TA Instruments TGA 2950 Operator's Manual
TA Instruments TGA 2950 Operator's Manual

TA Instruments TGA 2950 Operator's Manual

Thermogravimetric analyzer
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TGA 2950
Thermogravimetric Analyzer
Operator's Manual
PN 925602.001 Rev. D (Text and Binder)
PN 925602.002 Rev. D (Text Only)
TA I
Issued July 2000
TGA 2950
i
NSTRUMENTS

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Summary of Contents for TA Instruments TGA 2950

  • Page 1 TGA 2950 Thermogravimetric Analyzer Operator’s Manual PN 925602.001 Rev. D (Text and Binder) PN 925602.002 Rev. D (Text Only) TA I Issued July 2000 TGA 2950 NSTRUMENTS...
  • Page 2 TA I TGA 2950 NSTRUMENTS...
  • Page 3: Table Of Contents

    Notes, Cautions, and Warnings ....xii Hotline Numbers ........xiv Safety ............xv Using This Manual ........xviii CHAPTER 1: Introducing the TGA 2950 ..........1-1 Introduction..........1-3 Components .......... 1-4 The 2950 Instrument ........1-5 2950 Display ........1-5 2950 Keypad ........1-6 HEATER Switch ......
  • Page 4 Table of Contents (continued) CHAPTER 2: Installing the TGA 2950 ..........2-1 Unpacking/Repacking the 2950 ....2-3 Unpacking the 2950 ......2-3 Repacking the 2950 ....... 2-6 Installing the Instrument ......2-7 Inspecting the System......2-8 Choosing a Location ......2-9 Filling the Heat Exchanger....
  • Page 5 Setting Up an Experiment ....3-14 Setting Up Accessories ...... 3-15 Using the Air Cool Option..3-16 Using a Purge Gas ...... 3-16 Using the Gas Switching Accessory ....3-19 Starting an Experiment ....... 3-20 TA I TGA 2950 NSTRUMENTS...
  • Page 6 Use in an Oxygen-Free Atmosphere ..3-22 Purge Gas System....... 3-22 Instrument Set-Up ......3-23 CHAPTER 4: Technical Reference ..4-1 Description of the TGA 2950 ..... 4-3 Components......... 4-5 Balance .......... 4-6 Sample Loading Assembly .... 4-8 Furnace .......... 4-9 TGA Standard Furnace ...
  • Page 7 Water Reservoir ....... 5-6 Replacing the Thermocouple ...... 5-9 Removing and Reinstalling the Furnace ......5-11 Furnace Removal ....... 5-11 Furnace Replacement ......5-14 Diagnosing Power Problems ..... 5-16 Fuses ........... 5-16 Power Failures ........5-18 TA I TGA 2950 NSTRUMENTS...
  • Page 8 TGA Option ..........B-1 Overview ............ B-5 Option Installation ........B-6 Using Hi-Res TGA ......... B-7 Background ......... B-7 The TA Instruments Hi-Res Technique ..........B-8 The Hi-Res Ramp Segment ....B-9 Calcium Oxalate Example Scans ..B-13 Advanced Hi-Res Techniques ....
  • Page 9 Data Analysis Effects ......B-32 Derivative Plots ........B-33 Adjusting Heating Rate ......B-34 Adjusting Resolution Setting ....B-37 Useful Resolutions Settings ....B-39 Temperature Calibration ......B-41 Hi-Res Transition Temperatures ... B-42 Hi-Res Sensitivity Segment ....B-43 TA I TGA 2950 NSTRUMENTS...
  • Page 10 Varying Resolution Setting ..B-61 Varying Sensitivity Setting..B-62 Constant Reaction Rate Scans ..B-63 Stepwise Isothermal Scans ..B-65 Monosodium Glutamate ....B-68 Banana Taffy ........B-69 Plastic Laboratory Tubing....B-71 References ..........B-75 TA I TGA 2950 NSTRUMENTS...
  • Page 11 APPENDIX C: TGA 2950 Autosampler Option ........ C-1 Introducing the Auto TGA ......C-3 Getting Started ........... C-4 The TGA 2950 Instrument ......C-6 Calibrating the Auto TGA ....... C-10 Running Experiments ......C-11 Preparing the Samples ....... C-12 Selecting Sample and Tare Pans ......
  • Page 12 Table of Contents (continued) Appendix D: TGA 2950 EGA Furnace Option ......D-1 Introducing the EGA Furnace ....D-3 EGA Furnace Specifications ....D-5 Installing the EGA Furnace ....... D-6 First-Time Installation ......D-6 Removing and Reinstalling the EGA Furnace ........D-14 EGA Furnae Removal....
  • Page 13: Notes, Cautions, And Warnings

    A CAUTION emphasizes a procedure that may CAUTION: damage equipment or cause loss of data if not followed correctly. A WARNING indicates a procedure that WARNING may be hazardous to the operator or to the environment if not followed correctly. TA I TGA 2950 xiii NSTRUMENTS...
  • Page 14 Hotlines To TA Instruments For Technical Assistance ..(302) 427-4070 To Order Instruments and Supplies ......(302) 427-4040 For Service Inquiries....(302) 427-4050 Sales ........(302) 427-4000 TA I TGA 2950 NSTRUMENTS...
  • Page 15: Safety

    Chemical Safety Do not use hydrogen or any other explosive WARNING gas in the TGA 2950 furnace or the TGA 2950 EGA furnace. Oxygen can be used as a purge gas in the TGA WARNING 2950. However, the furnace must be kept clean so that volatile hydrocarbons (which might combust) are removed.
  • Page 16 Safety (continued) The TGA 2950 furnace assembly contains a WARNING layer of refractory ceramic fiber (RCF) insulation. This insulation is completely encapsulated within the ceramic subassem- bly, which is not meant to be disassembled. If the subassembly should break in such a...
  • Page 17 Avoid contact with the furnace base during experiments. Mechanical Safety Keep your fingers and all other objects out WARNING of the path of the furnace when it is mov- ing. The furnace seal is very tight. TA I TGA 2950 xvii NSTRUMENTS...
  • Page 18: Using This Manual

    Using This Manual Chapter 1 Describes your TGA 2950 instrument and its acces- sories and specifications. Chapter 2 Describes how to unpack and install the TGA and how to connect the TGA to the rest of your system. Chapter 3...
  • Page 19 Using This Manual (continued) Appendix C Provides instructions needed to operate the TGA Autosampler option to automatically load and run samples. Appendix D Provides instructions needed to install and use the EGA furnace with the TGA 2950. TA I TGA 2950 NSTRUMENTS...
  • Page 20 TA I TGA 2950 NSTRUMENTS...
  • Page 21 CHAPTER 1: Introducing the TGA 2950 Introduction..........1-3 Components .......... 1-4 The 2950 Instrument ........1-5 2950 Display ........1-5 2950 Keypad ........1-6 HEATER Switch ......1-10 POWER Switch ......1-10 Accessories ..........1-11 Gas Switching Accessory ....1-11 Other Accessories ......
  • Page 22: Chapter 1: Introducing The Tga 2950

    Introducing the TGA 2950 1–2 TA I TGA 2950 NSTRUMENTS...
  • Page 23: Introduction

    Your TA Instruments Thermogravimetric Analyzer (TGA) 2950 is a thermal weight- change analysis instrument, used in conjunction with a TA Instruments thermal analysis control- ler and associated software, to make up a thermal analysis system. The Thermogravimetric Analyzer 2950 mea-...
  • Page 24: Components

    Introducing the TGA 2950 Components The TGA 2950 has five major components, illustrated in Figure 1.1: • The balance, which provides precise measurement of sample weight. The balance is the key to the TGA system. • The sample platform, which loads and unloads the sample to and from the balance.
  • Page 25: The 2950 Instrument

    The 2950 Instrument The 2950 Instrument The parts of the TGA 2950 instrument that provide for operator control are: · The instrument display · The instrument keypad. Standby 23.25°C Weight 238.247 mg TGA 2950 Thermogravimetric Analyzer Figure 1.2 TGA 2950...
  • Page 26: 2950 Keypad

    Introducing the TGA 2950 A pound sign (#) after the weight signal indi- cates that the balance reading has not yet stabilized. When the weight stabilizes, the pound sign will disappear. 2950 Keypad The instrument keypad (see Figure 1.2) contains the keys found in Table 1.1 and the HEATER...
  • Page 27 The 2950 Instrument Table 1.1 TGA 2950 Keypad Function Keys (continued) Key/Function Explanation LOAD Loads a sample pan from the sample platform onto the balance. UNLOAD Unloads the sample pan from the balance onto the sample platform. ∆ FURNACE Toggles between the...
  • Page 28 Introducing the TGA 2950 Table 1.1 TGA 2950 Keypad Function Keys (continued) Key/Function Explanation STOP If an experiment is running, this key ends the method normally, as though it had run to completion; i.e., the method-end conditions go into effect and the data that has been generated is saved.
  • Page 29 The 2950 Instrument Table 1.1 TGA 2950 Keypad Function Keys (continued) Key/Function Explanation NOTE: The SCROLL key operates normally (scrolls the realtime signals) until the STOP key is pressed. If an experiment is not running, SCROLL-STOP works like the STOP key.
  • Page 30: Heater Switch

    Introducing the TGA 2950 HEATER Switch The HEATER on/off switch (see Figure 1.2) turns the power to the instrument heater on and off. This switch should be in the ON (1) position before you start an experiment. NOTE: The light in the HEATER switch will glow only when an experiment is in progress.
  • Page 31: Accessories

    TGA experiments. Evolved Gas Analysis Furnace The TGA 2950 EGA furnace is an accessory to the instrument which allows you to perform combined TGA and evolved gas analysis experiments. Other Accessories...
  • Page 32: Specifications

    Introducing the TGA 2950 Specifications Tables 1.2 through 1.4 contain the technical specifications for the TGA 2950. Table 1.2 TGA 2950 Operating Parameters Temperature range C to 1000 Thermocouple Platinel II* Heating rate with standard furnace 0.1 to 100 C/min with EGA furnace 0.1 to 50°C/min...
  • Page 33 5 gm. The TGA balance mechanism is sensitive to changes in the surrounding room tempera- ture. For optimum accuracy, you must regulate the ambient temperature. (table continued) TA I TGA 2950 1–13 NSTRUMENTS...
  • Page 34 Introducing the TGA 2950 Do not use hydrogen or WARNING any other explosive gas in the TGA 2950 furnace or the TGA 2950 EGA furnace. Oxygen may be used. How- ever, the furnace must be kept clean of volatile hydro- carbons to prevent combus- tion.
  • Page 35: Chapter 2: Installing The Tga 2950

    CHAPTER 2: Installing the TGA 2950 Unpacking/Repacking the 2950 ....2-3 Unpacking the 2950 ......2-3 Repacking the 2950 ....... 2-6 Installing the Instrument ......2-7 Inspecting the System......2-8 Choosing a Location ......2-9 Filling the Heat Exchanger....2-10 Connecting Cables and Gas Lines ..
  • Page 36 Installing the 2950 2–2 TA I TGA 2950 NSTRUMENTS...
  • Page 37: Unpacking/Repacking The 2950

    Unpacking the 2950 Refer to Figures 2.1 to 2.3 while unpacking your instrument. Have an assistant help you unpack this WARNING unit. Do not attempt to do this alone. Figure 2.1 Shipping Boxes TA I TGA 2950 2–3 NSTRUMENTS...
  • Page 38 Then lift and rotate the unit so that the other end hangs over the edge of the bench. Someone must hold onto the unit at all times while it is in 2–4 TA I TGA 2950 NSTRUMENTS...
  • Page 39 2.3). Rotate the unit and install the two remaining mounting feet in the same man- ner. 9. Remove the furnace clamp before turning on the power to the unit. Figure 2.3 Installing the Mounting Feet TA I TGA 2950 2–5 NSTRUMENTS...
  • Page 40: Repacking The 2950

    Installing the 2950 Repacking the 2950 To pack and ship your instrument, use the hardware retained during unpacking and reverse the instructions found on pages 2-3 to 2-5. 2–6 TA I TGA 2950 NSTRUMENTS...
  • Page 41: Installing The Instrument

    Installing the Instrument Installing the Instrument Before shipment, the TGA 2950 instrument is inspected both electrically and mechanically so that it is ready for operation upon proper instal- lation. Installation involves the following procedures, described in this chapter: · Inspecting the system for shipping damage and missing parts ·...
  • Page 42: Inspecting The System

    Installing the 2950 Inspecting the System When you receive your TGA 2950, look over the instrument and shipping container carefully for signs of shipping damage, and check the parts received against the enclosed shipping list. • If the instrument is damaged, notify the carrier and TA Instruments immediately.
  • Page 43: Choosing A Location

    50 or 60 Hz, 15 amps). A step up/down line transformer may be required if the unit is oper- ated at a higher or lower line voltage..your TA Instruments thermal analysis controller..compressed lab air and purge gas supplies with suitable regulators and flowmeters.
  • Page 44: Filling The Heat Exchanger

    2-12). To fill the heat ex- changer, follow the directions given below. Water Reservoir Cap Heat Exchanger Cable Figure 2.4 Rear Panel of Screws Heat Exchanger 1. Unscrew the water reservoir cap on the heat exchanger (see Figure 2.4). 2–10 TA I TGA 2950 NSTRUMENTS...
  • Page 45 Fill to bottle’s inner rim. Figure 2.5 Heat Exchanger Bottle 2. Add TA Instruments TGA Conditioner (PN 952377.901) into the water reservoir bottle. Refer to the instructions on the bottle for the amount of conditioner to add to the reser- voir.
  • Page 46: Connecting Cables And Gas Lines

    1. Locate the cooling accessory connector on the left rear of the instrument cabinet (Figure 2.6). 2. Connect the heat exchanger cable to the connector. The heat exchanger cable is the only cable that fits into this connector. 2–12 TA I TGA 2950 NSTRUMENTS...
  • Page 47 Installing the Instrument Figure 2.6 TGA 2950 Connector Panel 3. Remove the water lines from the packing. 4. Connect one end of the water line marked “SUPPLY” to the connector labeled “SUP- PLY” on the right side of the instrument cabinet.
  • Page 48 Air Cool from the controller. Refill the coolant reservoir as needed. Repeat this process until all the air has been purged from the system and the instrument stops reporting an “Err 119.” 2–14 TA I TGA 2950 NSTRUMENTS...
  • Page 49: Gpib Cable

    4. Connect the other end of the GPIB cable to the controller or to the GPIB cable of another TA Instruments instrument con- nected to the controller. (For more informa- tion, see your controller manual.) 5. Select an address from 1 to 9. Then use the...
  • Page 50 0 1 0 0 0 0 1 0 0 1 *0 = OFF; 1 = ON A D D R E S S Figure 2.8 4/86 010161-26C Binary Address Switches (Showing an Address of 7) 2–16 TA I TGA 2950 NSTRUMENTS...
  • Page 51: Purge Lines

    NOTE: If you are using laboratory purge, rather than bottled purge, you will need to install an external drier. The use of corrosive gases is not recommended. CAUTION: TA I TGA 2950 2–17 NSTRUMENTS...
  • Page 52: Cooling Gas Line

    TGA instrument, see Chapter 1. Oxygen may be used as a purge gas, but the furnace must be kept clean of volatile hydrocarbons to prevent combustion. Cooling Gas Line 2–18 TA I TGA 2950 NSTRUMENTS...
  • Page 53: Power Cable

    Before plugging the TGA power cable into the wall outlet, make sure the instrument is compatible with the line voltage. Check the label on the back of the unit to verify the voltage. 3. Plug the power cable into the wall outlet. TA I TGA 2950 2–19 NSTRUMENTS...
  • Page 54: Unpacking The Balance

    Installing the 2950 Unpacking the Balance When unpacking the balance, be careful not to CAUTION: damage the balance arm or hang-down loops. Tare Sample Side Side Balance Cover Balance Cover Screw Tare Hang-Down Tube Loop 2–20 TA I TGA 2950 NSTRUMENTS...
  • Page 55 Unpacking the Balance Foam Insert TA I TGA 2950 2–21 NSTRUMENTS...
  • Page 56: Installing The Hang-Down Wires

    Installing the 2950 Installing the Hang-Down Wires During installation, take care not to bend the CAUTION: hang-down wires or damage the hang-down loops. FURNACE 2–22 TA I TGA 2950 NSTRUMENTS...
  • Page 57 To make the hang-down loops easier to see, we NOTE: suggest sliding a piece of white paper into the balance chamber behind each loop before you hook the hang-down wire into it. (Do not forget to remove the paper when finished.) TA I TGA 2950 2–23 NSTRUMENTS...
  • Page 58 Installing the 2950 2–24 TA I TGA 2950 NSTRUMENTS...
  • Page 59: Aligning The Sample Hang-Down Wire

    Installing the Hang-Down Wires Aligning the Sample Hang-Down Wire LOAD TA I TGA 2950 2–25 NSTRUMENTS...
  • Page 60 Installing the 2950 2–26 TA I TGA 2950 NSTRUMENTS...
  • Page 61 Installing the Hang-Down Wires FURNACE STOP Thermocouple Tube Sample Furnace Sample Furnace Housing TOP VIEW Sample Pan Should be Centered Within Furnace Furnace Base TA I TGA 2950 2–27 NSTRUMENTS...
  • Page 62 Installing the 2950 FURNACE UNLOAD 2–28 TA I TGA 2950 NSTRUMENTS...
  • Page 63: Adjusting The Sample Platform

    Adjusting the Sample Platform Adjusting the Sample Platform This procedure assumes that the instrument has NOTE: been properly levelled (see page 2-26) and that the sample hang-down wire is straight. TA I TGA 2950 2–29 NSTRUMENTS...
  • Page 64: Starting The 2950

    Installing the 2950 Starting the 2950 POWER HEATER The HEATER and POWER indicator lamps may NOTE: flicker under low AC voltage conditions. 2–30 TA I TGA 2950 NSTRUMENTS...
  • Page 65 Starting the TGA 2950 Standby 23.25°C Weight 238.247 mg TGA 2950 Thermogravimetric Analyzer Allow the TGA to warm up for at least 30 minutes NOTE: before performing an experiment. TA I TGA 2950 2–31 NSTRUMENTS...
  • Page 66: Shutting Down The 2950

    Installing the 2950 Shutting Down the 2950 POWER HEATER 2–32 TA I TGA 2950 NSTRUMENTS...
  • Page 67: Chapter 3: Running Experiments

    CHAPTER 3: Running Experiments TA I TGA 2950 3–1 NSTRUMENTS...
  • Page 68 Running Experiments 3–2 TA I TGA 2950 NSTRUMENTS...
  • Page 69: Overview

    Overview Overview Before You Begin TA I TGA 2950 3–3 NSTRUMENTS...
  • Page 70 Running Experiments 3–4 TA I TGA 2950 NSTRUMENTS...
  • Page 71: Calibrating The Tga

    Calibrating the TGA Calibrating the TGA Temperature Calibration TA I TGA 2950 3–5 NSTRUMENTS...
  • Page 72: Weight Calibration

    Running Experiments Weight Calibration You must be sure to determine the exact weight NOTE: of the calibration weights before they are used to calibrate the instrument. Sample Platform Calibration 3–6 TA I TGA 2950 NSTRUMENTS...
  • Page 73: Running A Tga Experiment

    Running a TGA Experiment Running a TGA Experiment Experimental Procedure TA I TGA 2950 3–7 NSTRUMENTS...
  • Page 74: Preparing Samples

    Running Experiments Preparing Samples Selecting Sample and Tare Pans 3–8 TA I TGA 2950 NSTRUMENTS...
  • Page 75: Taring The Sample Pan

    Running a TGA Experiment Taring the Sample Pan TA I TGA 2950 3–9 NSTRUMENTS...
  • Page 76: Automatic Tare

    Running Experiments Automatic Tare TARE Manual Tare LOAD FURNACE 3–10 TA I TGA 2950 NSTRUMENTS...
  • Page 77: Loading The Sample

    Always use brass tweezers to handle the sample NOTE: pans. Manually loading the sample pan onto the hang- CAUTION: down wire may damage the balance mechanism. Sample Sample Holder Thermocouple Sample Sample Platform Hook Furnace Housing TA I TGA 2950 3–11 NSTRUMENTS...
  • Page 78 Running Experiments LOAD The position of the thermocouple should be the NOTE: same as it was during temperature calibration. Thermocouple Thermocouple Sample Hook should be about 2 mm from pan surface. Sample Pan Furnace 3–12 TA I TGA 2950 NSTRUMENTS...
  • Page 79 Running a TGA Experiment FURNACE TA I TGA 2950 3–13 NSTRUMENTS...
  • Page 80: Setting Up An Experiment

    Running Experiments Setting Up an Experiment 3–14 TA I TGA 2950 NSTRUMENTS...
  • Page 81: Setting Up Accessories

    Running a TGA Experiment Setting Up Accessories TA I TGA 2950 3–15 NSTRUMENTS...
  • Page 82: Using The Air Cool Option

    NOTE: used with the furnace closed. However, if the temperature is above 500°C, the EGA furnace will cool naturally until it is 500°C or less, then Air Cool will begin. Using a Purge Gas 3–16 TA I TGA 2950 NSTRUMENTS...
  • Page 83 Running a TGA Experiment Do not use hydrogen or any other explosive WARNING gas in the TGA 2950 furnace or the TGA 2950 EGA furnace. *Oxygen may be used as a purge gas, but the furnace must be kept clean of volatile hydrocarbons to prevent combustion.
  • Page 84 Running Experiments 3–18 TA I TGA 2950 NSTRUMENTS...
  • Page 85: Using The Gas Switching Accessory

    Running a TGA Experiment Using the Gas Switching Accessory TA I TGA 2950 3–19 NSTRUMENTS...
  • Page 86: Starting An Experiment

    Experiment Once the experiment is started, operations are NOTE: best performed at the controller keyboard. The TGA 2950 is very sensitive to motion and might pick up the vibration caused by pressing a key on the instrument keypad. START START...
  • Page 87: Stopping An Experiment

    The Heat Exchanger will continue to run as long as NOTE: the Air Cool option is activated or until the indi- cated temperature is below 50 The REJECT function discards all experiment data. CAUTION: Unloading the Sample UNLOAD TA I TGA 2950 3–21 NSTRUMENTS...
  • Page 88: Use In An Oxygen-Free Atmosphere

    Running Experiments Use in an Oxygen- Free Atmosphere Purge Gas System 3–22 TA I TGA 2950 NSTRUMENTS...
  • Page 89: Instrument Set-Up

    Use in an Oxygen-Free Atmosphere Instrument Set-Up When the TGA is idle, leave the system closed and NOTE: continue purging with nitrogen. TA I TGA 2950 3–23 NSTRUMENTS...
  • Page 90 Running Experiments 3–24 TA I TGA 2950 NSTRUMENTS...
  • Page 91: Chapter 4: Technical Reference

    CHAPTER 4: Technical Reference Description of the TGA 2950 ..... 4-3 Components ......... 4-5 Balance .......... 4-6 Sample Loading Assembly .... 4-8 Furnace .......... 4-9 TGA Standard Furnace ... 4-9 EGA Furnace ......4-11 Cabinet ......... 4-13 Heat Exchanger ......4-15 Theory of Operation .........
  • Page 92 Technical Reference 4–2 TA I TGA 2950 NSTRUMENTS...
  • Page 93: Description Of The Tga 2950

    This current is converted to the weight signal. The TGA 2950 has two weight ranges: 1 gm and 100 mg. Both ranges are continuous over their weight loss operating range, which means that the entire weight loss range can be viewed without any loss of information.
  • Page 94 (standard furnace = 40 mL/min, EGA furnace = 10 mL/min). An inert gas must be used to prevent contamination or corrosion of the balance. Heating rate and sample temperature are mea- sured by the thermocouple located above the sample. 4–4 TA I TGA 2950 NSTRUMENTS...
  • Page 95: Components

    Description of the TGA 2950 Components The TGA 2950 has five major components, illustrated in Figure 4.1: the balance, the sample loading assembly, the furnace, the cabinet, and the heat exchanger. Figure 4.1 TGA 2950 Components The balance, the most important part of the TGA system, provides precise measurement of the sample weight.
  • Page 96: Balance

    The balance arm is a rhombic piece of alumi- num attached to the meter movement. It is in a null balance system. A hang-down loop is attached to each end to hold the hang-down wires. 4–6 TA I TGA 2950 NSTRUMENTS...
  • Page 97 Description of the TGA 2950 The balance arm sensor is a printed circuit board assembly that detects the null position of the meter movement. The balance beam sensor is mounted above the balance arm. It is used in conjunction with the analog circuitry to maintain a null position.
  • Page 98: Sample Loading Assembly

    It also pivots the platform away from the furnace area for easy sample loading and unloading. Figure 4.3 Sample Loading Assembly 4–8 TA I TGA 2950 NSTRUMENTS...
  • Page 99: Furnace

    Description of the TGA 2950 Furnace Two types of furnaces may be used with the TGA 2950 instrument, the standard TGA furnace, or the Evolved Gas Analysis (EGA) furnace. The EGA Furnace (see Appendix D) is an optional accessory that allows you to connect...
  • Page 100 The furnace base moves the furnace assembly up around the sample pan to the closed position, or down away from the sample pan to the open position. 4–10 TA I TGA 2950 NSTRUMENTS...
  • Page 101: Ega Furnace

    Description of the TGA 2950 EGA Furnace The (Evolved Gas Analysis) EGA furnace consists of a quartz glass sample tube sur- rounded by an electric resistance heater, both of which are contained within a water-cooled furnace housing. The housing is mounted to a furnace base that raises and lowers the furnace for sample loading and unloading.
  • Page 102 1000°C with heating rates up to 50°C/min. The thermocouple and furnace base are the same as those described above for the standard TGA furnace. *Platinel II is a registered trademark of Engelhard Industries. 4–12 TA I TGA 2950 NSTRUMENTS...
  • Page 103: Cabinet

    Description of the TGA 2950 Cabinet The TGA cabinet (Figure 4.6) consists of the cabinet housing, the instrument display and keypad, the electronics compartment, the purge and cooling gas fittings, and the rear panel. Electronics Compartment Instrument Display and Keypad...
  • Page 104 The rear panel (Figure 4.7) has the signal and power connections for the instrument, the fuses, the ready light, the address switches, and the Reset button. Figure 4.7 Rear Panel 4–14 TA I TGA 2950 NSTRUMENTS...
  • Page 105: Heat Exchanger

    Description of the TGA 2950 Heat Exchanger The heat exchanger (Figure 4.8) consists of a fan, a radiator, a water reservoir, a pump, a temperature switch, and a flow switch. The fan blows cool air through the radiator. The radiator exchanges heat between the water and air.
  • Page 106: Theory Of Operation

    Two modes are commonly used for investigating thermal stability behavior in controlled atmospheres: (1) dynamic, in which the temperature is increased at a linear rate, and (2) isothermal, in which the tempera- ture is kept constant. 4–16 TA I TGA 2950 NSTRUMENTS...
  • Page 107: Status Codes

    This may be caused by a large ballistic jump in the program, a faulty heater, or a faulty control thermo- couple signal. Complete The thermal method has finished. (table continued) TA I TGA 2950 4–17 NSTRUMENTS...
  • Page 108 Heating The heater temperature is increasing, as specified by a Ramp segment. Holding Thermal experiment conditions are holding; the program is suspended. Choose Start to continue the run. (table continued) 4–18 TA I TGA 2950 NSTRUMENTS...
  • Page 109 Load The TGA is loading a sample pan onto the balance. No Power No power is being applied to the heater. Check the heater switch and fuse. (table continued) TA I TGA 2950 4–19 NSTRUMENTS...
  • Page 110 Set Up The system is loading the sample, closing the furnace, and letting the weight stabilize before beginning the first seg- ment. Stand by The method and method- end operations are com- plete. (table continued) 4–20 TA I TGA 2950 NSTRUMENTS...
  • Page 111 Temperature calibration is in effect. The heater is in stand-by mode, and the experiment has been terminated. Unload The TGA is unloading a sample from the balance. Weight # The weight reading is not stable. TA I TGA 2950 4–21 NSTRUMENTS...
  • Page 112 Technical Reference 4–22 TA I TGA 2950 NSTRUMENTS...
  • Page 113: Chapter 5: Maintenance And Diagnostics

    Water Reservoir ....... 5-6 Replacing the Thermocouple ...... 5-9 Removing and Reinstalling the Furnace ......5-11 Furnace Removal ....... 5-11 Furnace Replacement ......5-14 Diagnosing Power Problems ..... 5-16 Fuses ........... 5-16 Power Failures ........5-18 TA I TGA 2950 5–1 NSTRUMENTS...
  • Page 114 Maintenance and Diagnostics TGA Test Functions ......... 5-19 The Confidence Test ......5-19 Replacement Parts ........5-21 5–2 TA I TGA 2950 NSTRUMENTS...
  • Page 115: Overview

    Overview The procedures described in this section are the customer’s responsibility. Any further mainte- nance should be performed by a representative of TA Instruments or other qualified service personnel. Because of the high voltages in this instru- WARNING ment, untrained personnel must not at- tempt to test or repair any electrical circuits.
  • Page 116: Routine Maintenance

    A household liquid glass cleaner and paper towel are best for cleaning the instrument keypad. Wet the towel, not the keypad, with the glass cleaner, and then wipe off the keypad and display. 5–4 TA I TGA 2950 NSTRUMENTS...
  • Page 117: Cleaning The Furnace Housing

    (e.g., lubricating oils), you need to clean the standard furnace more frequently to prevent dangerous buildup of debris in the furnace. This is particularly important if you are using oxygen as a purge gas. TA I TGA 2950 5–5 NSTRUMENTS...
  • Page 118: Heat Exchanger

    Add distilled water to the reservoir, if necessary, to keep the reservoir at least 2/3 full. If algae growth is visible, drain the reservoir bottle, refill it with distilled water, and add TA Instruments TGA Conditioner, as described in the next section.
  • Page 119 4. Dispose of the water and fill the bottle with TGA Conditioner (PN 952377.901) and fresh distilled water as directed in Chapter 2. TA I TGA 2950 5–7 NSTRUMENTS...
  • Page 120 Cool, and circulate the water until the air bubbles disappear from the water lines. (You may see “Err 119” on the instrument display until all the air has been removed.) 6. Replace and tighten the water reservoir cap. 5–8 TA I TGA 2950 NSTRUMENTS...
  • Page 121: Replacing The Thermocouple

    4. Push the thermocouple up from the bottom, to feed it back into the balance chamber (Figure 5.1). Figure 5.1 Removing the Thermocouple 5. Unplug the thermocouple from its connector and remove the thermocouple from the balance chamber. TA I TGA 2950 5–9 NSTRUMENTS...
  • Page 122 (Figure 5.2). Figure 5.2 Checking Position of Thermocouple 10. Make sure that the hang-down wire does not touch the top of the thermocouple inside the balance chamber. 11. Replace the balance chamber faceplate and screws. 5–10 TA I TGA 2950 NSTRUMENTS...
  • Page 123: Removing And Reinstalling The Furnace

    To obtain access to the upper left screw and cleat, NOTE: loosen the three hold-down screws on the furnace base. Rotate the furnace housing gently counter- clockwise to move the coolant connections away from the front of the cabinet slot. TA I TGA 2950 5–11 NSTRUMENTS...
  • Page 124 6. Loosen the hold-down screws, if necessary, and remove the furnace housing from the furnace base, being careful not to disturb the coolant connections. Lay the furnace housing on the front ledge of the cabinet. 5–12 TA I TGA 2950 NSTRUMENTS...
  • Page 125 7. Unplug the Air Cool line from the bottom of the furnace arm/base (Figure 5.4). The furnace arm/base is now completely free of the instrument. When you remove the Air Cool line, do not let it NOTE: slip back into the instrument cabinet. TA I TGA 2950 5–13 NSTRUMENTS...
  • Page 126: Furnace Replacement

    5. Using the ball driver, tighten the two screws on either side of the furnace arm connection, making sure that the curved edges of all four cleats engage the groove on the furnace arm. 5–14 TA I TGA 2950 NSTRUMENTS...
  • Page 127 This will move the purge and coolant connec- tions away from the front of the cabinet slot. 7. Rotate the furnace housing clockwise until it is aligned correctly, and tighten the three hold-down screws completely. TA I TGA 2950 5–15 NSTRUMENTS...
  • Page 128: Diagnosing Power Problems

    Both are housed in safety-approved fuse carriers, labeled F1 and F2 (Figure 5.5). Always unplug the instrument before you WARNING examine or replace the fuses. Fuse 1 Fuse 2 Figure 5.5 Fuse Locations 5–16 TA I TGA 2950 NSTRUMENTS...
  • Page 129 Power supplied by this circuit is switched by a computer-controlled relay as well as by the HEATER switch located on the instrument’s front panel. When both devices are active, the light in the HEATER switch will glow. TA I TGA 2950 5–17 NSTRUMENTS...
  • Page 130: Power Failures

    Do not try to repair it yourself; call your TA Instruments service representative. The TGA is designed for a nominal line voltage of 115 volts AC (+ 10%), 50 or 60 Hz. It should not be operated outside this range.
  • Page 131: The Confidence Test

    TGA 2950 Test Functions TGA 2950 Test Functions The TGA 2950 has three levels of test and diagnostic functions: • The confidence test that is run every time the instrument is started. • Cycling test functions that continuously test specific.
  • Page 132 The system stops when the fatal error is posted, and the Ready light remains off. Table 5.1 summarizes the primary confidence tests for the TGA. If any errors occur during the confidence test, call your TA Instruments service representative. Table 5.1 TGA Confidence Test...
  • Page 133: Replacement Parts

    Replacement Parts Replacement Parts Replacement parts for the TGA 2950 are avail- able from TA Instruments and are listed in Table 5.2. Table 5.2 List of TGA 2950 Parts Part Number Description 952018.906 100 µL platinum sample pan kit 952018.907 100 µL ceramic sample...
  • Page 134 Furnace motor assembly 952121.001 Work surface tray 952183.901 Aluminum temperature calibration standard 900905.901 Calcium oxalate sample 990806.901 Air purge valve assembly 952324.001 TGA 2950 keypad assembly 990820.010 Instrument keypad 990828.901 Power supply assembly 990850.901 Central processor PCB 990880.901 Communications PCB 990870.901 Triac drive PCB 259508.000...
  • Page 135 Replacement Parts Table 5.2 (continued) Part Number Description 269930.001 Class C calibration weight kit (1 mg to 500 mg) 952160.901 TGA 2950 Cooling Accessory 952160.903 Heat exchanger fan/ assembly 952162.901 Cooling Accessory tubing 952166.901 Cooling Accessory water reservoir bottle 952172.901...
  • Page 136 Maintenance and Diagnostics 5–24 TA I TGA 2950 NSTRUMENTS...
  • Page 137: Appendix A: Ordering Information

    Appendix A: Ordering Information TA I TGA 2950 A–1 NSTRUMENTS...
  • Page 138 Appendix A A–2 TA I TGA 2950 NSTRUMENTS...
  • Page 139: Appendix B: High Resolution Tga Option

    Hi-Res Option Appendix B: High Resolution TGA Option TA I TGA 2950 B–1 NSTRUMENTS...
  • Page 140 Appendix B B–2 TA I TGA 2950 NSTRUMENTS...
  • Page 141 Hi-Res Option TA I TGA 2950 B–3 NSTRUMENTS...
  • Page 142 Appendix B B–4 TA I TGA 2950 NSTRUMENTS...
  • Page 143: Overview

    Hi-Res Option Overview TA I TGA 2950 B–5 NSTRUMENTS...
  • Page 144: Option Installation

    Appendix B Option Installation B–6 TA I TGA 2950 NSTRUMENTS...
  • Page 145: Using Hi-Res Tm Tga

    Hi-Res Option Using Hi-Res Background TA I TGA 2950 B–7 NSTRUMENTS...
  • Page 146: The Ta Instruments Hi-Res

    Appendix B The TA Instruments Hi-Res Technique B–8 TA I TGA 2950 NSTRUMENTS...
  • Page 147: The Hi-Res Tm Ramp Segment

    Hi-Res Option The Hi-Res Ramp Segment Ramp <rate> ° C/min res <res_setting> to ° <temp> ° Ramp 50.00 C/min res 4.0 to 800.00 ° TA I TGA 2950 B–9 NSTRUMENTS...
  • Page 148 Appendix B B–10 TA I TGA 2950 NSTRUMENTS...
  • Page 149 Hi-Res Option TA I TGA 2950 B–11 NSTRUMENTS...
  • Page 150 Appendix B B–12 TA I TGA 2950 NSTRUMENTS...
  • Page 151: Calcium Oxalate Example Scans

    Hi-Res Option Calcium Oxalate Example Scans TA I TGA 2950 B–13 NSTRUMENTS...
  • Page 152 Appendix B B–14 TA I TGA 2950 NSTRUMENTS...
  • Page 153 Hi-Res Option TA I TGA 2950 B–15 NSTRUMENTS...
  • Page 154 Appendix B (a) 1 ° C/min, Normal Ramp; (b) Res 5.0, 50 ° C/min; (c) Res 4.0, 50 ° min; (d) Res 3.0, 50 ° C/min; (e) 20 ° C/min, Normal Ramp B–16 TA I TGA 2950 NSTRUMENTS...
  • Page 155 Hi-Res Option TA I TGA 2950 B–17 NSTRUMENTS...
  • Page 156: Advanced Hi-Res Tm Techniques

    Appendix B Advanced Hi-Res Techniques What Can Be Resolved and What Cannot? B–18 TA I TGA 2950 NSTRUMENTS...
  • Page 157 Hi-Res Option Unresolvable Transitions TA I TGA 2950 B–19 NSTRUMENTS...
  • Page 158 Appendix B B–20 TA I TGA 2950 NSTRUMENTS...
  • Page 159 Hi-Res Option TA I TGA 2950 B–21 NSTRUMENTS...
  • Page 160: Selecting A Hi-Res Tm Technique

    Appendix B Selecting a Hi-Res Technique Dynamic Rate Hi-Res Ramp B–22 TA I TGA 2950 NSTRUMENTS...
  • Page 161: Constant Reaction Rate Hi-Res Tm Ramp

    Hi-Res Option Constant Reaction Rate Hi-Res Ramp TA I TGA 2950 B–23 NSTRUMENTS...
  • Page 162 Appendix B B–24 TA I TGA 2950 NSTRUMENTS...
  • Page 163 Hi-Res Option TA I TGA 2950 B–25 NSTRUMENTS...
  • Page 164: Weight Gain Experiments

    Appendix B Weight Gain Experiments B–26 TA I TGA 2950 NSTRUMENTS...
  • Page 165: Signature Analysis

    Hi-Res Option Signature Analysis TA I TGA 2950 B–27 NSTRUMENTS...
  • Page 166: Sample Quantity And Orientation

    Appendix B Sample Quantity and Orientation Exposed Surface Area B–28 TA I TGA 2950 NSTRUMENTS...
  • Page 167: Bubble Formation

    Hi-Res Option Bubble Formation TA I TGA 2950 B–29 NSTRUMENTS...
  • Page 168 Appendix B B–30 TA I TGA 2950 NSTRUMENTS...
  • Page 169 Hi-Res Option TA I TGA 2950 B–31 NSTRUMENTS...
  • Page 170: Thermocouple Placement

    Appendix B Thermocouple Placement Data Analysis Effects B–32 TA I TGA 2950 NSTRUMENTS...
  • Page 171: Derivative Plots

    Hi-Res Option Derivative Plots TA I TGA 2950 B–33 NSTRUMENTS...
  • Page 172: Adjusting Heating Rate

    Appendix B Adjusting Heating Rate B–34 TA I TGA 2950 NSTRUMENTS...
  • Page 173 Hi-Res Option TA I TGA 2950 B–35 NSTRUMENTS...
  • Page 174 Appendix B B–36 TA I TGA 2950 NSTRUMENTS...
  • Page 175: Adjusting Resolution Setting

    Hi-Res Option Adjusting Resolution Setting TA I TGA 2950 B–37 NSTRUMENTS...
  • Page 176 Appendix B B–38 TA I TGA 2950 NSTRUMENTS...
  • Page 177: Useful Resolutions Settings

    Hi-Res Option Useful Resolution Settings TA I TGA 2950 B–39 NSTRUMENTS...
  • Page 178 Appendix B B–40 TA I TGA 2950 NSTRUMENTS...
  • Page 179: Temperature Calibration

    Hi-Res Option Temperature Calibration TA I TGA 2950 B–41 NSTRUMENTS...
  • Page 180: Hi-Res Tm Transition Temperatures

    Appendix B Hi-Res Transition Temperatures B–42 TA I TGA 2950 NSTRUMENTS...
  • Page 181: Hi-Res Tm Sensitivity Segment

    Hi-Res Option Hi-Res Sensitivity Segment Hi-Res sensitivity <sens_setting> Hi-Res sensitivity 2.0 TA I TGA 2950 B–43 NSTRUMENTS...
  • Page 182: Understanding Sensitivity Setting

    Appendix B Understanding Sensitivity Setting B–44 TA I TGA 2950 NSTRUMENTS...
  • Page 183: Adjusting Sensitivity In Dynamic Rate Mode

    Hi-Res Option Adjusting Sensitivity in Dynamic Rate Mode TA I TGA 2950 B–45 NSTRUMENTS...
  • Page 184 Appendix B B–46 TA I TGA 2950 NSTRUMENTS...
  • Page 185: Adjusting Sensitivity In Constant Reaction Rate Mode

    Hi-Res Option Adjusting Sensitivity in Constant Reaction Rate Mode TA I TGA 2950 B–47 NSTRUMENTS...
  • Page 186 Appendix B B–48 TA I TGA 2950 NSTRUMENTS...
  • Page 187 Hi-Res Option TA I TGA 2950 B–49 NSTRUMENTS...
  • Page 188 Appendix B B–50 TA I TGA 2950 NSTRUMENTS...
  • Page 189: Abort Segment

    If the segment following the abort segment is equilibrate, initial temperature, ramp, Hi-Res ramp, isothermal or step, and the limit has not been reached yet, the limit will be tested TA I TGA 2950 B–51 NSTRUMENTS...
  • Page 190 An abort segment in front of a repeat segment provides a mechanism to terminate a loop prematurely. Abort segments B–52 TA I TGA 2950 NSTRUMENTS...
  • Page 191: Stepwise Isothermal Heating

    Then the sample heating is continued until the next transition is detected, whereupon, isothermal holding is TA I TGA 2950 B–53 NSTRUMENTS...
  • Page 192 The isothermal time is set to an arbitrary time, which is sufficiently large such that the segment will not terminate until the percent/minute limit has been reached. B–54 TA I TGA 2950 NSTRUMENTS...
  • Page 193 Another disadvantage of stepwise heating is that the decision to leave isothermal mode and continue heating is some- what arbitrary and may lead to incorrect assump- tions about the number and size of transitions. TA I TGA 2950 B–55 NSTRUMENTS...
  • Page 194 The second cause of anomalies is leaving the isothermal holding period prematurely during a transition because the percent/minute threshold for aborting the isothermal segment was set too high. This situation leaves a significant amount B–56 TA I TGA 2950 NSTRUMENTS...
  • Page 195 (%/minute) to a high level and either triggers another isothermal hold period or shows up as a backside shoulder on the weight loss curve. An example of using stepwise isothermal heating is shown in the following “Hi-Res TGA Examples” section. TA I TGA 2950 B–57 NSTRUMENTS...
  • Page 196: Hi-Res Tm Tga Examples

    (NaHCO ). Inadequate mixing or large granule size will reduce weight loss reproducibility. Note that potassium bicarbon- ate is very hygroscopic. The mixture must not be exposed to ambient humidity for long or a B–58 TA I TGA 2950 NSTRUMENTS...
  • Page 197: Dynamic Rate Scans

    TGA in about twice the time of the 20 C/minute ° scan, and about one tenth the time of the 1 minute scan. The method used for all scans was a single ramp segment. TA I TGA 2950 B–59 NSTRUMENTS...
  • Page 198 Ramp of NaHCO ; (c) 50 ° C/min Res 4.0 Hi-Res Ramp of Mixture; (d) 20 ° C/min Res 4.0 Hi-Res Ramp of KHCO ; (e) 20 ° C/min Normal Ramp of Mixture. Figure B.12 B–60 TA I TGA 2950 NSTRUMENTS...
  • Page 199: Varying Resolution Setting

    1% on each curve are due to the evaporation of surface water absorbed by the mixture. (a) 1 ° C/min Normal Ramp; (b) 20 ° C/min Normal Ramp; (1-8) Resolution setting Figure B.13 TA I TGA 2950 B–61 NSTRUMENTS...
  • Page 200: Varying Sensitivity Setting

    (a) 1 ° C/min Normal Ramp; (b) Sensitivity setting 1; (c) Sensitivity setting 2; (d) Sensitivity setting 4; (e) Sensitivity setting 8. Figure B.14 B–62 TA I TGA 2950 NSTRUMENTS...
  • Page 201: Constant Reaction Rate Scans

    As with dynamic rate mode (Figure B.13), we see that higher resolution setting (larger negative number) reduces transi- tion temperature. TA I TGA 2950 B–63 NSTRUMENTS...
  • Page 202 (a) Res -5.0, Sens 2.0, Semi-hermetic Pan; (b) Res -4.0, Sens 1.0, Open Pan; (c) 1 ° C/min Normal Ramp; (d) Res -4.0, Sens 2.0, Semi-hermetic Pan; (e) 20 ° C/min Normal Ramp. Figure B.15 B–64 TA I TGA 2950 NSTRUMENTS...
  • Page 203: Stepwise Isothermal Scans

    1: Abort next seg if %/min > 0.05 2: Ramp 1 ° C/min to 300 ° 3: Abort next seg if %/min < 0.005 4: Isothermal for 500 minutes 5: Repeat segment 1 til 300 ° TA I TGA 2950 B–65 NSTRUMENTS...
  • Page 204 It is usually wise to run confirming experiments by other TGA techniques, particularly if the sample material is of relatively unknown compo- sition. B–66 TA I TGA 2950 NSTRUMENTS...
  • Page 205 Hi-Res Option Figure B.16 Figure B.17 TA I TGA 2950 B–67 NSTRUMENTS...
  • Page 206: Monosodium Glutamate

    C/min; (e) 50 ° C/min; (f) 20 ° C/min. Figure B.18 If you should decide to run this sample, be aware that MSG foams significantly at these temperatures. If a sample size greater than B–68 TA I TGA 2950 NSTRUMENTS...
  • Page 207: Banana Taffy

    B.19 shows the result of a conventional constant ° heating rate scan of taffy at 10 C/minute. Figure B.20 shows the result of a 50 ° C/minute dynamic rate Hi-Res scan at resolution setting 4.0 and sensitivity setting 1.0. Figure B.19 TA I TGA 2950 B–69 NSTRUMENTS...
  • Page 208 ° C/minute Hi-Res scan of ° this sample takes about the same time as a 20 minute conventional scan while providing resolution improvement similar to that observed ° with the 50 C/minute Hi-Res scan. B–70 TA I TGA 2950 NSTRUMENTS...
  • Page 209: Plastic Laboratory Tubing

    Hi-Res scan. ° Maximum heating rates of 50 C/minute (Figure ° ° B.23), 20 C/minute (Figure B.24) and 10 minute (Figure B.25) were used with a method consisting of a single Hi-Res ramp segment. TA I TGA 2950 B–71 NSTRUMENTS...
  • Page 210 Here we can see the real beauty of dynamic rate Hi-Res TGA: better results in the same or less time as traditional constant heating rate TGA. Figure B.21 B–72 TA I TGA 2950 NSTRUMENTS...
  • Page 211 Hi-Res Option Figure B.22 Figure B.23 TA I TGA 2950 B–73 NSTRUMENTS...
  • Page 212 Appendix B Figure B.24 Figure B.25 B–74 TA I TGA 2950 NSTRUMENTS...
  • Page 213: References

    Thermochimia Acta., 100 (1986) 23-59. 2. Controlled Transformation Rate Thermal Analysis: The Hidden Face of Thermal Analysis, J. Rouquerol, Thermochimica Acta., 144 (1989) 209-224. Hi-Res is a trademark of TA Instruments, Inc. ® TYGON is a registered trademark of NORTON Co. ACCENT ®...
  • Page 214 Appendix B B–76 TA I TGA 2950 NSTRUMENTS...
  • Page 215: Appendix C: Tga 2950 Autosampler Option

    TGA 2950 Autosampler Option Appendix C: TGA 2950 Autosampler Option TA I TGA 2950 C–1 NSTRUMENTS...
  • Page 216 Appendix C C–2 TA I TGA 2950 NSTRUMENTS...
  • Page 217: Introducing The Auto Tga

    TGA 2950 Autosampler Option Introducing the Auto TGA TA I TGA 2950 C–3 NSTRUMENTS...
  • Page 218 Appendix C C–4 TA I TGA 2950 NSTRUMENTS...
  • Page 219: Getting Started

    TGA 2950 Autosampler Option Getting Started TA I TGA 2950 C–5 NSTRUMENTS...
  • Page 220: The Tga 2950 Instrument

    Appendix C The TGA 2950 Instrument AUTO SELECT TGA 2950 Thermogravimetric Analyzer C–6 TA I TGA 2950 NSTRUMENTS...
  • Page 221 TGA 2950 Autosampler Option SCROLL AUTO SELECT, TARE, LOAD AUTO SELECT SCROLL AUTO SELECT SCROLL AUTO SELECT TA I TGA 2950 C–7 NSTRUMENTS...
  • Page 222 Appendix C TARE SCROLL/TARE SCROLL TARE LOAD C–8 TA I TGA 2950 NSTRUMENTS...
  • Page 223 TGA 2950 Autosampler Option SCROLL/LOAD LOAD functions can NOTE: be stopped by pushing the STOP key on the instrument keypad. UNLOAD FURNACE START STOP REJECT (SCROLL/STOP) TA I TGA 2950 C–9 NSTRUMENTS...
  • Page 224: Calibrating The Auto Tga

    Appendix C Calibrating the Auto TGA C–10 TA I TGA 2950 NSTRUMENTS...
  • Page 225: Running Experiments

    TGA 2950 Autosampler Option Running Experiments TA I TGA 2950 C–11 NSTRUMENTS...
  • Page 226: Preparing The Samples

    Appendix C Preparing the Samples Selecting Sample and Tare Pans Tare Pan C–12 TA I TGA 2950 NSTRUMENTS...
  • Page 227: Taring The Sample Pans

    TGA 2950 Autosampler Option Taring the Sample Pans View the Autosampler log, found on the Instrument NOTE: Control software, after taring to determine which pan, if any, does not tare during the procedure (Error 118). If a tare error occurs, replace the pan and manually retare it.
  • Page 228 Appendix C Automatic Tare C–14 TA I TGA 2950 NSTRUMENTS...
  • Page 229 TGA 2950 Autosampler Option SCROLL TARE The advantage to using the Auto TGA is to save NOTE: time and effort; therefore, it would not be efficient to perform manual tare operations on each sample, as that would defeat the purpose of an automatic operation.
  • Page 230: Loading The Samples

    Manually loading the sample pan onto the hang- CAUTION: down wire may damage the balance mechanism. LOAD The position of the thermocouple should be the NOTE: same as it was during temperature calibration. C–16 TA I TGA 2950 NSTRUMENTS...
  • Page 231 TGA 2950 Autosampler Option UNLOAD TA I TGA 2950 C–17 NSTRUMENTS...
  • Page 232: Setting Up An Experiment

    Setting Up an Experiment If you are planning to run the Autosampler, be sure to specify furnace open at method end, as NOTE: well as air cool, to cool down the furnace between samples. C–18 TA I TGA 2950 NSTRUMENTS...
  • Page 233: Manual Operation

    TGA 2950 Autosampler Option Manual Operation AUTO SELECT SCROLL/ AUTO SELECT Tracking the TGA Autosampler Status TA I TGA 2950 C–19 NSTRUMENTS...
  • Page 234: Interrupting A Run

    Appendix C Interrupting a Run Stop Reject C–20 TA I TGA 2950 NSTRUMENTS...
  • Page 235: Appendix D: Tga 2950 Ega Furnace Option

    TGA 2950 EGA Furnace Option Appendix D: TGA 2950 EGA Furnace Option Introducing the EGA Furnace ....D-3 EGA Furnace Specifications ....D-5 Installing the EGA Furnace ....... D-6 First-Time Installation ......D-6 Removing and Reinstalling the EGA Furnace ........D-14 EGA Furnae Removal ....
  • Page 236 Appendix D D–2 TA I TGA 2950 NSTRUMENTS...
  • Page 237: Introducing The Ega Furnace

    The EGA furnace and the standard TGA furnace can be exchanged easily on the instrument after initial hardware installa- tion. Version 3.3B (or higher) of the TGA 2950 instrument software is required for the EGA furnace.
  • Page 238 50°C/min. A Platinel II* thermocouple is positioned in the furnace, just above the sample pan, where it monitors the sample environment temperature. *Platinel II is a registered trademark of Engelhard Industries. D–4 TA I TGA 2950 NSTRUMENTS...
  • Page 239: Ega Furnace Specifications

    TGA 2950 EGA Furnace Option The furnace base moves the furnace assembly up around the sample pan to the closed position, or down away from the sample pan to the open position. EGA Furnace Specifications Refer to Table D.1 below for the specifications of the EGA furnace.
  • Page 240: Installing The Ega Furnace

    Make sure that you place the heater power WARNING switch in the off position before removing or installing the furnace on the TGA 2950 instrument. Version 3.3B (or higher) of the TGA 2950 instrument software is required for the EGA furnace.
  • Page 241 TGA 2950 EGA Furnace Option Make sure that you do not remove the furnace from its housing. 3. Unplug the AIR COOL line from the bottom of the furnace arm/base. When you remove the AIR COOL line, do not let it NOTE: slip back into the instrument cabinet.
  • Page 242 Refer to Figure D.3. Replace the upper screws using the long screws with spacers and replace the lower screws using the short screws without spacers. D–8 TA I TGA 2950 NSTRUMENTS...
  • Page 243 TGA 2950 EGA Furnace Option Spacer Cleat Cleat Short Screw Long Screw Figure D.3 Installing the EGA Mounting Screws, Spacers, and Cleats 8. Tighten the upper two mounting screws fully, then loosen each of them no more than one full turn, so that the flat sides of the cleats are aligned vertically as shown in Figure D.4.
  • Page 244 See Figure D.5 for the correct placement of the lines. Be sure to install the wire ties (supplied in the kit) around the cooling lines to prevent water leakage. D–10 TA I TGA 2950 NSTRUMENTS...
  • Page 245 11. Plug the EGA furnace arm into the connec- tor on the carriage and tighten the lower two mounting screws using the 3/32-inch ball driver supplied with the TGA 2950 EGA. See Figure D.6 on the next page. TA I TGA 2950 D–11...
  • Page 246 To reach the upper left mounting screw, insert the ball driver between the water connections on the left side of the furnace housing as shown in Figure D.7. D–12 TA I TGA 2950 NSTRUMENTS...
  • Page 247 TGA 2950 EGA Furnace Option Figure D.7 Tightening the Upper Mounting Screws 13. Connect the purge hose to the gas purge inlet on the right side of furnace. Hold onto the glass purge tube with one hand CAUTION: while you install the purge hose to avoid breaking the glass.
  • Page 248: Removing And Reinstalling The Ega Furnace

    Make sure that you place the heater power WARNING switch in the off position before removing or installing the furnace on the TGA 2950 instrument. To remove or reinstall the furnace, you will have to remove the furnace arm from its connection inside the slot on the front of the instrument cabinet.
  • Page 249 TGA 2950 EGA Furnace Option 4. Loosen the bottom two mounting screws using the 3/32-inch ball driver supplied with the TGA 2950 EGA. See Figure D.6. 5. Unplug and remove the EGA furnace arm/ base from the instrument cabinet. 6. Unplug the AIR COOL line from the bottom of the furnace arm/base.
  • Page 250: Ega Furnace Installation

    4. Press the FURNACE key to raise the furnace carriage until the lower mounting screws are just below the top edge of the enlarged cutout in the instrument faceplate. Then press the STOP key. D–16 TA I TGA 2950 NSTRUMENTS...
  • Page 251 TGA 2950 EGA Furnace Option 5. Plug the EGA furnace arm into the connec- tor on the carriage and tighten the lower two mounting screws using the 3/32-inch ball driver supplied with the EGA. See Figure D.6 on page D-12.
  • Page 252: Connecting The Spectrometer

    Appendix D Connecting the Spectrometer The TGA 2950 EGA furnace allows you to connect a spectrometer, such as a FTIR spec- trometer, to the instrument. To connect any spectrometer, you will need to use a transfer line (supplied by the spectrometer manufacturer) to transport the gas evolved from the sample on the TGA to the spectrometer.
  • Page 253 TGA 2950 EGA Furnace Option To connect your spectrometer to the EGA furnace follow these steps: 1. Install a Swagelok nut, drive ring, and ferrule on the correct length of transfer line, leaving more than two inches of transfer line projecting beyond the ferrule.
  • Page 254 3/8-inch wrench on the exhaust fitting flats to prevent them from turning. If the transfer line is not straight, or has WARNING heavy oxide deposits on it, the sample tube may be broken as the line is inserted. D–20 TA I TGA 2950 NSTRUMENTS...
  • Page 255: Using The Ega Furnace

    TGA 2950 EGA Furnace Option Using the EGA Furnace After proper installation, the EGA furnace can be used as you would normally use the TGA standard furnace. No special procedures must be followed when preparing TGA samples, setting up methods, or running experiments.
  • Page 256: Cleaning The Quartz Furnace Tube

    Do not disturb the hangdown wire and WARNING furnace thermocouple located directly above the furnace when cleaning the fur- nace, as damage may result. FURNACE D–22 TA I TGA 2950 NSTRUMENTS...
  • Page 257 TGA 2950 EGA Furnace Option TA I TGA 2950 D–23 NSTRUMENTS...
  • Page 258 Appendix D D–24 TA I TGA 2950 NSTRUMENTS...
  • Page 259: Index

    Cooling (status code) 4-18 arm 4-6 arm sensor 4-6 cooling gas line 2-18 unpacking 2-20 binary address switches 2-16 description TGA 2950 4-3 cabinet 1-4, 4-13 display 1-5 cable GPIB 2-15 EGA furnace 1-11, 4-11 Calib (status code) 4-17 Ending (status code) 4-18...
  • Page 260 HEATER switch 1-10 furnace housing 4-10 Heating (status code) 4-18 furnace tube High Resolution option B-5 to cleaning D-22 B-12 FURNACE up key 1-7 Holding (status code) 4-18 fuses 5-16 Hot (status code) 4-19 I–2 TA I TGA 2950 NSTRUMENTS...
  • Page 261 Index ordering information A-1 Initial (status code) 4-19 oxygen-free atmosphere 3-22 instrument. See TGA 2950 Iso (status code) 4-19 pans 3-8, 4-7 cleaning 3-9 unloading 3-21 Jumping (status code) 4-19 parts 5-21 power problems failures 5-18 keypad 1-6 POWER switch 1-10...
  • Page 262 1-4 Temp* (status code) 4-21 adjusting 2-29 calibration 3-6 test functions 5-19 SCROLL key 1-6 TGA 2950 accessories 1-11 to 1-12 SCROLL-STOP keys 1-8 address switches 2-15 air cool 3-16 Set Up (status code) 4-20 autosampler C-3 to C-20...
  • Page 263 Index TGA 2950 (cont’d) instrument characteristics 1-12 Unload (status code) 4-21 keypad 1-6 lines UNLOAD key 1-7 cooling gas 2-18 purge 2-17 loading samples 3-11 location 2-9 operating parameters 1-12 Weight # (status code) 4-21 power problems 5-18 power switch 1-10...
  • Page 264 Index I–6 TA I TGA 2950 NSTRUMENTS...

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