TA Instruments TMA 2940 CE User manual

TA I NSTRUMENTS TMA 2940 CE I
TMA 2940 CE
Thermomechanical Analyzer
Operator’s Manual
PN 825615.001 Rev. C (Text and Binder)
PN 825615.002 Rev. C (Text Only)
Issued November 1999
109 Lukens Drive New Castle, DE 19720
Thermal Analysis & Rheology
A S UBSIDIARY OF W ATERS C ORPORATION

TA I NSTRUMENTS TMA 2940 CE II
© 1997, 1999 by TA Instruments, Inc.
109 Lukens Drive
New Castle, DE 19720
Notice
The material contained in this manual is believed
adequate for the intended use of this instrument.
If the instrument or procedures are used for
purposes other than those specified herein,
confirmationoftheirvalidityandsuitabilitymust
be obtained from TA Instruments, Inc. Other-
wise, TA Instruments does not guarantee results
and assumes no obligation or liability. This
publication is not a license to operate under nor a
recommendation to infringe upon any process
patents.
TA Instruments TA Operating Software and
Instrument, Data Analysis, and Utility Software
and their associated manuals are proprietary and
copyrighted by TA Instruments, Inc. Purchasers
are granted a license to use these software
programs on the instrument and controller with
which they were purchased. These programs
may not be duplicated by the purchaser without
the prior written consent of TA Instruments.
Each licensed program shall remain the exclusive
property of TA Instruments, and no rights or
licenses are granted to the purchaser other than
as specified.

TA I NSTRUMENTS TMA 2940 CE III
Table of Contents
Notes, Cautions, and Warnings ............... xi
Helplines .................................................. xii
Safety .......................................................... xiii
CE Compliance..................................... xiii
InstrumentSymbols .............................. xiv
Electrical Safety .................................... xv
HandlingLiquidNitrogen....................... xv
Lifting the Instrument .......................... xvii
Using This Manual ................................. xvii
CHAPTER 1: Introducing
the TMA 2940 CE ................................... 1-1
Introduction 1-3
Components .......................................... 1-3
The 2940 CE Instrument............................. 1-5
2940 CE Display................................... 1-7
2940 CE Keypad .................................. 1-7
HEATER Switch.......................... 1-11
POWER Switch ........................... 1-11

TA I NSTRUMENTS TMA 2940 CE IV
Table of Contents
(continued)
Accessories............................................... 1-12
Standard Accessories ......................... 1-12
OptionalAccessories .......................... 1-13
Specifications ............................................ 1-14
CHAPTER 2: Installing
the TMA 2940 CE ................................... 2-1
Unpacking/Repacking the 2940 CE ............ 2-3
Unpacking the 2940 CE........................ 2-3
RemovingtheShippingMaterial ........... 2-6
Repacking the 2940 CE........................ 2-8
Installingthe Instrument.............................. 2-9
Inspecting the System......................... 2-10
Choosing a Location ........................... 2-11
Installing the Weight Tray Door ......... 2-12
Installing the Stage ............................. 2-13
InstallingtheExpansion/
Penetration Probes ............................. 2-17
Installing a Probe ......................... 2-17
Removing a Probe ....................... 2-18
Connecting Cables and Gas Lines...... 2-19
GPIB Cable.................................. 2-19
Purge Line ................................... 2-22
Air Cool Line ............................... 2-24
Power Cable ................................ 2-25

TA I NSTRUMENTS TMA 2940 CE V
Table of Contents
(continued)
Starting the 2940 CE ................................. 2-26
Shutting Down the 2940 CE...................... 2-28
CHAPTER 3: Running
Experiments ............................................. 3-1
Overview .................................................... 3-3
Before You Begin ................................ 3-4
Calibrating the TMA ................................... 3-5
ForceCalibration .................................. 3-5
ProbeCalibration .................................. 3-6
TemperatureCalibration ....................... 3-6
Heater Temperature Calibration .......... 3-8
Cell Constant ........................................ 3-9
Running a TMA Experiment..................... 3-10
Experimental Procedure ..................... 3-10
Selecting a Probe................................ 3-11
Zeroing the Auto Measure System .... 3-12
Sample Preparation and Loading .............. 3-13
Sample Preparation ...................... 3-13
SampleLoading............................ 3-13

TA I NSTRUMENTS TMA 2940 CE VI
Table of Contents
(continued)
ThermocouplePositioning................... 3-15
Measuring the
Sample Length.................................... 3-15
Setting Up an Experiment................... 3-16
Setting Up Accessories ...................... 3-17
Using Air Cool ............................. 3-17
Using a Purge Gas ....................... 3-18
Suggestions ............................ 3-18
Starting an Experiment ....................... 3-19
StoppinganExperiment ...................... 3-20
RemovingSamples....................... 3-20
SubambientExperiments........................... 3-22
Performing a Cooling Experiment ...... 3-22
Techniques for Improved
SubambientOperation ........................ 3-23
CHAPTER 4: Using
Your Options ............................................ 4-1
Overview .................................................... 4-3
Film/Fiber Accessory .................................. 4-4
Description ........................................... 4-4
Operating Procedures........................... 4-5

TA I NSTRUMENTS TMA 2940 CE VII
Table of Contents
(continued)
Accessory Installation .......................... 4-5
Removing the Existing Probe ......... 4-6
Removing the Stage....................... 4-6
Changing the Instrument Mode ..... 4-7
InstallingtheFilm/FiberProbe ....... 4-7
InstallingtheFilm/FiberStage ....... 4-8
Calculating the Offset .................... 4-9
Calibration........................................... 4-11
Sample Preparation ............................ 4-12
Using the Aluminum Balls ........... 4-12
Using the Stainless
Steel Clamps ................................ 4-14
Flexure Accessory .................................... 4-17
Description ......................................... 4-17
Accessory Installation ........................ 4-18
Calibration........................................... 4-18
Sample Preparation ............................ 4-19
Dilatometer Accessory ............................. 4-21
Description ......................................... 4-21
Operating Procedures......................... 4-23
Considerations .............................. 4-23
Accessory Installation ........................ 4-23
Calibration........................................... 4-24
BaselineCalibration ..................... 4-24
DisplacementCalibration ............. 4-25

TA I NSTRUMENTS TMA 2940 CE VIII
Table of Contents
(continued)
Sample Preparation ............................ 4-26
Parallel Plate Rheometer Accessory ........ 4-29
Description ......................................... 4-29
Accessory Installation ........................ 4-29
Calibration........................................... 4-30
Sample Preparation ............................ 4-31
Sample Encapsulating Press ........ 4-31
Preparing Moldable Powders....... 4-35
Preparing Resinous Materials ...... 4-38
Preparing Sheet Materials. .......... 4-40
SampleLoading .................................. 4-41
Cleanup ........................................ 4-42
Calculations ........................................ 4-43
Hemispherical Probe ................................. 4-47
CHAPTER 5: Technical
Reference.................................................. 5-1
Description of the TMA 2940 CE ............. 5-3
Uses of
ThermomechanicalAnalysis ................ 5-4
Calculatingthe
Coefficient of Expansion ...................... 5-5

TA I NSTRUMENTS TMA 2940 CE IX
Table of Contents
(continued)
MethodConsiderations ............................... 5-6
Status Codes ............................................... 5-7
CHAPTER 6: Maintenance
and Diagnostics ........................................ 6-1
Overview .................................................... 6-3
Routine Maintenance .................................. 6-4
Inspection ............................................. 6-4
Cleaning ................................................ 6-5
Cleaning the Keypad...................... 6-5
Cleaning the Probe Assembly ........ 6-5
Cleaning the Stage ......................... 6-6
Cleaning the Thermocouple ........... 6-7
Replacements.............................................. 6-8
Replacing the Thermocouple ................ 6-8
Diagnosing Power Problems..................... 6-11
Fuses .................................................. 6-11
Furnace Power Check ................. 6-12
Heater Indicator Light ........................ 6-13
Power Failures ................................... 6-14

TA I NSTRUMENTS TMA 2940 CE X
Table of Contents
(continued)
TMA 2940 CE Test Functions.................. 6-15
The TMA Confidence Test................ 6-15
Replacement Parts .................................... 6-18
APPENDIX A: Ordering
Information............................................... A-1
INDEX ........................................................I-1

TA I NSTRUMENTS TMA 2940 CE XI
Notes, Cautions,
and Warnings
This manual uses NOTES, CAUTIONS, and
WARNINGS to emphasize important and critical
instructions under the guidelines described below:
Highlights important information about equip-
ment or procedures.
Emphasizes a procedure that may damage
equipment or cause loss of data if not followed
correctly.
Marks a procedure that may be hazardous
to the operator or to the environment if not
followed correctly.
! WARNING
NOTE:
t CAUTION:

TA I NSTRUMENTS TMA 2940 CE XII
Helplines
To TA Instruments
For Technical Assistance......... [phone]
To Order Instruments and
Supplies .................................... [phone]
For Service Inquiries ................ [phone]
Sales......................................... [phone]

TA I NSTRUMENTS TMA 2940 CE XIII
Safety This equipment, when used with the stepdown
transformer (PN 994560.901), has been designed
to comply with the following standards on safety:
 IEC 1010-1/1990 + A1/1992 + A2/1995
 IEC 1010-2-010/1992 + A1/1996
 EN 61010-1/1993 + A2/1995
 EN61010-2-010/1994
 UL 3101-1, First Edition.
CE Compliance
In order to comply with European Council
Directive 89/336/EEC (EMC Directive) and
Council Directive 73/23/EEC on safety as
amended by Council Directive 93/68/EEC, the
following specifications apply to the TMA 2940
CE instrument, when used with the stepdown
transformer (PN 994560.901):
Safety:
EN 61010-1/1993 + A2/1995 Installation
Category II
EN61010-2-010/1994
Emissions:
EN 55022: 1995, Class B (301000 MHz)
radiated
EN 55022: 1995, Class B (0.1530 MHz)
conducted
Immunity:
EN 50082-1: 1992 Electromagnetic
CompatibilityGenericimmunitystandard
Part 1. Residential, commercial, and light
industry.
 IEC 801-2: 1991, 8 kV air discharge.
 IEC 801-3: 1984, 27500 MHz, 3V/m.
No response above 20 µm and 5.0°C
sample temperature.
 IEC 801-4: 1988 Fast transients com-
mon mode 1kV AC power.

TA I NSTRUMENTS TMA 2940 CE XIV
Safety
(continued)
Instrument Symbols
The following labels are displayed on the TMA
2940 CE instrument for your protection:
Symbol Explanation
Thissymbol,which
appears on the furnace
enclosure and on the stage
can of the TMA 2940 CE,
indicates that a hot
surface may be present.
Take care not to touch
these areas or allow any
material that may melt or
burn to come in contact
with these hot surfaces.
Please heed the warning labels and take the
necessary precautions when dealing with those
parts of the instrument. The TMA 2940 CE
Operator's Manual contains cautions and
warnings that must be followed for your own
safety.

TA I NSTRUMENTS TMA 2940 CE XV
Safety
(continued)
Electrical Safety
Voltages exceeding 110 V ac are present in this
system. Always unplug the instrument before
performing any maintenance.
Because of the high voltages in this instru-
ment, untrained personnel must not remove
the cabinet cover unless specifically directed
to do so in the manual. Maintenance and
repair of internal parts must be performed
by TA Instruments or other qualified service
personnel only.
After transport or storage in humid condi-
tions, this equipment could fail to meet all
the safety requirements of the safety
standards indicated. Refer to the NOTE on
page 2-10 for the method of drying out the
equipment before use.
Handling Liquid Nitrogen
The TMA 2940 CE can use the cryogenic (low-
temperature) agent, liquid nitrogen, for cooling in
subambient experiments. Because of its low
temperature (195°C), liquid nitrogen will burn
the skin. Use extreme caution when working
with liquid nitrogen and other cryogenic materials
to ensure that you do not burn yourself.
Personnelworkingwithliquidnitrogenshould
take the precautions listed on the next page.
! WARNING
! WARNING

TA I NSTRUMENTS TMA 2940 CE XVI
Safety
(continued)
WARNING: Liquid nitrogen evaporates
rapidly at room temperature. Be certain
that areas where liquid nitrogen is used are
well ventilated to prevent depletion of
oxygen in the air.
1. Wear goggles or a face shield, gloves that
are large enough to be removed easily, and a
rubber apron. For extra protection, wear
high-topped, sturdy shoes, and leave your
pant legs outside the shoe tops.
2. Transfer the liquid slowly to prevent thermal
shock.
3. Use containers that have adequate low-
temperature properties. Ensure that closed
containers have vents to relieve pressure;
liquid nitrogen evaporates rapidly at room
temperature.
4. The purity of liquid nitrogen alters as it
evaporates. If much of the liquid in the
container has evaporated, check the remain-
ing liquid before using it for any purpose in
which high oxygen content is dangerous.
! WARNING

TA I NSTRUMENTS TMA 2940 CE XVII
Safety
(continued)
IF BURNED BY LIQUID NITROGEN...
1. Flood the area (skin or eyes) with large
quantities of cool water IMMEDIATELY;
then apply cold compresses.
2. See a doctor IMMEDIATELY if the skin is
blistered or if there is a chance of eye
infection.
Lifting the Instrument
The TMA 2940 CE is a fairly heavy instrument.
In order to avoid injury, particularly to the back,
please follow this advice:
Use two people to lift and/or carry the
instrument. The instrument is too heavy for
one person to handle safely.
! WARNING

TA I NSTRUMENTS TMA 2940 CE XVIII
Using This Manual
CHAPTER 1 Introduces the TMA 2940
CE and lists its specifica-
tions.
CHAPTER 2 Describes how to install
and assemble your TMA
2940 CE.
CHAPTER 3 Describes routine opera-
tion of the TMA instru-
ment,includingsubambi-
ent operations.
CHAPTER 4 Contains the procedures
used to operate the TMA
with the optional accesso-
ries.
CHAPTER 5 Explains thetechnical
aspects of the TMA and
itsoperation.
CHAPTER 6 Provides maintenance and
diagnostic procedures.
Appendix A Lists TA Instruments
offices that you can
contact to place orders,
receive technical assis-
tance, and request ser-
vice.
Index Contains an alphabetical
list of topics and page
number references.

TA I NSTRUMENTS TMA 2940 CE XIX
Potential Asphyxiant
Liquid nitrogen can cause rapid suffocation without
warning.
Store and use in an area with adequate ventilation.
Do not enter confined spaces where nitrogen gas
may be present unless the area is well ventilated.
The warning shown above applies to the use of liquid nitrogen.
Oxygen depletion sensors are sometimes utilized where liquid
nitrogen is in use.
! WARNING

TA I NSTRUMENTS TMA 2940 CE XX