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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 NSTRUMENTS...
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 ......
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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....
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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...
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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 ...
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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...
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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 ....
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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...
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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 ......
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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....
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...
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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...
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.
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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...
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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...
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...
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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...
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-...
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.
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...
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...
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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...
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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.
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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.
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.
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...
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...
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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...
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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.
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 ..
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Installing the 2950 2–2 TA I TGA 2950 NSTRUMENTS...
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...
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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...
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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...
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...
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 ·...
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.
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.
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...
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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.
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...
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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.
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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...
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...
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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...
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...
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...
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...
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...
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Unpacking the Balance Foam Insert TA I TGA 2950 2–21 NSTRUMENTS...
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...
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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...
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Installing the 2950 2–24 TA I TGA 2950 NSTRUMENTS...
Installing the Hang-Down Wires Aligning the Sample Hang-Down Wire LOAD TA I TGA 2950 2–25 NSTRUMENTS...
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Installing the 2950 2–26 TA I TGA 2950 NSTRUMENTS...
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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...
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Installing the 2950 FURNACE UNLOAD 2–28 TA I TGA 2950 NSTRUMENTS...
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...
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...
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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...
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...
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...
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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...
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Running a TGA Experiment FURNACE TA I TGA 2950 3–13 NSTRUMENTS...
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...
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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.
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Running Experiments 3–18 TA I TGA 2950 NSTRUMENTS...
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...
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...
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...
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Running Experiments 3–24 TA I TGA 2950 NSTRUMENTS...
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.
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(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...
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.
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...
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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.
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...
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...
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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...
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.
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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...
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...
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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...
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.
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...
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...
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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...
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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...
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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...
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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...
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Technical Reference 4–22 TA I TGA 2950 NSTRUMENTS...
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...
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Maintenance and Diagnostics TGA Test Functions ......... 5-19 The Confidence Test ......5-19 Replacement Parts ........5-21 5–2 TA I TGA 2950 NSTRUMENTS...
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.
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...
(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...
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.
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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...
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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...
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...
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(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...
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...
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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...
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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...
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...
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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...
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...
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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...
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.
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.
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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...
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...
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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...
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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...
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Maintenance and Diagnostics 5–24 TA I TGA 2950 NSTRUMENTS...
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...
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Appendix B B–10 TA I TGA 2950 NSTRUMENTS...
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Hi-Res Option TA I TGA 2950 B–11 NSTRUMENTS...
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Appendix B B–12 TA I TGA 2950 NSTRUMENTS...
Hi-Res Option Calcium Oxalate Example Scans TA I TGA 2950 B–13 NSTRUMENTS...
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Appendix B B–14 TA I TGA 2950 NSTRUMENTS...
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Hi-Res Option TA I TGA 2950 B–15 NSTRUMENTS...
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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...
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Hi-Res Option TA I TGA 2950 B–17 NSTRUMENTS...
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...
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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...
Then the sample heating is continued until the next transition is detected, whereupon, isothermal holding is TA I TGA 2950 B–53 NSTRUMENTS...
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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...
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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...
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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...
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(%/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...
(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...
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...
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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...
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...
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...
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(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...
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...
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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...
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Hi-Res Option Figure B.16 Figure B.17 TA I TGA 2950 B–67 NSTRUMENTS...
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...
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...
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° 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...
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...
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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...
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Hi-Res Option Figure B.22 Figure B.23 TA I TGA 2950 B–73 NSTRUMENTS...
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Appendix B Figure B.24 Figure B.25 B–74 TA I TGA 2950 NSTRUMENTS...
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 ®...
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Appendix B B–76 TA I TGA 2950 NSTRUMENTS...
Appendix C The TGA 2950 Instrument AUTO SELECT TGA 2950 Thermogravimetric Analyzer C–6 TA I TGA 2950 NSTRUMENTS...
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TGA 2950 Autosampler Option SCROLL AUTO SELECT, TARE, LOAD AUTO SELECT SCROLL AUTO SELECT SCROLL AUTO SELECT TA I TGA 2950 C–7 NSTRUMENTS...
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Appendix C TARE SCROLL/TARE SCROLL TARE LOAD C–8 TA I TGA 2950 NSTRUMENTS...
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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...
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.
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Appendix C Automatic Tare C–14 TA I TGA 2950 NSTRUMENTS...
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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.
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...
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TGA 2950 Autosampler Option UNLOAD TA I TGA 2950 C–17 NSTRUMENTS...
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...
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 ....
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Appendix D D–2 TA I TGA 2950 NSTRUMENTS...
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.
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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...
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.
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.
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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.
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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...
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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.
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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...
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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...
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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...
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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.
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.
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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.
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...
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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.
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.
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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.
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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...
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.
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...
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TGA 2950 EGA Furnace Option TA I TGA 2950 D–23 NSTRUMENTS...
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Appendix D D–24 TA I TGA 2950 NSTRUMENTS...
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