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Discovery TGA™ Getting Started Guide

Page 25

Discovery TGA Sampling System

The following tables contain the specifications associated with the TGA sample pans, balance mechanism, 
and furnace.

WARNING: Do not use corrosive gases, hydrogen, or any other explosive gas in the TGA fur-
nace.

AVERTISSEMENT: N'utilisez pas de gaz corrosifs, d'hydrogène ou tout autre gaz explosif dans 
le four TGA.

WARNING: Oxygen can be used as a purge gas in the TGA. However, if you use oxygen as a 
purge gas, you must make sure the furnace is cleaned of hydrocarbons that could combust.

AVERTISSEMENT: L'oxygène peut être utilisé comme gaz de drainage dans le TGA. Toutefois le 
four doit rester propre pour que les hydrocarbures volatils, qui peuvent brûler, soient éliminés.

Table 4:

Sample Pan Options for 25-Pan Tray

Item/Area

Specifications

Types of pans available

Platinum, ceramic (Al

2

O

3

), aluminum

Volume capacity and temperature range

  20 µL Sealed aluminum (to 600°C)
  50 µL Platinum (to 1000°C)
  80 µL Aluminum (bottom of sealed pan, to 600°C)
100 µL Platinum (to 1000°C)
100 µL Platinum-HT (to 1000°C)
100 µL Ceramic (to 1200°C)
250 µL Ceramic (to 1200°C)

Number of pans per tray

25 Pans

Table 5:

Balance Mechanism

Item/Area

Specifications

Weighing capacity (sample)

1.0 gram

Dynamic weighing range

Low range: 100 mg
High range: 1000 mg

Resolution

0.01 µg

Accuracy

< + 0.1% of value or 10 µg, whichever is greater

Summary of Contents for TGA5500

Page 1: ...Getting Started Guide for Models 55 550 5500 Revision C Issued February 2018 Discovery TGA Thermogravimetric Analyzer...

Page 2: ...tents trademarks copyrights or other intellectual property TA Instruments Operating Software as well as Module Data Analysis and Utility Software and their asso ciated manuals and online help are prop...

Page 3: ...Manual Supplement Please click the TA Manual Supplement link to access the following important information supplemental to this Getting Started Guide TA Instruments Trademarks TA Instruments Patents O...

Page 4: ...the heating of materials CAN CSA C22 2 No 61010 2 081 04 Particular requirements for automatic and semi automatic labora tory equipment for analysis and other purposes For European Economic Area In ac...

Page 5: ...ance with Council Directive 2014 30 EC of the European Parliament and of the Council of 26 February 2014 on the harmonization of the laws of the Member States relating to electromagnetic compatibility...

Page 6: ...e not trained in electrical procedures do not remove the cabinet covers unless specifically instructed to do so in the manual Maintenance and repair of internal parts must be performed only by TA Inst...

Page 7: ...sez pas d hydrog ne ou tout autre gaz explosif dans le four TGA WARNING Oxygen can be used as a purge gas in the TGA However the furnace must be kept clean so that volatile hydrocarbons which may comb...

Page 8: ...he furnace when it is mov ing The seal is very tight AVERTISSEMENT cartez vos doigts et tous les autres objets du chemin du four lorsqu il est en mouvement L tanch it est tr s herm tique WARNING Use t...

Page 9: ...EGA Furnace for TGA 55 and TGA 550 15 Infrared IR Furnace for TGA 5500 16 Discovery TGA Autoloader or Autosampler 17 Hi Res TGA 18 Modulated TGA MTGA 19 Other Discovery TGA Accessories 19 The Discove...

Page 10: ...Lower Furnace Assembly on the TGA 5500 48 Closing the Balance Assembly 51 Balance Conditioning 51 Filling the Heat Exchanger Reservoir 51 Purging Air from the Heat Exchanger System 52 Installing the A...

Page 11: ...Discovery TGA Getting Started Guide Page 11 Replacing Fuses 65 Maintaining the Heat Exchanger 65 Replacement Parts 66...

Page 12: ...erial that exhibits a weight change and to detect phase changes due to decom position oxidation or dehydration This information helps the scientist or engineer identify the percent weight change and c...

Page 13: ...he components of the TGA Balance Assembly The TGA balance assembly is a null balance system consisting of the balance meter movement the bal ance arm the balance position sensor the hang down wire ass...

Page 14: ...re wound furnace is a resistance heater wound on alumina ceramic which allows sample zone temperatures as high as 1 000 C with heat ing rates up to 100 C min The housing is mounted to a furnace base t...

Page 15: ...the housing allows connection of a transfer line to carry exhaust gas to a spectrometer such as a mass spectrometer Because the heater is external to the sample tube evolved gases from sample decompo...

Page 16: ...es a second independent thermocouple to protect the furnace from excessive temperature Heat shield assemblies above and below the energy absorbing tube reduce heat losses from the ends of the furnace...

Page 17: ...oloader To calibrate the Autoloader refer to TRIOS Online Help Autosampler The Discovery TGA Autosampler shown below allows you to place multiple samples on the platform for automatic loading and run...

Page 18: ...ntinuously modified in response to changes in the rate of decomposition of the sample so as to optimize both weight change resolution and time of analysis This TGA technique supplied with the Discover...

Page 19: ...on energy continuously allows you to follow changes in the activation energy during the reaction as a function of temperature or conversion The calculation of activation energy is model free no knowle...

Page 20: ...y describes the basic layout of these functions Figure 8 Discovery TGA user interface display TGA 5500 shown The instrument user interface has three basic sections The status line along the top of the...

Page 21: ...into effect and the data that has been generated is saved This is the same function as Stop on the instrument control software If an experiment is not running the instrument is in a standby or method...

Page 22: ...splays options for manual controls such as Event Air Cool and Heat Exchanger Autosampler Autoloader Autosampler Displays a graphical representation of the Autosampler tray indicating the status of the...

Page 23: ...Name Description Help The Help button can be found on the lower right side of some screens and displays information regarding use of the currently displayed touch screen Motion Stop Displayed while th...

Page 24: ...condensing Installation Category II Pollution Degree 2 Maximum altitude 2000 m The degree of protection for this instrument according to IEC 529 is IP20 Temperature range TGA 55 TGA 550 TGA 5500 Room...

Page 25: ...xyg ne peut tre utilis comme gaz de drainage dans le TGA Toutefois le four doit rester propre pour que les hydrocarbures volatils qui peuvent br ler soient limin s Table 4 Sample Pan Options for 25 Pa...

Page 26: ...llation which includes removing the shipping bracket and unpacking the balance 4 Setting up system communication between the instrument and computer controller 5 Connecting purge gas lines to the GDM...

Page 27: ...the following guidelines The Discovery TGA system should be In A temperature controlled area Temperatures should be in range 20 to 35 C A clean vibration free environment preferably on the ground floo...

Page 28: ...that the step was not completed previously To remove the shipping bracket 1 Cut the wire tie securing the air cool line to the water circulator tubing then loosen the foot of the furnace shipping bra...

Page 29: ...the balance This very important procedure must be completed before you can use the Discovery TGA 1 Carefully remove the balance housing cover by loosening the screws Figure 10 Removing the balance hou...

Page 30: ...nate contact with the beam Gently remove the foam inserts from the sample and tare sides being careful not to touch the balance Refer to the figure below Figure 12 Removing the foam inserts 4 Put the...

Page 31: ...k Panel Port Function Power Entry Module power cord and switch Provides power and protective earthing to the system Fuses Provides overcurrent protection REACTIVE GAS Port for introducing an additiona...

Page 32: ...s control of heat exchanger WARNING If connecting oxygen it should ONLY be connected to the GAS 2 and REACTIVE GAS ports AVERTISSEMENT En cas de connexion de l oxyg ne il ne doit tre connect aux ports...

Page 33: ...stall an external drier and a 5 m filter 1 Locate the GAS 1 port on the back of the Discovery TGA The GAS 1 port is used to purge both the sample and balance areas As such an inert gas such as nitroge...

Page 34: ...valves that are set to 140 kPa gauge 20 psig The source pressure setting should not go above this value MISE EN GARDE Les conduites de gaz 1 et 2 alimentent une soupape de d tente de pression r gl e 1...

Page 35: ...s into a pressure relief valve that is set to 140 kPa gauge 20 psig The source pressure setting should not go above this value MISE EN GARDE La conduite de refroidissement de l air alimente une soupap...

Page 36: ...d of this hose to the connector labeled SUPPLY on the side of the instrument Figure 15 SUPPLY and RETURN connectors on the side of the instrument 4 Connect the other end of the water hose marked SUPPL...

Page 37: ...nto the power entry module shown below Figure 16 Power cable in power entry module on back panel of the instrument 3 Plug the power cable into the wall outlet Installing the Autosampler Tray Follow th...

Page 38: ...for Installation on page 28 have been completed Both the balance housing cover and balance cover should already be removed at this point in the installation 2 Loosen the three screws circled below on...

Page 39: ...des from the opening in the purge control cap Be sure to hold the installation tool in place as it will fall out of the tare tube opening if released Figure 20 8 Usingtweezers gentlyhangthedouble bend...

Page 40: ...g Down Wire on the TGA 5500 Before you can install the sample hang down wire you must install the sample tube upper reflective assembly that surrounds the wire Follow these steps 1 Locate the upper re...

Page 41: ...length of the upper reflective assembly tube until the sample hang down wire has been fully installed CAUTION During installation take care not to bend the hang down wires or damage the hang down loop...

Page 42: ...ouble bend hook is at the top 10 With the sample hang down wire still in its case insert the bottom of the wire into the sample hang down installation tool as shown below Then remove the installation...

Page 43: ...it slowly feeding it through the purge control cap until the top of the wire protrudes from the opening in the cap 14 Cover the furnace opening with a flat object that will completely block the openin...

Page 44: ...fils suspendus et de ne pas endommager les boucles suspendues 1 Verify that the instructions found in Preparing the Discovery TGA for Installation on page 28 have been completed Both the balance housi...

Page 45: ...procedures These procedures are performed with pans loaded on the hang down wires Leveling the Instrument Place a level across the rails of the instrument as shown below Figure 29 Leveling the instru...

Page 46: ...s used for TGA 55 and TGA 550 and the short edge shown here as the right edge is used for the TGA 5500 d Tighten the up down screws to lock them in position e Turn the center balance assembly hex head...

Page 47: ...sample pan is not centered and hanging freely within the furnace level the instrument by adjusting the two front feet on the bottom Turn the feet clockwise to lengthen or counterclockwise to shorten...

Page 48: ...ccessory kit 4 Carefully remove the lower furnace assembly from the plastic shipping tube 5 Orient the lower furnace assembly shown below so that the air cool inlet points to the left as you slide it...

Page 49: ...Figure 37 B should align with the inlet and outlet ports on the furnace housing allowing for light to pass through Figure 38 Rotate the lower furnace assembly until achieving the proper alignment Figu...

Page 50: ...er furnace accessory cable installed 13 Connect the 1 8 inch Teflon TFE tubing from the base of the instrument to the LFA air cool inlet as shown in the figure below Note that the figure below also di...

Page 51: ...irst installed Whenever the balance housing is opened Whenever the instrument is powered off for an extended period of time For more information related to conditioning the balance see Conditioning th...

Page 52: ...CAUTION Do not put any liquid other than distilled water and TA Instruments TGA Conditioner in the heat exchanger reservoir MISE EN GARDE Ne versez aucun liquide autre que de l eau distill e et l agen...

Page 53: ...instrument After unpacking the instrument and installing the instrument completely see instructions in this chapter you will be ready to run samples using the Autosampler 1 Locate the open slot on the...

Page 54: ...le connection and fuses The power switch is used to turn the TGA system on and off To power on the system 1 Check the connection between the TGA Ethernet switch and the controller Make sure each compo...

Page 55: ...task it is recommended that you leave the instrument on To ensure proper shutdown of the instrument it is recommended that you execute a shutdown from the user interface or TRIOS software before turn...

Page 56: ...ing flow rates Creating or choosing the test procedure and entering experiment information in TRIOS software Selecting and taring the sample pan Loading the sample Starting the experiment Unloading th...

Page 57: ...ument is not level See Leveling the Discovery TGA and Aligning the Balance on page 45 for instructions to solve this problem The hang down wire is not straight Replace the hang down wire see Installin...

Page 58: ...s the standard goes through its Curie Point its attraction to the magnet changes appearing as a weight change The extrapolated endpoint of this weight change is adjusted to agree with the material s k...

Page 59: ...the pans that can be used with the Discovery TGA Autosampler Taring the Sample Pan s Taring of all sample pans on the tray must be done before the sample is loaded to ensure that the balance gives yo...

Page 60: ...xperiment if desired in order to obtain a record of the weight A preweight is valuable for highly volatile materials This function is performed before you start an experiment and the weight is stored...

Page 61: ...periment you can stop it at any point by selecting Stop through the instrument control software or by touching the STOP button on instrument user interface NOTE See Shutting Down the Discovery TGA on...

Page 62: ...n one full turn may cause the screws to interfere with the inside of the instrument cabinet causing damage to the instrument MISE EN GARDE Desserrer les deux vis sup rieures de fixation plus d un tour...

Page 63: ...e optimum performance from your instrument and keep the balance housing dry Perform a balance conditioning when the instrument is first installed and whenever the balance housing is opened In order to...

Page 64: ...s may damage the pans MISE EN GARDE N utilisez pas de lavage l eau acidul e pour nettoyer les bacs en platine HT car cela risque d endommager les bacs Cleaning the User Interface Screen You can clean...

Page 65: ...the level and quality of the liquid coolant If the level drops too low or the coolant becomes contaminated this could result in problems with your instrument CAUTION Do not put any liquid other than...

Page 66: ...ls and Parts Part Number Description 259508 000 Brass tweezers 259509 000 Spatula curved 165 mm long 271621 001 O ring furnace housing to balance chamber 269920 006 Balldriver 9 64 hex tool 269920 004...

Page 67: ...ard with TGA 5500 957207 903 957207 904 50 L platinum sample pans package of 3 100 L platinum sample pans package of 3 957387 902 100 L platinum HT sample pans package of 3 957329 903 957329 904 100 L...

Page 68: ...1001 002 Mass Spectrometer Interface Kit for the EGA furnace TGA 55 and TGA 550 200413 002 Calibration weight 100 mg Class 1 200413 001 Calibration weight 50 mg Class 1 900905 901 Calcium oxalate mono...

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