rheometric scientific sr5 manual

Ins trum en t M anua l9 02 -‐3 0014R ev is ion X 12 4 O c tober 1 99 7

This document is to be used solely by owners of the Rheometric Scientific SR5. Reproduction is prohibited without permission of Rheometric Scientific, Inc. The products described herein are under continuous development. Consequently, product operation may vary from that described. All information is subject to change without notice.

Rheometric Scientific, Inc.One Possumtown RoadPiscataway, NJ 08854, USAVoice: 732-560-8550Fax: 732-560-7451Service: 732-560-8990http://www.rheosci.com

SR5 INSTRUMENT MANUAL Revision X1 24 October 1997

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GENERAL INFORMATION

NOTICES

Disclaimer Rheometric Scientific, Inc. has taken due care in the preparation of this document. Insofar as specific mention is made of particular product features, Rheometric Scientific believes the information to be true and representative of the stated product at the time this document was published. No warranty is made regarding the veracity of such material. In no event will Rheometric Scientific be liable for damages of any kind, incidental or consequential, in regard to or arising out of the performance, form, or application of the material contained in this document. No representation is made regarding the suitability of this product information for any particular purpose. Rheometric Scientific reserves the right to revise this document and to make changes in its content without obligation to notify any person of such revision or change.

Instrument Development

Although this document is intended to describe the initial production version of the SR5, all information is based upon a prototype evaluation instrument. All products described herein are currently under continuous development. Therefore, product operation may vary from that described in this document.

Document Propriety

This document, and RSI Orchestrator Online Help, are the only Rheometric Scientific authorized publications concerning operation and calibration of this instrument. Copyright © 1997, Rheometric Scientific, Inc.

TERMS AND SYMBOLS USED IN THIS MANUAL

Term or Symbol Meaning

DANGER An immediately hazardous situation that, if not avoided, will result in either personal injury or death.

WARNING A potentially hazardous situation that, if not avoided, will result in either personal injury or death.

CAUTION A situation that, if not avoided, will result in damage to either this instrument or other inanimate property.

NOTE Information that is emphasized by being placed prior to the procedural step to which it pertains.

General identification symbol for safety notices. Also defines information pertaining to the portion of the instrument to which the symbol is affixed.


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SAFETY Service Do not attempt to service this instrument, as it contains no user-serviceable

components.

Electrical Hazards

Do not make physical contact with any component inside the instrument unless a set of procedural steps specifically instructs you to do so. In such cases, follow the procedure step-by-step.

Required Equipment

While operating this instrument, you must wear eye protection that either meets or exceeds ANSI Z87.1 standards. Additionally, wear protective clothing that has been approved for protection against the materials under test and the test temperatures.

Safety Notices The following safety notices that appear throughout this document are repeated here for emphasis.

Page 8

CAUTION POSSIBLE DAMAGE TO INSTRUMENT

The membrane air dryer must be connected between your house air and the Test Station. Failure to do so will result in extensive damage to this instrument.

Page 10


ANVIL

The Stress Head uses a precision air bearing that must be operated with instrument-quality air at a pressure of 60 psi (4.1 bar).

The Anvil (left) is an integral part of the bearing. Movement of the Anvil when no air is applied will score the air bearing, causing extensive damage to the instrument.

If the air supply is accidentally interrupted, do not touch the Anvil, or otherwise allow it to move, until air is restored.

The instrument is shipped with a bearing lock that prevents movement of the Anvil. If the air supply must be intentionally interrupted, as when transporting the instrument, install the bearing lock prior to removing air.


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Page 10


Read the operating and maintenance instructions that were supplied with your air dryer. Failure to properly maintain the dryer, moisture-trap, and coalescing filters will result in extensive damage to this instrument.

Pages 15 and 32

DANGER POSSIBLE PERSONAL INJURY

POSSIBLE DAMAGE TO INSTRUMENT

Turn OFF the Circulator prior to removing or installing any Lower Fixture. The Fluid Bath is an open vat of fluid that is sealed only when a Lower Fixture is installed. Failure to turn OFF the Circulator prior to fixture removal and installation will cause the Fluid Bath to overflow, resulting in possible injury and extensive damage to this instrument.

Page 32

WARNING TOXICITY

In Table 5-1 below, SF 96-50 silicon fluid emits toxic fumes when heated to a temperature greater than +140°C. Use SF 96-50 silicon fluid above +140°C only if an externally-vented exhaust hood is installed above the circulator. Ensure that exhaust airflow is adequate to expel fumes emitted from the circulator. Failure to heed this warning may result in injury or death.

Page 37



Turn OFF the Circulator prior to removing or installing the Peltier Fixture. The Fluid Bath is an open vat of fluid that is sealed only when the Peltier Fixture is installed. Failure to turn OFF the Circulator prior to fixture removal and installation will cause the Fluid Bath to overflow, resulting in possible injury and extensive damage to this instrument.


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CONTENTS

1 INTRODUCTION ....................................................................................................................................... 7

1-1 OVERVIEW ...................................................................................................................................... 7 1-1.1 Organization ........................................................................................................................... 7 1-1.2 Related Sources of Information .............................................................................................. 7

1-2 DESCRIPTION OF INSTRUMENT .................................................................................................. 7 1-2.1 General Principle .................................................................................................................... 7

1-3 SPECIFICATIONS ........................................................................................................................... 8 1-3.1 Base System .......................................................................................................................... 8 1-3.2 Environmental Control Systems ............................................................................................. 8

1-4 REQUIREMENTS ............................................................................................................................ 8 1-4.1 Pneumatic .............................................................................................................................. 8

2 COMPONENT OPERATION ..................................................................................................................... 9

2-1 MODULES ....................................................................................................................................... 9 2-2 REQUIRED READING: PREVENTING DAMAGE TO THE INSTRUMENT .................................. 10

2-2.1 Air Bearing ............................................................................................................................ 10 2-2.2 Air Dryer ............................................................................................................................... 10

2-3 TEST STATION COMPONENTS .................................................................................................. 11 2-3.1 Stage .................................................................................................................................... 12 2-3.2 User Interface ....................................................................................................................... 12 2-3.3 Anvil Components ................................................................................................................ 12

2-4 ENVIRONMENTAL CONTROLLER .............................................................................................. 13 2-4.1 Overview .............................................................................................................................. 13 2-4.2 Status Panel ......................................................................................................................... 13

3 FROM FIXTURE INSTALLATION TO SAMPLE LOADING ................................................................... 14

3-1 OVERVIEW .................................................................................................................................... 14 3-2 FIXTURE INSTALLATION AND REMOVAL .................................................................................. 15

3-2.1 Lower Fixture ........................................................................................................................ 15 3-2.2 Upper Fixture ........................................................................................................................ 17

3-3 ZEROING NORMAL FORCE ......................................................................................................... 17 3-4 AUTOCAL ...................................................................................................................................... 18

3-4.1 Overview .............................................................................................................................. 18 3-4.2 Procedure ............................................................................................................................. 18

3-5 TRACK MODE ............................................................................................................................... 19 3-5.1 Overview .............................................................................................................................. 19 3-5.2 Procedure ............................................................................................................................. 19

3-6 ZEROING AND SETTING THE GAP ............................................................................................. 19 3-6.1 Overview .............................................................................................................................. 19 3-6.2 Zeroing the Gap ................................................................................................................... 19 3-6.3 Setting the Gap .................................................................................................................... 20

3-7 SAMPLE LOADING GUIDELINES ................................................................................................ 20 3-7.1 Parallel Plate ........................................................................................................................ 20


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3-7.1.1 Gap Setting ................................................................................................................. 20 3-7.1.2 Loading ....................................................................................................................... 20

3-7.2 Cone and Plate ..................................................................................................................... 21 3-7.2.1 Gap Setting ................................................................................................................. 21 3-7.2.2 Test Temperatures ...................................................................................................... 21 3-7.2.3 Loading ....................................................................................................................... 21

3-7.3 Couette ................................................................................................................................. 22

4 CALIBRATION ........................................................................................................................................ 23

4-1 OVERVIEW .................................................................................................................................... 23 4-1.1 Operations ............................................................................................................................ 23 4-1.2 Calibration Kit ....................................................................................................................... 24

4-2 TORQUE CALIBRATION ............................................................................................................... 25 4-2.1 Overview .............................................................................................................................. 25 4-2.2 Procedure ............................................................................................................................. 25

4-3 SPIN CORRECTION ..................................................................................................................... 28 4-3.1 Overview .............................................................................................................................. 28 4-3.2 Procedure ............................................................................................................................. 28

4-4 EXAMINATION OF CAL CURVE ................................................................................................... 29 4-4.1 Overview .............................................................................................................................. 29 4-4.2 Procedure ............................................................................................................................. 29

4-5 NORMAL FORCE CALIBRATION ................................................................................................. 30 4-5.1 Overview .............................................................................................................................. 30 4-5.2 Procedure ............................................................................................................................. 30

5 APPENDICES ......................................................................................................................................... 31

5-1 OVERVIEW .................................................................................................................................... 31 5-1.1 Purpose ................................................................................................................................ 31 5-1.2 Content ................................................................................................................................. 31

5-2 FLUID BATH ENVIRONMENTAL CONTROL SYSTEM ................................................................ 32 5-2.1 Principle ................................................................................................................................ 32 5-2.2 Circulator Connection ........................................................................................................... 32 5-2.3 Filling the Circulator .............................................................................................................. 32 5-2.4 RSI Orchestrator Fluid Bath Configuration ........................................................................... 34

5-3 PELTIER ENVIRONMENTAL CONTROL SYSTEM ...................................................................... 35 5-3.1 Principle ................................................................................................................................ 35 5-3.2 Tentative Specifications ....................................................................................................... 36 5-3.3 Selecting a Thermal Operating Range ................................................................................. 36 5-3.4 Installation ............................................................................................................................ 37 5-3.5 Circulator Options ................................................................................................................. 39 5-3.6 RSI Orchestrator Peltier Configuration ................................................................................. 39

5-4 HUMIDITY COVER ........................................................................................................................ 39 5-4.1 Principle ................................................................................................................................ 40 5-4.2 Usage ................................................................................................................................... 40


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1 INTRODUCTION

1-1 OVERVIEW 1-1.1

Organization This manual describes instrument-specific features of the Rheometric Scientific Universal Stress Rheometer SR5. The following information is contained herein:

• Chapter 1 Introduction Provides an overview of your documentation and the instrument, and lists instrument performance specifications.

• Chapter 2 Component Operation Identifies and describes components of the base instrument.

• Chapter 3 From Fixture Installation to Sample Loading Details, in sequence, procedures that you must perform prior to conducting a test.

• Chapter 4 Calibration Contains instrument calibration procedures.

• Chapter 5 Appendices Add-on sections that describe Environmental Control Systems and various options as they become available.

1-1.2 Related Sources

of Information

This instrument is operated using Rheometric Scientific RSI Orchestrator™ software for Microsoft® Windows 95™ and NT™. The dynamic nature of RSI Orchestrator has necessitated that, wherever possible, all technical information concerning the software be segregated from hard copy and supplied in the form of Windows Online Help. Please refer to the following sources concerning RSI Orchestrator: • RSI Orchestrator Startup Guide 902-30010 Current Revision

Installation instructions, general procedures, and a brief tour of the software. • RSI Orchestrator Online Help Current Revision

Online WinHelp™ guide to software reference and operational information.

1-2 DESCRIPTION OF INSTRUMENT 1-2.1

General Principle

The SR5 is a controlled-stress rheometer, i.e., the instrument deforms a sample by applying the controlled stress that you specify. The resultant angular deflection (strain) required to apply the stress is then measured. All material properties are then calculated by analysis of the applied stress and resulting strain. Controlled stress is applied to the sample by the Stress Head. This is essentially a drag cup motor mounted on a precision air bearing. Position sensors mounted on the motor provide angular deflection (strain) information for any applied stress. Selected tests also allow you to choose a strain (desired angular deflection) to which the sample is subjected, thereby allowing test conditions to be specified as they would using a controlled-strain rheometer.


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1-3 SPECIFICATIONS 1-3.1

Base System Torque Range 0.01 to 500 g·cm (0.001 to 50 mNm)

Rotation Rate 0 to 100 radians per second Dynamic Frequency Range 0.00005 to 500 radians per second

Angular Resolution

When the instrument is in Track Mode, an angular displacement of better than 1 microradian can be resolved around the starting position (see paragraph 3-5 TRACK MODE on page 19).

Normal Force Range 5 to 2000 grams

1-3.2 Environmental

Control Systems Fluid Bath See paragraph 5-2.3 Filling the Circulator on

page 32

Peltier See paragraph 5-3.2 Tentative Specifications on

page 36 Electrically Heated Plates Ambient to +350°C (preliminary specification) Furnace -150°C to +500°C (preliminary specification)

1-4 REQUIREMENTS 1-4.1

Pneumatic Air Pressure Into the Instrument 60 psi (4.1 bar)

Air Flow Into the Instrument 2.5 scfm

Air Quality Into the Membrane Dryer

Instrument-quality air with a dew point of -40°C, and containing particles no larger than 5 microns in diameter.


The membrane air dryer must be connected between your house air and the Test Station. Failure to do so will result in extensive damage to this instrument.


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2 COMPONENT OPERATION

2-1 MODULES Throughout this manual, references are made to the following instrument modules:

• Test Station The Test Station (Figure 2-1) is the single chassis comprising the SR5 Base

System. It houses the Stress Head, Fluid Bath, and all support electronics.

TESTSTATION

ENVIRONMENTALCONTROLLER

Figure 2-1 Test Station and Environmental Controller

• Environmental Controller The Environmental Controller (Figure 2-1) contains all support electronics

necessary to operate optional environmental control systems. Although not needed to operate the Fluid Bath, the Environmental Controller is supplied with options such as Peltier.

• Personal Computer (PC) The Personal Computer (IBM®-compatible PC) operates RSI Orchestrator software. Please refer to the manufacturer’s literature for hardware-specific details concerning your PC. For minimum PC requirements, refer to the current revision of the RSI Orchestrator Startup Guide 902-30010.


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2-2 REQUIRED READING: PREVENTING DAMAGE TO THE INSTRUMENT 2-2.1

Air Bearing The Stress Head contains a precision air bearing, which is essentially a journal that rotates within a race. A column of air less than 0.001 inch separates the two, providing almost friction-free rotation during testing. If air flow to this instrument is interrupted, rotating the Stress Head will result in incredibly expensive damage to this instrument. Note the following caution.


ANVIL

The Stress Head uses a precision air bearing that must be operated with instrument-quality air at a pressure of 60 psi (4.1 bar).

The Anvil (left) is an integral part of the bearing. Movement of the Anvil when no air is applied will score the air bearing, causing extensive damage to the instrument.

If the air supply is accidentally interrupted, do not touch the Anvil, or otherwise allow it to move, until air is restored.

The instrument is shipped with a bearing lock that prevents movement of the Anvil. If the air supply must be intentionally interrupted, as when transporting the instrument, install the bearing lock prior to removing air.

2-2.2 Air Dryer

This instrument is supplied with a membrane-type air dryer that blocks moisture by passing air through a filter that blocks water molecules. Moist air is continuously purged from the dryer through a series of purge holes. The amount of purge can be adjusted by rotating the purge knob on the dryer. Settings range from zero (no purge and, hence, no drying) to 3 (high purge and maximum drying). We recommend a setting of 2. Do not set the purge below 2, as this will not sufficiently dry the air into the instrument. Depending upon the membrane dryer you receive, the dryer may require periodic maintenance. Preceding and in line with the air dryer are a moisture-trap filter and a coalescing filter. It is vital that you maintain both the moisture-trap and coalescing filters in accordance with the instructions provided with the filters. In general, maintenance of these filters usually involves no more than draining them at the intervals specified by the manufacturer. Note the following caution.


Read the operating and maintenance instructions that were supplied with your air dryer. Failure to properly maintain the dryer, moisture-trap, and coalescing filters will result in extensive damage to this instrument.


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2-3 TEST STATION COMPONENTS Refer to Figure 2-2 during the following discussion of Test Station Components.

USER INTERFACE

STAGE

ANVIL STOP

ANVIL

ANVIL STOP CONTROL

Figure 2-2 Test Station Components


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2-3.1

Stage The stage is a motorized platform that supports the Stress Head. The stage can be manually raised and lowered using the Stage Control on the User Interface (next topic), or automatically adjusted to a specific height using RSI Orchestrator (see paragraph 3-6 ZEROING AND SETTING THE GAP on page 19). To raise the Stage to maximum height: Perform the following steps using RSI Orchestrator:

a. Click either the Gap Control Panel function (Control menu), or the Gap

Control button . The Gap Control dialog box is displayed. b. Click Send To Top.

2-3.2

User Interface The User Interface is a control panel that allows control and display of selected Test Station functions, as described in Figure 2-3.

• Stage Control

+

+

Press To move Stage

Up slowly

Up quickly

Down slowly

Down quickly • Power

Illuminated when power is applied to the instrument

• Environmental Off Press to unconditionally remove power from the Environmental Control System.

• Display • Temperature currently being measured by the Environmental Control

System • Gap between Upper and Lower Fixtures, relative to a zero reference

established when you zero the Gap (see paragraph 3-6 ZEROING AND SETTING THE GAP on page 19)

2-3.3 Anvil

Components

Upper Test Fixtures mount onto the Anvil. As mentioned in paragraph 2-2.1 Air Bearing (page 10), the Anvil is an extension of the air bearing that rotates during testing. The Anvil Stop, essentially a pneumatic piston, steadies the Anvil during Upper Fixture installation and sample loading. To hold the Anvil in its current position, turn the Anvil Stop Control to the Lock position. To allow the Anvil to rotate freely, turn the Anvil Stop Control to the Unlock position. Fixture installation procedures are given in paragraph 3-2 FIXTURE INSTALLATION AND REMOVAL on page 15.

Figure 2-3 User Interface


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2-4 ENVIRONMENTAL CONTROLLER 2-4.1

Overview Used with Environmental Control options other than the Fluid Bath, the Environmental Controller contains all electronics necessary to operate and monitor Environmental Control systems such as Peltier and Heated Plates.

2-4.2 Status Panel

Although all Environmental Control functions are initiated using RSI Orchestrator, the Environmental Controller provides the following monitoring on the Environmental Control Status Panel (Figure 2-4).

Each LED is illuminated when...

...the Peltier environmental control system is decreasing temperature

...the Peltier environmental control system is increasing temperature

...power is applied to the Lower Heated Plate

...power is applied to the Upper Heated Plate

...nitrogen purge is enabled

...the Heated Plates environmental control system is enabled

...all SR5 environmental control system electronics are ready for use

...the Test Station electronics can communicate with the Environmental

Controller

...the Peltier environmental control system is enabled

Figure 2-4 Environmental Control Status Panel


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3 FROM FIXTURE INSTALLATION

TO SAMPLE LOADING

3-1 OVERVIEW This chapter contains procedures that must be performed prior to executing a test using RSI Orchestrator software. Perform these procedures in the sequence presented, as outlined below:

• Fixture Installation and Removal Instructions are provided to install and remove Upper and Lower Fixtures used in conjunction with the base (standard) instrument.

• Zeroing Normal Force A method is given to establish a zero reference normal force.

• AutoCal General information concerning AutoCal (Automatic Fixture Inertia Calculation) is provided with instructions for implementation.

• Track Mode A procedure is given to use Track Mode, which allows the instrument to provide optimum angular resolution.

• Zeroing and Setting the Gap Separate procedures are given for manually adjusting the gap, or allowing RSI Orchestrator to adjust the gap for you.

• Sample Loading Guidelines Guidelines to use while loading samples are provided for each geometry. Geometry constants and formulas used for data calculation are included in RSI Orchestrator Online Help (see the Reference Guide in the Online Help Table of Contents).


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3-2 FIXTURE INSTALLATION AND REMOVAL 3-2.1

Lower Fixture The following procedure describes Lower Fixture installation when tests are conducted using the Fluid Bath, which is supplied with all instruments. For procedures covering Environmental Control options, please see the relevant Appendix.




Refer to Figure 3-1 during the following procedures.

Installation a. Raise the stage to maximum height (see paragraph 2-3.1 Stage on page 12). b. Push the Lower Fixture fully into the base, aligning the four captive screws

with the holes in the base. c. Tighten the four captive screws in the Lower Fixture (do not over-torque).

Removal a. Raise the stage to maximum height (see paragraph 2-3.1 Stage on page 12). b. Loosen the four captive screws in the Lower Fixture. c. Pull the Lower Fixture from the base.


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FRONT OF INSTRUMENT

VIEW LOOKING DOWNWARD FROM THE TOP OF THE INSTRUMENT

LOWER FIXTURE

CAPTIVE SCREWS

NOTE

Early production units are equipped with eight mounting holes. If your unit is so equipped, align the captive screws on the Lower Fixture with the holes shown (at left) filled in black.

Figure 3-1 Lower Fixture Installation onto Fluid Bath


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3-2.2

Upper Fixture The following procedure describes Upper Fixture installation for all Environmental Control options. Refer to Figure 3-2 during the following procedure.

Installation a. Raise the stage to maximum height

(see paragraph 2-3.1 Stage on page 12).

b. Hold the Anvil in its current position by turning the Anvil Stop Control to the Lock position (see paragraph 2-3.3 Anvil Components on page 12).

c. Align the tapped hole in the fixture with the threaded rod in the anvil.

d. Fasten the fixture to the anvil by rotating the threaded rod until it draws the fixture fully upward into the anvil (hand tighten only).

e. If you are about to load a sample, keep the Anvil Stop Control locked; otherwise, turn it to the Unlock position.

Removal a. Raise the stage to maximum height

(see paragraph 2-3.1 Stage on page 12). b. Hold the Anvil in its current position by turning the Anvil Stop Control to the

Lock position (see paragraph 2-3.3 Anvil Components on page 12). c. While holding the fixture, rotate the threaded rod until it disengages the

fixture.

3-3 ZEROING NORMAL FORCE Normal (Axial) Force sensed by the instrument must next be set to zero. Do this

clicking the Zero Normal Force function in the Control menu of RSI Orchestrator software.

THREADED ROD

ANVIL

FIXTURE Figure 3-2 Upper Fixture

Installation


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3-4 AUTOCAL 3-4.1

Overview AutoCal (Automatic Fixture Inertia Calculation) is a function that measures the mass of an Upper Fixture, and adds this mass to the mass of the air bearing and its associated components. The inertia of the total mass is then calculated for use in compensating for inertia during testing. The inertia value is stored with the geometry information and can be used in all subsequent experiments using that Upper Fixture. During Dynamic testing, accurate angular displacement of the Upper Fixture can be achieved only if the fixture’s inertia is overcome at each peak deflection point. Inertia compensation therefore becomes more important as the Dynamic test frequency (and consequently inertia) increases. AutoCal must be performed prior to the first time an Upper Fixture is used to run tests. Subsequent use of the same fixture does not require AutoCal.

3-4.2 Procedure

Perform the following procedure to AutoCal:

a. Install an Upper Fixture (see paragraph 3-2.2 Upper Fixture on page 17). b. Release the Anvil by turning the Anvil Stop Control to the Unlock position

(see paragraph 2-3.3 Anvil Components on page 12). The Anvil must be free to rotate.

b. Select the Start Test function. The Edit/Start Test dialog box is displayed. c. From the displayed list, select the geometry that corresponds to the Upper

Fixture in use. Click Edit Geometry. The form for the selected geometry type is displayed.

d. Click Options. The AutoCal dialog box (Figure 3-3) is displayed.

Figure 3-3 AutoCal Dialog Box

e. Ensure that the Upper Fixture meets the following conditions: 1. It is clear of obstructions and free to rotate. 2. It is either not rotating (ideal condition), or rotating at a rate of less than 1/4

revolution per second. f. Click AutoCal, then wait until the inertia value is displayed (Figure 3-3). g. Save the inertia value by clicking Ok. The form for the selected geometry is

again displayed. h. Return to the Edit/Start Test dialog box by clicking Ok.


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3-5 TRACK MODE 3-5.1

Overview Activating the RSI Orchestrator Track Mode function synchronizes the instrument’s position control sensors. When the instrument is in Track Mode, an angular displacement of better than 1 microradian can be resolved around the starting position. When the instrument is not in Track Mode, the angular resolution depends upon the absolute position of the stress head. You must activate Track Mode under the following conditions: • Immediately after applying power to the instrument (the instrument discards

Track Mode information after power has been removed) • If your test requires resolving an angular displacement of less than 1

microradian Unless you must begin a test at a certain angular position, we recommend that you activate Track Mode prior to making contact between the Upper Fixture and the sample.

3-5.2 Procedure

Prior to making contact between the Upper Fixture and the sample, activate Track Mode by clicking the Track Mode function (Control menu) of RSI Orchestrator. The Anvil subsequently rotates to a fixed position that it maintains until a test begins.

3-6 ZEROING AND SETTING THE GAP 3-6.1

Overview You must zero and set the Gap between Upper and Lower fixtures when using Parallel Plate or Cone and Plate fixtures. The RSI Orchestrator Gap Control Panel function provides a single dialog box that allows you to both zero and set the Gap.

3-6.2

Zeroing the Gap If conducting tests at other than ambient temperature, ensure that the fixtures are at the starting or working temperature prior to proceeding.

a. Ensure that a sample is not loaded and the upper and lower fixtures are clean.

b. Using the Stage Control on the User Interface (see paragraph 2-3.2 User Interface on page 12), lower the stage to achieve a Gap of about 0.5 mm (as judged visually).

c. Click either the Gap Control Panel function (Control menu), or the Gap

Control button . The Gap Control dialog box is displayed. d. Click Zero Fixture. An information form is displayed showing the duration

(Elapsed Time) of the zeroing operation. The present gap is displayed in the Current Gap field, which updates at one second intervals. The following events occur during the zeroing operation: 1. The stage lowers to achieve contact between fixtures. 2. Following contact, Current Gap is zeroed, and the information form is no

longer displayed. e. In preparation for loading the sample, raise the Stage to maximum height by

clicking Send to Top. f. Remain in the Gap Control Panel and proceed to the next paragraph Setting

the Gap.


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3-6.3

Setting the Gap After zeroing the Gap, set it as follows:

a. Place the sample onto the lower fixture (see paragraph 3-7 SAMPLE LOADING GUIDELINES on page 20).

b. Enter the following information: 1. Commanded Gap Position

Enter the desired Gap in millimeters. 2. Max Allowed Force

Enter the maximum Normal Force (in grams-force) that will be generated while the sample is being compressed during the gap setting operation. When Normal Force exceeds this value, the stage stops descending until Normal Force relaxes and drops below this value. Stage movement then resumes.

c. Click Set Gap. An information form appears, indicating the time elapsed since the button was clicked. The Stage should descend relatively quickly (typically 5 mm/sec) until the Upper Fixture is 3 mm from the Commanded Gap Position, at which time it will slow its rate of descent until the Gap is achieved. The gap is set when the information form is no longer displayed.

3-7 SAMPLE LOADING GUIDELINES 3-7.1

Parallel Plate Prior to loading the sample, ensure that all previous procedures in this chapter have been performed (if applicable, as indicated within each procedure).

3-7.1.1 Gap Setting

The recommended Gap setting between Parallel Plates is between 0.5 and 2 millimeters.

3-7.1.2 Loading

Perform the following procedure to load samples using the Parallel Plate fixtures. In general, Figure 3-4 shows properly loaded Calibration Samples, included in the Calibration Kit (see paragraph 4-1.2 Calibration Kit on page 24), which are representative of most samples. At the left is the PDMS Calibration Sample, at the right is the 100 cP Calibration Sample. Note that samples such as PDMS should bulge somewhat from the edges of the plates, while the 100 cP fluid should taper downward from the bottom edge of the Upper Fixture.

UPPER FIXTURE

SAMPLE

LOWER FIXTURE

Figure 3-4 Parallel Plates with Sample Loaded

a. Zero the gap (see paragraph 3-6.2 Zeroing the Gap on page 19). b. Raise the Stage to maximum height (see paragraph 2-3.1 Stage on page 12). c. Activate Track Mode (please read paragraph 3-5 TRACK MODE on page

19). d. Hold the Anvil in its current position by turning the Anvil Stop Control to the

Lock position (see paragraph 2-3.3 Anvil Components on page 12). e. Place the sample onto the Lower Fixture.

NOTE


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In the next step: Although loading technique will vary depending on the sample, we generally recommend lowering the stage to within about 50 microns of the desired gap, trimming the edges sample, then lowering to the desired gap.

f. Set the gap (see paragraph 3-6.3 Setting the Gap on page 20). g. Release the Anvil by turning the Anvil Stop Control to the Unlock position.

3-7.2 Cone and Plate

Prior to loading the sample, ensure that all previous procedures in this chapter have been performed (if applicable, as indicated within each procedure).

3-7.2.1 Gap Setting

The actual gap setting for each Cone and Plate fixture is stated on the Certificate of Calibration that is included in the fixture kit. If no Certificate of Calibration is available, contact our Technical Service department.

3-7.2.2 Test Temperatures

Use Cone and Plate for isothermal testing only. Transitions to elevated temperatures cause expansion of the fixture. Since the nominal gap setting for cone and plate geometry is 50 microns (0.05 millimeter), thermal expansion can cause contact between fixtures, resulting in erroneous test data.

3-7.2.3 Loading

Perform the following procedure to load samples using Cone and Plate fixtures. In general, Figure 3-5 shows properly loaded Calibration Samples, included in the Calibration Kit (see paragraph 4-1.2 Calibration Kit on page 24), which are representative of most samples. At the left is the PDMS Calibration Sample, at the right is the 100 cP Calibration Sample. Note that samples such as PDMS should bulge somewhat from the edges of the plates, while the 100 cP fluid should taper downward from the bottom edge of the Upper Fixture.

UPPER FIXTURE

SAMPLE

LOWER FIXTURE

Figure 3-5 Cone and Plate with Sample Loaded

a. Zero the gap (see paragraph 3-6.2 Zeroing the Gap on page 19). b. Raise the Stage to maximum height (see paragraph 2-3.1 Stage on page 12). c. Activate Track Mode (please read paragraph 3-5 TRACK MODE on page

19). d. Hold the Anvil in its current position by turning the Anvil Stop Control to the

Lock position (see paragraph 2-3.3 Anvil Components on page 12). e. Place the sample onto the Lower Fixture.

NOTE In the next step: Although loading technique will vary depending on the sample, we generally recommend lowering the stage to within about 50 microns of the desired gap, trimming the edges sample, then lowering to the desired gap.

f. Set the gap (see paragraph 3-6.3 Setting the Gap on page 20).


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g. Release the Anvil by turning the Anvil Stop Control to the Unlock position.

3-7.3 Couette

Prior to loading the sample, ensure that all previous procedures in this chapter, except Zeroing and Setting the Gap, have been performed (if applicable, as indicated within each procedure). You need not set the gap when using a Couette. The following sample loading procedure supports both standard and DIN Couettes. a. Raise the Stage to maximum height (see paragraph 2-3.1 Stage on page 12). b. Activate Track Mode (please read paragraph 3-5 TRACK MODE on page

19). c. Hold the Anvil in its current position by turning the Anvil Stop Control to the

Lock position (see paragraph 2-3.3 Anvil Components on page 12). d. Pour the sample into the Cup (Lower Fixture). e. Using the Stage Control buttons on

the User Interface (see paragraph 2-3.2 User Interface on page 12), lower the Bob into the Cup until the sample level reaches the upper surface of the Bob, and the following criteria are met (see Figure 3-6): 1. The sample forms a meniscus

between the edges of the Bob and Cup, but does not flow over the upper surface of the Bob.

2. The upper surface of the Bob is between zero and 5 millimeters below the upper surface of the Cup. If this is not the case, adjust the sample volume accordingly.

f. Release the Anvil by turning the Anvil Stop Control to the Unlock position.

BOB CUP

UPPER SURFACEOF BOB

UPPER SURFACEOF CUP

SAMPLE

Figure 3-6 Couette with Sample

Loaded


23

4 CALIBRATION

4-1 OVERVIEW 4-1.1

Operations This chapter contains calibration operations that you should perform. Table 4-1 lists these operations in the required order of performance and the mandatory or recommended frequency of performance.

Table 4-1 Calibration Operations

Operation in required order of performance Frequency of Performance

Torque Calibration

Mandatory: • During instrument installation • Following replacement of stress head

Recommended once per month

Spin Correction

Mandatory: • During instrument installation • Following movement and re-leveling of

the instrument Recommended following Torque Calibration

Examination of Cal Curve Mandatory during instrument installation Recommended following Spin Correction

Normal Force Calibration

Mandatory: • During instrument installation • Following replacement of stress head

Recommended once per month


24

4-1.2

Calibration Kit This instrument is supplied with a Calibration Kit. It should contain the items listed in Table 4-2.

Table 4-2 Calibration Kit

Item Description and Purpose

Calibration Fixture

Upper Fixture used to apply a known mass to the stress head during Torque and Normal Force Calibration.

Hex Key Set Six-piece (1.5- to 5-mm) metric balldriver set.

Level

Circular bubble level used to level the instrument.

Monofilament Line

Five-pound-test fishing line used to hang Weight from Calibration Fixture during Torque Calibration.

Pulley

Pulley that supports the monofilament line during torque calibration (used to reduce friction).

Screw (extra Bearing Lock Screw)

M4 X 0.7 X 8-mm machine screw supplied as an extra bearing lock screw, which must be installed when air is not applied to the instrument.

Calibration Samples (used to provide a known viscosity)

100 centiPoise calibration sample (2 ounce bottle). 10 centiPoise calibration sample (2 ounce bottle). GE# SE-30 PDMS viscoelastic sample (1 ounce bottle).

Weights

Precision weights used to apply a known mass to the stress head during Torque and Normal Force Calibration.

Torque Calibration Weight: 50 grams Normal Force Calibration Weight: 1000 grams


25

4-2 TORQUE CALIBRATION 4-2.1

Overview Torque Calibration involves hanging a precision weight from the Calibration Fixture, which provides a 2.5 centimeter moment of torque. The instrument then determines and applies the corresponding counter-torque required to support the weight.

4-2.2 Procedure

Using the items provided in your Calibration Kit, perform Torque Calibration as follows:

a. Raise the Stage to maximum height (see paragraph 2-3.1 Stage on page 12). b. Release the Anvil by turning the Anvil Stop Control to the Unlock position

(see paragraph 2-3.3 Anvil Components on page 12). The Anvil must be free to rotate.

c. Install the Calibration Fixture as shown in Figure 4-1. Note that the rod must be positioned to the rear of the instrument, and must fit into the channel as shown.

d. Insert the Pulley into the Test Station frame as shown in Figure 4-1, ensuring that the flat machined into the Pulley shaft faces toward the left.

Secure the Pulley by tightening the setscrew in the access hole using a hex wrench.

e. Prepare a piece of monofilament line with a knot at one end and a loop at the other end.

f. Perform the following steps (refer to Figure 4-2): 1. Place the knotted end of the line through the slot in the Calibration Fixture,

and place the line in the groove of the pulley. 2. Hang the 50 gram weight (part number 613-02061) from the loop in the

line, ensuring that the weight hangs freely. The weight should cause the Calibration Fixture to rotate counterclockwise (as viewed from the top of the instrument), pulling the rod to rest against the left side of the channel (as viewed facing the front of the instrument).

3. Adjust the line so it rests neither on the upper nor the lower surface of the calibration fixture, as shown in Figure 4-2.

4. Ensure that the weight is free to hang without obstruction, and that the weight is steady (not swinging from side-to-side).

g. Using RSI Orchestrator software, select Calibrate Instrument (Utilities menu). The Transducer Setup form is displayed.

h. Click XducerCal. A calibration information form is displayed. i. Click Torque Calibration. Yet another information form is displayed. j. Click Ok. Calibration is complete when the following events have taken

place: From the starting position, the Calibration Fixture should rotate clockwise, moving the rod to the right. When calibration is complete, the rod should return to the starting position, and the numbers in the Torque Calibration Value and Motor Temp Reference fields should change value.

k. Exit the calibration by clicking Ok. l. Remove the weight, line, pulley, and Calibration Fixture.


26

CALIBRATION FIXTUREPULLEY

ROD

Figure 4-1 Installation of Calibration Fixture and Pulley


27

CALIBRATION FIXTURE

UPPER SURFACE

LOWER SURFACELINE

CALIBRATION FIXTURE

LINE

WEIGHT

Figure 4-2 Applying Torque Using Calibration Weight


28

4-3 SPIN CORRECTION 4-3.1

Overview Spin Correction compensates for any air bearing rotation that may occur due to air flow or precession.

4-3.2 Procedure

Before proceeding, ensure that Torque Calibration (paragraph 4-2 on page 25) has been performed, and the instrument has been properly leveled.

a. Raise the Stage to maximum height (see paragraph 2-3.1 Stage on page 12). b. Install a 25 mm Parallel Plate fixture. c. Zero the Gap (see paragraph 3-6.2 Zeroing the Gap on page 19). d. Load a quantity of the 10cP Calibration Sample from the Calibration Kit (see

paragraph 3-7.1 Parallel Plate on page 20). The quantity should be sufficient to set a Gap of 1 millimeter.

e. Ensure that the Anvil Stop Control is in the Unlock position (see paragraph 2-3.3 Anvil Components on page 12). The Anvil must be free to rotate.

f. Set the Gap to 1 millimeter (see paragraph 3-6.3 Setting the Gap on page 20).

f. Using RSI Orchestrator software, select the Calibrate Instrument function (Utilities menu). The Transducer Setup form is displayed.

g. Click SpinCorr. An information form is displayed, notifying you that Spin Correction is about to begin.

h. Begin Spin Correction by clicking Ok. An information form is displayed, notifying you that the instrument should not be disturbed during Spin Correction.

i. Wait until Spin Correction is complete, as indicated by both of the following events: 1. The information screen is no longer displayed. 2. The number in the Spin Correction field of the Transducer Setup form

changes value. j. Click Ok. k. Raise the stage to maximum height, then remove the Calibration Sample and

(if desired) Parallel Plate.


29

4-4 EXAMINATION OF CAL CURVE 4-4.1

Overview During Spin Correction, the instrument generates a Cal Curve, which is a profile of stress head rotational characteristics at selected positions. A Cal Curve that is within tolerances specified in step b of this procedure indicates that the instrument is properly leveled and is a confirmation of the overall integrity of the stress head and support electronics. Before proceeding, ensure that the following calibration operations have been performed in the order listed: • Torque Calibration (paragraph 4-2 on page 25) • Spin Correction (paragraph 4-3 on page 28)

4-4.2

Procedure Examine the Cal Curve as follows:

a. Using RSI Orchestrator, select the Get Stress Head Cal Curve function (Utilities: Service menu). The Cal Curve is displayed.

b. Ensure that Cal Curve parameters are within tolerances (subject to change without notice), as follows (see Figure 4-3 for a definition of the parameters): 1. Amplitude (maximum peak-to-peak amplitude of the Cal Curve) must be

less than 12 mg•cm. 2. Variation (maximum point-to-point deviation along the Cal Curve) must be

less than 2 mg•cm.

Figure 4-3 Cal Curve Parameters


30

4-5 NORMAL FORCE CALIBRATION 4-5.1

Overview Normal Force Calibration involves hanging a precision weight from a hook mounted to the Calibration Fixture. The instrument then scales the weight to ensure accurate Normal Force measurement.

4-5.2 Procedure

Using the items provided in your Calibration Kit, perform Normal Force Calibration as follows:

a. Raise the Stage to maximum height (see paragraph 2-3.1 Stage on page 12). b. Install the Calibration Fixture in the same manner as for the Torque

Calibration (see Figure 4-1). Do not install the pulley. c. Ensure that the Anvil Stop Control is in the Unlock position (see paragraph

2-3.3 Anvil Components on page 12). The Anvil must be free to rotate. d. Using RSI Orchestrator software, select Calibrate Instrument (Utilities

menu). The Transducer Setup form is displayed. e. Click XducerCal. A Calibration information form is displayed. f. Click NormalCal. g. Click Zero. An information form is displayed, notifying you that Normal Force

is being zeroed. Before proceeding, wait until the Transducer Setup form is again displayed.

h. Hang the 1000 gram weight from the hook that is mounted to the bottom of the Calibration Fixture.

i. Click NormCal. A form is displayed, prompting you to enter the applied weight.

j. Enter 1000. k. Click Calibrate. Calibration is complete when the Transducer Setup form is

again displayed. l. Exit the calibration by clicking Ok. m. Remove the weight and Calibration Fixture.


31

5 APPENDICES

5-1 OVERVIEW 5-1.1

Purpose The Appendices in this chapter describe instrument options and provide instructions that do not necessarily apply to operation and calibration of the base instrument.

5-1.2 Content

Topics following topics are currently included in this chapter:

• FLUID BATH ENVIRONMENTAL CONTROL SYSTEM (paragraph 5-2, page 32)

• PELTIER ENVIRONMENTAL CONTROL SYSTEM (paragraph 5-3, page 35)

• HUMIDITY COVER (paragraph 5-4, page 39)


32

5-2 FLUID BATH ENVIRONMENTAL CONTROL SYSTEM 5-2.1

Principle The Fluid Bath environmental control system continuously cycles fluid through an open transfer system between a circulator and the Fluid Bath, which is located directly beneath the Lower Fixture.




5-2.2

Circulator Connection

Fluid and electrical connections to the circulator are shown in Figure 5-1. At the time this document was published, it was determined that the fluid hoses should be pushed over the Circulator fluid nozzles and secured with hose clamps.

5-2.3

Filling the Circulator

Depending on the desired operating range of the circulator, fill the circulator with fluid as specified in Table 5-1.

WARNING TOXICITY

In Table 5-1 below, SF 96-50 silicon fluid emits toxic fumes when heated to a temperature greater than +140°C. Use SF 96-50 silicon fluid above +140°C only if an externally-vented exhaust hood is installed above the circulator. Ensure that exhaust airflow is adequate to expel fumes emitted from the circulator. Failure to heed this warning may result in injury or death.

Table 5-1 Circulator Operating Ranges and Fluids

Desired Circulator Operating Range (bath range is slightly less) Fluid

-20°C to +30°C 100% Dow Corning® Syltherm® XLT

+1°C to +99°C 100% water

-5°C to +90°C 20% ethylene glycol / 80% water

+40°C to +130°C 100% ethylene glycol

0°C to +200°C (see WARNING above) 100% SF 96-50 silicon fluid


33

Figure 5-1 Circulator Connections


34

5-2.4

RSI Orchestrator Fluid Bath

Configuration

Prior to using RSI Orchestrator software to control circulator temperature, ensure that RSI Orchestrator Instrument Testing Limits are set to use the bath as follows:

a. Select the Instrument Configuration function (Utilities: Service menu). The Instrument Options dialog box (Figure 5-2) is displayed.

Figure 5-2 Bath Instrument Configuration

b. Select the following items from the drop lists: Instrument Setup ............... Temperature Control Temperature Control ............. Bath (Instrument Controlled Only) c. Enter the Maximum and Minimum Temperatures corresponding to the

desired circulator operating range and fluid (see paragraph 5-2.3 Filling the Circulator on page 32).

d. Select either Temperature Loop Control option, using the following information as a guideline: 1. Circulator Temperature When selected, the temperature of the fluid in the circulator is maintained

at the commanded temperature. This is monitored independent of the instrument. Commanded temperature will be achieved faster than selecting Tool Temperature (below), but Bath temperature will differ slightly from that commanded.

2. Tool Temperature When selected, the temperature of the lower test fixture is maintained at

the commanded temperature. Tool Temperature is the recommended setting for general testing. Compared to Circulator Temperature (above), bath temperature will more closely match that commanded, but it will require 20 to 30 minutes for the commanded temperature to be achieved.


35

5-3 PELTIER ENVIRONMENTAL CONTROL SYSTEM 5-3.1

Principle The Peltier environmental control system utilizes a solid-state heat pump (thermopile) to control the temperature of the lower fixture, which is an integral part of the Peltier assembly. In general, the solid state heat pump consists of multiple semiconductor devices in series, each composed of an N-P junction. The devices are placed between the lower fixture and a heat sink (Figure 5-3).

Figure 5-3 Solid State Heat Pump (Peltier Element) Schematic

A DC voltage is applied across the semiconductors to either heat or cool the

lower fixture, depending on the polarity of the voltage. The semiconductors transfer thermal energy between the lower fixture and the heat sink, which is essentially a heat exchanger through which fluid (typically water) is circulated. The fluid temperature determines the amount of thermal energy that the heat sink can source to or sink from the lower fixture. The fluid temperature thereby determines the Peltier system thermal operating range (see paragraph 5-3.3 Selecting a Thermal Operating Range on page 36).


36

5-3.2

Tentative Specifications

Temperature Range -40°C to +210°C, depending on circulator fluid temperature (see the next paragraph 5-3.3 Selecting a Thermal Operating Range)

Ramp Rate 50°C per minute from 0°C to +100°C (at 20°C circulator fluid temperature)

Stability ±0.1°C

5-3.3

Selecting a Thermal

Operating Range

Thermal operating range is the Peltier system temperature range at a given fluid temperature. To select a thermal operating range, fluid temperature must be set in accordance with the following guideline.

NOTE The temperature differentials given below are estimated.

Assuming that the ambient temperature in the vicinity of the heat sink is +20°C, a differential (ΔT) of -40°C exists between the fluid temperature and the lower limit of the thermal operating range. A ΔT of +80°C exists between the fluid temperature and the upper limit of the thermal operating range. To determine thermal operating range, add these differentials to the fluid temperature. For example, at a fluid temperature of +20°C, the thermal operating range of the Peltier system is -20°C to +100°C, calculated as follows:

Lower Limit Upper Limit

ΔT + (+20°C) = ΔT + (+20°C) = -40°C + (+20°C) = -20°C +80°C + (+20°C) = +100°C

At a fluid temperature of +40°C, the thermal operating range of the Peltier system is 0°C to +120°C, calculated as follows:

Lower Limit Upper Limit

ΔT + (+40°C) = ΔT + (+40°C) = -40°C + (+40°C) = 0°C +80°C + (+40°C) = +120°C


37

5-3.4

Installation The Peltier Fixture is a self-contained unit that simply mounts onto the base of the instrument.



Turn OFF the Circulator prior to removing or installing the Peltier Fixture. The Fluid Bath is an open vat of fluid that is sealed only when the Peltier Fixture is installed. Failure to turn OFF the Circulator prior to fixture removal and installation will cause the Fluid Bath to overflow, resulting in possible injury and extensive damage to this instrument.

Refer to Figure 5-4 during the following procedure.

Installation a. Raise the stage to maximum height (see paragraph 2-3.1 Stage on page 12). b. Push the Peltier Fixture fully into the base, aligning the four captive screws

with the tapped holes in the base. c. Tighten the four captive screws in the Peltier Fixture (do not over-torque). d. Connect the cable to the receptacle.

Removal a. Raise the stage to maximum height (see paragraph 2-3.1 Stage on page 12). b. Disconnect the cable from the receptacle. c. Loosen the four captive screws in the Peltier Fixture. c. Pull the Peltier Fixture from the base.

NOTE The Peltier fixture is a Lower Fixture for use only with Parallel Plate or Cone and Plate Upper Fixtures.


38

FRONT OF INSTRUMENT

VIEW LOOKING DOWNWARD FROM THE TOP OF THE INSTRUMENT

PELTIER FIXTURE

CABLE

RECEPTACLE(connected to

EnvironmentalController)

NOTE

Early production units are equipped with eight mounting holes. If your unit is so equipped, align the captive screws on the Peltier Fixture with the holes shown (at left) filled in black.

CAPTIVE SCREWS

Figure 5-4 Installation of Peltier System

5-3.5 Supply fluid to the Peltier system by connecting the fluid source to the instrument


39

Circulator Options

Bath hoses (see Figure 5-1). You have a choice of two fluid sources, depending upon your needs: • Peltier Circulator (specifications not yet available) Manufactured by Rheometric Scientific, the Peltier Circulator is an effective

yet inexpensive means of providing recirculant. Instructions for use of the Peltier Circulator are printed on the label that is affixed to the circulator.

• Commercial Circulator A commercial fluid circulator must be used to operate the Peltier system over

its entire specified temperature range. For information concerning fluid connection to the instrument, as well as fluids for use in achieving specified temperature ranges, see the following paragraphs: • Paragraph 5-2.2 Circulator Connection on page 32 • Paragraph 5-2.3 Filling the Circulator on page 32

5-3.6 RSI Orchestrator

Peltier Configuration

Prior to using RSI Orchestrator software to control circulator temperature, ensure that RSI Orchestrator Instrument Testing Limits are set to use the bath as follows:

a. Select the Instrument Configuration function (Utilities: Service menu). The Instrument Options dialog box is displayed.

Figure 5-5 Peltier Instrument Configuration

b. Select the following items from the drop lists: Instrument Setup ............... Temperature Control Temperature Control ............. Peltier (Thermopile Heat Pump) c. Enter the Maximum and Minimum Temperatures in accordance with the

heat sink fluid temperature and the corresponding thermal operating range (see paragraphs 5-3.1 Principle on page 35, and 5-3.3 Selecting a Thermal Operating Range on page 36).

For example, if the fluid temperature is +20°C, Set the Minimum Temperature to -20°C, and the Maximum Temperature to +100°C.

5-4 HUMIDITY COVER


40

5-4.1 Principle

When used with the Fluid Bath or Peltier Environmental Control Systems, the Humidity Cover helps prevent evaporation of samples and/or solvents. This device consists of the following components (see Figure 5-6): a. Cover The two-piece Cover is placed onto the Lower Fixture, providing a more

closed environment than open atmosphere. b. Well The steel Well is placed onto the Cover. The solvent for the sample under

test is placed in the Well, which is removable for cleaning. c. Trap The spring-loaded Trap is placed onto the Upper Fixture. After the sample is

loaded and the Gap set, the Trap is lowered until immersed in the solvent-filled Well.

TRAP

COVER(LEFT HALF)

WELL(REMOVABLE)

COVER(RIGHT HALF)

Figure 5-6 Humidity Cover

The Cover, Well, and Trap form a relatively sealed chamber. As the sample and/or solvent evaporates, the atmosphere within the chamber nears saturation, thus slowing evaporation.

5-4.2 Usage

To use the Humidity Cover, perform the following steps:

a. Install the Trap onto the Upper Fixture as follows: 1. Separate the two halves of the Trap by removing the spring that holds

them together. 2. Place each half on either side of the fixture shaft, and fasten the halves

together by replacing the spring. 3. Push the Trap as far as it will go toward the top of the fixture.

b. Install the Upper Fixture. c. Perform AutoCal (see paragraph 3-4 AUTOCAL on page 18). This is

necessary because the Trap has added mass to the Upper Fixture. d. Load the sample (complete procedures are contained in Chapter 3, which

begins on page 14). e. Place the left and right halves of the Cover onto the Lower Fixture, and seal

the two halves by pressing them together.


41

f. If you wish to purge the internal atmosphere of the Cover, connect a nitrogen gas purge line to the connector (not shown) that is mounted on the Cover.

g. Place the Well onto the Cover. h. Fill the Well with the sample solvent.

NOTE In the next step, do not allow the Trap to touch the Well. The Upper Fixture must be able to rotate freely.

i. Push the Trap downward until it is submersed in the solvent that is contained in the Well.


42

INDEX

Air Bearing

caution concerning instrument damage, 10 Air Dryer

caution concerning instrument damage, 10 Anvil

identification, 12 locking and unlocking, 12

Anvil Stop Control, 12 AutoCal (Automatic Fixture Inertia Calculation), 18

Cal Curve, 29 Calibration

Cal Curve Examination, 29 Kit, 24 list of required calibrations, 23 Normal Force, 30 Spin Correction, 28 Torque, 25

Cone and Plate Gap setting, 21 loading samples, 21 test temperatures, 21

Couette loading samples, 22

Environmental Controller monitoring, 13

Fixtures Lower, installation/removal, 15 Upper, installation and removal, 17

Fluid Bath configuration, 34 filling the circulator, 32

principle, 32 Gap

setting, 20 zeroing, 19

Humidity Cover principle of operation, 40 usage, 40

Instrument description, 7 Manual Organization, 7 Normal Force

Calibration, 30 Parallel Plate

Gap setting (recommended), 20 loading samples, 20

Peltier Option circulator options, 39 configuration, 39 installation, 37 specifications, 36 thermal operating range, 36

Peltier System principle of operation, 35

RSI Orchestrator Online Help, 7 Specifications, instrument, 8 Spin Correction, 28 Stage, 12 Test Station

component identification, 11 Torque

Calibration, 25 Track Mode, 19 User Interface, 12

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