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Thermo Scientific TGA User Manual

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

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  • Page 1 TGA Interface with OMNIC Paradigm software User Guide 269-362100 Revision A March 2023...
  • Page 2 © 2023 Thermo Fisher Scientific Inc. All rights reserved. For technical support, please contact: www.thermofisher.com Thermo Fisher Scientific Inc. provides this document to its customers with a product purchase to use in the product operation. This document is copyright protected and any reproduction of the whole or any part of this document is strictly prohibited, except with the written authorization of Thermo Fisher Scientific Inc.
  • Page 3 Safety label locations The TGA-IR Module comes with numerous safety labels. Heed the label content to avoid injury or hazard.
  • Page 4 Chapter 1 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.
  • Page 5 Nicolet iS50 FTIR spectrometer TGA-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.

  • Page 6: Table Of Contents

    TGA-IR Module Performing a TGA-IR measurement Preparing the TGA-IR system for sampling Samples compatible with TGA-IR Analyzing a test sample Import TGA data Configuring series data collection to start automatically Turning off the TGA-IR system Removing the TGA-IR Module Maintenance...
  • Page 7 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.
  • Page 8 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...
  • Page 9 [This page intentionally left blank]...
  • Page 10 Chapter 2 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...
  • Page 11 About the TGA-IR Module Nicolet iS50 FTIR Spectrometer Temperature controllers (2) TGA-IR Module Heated transfer line Important features Figure 2-2: TGA-IR Module front view TGA Module User Guide Thermo Scientific...
  • Page 12 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.
  • Page 13 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.
  • Page 14 Horizontal movement 20 cm (8 inches) Attach a flow meter to exhaust tube on TGA-IR Module to measure flow rate. Higher 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.
  • Page 15 Higher pressures could cause leaks or damage flow cell windows in TGA-IR Module. A 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.
  • Page 16 About the TGA-IR Module Compatible software Table 2-2: Software compatible with the TGA-IR Module Software Use for... OMNIC Collecting and analyzing your data. For more information, see Paradigm™ "Performing a TGA-IR measurement". Creating quantitative and classification methods that can be used with OMNIC Paradigm software.
  • Page 17 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.
  • Page 18 Safety and operating precautions 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 FTIR analysis. Do not use excessive amounts of liquid to clean the module housing or allow the liquid cleaner to get inside the module.
  • Page 19 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. TGA Module User Guide...
  • Page 20 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.
  • Page 21 [This page intentionally left blank]...
  • Page 22 Chapter 4 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 (or other compatible spectrometer) or the AEM (Auxiliary Experiment Module) Thermo Scientific TGA-IR Module...
  • Page 23 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).
  • Page 24 “open” position to allow the IR beam to pass through the module. 5. Turn on the spectrometer and verify that it is operating properly before you install the TGA-IR Module. Refer to any topics on verifying you spectrometer's performance in the spectrometer user guide.
  • Page 25 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 "Preparing the TGA furnace"...
  • Page 26 Support the transfer line while you transport the TGA-IR Module to avoid damaging or breaking 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.
  • Page 27 Setting up the TGA-IR system Figure 4-3: 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).
  • Page 28 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.
  • Page 29 Figure 4-5: 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...
  • Page 30 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).
  • Page 31 1/8-inch adapter. Note If the TGA furnace is a horizontal model with about 7 inches of vertical travel, you may need to gently bend the transfer line into a soft “S curve” to compensate for the furnace’s open/close mechanism.
  • Page 32 Make sure the table supports the transfer line to reduce wear at the connections. Here are examples of the TGA-IR Module installed in right and left side spectrometer configurations with the transfer line properly connected and supported.
  • Page 33 60 mL/min and 80 mL/min (flow rate should be 0.4 to 85 mL/min). Note We recommend connecting an aspirator or peristaltic pump to the exhaust tube to help draw carrier gas through the TGA-IR system, especially when using a high resolution TGA furnace (which typically have a low flow rate).
  • Page 34 If you plan to use a pump, use clear, flexible Tygon™ or other non-reactive tubing to connect the exhaust tube on the TGA-IR Module to the pump inlet. Make sure you connect the pump so it draws the sample/carrier gas mixture out of the TGA-IR Module. Use another piece of tubing to direct the pump outlet to a fume hood or other venting system.
  • Page 35 Setting up the TGA-IR system Figure 4-11: Connecting the exhaust tube to a peristaltic pump Transfer line Cell Tubing Purge tubing Soft rubing to make connection Soft tubing through rollers Exhaust tube Peristaltic pump To exhaust (hood) TGA Module User Guide...
  • Page 36 Ensure the power switch for the TGA-IR Module is in the off position, then plug one end of the AC power cord into the power receptacle on the front of the module. Plug the other end of the power cord into a properly grounded AC power source.
  • Page 37 200 °C to 300 °C (392 °F to 572 °F) The TGA-IR Module must be plugged in and powered up before you set the flow cell and transfer line temperature. The carrier gas from the TGA furnace should flow through the flow cell at the recommended rate (TGA furnace door must be closed).
  • Page 38 Setting up the TGA-IR system NOTICE Install the beam port shutters in the “closed” position while the TGA-IR Module heats up for the first time (and after it has been stored). Wait the recommended time (4 hours) at the recommended temperature (300 C) before you attempt to collect data.
  • Page 39 After the heaters have reached their set points, they will remain at that temperature until you turn off the TGA-IR Module power switch. The time required to reach the target temperature depends on the starting temperature and the target temperature (see "Specifications"...
  • Page 40 If an error condition occurs, press the s and t keys once simultaneously to reset the temperature controller and clear the error, then turn off the TGA-IR Module power switch, wait 1 minute, and turn the power switch back on. If that doesn’t correct the problem, call our local service representative.
  • Page 41 ❖ 1. Open OMNIC Paradigm software. The software automatically loads the default, commonly used settings as Smart TGA - Factory Preset, but you can create your own settings based on your analysis needs. 2. Select More to see the live interferogram. The voltage of at least one of the interferogram peaks (positive or negative) should be greater than 5 volts for KBr windows and 4 volts for ZnSe windows.

  • Page 42: Performing A Tga-Ir Measurement

    Preparing the TGA-IR system for sampling Follow these steps to prepare the TGA-IR system for sampling after it has been turned off. The TGA- IR system must have been properly installed and the installation verified. See "Setting up the TGA-IR...
  • Page 43 Make sure the carrier gas for the TGA furnace is set to 5.0 psi or less and the flow rate is between 30 mL/min and 100 mL/min. Refer to the operating manual that came with your TGA furnace for more information.

  • Page 44: Samples Compatible With Tga-Ir

    Beam port shutters in the "open" position (blue label at top) Samples compatible with TGA-IR Any sample that can be measured by TGA will work with the TGA-IR application. TGA and TGA-IR are useful for two types of heat activated analyses: deformation (where intact molecules of the material vaporize) and breakdown (where materials such as carbon dioxide, water, and ammonia form under high heat).
  • Page 45 ❖ 1. Take a high-temperature platinum or ceramic TGA pan. 2. Close the TGA furnace to permit the carrier gas to flow from the furnace to the TGA-IR Module. This step is necessary for correct background collection. 3. Specify the ramp rate and target temperature for the TGA furnace.
  • Page 46 8. Select Start Background Measurement and wait for the process to complete. 9. Place a measured quantity of the sample onto the pan in the TGA furnace and start the TGA run. For our test, we are using 50 mg.

  • Page 47: Import Tga Data

    For most samples (CaOx is an exception), a weight loss of about 10 mg usually gives an adequate infrared signal. For example, is a sample loses 50% of its weight during the TGA run, a 20 mg sample size will probably be accurate. Do not use excessively large sample sizes.

  • Page 48: Configuring Series Data Collection To Start Automatically

    If you have the optional Thermo Scientific remote start cable for your spectrometer, you can set up OMNIC Paradigm software to start automatically at the start of each TGA sample analysis. To order a cable, call your local Thermo Scientific sales or service representative or use the information at the beginning of this document to contact us.
  • Page 49 Performing a TGA-IR measurement Figure 5-5: TGA - Start from external trigger checkbox Note To configure your TGA furnace for remote start, see the user guide that came with the furnace. TGA Module User Guide Thermo Scientific...

  • Page 50: Turning Off The Tga-Ir System

    If the spectrometer is purged with dry air or nitrogen, leave the beam port shutters in the “open” position and the carrier gas flowing through the TGA-IR Module. If the spectrometer is sealed and desiccated (with KBr sample compartment windows), install the beam port shutters in the closed position.
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  • Page 52: Removing The Tga-Ir Module

    Non-powdered latex-free gloves (to handle fiberglass insulation around transfer line) To remove the TGA-IR Module ❖ 1. Turn off the power switch on the front of the TGA-IR Module and unplug the power cord. CAUTION 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.
  • Page 53 6. Release the anti-rock clip at the back of the sample compartment. Figure 7-1: Release anti-rock clip 7. Lift the TGA-IR Module straight up using the designated hand holds. The transfer line should be loosely coiled and supported as shown below.
  • Page 54 TGA-IR Module. Fingerprints will permanently damage the windows and degrade system performance. 8. Replace the protective caps in the beam ports on the right and left side of the TGA-IR Module and store the module properly in a clean, dry environment. See "Storing the TGA-IR...
  • Page 55 Removing the TGA-IR Module Beam port cap (2) Lift point (2) NOTICE "Storing the TGA-IR Module" for important information about how to properly store the module to prevent damage to internal components due to excessive moisture, dust and dirt. 9. Install the sample compartment cover on the spectrometer, if applicable.

  • Page 56: Maintenance

    Storing the TGA-IR Module When the TGA-IR Module is not in use for a short period (a day or two), leave it in the spectrometer or AEM with the power on and the carrier gas flowing through it. Set the flow cell and transfer line heaters between 120 °C and 130 °C (248 °F and 266 °F).

  • Page 57: Cleaning The Tga-Ir Module Housing

    Support the transfer line while you transport the TGA-IR Module to avoid damaging or breaking 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.

  • Page 58: Flow Cell Maintenance

    NOTICE 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 FTIR analysis. Do not use excessive amounts of liquid to clean the module housing or allow the liquid cleaner to get inside the module.
  • Page 59 To remove the flow cell assembly ❖ 1. Set the transfer line and flow cell heaters for the TGA-IR Module to 20 °C (68 °F). 2. Turn off the power switch for the TGA-IR Module and unplug the power cord.
  • Page 60 Use a #2 Phillips head screwdriver to loosen the two back screws that secure the flow cell compartment cover. This will prevent them from falling inside the TGA-IR Module. Remove the two front screws that secure the cover and then slide the cover forward and off the TGA-IR Module.
  • Page 61 Loosen these two screws so they don't fall inside the TGA-IR Module. This is the flow cell compartment cover. Remove these two screws and slide the cover forward to remove it from the TGA-IR Module. 7. Remove the insulating block and metal heat shield from the flow cell compartment and set them aside.
  • Page 62 Remove the metal heat shield underneath the insulating block. NOTICE Save the insulating block and heat shield. You will need to replace them after you reinstall the flow cell. 8. Unplug the AC power and temperature controller connectors for the transfer line. Thermo Scientific TGA Module User Guide...
  • Page 63 Disconnect temperature controller connector for the transfer line. Disconnect AC power connector for transfer line. 9. Remove the two insulating blocks to expose the flow cell connectors. Figure 8-6: Remove insulating blocks to expose flow cell connectors Remove insulating blocks (2) TGA Module User Guide Thermo Scientific...
  • Page 64 Insert the two cotter pins into their original holes in the copper sleeve to hold the sleeve out of the way, behind the nut. Figure 8-7: Remove cotter pins and slide copper sleeve toward transfer line to expose connecting Slide the copper sleeve towards the transfer line. Remove cotter pins (2). Thermo Scientific TGA Module User Guide...
  • Page 65 Follow these instructions to clean it. 11. Use a #2 Phillips head screwdriver to loosen the clip that secures the exhaust tube to the TGA-IR Module. Slide the clip off the exhaust tube. Figure 8-9: Loosen the clip securing the exhaust tube to the TGA-IR Module 12.
  • Page 66 13. Lift the flow cell assembly (with the exhaust tube connected) out of its housing and set it on a table. Figure 8-11: Remove flow cell from TGA-IR Module (with exhaust tube connected) Remove the flow cell. Leave the exhaust tube connected.
  • Page 67 1. Remove the KBr or ZnSe window from each end of the flow cell. Use a #1 Phillips head screwdriver to remove the three screws that secure the end cap on one end of the cell body. TGA Module User Guide Thermo Scientific...
  • Page 68 KBr o ZnSe window End cap Repeat the steps above to remove the end cap and window from the other end of the flow cell. 2. Remove the manifold plugs from the flow cell. Thermo Scientific TGA Module User Guide...
  • Page 69 Wear nitrile gloves to handle the flow cell windows and hold them only by the edges. Fingerprints, even while wearing gloves,will permanently damage the windows and degrade system performance. Do not allow liquids to come into contact with the windows. TGA Module User Guide Thermo Scientific...
  • Page 70 On one end of the flow cell body, carefully insert the following parts from the replacement kit in the order shown below and then start the three screws that secure the end cap. Before you tighten the screws, verify that the window opening is not blocked by a portion of a gasket. Thermo Scientific TGA Module User Guide...
  • Page 71 To determine the coated side, inspect both sides of the window at an angle to the ceiling light. When the uncoated side faces up, the bottom edge of the window is visible through the window material. TGA Module User Guide Thermo Scientific...
  • Page 72 1. Connect the exhaust tube to the flow cell assembly. Slide the exhaust tube onto the bottom (flow cell outlet) connector on the flow cell assembly, then tighten the Swagelok nut with a 9/16-inch and a 1/2-inch open ended wrench. Thermo Scientific TGA Module User Guide...
  • Page 73 Line up the pin holes on the bottom of the flow cell assembly with the alignment pins on the bottom of the flow cell compartment. Figure 8-19: Line up pin holes on flow cell with alignment pins in flow cell compartment TGA Module User Guide Thermo Scientific...
  • Page 74 Maintenance Position the flow cell assembly with the large screw hole facing up; the connectors should face the front of the TGA-IR Module. Figure 8-20: Install flow cell assembly in flow cell compartment The flow cell assembly should sit flat against the heater plate at the bottom of the compartment.
  • Page 75 Connect the transfer line to the flow cell assembly Orient the transfer line so it will extend in the direction of the TGA furnace when the flow cell is installed; there should not be excessive bending at either end of the transfer line.
  • Page 76 Insert the two cotter pins to secure the sleeve. If you position the sleeve correctly, the pins will easily slide into place. Figure 8-25: Slide copper sleeve toward TGA-IR Module and insert the cotter pins Thermo Scientific TGA Module User Guide...
  • Page 77 Figure 8-26: Install insulating blocks (grooved block goes on left side) Insert plain insulating block here. Insert grooved insulating block here (groove faces up). Groove. 6. Plug the AC power and temperature controller connectors for the transfer line into their corresponding receptacles. TGA Module User Guide Thermo Scientific...
  • Page 78 Place the metal heat shield over the flow cell (make sure the wires are neatly gathered into the slot so the heat shield lies flat). Place the large insulating block over the heat shield. Thermo Scientific TGA Module User Guide...
  • Page 79 Install the metal heat shield first. 8. Replace the flow cell compartment cover and insert or tighten the screws. Slide the cover back onto the TGA-IR Module and use a #2 Phillips head screwdriver to tighten the 4 screws that secure the cover.
  • Page 80 Replace and tighten front screws (2). 9. Use your hand to stretch the protective tubing over the exposed insulation so the tubing and the insulation press against the flow cell compartment with no air gaps. Thermo Scientific TGA Module User Guide...
  • Page 81 10. Replace the TGA-IR Module main cover. Press the electrical wires toward the center of the module, away from the edges (to avoid catching them in the cover latch). Figure 8-31: Press electrical wires away from edges of TGA-IR Module TGA Module User Guide Thermo Scientific...

  • Page 82: Transfer Line Maintenance

    11. Install the beam port shutters in the closed position. 12. Make sure the TGA-IR Module power switch is off. 13. Plug in the power cord for the TGA-IR Module and turn on the power switch. NOTICE To prevent the flow cell windows from becoming contaminated, make sure that carrier gas is flowing through the flow cell before you turn on the flow cell and transfer line heaters.
  • Page 83 ❖ 1. Set the heaters for the TGA-IR Module to 20 °C (68 °F). 2. Turn off the power switch for the TGA-IR Module and unplug the power cord CAUTION 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.

  • Page 84: Replacing Fuses

    Replacing fuses Two fuses protect the TGA-IR Module from excessive current. Use replacement fuses of the correct size and specifications (see below). The fuse box is at the front of the TGA-IR Module, next to the power switch. Figure 8-33: Location of fuse box If a fuse blows, the TGA-IR Module will automatically power off.
  • Page 85 3. Replace the two fuses with two new ones of the correct size and with the same specifications. Figure 8-35: Replace both fuses 4. Install the fuse box. Insert the fuse box with the prong facing the right side of the TGA-IR Module and slide the box into the module. TGA Module User Guide...
  • Page 86 Maintenance Figure 8-36: Install fuse box 5. Plug in the power cord for the TGA-IR Module and turn on the power switch. Thermo Scientific TGA Module User Guide...
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  • Page 88: Troubleshooting

    Help menu in OMNIC Paradigm software. Power indicator does not light If the power indicator on the front of the TGA-IR Module does not light after you turn on the power switch, check the following: Make sure the power switch is on and the voltage select switches are set correctly for the local electricity supply.

  • Page 89: No Heat Or Heats Slowly

    Temperature controller connector for transfer line. Power connector for flow cell. Power connector for transfer line. If the problem persists, the heater element may need replacement. Use the information at the beginning of this document to contact Technical Support. TGA Module User Guide Thermo Scientific...

  • Page 90: Transfer Line And Flow Cell Heat Too Rapidly (Or Very Slowly)

    Transfer line and flow cell heat too rapidly (or very slowly) If the transfer line and flow cell heat up very rapidly or very slowly, turn off the TGA-IR Module power switch and disconnect the AC power cord. Then check that the voltage select switches are set correctly for the local electricity supply.

  • Page 91: Temperature Overshoot Or Undershoot

    Select the Diagnostic tab in Experiment Setup and click Align to align the spectrometer. If the problem persists, use the information at the beginning of this document to contact Technical Support. No detectable sample gas If the Gram-Schmidt profile has no sample peaks, check the following: TGA Module User Guide Thermo Scientific...

  • Page 92: Spectroscopic Ir Signal Is Reduced

    Record the flow cell temperature, number of scans collected, and resolution setting. By keeping track of this information, you can monitor the system integrity over time. If the spectroscopic signal in the TGA-IR Module shows a sudden loss in intensity, check the following: For spectrometers that are sealed and desiccated (rather than purged with dry air or nitrogen), the sample compartment windows may be damaged or fogged.
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