TA Instruments AR 2000 Operator's Manual
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TA Instruments AR 2000 Operator's Manual

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AR 2000
Rheometer
Rheometrics Series
Operator's Manual
PN 500106.002 Rev. L
Issued January 2007
1
AR 2000 Operator's Manual

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  • Page 1 AR 2000 Rheometer Rheometrics Series Operator's Manual PN 500106.002 Rev. L Issued January 2007 AR 2000 Operator's Manual...
  • Page 2 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.

  • Page 3: Important: Ta Instruments Manual Supplement

    Please click on the links below to access important information supplemental to this Getting Started Guide: • TA Instruments Trademarks • TA Instruments Patents • Other Trademarks • TA Instruments End-User License Agreement • TA Instruments Offices AR 2000 Operator's Manual...

  • Page 4: Table Of Contents

    If a Person is Burned by Liquid Nitrogen ......................19 Chemical Safety ................................19 Usage Instructions ................................ 20 Maintenance and Repair .............................. 20 Chapter 2: Description of the AR 2000 ........................21 Overview ..................................21 A Brief History of Controlled-Stress Rheometers ....................21 TA Instruments AR Rheometers ..........................22 Schematics of the AR 2000 Rheometer ........................
  • Page 5 Installing the Low Temperature Accessory ......................46 Operating Hints ..............................49 Controlling Cooling ............................49 Low Temperature System Maintenance ....................... 49 General Operating Guidelines ............................. 50 Do ..................................... 50 Do Not ..................................50 Keypad Functionality ..............................51 AR 2000 Operator's Manual...
  • Page 6 Chapter 7: Using the Upper Heated Plate ........................ 67 Introduction to the Upper Heated Plate ........................67 Attaching the Upper Heated Plate to the AR 2000 ....................68 Installing the (Optional) Vortex Air Cooler ......................70 Configurations for the Cooling Water ........................72 Connecting the Cooling Control Unit ......................
  • Page 7 Running Experiments in External Pressurization Mode ..................104 Maintaining the Cell ..............................106 Cleaning the Pressure Cell Cup .......................... 106 Cleaning the Rotor Assembly ..........................106 Disassembling the Rotor ..........................107 Reassembling the Rotor ..........................108 Replacement Parts ............................... 110 AR 2000 Operator's Manual...
  • Page 8 Chapter 9: AR 2000 Interfacial Accessory ......................111 Overview ..................................111 Specifications ................................112 Setting up the Interfacial Accessory .......................... 113 Calibration and Mapping ............................114 Zeroing the Gap ..............................114 Mapping and Other Calibrations ........................114 Experimental Procedure ............................. 115 Determining Each Fluid's Contribution ......................
  • Page 9 Temp system environment ..........................130 Temp system sensor fault ............................ 131 Other Messages ..............................131 Appendix E: TA Instruments ETC Kits ........................133 ETC Torsion Rectangular Kit (543307.901) ....................... 133 ETC Parallel Plate Kit (543306.901) ........................133 ETC Disp. Parallel Plate Kit (543308.901) ......................133 Index .....................................

  • Page 10: Notes, Cautions, And Warnings

    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. AR 2000 Operator's Manual...

  • Page 11: Chapter 1: Introducing The Ar 2000

    This manual relates to all hardware aspects of the AR 2000 Rheometer. For complete information on the operation of the instrument, you may also have to refer to the relevant software manuals supplied with the instrument.
  • Page 12 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.

  • Page 13: Attention

    être à l’origine d’une formation de glace. Cette condensation risque de goutter par terre. Afin d’éviter tout accident dû à un sol glissant, il serait préférable de garder le sol aussi sec que possible. AR 2000 Operator's Manual...
  • Page 14 Lors de toute maintenance, couper l'alimentation. Toute maintenance ou réparation doivent être effectuées par TA Instruments ou un personnel de service qualifié. Cet appareil doit être connecté à la terre. Toute rallonge utilisée avec cet appareil doit comporter une masse de securité.

  • Page 15: 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 2000 has been tested to the following specifications: Safety This equipment has been designed to comply with the following standards on safety: •...

  • Page 16: La Sûreté Et Emc Conformité

    Spécifications Afin de se conformer aux directives du Conseil européen, 73/23/EEC (LVD) et 89/336/EEC (directive d'cEmc), comme modifié par 93/68/EEC; l'Ar 2000 a été testé selon les caractéristiques suivantes: Sûreté Ce matériel a été conçu pour être conforme aux normes de sécurité suivantes: •...

  • Page 17: Lifting And Carrying Instructions

    You should always use two people to lift the instrument. • Treat the AR 2000 with the same degree of care you would take with any scientific laboratory instrument. Electrical Safety Always unplug the instrument before performing any maintenance.

  • Page 18: Liquid Nitrogen Safety

    Wear safety gloves before removing hot or cold geometries. Températures extremes. Lors du fonctionnement, des surfaces extrèmement chaudes ou froides peuvent être exposées. Prendre toutes précautions necessaires telles que l'utilisation de gants de protection avant d'enlever les géométries chaudes ou froides. AR 2000 Operator's Manual...

  • Page 19: Handling Liquid Nitrogen

    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. AR 2000 Operator's Manual...

  • Page 20: Usage Instructions

    Le réglage, le remplacement des pièces, l'entretien et la réparation devraient être effectués exclusivement par le personnel qualifié de TA Instruments. Avant l'ouverture du châssis, débrancher l'instrument. WARNING: The cover should only be removed by authorized personnel. Once the cover has been removed, live parts are accessible.

  • Page 21: Chapter 2: Description Of The Ar 2000

    Chapter 2 Description of the AR 2000 Overview This chapter describes the main components of the rheometer and provides technical information on perfor- mance and design. Please read this chapter thoroughly to become familiar with the nomenclature used throughout this manual.

  • Page 22: Ta Instruments Ar Rheometers

    TA Instruments AR Rheometers The TA Instruments AR Rheometers are fifth-generation instruments that function as either controlled-stress or controlled-rate instruments. The rheometers are designed to fulfill the requirements of measurement as implied by the full meaning of the term rheology—defined as the "study of the deformation and flow of matter."...

  • Page 23: Instrument Components

    Figure 2.4 shows the rear of the electronics control box. The AR 2000 Rheometer contains an electronically- controlled induction motor with an air bearing support for all the rotating parts. The drive motor has a hollow spindle with a detachable draw rod inserted through it.
  • Page 24 AR 2000 Operator's Manual...

  • Page 25: Chapter 3: Technical Descriptions

    Chapter 3 Technical Descriptions Overview In order to fully utilize the advanced capabilities available with the AR 2000 Rheometer, some of the important components require a more detailed explanation. This chapter describes in detail the design and functions of the: •...

  • Page 26: Rotational Mapping

    The microprocessor can allow for these automatically by carrying out a baseline correction of the torque. This results in a very wide bearing operating range, without operator intervention; i.e., a confidence check in bearing performance. Instructions for performing the rotational mapping can be found in the Rheology Advantage™ online help. AR 2000 Operator's Manual...

  • Page 27: Auto Gapset Mechanism

    'automatic gap options' set in the Rheology Advantage software. There are four closure options available with the AR 2000 Rheometer-—Standard, Linear, Exponential, and Normal Force. The options available are described in detail in the online help for the rheology software.

  • Page 28: Smart Swap

    & pump -5°C to 100°C pumped water supply (20°C) -20°C to 200°C water at 60°C 10°C to 200°C water at 40°C 0°C to 200°C water at 1°C -30°C to 180°C fluid at -20°C -40°C to 160°C AR 2000 Operator's Manual...

  • Page 29: Normal Force Transducer

    The AR 2000 Rheometer keeps the upper geometry positioned as accurately as is possible with an air bearing, and movement is kept to an absolute minimum. This ensures good bearing performance.
  • Page 30 AR 2000 Operator's Manual...

  • Page 31: Chapter 4: Technical Specifications

    Chapter 4 Technical Specifications Overview This chapter contains the technical specifications for the AR 2000 Rheometer. You can obtain further informa- tion from your local Sales Representative. Specifications The following specifications apply to the TA Instruments AR 2000 Rheometer: Table 4.1...
  • Page 32 Table 4.2 AR 2000 Rheometer Specifications Angular Displacement 40 nRad Resolution Minimum Strain 0.00006 Normal Force Range 1 g to 5000 g Table 4.3 Peltier Plate System Specifications Temperature Range tank & pump -5°C to 100°C pumped water supply (20°C) -20°C to 200°C...
  • Page 33 Optional Accessory Specifications for Upper Heated Plate Temperature range plumbed water supply (11°C) 20°C to 150° low viscosity silicone circulating fluid at -40°C -30°C to 55°C vortex air cooler -5°C to 150°C Ramp rate 15°C maximum Maximum temperature difference between plates 0.1°C AR 2000 Operator's Manual...
  • Page 34 AR 2000 Operator's Manual...

  • Page 35: Chapter 5: 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.

  • Page 36: Installation Requirements

    Poorly ventilated areas. After you have decided on the location for your instrument, refer to the following sections to unpack and install the AR 2000 Rheometer. NOTE: Internal Fuse: FS1 & FS2 on cmd 069 pcb. It is strongly recommended that the internal fuse be replaced only by trained and skilled TA Instrument personnel.

  • Page 37: Connecting The System Together

    NOTE: You must configure the software for the appropriate communications port—refer to the online help for instructions on how to do this. Vous devez configurer le logiciel en fonction du port de transmissions utilisé—se référer à l'aide fournie dans le logiciel. AR 2000 Operator's Manual...

  • Page 38: Connecting Air And Water To The Rheometer

    Refer to Figure 5.4 on the previous page for information on the location of the relevant connections in the instructions below. 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. AR 2000 Operator's Manual...

  • Page 39: Using Smart Swap

    Press the Release Button Figure 5.5 Fitting the Attachment Connect the power and fluid cables. See Figure 5.6. Figure 5.6 Connecting Power and Fluid Cables When the green status light goes out, the rheometer is ready for use. AR 2000 Operator's Manual...

  • Page 40: Removing The Peltier Plate

    NOTE: The release state will stay active for 10 seconds and then revert to locked. Le dévérouillage restera actif pendant 10 secondes. A l'issue de ces 10 secondes la plaque sera vérouillée automatiquement. Figure 5.8 Removing the Peltier Plate AR 2000 Operator's Manual...

  • Page 41: Setting Up The Concentric Cylinder System

    Figure 5.11 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. Figure 5.11 Connecting Fluid Cables AR 2000 Operator's Manual...

  • Page 42: Changing The Cup

    Undo the two screws on the cup. Turn and lift it out as shown in the figure below. Replace with the required cup size and twist into place. Figure 5.12 Tighten the two screws by hand. Lowering Rheometer Head Figure 5.13 Changing the Cup AR 2000 Operator's Manual...

  • Page 43: Using The Etc

    Connect the two cables on the ETC to the attachment connectors on the rheometer as shown in Figure 5.16. 10. Open the ETC oven doors to gain access to the Smart Swap™ mounting. Figure 5.16 Connecting the Cables AR 2000 Operator's Manual...
  • Page 44 Figure 5.19 Connecting the Cable from the Lower 17. Insert the shorting plug into the Attachment to the Rheometer Event A connection on the rheometer as shown here. AR 2000 Operator's Manual...
  • Page 45 ETC Connections Using Nitrogen as the Agitation Gas 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. AR 2000 Operator's Manual...

  • Page 46: Installing The Low Temperature Accessory

    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. AR 2000 Operator's Manual...
  • Page 47 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 plate—do not apply any force to the ceramic part of the geometry. AR 2000 Operator's Manual...
  • Page 48 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. AR 2000 Operator's Manual...

  • Page 49: Operating Hints

    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 housekeep- ing, maintenance and periodic examination of cryogenic pressure vessels."...

  • Page 50: General Operating Guidelines

    Leave the high temperature system switched on or the nitrogen tank tap open, when not in use. • Attempt to remove a hot geometry without wearing safety gloves. • Forcibly remove a geometry. • Allow any object to obstruct the safety interlock sensors at the rear of the ETC housing. AR 2000 Operator's Manual...

  • Page 51: Keypad Functionality

    To maximize gap zeroing time, you should position the geometry to within 5 mm above the plate before pressing this button. Release Activates the release mechanism for Smart Swap (see previous page for more information). AR 2000 Operator's Manual...

  • Page 52: Levelling The Rheometer

    If all of these actions result in the correct response, you can be confident that you have installed the system correctly and it is ready for use. If you have problems, please contact your local TA Instruments office or their appointed agent.

  • Page 53: Calibrating The Rheometer

    Determine the Newtonian viscosity. If this value is more than 4% different from the certified value, repeat the experiment. If there is still an error, call your local TA Instruments office for advice. There are several sources of operator error that can give erroneous answers. This does not necessarily mean that your instrument is not working properly.

  • Page 54: Cleaning The Filter Regulator Assembly

    Unscrew the filter bowl plug and dry the inside thoroughly. Replace the plug and purge with air before reconnecting to the rheometer. The filter elements must also be replaced when there is a visible buildup of dirt. AR 2000 Operator's Manual...

  • Page 55: Chapter 6: Measuring Systems

    Some theoretical considerations are given that will provide guidance and help you maximize the use of the AR Rheometers. TA Instruments offers a range of geometries. The geometries are divided into the following groups, each with a range of sizes available: •...

  • Page 56: Plastic

    Samples containing particulate matter are usually unsuitable for cone and plate geometries as the particles will tend to migrate to the apex of the cone and will get jammed in the truncation area. Erroneous data will result. AR 2000 Operator's Manual...

  • Page 57: Parallel Plate

    However, the software compensates for this fact. The shear stress and shear rate factors given are with respect to the rim. A schematic of a parallel plate is shown in Figure 6.2. Figure 6.2 The Parallel Plate AR 2000 Operator's Manual...

  • Page 58: Concentric Cylinders

    Vane system. Figure 6.3 Recessed End The shear stress factor is the same as the geometry shown in Figure 6.3. The conical end aids penetra- tion and even distribution of stiffer samples. Figure 6.4 Conical End AR 2000 Operator's Manual...

  • Page 59: Using The Stress And Shear Rate Factors

    Using the Stress and Shear Rate Factors The TA Instruments operating system software calculates the stress and shear rate factors, which are used by the software in all subsequent calculations. However, there may be occasions when you will need to enter these factors manually. If you do, follow the sequence given below: Multiply the angular velocity (ω) by the shear rate factor ( F ) to obtain the shear rate (s...

  • Page 60: Choosing The Best Geometry

    Angles Cones are supplied by TA Instruments in any angle from 0° to 4°, usually in 0.5° increments. The 4° cone is the largest available, as the sample velocity profile becomes unpredictable at higher angles and the math- ematical expression of α...

  • Page 61: Material

    Acrylic geometries are very light and are, therefore, most suitable to use with low viscosity samples. However, you should not use acrylic geometries above 40°C. See the beginning of this chapter for more details on materials. AR 2000 Operator's Manual...

  • Page 62: Preventing Solvent Evaporation

    If you are using samples that contain volatile solvents or are water-based, evaporation can cause problems during measurements. TA Instruments has overcome this problem by using a solvent trap cover, which sits over the geometry (but does not touch it).

  • Page 63: Removing The Air-Bearing Clamp

    Bearing Lock implemented with the Mobius Drive provides the same function without the risk of leaving Figure 6.9 it in place at the start of a measurement. Slide Lock Away AR 2000 Operator's Manual...

  • Page 64: Attaching A Geometry

    Screw the draw rod upwards (clockwise). It should be screwed finger tight, but not forced. To remove the geometry, use the reverse process. Clockwise Counterclockwise (Anticlockwise) Figure 6.10 Attaching/Removing A Geometry AR 2000 Operator's Manual...

  • Page 65: Ensuring That The Sample Is Loaded Correctly

    Loading the sample correctly is a skill that is learned with time. It may help you to spend some time initially simply loading and reloading a sample. The correct loading is vital to accurate and meaningful results. AR 2000 Operator's Manual...
  • Page 66 AR 2000 Operator's Manual...

  • Page 67: Chapter 7: Using The Upper Heated Plate

    Using the Upper Heated Plate Introduction to the Upper Heated Plate At the standard AR 2000 Smart Swap™ Peltier plate's temperature range extremes, a temperature gradient may be introduced across the sample, the significance of which will depend on the sample’s thermomechanical properties.

  • Page 68: Attaching The Upper Heated Plate To The Ar 2000

    Attaching the Upper Heated Plate to the AR 2000 Follow the steps below to attach the Upper Heated Plate to the AR 2000 rheometer head. Ensure that air at the correct pressure is supplied to the air-bearing, and remove the bearing cap. Turn on the rheometer and raise the head to the maximum (use the Head UP button located on the instrument control panel).
  • Page 69 Smart Swap™ socket. WARNING: Do not remove the heating element cover. ATTENTION: N’enlevez Figure 7.4 pas la couverture Connection of the UHP Adaptor to the Smart Swap™ Socket d’élément de chauffe. AR 2000 Operator's Manual...

  • Page 70: Installing The (Optional) Vortex Air Cooler

    Installing the (Optional) Vortex Air Cooler Follow the steps below to attach and connect the vortex air cooler to the AR 2000. Refer to the figures as needed. Use the two screws provided to mount the vortex air cooler bracket to the rear of the AR 2000 casting as shown in Figure 7.5 to the right.
  • Page 71 100 psi, –30°C 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. Connect the event socket on the valve bracket to the EVENT B socket on the rear of the AR 2000 rheometer using the cable provided.

  • Page 72: Configurations For The Cooling Water

    Cooling Water Configuration 1 Mains Water Supplying Both Peltier and Upper Heated Plate Air Inlet Reducer Return Circulator Water Flow "Y" "Y" Piece Piece Figure 7.9 Cooling Water Configuration 2 Fluid Circulator Supplying Both Peltier and Upper Heated Plate AR 2000 Operator's Manual...

  • Page 73: Connecting The Cooling Control Unit

    Important: Note the direction of flow through this valve. Figure 7.12 Non-Return Valve (For use with mains water supply only. Important: Notez la direction d’écoulement à travers de la valve. Note the direction of flow through the valve.) AR 2000 Operator's Manual...

  • Page 74: Using Circulating Fluids Other Than Water

    A 4-mm to 6-mm adaptor and 6-mm "Y" piece are provided for the connection to the fluid circulator. Connect the EVENT socket on the CCU to the EVENT B socket on the rear of the AR 2000 Rheometer, using the cable provided.
  • Page 75 Upper Heated Plate is not required. Connect the EVENT socket on the valve bracket to the EVENT B socket on the rear of the AR 2000 rheometer, using the cable provided.

  • Page 76: Connecting And Disconnecting The Geometry Holder

    Removing the Geometry and Holder To remove the upper geometry and holder from the AR 2000 rheometer follow these steps: Raise the instrument head fully, using either the Rheology Advantage™ software or the Head UP button located on the instrument control panel.

  • Page 77: Configuring The Upper Heated Plate

    • 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.

  • Page 78: Calibration Of The Upper Heated Plate

    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. AR 2000 Operator's Manual...
  • Page 79 The Upper Heated Plate calibration box Figure 7.17 and zero value plug are shown in Figure 7.18 Zero Value Determination Instructions below. Figure 7.18 Upper Heated Plate Calibration Box (Left) and Zero Value Plug (Right) AR 2000 Operator's Manual...
  • Page 80 When the calibration is finished, raise the instrument head, and remove the calibration sensor. Remove the connector from the electronics box. 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. AR 2000 Operator's Manual...

  • Page 81: Clamping The Air Bearing

    Replace the geometry holder Push the clamp up onto the drawrod and attach it by turning the drawrod counterclockwise (anticlockwise). To remove the clamp hold it firmly and release it by turning the drawrod clockwise. Figure 7.23 Air-Bearing Clamp AR 2000 Operator's Manual...

  • Page 82: Using An Inert Gas Atmosphere

    (white) and the connector provided. 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. AR 2000 Operator's Manual...

  • Page 83: Using The 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 échantillon peut être chaud. Assurez-vous qu’il est froid avant d’essayer de l’enlever. AR 2000 Operator's Manual...
  • Page 84 AR 2000 Operator's Manual...

  • Page 85: Chapter 8: The Pressure Cell

    The Pressure Cell Overview WARNING: TA Instruments' Pressure Cell is designed for use at temperatures up to 150°C 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.

  • Page 86: Specifications

    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. AR 2000 Operator’s Manual...

  • Page 87: Pressure Cell Components

    The Pressure Cell is shown assembled on the AR rheom- eter, with the instrument head in the DOWN position, in Figure 8.2 to the left. Peltier Heating Jacket Manifold Assembly Figure 8.2 Pressure Cell on AR Rheometer AR 2000 Operator’s Manual...

  • Page 88: The Pressure Cell Cup

    "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 8.4 Pressure Gauge Port (Gauge and Valve Shown) AR 2000 Operator’s Manual...

  • Page 89: Safety Relief Port

    The rupture disc should only be replaced by a qualified TA Instruments Service Repre- sentative.

  • Page 90: Magnet Assembly

    Cover tains a powerful magnet capable of destroying magnetically recorded material. Adapter Insert (Used with AR 2000/AR 2000ex.) (Remove for AR-G2.) Figure 8.7 Magnet Assembly with AR 2000/ AR 2000ex Adapter Insert AR 2000 Operator’s Manual...

  • Page 91: Pressure Manifold

    Pressure Manifold Assembly • 1/8-inch and 1/4- inch 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. AR 2000 Operator’s Manual...

  • Page 92: Requirements For External Pressure Source

    Figure 8.9 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.

  • Page 93: Installing And Using The Pressure Cell

    The steps on the next several page provide the instructions needed to install and use the pressure cell. Pressure Cell Cup Tommy Bar Manifold Assembly with Gauge Angled Pipe Rotor Assembly Figure 8.10 Entire Pressure Cell Configuration Disassembled AR 2000 Operator’s Manual...

  • Page 94: Step 1: Install High-Pressure Piping Manifold

    M5 using the cap head screws provided, as shown in Figure 8.12 below. Attach manifold here Manifold Sorbothane Block Cap Head Screws Figure 8.11 Attach Manifold to Back of Rheometer Manifold Bracket Figure 8.12 Manifold Installed AR 2000 Operator’s Manual...

  • Page 95: Step 2: Install And Configure Pressure Cell Cup And Rotor

    Rotor Assembly with Small Magnet Position the small magnet on the rotor to face in the front center of the Peltier Jacket as shown in Figure 8.15 Figure 8.15 to the left. Orientation of Small Magnet AR 2000 Operator’s Manual...
  • Page 96 Newtons Small will be seen in the normal force reading.). Immedi- Magnet ately stop moving the rotor assembly down and remove the small magnet. Figure 8.16 Aligning the Reference Mark Figure 8.17 Magnets Engaging AR 2000 Operator’s Manual...

  • Page 97: Step 3: Positioning Gap And Pressure Cell Calibrations

    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 µN.m. AR 2000 Operator’s Manual...

  • Page 98: Step 4: Loading A Sample

    Rotor. Ensure that the reference mark on the upper 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 8.18. Small Magnet Figure 8.18 Aligning the Reference Mark AR 2000 Operator’s Manual...
  • Page 99 Immediately stop mov- ing the rotor assembly down and remove the small magnet. 10. Lower the instrument head to the geometry gap (default 3500 µm). Do not zero the gap. Figure 8.19 Magnets Engaging AR 2000 Operator’s Manual...

  • Page 100: Step 5: Align Manifold And Make Manifold Connections

    Then disconnect the compression connector indicated in Figures 8.20 and 8.21. 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. AR 2000 Operator’s Manual...

  • Page 101: Step 6: Pressurizing/Depressurizing The Cell And Running Experiments

    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 8.22 Three-Way Valve Positions AR 2000 Operator’s Manual...

  • Page 102: Running Experiments In Self-Pressurization Mode

    (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. AR 2000 Operator’s Manual...
  • Page 103 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. AR 2000 Operator’s Manual...

  • Page 104: Running Experiments In External Pressurization Mode

    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 25°C (ambient temperature) before attempting to relieve the pressure in the cell. AR 2000 Operator’s Manual...
  • Page 105 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. AR 2000 Operator’s Manual...

  • Page 106: Maintaining The Cell

    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. AR 2000 Operator’s Manual...

  • Page 107: Disassembling The Rotor

    See the figure below for reference. Upper Sapphire Bearing Thumbscrew Rotary Cap Magnet Shaft Rotor Sapphire Locking Nut Bearing Holder Figure 8.25 Parts of the Rotary Assembly (In correct order of assembly) AR 2000 Operator’s Manual...

  • Page 108: Reassembling The Rotor

    DO NOT CONTINUE TIGHTENING Figure 8.26 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. AR 2000 Operator’s Manual...
  • Page 109 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. AR 2000 Operator’s Manual...

  • Page 110: Replacement Parts

    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 &...

  • Page 111: Chapter 9: Ar 2000 Interfacial Accessory

    Figure 9.1 below shows a schematic of TA Instruments Interfacial Rheology Accessory. Liquid A is the more dense fluid, Liquid B the less dense fluid, R...

  • Page 112: Specifications

    34 mm (1.43 in) Bicone angle 10° Inertia 20.3 mNm s2 (approx) Material BS970-303 S31 grade stainless steel Geometry gap with disc edge level with the cup half full mark (22.5 mm): 19,500 µm (approx) Temperature Control: Ambient only AR 2000 Operator's Manual...

  • Page 113: Setting Up The Interfacial Accessory

    Setting up the Interfacial Accessory Follow the instructions below to set up the AR 2000 with the interfa- cial accessory: Raise the instrument head, and attach the cup holder base to the rheometer using the Smart Swap connector, as shown in Figure 9.2 to the right.

  • Page 114: Calibration And Mapping

    Mapping and Other Calibrations Mapping and other calibrations (such as for geometry inertia and bearing friction), are best carried out at this stage. Set a gap of 19500 µm, and perform the mapping and calibrations in the usual way. AR 2000 Operator's Manual...

  • Page 115: Experimental Procedure

    Any temperature settings in the procedure will be ignored. After running the procedure, raise the instrument head. Remove, clean and replace the cup. Repeat the procedure for the Sample Fluid B, to obtain M (Ω) then remove, clean and replace the Bcalibration cup. AR 2000 Operator's Manual...

  • Page 116: Finding The Interface Position

    Plot the results as normal force versus 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 9.5. Figure 9.5 Graph to Identify the Interface Position AR 2000 Operator's Manual...
  • Page 117 The viscosity of the total system including the interface can now be mea- sured. 11. Run the Flow procedure used to determine the contributions of the two bulk fluids, described above, to obtain the total torque M (Ω). total AR 2000 Operator's Manual...

  • Page 118: Analyzing The Results

    Then: (Ω) = M (Ω) - [(M (Ω) / 2) + (M (Ω) / 2)] interfacial total Acalibration Bcalibration (Ω) = M (Ω) - [M (Ω) + (M (Ω)] / 2 interfacial total Acalibration Bcalibration AR 2000 Operator's Manual...

  • Page 119: Interfacial Shear Stress And Shear Rate Calculation

    Heinemann, Boston (1991). [2] S-G. Oh and J.C. Slattery, Journal of Colloid and Interface Science, 67, 516 - 525 (1978). [3] E. Shotton, K. Wibberley, B. Warburton, S.S. Davis and P.L. Finlay, Rheologica Acta, 10, 142-152 (1971). AR 2000 Operator's Manual...
  • Page 120 AR 2000 Operator's Manual...

  • Page 121: Chapter 10 Do's And Don'ts

    Peltier plate before switching the instrument on. use good laboratory practice when using the instrument. Wear safety glasses and protective clothing where necessary. AR 2000 Operator's Manual...

  • Page 122: Don't

    Peltier System. disconnect or connect any cables, leads etc. while the power is on. be frightened of using the instrument for the first time. AR 2000 Operator's Manual...

  • Page 123: Appendix A Useful Information

    Useful Information Moments of Inertia The inertia of each geometry can be measured directly via TA Instruments rheology software. Below is a table that shows the approximate inertia values for cone and plate and parallel plate systems. You are advised to use the automatic inertia measurement feature in the software.

  • Page 124: Cylinder

    Cylinder Axis through center of cylinder. height of cylinder The approximate densities (x 10 µNm ) are: Steel 7.83 Acrylic 1.19 Aluminium 2.71 AR 2000 Operator's Manual...

  • Page 125: Appendix B Symbols And Units

    10 Modulus Shear Rate No change γ Shear Strain No change σ Shear Stress dyne cm (Pa) x 10 τ Torsional Force dyne cm x 10 η Viscosity Poise (P) Pa.s 1 cP = 1 mPa.s AR 2000 Operator's Manual...
  • Page 126 AR 2000 Operator's Manual...

  • Page 127: Appendix C: Geometry Form Factors

    R1 (mm) DIN (conical) 14 5920 Recessed 4000 Vaned 4000 Rotor Type Stator Rotor Rotor Immersed Outer Inner Outer Height (microns) Radius Radius Radius (mm) R1 (mm) R2 (mm) R3 (mm) Double Gap 20.38 21.96 59.5 AR 2000 Operator's Manual...
  • Page 128 AR 2000 Operator's Manual...

  • Page 129: Appendix D: Lcd Display Messages

    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. AR 2000 Operator's Manual...

  • Page 130: Bearing Pressure Too Low

    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. AR 2000 Operator's Manual...

  • Page 131: 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. AR 2000 Operator's Manual...
  • Page 132 AR 2000 Operator's Manual...

  • Page 133: Appendix E: Ta Instruments Etc Kits

    Melt Ring Tommy Bar Brass brush Brass scraper ETC Disp. Parallel Plate Kit (543308.901) Item No. Description Quantity Lower Plate Assembly Upper Shaft 25 mm Parallel disposable plates 10 set Tommy Bar Hex key Spare clamping screws AR 2000 Operator's Manual...
  • Page 134 AR 2000 Operator's Manual...

  • Page 135: Index

    31, 32 temperature control thermocouple using the stress and shear rate factors water bath AR 2000 Operator's Manual...
  • Page 136 56, 60 angles material moments of inertia cone and plate systems form factors controlled-stress technique cooling controlled Cooling Control Unit (CCU) cross threading AR 2000 Operator's Manual...
  • Page 137 EMC Conformité EMC Conformity encoder disc Environmental Test Chamber (ETC) specifications Environmental Testing Chamber. See ETC. See also ETC Environmental Testing Chamber (ETC) installing installing the low temperature accessory internal components kits oven setting up equilibrium time AR 2000 Operator's Manual...
  • Page 138 Upper Heated Plate cross-hatched description disconnecting for Upper Heated Plate form factors intertia materials 55 to 60 parallel plate plastic solvent trap version stainless steel AR 2000 Operator's Manual...
  • Page 139 LCD display messages levelling lifting and carrying liquid nitrogen handling safety lithium battery AR 2000 Operator's Manual...
  • Page 140 123 to 124 motor spindle Newtonian viscosity normal force transducer Notes, Cautions, and Warnings operation general guidelines rheometer optical encoder packaging removing parallel plate system moments of inertia parallel plate systems AR 2000 Operator's Manual...
  • Page 141 85 loading a sample 98 magnet assembly 90 maintenance 106 manifold 91 operational limits 86 positioning gap 97 pressurizing 101 reassembling rotor 108 replacement parts 110 requirements for external pressure source 92 rotor assembly 89 AR 2000 Operator's Manual...
  • Page 142 Rotational Mapping 26, 26 to 27 Rotor safety chemical electrical EMC Conformity warnings sample loading sample cover samples preventing evaporation shear rate shear stress shut down Sir Isaac Newton Smart Swap™ using AR 2000 Operator's Manual...
  • Page 143 Cooling Control Unit (CCU) connection configurations cooling water description gas atmosphere 67, 82 geometry holder disconnecting introduction modeling enabled Pt100 sample cover using inert gas atmosphere zero heat flow sensor zero value plug AR 2000 Operator's Manual...
  • Page 144 Zero Gap zero heat flow sensor Upper Heated Plate (UHP) AR 2000 Operator's Manual...

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