Thermo Scientific TGA-IR User Manual
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Thermo Scientific TGA-IR User Manual

Thermo Scientific TGA-IR User Manual

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

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Summary of Contents for Thermo Scientific TGA-IR

  • Page 1 Nicolet Series FT-IR Spectrometers TGA-IR Module User Guide 269-297200 Revision A July 2014...
  • Page 2 © 2014 Thermo Fisher Scientific Inc. All rights reserved. Microsoft, Windows and Excel are either trademarks or registered trademarks of Microsoft Corporation in the United States and/or other countries. Swagelok is either a trademark or a registered trademark of Swagelok Company in the United States and/or other countries.

  • Page 3: Table Of Contents

    Setting Up the TGA-IR System........10 Performing a TGA-IR Experiment ........25 Turning Off the TGA-IR System .

  • Page 5: Tga-Ir Module

    TGA-IR module TGA-IR module fits in sample compartment of spectrometer or AEM module 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.
  • Page 6 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.

  • Page 7: About The Tga-Ir Module

    Tip Provides information that can make a task easier. 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.
  • Page 8 • 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).
  • Page 9 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 10 A 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.

  • Page 11: Safety And Operating Precautions

    • 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.
  • Page 12 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.

  • Page 13: Tga-Ir Sampling

    • 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.

  • Page 14: Setting Up The Tga-Ir System

    TGA-IR Module Setting Up the TGA-IR System 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.
  • Page 15 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.
  • Page 16 • 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.
  • Page 17 TGA-IR Module Setting Up the TGA-IR System  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 Beam port caps (2) 2.
  • Page 18 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.
  • Page 19 TGA-IR Module Setting Up the TGA-IR System 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.
  • Page 20 • 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.
  • Page 21 Be careful not to compress the insulation too much by overtightening the strap. Figure 10. Example of TGA-IR attachment at TGA furnace Stretch tubing to Position and...
  • Page 22 Setting Up the TGA-IR System 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 23 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). See...
  • Page 24 Click here for details. 8. Verify that the voltage select switches on the TGA-IR module are set correctly for the local electricity requirements and then connect the power cord. Slide both voltage select switches to 115 V or 230 V to match the AC line voltage of your power source.
  • Page 25 Make sure the power switch for the TGA-IR module is in the off position and then plug one end of the AC power cord into the power receptacle on the front of the module.
  • Page 26 Temperature indicators 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 for details).
  • Page 27   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. CAUTION Avoid burn hazard. If the “over temperature” error message appears on a...
  • Page 28 Verifying the System Performance After you have installed the TGA-IR module and connected it to the TGA furnace, follow these steps to verify the installation. (You don’t need to wait for the TGA-IR module to heat up to verify its performance.) ...

  • Page 29: Performing A Tga-Ir Experiment

    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 System for details.
  • Page 30 30 mL/min and 100 mL/min. Refer to the operating manual that came with your TGA furnace for more information. NOTICE To prevent the flow cell windows in the TGA-IR module from becoming contaminated, make sure carrier gas from the TGA furnace is flowing through the flow cell before you turn on the flow cell and transfer line heaters.
  • Page 31 To analyze a test sample 1. Tare 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.
  • Page 32 TGA-IR Module Performing a TGA-IR Experiment 5. Use the temperature controllers on the TGA-IR module to manually set the flow cell and transfer line to the proper operating temperature for your sample material (must be between 200 °C and 300 °C).
  • Page 33 Auto Scale Profiles Select Time Sequence Set Save: to 48 minutes to save all the data collected during the TGA-IR run (double-click Save: to edit) External trigger Select if using a remote start cable to start Series data collection automatically...
  • Page 34 TGA-IR Module Performing a TGA-IR Experiment 9. Click OK to start collecting a background spectrum. The background spectrum appears in the bottom pane of the Series Profile window. Figure 19. Collecting a background spectrum When the background collection is completed, the system begins collecting a set of basis vectors which are used to calculate the Gram-Schmidt profile.
  • Page 35 As the experiment proceeds, the Gram-Schmidt profile gradually appears, left to right, in a time response display. The Gram-Schmidt profile is a plot showing how overall spectral intensity changed during the experiment. In the TGA-IR example below, the peaks in the Gram-Schmidt plot indicate when different compounds in the sample vaporized, passed through the flow cell and absorbed infrared energy.
  • Page 36 TGA-IR Module Performing a TGA-IR Experiment Here is an example showing the cursor located at the top of a peak in the time response display and the corresponding spectrum in the spectral data display. Figure 23. Using the spectral cursor tool to display the spectrum collected at a specific time in...
  • Page 37 Figure 24. Series profile window showing TGA-IR results for CaOx 13. To identify the displayed TGA-IR spectrum, use the library search features in the Analyze menu of OMNIC software. Use Library Manager to select a TGA spectral library that contains compounds that are similar to your sample material.

  • Page 38: Turning Off The Tga-Ir System

    • 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 39 TGA-IR Module Removing the TGA-IR Module 3. Turn off the carrier gas at the TGA furnace. 4. Disconnect the transfer line from the evolved gas outlet on the TGA furnace. Loosen the strap and let it slide down the transfer line.
  • Page 40 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.
  • Page 41 TGA-IR Module Removing the TGA-IR Module 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. Figure 27. Install beam port caps before storing TGA-IR module...

  • Page 42: 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 43 If the outside of the TGA-IR module needs cleaning, turn it off, disconnect the power cord and wait 2 hours for the TGA-IR module and transfer line to cool. Then use a clean, soft cloth slightly dampened with a mild soap solution to clean the outside of the module. Wipe dry.
  • Page 44 • Do not allow liquids to come into contact with flow cell windows.  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). Turn off the power switch for the TGA-IR module and unplug the power cord.
  • Page 45 5. Remove the main cover from the TGA-IR module. Use the large slotted screwdriver to rotate the two cover screws counter clockwise to release the cover and then lift the cover straight up and off the TGA-IR module. Figure 29. Release TGA-IR module main cover...
  • Page 46 Use a #2 Phillips head screwdriver to loosen the two back screws that secure the flow cell compartment cover. (The 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 47 Figure 31. Remove insulating block and metal heat shield Remove insulating block Remove metal heat shield (underneath insulating block) NOTICE Save the insulating block and heat shield. You will need to replace them after you reinstall the flow cell. Thermo Scientific TGA-IR Module User Guide...
  • Page 48 9. Remove the two insulating blocks to expose the flow cell connectors. Figure 33. Remove insulating blocks to expose flow cell connectors Remove insulating blocks (2) NOTICE Save the insulating blocks. You will need to replace them after you reinstall the flow cell. TGA-IR Module User Guide Thermo Scientific...
  • Page 49 (behind the nut). Figure 34. Remove cotter pins and slide copper sleeve toward transfer line to expose connecting nut Remove cotter pin Slide copper sleeve toward transfer line Remove cotter pin Thermo Scientific TGA-IR Module User Guide...
  • Page 50 Figure 35. Loosen Swagelok nut to release transfer line Carefully set the transfer line aside. Note If the flow cell windows are contaminated, the transfer line may also be clogged. Follow these instructions to clean it. TGA-IR Module User Guide Thermo Scientific...
  • Page 51 TGA-IR module. Slide the clip off the exhaust tube. Figure 36. Loosen clip that secures exhaust tube to TGA-IR module 12. Use a 3/16-inch hex key to remove the center screw from the flow cell assembly. Figure 37. Remove center screw from flow cell assembly...
  • Page 52 TGA-IR Module Maintenance 13. Lift the flow cell assembly (with the exhaust tube connected) out of its housing and set it on a table. Figure 38. Remove flow cell from TGA-IR module (with exhaust tube connected) Remove flow cell Leave...
  • Page 53 Use a #1 Phillips head screwdriver to remove the three screws that secure the end cap on one end of the cell body. Figure 40. Remove end cap screws on flow cell assembly Remove end cap screws (3) Thermo Scientific TGA-IR Module User Guide...
  • Page 54 Figure 42. Remove manifold plugs and gaskets Gasket Manifold plug Gasket Manifold plug Remove the gaskets from the plugs. Set the plugs aside. Discard the gaskets (both kits include a new set of gaskets). TGA-IR Module User Guide Thermo Scientific...
  • Page 55 (available from a laboratory equipment supply company). ZnSe windows are easily scratched and cannot be polished to remove residue. Note If the flow cell windows are extremely dirty or damaged, contact us to order new ones. Replacement windows include replacement gaskets, washers and screws. Thermo Scientific TGA-IR Module User Guide...
  • Page 56 • KBr or ZnSe window. For ZnSe, make sure coated side of window faces out of flow cell so it does not contact the sample material. • large round washer (align with gasket and window) TGA-IR Module User Guide Thermo Scientific...
  • Page 57 To tighten the screws, hold the cell body with your thumb and finger to keep everything aligned. Then use a #1 Phillips head screwdriver to partially tighten each screw, rotating from one to the next until all three screws are secure. Thermo Scientific TGA-IR Module User Guide...
  • Page 58 When the coated side faces up, the light is fully reflected off the coating and you cannot see the bottom edge. Figure 45. To determine the coated side of a ZnSe window When coated side faces up, the bottom edge is not visible (coated surface is opaque) TGA-IR Module User Guide Thermo Scientific...
  • Page 59 Slide the exhaust tube onto the bottom (flow cell outlet) connector on the flow cell assembly and tighten the Swagelok nut with a 9/16-inch and a 1/2-inch open ended wrench. Figure 46. Connect exhaust tube to bottom (flow cell outlet) connector Connect exhaust tube Thermo Scientific TGA-IR Module User Guide...
  • Page 60 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 47. Line up pin holes on flow cell with alignment pins in flow cell compartment Alignment pins (2) TGA-IR Module User Guide Thermo Scientific...
  • Page 61 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 48. 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 62 TGA-IR Module Maintenance 3. Slide the clip over the exhaust tube and tighten it with a #2 Phillips head screwdriver. Figure 50. Tighten clip that secures exhaust tube to TGA-IR module Tighten clip TGA-IR Module User Guide Thermo Scientific...
  • Page 63 Slide the transfer line onto the top flow cell connector and tighten the Swagelok nut finger tight. Figure 51. Connect transfer line to top (flow cell inlet) connector and tighten finger tight Flow cell inlet connector Transfer line connector Thermo Scientific TGA-IR Module User Guide...
  • Page 64 Use two 7/16-inch open ended wrenches to slowly tighten the Swagelok nut until you feel resistance, then continue tightening the nut 1/8 of a turn more. To ensure the best seal, do not overtighten the Swagelok nut. Figure 52. Use two 7/16-inch open ended wrenches to tighten nut TGA-IR Module User Guide Thermo Scientific...
  • Page 65 Insert the two cotter pins to secure the sleeve. (If you position the sleeve as shown below, the pins will easily slide into place.) Figure 53. Slide copper sleeve toward TGA-IR module and insert cotter pins Insert cotter pin Slide copper...
  • Page 66 Plug in AC power connector for transfer line Press wires into slot Gather the wires and press them into the slot at the edge of the flow cell compartment. TGA-IR Module User Guide Thermo Scientific...
  • Page 67 Place the large insulating block over the heat shield. Figure 56. Install metal heat shield and large insulating block Install insulating block on top of heat shield Install metal heat shield first Thermo Scientific TGA-IR Module User Guide...
  • Page 68 Maintenance 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. Figure 57. Install flow cell compartment cover and insert or tighten screws...
  • Page 69 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 59. Press electrical wires away from edges of TGA-IR module Press electrical wires toward transfer line...
  • Page 70 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 carrier gas is flowing through the flow cell before you turn on the flow cell and transfer line heaters.
  • Page 71 TGA-IR Module Maintenance If your TGA-IR system clogs up frequently, contact your local sales or service representative. NOTICE Handle the transfer line gently and do not exceed its minimum bend radius of 7.6 cm (3.0 in).  To disconnect the transfer line Set the heaters for the TGA-IR module to 20 °C (68 °F).
  • Page 72 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 61. Location of fuse box Fuse box If a fuse blows, the TGA-IR module will automatically be powered off.
  • Page 73 Figure 63. Replace both fuses Fuse (2) 4. Install the fuse box. Position the fuse box with the prong facing the right side of the TGA-IR module and then slide the box into the module. Figure 64. Install fuse box...

  • Page 74: Troubleshooting

    Help menu in OMNIC 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...
  • Page 75 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, first turn off the TGA-IR module power switch and disconnect the AC power cord. Then check that the...
  • Page 76 If a temperature controller displays a high temperature value and then displays an “input/fail” message, check that the transfer line and flow cell electrical connectors are plugged into the correct receptacles. The connectors are located under the TGA-IR module main cover.
  • Page 77 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.
  • Page 78 (blue label on top). • Spectrometer component has failed. (See the Troubleshooting section of Spectrometer Help Topics.) If the problem persists, use the information at the beginning of this document to contact Technical Support. TGA-IR Module User Guide Thermo Scientific...

  • Page 79: Index

    TGA-IR disconnect exhaust tube aperture disconnect transfer line set for TGA-IR module install autostart install manifold plugs configure for Series data collection...
  • Page 80 Index: D FT-IR spectrometer prepare for TGA-IR sampling data collection furnace and beam port shutter position connect to TGA-IR module detector prepare for TGA-IR sampling select for TGA-IR module fuse specifications specifications disconnect fuses exhaust tube from flow cell replace...
  • Page 81 TGA-IR module reduced TGA-IR module signal remote start OMNIC configure for Series data collection Bench tab settings for TGA-IR analysis remove Collect tab settings for TGA-IR analysis exhaust tube from TGA-IR module configure remote start flow cell assembly...
  • Page 82 TGA-IR module lift points minimum voltage for TGA-IR module maintenance prepare for TGA-IR sampling prepare for sample analysis TGA-IR Module User Guide Thermo Scientific...
  • Page 83 TGA-IR module set voltage select switches voltage select switches specifications set for TGA-IR module store volume troubleshoot of flow cell...

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