Thermo Scientific TGA User manual

TGA Interface
with OMNIC Paradigm software
User Guide
269-362100 Revision A March 2023

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For Research Use Only. This instrument or accessory is not a medical device and is not
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WARNING
Avoid an explosion or fire hazard.
This instrument or accessory is not designed for use in an explosive
atmosphere.

Safety label locations
The TGA-IR Module comes with numerous safety labels. Heed the label content to avoid
injury or hazard.

TGA-IR Module
The TGA-IR Module allows you to couple your Thermo Scientific Nicolet™ iS™50 and iS20
spectrometers with a Thermogravimetric Analysis (TGA) furnace to run TGA-IR deformulation
experiments when used with our OMNIC Paradigm software. The infrared spectrometer and the
accompanying software provide state-of-the art tools to identify evolved gases and gas mixtures.
Figure 1-1: Nicolet iS50 spectrometer with TGA-IR Module installed
Thermo Scientific TGA Module User Guide 4
Chapter 1

TGA-IR Module
ANicolet iS50 FTIR spectrometer
BTGA-IR Module
Before operating the TGA-IR Module, you should have a working knowledge of your FTIR
spectrometer and the OMNIC™ Paradigm software. You will also need to know the fundamentals of
thermogravimetric analysis and the operating characteristics of your TGA furnace.
Safety label locations 3
TGA-IR Module 4
About the TGA-IR Module 10
Important features 11
Specifications 14
Compatible software 16
Safety and operating precautions 17
TGA-IR sampling 20
Setting up the TGA-IR system 22
Preparing the TGA furnace 22
Preparing the FTIR spectrometer 23
Installing the TGA-IR Module 25
Setting the flow cell and transfer line temperature 37
Checking the detector signal 40
5 TGA Module User Guide Thermo Scientific

Performing a TGA-IR measurement 42
Preparing the TGA-IR system for sampling 42
Samples compatible with TGA-IR 44
Analyzing a test sample 44
Import TGA data 47
Configuring series data collection to start automatically 48
Turning off the TGA-IR system 50
Removing the TGA-IR Module 52
Maintenance 56
Storing the TGA-IR Module 56
Cleaning the TGA-IR Module housing 57
Flow cell maintenance 58
Transfer line maintenance 82
Replacing fuses 84
Troubleshooting 88
Power indicator does not light 88
No heat or heats slowly 89
Transfer line and flow cell heat too rapidly (or very slowly) 90
Input/fail error 90
Temperature overshoot or undershoot 91
No spectroscopic IR signal 91
No detectable sample gas 91
Spectroscopic IR signal is reduced 92
Thermo Scientific TGA Module User Guide 6
TGA-IR Module

TGA-IR Module
WARNING
Avoid personal injury or equipment damage. Read and understand the
accompanying documentation and all safety labels before attempting to install
or use this equipment.
Using this document
This document describes how to install, operate, and maintain the TGA-IR Module and conduct TGA-
IR experiments. It includes important safety precautions; always read and follow these precautions.
For more information about TGA-IR Module safety, refer to the TGA-IR Module Site and Safety
Supplement, which is included in your Thermo Scientific electronic documentation set.
Conventions used
This document uses these conventions for providing safety as well as other important information:
CONVENTIONS USED IN THIS DOCUMENT
DANGER
Avoid hazard. Indicates a hazardous situation which, if not avoided, will
result in serious injury or death.
WARNING
Avoid hazard. Indicates a hazardous situation which, if not avoided,
could result in serious injury or death.
7 TGA Module User Guide Thermo Scientific

CAUTION
Avoid hazard. Indicates a hazardous situation which, if not avoided,
could result in minor or moderate injury.
NOTICE
Follow instructions with this label to avoid damaging the system hardware or losing data.
Note Contains helpful supplementary information.
Tip Provides helpful information that can make a task easier.
Thermo Scientific TGA Module User Guide 8
TGA-IR Module

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About the TGA-IR Module
The TGA-IR Module fits in the sample compartment of a Nicolet Series FTIR spectrometer or AEM,
and connects to the TGA furnace through a heated transfer line.
Figure 2-1: Nicolet iS50 spectrometer with TGA-IR Module installed
Thermo Scientific TGA Module User Guide 10
Chapter 2

About the TGA-IR Module
ANicolet iS50 FTIR Spectrometer
BTemperature controllers (2)
CTGA-IR Module
DHeated transfer line
Important features
Figure 2-2: TGA-IR Module front view
11 TGA Module User Guide Thermo Scientific

ABeam port shutters (2)
BAir vents
CBeam ports (2)
DTransfer line
EPower button
FVoltage select switches (2)
GExhaust tube
HPower switch
IAC power receptacle
TGA-IR Module features include:
lTemperature controllers. Two temperature controllers allow you to specify the temperature of the
flow cell and transfer line. See "Setting the flow cell and transfer line temperature" for more
information.
NOTICE
The temperature controllers are configured at the factory and should be adjusted only by
increasing or decreasing the temperature setting. Do not attempt to reprogram the controllers.
Transfer line. Evolved sample gases from the TGA furnace travel through this precisely heated
line to the heated flow cell inside the TGA-IR Module and then out the exhaust tube, which must
be connected to a fume hood (via an optional peristaltic pump if used). The flow cell is where the
sample interacts with the infrared beam to produce the detector signal in the FTIR spectrometer.
lBeam ports. Infrared light from the spectrometer passes through these ports to the flow cell in the
TGA-IR Module and then continues back to the detector in the spectrometer.
Thermo Scientific TGA Module User Guide 12
About the TGA-IR Module

About the TGA-IR Module
lBeam port shutters. Depending on how these shutters are installed, they allow or prevent the
infrared beam to pass through the TGA-IR Module and back to the spectrometer. The shutters
slide into the holders on the right and left sides of the TGA-IR Module. They must have the end
labeled “Open” positioned on top before the system can collect data.
Open
Allows the infrared beam to enter and
exit the TGA-IR Module during data
collection and seals out the
laboratory environment.
Closed
Blocks beam ports in spectrometer
while the TGA-IR Module heats up,
allowing any excessively humid air to
escape vertically.
NOTICE
Closing the beam port shutters prevents any excessively humid air released from the TGA-IR
Module while it heats up from damaging sample compartment windows or other moisture-
sensitive components in the spectrometer.
l AC power receptacle. Connector for the AC power cord input.
lVoltage select switches. Must be set to match the voltage of the local electricity supply before the
power cord for the TGA-IR Module is plugged into a power outlet.
NOTICE
Always verify that the voltage select switches are set correctly for local electricity requirements
before you plug in the power cord for the TGA-IR Module. If the switches are set incorrectly, the
module may overheat and cause a failure. See "Setting up the TGA-IR system" for details.
lPower switch. Powers the TGA-IR Module on and off. A built-in fuse automatically shuts off power
to the instrument if an over-current condition occurs. For information on recovering from an over
current condition, see "Replacing fuses".
lPower indicator. Illuminates when the power is on.
lAir vents. Release excess heat generated by the TGA-IR Module.
13 TGA Module User Guide Thermo Scientific

CAUTION
Avoid fire hazard. To prevent the TGA-IR Module from overheating, never
block the air vents on the module housing.
Specifications
Feature Specification
Carrier gas (from TGA
furnace)
Recommended materials
Recommended pressure
Recommended flow rate1
Typically nitrogen (inert) or air (oxidative)
5 psi or less
30 mL/min to 100 mL/min2
Transfer line
TGA furnace connector
Vertical movement
Horizontal movement
Connects to 1/8-inch Swagelok™ fitting on most
commercially available TGA furnaces
20 cm (8 inches)
20 cm (8 inches)
Table 2-1:
TGA-IR Module specifications
1Attach a flow meter to exhaust tube on TGA-IR Module to measure flow rate.
2Higher flow rates will greatly reduce TGA-IR sensitivity and TGA balance stability. Check the
documentation that came with your TGA furnace for recommended flow rates.
Thermo Scientific TGA Module User Guide 14
About the TGA-IR Module

About the TGA-IR Module
Feature Specification
Flow cell (inside TGA-IR
Module)
Window material
Volume (total gas volume
inside cell)
Pathlength (inside dimension
window-to-window)
Recommended
pressure/vacuum1
Potassium bromide (KBr) or zinc selenide (ZnSe)
1.332 cubic inches (21832.65 cubic mm)
3.945 inches (100.2 mm)
1 psi (7 kPa) to -3 psi (21 Kpa) vacuum
Variable-flow peristaltic
pump (optional)2
Pump tubing
Recommended flow rate
Silicon (0.25 in internal diameter)
0.4 to 85 mL/min
Operating temperatures3
Flow cell
Transfer line
Ambient to 300 °C (572 °F)
Ambient to 300 °C (572 °F)
FTIR detector
(inside FTIR spectrometer)
Typically DTGS or MCT-B (for faster data collection; for
example, to capture dynamic events)
WARNING
Avoid fire and explosion hazard.
Do not connect a flammable carrier gas to the TGA-IR system.
Keep the workspace clear of flammable materials when the TGA-IR Module
heaters and TGA furnace are powered on and for up to 2 hours after the TGA-
IR Module and furnace are turned off.
1Higher pressures could cause leaks or damage flow cell windows in TGA-IR Module.
2A pump or similar source of suction can be used to draw TGA gases through flow cell at the
optimal rate. The pump must be suitable for liquids and gases. Attach pump to TGA-IR Module
exhaust tube. Direction of flow should pull air through TGA-IR system.
3Both temperature controllers require 30 min to heat from 20 °C to 200 °C (60 min from 20 °C to
300 °C).
15 TGA Module User Guide Thermo Scientific

Compatible software
Software Use for...
OMNIC
Paradigm™
Collecting and analyzing your data. For more information, see
"Performing a TGA-IR measurement".
TQ Analyst
Creating quantitative and classification methods that can be used with
OMNIC Paradigm software. TQ Analyst provides an extensive suite of
chemometrics features you can use to identify raw materials, perform
quantitative analysis and take spectral measurements. For more
information, refer to the help system in TQ Analyst software.
Security Suite Security Suite provides software for security administration, audit
management, control access, and event logging.
Table 2-2:
Software compatible with the TGA-IR Module
Thermo Scientific TGA Module User Guide 16
About the TGA-IR Module

Safety and operating precautions
Safety and operating precautions
Follow these precautions to avoid injury to yourself or others and avoid damaging the TGA-IR Module
during setup or operation.
lThe transfer line is configured at the factory to accommodate a TGA furnace that is located on the
right side of the spectrometer. If your TGA furnace is on the left side of the spectrometer, gently
bend the transfer line so it exits the flow cell to the left. Do not twist the transfer line or exceed its
minimum bend radius of 7.6 cm (3.0 in).
lHandle the transfer line gently and do not exceed its minimum bend radius of 7.6 cm (3.0 in).
Support the transfer line while you transport the TGA-IR Module to avoid damaging or breaking it.
lDo not touch the exposed flow cell windows inside the beam ports on both sides of the TGA-IR
Module. Fingerprints will permanently damage the windows and degrade system performance.
lMake sure the TGA-IR Module voltage select switches are set correctly before you plug in the
power cord. If the switches are set incorrectly for the AC line voltage of your power source, the
module may heat more slowly than expected or overheat and cause a failure.
lBefore you disconnect the transfer line or its electrical connectors, turn off the TGA-IR Module
and unplug the power cord. The transfer line and its electrical connectors serve as the electrical
ground for the flow cell. Do not operate the TGA-IR Module when the transfer line is
disconnected.
lAfter you install the TGA-IR Module, insert the beam port shutters in the “closed” position before
you start the heaters. Leave the shutters in the closed position for the recommended time (4
hours) before you continue, or you may permanently damage the sample compartment windows
or other moisture-sensitive components in the spectrometer.
lThe temperature controllers are configured at the factory and should be adjusted only by
increasing or decreasing the temperature setting. Do not attempt to reprogram the controllers.
lTo prevent the flow cell windows from becoming contaminated, do not turn on the flow cell or
transfer line heaters unless the carrier gas from the TGA furnace is flowing through the flow cell.
lIf your TGA furnace has a separate heater for the evolved gas outlet, we recommend that you turn
on that heater before you start the analysis.
lOperating temperatures below 200 °C (392 °F) can cause the transfer line to become clogged.
17 TGA Module User Guide Thermo Scientific

lDo not use harsh detergents, solvents, propellant gas dusters (“canned air”), chemicals, or
abrasives to clean the TGA-IR Module housing; these can damage the finish and show up as
contaminates during the FTIR analysis.
lDo not use excessive amounts of liquid to clean the module housing or allow the liquid cleaner to
get inside the module.
WARNING
Avoid health hazard. Do not inhale the TGA-IR exhaust. Keep the work area
properly ventilated and connect the exhaust tube to a source of slight vacuum
if used and then to a fume hood.
WARNING
Avoid fire and explosion hazards.
Do not connect a flammable carrier gas to the TGA-IR system.
Keep the workspace clear of flammable materials when the TGA-IR Module
heaters and TGA furnace are powered on and for up to 2 hours after they are
powered off.
Never block the vents on the TGA-IR Module housing or the module may
overheat.
CAUTION
Avoid burn hazards.
Do not touch the flow cell windows, the transfer line fittings, or the exhaust tube
with your body when the heaters are on and for up to 2 hours after you turn
them off. Temperatures can exceed 300 °C (572 °F). Never remove the
insulating material from the transfer line.
If the temperature indicator is red and an “over temperature failure” message
appears on a temperature controller display, turn off the TGA-IR Module power
switch and do not touch the flow cell windows, the transfer line fittings, or the
exhaust tube. Contact us for assistance.
Thermo Scientific TGA Module User Guide 18
Safety and operating precautions

Safety and operating precautions
For more information, refer to the TGA-IR Module Site and Safety Supplement , the site and safety
guide that came with your FTIR spectrometer, and the documentation that came with your TGA
furnace.
19 TGA Module User Guide Thermo Scientific

TGA-IR sampling
Thermogravimetric analysis (TGA) measures a sample’s weight change in a controlled atmosphere
as a function of temperature or time. The change in weight occurs as the sample decomposes or
evaporates and is usually accompanied by evolved gases.
Combining the TGA system with an FTIR spectrometer provides a simple and accurate technique for
identifying the evolved gases from a TGA experiment. This provides information on sample
characteristics such as thermal stability or decomposition pathways.
The sample is loaded onto the balance of the thermogravimetric analyzer. A furnace heats the
sample at a programmed rate from room temperature to high temperatures. The analyzer plots a
weight loss curve of the data file as a function of temperature or time.
A carrier gas continuously sweeps evolved gases from the furnace tube chamber. The carrier gas
may be inert, such as nitrogen, or oxidative, such as air. As the compounds in the sample vaporize,
the carrier gas sends them through a heated transfer line to a heated flow cell in the TGA-IR Module.
There the gases are scanned by the infrared beam and the spectral data recorded. The gases exit the
flow cell through the exhaust tube, which should be vented to a fume hood via tubing or an optional
aspirator or peristaltic pump, if used.
The TGA-IR Module is a single removable assembly that mounts in the sample compartment of the
spectrometer or AEM. The flow cell and transfer line can be removed for cleaning or replacement.
See "Maintenance" for more information.
Thermo Scientific TGA Module User Guide 20
Chapter 3