.00 2000 11.65
MeasuringSystemFactors(S.I.)*
ShearRate ShearStress Measuring Fluid Normal

_ m3 m3 m5
17.29 5313 307.3 1.029E9
Double-Gap Concentric Cylinders Mk1

GeometryDimensions
Rotorouter Rotorinner Statorinner Cylinder Gap Sample

radius radius radius immersed volume
height (approx)
mm mm mm mm m mL
21.96 20.38 20.00 59.50 500 6.48
MeasuringSystemFactors(S.I.)*
ShearRate ShearStress Measuring Fluid Normal

_ m3 m3 m5
53.14 2976 56.01 9.514E10

Interfacial Measuring Systems
GeometryDimensions MeasuringSystemFactors(S.I.)*
Cupor Biconeor Sample Shear Shear Measuring Fluid Normal

DishInner Ring Volume Rate Stress System Density Force
Diameter Diameter (approx.)
mm mm mL m2 m2
80.00 68.00 226 6.207 118.6 19.10

66.00 20.00 50 1.202 868.8 722.8
Solid Sample (Rectangular): Exact

SampleDimensions MeasuringSystemFactors(S.I.)*
Thickness Width Length Shear Shear Measuring Density Normal

Rate Stress System Force
mm mm mm m3 m3 m5
5.00 13.0 50.0 0.09727 1.185E7 1.218E8 2.627E11

2.50 13.0 50.0 0.04998 4.200E7 8.403E8 1.187E11
5.00 6.50 50.0 0.07927 2.755E7 3.475E8 4.553E12
2.50 6.50 50.0 0.04864 9.479E7 1.949E9 1.642E12
5.00 13.0 25.0 0.1945 1.185E7 6.091E7 1.314E11
2.50 13.0 25.0 0.09995 4.200E7 4.201E8 5.933E12
5.00 6.50 25.0 0.1585 2.755E7 1.738E8 2.277E12
2.50 6.50 25.0 0.09727 9.479E7 9.745E8 8.210E13
Solid Sample (Rectangular): Approximation 1


mm mm mm m3 m3 m5
5.00 13.0 50.0 0.1393 1.694E7 1.216E8 2.627E11

2.50 13.0 50.0 0.1324 1.112E8 8.398E8 1.187E11
5.00 6.50 50.0 0.08201 2.839E7 3.461E8 4.553E12
2.50 6.50 50.0 0.06964 1.355E8 1.946E9 1.642E12
5.00 13.0 25.0 0.2786 1.694E7 6.082E7 1.314E11
2.50 13.0 25.0 0.2648 1.112E8 4.199E8 5.933E12
5.00 6.50 25.0 0.1640 2.839E7 1.731E8 2.277E12
2.50 6.50 25.0 0.1393 1.355E8 9.732E8 8.210E13

Solid Sample (Rectangular): Approximation 2

mm mm mm m3 m3 m5
5.00 13.0 50.0 0.09441 1.136E7 1.203E8 2.627E11

2.50 13.0 50.0 0.04930 4.118E7 8.353E8 1.187E11
5.00 6.50 50.0 0.07763 2.698E7 3.476E8 4.553E12
2.50 6.50 50.0 0.04720 9.0888E7 1.925E9 1.642E12
5.00 13.0 25.0 0.1888 1.136E7 6.017E7 1.314E11
2.50 13.0 25.0 0.09860 4.118E7 4.177E8 5.933E12
5.00 6.50 25.0 0.1553 2.698E7 1.738E8 2.277E12
2.50 6.50 25.0 0.09441 9.0888E7 9.627E8 8.210E13
*Conversion of System Factors From S.I. to c.g.s.
SystemFactor S.I.Units C.G.S.Units Conversion(S.I.toc.g.s.)
ShearRate x1
ShearStress m3 cm3 x106
MeasurementSystem m3 cm3 x106
FluidDensity m5 cm5 x1010
NormalForce m2 cm2 x104

Appendix E
Materials List
Materials Used in TA Instruments AR Components

Note that these descriptions apply only to the surfaces of each component in contact with the sample. Other
parts may be constructed from different materials.
Peltier Plate Materials

Geometries
Stainless steel: grade 303-S31 (BS 970)
Aluminium: grade 6082-T6 (BS 1474), hard anodized to BS 5599
Titanium: grade 2 (ASTM B348).
Acrylic: poly(methyl methacrylate).
Plate
Coating: hard chrome plating (BS 4641)
Seal: graphite-filled polytetrafluoroethylene
Concentric Cylinder Materials

Rotors (DIN, recessed end
and double gap): Aluminium grade 6082-T6 (BS 1474), hard anodized to BS 5599
Rotors (vane): Stainless steel grade 303-S31 (BS970)
Immersion cell
sample holder: Stainless steel grade 303-S31 (BS970)
Cup: Aluminium grade 6082-T6 (BS 1474), hard anodized to BS 5599
Cup base (double gap

and immersion cell only): Stainless steel grade 303-S31 (BS970)
Cup base 'O' ring seals: Neoprene

Bicone: Stainless steel grade 303-S31 (BS970)
Cup and lid: Poly(tetrafluoroethylene)
Du Nouy ring: Platinum / iridium (ASTM D971)
Dish: Duran glass (Schott AG)
Pressure Cell
Rotor: Titanium grade 5, 6Al-4V
Cap: Titanium grade 5, 6Al-4V
Cup: Stainless steel grade 316
Shaft: Carbide grade C2
Bearings: Sapphire
O-ring Seals: Kalrez (DuPont Dow Elastomers)
Plug: Brass grade C36000 H02
Thread Sealant: Poly(tetrafluoroethylene) tape
Other Components: Titanium grade 5, 6Al-4V or Stainless steel grade 303, 304 or 316
Starch Cell
Impeller: Torlon 4301 (Solvay Advanced Polymers LLC)
Cup: Aluminium grade 6082-T6 (BS 1474)
Environmental Testing Chamber (ETC)

Geometries: Stainless steel grade 316-S31 (BS 970)
Shield
Shield: polycarbonate, non-UV-stabilised, virgin grade

Index
A
accessory
UV curing 155
air bearing (AR 2000ex) 39
air-bearing clamp 31
Upper Heated Plate (UHP) 65
angular velocity 27
asphalt submersion cell 153
auto gap set facility 44
ball slide 37
bicone 109
bob
attaching 70
cables
connecting 70
calibrating 85
calibration
chemical safety 24
components
materials used 203
computer
connecting to electronics box 33
connecting to electronics control box 33
concentric cylinder system

attaching bob 70
finding zero position 70

installation 69
solid sample submersion clamps 71
concentric cylinders 165
cone and plate 161
constant of proportionality 27
control electronics 123
cooling
controlled 130
Cooling Control Unit (CCU) 51, 102
cryogenic pressure vessel 130
cup
changing 70
depressurizing 89
depth 185
double gap concentric cylinders 166
drag cup motor 29
draw rod 31
inserting 31
Du Noy ring 109, 119

calculation of interfacial viscoelastic properties 122
cleaning 122
loading the sample 121
mapping 121
mounting 120
setting up 120
electrical safety 22
Electrically Heated Plates (EHP)

components 141
Crash Cool outlet 146
Crash Cool upper exhaust pipe 146
gas purge inlet 144
geometry holder 141

installation 143
installing manifold 143
installing upper and lower fixtures 145
lower fixture 141
manifold 142, 146
motor cooling outlet 146
purge gas cover 148
purge gas cover fixing tool 148
running experiments using the purge gas cover 149
setting gas flow rates 150
Smart Swap adaptor 145
upper fixture 141
electronics box
connecting to computer 33
EMC Conformit 21
EMC Conformity 20
Environmental Test Chamber (ETC)
specifications 187
Environmental Test Chamber. See also

ETC 123
Environmental Testing Chamber (ETC)

installing 125
installing the low temperature accessory 128
internal components 15
oven 125
setting up 125
equilibrium time 130
error codes 191

errors 181
ETC
control electronics 123
gas ring 123
heat shield 123
heating chamber 123
thermocouple 123
ETC Viewer
data analysis 138
image controls 137
image playback 140
installation 131
introduction 131
schematics 134
signal/power connector 133
software 136

USB adapter 133
evaporation 182
EVENT socket 59
extensional fixture 173
flow rate 50, 128
fluid cables
connecting 70
fluids
used with the Upper Heated Plate (UHP) 58
gap 44
closing 44
zeroing 44
gap closure rate 181
gap zeroing 44
gas ring 123
geometries 129
geometry
attaching 172
connecting for Upper Heated Plate 60
disconnecting for Upper Heated Plate 60
wizard 179
geometry gap 101
geometry holder 146, 147
geometry holder spanner 147
geometry materials 160
geometry wizard 179
heat shield 123

heating chamber 123
interior 124
height 185
history of rheology 27
Hooke's Law 28
impeller 101
impeller blades 17
inert gas 66
installation 31
location requirements 32
requirements 32
instrument
body 37
cable connections 33
changing the cup 70
components 37
connecting to air 34
connecting to electronics box 33
connecting to water 34
description 27, 29
dimensions 185
error codes 191
installation 31
LCD display messages 191
lifting and carrying 22
materials used 203
motor (AR-G2) 41
normal force transducer 42
optical encoder 41
preparation for installation 31
technical specifications 185
unpacking 31
variables 196
instrument head 29
instrument symbols 13
instrument. See also

rheometer 29
analyzing results 117

bicone 112
zeroing the gap 114
calculation of viscoelastic properties 118
data treatment 113
determining fluid contribution 115
determining interface position 115
experiments 113
geometry details 111
installation 114
interface position
determining 115
rotational mapping 114
set up 114
interfacial analogues 110
interfacial measuring system factors 110
interfacial measuring systems 199

interfacial rheology 109
l'azote liquide 23
lab air 32
LCD display messages 191
lifting and carrying 22
liquid nitrogen 16
handling 24
safety 23
location 32
location of instrument 32
low temperature accessory 128
lower fixtures 145
lower stage 29
magnetic strip 175

magnetically-levitated bearing 38
making connections 88
mapping procedure 130
measuring system factor

cone and plate 197
measuring system factors 197

concentric cylinders 198
conversion 201
double-gap concentric cylinders 199
parallel plate 198
solid sample 200
measuring system variables 196
measuring systems 159

angles 170
choosing 169
concentric cylinders 165, 170
cone and plate 161, 169
curing 170
diameters 170
double gap concentric cylinders 166
factors 159
parallel plate 163, 169
types 159
motor 41
Newton's postulate 27
normal force control 183
normal force factor 197
normal force transducer 42
Notes, Cautions, and Warnings 12
operation
rheometer 130
optical encoder 29, 41
oven 123

P
packaging
removing 31
parallel plate 163
parallel plates 129

cleaning 129
Peltier Concentric Cylinder System

specifications 188
Peltier Plate 49
description 49
Peltier plate
specifications 50
Peltier Plate System
specifications 187
polymers 130
power cable 33
power cables 16
connecting 70
power outlet 32
pressure 128
Pressure Cell
aligning manifold 88
cleaning the cup 94
cleaning the rotor assembly 94
components 75
Concentric Cylinder rotor 77
cup 76
disassembling rotor 95
gauge port 76
inlet port 76
installation 81
installation of cup and rotor 83
installation of manifold 82
loading a sample 86
magnet assembly 78
maintenance 94
manifold 79
operational limits 74
positioning gap 85
pressurizing 89

reassembling rotor 96
replacement parts 98
requirements for external pressure source 80
rotor assembly 77
running experiments in external pressurization mode 92
running experiments in self-pressurization mode 90
safety relief port 77
safety specifications 74
specifications 74
three-way valve 89
purge gas
connecting to rheometer 127
radial air bearings (AR-G2) 40
rectangular solid samples 167
rheometer
additional precautions 129
connecting the purge gas 127
connecting to electronics control box 33
cooling 130
description 15
installation requirements 32
location requirements 32
preparing for installation 31
removing packaging 31
repair 25
thermocouple 130
rheometer. See also

instrument 37
rotational mapping 40
Safety 13
impeller blades 17
toxic gases 17
safety
chemical 24
electrical 22
EMC Conformity 20
warnings 15
sample cover 67
sample filling 181
samples 181
filling 181
fluids 181
particulate 183
preventing slippage 183
reducing evaporation 182
rubbery 184
solid 167
solids 184
temperature compensation 183
thixotropic 181
sensor
for Smart Swap geometries 175
serial number 175, 178
shear rate factor 197
shear strain factor 197

shear stress factor 197
slippage 183
Smart Swap 29, 44

database 180
EHP adaptor 145
geometries 175
serial number 175
serial numbers 178
using 46
Smart Swap geometries

geometry wizard 179
magnetic strip 175
reading 178
using 176
Smart Swap Peltier plate 51
solid sample submersion clamps 71
sources of error 181
specifications 185
AR-G2 185
ETC 187
Peltier concentric cylinder system 188
Peltier plate system 187
starch
testing of 99
Starch Pasting Cell (SPC)

assembling 104
calibrating measuring system 105
components 100
conical rotor 107
cooling 101
Cooling Control Unit (CCU) 101
heating 101
Pt 100 probe 101
sample
cooling 101
temperature control 101
symbols 195
Table of Contents 4
thermal compensation 44
thermocouple 123, 130
thrust bearing 29
units 195
unpacking 31
upper fixtures 145
Upper Heated Plate (UHP)

air-bearing clamp 65
attaching to rheometer 52
calibrating 62
circulating fluids 58
configuring 61
connecting the Cooling Control Unit (CCU) 57
connection configurations 56
coolant inlet 58
coolant outlet 58
cooling water 56
description 51
gas atmosphere 51, 66
geometry holder
disconnecting 60
installing vortex air cooler 54
introduction 51
modeling enabled 61
Pt100 51
sample cover 67
using inert gas atmosphere 66
zero heat flow sensor 64

zero value plug 63
upper stage. See also

geometry 29
using 81
UV curing accessory 155
variables 195
instrument 196
viscosity of the liquid 27
vortex air cooler

installing 54
temperature range 55
warnings
important information 15
water
connecting to rheometer 34
weight 185
width 185
work surface 32
zero heat flow sensor

zero position 70

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AR-G2

Notes, Cautions, and Warnings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12

Chapter 1: Introducing the AR-G2,AR 2000ex, and AR1500ex . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15

Safety and EMC Conformity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20

La sret et EMC Conformit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21

Handling Liquid Nitrogen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24

Maintenance and Repair . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25

Chapter 2: Description of the Instruments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27

The AR-G2, AR 2000ex and AR 1500ex . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29

Chapter 3: Unpacking, Installation, and Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31

Removing the Packaging and Preparing for Installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31

Connecting the System Together . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33

Start-Up and Shut-Down Procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35

Chapter 4: Key Rheometer Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37

Magnetically-Levitated Bearing (AR-G2) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38

Air Bearing (AR 2000ex/AR 1500ex) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39

Radial Air Bearings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40

Normal Force Transducer (AR-G2 and AR 2000ex Only) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42

Auto GapSet Mechanism . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44

Chapter 5: Smart Swap Temperature Systems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45

Using the Smart Swap . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46

Introducing the Peltier Plate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49

Chapter 7: The Upper Heated Plate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51

Introduction to the Upper Heated Plate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51

Attaching the Upper Heated Plate to the Rheometer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52

Calibration of the Upper Heated Plate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62

Clamping the Bearing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65

Using an Inert Gas Atmosphere . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 66

Using the Sample Cover . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 67

Using the UHP for Asphalt Testing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 67

Chapter 8: The Peltier Concentric Cylinders . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69

Setting Up the Concentric Cylinder System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69

Attaching the Bob and Finding the Zero Position . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 70

Changing the Cup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 70

Solid Sample Submersion Clamps . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 71

Chapter 9: The Pressure Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73

Pressure Cell Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 75

Installing and Using the Pressure Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 81

Running Experiments in Self-Pressurization Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 90

Running Experiments in External Pressurization Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 92

Maintaining the Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94

Chapter 10: The Starch Pasting Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 99

System Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 100

Temperature Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 101

Connecting the CCU . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 102

Calibration of the Measuring Sytem Factor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 105

Conical Rotor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 107

Chapter 11: The Interfacial Accessory and Du Noy Ring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 109

Bicone Interfacial Accessory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 112

Analyzing Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 117

The Du Noy Ring (AR-G2 Only) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 119

Chapter 12: The Environmental Test Chamber . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 123

Using the ETC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 125

Chapter 13: The ETC Viewer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 131

Installing the ETC Viewer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 131

Chapter 14: The Electrically Heated Plates (EHP) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 141

Installing the Electrically Heated Plates . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 143

Setting the Gas Flow Rates . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 150

EHP Temperature Calibration Factors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 151

Chapter 15: Asphalt Submersion Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 153

Chapter 16: Curing Accessory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 155

Chapter 17: Small Angle Light Scattering Accessory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 157

Chapter 18: The Measuring Systems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 159

General Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 159

(TA, 2008) AR-G2, AR 2000ex and AR 1500ex Rheometers - Operator's Manual

(TA, 2008) AR-G2, AR 2000ex and AR 1500ex Rheometers - Operator's Manual