Waters TA Instruments Sample/Temperature Stage Manual

TA I NSTRUMENTS S AMPLE /T EMPERATURE S TAGE i
Thermal Analysis & Rheology
A SUBSIDIARY OF WATERS CORPORATION
Sample/
Temperature
Stage
Accessory for the µTA 2990
TM
Operator's Guide
PN 899038.001 Rev. A
Issued July 2000

ii TA I NSTRUMENTS S AMPLE /T EMPERATURE S TAGE
Sample/Temperature Stage
© 2000 by TA Instruments
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,
confirmation of their suitability must be obtained
from TA Instruments. Otherwise, TA Instru-
ments does not guarantee any results and
assumes no obligation or liability. This publication
is not a license to operate under or a recommen-
dation to infringe upon any process patents.
TA Instruments Instrument Control, Data
Analysis, and Utility Software and their associ-
ated 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 dupli-
cated by the purchaser without the prior written
consent of TA Instruments. Each licensed
program shall remain the exclusive property of
TA Instruments, and no rights or licenses are
granted to the purchaser other than as specified
above.

TA I NSTRUMENTS S AMPLE /T EMPERATURE S TAGE iii
Hotlines to TA Instruments ............................ v
Part Numbers................................................ vii
Notes, Cautions and Warnings ..................... viii
Safety .............................................................ix
HighVoltage ............................................ix
Safe Handling of
Cryogenic Materials ................................ x
Handling Liquid
Nitrogen ................................................... x
If Burned by
Liquid Nitrogen ........................................xi
RoomVentilation .....................................xi
OxygenAbsorption ..................................xi
Instrument Symbols ............................... xiii
Introducing the Sample/
Temperature Stage ...................................... 1-1
Description ........................................... 1-2
Specifications........................................ 1-4
Principles of Operation ......................... 1-5
Installing theSample/
Temperature Stage ...................................... 1-7
Choosinga Location ............................. 1-7
Power Requirements ..................... 1-7
Unpacking andAssembly ..................... 1-8
Installing the Sample Cover ................ 1-11
Filling the Cooling Canister ................. 1-13
Operating the Sample/
Temperature Stage .................................... 1-15
Basic Procedure ................................. 1-15
Using the Stage Controller ................. 1-17
Setting the Rate............................ 1-18
Table of Contents

i v TA I NSTRUMENTS S AMPLE /T EMPERATURE S TAGE
Sample/Temperature Stage
Selecting the
Target Temperature ..................... 1-20
Using the Start/Finish Button ....... 1-21
Using the Hold Button ................. 1-22
Using the Heat/Cool Button......... 1-23
Sample Procedure........................ 1-24
PerformingTemperature Calibration ........ 1-25
Removing the
Old Calibration Factors....................... 1-25
Obtaining New Positive
Calibration Factors ............................. 1-26
Entering the New
Calibration Factors ............................. 1-27

TA I NSTRUMENTS S AMPLE /T EMPERATURE S TAGE v
Hotlines to TA Instruments
TA Instruments, Inc.
109 Lukens Drive
New Castle, DE 19720
Telephone: [phone] or 1-302-427-4040
Fax: [phone]
Email address: http://www.tainst.com; click
on Answerman icon.
HELPLINEU.S.A.: For technical assis-
tance with current or potential thermal
analysis applications, phone the Thermal
Analysis Help Desk at (302)427-4070.
SERVICEU.S.A.: For instrument service
and repairs, phone [phone].
TA Instruments Ltd.
Europe House, Bilton Centre
Cleeve Road
Leatherhead, Surrey KT22 7UQ
England
Telephone: [phone]
Fax: [phone]
TA Instruments Spain
Waters Cromatografía, S.A.
División TA Instruments
Avda. Europa, 21. Pta. Baja
28108 Alcobendas
Madrid
Spain
Telephone: [phone]
Fax: [phone]
TA Instruments France
B.P. 608
78056 Saint-Quentin-Yvelines
Cedex
France
Telephone: [phone]
Fax: [phone]

v i TA I NSTRUMENTS S AMPLE /T EMPERATURE S TAGE
Sample/Temperature Stage
TA Instruments GmbH
Max-Planck-Strasse 11
D-63755 Alzenau
Germany
Telephone: [phone]
Fax: [phone]
TA Instruments Belgium, a Division of Waters
s.a/n.v.
Raketstraat 60
B-1130 Brussels
Telephone: [phone]
Fax: [phone]
TA Instruments The Netherlands
A Division of Waters Chromatography B.V.
Florijnstraat 19
4879 AH Etten-Leur
Telephone: [phone]
Fax: [phone]
TA Instruments, Japan
No. 5 Koike Bldg.
1-3-12 Kitashinagawa
Shinagawa-Ku, Tokyo 140
Japan
Telephone: [phone]
Fax: [phone]
TA Instruments Australia
Unit 3
38-46 South Street
Rydalmere NSW 2116
Australia
Telephone: [phone]
Fax: [phone]
TA Instruments Italy
Division of Waters SpA
via Achille Grandi 27
20090 Vimodrone (MI)
Italy
Telephone: [phone]
Fax: [phone]

TA I NSTRUMENTS S AMPLE /T EMPERATURE S TAGE vii
Part Numbers
If you need to order a replacement part for your
Sample/Temperature Stage, refer to the follow-
ing list of parts and then contact your service
representative or the TA Instruments office
closest to you. A list of the offices can be found
on page v.
Part Number Description
899037.001 Funnel
899036.001 Sample Cover
899038.001 Manual Sample/Tempera-
ture Stage
271446.001 Spacer

viii TAI NSTRUMENTS S AMPLE /T EMPERATURE S TAGE
Sample/Temperature Stage
Notes, Cautions and Warnings
The following conventions are used throughout
this manual to point out items of importance and
safety as you read through the instructions.
A NOTE highlights important information
about equipment or procedures.
A CAUTION emphasizes a procedure that
may damage equipment or cause loss of data
if not followed correctly.
A WARNING indicates a procedure that may
be hazardous to the operator or to the
environment if not followed correctly.
NOTE:
t CAUTION:
! WARNING

TA I NSTRUMENTS S AMPLE /T EMPERATURE S TAGE ix
Safety
Please read the safety information contained in
this section carefully BEFORE using the instru-
ment. The knowledge that you gain could save
you from injury or equipment damage as you use
the Sample/Temperature Stage.
High Voltage
Wherever high voltage is present on the
system, extreme care should always be
taken to avoid direct contact while the
instrument hardware is powered on. Call TA
Instruments Service for repairs. We do not
recommend that you make any attempt to
remove the panels on the instrument. If
you do attempt your own repairs, always
turn the power off before attempting to
remove any panels or PC boards and before
touching any connectors by hand or with
electrically conductive tools. High voltage is
present at the following locations on the
system and where the symbol is
located:
• Power/connection cables: Temperature
Stage and Controller.
! WARNING

x TA I NSTRUMENTS S AMPLE /T EMPERATURE S TAGE
Sample/Temperature Stage
Safety
(continued)
Safe Handling of
Cryogenic Materials
Liquid nitrogen is used as a cooling agent in
many thermal analysis tests. Becuase of its
extremely low temperature (196°C), it will burn
the skin. You must use extreme care when
working with liquid nitrogen or other cryogenic
materials.
Liquid nitrogen can:
1. Cause serious skin burns.
2. Replace the air in the room you are in.
3. Generate very high pressures if trapped in
lines or containers.
Handling Liquid
Nitrogen
1. Wear goggles or a face shield, gloves large
enough to be removed easily, and a rubber
apron. For extra protection, wear high-
topped, sturdy shoes, and leave your pant
legs outside the shoe tops.
2. Transfer the liquid slowly to prevent thermal
shock to the container and excessive turbu-
lence to the liquid nitrogen, If liquid nitrogen
is poured into a container that is at room
temperature, the liquid nitrogen will boil
violently. Use extreme caution to prevent the
boiling liquid from contacting you.

TA I NSTRUMENTS S AMPLE /T EMPERATURE S TAGE xi
Safety
(continued)
3. Use only approved low-temperature contain-
ers.
4. Make sure liquid nitrogen cointainers are
vented to prevent pressure buildup.
If Burned by
Liquid Nitrogen
1. Flood the area (skin or eyes) IMMEDI-
ATELY with large quantities of cool water,
and then apply cold compresses.
2. See a doctor IMMEDIATELY if the skin is
blistered or if the liquid nitrogen came in
contact with your eyes.
Room Ventilation
Liquid nitrogen evaporates quickly at room
temperature and could replace the air in a room.
Use liquid nitrogen in a well-ventilated room
ONLY. Importantsee the Warning on page ?.
Oxygen Absorption
Liquid nitrogen absorbs oxygen from the air. It is
possible for the purity of liquid nitrogen to change
as it evaporates from a container. If you suspect
that a lot of liquid nitrogen has evaporated, the
remaining liquid should be analyzed for oxygen
content before being used for any purpose for
which a high oxygen content is dangerous.

xii TAI NSTRUMENTS S AMPLE /T EMPERATURE S TAGE
Sample/Temperature Stage
Potential Asphyxiant
Liquid nitrogen can cause rapid suffocation without warning.
Store and use in an area with adequate ventilation.
Do not vent a liquid nitrogen container in a confined space.
Do not enter a confined space where nitrogen gas may be
present unless the area is well ventilated.
The above warning applied to the use of liquid
nitrogen. Oxygen depletion sensors are some-
times utilized where liquid nitrogen is in use.
Please refer to the rest of this section for more
detailed instructions regarding safety in the use
of the Temperature Stage.
! WARNING

TA I NSTRUMENTS S AMPLE /T EMPERATURE S TAGE xiii
Instrument Symbols
The following labels are displayed on the µTATM
Sample/Temperature Stage for your protection:
Label Explanation
Indicates the presence of
high voltage. Turn off the
power to the instrument
when directed. Follow all
safety precautions listed in
this manual to avoid injury.
Please heed these labels and take the necessary
precautions when dealing with those parts of the
instrument. This manual contains cautions and
warnings that must be followed for your own
safety.

xiv TAI NSTRUMENTS S AMPLE /T EMPERATURE S TAGE
Sample/Temperature Stage

TA I NSTRUMENTS S AMPLE /T EMPERATURE S TAGE 1
Introducing the Sample/
Temperature Stage
The TA Instruments Sample/Temperature Stage
is designed to be used with the TA Instruments
µTATM* (Micro-Thermal Analyzer) 2990, in
place of the AFM sample stage originally
supplied with the µTA 2990.
Just as with the original sample stage, you can
run experiments by affixing the sample to a
mount and then placing it on the Sample/Tem-
perature Stage. Then place the µTA 2990 head
on the Sample/Temperature Stage and you can
begin scanning as described in the µTA 2990
Operator's Manual.
You will find that using the Sample/Temperature
Stage has the following advantages when
performing µTA experiments:
 You can adjust the sample position up and
down manually to minimize the need for
motor controls on the µTA head. A
magnetic plate holds the sample in place,
and you can make Z adjustments by turning
the knurled wheel to move the sample.
 Rather than having to move the sample to
make adjustments in the X and Y directions,
you can move the µTA head for finer
control of such adjustments.
*µTATM is a trademark of TA Instruments, Inc.
Introduction

Sample/Temperature Stage
2 TA I NSTRUMENTS S AMPLE /T EMPERATURE S TAGE
 The Temperature Stage Controller enables
you to image and analyze the sample at
other than ambient temperatures: (1) above
room temperature or (2) below room
temperature with the use of liquid nitrogen.
This manual provides the information necessary
to understand, install, operate, maintain, and
order parts for the TA Instruments Sample/
Temperature Stage.
Description
The Sample/Temperature Stage, shown in
Figure 1 on the next page, consists of the
following:
 A platform with a magnetic plate on three
legs: Two knurled knobs on the sides allow
the sample platform to be moved in the X
and Y directions. A large knurled wheel at
the bottom moves the sample in the Z
direction. Two hold-down screws lock the
sample platform in place.
 A canister mounted below the sample
platform that can be filled with liquid
nitrogen for cooling experiments.
A canister without temperature control capabil-
ity (Ambient Sample Stage) is also available.
 A Sample Cover (metal holder and plastic
shield) to be mounted on the head during
cooling scans: This cover keeps moisture
away from the sample when the
Temperature Stage is used below room
temperature.
NOTE:

TA I NSTRUMENTS S AMPLE /T EMPERATURE S TAGE 3
The Sample Cover must be removed if tem-
peratures above 70°C are to be used. The
plastic in this part will melt at higher tem-
peratures.
 The Temperature Stage Controller, which is
used to control heating and cooling of the
sample during scans at other than ambient
temperatures.
Do not heat the Temperature Stage above
250°C. Doing so would depolarize the sample
mounting magnets.
Figure 1
The Sample/Temperature Stage
and Controller
Introduction
t CAUTION:
Platform
Magnetic
Plate
Knurled Side Knobs
Large Knurled
Bottom Knob
Cooling
Cannister
Hold-Down Screws
t CAUTION:

Sample/Temperature Stage
4 TA I NSTRUMENTS S AMPLE /T EMPERATURE S TAGE
NOTE:
The Sample Stage has no electrical connection,
connector to a controller, or barrel for tem-
perature control.
Specifications
Table 1 contains information about the Sample/
Temperature Stage product specifications.
Table 1
Sample/Temperature
Stage Specifications
Dimensions
Stage Height: 24 cm (9.5 in.)
Width: 18 cm (7 in.)
Depth: 22 cm (8.5 in.)
Controller Height: 8 cm (3.5 in.)
Width: 23 cm (9 in.)
Depth: 33 cm (13 in.)
Power 110/220 or 110/240
Requirements Vac + 10%, de-
pending on country
Temperature 75 to 250°C
Range
Heating/Cooling 0 to 90°C/min
Specifications are subject to change

TA I NSTRUMENTS S AMPLE /T EMPERATURE S TAGE 5
Introduction
Principles of Operation
A DC signal is used to control the temperature
of the Stage. A sample, on a conductive mount,
is held in place by magnets on the Temperature
Stage. A heater mounted under the stage heats
the stage to temperatures as high as 250°C.
Subambient operation is provided by liquid
nitrogen coolant. The heater furnishes heating to
overcome the cryogenic temperature of the liquid
nitrogen to temperatures as low as 75°C.
The Temperature Stage uses a platinum resistor
to sense the temperature. The temperature is
displayed by the Stage Controller to 0.1°C. The
temperature sensor is located near the sample
mount for temperature accuracy.
The Stage Controller has been specifically
designed for precise temperature control of the
Temperature Stage. The Stage sensor is digitally
linearized to give an accurate temperature
readout, and the controls and their functions have
been carefully chosen for simple and easy
operation.
The Temperature Stage is primarily used to
maintain the sample at a constant temperature.
Do not attempt to obtain images or perform
LTA experiments while the sample is being
heated or cooled using the Temperature
Stage as you may damage the Z scanner.
During subambient operation, the magnetic plate
for the sample is positioned over a metal cold
finger, which transmits cold from the canister of
liquid nitrogen to the sample. The sample heater,
t
CAUTION:

Sample/Temperature Stage
6 TA I NSTRUMENTS S AMPLE /T EMPERATURE S TAGE
which surrounds the top of the cold finger,
controls the rate and limit of cooling of the
sample.
The Sample Stage provides the X, Y, and Z
sample movements without temperature adjust-
ment capability.
The Temperature Stage can be used with both
Thermal probes (stage temperature range = 75
to 100°C) and AFM probes (stage temperature
range = 75 to 250°C).