Thermo Scientific TGA-IR User manual

Nicolet Series FT-IR Spectrometers
TGA-IR Module
User Guide
269-297200 Revision A July 2014

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Thermo Scientific TGA-IR Module User Guide iii
C
Chapter 1 TGA-IR Module . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1
About the TGA-IR Module. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
Safety and Operating Precautions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
TGA-IR Sampling. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
Setting Up the TGA-IR System. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
Performing a TGA-IR Experiment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
Turning Off the TGA-IR System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
Removing the TGA-IR Module . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38
Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 70
Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .75
Contents

Thermo Scientific TGA-IR Module User Guide 1
TGA-IR Module
The TGA-IR module allows you to couple your Thermo Scientific Nicolet™ iS™50,
Nicolet iS10, Nicolet iZ10, Nicolet X700 Series or Nicolet 380 FT-IR spectrometer or AEM
(Auxiliary Experiment Module) with a Thermogravimetric Analysis (TGA) furnace to run
TGA-IR deformulation experiments. The infrared spectrometer and our OMNIC Series
software provide state-of-the art tools for identifying evolved gases and gas mixtures.
Figure 1. Nicolet iS50 spectrometer with TGA-IR module installed
Before operating the TGA-IR module, you should have a working knowledge of your FT-IR
spectrometer and the OMNIC™ Series software. You will also need to know the fundamentals
of thermogravimetric analysis and the operating characteristics of your TGA furnace.
TGA-IR module fits in sample compartment of spectrometer or AEM module
Nicolet iS50
FT-IR spectrometer TGA-IR module

TGA-IR Module
2TGA-IR Module User Guide Thermo Scientific
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 and other important information:
Contents
•About the TGA-IR Module
•Safety and Operating Precautions
•TGA-IR Sampling
•Setting Up the TGA-IR System
•Performing a TGA-IR Experiment
•Turning Off the TGA-IR System
•Removing the TGA-IR Module
•Maintenance
•Troubleshooting
Avoid personal injury or equipment damage. Read and understand the accompanying
documentation and all safety labels before attempting to install or use this equipment.
WARNING
WARNING Indicates a hazardous situation which, if not avoided, could result in death or
serious injury.
CAUTION 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.

TGA-IR Module
About the TGA-IR Module
Thermo Scientific TGA-IR Module User Guide 3
About the TGA-IR Module
The TGA-IR module fits in the sample compartment of a Nicolet Series FT-IR spectrometer
or AEM and connects to the TGA furnace through a heated transfer line.
Figure 2. Nicolet iS50 spectrometer with TGA-IR module installed
This section covers these topics:
•Important Features
•Specifications
•Compatible Software
Note Contains helpful supplementary information.
Tip Provides information that can make a task easier.
Nicolet iS50
FT-IR spectrometer TGA-IR module
Heated
transfer line
Temperature controllers (2)

TGA-IR Module
About the TGA-IR Module
4TGA-IR Module User Guide Thermo Scientific
Important Features
Figure 3. TGA-IR module front view
TGA-IR module features include:
•Temperature 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.
•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 FT-IR spectrometer.
•Beam 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.
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.
Exhaust tube
Power switch
Beam ports (2)
Beam port
shutters (2)
AC power receptacle
Power indicator
Air vents
Voltage select switches (2)
Transfer line

TGA-IR Module
About the TGA-IR Module
Thermo Scientific TGA-IR Module User Guide 5
•Beam 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.
•AC power receptacle. Connector for the AC power cord input.
•Voltage 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 in to a power outlet.
•Power 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.
•Power indicator. Illuminates when the power is on.
•Air vents. Release excess heat generated by the TGA-IR module.
Open Allows infrared beam to enter and exit TGA-IR
module during data collection and seals out the
laboratory environment.
Closed Blocks beam ports in spectrometer while 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.
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.
CAUTION Avoid fire hazard. To prevent the TGA-IR module from overheating, never
block the air vents on the module housing.

TGA-IR Module
About the TGA-IR Module
6TGA-IR Module User Guide Thermo Scientific
Specifications
Table 1. TGA-IR module specifications
Feature Specification
Carrier gas (from TGA furnace)
Recommended materials
Recommended pressure
Recommended flow ratea
aAttach a flow meter to exhaust tube on TGA-IR module to measure flow rate.
Typically nitrogen (inert) or air (oxidative)
5psiorless
30 mL/min to 100 mL/minb
bHigher 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.
Tran sf e r l i n e
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)
Flow cell (inside TGA-IR module)
Window material
Volume (total gas volume inside cell)
Pathlength (inside dimension
window-to-window)
Recommended pressure/vacuumc
cHigher pressures could cause leaks or damage flow cell windows in TGA-IR module.
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)d
Pump tubing
Recommended flow rate
dA pump or similar source of suction can be used to draw TGA gases through flow cell at the optimal rate. 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.
Silicon (0.25 in internal diameter)
0.4 to 85 mL/min
Operating temperaturese
Flow cell
Tr a n s f e r l i n e
eBoth temperature controllers require 30 min to heat from 20 °C to 200 °C (60 min from 20 °C to 300 °C).
ambient to 300 °C (572 °F)
ambient to 300 °C (572 °F)
FT-IR detector
(inside FT-IR spectrometer) Typically DTGS or MCT-B (for faster data
collection, for example to capture dynamic
events)

TGA-IR Module
Safety and Operating Precautions
Thermo Scientific TGA-IR Module User Guide 7
Compatible Software
Safety and Operating Precautions
Follow these precautions to avoid damaging the TGA-IR module or injuring yourself or
others while setting up or operating the module.
• The 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).)
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.
Table 2. Software compatible with the TGA-IR module
Software Use for...
OMNIC™ Configuring your TGA-IR experiment or workflow including
quantitative analysis and spectral search and collecting and analyzing
TGA-IR spectra. For more information, see Performing a TGA-IR
Experiment.
OMNIC Series Collecting, processing and searching time evolved series data. When
Series software is installed with OMNIC, a Series menu appears in the
OMNIC main window.
Series version 9.0 and higher includes Mercury TGA, a dedicated
multi-component search tool for TGA-IR analysis. For details, find
Mercury TGA in Series Help Topics, available from the Help menu in
OMNIC software.
OMNIC Specta™
(optional)
Analyzing unknowns. Includes multi-component search feature for
identifying the spectra of mixtures, a 9,000 compound spectral
database and features for using your computer’s hard drive as a library.
For details, refer to the Help system in OMNIC Specta software.
TQ Analyst
(optional)
Creating quantitative and classification methods that can be used with
OMNIC 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.

TGA-IR Module
Safety and Operating Precautions
8TGA-IR Module User Guide Thermo Scientific
• Handle 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.
• Do 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.
• Make 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.
• Before 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.
• After 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.
• 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.
• To 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.
• If 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.
• Operating temperatures below 200 °C (392 °F) can cause the transfer line to become
clogged.
• Do 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 FT-IR analysis.
• Do 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.

TGA-IR Module
TGA-IR Sampling
Thermo Scientific TGA-IR Module User Guide 9
For more information, refer to the TGA-IR Module Site and Safety Supplement, the site and
safety guide that came with your FT-IR spectrometer, and the documentation that came with
your TGA furnace.
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 FT-IR 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).
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.

TGA-IR Module
Setting Up the TGA-IR System
10 TGA-IR Module User Guide Thermo Scientific
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.
Setting Up the TGA-IR System
This section explains how to set up a TGA-IR system, which includes the following
components:
• Thermo Scientific Nicolet iS50, Nicolet iS10, Nicolet iZ10, Nicolet X700 series or
Nicole 380 FT-IR spectrometer or AEM (auxiliary experiment module)
• Thermo Scientific TGA-IR module
• Thermogravimetric analyzer (TGA furnace)
Follow these steps to set up the TGA-IR system:
1. Prepare the TGA furnace
2. Prepare the FT-IR spectrometer
3. Install the TGA-IR Module
4. Set the flow cell and transfer line temperature
5. Verify the installation
After you have set up the system, see “Performing a TGA-IR Experiment” for information on
using the TGA-IR module to collect sample data.
Preparing the TGA Furnace
Follow the instructions in the documentation that came with your TGA furnace to set up the
furnace. For best results, place the furnace on a strong, flat, vibration-free table. We
recommend that you use a source of clean, dry air or nitrogen as the carrier gas and set the
carrier gas pressure and flow rate as follows:
Note The Nicolet iS10 and iZ10 spectrometer require a sample compartment extension
to accommodate the TGA-IR module. For more information, call your local Thermo
Scientific representative.
Table 3. Carrier gas recommended pressure and flow rate
Pressure Flow rate
5 psi or less 30 mL/min to 100 mL/mina
aHigher 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.

TGA-IR Module
Setting Up the TGA-IR System
Thermo Scientific TGA-IR Module User Guide 11
Preparing the FT-IR Spectrometer
This section describes how to configure a Thermo Scientific FT-IR spectrometer or AEM for
use with the TGA-IR module.
To configure the FT-IR spectrometer or AEM
1. Remove any sample or accessory from the sample compartment of the spectrometer or
AEM where you will be installing the TGA-IR module.
2. Remove the sample compartment cover if necessary.
Refer to the documentation that came with your spectrometer or AEM for instructions.
3. Remove the standard sample compartment transmission baseplate if it is installed.
4. If your spectrometer is sealed and desiccated, we recommend that you install a purge kit.
To order a purge kit, use the information at the beginning of this document to contact us.
After the purge kit is installed and connected to a source of dry air or nitrogen at the
proper pressure and flow rate, you can remove the two sample compartment windows
from the spectrometer (not necessary for the iS10 and iZ10 spectrometers).
WARNING Avoid fire and explosion hazard. Do not connect a flammable carrier gas to
the TGA-IR system.
NOTICE The TGA-IR module is configured to connect to a TGA furnace that is
positioned on the right side of the spectrometer. If your TGA furnace is on the left side,
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).)
Note
• Purge is recommended for the spectrometer connected to a TGA-IR module. Purging
the spectrometer ensures spectral features in TGA-IR data relate to the gas phase
sample and not to changes in the room environment.
• The Nicolet iS10 and iZ10 spectrometer require a sample compartment extension to
accommodate the TGA-IR module. For more information, call your local Thermo
Scientific representative.

TGA-IR Module
Setting Up the TGA-IR System
12 TGA-IR Module User Guide Thermo Scientific
5. Turn on the spectrometer and verify that it is operating properly before you install the
TGA-IR module.
This could be the Advanced Diagnostics Performance Test in OMNIC software or a
spectrometer PV test. For more information, open Spectrometer Help Topics from the
Help menu in OMNIC software and search for the Advanced Diagnostics and
Performance Verification (PV) topic names.
Installing the TGA-IR Module
This section explains how to install the TGA-IR module in a compatible Thermo Scientific
spectrometer or AEM and attach the module to your TGA furnace. Before you begin, make
sure you have prepared the TGA furnace and the spectrometer or AEM. The TGA-IR module
power switch should be off and the power cord unplugged at both ends.
Tools needed:
• 7/16 inch open ended wrench
NOTICE
• If you are converting a sealed and desiccated spectrometer to a purged
spectrometer, install the purge kit before you remove the sample compartment
windows. For information on how to install purge equipment, set the controls for
the first time, and inspect and clean the purge filter, find “Installing Purge
Controls” in Spectrometer Help Topics, available from the Help menu in
OMNIC software. For instructions to remove sample compartment windows,
search for that topic in the spectrometer Help in OMNIC software.
• If you choose not to purge the spectrometer, make sure you install the beam port
shutters in the “closed” position while the TGA-IR module heats up for the first
time and wait the recommended time (4 hours) at the recommended temperature
(300 °C) before you begin analyzing samples. Closing the beam ports prevents
any excessively humid air released from the TGA-IR module from damaging the
sample compartment windows or other moisture-sensitive components in the
spectrometer. Before you begin analyzing samples, switch the beam port shutters
to the “open” position to allow the IR beam to pass through the module.

TGA-IR Module
Setting Up the TGA-IR System
Thermo Scientific TGA-IR Module User Guide 13
To install the TGA-IR module
1. Remove the protective caps from the beam ports on both sides of the TGA-IR module.
Figure 4. Remove both beam port caps
2. Install the TGA-IR module in the sample compartment of the spectrometer or AEM.
Lift the TGA-IR module using the designated hand holds and gently place it in the
sample compartment. The transfer line should be loosely coiled and supported as shown
below.
Figure 5. Lift points to properly carry TGA-IR module
Beam port caps (2)
Lift point
Lift point

TGA-IR Module
Setting Up the TGA-IR System
14 TGA-IR Module User Guide Thermo Scientific
Line up the alignment pins on the sample compartment baseplate with the alignment
holes in the bottom of the TGA-IR module. The base of the TGA-IR module should sit
flat against the bottom of the sample compartment.
Figure 6. TGA-IR module properly installed in spectrometer sample compartment
3. Engage the anti-rock clip at the back of the sample compartment.
The anti-rock clip for the Nicolet iS50 spectrometer is shown below (your spectrometer
or AEM may have a different style clip).
Figure 7. Nicolet iS50 spectrometer anti-rock clip fully engaged
NOTICE
• Handle 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.
• Do 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.
Alignment pins (2)
Make sure TGA-IR
module is seated on
alignment pins in
sample compartment
baseplate
Engage anti-rock clip

TGA-IR Module
Setting Up the TGA-IR System
Thermo Scientific TGA-IR Module User Guide 15
4. Install both beam port shutters in the closed position on each side of the TGA-IR
module.
Install the beam port shutters with the white “Closed” label on top while the TGA-IR
module heats up for the first time. Leave them installed until the module has been heated
at 300 °C for at least 4 hours to ensure that no moisture remains inside the module.
Figure 8. Install beam port shutters in “closed” position (white label at top)
NOTICE Make sure you install the beam port shutters in the “closed” position while
the TGA-IR module heats up for the first time (and after being stored). Wait the
recommended time (4 hours) at the recommended temperature (300 °C) before you
continue or you may permanently damage the sample compartment windows or
other moisture-sensitive components in the spectrometer.
Beam port
shutters closed
(white label at
top)

TGA-IR Module
Setting Up the TGA-IR System
16 TGA-IR Module User Guide Thermo Scientific
5. Connect the opposite end of the transfer line to the TGA furnace.
Remove the Velcro™ strap from the end of the transfer line and gently spread apart the
insulation to expose the Swagelok nut.
Figure 9. Free end of transfer line ready to connect to TGA furnace
Lower the TGA furnace using the application software for the furnace. This will make the
plumbing connection m ore accessible.
NOTICE
• Handle the transfer line gently and do not exceed its minimum bend radius of
7.6 cm (3.0 in).
• The outside surface of the transfer line is abrasive; if it consistently rubs against
another surface such as the outside of your TGA furnace, it may cause scratches.
• Make sure the transfer line is supported while you are connecting it to the TGA
furnace and afterwards. Do not allow the transfer line to hang unsupported
between the TGA-IR module and the TGA furnace. The extra weight my
interfere with the transfer line’s lifetime performance.
• The 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, 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).)
Swagelok nut
Velcro strap