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)