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LINSEIS STA PT1600

Thermogravimetric Analyzer
Instruction Manual

Linseis Messgeräte GmbH
Vielitzer Str. 43
D-95100 Selb

Tel.: 0049 9287 880-0
Fax: 0049 9287 70488
Mail: info@linseis.de
Internet: www.linseis.com

Notes:

1. GENERAL INFORMATION .................................................................................................... 1

2. BASIC SYSTEM SAFETY INFORMATION .......................................................................... 2

3. PRECAUTIONS & REQUIREMENTS ................................................................................... 4

3.1. Protecting the Operator..................................................................................................................... 4
3.2. Protecting the instrument ................................................................................................................. 4

4. REQUIRED FACILITIES FOR INSTALLATION ................................................................. 5

5. INSTRUMENT DESCRIPTION .............................................................................................. 6

5.1. General information .......................................................................................................................... 6
5.2. Specifications..................................................................................................................................... 7
5.3. Measuring Systems ............................................................................................................................ 8
5.3.1. Linseis STA and High temperature DSC Measuring Heads .................................................................. 9
5.3.2. Type / temperature range / atmospheres ......................................................................................... 10

5.4. Furnaces .......................................................................................................................................... 11
5.5. Front Image of Instrument............................................................................................................... 12
5.6. Rear Image of Instrument ................................................................................................................ 13

6. INSTALLATION..................................................................................................................... 14

6.1. Set Up Equipment Placement .......................................................................................................... 14
6.2. Electrical wiring ............................................................................................................................... 14
6.3. Installing the TA-WIN & WIN-STA Software ..................................................................................... 15
6.4. Installation and change of the measuring System ............................................................................ 16
6.4.1. Preparation ........................................................................................................................................ 16
6.4.2. Disassemble measuring system ......................................................................................................... 17
6.4.3. Assemble measuring system ............................................................................................................. 17
6.4.4. Tare Balance ...................................................................................................................................... 18
6.4.5. Correction measurement .................................................................................................................. 19

7. FURNACE MAINTANACE ................................................................................................... 24

7.1. Dismount furnace ............................................................................................................................ 24
7.2. Replacing the furnace heating elements .......................................................................................... 25
7.2.1. 1400°C and 1600 °C furnace .............................................................................................................. 25
7.2.2. 1750°C furnace .................................................................................................................................. 28

7.3. Change furnace thermocouple......................................................................................................... 30

8. PREPARING A MEASUREMENT ....................................................................................... 32

..................................................4..........................................3...................................... PERFORMING A SAMPLE CURVE ................................ Load Controller Set Values .......... GAS FLOW IN THERMOGRAVIMETRIC EXPERIMENTS ......................... 43 13.................... 54 15....................................6..............................3.................3...............3..................... 49 13....................................3.......................................................................................................................................................................7.............................1.............................................. 43 13.. 46 13...... 51 13................................................................................................... GASES AND THEIR LIMITATIONS .................................. Display Current Values ........................................ PERFORMING A ZERO BASELINE CURVE................................................................1.....................5................................................. Graphic Display ............................................ Relays ................3. TG+DTA/HDSC Measurement .................................8................................. 51 13......... Program the Controller Set Values .............................................................................................. Manual Adjustment ....................................... 53 13.3....................... Balance Setup .........3.........................3....................... 44 13................. DTA/HDSC Measurement ........................10.................9..................................................... 39 12..............2........ 46 13.......... 49 13..................... Adjust Cold Junction Reference .. Setup Data Acquisition .......................................................................................................9............. Program Controller ......................................6.............................................................................. 52 13............................................2.............................. SELECTION OF THE GAS ATMOSPHERE...............2........................6................ 42 13..........3.................5......................3......... 47 13...................................................... 61 ................. 42 13........................................ COMPATIBILITY OF CRUCIBLE MATERIALS AND SOME SUBSTANCES .................................................................................................................. 48 13........................................ PID-Parameters.......................................... 52 13.....................3................................. Delete Controller Set Values................... Start and Stop Measurement........................1........2............................................................................................... 52 13.................................2......... 46 13...... 44 13......1.. 53 14................................................ 43 13...... Real-time graphic ...............3................................. 41 13............................................................................. 47 13.................... 37 11............................. 47 13............. Type of Measurement .............................................................................................................. 47 13................................................................2....2................2............................................................................................................................................ 42 13...... 50 13...................................1.................................................................. Example TG Measurement ................................... Store Controller Set Values..1...4...............6......... Zero Point Definition .................................1....................................................................................................................................... Controller Set Values ............... Zero Adjustment .........................4....... Automatic Adjustment .............. LINSEIS STA MEASUREMENT SOFTWARE . 52 13... TG Measurement ........ 36 10...................... 42 13.........3.. Description of the Input Parameter.................1.....................................7................................. Example TG – DTA Measurement ....................................4......... 42 13. Example DTA Measurement .............................................................................6......................3...............................................2....... Uncontrolled Preheating ...............6......................................

..........................5....................................1....8..............4...............................1... Legend .................2........................................................... 81 16............................................................................................... Evaluate Traces ............................. Introduction .................................................................................................5................... How to perform an ASCII export ...... 84 16........................................................ LINSEIS STA EVALUATION SOFTWARE .............1........... 87 16................ Menu and Dialog Sequence ........................................................................... Lines ............. Correction Procedure .... 72 16..........................3.....................................................................6......5................ 71 16......2................... Evaluation Icon ..4............................ 79 16....................................9............................................. Open Existing Evaluation ......... 69 16.................. 80 16................ 69 16.................................................... Evaluation of Measurements ........................................................................................................ 69 16............. Info Field ..........................6...... 75 16....... 71 16...............1............................................................... Print .................2.. 74 16.....................................6.2...............................7..............................................................................................4........................................................................................................................................... Program description ..... 88 16.....................1..................................................................... 74 16...............7.................. 74 16..........................................................................................................12.................................. 86 16..............................................................3........ Various Evaluations Simultaneously ..........................6..........................1..................................................................2.5.............................................................................4................................................................................................................................... Name and Directory Conventions ...........................................6..................................................5.......... 98 16......................... Miscellaneous ............ 68 16.............................................. Data Formats ................................................................... 73 16.................................................... Minimum Hardware + Software Requirements ....6......................5.........................................6...............................6.........................................2.................................................. 75 16...............................3............. 90 Data Structures ..10............................................................................. Hints ..................5................................................................................................................3................ 72 16............................... Traces in the Evaluation ........................4............. Curve Arithmetic................................6................................. 73 16............................................................................................................. 83 16.......................... Delete Traces ................................................................................................................2............... Start new Evaluation ......3.............................................................. Defaults for Traces........6...........................................................3......3..............................................11..... Arrange Evaluation Windows ...................... Add Traces ............................................................................ Temperature profile Icon .............................................2..................................... 70 16....4.........6........2...16. 77 16......... Recommended Equipment ........................1..... Hide and Restore Trace Names .............1.. 73 16......................1.....................................................3..................................................................................................................................................6.............................6......................................... Select Trace Display .......................................... Function Groups ...................................... Hide and Restore Traces ...................3......................... 97 16. 97 16................................................................. 76 16...................6...................................... Creation of a Collection File ............................................... 89 16.................................................................................................. Change of Active Evaluation Windows ...................... Summery of Functions ..............................8....................... 74 16................... 102 ........7.......................... 77 16...........................................3.......................................................2.......................... 81 16................................................6. 73 16..................................... 69 16...... Save Evaluation............................................................ 97 16......................................................................3.................................... Select Actual Trace ...1...........2.............. Created Data ....................................... 100 16.................................2........... Tool box .3.................6............................................................13................ 82 16.... 99 16............................. DSC and HDSC calibration file ....................................... Explanation of Tools ..................3....... 71 16......

.......... Graphite Crucibles .................... 132 24..................... 104 17........... TG evaluation flowchart ................................................................... LINSEIS STANDARD REFERENCE MATERIAL ........ 103 17.....2........... CHEMICAL BEHAVIOR OF CRUCIBLES ...................... SAPPHIRE SPECIFIC HEAT CAPACITY LITERATURE VALUES...............................................................8............ 115 18............ 108 18......................................................................1....... 102 16................................................ 139 ...................................4..................... Aluminumoxid Crucibles ................ ENTHALPY OF MELTING FOR STANDARDS ................ Problems with Trace Display ............ 137 26.......... Limitation of Trace Section ...... 102 16....................................... DSC evaluation flowchart ...............8................................... 134 24......................................................................................................................... 131 24.................................................................................. (H)DSC Calibration with Heat-Capacity Standard ....... ERROR CODES ................................................................................1............................................................................ 135 25................................................................................... 116 18.............................................................. Important hint for HDSC measuring system .. Recommended Standard Evaluation ....................1....................... 114 18....... 132 24............... (H)DSC Calibration by Measurement of Phase Change Enthalpies ........... 136 25............... 102 17..................................................................... 136 25....... Measurement with sample (1600 °C) ..............................4...............................................................................................2............2...................................................8......................3............ Cp evaluation flowchart......................3..... 117 19.............................2............................. 16..................... DTA evaluation flowchart .....................................3........................1.................................... 118 20........ 119 21.......... HOW TO CREATE A DSC OR HDSC CALIBRATION FILE .......................................................... EVALUATION FLOWCHARTS ...................................................4...2..........................1............. 114 18.............................................................................. 102 16....................................... 138 27. THERMOGRAVIMETRIC ANALYSIS OF CALZIUMOXALATE ........................ QUICK START MANUAL FOR THERMOBALANCE PT 1600 ....................................................................... 129 23.......................8................................................ SOME THERMO ANALYTICAL STANDARDS .............................................................. APPENDIX ....... Information Field .................................................................................................. Measurement zero file (1600 °C) ................. 133 24............................................................ 127 22......... Platinum Crucibles .

43 D-95100SELB Telephone: (+49) 9287 880-0 Fax: (+49) 9287/70488 E-Mail info@linseis. A service contract for your thermal analyzer is available on request. All instrument features. Linseis Messgeraete GmbH welcomes any remarks. Please send any comments to the following address: LINSEIS Messgeräte GmbH Vielitzer Str.General Information 1. Electronic or mechanical distribution or duplication of this/these instructions requires written permission from LINSEIS MESSGERÄTE GmbH. LINSEIS Messgeräte GmbH will accept no liability for damage following-on improper use.de Internet http://www. suggestions or new ideas regarding the instrument and these operating instructions.com Any type of maintenance or service of the instrument must be carried out by LINSEIS trained customer service personnel.linseis. we try to take individual solutions into account and to include these in the documentation. Nevertheless. 1 . This instrument instruction manual is designed to allow proper operation of the instrument by the customer. technical data and other information described in these system operating instructions are provided to the best of our knowledge and in agreement with the technical standards at the time of creation of this document. the instrument manual/description has to be limited to common or standard model. the keep the range of the instrument documentation at a level which can be handled. GENERAL INFORMATION In the design of your Linseis instrument.

Instrument Design • Your Thermal Analyzer has been designed and manufactured with state-of-the-art expertise and is secure to operate. General Requirements • Manufacturer approved operation of the instrument includes training of personnel and compliance with manufacturer's requirements regarding installation. Instrument Operation Guideline • The operator must make sure that only trained personnel work on the instrument. operation and maintenance must be clearly defined and compliance must be ensured. The resulting responsibilities can be clearly resolved under the aspect of safety. trained and individually instructed personnel. Training of User Personnel • Your Linseis instrument may only be operated and maintained by authorized. The producer cannot be held accountable for any damage follow-on such unauthorized use of the instrument. BASIC SYSTEM SAFETY INFORMATION Allowed instrument operation • Any operation or misuse of the instrument other than explicitly certified requires written approval from LINSEIS. • Any type of operation of the instrument which reduces the safety of the instrument user and the operability of the analyzer should be avoided. commissioning. • The person using the analyzer is obligated to immediately report to the operator in charge any changes to the instrument which affect the safety of the system. Responsibility for Commissioning. 2 . • Any use exceeding the (expanded) authorized system operation is considered unauthorized. Unauthorized changes to the system • Unauthorized modifications and changes which affect the safety of the thermal analyzer are not permitted. Operation and Training • Responsibility for commissioning.Basic System Safety Information 2. operation and maintenance.

). 3 . • Instruments or parts sent in for maintenance or repair should. Only then should the instrument be started. Accident Prevention Regulations: Industry-specific • The relevant regulations and protective measures must be observed by the user when handling the required gases. • During Maintenance and inspection the instrument must be switched off and unplugged. Otherwise. the operator should arrange additional internal operating instructions which specify the actions and tasks required for additional safe operation. be free of dangerous or harmful substances (e. Consider possible reactions with the materials. toxic. Any industry specific regulations for the analyzer are always relevant. At operating temperatures above 50°C. to the extent possible. • Warning signs should be hung in the appropriate places in accordance with national and regional regulations. possible dangerous reactions with the materials used must be considered.Basic System Safety Information Instrument Maintenance Obligation • The thermal analyzer operator of must ensure that the instrument is operated in perfect condition at all times. Furthermore. protective gloves must be worn. etc. • The operating instructions should be easily accessible at the work place of the instrument. the type of contamination must be declared. a check should be made to ensure that all protective devices are in place and operate properly. radioactive. Use of the Operating Instructions • Using guidelines from the system Operation Manuals. Instruments or parts not explicitly stated to be “not dangerous to handle” will be decontaminated at the expense of the owner. Checks following Maintenance or Repair Work • After maintenance or repair work. Removals of Production Materials • Any type of waste occurring out of the use of the analyzer is to be disposed in accordance with local regulation. Using Gases • Obey the appropriate national or international rules and protective measures when using gases for a measurement.g.

Use a filter trap on the purge gas outlet when noxious fumes are likely to be generated. Opening vacuum valves quickly will damage the internal balance parts. PROTECTING THE OPERATOR The following safety precautions must be followed: 1. and protection tubes with care. 4. Do not use any mechanical force when working with the counter weights or measuring systems.PRECAUTIONS & REQUIREMENTS 3. measuring systems. It will cause thermal shock to the alumina components 4. The internal balance parts are very fragile. 2. thermocouples.2. PROTECTING THE INSTRUMENT The following precautions will help protect the instrument: 1. When operating in a vacuum.1. slowly vent the system back to atmosphere. 3. Do not remove instrument covers or attempt internal adjustments without unplugging the instrument. 4 . do not handle any items when the furnace is above room temperature. Plug all instruments into 3-prong receptacles to assure proper grounding 2. Do not disconnect power if the furnace is above 500oC. To prevent the possibility of burns. 3. PRECAUTIONS & REQUIREMENTS 3. Handle the furnace. 3.

0. Cooling water: flow rate minimum: approx. 5 .Required facilities for installation 4. STA and power supply NOTE: Receptacles can be substituted with approved replacements.5 l / min. 16 Amp for computer. approx. cooling water within 3m from outlet. 4 receptacle 230 V AC. 3. Bench for STA Bench for STA must be built in a stable way to insure no vibration and stable condition for measurements. for example Linseis model no. printer. L75/WCU. AC Voltage requirement: Qty. please notify Linseis of change. 25 kg 2. 25 kg b) Floor space: power supply unit. There should be no interference with heavy machineries and other type of vibrations. printer and balance Balance: 430 wide x 540 deep x 620 (mm) high Approx. REQUIRED FACILITIES FOR INSTALLATION 1. 4. Stand alone chillers are acceptable. 444 x 405 x 270 mm. Space requirement: (W x D x H) a) Bench space for computer. flexible hose with 6mm inner diameter supplied.

6 . GENERAL INFORMATION The STA PT1600 is a highly versatile research instrument for measuring the following thermo physical properties: • weight loss or weight gain of a sample as it is subjected to a controlled temperature environment (TG) Optional measurements include: • differential thermal analysis (DTA) • differential scanning calorimeter (DSC) • coupling with EGA (evolved gas analysis) (MS/FTIR) The balance hardware is based on a taut band balance mechanism. The magnetic coils are also used to electronically tare the system. This current is amplified and produces the TGA signal. Highly sensitive optical transducers detect the balance arm displacement. INSTRUMENT DESCRIPTION 5. The transducers regulate the current to the magnetic coils that compensate for the weight changes keeping the balance arm at a constant zero position.Instrument Description 5.1.

** Max. Segments: 16 programmable temperature segments program heating * Different furnaces ** Different measuring systems 7 .Instrument Description 5. whichever is greater Repeatability: + 0. Vacuum: 10-5 mbar Resolution: 0.5/0.1s Temp.2.1 to 100oC/min. Sample weight: (depends on model) Tare: electronic Max.5% full scale or 10µg. SPECIFICATIONS STA PT1600 balance and amplifier Temperature range: -150 to 1750oC* Heating rate: 0.1µg Accuracy: + 1% full scale or 10µg. whichever is greater PID control: One or two stage cascade controller Thermocouples: 6 different thermocouple types Resolution: 1/20K Resolution: 0.

MEASURING SYSTEMS TG Measuring DSC Measuring DTA Measuring DSC Cp Measuring System System System System STA PT1600 Simultaneous Thermal Analyzer 8 .3.Instrument Description 5.

C DSC E. B 9 . K. S. S. B.Cp E.1. K. Linseis STA and High temperature DSC Measuring Heads Type Available thermocouple types DTA E.3.Instrument Description 5. S. B DSC . K.

Instrument Description 5. Not practical below 400°C.3. Type / temperature range / atmospheres Type Temperature range Atmospheres Type B (Pt18%/Pt-Rh) RT to 1750°C oxidizing reducing (reduces sensor lifetime) inert vacuum (reduces sensor lifetime) Type C (W/W-Rh) RT to 2320°C Vacuum Inert Not for oxidizing atmospheres. Type E (Chromel / -150 to 700°C oxidizing to 500°C Konstantan) reducing (reduces sensor lifetime) inert vacuum (reduces sensor lifetime) Type K (Chromel / Alumel) RT to 800°C oxidizing to 700°C reducing (reduces sensor lifetime) inert vacuum (reduces sensor lifetime) Type S (Pt10%/Pt-Rh) RT to 1650°C oxidizing reducing (reduces sensor lifetime) inert vacuum (reduces sensor lifetime) 10 .2.

Depending on the configuration and the required measurement speed. FURNACES The Linseis STA PT1600 can use a large selection of different exchangeable furnaces listed below. accuracy and type.Instrument Description 5. Air Air Air Air Atmosphere Vacuum Temperature Type K Type K/S Type S Type S Type B Measurement Tubular Heating Element Element Kanthal SiC SiC MoSi2 11 . Type of Furnace L75/264 L75/220 L75/230 L75/240 L75/PT Temperature range -150°C – RT – RT – 1000°C RT – 1400°C RT – 1600°C (RT = Room 600°C 1750°C Temperature) Cooling medium LN2 Furnace cooling Air Air Air Water Furnace Inert.4. the following furnaces can be mounted onto the system. Gas.

Instrument Description 5.5. FRONT IMAGE OF INSTRUMENT Optional open ended protection tube for evolved gas analysis Furnace optional turntable for second furnace Front display Balance lift Power ON/OFF Gas flow 12 .

REAR IMAGE OF INSTRUMENT Connector for sample gas Purge gas Gas out Vacuum connector Connector for thyristor power supply Power supply for furnace (150V) USB connector water „in“ water „out“ Connection for cooling water Connector for automatic gas box or KREG for low temperature furnace (Option) 13 .6.Instrument Description 5.

large energizing resistance loads. the computer and other additional Linseis devices if it is possible and permitted.2. If this is impossible make sure that the neutral conductor and the ground conductor is potential-free! Connect up the control signals first. The Instrument STA PT1600 has to be connected to the PC via the USB cable. SET UP EQUIPMENT PLACEMENT The room where the instrument is placed should be free of vibration sources. The plug for the USB is indicated on the rear of the instrument. Place the cabinet on a stable floor out of the high traffic areas. large motors. INSTALLATION 6. ELECTRICAL WIRING To prevent the system or the user from damage and for action safety and error free operating is a low-impedance ground connection essential. the Thyristor power supply. then the furnace power supply and finally connect the whole system the mains. The room floor should be stable and not flex when individuals walk around or towards the thermobalance. and purge gas outlets. cooling water. 14 . Place the thermobalance on a sturdy vibration-free floor with close access to power.Installation 6. The area should be free of drafts and extreme changes in the room air temperatures. 6.1. Use only one power outlet (or a power board) for the instrument. or capacitor discharges.

exe” located on the CD. 15 . Normally Windows will automatically detect and install the driver. Confirm that the automatic search shall be performed. WINDOWS will tell you that it has found a new hardware device. (The exact Model will be indicated). Installation procedure: 1. 3. INSTALLING THE TA-WIN & WIN-STA SOFTWARE For USB connection !!!! Before connecting Thermo analytical Devices with your PC. In case this does not happen. make sure that the Software installation has been completed!!!! To perform a correct software installation. 4. you can now start to perform measurements with your Thermal Analyzer. 5. Place the CD-Rom with the Linseis TAWIN software in the CD-drive. you should now find the LINSEIS TAWIN software ICONS on your desktop. Follow the instructions displayed on your monitor. Normally the installation will now start automatically. 2. do not leave out any point. select the driver manually. start the file “setup. 6. Windows will now ask how the search for the appropriate driver shall be performed: „automatically or manually“. The appropriate driver location is as follows: C:\tawin\driver After successfully completing the installation. Now please switch on your Thermal Analyzer and connect it with the computer via the USB cable provided from LINSEIS.3. In the event that Windows does not automatically find the correct driver.Installation 6. The displayed message will indicate that the found device is a Thermal Analyzer. follow the points outlined in the appropriate order. After successfully installing the appropriate software for your ordered thermo analytical device.

Open the balance chamber (unlock the screws and remove the cover) Screws 16 . Shut off instrument and computer. 2. Remove heat shields (if installed). 4.1. Screws 5.4.4.Installation 6. 3. INSTALLATION AND CHANGE OF THE MEASURING SYSTEM 6. Raise furnace with furnace lift to the upper position. Open the device on the left side through loosening the 3 screws. Preparation 1.

Adjust with the knurled screw and additional counterweights on the left side of the balance beam the balance.4. which has to fit into the flat side of the receptacle.Installation 6. so that the balance beam touches just the lower end stop. 4. do not remove the screw). tighten the fixing screw. Assemble measuring system 1. 3. Place Al2O3 crucibles on the measuring system. When the measuring system locked in place properly. 17 . 2.2. Meanwhile hold the measuring system from the outside. Please note that the plug of the measuring system has a flat side. Disassemble measuring system 1. Loosen the fixing screw (only loosen. Now insert new measuring system from above into the balance housing.3. 3. 2. Remove the measuring system upwards and put it in the container.4. Measurement system Groove End stop Fixing screw Balance beam 6. snap in the groove below the measuring system and lever it out. Take a small screwdriver.

the balance beam is not correct tared. Alternatively the balance can be tared with the knurled screw and counterweights in the balance chamber. Tare Balance 1.Installation 6. 3. Switch on the instrument.4. touch the funnel or sample holder slightly. If balance movement stops promtly. Rough tuning: When device is switched off put weights into the funnel. Fine tuning: Put weights into or take weights from the funnel in order that the weight display on the front of the device shows a value between -80 and -90 mg.4. 2. in order that the balance beam floats free. To check free movability . 18 . 5. 4. but do not start the measurement software. Remount the cover of the balance housing and tighten the 6 screws and next remount the left cover with 3 screws. Open screw cap beside the furnace lift. then balance movement slowly die away.

5. For other crucibles or heavier probes you must repeat the tare procedure. Correction measurement 1. 19 . 150 mg. Do a correction measurement up to the maximum allowed temperature of measuring system. etc. 2. Note: According to this tutorial the balance is tared for Al2O3 crucibles and a probe weight (probe material and reference material) about max.Installation 6. Start the PC and launch the respective measuring program (Type S.4.). Type K.

20 . Remove the platinum cylinder. 2. Remove the thermal shield stack.Installation Manual for change of thermal shield of a cryogenic furnace 1.

21 . Insert the heat shield plates and rotate those with a pair of tweezers (or something like that) so that the hole becomes minimal. 4.Installation 3. Fit the flange and fix it with a clamp.

Installation 5. Insert the shared insulation material and ensure it with the metal ring (beveled edge upside). Make sure that there is no contact between insulation and measuring system. 6. 22 . Mount the O-ring (metal nose downside) on flange.

8. 23 . Measurement system will be destroyed. Please check while lowering. that there isn’t contact between insulation and furnace. Make sure that the cryogenic furnace is into the correct position. Insert sample and reference crucible and put the platinum ring on the head of measuring system. Then cover the measuring system with the ceramic lid. Bring furnace carefully to lower position.Installation 7.

Furnace maintanace 7. Furnace weight amounts roughly 7 kg. first raise the furnace lift in the upper position and disconnect the instrument and the Thyristor power supply from the mains. Furnace control line Furnace power supply Picture 1: Electrical connections Cooling water out Cooling water in Fixing screws Picture 2: Water connections (view from below) Precautions: When releasing the water cooling connectors from the flask the remaining water may spoil over the system. 24 . Then four connections have to be released as shown in the pictures below. DISMOUNT FURNACE For dismounting furnace. Finally loosen the three fixing screws and heave the furnace carefully upwards away.1. FURNACE MAINTANACE 7.

Carefully lift the cover straight up and set aside. Insulation Electrical connections 25 .2. which securing the top furnace cover. 2. Switch off the power. REPLACING THE FURNACE HEATING ELEMENTS 7. Loosen the electrical connections. Carefully remove the heat insulation parts from the heating element and next to the power connections. Remove the 4 Philips countersunk screws. 3.Furnace maintanace 7. Countersunk screws 4. 1. Disconnect the power cable from instrument and power supply.2. 1400°C and 1600 °C furnace Attention: Reparation should only executed by skilled personnel.1.

Furnace maintanace

5. Remove the heating element straight up.

6. Check if the new SiC heating element tallies already with the demounted one,
especially the length and the shape of the power connection tapes. If necessary
adapt them with a side cutter. Attention: For shorten the power connection tapes,
demount the tapes and cut the end without ferule. Do not cut off the ferule. Finally
check the direction of the fixing screws.

Original heating element

New heating element
Fixing screws

26

Furnace maintanace

7. Insert the new heating element completely and control if it fits. Next tighten the
nuts for the power connection tapes. Take sure, that there is no electrical short and
no contact between voltage carrying parts and body. Also wires mustn’t touch the
heating element. Insert the insulation between body and electrical connections and
the insulation plug in the middle of the heating element.

8. Fit the cover and secure it with the 4 countersunk screws.

27

Furnace maintanace

7.2.2. 1750°C furnace

Hint:

The following example is for the LINSEIS L81/250M MoSi2 furnace. Its temperature range
reaches from RT up to 1750°C. Considering the furnaces in our program, there are
maybe slight differences, hence please contact our service hotline for detailed
instructions.

Basic precautions:

1. Switch off the power.
2. Disconnect the power cable from instrument and power supply.
3. Reparation should only executed by skilled personnel.

General Instructions:

Remove the 4 black Philips head screws securing the top furnace cover.
Carefully lift the cover straight up and set aside.

Example for: L81/250M furnace and heating element

MoSi2 heating element

Connection terminal

28

2.Furnace maintanace 1. 4. Disconnect the power connectors. 7. Place the new heating into the furnace. Connect the furnace power connectors. 29 . Reconnect the power connectors. Remove the new heating elements from its package. 8. 3. Close the furnace. Disconnect the heating element power connectors. 6. Carefully pull out the heating elements. 5.

3. CHANGE FURNACE THERMOCOUPLE Attention: Reparation should only executed by skilled personnel. Disconnect the old thermocouple. 30 .3. Disconnect instrument and power supply from mains. 2. Remove the broken thermocouple and insert the new one.Furnace maintanace 7. Open the furnace and remove the heating element. 1. 4.

and look for troubleshooting. Reset the CJR adjustment. Cool down the system. there must a mistake. Normally the plus wire is marked with a black mark. that there is no contact between wires and hot parts. In this case promptly stop heating. If the temperature doesn’t rise. 31 . Regard the polarity of the thermocouple. Start heating with a slow heating rate and check if the temperature rise. and check if there is shown the real temperature. and is connected with the black wire.Furnace maintanace 5. Remount the heating element. Connect the thermocouple on the terminal block. Very important: After reparation you must check the shown temperature in the measurement program. Look to it. 6.

Calibration Kit's Calibration kit's for enthalpy/temperature calibration can be ordered from LINSEIS Messgeräte GmbH: 1. A new calibration is required any time the instrument is repaired and when there are significant changes in the measurement conditions.g. repairs and considerable changes in the test parameters (e. One distinguishes between temperature and enthalpy calibration. changing the sample holder). DSC/DTA calibration kit (temperature and enthalpy) Calibration of the Balance We recommend that the balance be recalibrated following transport. Information regarding the specific effects of the individual test parameters on the results of STA measurements can be found in the special literature The following parameters should be considered when preparing the measurement: • calibration • sample preparation • sample weight • reference material • sample chamber temperature • temperature program • atmosphere What do you Assemble the required materials before starting the need for the measurement? measurement: • purge gases (sample chamber and balance) • sealing tool for pressure-tight crucibles • tweezers Calibration Calibration of the instrument is a prerequisite for quantitative analysis of STA measurements.Preparing a measurement 8. the test measurement parameters have a significant influence on the results. DSC/DTA calibration kit (temperature and enthalpy) 2. 32 . PREPARING A MEASUREMENT Preparing the In thermo analytical investigations.

Direct application of the sample material increases the danger of contaminating the sensor! Films Discs are punched from films with a hollow drill or punch pliers. the lid should be placed on the crucible. scalpel or razor blade. with the convex side down. The significance of the experimental results can be increased in all cases by adding a drop of silicone oil (improves the heat transfer). the bottom of the crucible is covered with thin slices of the material. Good thermal contact between the sample and heat-flux sensor is an indispensable requirement for optimum results. For the analysis. (The weight of the sample can be increased with voluminous fiber materials. A bundle of fibers is wrapped with aluminum foil and cut at both ends. which are then spread parallel on the bottom of the crucible. e. A sample crucible must always be used.Preparing a measurement Preparing the sample When preparing the sample. are cut into thin slices with a knife. The methods most frequently used for preparation of solid and liquid samples are described below.) The fiber material with the foil wrapping is then placed in the crucible. If it is not possible to punch out a suitably sized disc. Fibers The fiber can be cut into small pieces. the effects to be interpreted and the consistency of the sample must be considered. The coiled fiber is then removed from the rod and placed in the crucible. Compact solids Compact solids.g. The fiber is wound around a small rod. In order to improve the contact between the sample and crucible bottom. Powdered solids The sample is evenly distributed in the bottom of the sample crucible. and sealed. rubber or thermoplastic. a hollow drill is used to punch out a sample disc of a suitable size from this larger disc (taken from the center of the whole sample). 33 . The discs should completely cover the bottom of the crucible.

Measurements in defined For measurements in defined atmospheres. evaporation of water of crystallization.Preparing a measurement Liquids Depending on the viscosity. a needle atmospheres should be used to pierce one to five holes in the lid of the crucible. Evaporation reactions When investigating evaporation reactions. e. Select the sample crucible Select the crucible depending on: • sample carrier system • sample material • purge gas atmosphere 34 .g. liquid samples can be dropped into the crucible with a thin glass rod. a micro-pipette or a syringe. The measuring unit must be recalibrated when pressure-tight crucibles are used. The hole should be punched prior to sealing to avoid deformation of the crucible later. a closed crucible with a small hole in the center of the lid should be used. Unstable samples Unstable samples are tested in special pressure-tight crucibles (optional).

• Take care that the lids do not stick to the crucible rim. • When filling the crucible. bottom and lid to improve the radiation behavior. no sample material may remain on the edge of the crucible. • Loosen the crucibles carefully (also on reference side) after every single run. • Place PtRh-crucibles with the crucible rim (facing downwards) on to the sensor plate before first heating. use Al2O3 crucibles.Preparing a measurement Selection and preparation of • Do not touch the crucibles by hand. This indicates that PtRh-crucibles should not be used.1 mg or better • Clean the crucible and lid with acetone or alcohol prior to use. • Cover the crucibles with a thin layer of platinum paint on the outer surface of wall. In this way the crucibles do not stick to the sensor plate. clean it with distilled water. Accuracy: 0. • Traces of reaction will be visible on the surface of the foil. • After treating the crucible with acids or solvents. • Heat up a small amount of sample on a piece of Pt-foil in a separate laboratory furnace. • Heat up the crucible to final working temperature to burn out the solvents before using the crucibles on DSC. Weigh the sample Weigh the sample with an analytical balance. • Check if a reaction between the crucible material and the sample will take place at the desired temperatures before measuring an unknown sample in a PtRh-crucible. • Dry the crucible and heat it up again to final working temperature. • PtRh-crucibles also tend to stick to the sensor plate of the sample holder when heated above 1000°C. • Lift up the crucibles and replace them. Use platinum crucibles tweezers! • Always heat up the crucible to the final working temperature before the first measurement. • If samples cannot be measured in PtRh- crucibles. • This treatment will have a positive effect on the Cp-data compared to those measured in Al2O3-crucibles. especially in the temperature range above 900°C. 35 .

tantalum W.Compatibility of crucible materials and some substances 9. m crucible material Ag. tungsten No solvability. Ga. molten mass dissolves the crucible material Crucible will melt Change of melting temperature may be ignored (partial solution process) Compatibility unknown Combination isn’t possible 36 . lead Zn. Corrosion of the crucible material may go to destruction of sample carrier and sensor. platinum silicate glass SiO2. fused silica Ta. no variation on the melting temperature Change of melting temperature. nickel Pt. Al. molybdenum Ni. gold aluminu Pb. iron fine steel Mo. silver Au. oxidized Al2O3. bornitride C. corundum Au. COMPATIBILITY OF CRUCIBLE MATERIALS AND SOME SUBSTANCES Measuring in metal crucibles requires special care. silver Al. tin water xH2O H2O. graphite Fe. aluminum Al. substances Ag. In. zinc gallium Li2SO4 indium C5H10 Sn. gold BN.

This has effects on the function of the weighing system. and dry) should continuously purge through the weighing system into the sample space. In the most positive case “only” air humidity deposits on the surface of the weighing system. Prior to starting the measurement the measuring system can be repeatedly evacuated and refilled with purge gas. How to create a particularly clean gas atmosphere: Use a vacuum pump (a diaphragm pump is sufficient) for evacuation. inert.Selection of the gas Atmosphere 10. The weighing system . resolution in the µg range and an excellent stability are standing out features of the STA PT1600 that are due above all to its highly sensitive weighing system. The protective gas (pure.the heart of the STA PT1600 . this deposit impairs the stability behavior of the STA PT1600. 37 . Measurements under static conditions In case of static measurements there is no protection of the weighing system by a continuous inert gas flow. SELECTION OF THE GAS ATMOSPHERE The STA PT1600 allows measurements under the following conditions: • Dynamic gas flow • Static gas atmosphere • Vacuum Our recommendation: Linseis recommends running the STA PT1600 in dynamic protective gas atmosphere. Dynamic protective gas atmosphere High precision.must be open towards the sample space.

Please really check: Are aggressive or condensable reaction products released? Attention! Under vacuum conditions these products are sucked off via the weighing system! A damage of the weighting is preprogrammed. if the sample does not release aggressive or condensable reaction products. This can lead to a damage of the weighing system: 1. Measurements in static gas atmosphere are only admitted. In this way you minimize the penetration of air humidity into the STA PT1600. being not lighter than air. Gas flow (vacuum) inside the STA PT1600 Measurements under vacuum . dynamic). The operator of the instrument is personally responsible that samples releasing aggressive. a) When changing the samples or during a measurement pause keep open the system only as long as really necessary.what should be considered! In case of measurements under vacuum a protection of the weighing system by an inert gas is not possible. inert. The weighing system must be protected for all operation modes (static. reactive or condensable reaction products are not measured under static conditions. 2. If nevertheless you want to do static measurements: Take care that the weighing system is protected by an inert gas. reactive or condensable reaction products are not measured under vacuum conditions. Measurements with closed outlet valve lead to a pressure increase inside the system. The measuring results are falsified (drift). Use a protective gas for the weighing system (dry. The operator of the instrument is personally responsible (for example by suitable pretests) that samples releasing aggressive. b) Fill the whole system with protective gas before longer measurement stops and leave it in this waiting position with closed valves up to the next measurement. pure). Therefore static gas operation should be an exceptional case. 38 . if aggressive gases reach the weighing system.Selection of the gas Atmosphere Higher problems arise.

sample holder. but sample reactions are possible. thermocouple). The following is a selection of purge gases including their limiting properties. Carbon monoxide (CO) Toxic (MAK-Wert 10 vpm).value 5000 vpm). Flammable. Application is possible above room temperature (maximum application temperature is determined by furnace material. GASES AND THEIR LIMITATIONS Under no circumstances may explosive gas mixtures be used! Information concerning the possibility of using various gases can be found in the appropriate technical literature or can be requested from the manufacturer or retailer of gases. corrosive The use is not allowed for safety reasons. Air Oxidizing No technical safety limitations. but sample reactions are possible. Flammable Corrosive The use is not allowed for safety reasons. The list makes no claim on being complete. The use is not allowed for safety reasons. Application is possible above room temperature (maximum application temperature is determined by furnace material. Oxygen (O2) Increases flammability (must not come into contact with fats or oils) No technical safety limitations. Carbon dioxide (CO2) Non-toxic (MAK. thermocouple). Ammonia (NH3) Toxic (MAK value 50 vpm). Flammable Danger of explosion when in contact with oxygen. but sample reactions are possible in the high temperature range. Hydrogen (H2) Flammable. Danger of explosion when in contact with oxygen The use is not allowed for safety reasons.Gases and their limitations 11. sample holder. 39 . Gas Properties Helium (He) Chemically inert (inert gas) No technical safety limitations Argon (Ar) Chemically inert (inert gas) Asphyxiating No technical safety limitations Nitrogen (N2) Largely inert Asphyxiating No technical safety limitations. Hydrogen sulphide Toxic (H2S) (MAK value 10 vpm). Corrosion of seals is possible. Non-flammable Application is possible above room temperature.

Very caustic. corrosive The use is not allowed for safety reasons. Hydrogen fluoride Very toxic (HF) (MAK value 3 vpm). Encourages burning. Fluor (F2) Very toxic (MAK value 0. Non-flammable. Sulphur dioxide Toxic (SO2) (MAK value 2 vpm). Non-flammable. corrosive. Non-flammable. Gas Properties Chlor (Cl2) Very toxic (MAK value 5 vpm).Gases and their limitations Other reducing gases or gas mixtures For safety reasons it is not possible to use these gases as contact with oxygen or air could result in an explosive compound. MAK values 1994 MAK-value (Maximum workspace concentration) We recommend that the expelled purge gas be passed into a suitable exhaust hood. The manufacturers of gases and gas mixtures can provide the required information. certain gas compounds with inert gases are possible where the mixture ratio excludes all technical safety doubts while complying with the required analytical conditions. The measuring part must be sufficiently purged with inert gas once the measurement is finished.1 vpm). corrosive The use is not allowed for safety reasons. corrosive. Gaseous Can form explosive gas mixtures with air hydrocarbon The use is not allowed for safety reasons. caustic The use is not allowed for safety reasons. caustic The use is not allowed for safety reasons. corrosive. However. 40 . Hydrogen chloride Toxic (HCl) (MAK value 5 vpm). caustic The use is not allowed for safety reasons.

could cause a continuously change of the gas concentration around the sample. If the reaction is reversible. no gas flow produces uneven temperature gradients in the system and poor temperature repeatability. should be used with extreme caution. Beside from concentration considerations. Reaction gas. as all gases. 5-10 psi) to prevent gas from rushing into the system. when switching from vacuum to gas flow. GAS FLOW IN THERMOGRAVIMETRIC EXPERIMENTS The control of gas flow in thermogravimetric experiments is essential for protecting the balance from corrosive gas conditions and to the success and repeatability of the experiments. the concentration of the evolved products will increase. if no reaction within the sample is the objective. if the system remains inert without gas flow. should be at low inlet pressure (approx. but no slower than 1 l/h and no faster than 10 l/h. such as hydrogen or oxygen. This rush will produce instability and could possibly blow sample out of the crucible. Precise rotameter control is recommended in this case. Reaction gas can be an inert gas. As the rate of decomposition increases. the reaction rate could decrease. in that weight changes are recorded against precisely controlled heating rates that produce a continuously changing temperature. All corrosive gases should be used with extreme care. This particularly occurs.7 l/h. such as nitrogen or argon. Thermogravimetry is in most cases a dynamic process. the concentration of the ambient static atmosphere around the sample will change. If the system is sealed to avoid back diffusion. 41 . Results would not be reproducible. Convection currents in the balance. Explosive gases. Since the sample evolves a gaseous product as the temperature increases. Reaction gases should flow at 5 . pressure build up will cause buoyancy changes and disturb the weight readings. Air is a safe substitute for oxygen. Generally a blend of a low percentage of hydrogen in an inert gas is a relatively safe procedure. Back diffusion of air will occur.GAS FLOW IN THERMOGRAVIMETRIC EXPERIMENTS 12.

select "Data Acquisition- Type . For a zero line measurement.1. select “Data Acquisition . For a zero line measurement.1. DTA measurement or one with both DTA/TG.Sample DTA (or HDSC)” for a sample measurement. The present type of measurement is displayed in the title of the program window. To start a zero line measurement.Type . The difference lies in the measuring head. you can choose between a DTA or a HDSC measurement. TYPE OF MEASUREMENT Before starting an STA measurement the type of measurement must be defined.Type .Zero Line TG”.Zero Line TG+DTA”. 13.Sample TG” for a sample measurement. To start a DTA/HDSC measurement. 42 . DTA/HDSC Measurement Depending on how your system is equipped. LINSEIS STA MEASUREMENT SOFTWARE 13.Type . 13. You must also decide if you want to measure a sample or a zero line. TG+DTA/HDSC Measurement To start a TG and a DTA/HDSC measurement simultaneously. select “Data Acquisition . It can be either a TG measurement.1. select “Data Acquisition .Type .Type .Linseis STA Measurement Software 13.2. 13.Zero Line DTA (or HDSC)”. select “Data Acquisition .1.Sample" to DTA” for a sample measurement. select “Data Acquisition .3. TG Measurement To start a TG measurement.1.

a dialog window will be displayed.” from the menu bar. 13. SETUP DATA ACQUISITION After selecting “Data Acquisition . Example DTA Measurement 43 .2.. Example TG Measurement 13.2.2.Linseis STA Measurement Software 13. The following pictures show examples of the various dialog windows for different types of measurements. Here you can enter all important parameters for the acquisition and the storage of the measured data. The appearance of the window depends on the type of measurement and might be slightly different.1.Settings.2..

even when they are not shown in all the dialog windows at the same time. 44 .Linseis STA Measurement Software 13. Comment: This field is for a short comment about the measurement. User: This field is for the name of the person. It is displayed together with the name of the gas in the comment field of the data evaluation program. Atmosphere: This field is for the gas atmosphere that is being used in the measurement.3. The name of the laboratory is also displayed in the comment field of the data evaluation program. The name of the gas is also displayed in the comment field of the data evaluation program. Example TG – DTA Measurement 13. The name of the user is also displayed in the comment field of the data evaluation program. It is also displayed in the comment field of the data evaluation program. Laboratory: This field is for the name of the laboratory doing the measurement.4.2. who is doing the measurement. Description of the Input Parameter Following is a list and description of all the parameters. Flow Rate: This field is for the flow rate of the gas.2.

This entry is very important. Duration: This field is for the duration of the data acquisition of the measurement. In a zero line measurement this field is deactivated. Reference Weight: This field is for the weight of the reference material used in the OTA measurement.Linseis STA Measurement Software Sample File: This input is for the name of the sample tile where measured data is stored. Sample: This input field is for a short description of the sample. No filename can be entered. The shut off is independent from the duration of the controller program (see also Duration). in DTA/HDSC measurements the extension is ". the shorter the time intervals and the higher the accuracy. especially in measurements with fast changing signals. that these two durations are not mixed up. The program will. In a sample measurement this entry can be used for later information during a data evaluation. The sample files for TO measurements always have the file extension “. For DTA-HDSC measurements the file extension is ". 45 .3). The smaller this value is. The acquisition will be slopped after one of the parameters has reached the entered value. the end temperature creates the ‘switch off conditions’ for the data acquisition. 10. It is important. The sample weight is also displayed in the comment field of the data evaluation program.TPR". This entry defines the name of the file where measured data is stored in a zero Fine measurement. Together with the end temperature. data files that need a longer time for the evaluation and more space on the hard disc.TPR". In case the sample weight contains a fraction. The zero files in TG measurements always have the file extension ". the faster sampling causes large. Reference: This field is for the reference material in a DTA measurement.g. Sample Weight: This input field is for the weight of the sample used in the measurement. This ending is automatically added when missing. This time constant controls the time that data will be stored onto the hard disc.GNL".: This field is for the temperature that ends the acquisition. It is also displayed in the comment field of the data evaluation program. This description is also displayed in the comment field of the data evaluation program. because all the initial data will be tabulated and stored with it. Zero File: This field is for the name of the zero file used in the measurement. The acquisition will stop after one of the parameters has reached the entered value (see also End Temp. it has to be entered with decimal point (e. the duration creates the ‘switch off conditions for the data acquisition. This duration is independent from the duration of the controller program. This weight is also displayed in the comment field of the data evaluation program. but on the other hand. End Temp. Sampling Interval: This value sets the time intervals in which data is measured and stored. Together with the duration. Range: The range must be chosen from a list of values that depend on the type of measurement and instrument.).GPR". It is also possible to choose an existent file through the use the symbol on the right side of this box. In other words: Entering a wrong value for the range causes all measured data to be stored and displayed incorrectly. automatically add the file extensions when they are missing.

Controller Set Values 13. Program the Controller Set Values With the programming of the controller set values a temperature profile is defined for the measurement. It is important that the temperature readings are the temperature of the sample and not the furnace.3. 13. With this feature it is defined when & which gas shall be used • Number of cycles Defines how often the program shall be repeated 46 . For every cycle four parameters must be programmed: • Segment: The Software offers up to 16 separate temperature segments • Rate (K/min) Defines the heating/cooling rate per segment • Target Temp. Up to 16 different cycles can be programmed. PROGRAM CONTROLLER The programming of the controller sets the temperature stages of a measurement. Each will be processed one after the other. as well as the regulator behavior are defined here.2. The pre-heat and cool-down periods of a measurement.3. (°C) Defines the target temperature per segment • Dwell Time (h)/(min) Defines how long the temperature should remain at the end temperature • P-max (%) Defines how much power the thyristor should use as % • Relay Option when using a gas control box.1.Linseis STA Measurement Software 13.3.

4. From this selection you can choose and activate the desired profile.3. It is useful to use a different temperature than the actual sample temperature when creating a new temperature profile.3. The starting temperature must be entered manually. A special feature is the choice of the starting temperature. Store Controller Set Values If a temperature profile should be needed at a later time for other measurements. Load Controller Set Values To load a temperature profile the field “Load” must be selected. with stored profiles listed.Linseis STA Measurement Software 13.3. Delete Controller Set Values If incorrect controller set values we entered in the dialog window. the whole input field may be deleted by selecting “Delete” on the screen. 47 . it can be stored by selecting “Store" on the screen and entering a name. the programmed temperature profile of a measurement as a function over time.3.3.6. Another dialog window will appear on screen. It can be either the actual sample temperature or any other temperature. because the system may still be warm after the last measurement and must be cooled down-first after the system is cooled-down a new temperature profile can be displayed and evaluated. 13. 13. Graphic Display This feature displays on screen.5. 13. This gives’ an exceptional optical control and the temperature profile can be changed if necessary.

Display Current Values It may be interesting during a measurement to get a view of the current temperature and control parameter of the system. . .Linseis STA Measurement Software 13.. . Relay conditions Sample Parameters: Power Output: . Maximum Temp..Thermocouple Type 48 . .7. Heating Rate . Segment number . This is possible by choosing the menu selection “Controller . Cycle number . Remaining Time . .” The following parameters will be displayed: Temperature Profile: Oven Parameters: .3.Current Values. Dwell Time . Target Temp. . Current Temp. .Reference Temp.State (on/off) . Thermocouple Type .Target Temp. Target Temp.Current Temp.

The accuracy of the adjustment cap is increased by repeating this step a few times. then the adjustment can be reset by using the field "Reset" and then started again. The thermocouple must be inserted into a known temperature (e. An adjustment dialog window can be displayed on the screen with “Controller ..Linseis STA Measurement Software 13. The Parameters of the uncontrolled preheating are displayed as follows: • Target Temp.8. Adjustment of the sample thermocouple can be done with the cold junction reference. the adjustment is made.9. even if the program is turned off.3. Once the calibration of the sample thermocouple is made the correction value will be stored. Uncontrolled Preheating The function of uncontrolled preheating is used. and the user can now enter the nominal sample temperature. Adjust Cold Junction Reference The controller board uses a built in reference cold junction to compensate for thermal voltages in the input connectors. the actual temperature of the thermocouple is displayed. CC in ice water).” Here. which is necessary for the control.. 49 .g.g.3. 0°C).g. with a radiation pyrometer from 400°C). (in CC) • Max. The normal controller program would fail in this case because the temperature. If by accident the thermocouple has been adjusted to an incorrect temperature.Adjust CJR. and used for future measurements. when a sample temperature can only be measured after a certain starting temperature (e. By using the field “Adjust”. the uncontrolled preheating is stopped and the normal controller program 13. Power Output (in %) • Ascent (in %/min) After the target temperature is reached. which was assumed to be measured (e. is below the starting temperature and cannot be determined.

4.10. Parameter Definition The PID-parameters have to be entered as separate P-.3.3. The defaults can be entered through selecting the field “Reset”.10. 13. The defaults are made according to known values of Linseis GmbH.3. The controller works as a cascade controller. Load Parameters To load an already stored set of parameters for a measurement the field “Load” must be selected in the window for the selling of the P ID-parameters. It will process the sample as well as the furnace temperature as controlling parameters.Linseis STA Measurement Software 13.3.2. 13. I. they can be stored after selecting “Store” and recalled for later measurements.10. Set Defaults Sometimes it can happen that unfavorable parameters were set for the controller and the proper parameters are lost.3.3. In this case.10.fractions for controller 1 (sample temperature) as well as controller 2 (furnace temperature).10. 13. The value range for each parameter can be between 0 and 32767.1. Store Parameters If various sets of parameters should be available for different measurements.and D. then the current value used for the control loop is only the furnace temperature. PID-Parameters The PID-Parameters directly change the controlling behavior of the electronic temperature controller and have to be selected carefully. 50 . If the controller should be used in single stage mode instead of a cascade mode1 then all the parameter fractions of controller one have to be set to zero. we recommend choosing the defaults and changing the parameters from there until the desired parameters are selected. 13.

Below the graphic display the measured parameters are shown as digital values. The graphic display is equipped with an automatic re-scaling function. In particular the data acquisition and the controller program can be started while a measurement is in progress. This procedure can repeat itself in a measurement. at the start.4. START AND STOP MEASUREMENT To start and stop a measurement there are two fields marked “Start” and “Stop” in the main menu. or the menu selection “Options . Active data acquisition DTA/HDSC 13. the lower side of the screen displays the following important information about the measurement: . Active controller program . a new range will be calculated and displayed on screen which includes the new data. The y-axis is set at the start to 10% of the selected range.Linseis STA Measurement Software 13. This means. that after one of the measured values (or of the passed by time) leaves the selected range.5. After selecting one of these options a dialog window appears on the screen showing the user his choices. Duration of the measurement . 51 . This means that the whole measurement is visible on screen. The graphic display of the measured data remains on the screen after a measurement until a new measurement is started. The graphic display of the measured values always starts with the beginning of the measurement. Number of stored data . According to the selected type of measurement a system of coordinates will be built on the screen that displays the time for the x-axis and the measured parameters for the y-axis.Clear Graphic” is chosen to erase the display. REAL-TIME GRAPHIC The real-time graphic displays the data during a measurement. The time axis always has. a scale from 0-10 mm. Active data acquisition TG .

For the adjustment.6. 13.6.Linseis STA Measurement Software 13. or if it should be shifted asymmetrical.6.6. the adjustment screw for the zero point must be turned (with the sample in place) until the needle in the right gauge is exactly in the middle. The right gauge displays the offset from the selected zero point. the position must be entered in % of the actual range. the zero point can be adjusted either manually or automatically. Depending on the instrument. Manual Adjustment The manual adjustment is always used when the instrument has no automatic zero adjustment. Zero Point Definition To define a zero point in an instrument range. After the position of the zero point is defined (see last section). If asymmetrical. 13. A dialog window will appear on the screen. The left gauge shows the total actual range from -100%to +100%. two gauges are displayed on a dialog window and are used for the adjustment. The advantage of a asymmetric zero point shift results in a wider range on one side. it can be shifted to get a asymmetric measurement.2. BALANCE SETUP 13. The zero point does not have to be in the middle of the physical range. The user can decide if the zero point must be in the middle of the range. To exit the zero point adjustment select "Close” in the dialog window. This requires knowledge of the expansion behavior of the sample to avoid an over-range situation during the measurement.1.Setup Scales”. Zero Adjustment To adjust the zero point of the thermal balance select the menu “Options .3. the field “Zero Point’ must be activated. 52 . and the digital display on both gauges show exactly the %-value of the zero point position.

g. .6. Automatic Adjustment After the position the zero point is defined (see section zero point definition).. In the section called [RELAYS] it is possible to define under the relay numbers 1-4 the names of the relay outputs.4. the field appears again and the dialog window can be left by selecting “Close” on the screen.7. To do this a few entries have to be made into the file “DIL. into “Gas Inlet”. These outputs may control valves for gas or cooling water supply. For instance: [RELAYS] 1=Relay&1 2=Relay&2 3=&Gas Inlet 4=Relay&4 53 . The condition of these outputs can be defined either in the controller set values for every cycle number (separate for every cycle) or. Then the field disappears and a remark that the zero point of the system is now adjusting is displayed. the automatic adjustment will be started when selecting the field "Automatic Zero Adjustment”. The active condition is displayed with a little mark in front of the relay number. After the adjustment is finished.Linseis STA Measurement Software 13. 13.Relays4.. These names can be changed to get a more accurate statement.INI” of the measurement program. e. The character following the &-character is used as a fast-choice with the keyboard. The menu points for the outputs are named by default Relays1. RELAYS The controller in the Instrument is equipped with relay outputs.

• Clean the crucible or replace it if the old sample can not be cleaned from the crucible. If it is contaminated replace with new Al2O3. Note: Sample is right. • The normal amount is 1/3 full (max. Switch the balance to “ON” 2.PERFORMING A ZERO BASELINE CURVE 14. reference is left. Please do not miss out any points in order to gain a satisfying result and to avoid damage to the system. • Inspect the Al2O3 reference material. • Place equal amounts of Al2O3 in the reference and sample crucibles. PERFORMING A ZERO BASELINE CURVE In order to perform a zero baseline curve please follow the outlined instructions carefully. 150 mg for sample and reference). Lift the furnace automatically by pressing the lift button located on the front of the instrument. Carefully remove the sample crucible. 1. Lift button 3. 54 .

PERFORMING A ZERO BASELINE CURVE 4. “SETTINGS…” 55 .“DATA ACQUISITION” . “TYPE”. Start the software STA data collection software using the desktop icon Desk top data collection icon 5. Now select in the Software . Now select in the Software . “ZERO LINE TG+DTA” 6.“DATA ACQUISITION” .

Click “OK” to complete settings.PERFORMING A ZERO BASELINE CURVE 7. Enter the data collection information: The data collection termination is control by the Duration and End Temp. will result in the data collection being terminated. 56 . Always select a time or temperature higher than the final data point needed. value. Whichever value reaches the “stop” criteria first.

Now select in the Software . Precaution: Do not exceed the heating rate of your selected furnace to prevent damage of the heating element! 57 . “TEMPERATURE PROFILE…” 9. Enter the desired heating rate to the maximum temperature.PERFORMING A ZERO BASELINE CURVE 8.“CONTROLLER” .

PERFORMING A ZERO BASELINE CURVE 10. Precaution: The temperature must be a room temperature before starting the system. “CURRENT VALUES” 11. 58 . Furnace Sample temp. Now select in the Software .“CONTROLLER” . Check the current furnace and sample temperature.

13.PERFORMING A ZERO BASELINE CURVE 12.“OPTIONS” . “BASELINE CORRECTION” . “SETUP SCALES”. Now select in the Software . “SELECT CORRECTION” 59 . Now select in the Software . Click to “TARA ADJUSTMENT” to calibrate the Tara 14.“OPTIONS” .

Start the measurement by selecting “Start” • Check data collection and controller.“BASELINE CORRECTION” .“NEW CORRECTION” • Enter an expressive description and choose a zero line file. • Choose “OPTIONS” . 19.PERFORMING A ZERO BASELINE CURVE 15. Monitor the run using the real time graphic and current values windows. Once the run is completed monitor the current values and do not lift the furnace and protection tube until the temperature is less than 100oC. Create a new baseline correction characteristic • Check if the zero baseline is repeatable for the used measuring system. • Click “OK” to start the measurement 17. 18. 60 . Check if “ACTUAL CORRECTION” is NONE 16.

2. Switch the balance to “ON”. • Clean the crucible or replace it if the old sample can not be cleaned from the crucible. • Weigh the reference and the sample before. reference is left. 150 mg for sample and reference). • Place Al2O3 in the reference and your sample in the sample crucibles. 61 . Lift button 3.PERFORMING A SAMPLE CURVE 15. PERFORMING A SAMPLE CURVE 1. Lift the furnace automatically by pressing the lift button located on the front of the instrument. Carefully remove the sample crucible. • Close the plug-in on the furnace top. Note: Sample is right. • The normal amount is 1/3 full (max. If it is contaminated replace with new Al2O3. • Inspect the Al2O3 reference material.

“OPTIONS” . Now select in the Software .PERFORMING A SAMPLE CURVE 4. “ZERO LINE TG+DTA” 6. 5. “TYPE” . Start the STA measurement software using the desktop icon. “BASELINE CORRECTION” . “DATA ACQUISITION” . “SELECT CORRECTION” 62 . Select in the Software .

8. “SETTINGS…” 63 . “DATA ACQUISITION” .PERFORMING A SAMPLE CURVE 7. Select in the Software . Select for the mounted measuring system the correct baseline correction.

Always select a time or temperature higher than the final data point needed.PERFORMING A SAMPLE CURVE 9. Click “OK” to complete settings.GPR extension will be automatically inserted. Atmosphere. The data acquisition termination is determined by the Duration “OR” End Temp. • Sample and Reference name. • Laboratory. Enter the sample weight. • Comments TG Sample File names: *. • Flow Rate. Whichever value first reaches the “stop” criteria will result in the data collection being terminated. Enter the data collection information Text fields: • Operator. 64 .TPR extension will be automatically inserted. value. DTA Sample File name: *.

“TEMPERATURE PROFILE…” 11. Enter the desired heating rate to the maximum temperature.PERFORMING A SAMPLE CURVE 10. 65 . “CONTROLLER” . Select in the Software .

“CURRENT VALUES” 13. 66 . Furnace Temperatur Sample e temp. Select in the Software .PERFORMING A SAMPLE CURVE 12. “CONTROLLER” . Precaution: The temperature must be at room temperature before starting the system. Check the current furnace and sample temperature.

“SETUP SCALES” 15. Select in the Software . Monitor the run using the real time graphic and current values windows. 67 . “OPTIONS” . Check data collection and controller. Start the measurement by selecting “Start”. Click “OK” to start the measurement. Click to TARA ADJUSTMENT to calibrate the Tara. 16. 17.PERFORMING A SAMPLE CURVE 14. Once the run is completed monitor the current values and do not lift the furnace and protection tube until the temperature is less than 100oC.

The complete software consists of 3 modules: temperature control. LINSEIS STA EVALUATION SOFTWARE Software All LINSEIS thermo analytical instruments are PC controlled. execution. and evaluation of a Thermogravimetric measurement.)  Zoom function  1 and 2 derivation  Programmable gas control  Statistical evaluation package  Free scaling TG – Features: • Mass change as % and mg • Rate Controlled Mass Loss • Evaluation of mass loss • Residue mass evaluation HDSC – Features: • Glass transition temperature • Curve subtraction • Complex peak evaluation • Multipoint calibration for sample temperature • Multipoint calibration for enthalpy • Enthalpy measurement • Specific heat measurement • Signal-steered measuring procedures Optional: • Cp measurement • Cp calibration for heat flow 68 . Thanks to our specialists and application experts. TMA. Features -Software:  Program capable of text editing  Data security in case of power failure  Thermocouple break protection  Repetition measurements with minimum parameter input  Evaluation of current measurement  Curve comparison up to 32 curves  Storage and export of evaluations  Export and import of data ASCII  Multi-methods analysis (DSC TG. data acquisition and data evaluation. LINSEIS was able to develop comprehensive easy to understand user friendly application software. etc. The individual software modules exclusively run under Microsoft® Windows® operating systems. DIL.Linseis STA Evaluation Software 16. The 32 bit software incorporates all essential features for measurement preparation.

1.2. 69 . The operation of the evaluation program is described in detail in the manual ”Display and Evaluation of Measured Data”. 16. It also includes a convert function of older data formats of the STA DOS version.1.1. INTRODUCTION The present Program module "Thermal Gravimetric Evaluation" is part of the program package "Thermal Analysis”. Recommended Equipment ⇒ Windows supported printer or plotter or both. for table and trace printout. 16. ⇒ It is also required. STA PT1000 and STA PT1600 which are controlled trough the Microsoft Windows version of the STA measurement program.1.1. For efficient operation. It is designed specifically for the evaluation of TG values with the Linseis thermal balances: L81/I. Evaluation of Measurements The ability of displaying the results of one or more measurements that are connected is called evaluation. If you are new to the Windows system. ⇒ The above listed hardware + software requirements are the minimum. that the user becomes familiar with all the functions of the TG evaluation program. please refer to the manuals. L81/II. Minimum Hardware + Software Requirements ⇒ State of the art PC ⇒ VGA screen ⇒ Mouse ⇒ MS-Windows operating system ⇒ MS-Windows XP etc. called “evaluation”. All traces and additional information is going to be displayed in an evaluation window. 16.3.Linseis STA Evaluation Software 16. we recommend: State of the art Windows PC 30 GB hard disk (or higher) with capability to backup data from the hard disk 256 MB RAM Appropriate screen Mouse ⇒ It is essential for the user to be familiar with the operation of the MS-Windows system to make the application of the TG evaluation program as simple as possible.

• For the name of the file only eight characters are allowed. Added to the name comes a file extension for configuration files (standardized .Linseis STA Evaluation Software 16. where the measured data can be displayed as a trace.CFG). To start a new evaluation. START NEW EVALUATION For every data evaluation an evaluation window has to be used. you have to choose “FILE” - “NEW” The File New dialog box is now displayed and the user is being asked to name this evaluation. 70 .2. The default is NONAME. This name is used to characterize the evaluation and should be used with an ending that characterizes the file.

Various Evaluations Simultaneously It is possible to work in different windows on more than one evaluation at the same time. etc. and repeat to load it. Hint: The menu bars as well as the status bar are displayed only once.2. 3. All the actions and information relate to the actual window. legends.2. as far as the matching data files were not deleted or overwritten. You can enter a new directory. In case the evaluation program can not find the data file. Save Evaluation To save an existing evaluation you have to choose “FILE” . After that a dialog box will appear. you can open it with the command “FILE” .Linseis STA Evaluation Software 16. 2.“SAVE AS.”. The windows. which will open up. can be changed in their size and can be arranged freely. but has been copied. To do so you have to load more evaluations. Open Existing Evaluation Once an evaluation is saved. or create new ones. will be restored. 71 . unnamed evaluation you have to choose “FILE” . To save a new. which was entered as a data source for a trace definition. In case the referring file does not exist anymore. 16. You can stop the evaluation. and the program saves the evaluation with its current name.1.. And the traces. if you think something is wrong. in case the file still exists.“OPEN”.‘SAVE”. you have the following choices: 1.2. 16. and the user is asked to name the evaluation.2. The program will go on to load the evaluation without the missing trace. The measured curve will then be created in the new sub directory.3. you can ignore the last mentioned hint..

2.Linseis STA Evaluation Software 16. The last mentioned is useful. when the requested window can not be selected because it is hidden by other windows. (Command “ARRANGE ICONS”).2. Then the windows can be arranged next to each other (command “TILE”) or on top of each other (command “CASCADE”). 16.4. 72 . In addition windows can be rearranged when they are displayed as icons. Arrange Evaluation Windows The evaluation windows can be arranged automatically by MS-Windows. or through selecting the evaluation name in the menu “FILE”. Change of Active Evaluation Windows The change of the actual evaluation window can either be done through selecting the requested window with the mouse.5. To arrange the windows you have to select “WINDOW’: on the menu bar.

” you can set the defaults for the parameters. You can change the actual trace by selecting the arrow on the right side of the name. which files have to be imported and which files can be loaded directly..3. asking the user how the program should proceed with the file.. Add Traces To add another trace to an evaluation you have to select “FILE” . to be able to use more files with extensions of the same type later on. because they were created through certain types of measurements or instruments. where you can select the requested one with the mouse. then it will be restored on the screen. Defaults for Traces In the menu select “TRACE”.2. In case the type of the file does not fit the format. This makes it possible to pre-select certain ways of scaling or displaying.1. If a file is selected whose type fits the binary data format of the evaluation program it is immediately used in the evaluation. which should be used as standard settings when loading a new trace.3. Hint: All the files with measured values have always exact defined extensions. where the endings and the meanings of the individual files are explained in detail. Another entry you can make now is to save the (until now unknown) file extension. “DEFAULTS. That opens up a box with a list of all available traces. You have now to select. They will be displayed on top of each other and in different colors. Besides the standard boxes of the windows-file selection system a combination field exists.3. if the file should be loaded directly. 16. then it has to be “imported” (which means it has to be transformed).3. Hint: When you select a trace that is hidden in the moment. where the type of the files can be entered which are displayed in the file box. When a file was selected where the program does not recognize the ending. The program recognizes automatically by the file ending which import filter needs to be used. a dialog box appears on the screen.. which are needed for the co-ordinate axes. To get more information about this subject. TRACES IN THE EVALUATION In a single evaluation window you can load various traces. This trace name creates a trace reference to the applied labels and the axis display. A file option menu will appear on the screen.3. Select Actual Trace In the tool bar (bar below the menu bar) on the left side you find a box for the actual displayed trace. or if it needs to be imported and with which filter.Linseis STA Evaluation Software 16.“LOAD DATA.”. 16. please refer to the additional chapters about the specific types of measurement or instruments.. Depending on the type of source file it is possible to enter various parameters during the import. 73 . 16. This way they do not have to be adjusted for every new trace.

.“DELETE. etc.. Hint: Deleting the trace and the stored parameters (labeling. where all the parameters for the trace display can be seen. 16.6. a trace name is created in the color of the trace.“HIDE. only the trace with its matching axis and labeling is drawn or is not drawn.3..“GLOBAL TRACE PARAMETER” . Hint: In case you want to delete the whole trace name..” one or more traces can be deleted.“CHANGE. line type ..“CHANGE.3.” .) will result in a complete loss of the trace.3. color. and is displayed together with the trace on the screen.” a dialog box appears.” and ‘TRACE” . etc.“TRACE VISIBLE”. 16. To do so. you have to select in the menu bar “OPTIONS” . Hereby nothing will be deleted.Linseis STA Evaluation Software 16. In case a lot of traces are displayed at the same time. The condition between visible/invisible is changed every time you select “TRACE NAME”. The present condition can also be changed by selecting “TRACE” .. lines.. if you really want to delete or only hide the trace (make it invisible). 74 . which is displayed in the evaluation.5. please go to section 6..4. To avoid this. a little check mark appears on the left side of “TRACE NAME”.“RESTORE.“TRACE NAME”. Hide and Restore Traces The menu selection “TRACE” . position.” are only valid for the present display of the traces. Ranges for X and Y: margins of the display . Global trace parameter: trace color. Select Trace Display After selecting “TRACE” .3. the amount of the labeling can be disturbing. You should decide. Delete Traces With “TRACE” .7.. 16. When the name is visible. Axis parameters: visible. (Change and Delete Single Labeling) and proceed as described.3. They include: . Hide and Restore Trace Names For every trace. it is possible to hide the trace names temporarily (they are not deleted!).

The selected Evaluation type is displayed in the line following the “Function Group” Icon.Linseis STA Evaluation Software 16.1. Icon Evaluation type Select this Icon when performing a single ADIDI Evaluation pushrod Dilatometer Evaluation Select this Icon when performing a Diff – Evaluation differential Dilatometer Evaluation Select this Icon when performing a Laser Laser – Dil – Evaluation Dilatometer Evaluation Select this Icon when performing a TMA TMA Evaluation Evaluation Select this Icon when performing a DTA DTA Evaluation Evaluation Select this Icon when performing a TG TG Evaluation Evaluation Select this Icon when performing a DSC DSC Evaluation Evaluation Select this Icon when performing a HDSC HDSC Evaluation (high temperature DSC) Evaluation These are special evaluation routines Corning/US-Customs etc. Since the program performs evaluations for all Linseis Thermal Analyzes. EVALUATION ICON 16. developed for customers.4. the type of instrument providing the measuring data has to be selected once. 75 . Function Groups This Icon defines the type of data that can be evaluated.4.

Temperature profile Icon This box provides information concerning the chosen temperature profile during the measurement.Linseis STA Evaluation Software 16. The example to the left shows: Heat up: 10K/min up to 1465°C Cool down: 30K/min down to 700°C 76 .2.4.

5. When the change in mass is moderately huh. Zero Correction A measurement without a sample creates a signal that will show only the expansion of the system itself (zero curve).1. 16. Different zero curves may be applied.3.Linseis STA Evaluation Software 16. The algorithm uses a spline function to calculate the derivation. The y axis smoothing is important to calculate the derivation. the zero curve can be neglected and no zero correction is applied. X Axis Smoothing The smoothing of the temperature signal (x axis smoothing) requires a steadily increasing or decreasing temperature signal. depending on the parameters. 16. Incorrect data will not be accented by the program in most steps of the evaluation.1.5.5. 16. 16. 77 .1.1.4. SUMMERY OF FUNCTIONS 16. Derivation It is possible to calculate a derivative of measured curves over time or over temperature (1st or 2nd derivation). In case the signal can not be corrected over temperature.1.2. Correction Procedure A successful evaluation of raw data requires a correction because of errors. Y Axis Smoothing The smoothing of the y axis is performed independent from the x axis smoothing.5. the zero curve must be subtracted from the sample curve (measurement with sample).1. it must be corrected over time.5. To avoid this error. The zero correction and the smoothing of the temperature signal will be described in the following two sections. which will occur during a measurement and resulting noise of the temperature signal.5.

The entry into the protocol includes the start and end temperature as well as the relative and absolute change in mass. M0 is the mass of the sample at room temperature. The ascent calculation is done with a two point differentiation which needs a smoothed trace.1.5. An optional function is the display of the abscissa.n) M k for every point k. In the graphic are the two tangents.1.8..9. 16. The entry into the protocol for this point includes the temperature and the relative and absolute change in mass over time. The two tangents must be before and after the reaction together with the turning tangent in the point of the largest ascent.5. Mk is the change of mass at the temperature tk.. A negative change in mass marks a weight loss.. Change in Mass The total change in mass for a marked section is calculated and entered into the graphic as a label.5. The entry into the protocol includes the temperature of the intersections as well as the relative and absolute mass difference between both points.5. the turning tangent as well as the coordinates of the intersection labeled (abscissa display optional)..5.1. so they can be used for a hard copy. Reaction Stage To mark a reaction stage. Relative Change in Mass The relative change in mass can be calculated with: ∆M k ∆Mrel (k) =  * 100 (where k=1. The ascent calculation is done with a two point differentiation which needs a smoothed trace. In case you want the results in a printout as a tabulated format. Mass calculation The following described procedures are interactive functional for every trace section.Linseis STA Evaluation Software 16. a calculation of the intersections of two tangents on the trace is needed. Reaction Maximum The reaction maximum (the point of the fastest change in mass of the sample in 1mg/mm]) for a marked section is calculated and entered into the graphic as a label.1.1. An optional calculation is the abscissa difference.5. The user enters the position of a tangent through two points.7. 16. 16.6. The tangents are calculated through linear regression and they are extrapolated with the intersections of the turning tangent. 78 . The results are entered as labels into the graphic. The number of calibrations per curve is practically infinite. 16. The unit is given in 1%. the program offers a protocol option.

2. Mean Curve To get information about the reproducibility of measured values a function exists to calculate the mean for a number of traces (traces with the same unit for X and Y axis). The following equations are given: The factor z is the so called standardization of the t diffusion. ⇒ One trace operations constant offset constant factor reflect through X axis ⇒ Two and more traces operations addition subtraction multiplication division 16. includes information about the confidence interval as well as values for its calculation. Important: Zero curves can only be connected with each other and not with sample or edited traces. For the sample range of n>30 is the difference between the Student and the Gauss diffusion negligible (where n<30). Arithmetic Operation Several different operations can be applied to correct data files. Usually only a few traces are in use. the zero curve must be smoothed first. The file. so that a diffusion function (Student or t diffusion) for correction must be applied.Linseis STA Evaluation Software 16. A special situation is the mean of a zero curve. Then the resulting mean curve can be converted back into a zero curve. created when calculating the mean curve. All traces must have identical units for X and Y axis. With the Student or t diffusion a clearly wider confidential interval can be calculated (when compared to the Gauss or the normal diffusion). A confidence interval is also calculated for the mean curve (means for every single data point). Because of the existing noise. 16.5. which is done automatically with the calculation of the mean.1.5. For further editing of a mean curve. The arithmetic operation of traces as well as the mean curve.2. the curve must be converted into an editing file.5.9% statistical confidence).2.2. This factor is listed for a variety of error possibilities (in this program package for 95%. 99% and 99. Curve Arithmetic The following section describes two ways to work with traces. 79 .

A collection file can be extended by adding new traces. the program will ask you if you want to overwrite or add the trace. 80 . The collection file exists as a binary data file. In case a trace is added. as long as they are from the same evaluation. It can be convened with the ASCII export filter into an easy readable form. For this reason it is appropriate to collect these files in a collection file. The loading of a collection file happens automatically through a specific import filter. In case you add a new trace with a name that already exists.5. longer than the first. it will be cut. This file holds. It creates new files considering empty entries. All traces must be from one evaluation and will be synchronized over the X axis grid of the first selected trace. the V columns for various traces. besides the columns of time and temperature. Creation of a Collection File Every step of an evaluation needs its own data file (see section ”Data Structures”).3. In the opposite case. non existing points will be marked as empty entries.Linseis STA Evaluation Software 16.

Both lines must have been marked before. This function field selects the tool used to edit lines. moved. With the left mouse button pressed the desired zoom area is selected. rotated or deleted. 81 . 7. 6. since some of the operations can't be performed if it is hidden. it can be marked. Display or hide X-axis scaling (selecting a trace with tool “1” will allow to hide or display the corresponding axis) 12. First the desired data point is clicked. Display or hide the tool box The tool box can be displayed or hidden by selecting "Options" "Toolbar" from menu. it can be moved. 8. edited or deleted. This function field selects the tool used to Edit text or value labels. This function field is used to determine the pint of intersection. After pressing the right mouse button the zoom is performed.6. 3. The position of the text label is defined by clicking to the desired position in the graphic window. Tool box 1 2 3 4 5 6 7 8 9 10 11 12 13 1. 9.6. 5. In the combo box the Trace name is displayed in the trace color. This function field selects the tool for magnification (Zoom). The line will be assigned to the actual trace. This function field selects the tool used to draw lines. All subsequent added text labels are always related to the actual trace. This function field is used to display and to select the actual trace. Display or hide Y-axis scaling 13. This function field turns off all previous zoom actions and restores all traces to their original appearance. This function filed selects the tool used for generation of Text labels.1.Linseis STA Evaluation Software 16. and to add the related value label. Usually the tool box should be set visible. then the desired position in the graphic window. 11. 4. 10. Both end points must be specified with a click. After clicking to one of the end points of a line. PROGRAM DESCRIPTION 16. 2. This tool displays the XY values while scrolling over the actual trace. This function field undoes the last zoom and the previous screen is displayed. All subsequent added value labels are always related to the actual trace. This function field selects the tool used for generation of Value labels. After clicking to a text or value label.

6. For that reason. outlined with a broken line. To get from any zoom # back to the whole trace (zoom 0). Display without Magnification In a lot of situations is it not only needed. the screen has a much smaller resolution (in most cases 1000 points). Normally the resolution of the whole trace good is enough to show. This magnification does not calculate (because of a time reasons) any new points in between. Compared to that. To open up the window. When this tool is used in the graph.000) not all the points are displayed on the screen. Explanation of Tools Zoom The internal resolution of a displayed trace is stored with approximately 20. a display can be magnified in size to a certain degree (up to about 100 times). you have to create another window by selecting a new corner and using your mouse. With every new magnification. even after the magnification. all the data points. select the crossed magnification glass icon in the tool bar. In this case a new image can be created through the choice of the section (“TRACE” - “CHANGE” . 82 . Pressing the right mouse button quickly will display the selected section on the screen. After releasing the left mouse button the window stays on the screen. to display and label the traces on the screen. You can get this tool by selecting the magnifying glass icon in the tool bar. which gives you a variety of functions for processing data files. The old window will then be overwritten by the program. press and hold down the left mouse button and move to the opposite corner. which is underneath the menu bar. and so on. Undo Last Magnification Magnifications can be selected as often as needed.000 points. To get a specific section. Magnify New Section (Zoom) To get a magnification of a certain section of the trace you need the “Zoom-Tool”.Linseis STA Evaluation Software 16. the cursor switches into the shape of a magnifying glass. the first zoom #1. so that in a file with a high amount of data points (more than 20. but to edit and evaluate them through specific. This icon in the tool bar makes it possible for you to get step by step back to previous magnifications.“RANGE MARGINS”). until certain resolution limits are reached. which can be changed in size and shape. the second zoom #2. To get the previous magnification. To magnify this section even more. This “Zoom Stage” is displayed as a number on the right side of the status bar. The whole trace has the 0. you have to choose the magnification glass icon with the mark “-1”in it. you first pick one corner of the desired section.000 data points.2. you can open up a window using your mouse. the old one will be stored in the so called “Zoom Stage”. numeric procedures. On the menu bar you will see the selection “EVALUATE”. The requested window is hereby displayed as a box. which now also has a resolution of 20.

3. Therefore it is recommended to turn on the function right after opening the evaluation window to get a complete protocol. where it belongs to. The protocol file has always the same name as the evaluation window. The file has always the default ending ‘. Hint: In some function directories the protocol file can start to store parameters as soon as data are available. In some applications a protocol is saved for the records or for documentation. In the first line of the edit menu appears the statement “FUNCTION GROUP”~. The name of the function appears in the second line of the menu. They are described in the documentation. you have to select “PRINT” – “PROTOCOL”. which are available separate from the source program. which comes with every additional directory.“PROTOCOL” can be selected. where the desired function group can be selected and activated. 83 . if the actual function directory is enabled to protocol evaluation steps. in which the protocol tile is printed. which can be printed out or can be stored.TXT”.Linseis STA Evaluation Software 16. The individual functions can then be selected in the following lines. depends on the actual function directory. This condition is changed every time you select “PROTOCOL”. Turn Protocol On/Off In the menu selection “OPTIONS” . The protocol file is stored in the ASCII-format and can be viewed and printed out with a regular editor. The form.6. Evaluation Protocol In some function directories certain evaluation results are held in a protocol file. Print Protocol To print out the protocol. Evaluate Traces These function groups’ suit additional directories. This way the function volume of the evaluation program can fit the needs of the user.

and the position for the legend can be selected. the labeling can be horizontal as well as vertical. In case you did not hit the trace exactly with the marker. Change and Delete individual Labels To change. which appears on top of the dialog box. you can move the label. “CHANGE” and “DELETE”. with the difference that the actual parameters are set (name. After entering “OK”. The position of the legend can be defined screen oriented.6. which means it is set with trace co-ordinates. like the one when entering a new label. The first option is to move the label. which means independent from the magnification. Now you can move the pointer to the desired text position and press the left button. as well as trace related.) The last option is to delete the label completely. it is possible to set labels within an evaluation. The form of the cursor changes now into the shape of the general labeling. move or delete a label. which gives you the choices between “MOVE”. which should be labeled. After releasing the mouse button. The legend is always related to the actual trace. use the icon named “ABC”. you need the tool to change the legend. you have to move the mouse cursor to the text on the screen and hit the left button and hold it down. it can be in the color of your choice and can also have several lines. is marked with a cross. Now the mouse cursor will appear in form of a little cross. Now you have to scroll. Labeling of a Data Point A special legend type exists for marking certain points on the trace. General Labeling To get a general labeling of a trace. the text will be displayed in the evaluation window. The second option is to change the label. To do this. After that a dialog box appears on the screen. After selecting it with your mouse. a dialog box is displayed on the screen where you have to confirm the action. etc. Another click of the left mouse button ends the move. After that a dialog box appears where the legend can be entered as well as information about the position. until the desired action is selected.4. It can only be related to a trace. Selecting this option will bring up a dialog box. which you use to select a point on the trace and confirm this by clicking the left mouse button. 84 . The point on the trace.Linseis STA Evaluation Software 16. you have to select the icon marked “XY” in the tool bar. You can get it by selecting the icon with the shaded area in the tool bar. which is displayed in the box below the menu bar. and an additional line. After “DELETE” is clicked on. you will get a mouse cursor in form of a 90-degree angle. These labels are always related to a trace. Legend In addition to the display of the traces. direction and color. color. To change the label. The following dialog to enter the text differs (because of the option to enter co-ordinate values) from the general labeling. the closest data point will be calculated and marked. Besides that.

a little check mark appears on the left side of “LABELS”. so that you can only see the trace on the screen. please refer to chapter 3.”. To delete a complete group of labels. Hint: The labels. All the labels from other traces will stay unchanged. you have to select in the menu bar “OPTIONS” . The condition between visible/invisible is changed every time you select “LABELS”. 85 .“DELETE LABELS. it makes them only invisible.7. a dialog box appears on the screen. To do so. with a list of all the groups. To hide and restore the trace names. you need to select “TRACE” .. Hiding the labels does not delete them.. which is displayed in the tool bar. which have to be deleted.Linseis STA Evaluation Software Delete Groups of Labels If you want to delete a whole group of labels at one time. you might want to make all the labels invisible. can only be from the actual trace. You can now select one or more groups you want to delete. Hide and Restore all Labels In an evaluation with lots of labels on a curve.“LABELS”. When the label is visible. rather than every label individually.

To calculate an intersection. which you selected. it is possible to draw lines within an evaluation. The other end of the line stays in place.Linseis STA Evaluation Software 16. you have to select “MOVE” in the dialog box. for line intersections). Calculate Line Intersection The icon in the tool bar with the two crossed lines. Then you have to go with the cursor to one of the ends of the line. they are linked to co-ordinates of the trace display. They are displayed always inverted to the background. MARK: With the command “MARK”. and select the icon in the tool bar. you need the “Line-Tool”.g. Lines Similar to labeling a trace. hit the left mouse button and hold it down. MOVE: To move a line parallel. 86 . you have to select one end of the line. you have to mark two lines which are related to the same trace. you first pick the starting point of the line and click the left mouse button. Change Lines To change lines. by selecting the line icon in the tool bar. The marking of a line is displayed as little quadrants on both ends of the line. and release the button. which is held in one spot. the intersection will be labeled with a data point and the line marks will disappear automatically. The line can now be rotated with the point. has to be selected. A dialog box appears on the screen. which offers the selection between “MARK”. which means. DELETE: With the option “DELETE” it is possible to delete a whole line. a line. and hit the left mouse button and hold it down. To draw a line. After that. ROTATE: To rotate a line. Now you can move your cursor in the window. “MOVE” and “DELETE”. and you see the line like a rubber band. Draw Lines To draw a line. which needs to be edited (e. The length of the line remains the same. which you would like to change. Go down to “ROTATE”.5.6. You can get this tool. is used to calculate an intersection. “ROTATE”. Hitting the left mouse button again will hold the line in the actual position. you need to pick the line icon with the arrows. These lines are always related to the trace.

Every time you select visible. After that a new window can be created. you need to select “OPTIONS” . For the text in the info field. To hide or restore the info field. Hide and Restore Info Field To be able to display the traces on the full screen. there is a maximum of six lines..“DELETE” the whole window will be deleted.”. Delete Info Field With “OPTIONS” . it makes it only invisible on the screen. It is displayed in a separate window below the trace.“INFO FIELD...” - “VISIBLE”. Info Field The info field is a text window. without loading already existent data. if a text is loaded from a file.”. Hint: You can enter a text into the info field. The (until now) existing text will be lost entirely.Linseis STA Evaluation Software 16. they can be loaded as a text file using the commands “OF’T’IONS” . you have the choice of hiding the info field.“LOAD. Hint: Hiding the info field does not delete it.” ..“INFO FIELD. you can change and edit the window with “EDIT. Load and Edit Info Field If a data file has additional information about a measurement..“INFO FIELD.6. The information for the info field will be taken from the same file as the actual trace. 87 . After that.. the actual text into the field will be overwritten.. However... which is capable of storing additional information about a measurement or evaluation.6.” .. the condition between visible and invisible changes.

change the settings of the printer.“PROTOCOL” the protocol file can be printed out in a tabulated format on the active printer. With “PRINT” . For the printout. or printed inaccurately.2.“PRINTER SETUP” enables to check and. Printer Setup The commands “PRINT” . Screen Dump “PRINT” . To use the better resolution of the printer or plotter. so make sure that enough space is left on the hard disk. where all the installed printers and selected interfaces are listed.6. we recommend to select the option “COLOR” to increase the quality of the printout. With “OPTIONS” . with the difference of the ending . When the graphic is stored temporarily in the print manager. the actual contents of the info field and the results of the previous peak evaluations.TXT. it is possible to continue to work with the program.“GRAPHIC” starts the screen dump on a printer or a plotter. even when the printer is still printing. you do not have to leave the evaluation program. An incorrect input to the paper size can cause that parts of the print out are missing. Print Evaluation Protocol For an evaluation where the protocol mode was turned on. 88 . Print The results of an evaluation can be printed on every Windows compatible printer or plotter. This includes the controller parameters of a DSC file.“SELECT PRINTER” you get into a dialog box. Printer and Interface selection To select a printer that is already installed under Windows. These settings can be changed temporarily as well as stored permanently in the Windows standard settings. The dialog window is different for every printer and can not be described in detail. The print speed of the graphic depends mostly on the used resolution and the color option. It can be edited with a standard text editor. This procedure and the use of the print manager need a little time. a new picture will be built up internal.7. The created file has the same name as the evaluation. The protocol can be turned on or off with “OPTIONS” -“PROTOCOL” (see chapter 5.Linseis STA Evaluation Software 16. instead of just using the screen copy. When using a color printer. if necessary. a text file is created which stores information about the evaluation results.). a large temporary file is installed.

89 .g. The delta mode is active as long as the left mouse button is pressed down.INI.Linseis STA Evaluation Software 16. where the program looks for certain files. Hereby. The condition between on and off is switched every time you select the button. is defined in the file TA. Word for Windows or Paintbrush. It will have the same resolution as the evaluation. One is marked “X”. which is then used as an editor. e. By moving the cursor. which was displayed on the screen.“DOS SHELL” you can start an application which makes that possible.“EDITOR” activates an editor. you will see the X and Y deviation from the zero position displayed. because some functions would be lost without it. For advanced users the command processor of MS-DOS could also be used as a pure DOS application. The picture can then be transferred into other Window programs. Copy Evaluation to Clipboard With “FILE” .INI. etc. Miscellaneous Co-ordinate Display In the status bar two buttons are displayed. In the menu selection “OPTIONS” .“TOOL BAR” can be determined. The evaluation program uses standardized the DOS-Surface of Windows 2. copy. delete. DOS-Shell Sometimes it is required to use certain DOS-commands (e. The File Manager for Windows 3. Respectively next to their right side. in TA. This is usually the Windows note pad. However.8. Which editor is used.INI another application can be applied.1. This display can be turned on or off by pressing the according button. if the tool bar below the menu bar is visible or not. the co-ordinate values of the actual trace are displayed. all the menus and visible windows are included in the picture. File Definition In the menu “OPTIONS” . the name of the according application has to be entered into the file TA.0 can also be used. The tool bar should be turned on all the time. The editor is hereby started as an individual Windows application and has to be ended the same way.g. To get into a delta mode.“FILE” the file categories are defined.).“COPY TO CLIPBOARD” it is possible to copy a picture of the actual evaluation window to the Windows clipboard (temporary storage). the cursor has to be positioned and the left mouse button has to be pressed down and held down.6. In this case. the other “r”. The actual position is now stored as the zero position. Hint: To copy the entire screen to the Windows clipboard. Editor The menu selection “OPTIONS” . you can use the buttons “PRINT” or “ALT-PRINT”. Hide and Restore Tool Bar In the menu “OPTIONS” .

Linseis STA Evaluation Software 16. 90 . Select “ASCII-Export” Select the data file which shall be exported into ASCII format.9. How to perform an ASCII export a) Perform an ASCII export in TAWIN Open the requested file with the TAWIN Data Evaluation Software.6.

Linseis STA Evaluation Software The Data Export manager: Export options: “please select which information shall be exported” • File info • Channel info • Information field • Data Values Channels “please select which channels shall be exported. etc. 91 . for example: Time. Temperature. • Decimal Comma: for USA etc. Weight.” File name: displays the name of the file to be exported into ASCII format Export parameters: • Skip factor: indicates how many data points shall be exported • Decimal Point: for EU etc. Delta L.

ASC (ASCII) file has been stored. Now the import filter will appear on your screen. double-click the .Linseis STA Evaluation Software b) Import the . Select “all data types” in the data type pull down menu. The created ASCII file will appear.ASC file into EXCEL Please open Microsoft EXCEL and select the “open a new file” icon Now go the folder where the created . 92 .ASC file.

Now select next and proceed to step 2 of the import assistant. 93 . STEP 1 of the import assistant a) At first please click the data type b) Then select the appropriate data source “Western European”.Linseis STA Evaluation Software The EXCEL import assistance will appear on your screen.

Linseis STA Evaluation Software

STEP 2 of the import assistant

Please select empty space as the separator

The separators will appear on the preview screen.

Now select next and proceed to step 3 of the import assistant.

94

Linseis STA Evaluation Software

STEP 3 of the import assistant

Please complete the import procedure by selecting the “FINISH” button.

The imported data file should now appear in a EXCEL spreadsheet.

95

Linseis STA Evaluation Software

Successful data import:

Example

96

Linseis STA Evaluation Software

DATA STRUCTURES

16.6.10. Data Formats

All programs from the Linseis program package’ Thermal Analysis’ use a unified binary
format for the data files. This Format makes the storage of numerous values with several
measuring channels in a 4byte slide format possible. It also allows the storage of data
and channel specific information.
Data files of older program versions (for example ADIDI-DOS) as well as files from other
instrument systems need import filters to convert these files into the Linseis binary
format. This happens automatically when opening the respective file (as long as a
suitable filter is available).
Export filters for the most common foreign formats are available, in case you want to
continue to work with the measurement and evaluation results in other systems (for
example for graphic presentation). Among them are filters for ASCII or ANSI text format,
which are importable from almost every system.
In the evaluation program for MS-windows, the usual data exchange mechanisms is
implemented (see documentation of MS-windows respectively of the evaluation
program).

16.6.11. Name and Directory Conventions

The following name extensions are valid for the Linseis data files:
⇒ .GPR Sample file (measured signal)
⇒ .GNL Zero file (for zero correction)
⇒ .Gzz (with zz between 0 and 99) evaluation file
⇒ .GSM Collection file

All of these files have the three columns, time, temperature, and dM (or diverted signal),
except:
⇒ Collection file: besides time and temperature, as many signal and result columns
as wanted.
⇒ Mean file (variance of .Gzz): besides time and temperature, channels for
confidential interval, number of the measured curves involved in the information
and the error sum.

The (importable) data files of the STA-DOS version (ASCII-format) carry additional name
extensions:
⇒ .PTG Sample file (measured signal)
⇒ .NTG Zero file (zero signal)

ln the ANSI-format (for printing and editing) the following files exist:
⇒ .GRF Reference file (supporting file for statistic dependencies), with
columns of the independence degree and the standardization of the
distribution functions
⇒ .TXT Protocol file

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Linseis STA Evaluation Software

As convention structures are provided (e.g. \TA as main-directory):
\TA\*.* Program files
\TA\DATA\*.GPR Data files
*GNL
*Gzz
*GSM
*PTG
*NTG
\TA\REF\*.GRF Reference files
\TA\CONFIG\*.CFG Configuration files
*.TXT Protocol files

16.6.12. Created Data

Whenever working with a file, a new data file is created. This file has in addition to the
columns for time and temperature one or more columns for the data of this stage. This
allows the user to recreate the evaluation at a later time. With the exception of collective
and calibration files the name of the new file is created from the main directory of the file
and from the extension ‘.Gzz’
The number of the name extension (.Gzz) is increased by one with every new file (the
search for the next free file extension always starts at 0 and ends, as soon as a file with
its name does not exist).
This prompts the user, after a maximum of 100 processing steps, to clear his data files
and to store only real important results (appropriate is also to store a collection file).
Traces from evaluation files can be loaded with “if - Load data...” selecting the filter TG.

98

28502e-011 Description: In the section [TEMPCAL] the materials used for the temperature calibration are listed.00197059 a3=8.DCF) has the same structure like a standard WINDOWS profile (*.80.536475 SrCO3=929. In the section [TCORR] the related coefficients are stored.0000.-11.55966 a2=-0.10 s=1.-5.5.0000.07 BaCO3=806. Sample calibration-file: [TEMPCAL] K2SO4_1=584.Linseis STA Evaluation Software 16.13.0000. The corrected temperature is calculated according the following equation:      .-6.INI) file.0000.6.2. DSC and HDSC calibration file The calibration file (*.959226 K2SO4_2=1069.871171171 m=1.25.231469 [HCORR] a0=-405.05297e-007 s=1.10.990864 BaCO3=806.115 a1=1.0000.086936937 b=75.-5.12 [TCORR] a=-0.0.0000.38 [ENTHCAL] K2SO4_1=584.

The heat flow is calculated according the following equation:   ∆   .     s is the standard deviation for the coefficients calculated In the section [ENTHAL] the materials used for the enthalpy calibration are listed. In the section [HCORR] the related coefficients are stored.

   .

    .

99 .      H = Heatflow [mJ/s or mW]. T = Temperature [°C] s is the standard deviation for the coefficients calculated. ∆T = DSC/HDTA Signal [mK or µV].

. because they are described in the documentation for the evaluation program. All other menus are ignored. ⇒ Menu Evaluation ⇒ Menu Function Group TG-Evaluation ..(further evaluations. dependent/Time dependent/none) Range (Whole traces / Zoom window / Controller stage) Following actions (depending on dialog answer): Controller stage Smoothing behavior Temperature Control Select zero file ⇒ Y-smoothing Trace Selection Smoothing a trace Range (Whole trace / Zoom window / Controller stage) Smoothing behavior ⇒ Derivation Trace Selection Derivation of a curve Degree (1st derivation / 2nd derivation) Base (Temperature / Time) Range (Whole trace / Zoom window / Controller stage) Following actions (depending on dialog answer): Controller stage ⇒ Relative mass change Trace Selection ⇒ Mass calculation Trace Selection Coefficients Mass change Point of reaction Step of reaction (difference) Display X-coordinate values (yes / no) Follow action: Selection of two or four data points 100 . MENU AND DIALOG SEQUENCE The following will give you a view over the dialog sequence for all TG specific commands from the menu "Evaluation”. X-smoothing Signal correction Zero correction (Temp. if enclosed in package) ⇒ Signal correction..7.Linseis STA Evaluation Software 16.

9%) Range (Whole trace(s) / Zoom window / Controller stage) Following actions (depending on dialog answer): Controller stage Smoothing behavior ⇒ Collection file Collection file Create new collection file Extend existing collection file Range (Whole trace(s) / Zoom window I Controller stage) Following actions (depending on dialog answer): Select collection file (file name .Linseis STA Evaluation Software ⇒ Curve arithmetic Trace Selection Curve arithmetic Connection of two curves Add curves Subtract curves Multiply curves Divide curves Evaluation of one curve Constant offset Constant factor Reflect through X-axis Range (Whole trace(s) / Zoom window / Controller stage) Following actions (depending on dialog answer): Trace Selection Enter constant Controller stage ⇒ Mean curve Mean curve Create new mean curve Extend existing mean curve Convert type of mean curve Statistical confidence (95% /99% 199.GSM) Trace Selection Controller stage 101 .

. However. 3.. The information in this field can be changed with the ”Edit.Restore.”.: ”File . the program is equipped to hide all traces. HINTS 16. They can be displayed by selecting ”Options .). Load Data. Under ”Trace”..Signal correction. Turn on protocol function: ”Options .1. 8. Signal smoothing: ”Y-smoothing”. Protocol printout: ”Print .. .Protocol” (The ”On” condition is marked with a little check mark on the left side.. selection of coefficients.8.”.2.” with TG-import <sample> (use appropriate import filter when importing data.8.Linseis STA Evaluation Software 16. . 6.. This function is also available in the main menu.Info field..Protocol.. 2..Load.) 7.Mass calculation .. Information Field The most important information about the trace is shown to the user while loading the trace. you will find commands such as “Hide. 16. Signal correction: ”Evaluation . 16. Create new evaluation window (”File .g.Function Group . when heat-up and cool down stages exist. Mass calculation: ”Evaluation .8. Limitation of Trace Section When using a full trace with its entire length...” the present information window can be overwritten by the original..New”) I enter name.Load Original.. 102 .4. except the last used trace (and perhaps directly related traces). (E.Adjust Ranges”. X-smoothing”... the processing time slows down or it is impossible to process the curve. Load function group (”Evaluation .) The use of the zoom function or the selection of a controller stage will give you a range of the trace to evaluate.” 16.3. Recommended Standard Evaluation We recommend the following procedure to create a standard evaluation: 1.. .TG-Evaluation”).Load Data. With the function ”Options . The window is constantly undated with new results of the evaluation.. Problems with Trace Display One problem that may occur is that the display becomes unclear when using too many traces.. 5.” function..8..8..Info field. 4. .

g. HOW TO CREATE A DSC OR HDSC CALIBRATION FILE There are two ways for calibration of Heat flow Calorimeters: • Measurement of Phase Change Enthalpies • Measurement of Heat Capacity of a Reference Sample (e. In this case a temperature calibration is not possible. but also the temperature scale can be calibrated. • Calibration with a Heat Capacity Standard uses one calibration run for the whole temperature range. 103 . Sapphire) Both Methods have advantages and disadvantages: • At Calibration with Substances (Enthalpy) only a few calibration points are possible.How to create a DSC or HDSC calibration file 17.

If it is desired to use the temperature calibration too.46 BaCO3=806.000. a calibration file (*.59 Zinn=231.24. a temperature calibration of measurements can’t be performed). To create a calibration file. containing the proper values of onset-temperature ([°C]) and enthalpy ([J/g]) of the desired calibration substances.60.000.How to create a DSC or HDSC calibration file 17. (H)DSC CALIBRATION BY MEASUREMENT OF PHASE CHANGE ENTHALPIES For signal calibration of DSC/HDSC measurements.103. If a substance has more than one peak. once for each peak.INI file additional substances may be added by the user: Indium=156. related to the used heating rate • Coefficients for enthalpy calibration (mK or µV to mW) as a function of the temperature For temperature calibration a first order polynomial function (offset and factor). • The data-files of the calibration measurements The set of calibration substances used should include the desired temperature range for sample measurements.112. using different names for each peak (see K2SO4.INI-file.210. the corrected value of the onset-temperature is extrapolated for heating rate 0K/min).80.91 K2SO4_2=1069. the second one the onset- temperature in [°C] and the third one the enthalpy in [J/g].000. 104 . The following substances are predefined in the DSCCAL.42.149.527.48 Blei=327. The calibration measurements should be run with the same crucibles and heating rates used for the sample measurement also. the following data is required: • A DSCCAL.DCF) is required.30 The first column contains the name of the substance used.66 SrCO3=929.36 K2SO4_1=584.462.000.86 Gallium=29. each sample must be measured with at least two different heating rates (the shift of the onset-temperature related to the heating rate will be calculated. the information for temperature calibration can be included (if it is not present.81 Zink=419. having two peaks). This file usually contains two kind of calibration information: • Coefficients for temperature calibration.28. it must be entered several times.1.7646. for enthalpy calibration a polynomial up to a fifth order may be used.928.5985. The information of the enthalpy calibration must be contained in the calibration file.

105 . • Use the name of the calibration substance used as the evaluation window name. you are asked either to append to or to delete the existing protocol file. The enthalpy for calibration purpose should always be set to grams. this name must match the MS-DOS naming conventions. • Choose DATA PEAK EVALUATION from menu EVALUATION. Then you are asked for several options. the data-files must be evaluated to create the protocol-files. Use the smoothing factor suggested by the program. 4 if the method of increase of the peak are is used. It is also suggested to use filenames. If the existing file holds valid information of earlier evaluations you should select append. if not already set up. marking those regions of the trace. you should choose delete and create a new protocol file. if not. heating rate 10K/min. Partition integration is not required for single peaks. containing the information for heating-rate. first run) to avoid confusing during evaluation of the measurements. • Create a new evaluation window (FILE-NEW). If an evaluation protocol with the same name exists. PB10-1 for: Substance lead. • Select the proper function library (EVALUATION-FUNCTION GROUP-DSC or HDSC). derivation is not required. the baseline is still identical to the trace). The following procedure is suggested: • Start the data-evaluation (if it not running yet). not to mol. corresponding to the used substance and heating rate (e. perform smoothing only.How to create a DSC or HDSC calibration file It is useful to create an own subdirectory for all calibration measurements.g. When all calibration measurements are completed. • Switch on the generation of the evaluation protocol (OPTIONS-PROTOCOL). • Click OK and mark the peak with the required count of points (2 if the straight line method is used for beginning and ending of the peak. • Optional you can zoom to the range of interest (peak) of the trace to increase evaluation speed on slower computers • Choose SMOOTHING and DERIVATION from menu EVALUATION. • Optional you can perform a zero-correction if desired (a corresponding zero measurement must be available). • Load the data file of the calibration measurement (FILE-LOAD). onset-temperature and peak-area. At least ONSET POINT and PEAK AREA must be activated. Selection of the manner to construct the base line is due to your preferences (straight line model or depending on the increase of the peak area).

the coefficients for temperature correction may be calculated (selection Calculate Te (β→0)). depending if you want to create a new calibration file or to add the new information to an existing one. must contain at least two measurements of the same substance. After calculation. using the menu topics TEMPARATURE and ENTHALPY. After this. If more than one protocol file is used for temperature calibration. If you have chosen NEW before and a calibration file with this name already exists. Select NEW or OPEN from menu CALFILE. using the same calibration substance are written to a single protocol file. C:\TAWIN\DSC\PARAM) and select the protocol file desired. This protocol file has the same name like the evaluation window and the ending ‘TXT’. If there are at least two entries with different heating rates. • Use the same procedure for all calibration substances measured. you are asked whether to over write it or not. you are asked for the name of the protocol file. Next you are asked for the calibration file name. For temperature calibration. The default name is CALIB. • When the evaluation of all data files of one calibration substance is completed. created with the same calibration substance and perform the same procedure described above. using DSCCAL or HDSCCAL.g. depending on the instrument used. an error message is displayed. So all information of multiple measurements. you are asked if you want to store the results in the calibration file. the average of all results is calculated. 106 . Now you can select the next protocol file (selection Other Protocol file) and perform the same actions as described above until all protocol files are processed. After this you can create entries for temperature an enthalpy calibration. the protocol file(s) used. When choosing TEMPERATURE from the menu. C:\TAWIN\DSC\PARAM). It is located in the PARAM directory of the related function library (e. but you can use any name desired (the name must match the MS-DOS naming conventions). choose EXIT from the file to close the active evaluation window. you are asked to select the desired entries in a list box (for default all entries are selected). If the selected protocol file contains only measurements with the same heating rate or a single measurement only.How to create a DSC or HDSC calibration file • Hide or delete all traces and load the next data-file. After this. Now you can close the data evaluation program and start the generation of the calibration file. measured at different heating rates. Switch to the proper directory containing the protocol files generated (e.g. the related PARAM-directory should contain one protocol file for each calibration substance used.

Before leaving (H)DSCCAL you may view the *. especially outside of the definition range (Temperature range of substances used). If the resulting correlation has a low value (1. After this. For this purpose. After calculation. C:\TAWIN\DSC\CALIB). 107 . a similar procedure is used.0 = best value. the same directory the calibration file (ending *. The polynomial order is chosen automatically to match the entered correlation • You can enter the desired polynomial order and the resulting correlation is calculated. the factor for enthalpy calibration may be calculated (selection Calculate Factor).5 = unusable) you should figure out which entry in the protocol file causes this failure and ignore it when calculation the calibration factor (usually this is caused by a wrong sample weight entered or a pollution of the sample itself). If the protocol file contains more than one peak entry. There are two different ways for calculation: • You can enter the desired correlation. At this point. the desired temperature range and file name must be entered. the calibration file contains one entry for every substance used. Now you can select the next protocol file (selection Other Protocol file) and perform the same actions as described above until all protocol files are processed. and for selecting the desired entries in the protocol file (for default all entries are selected).How to create a DSC or HDSC calibration file For enthalpy calibration. you are asked if you want to store the results in the calibration file.DCF) is stored also.TXT) file(s) by means of the Notepad editor (menu topic EDIT). After this the calibration file is ready to use by the evaluation program. You are also asked for the protocol file to use.DCP) will be stored in the CALIB-directory (e. with the onset temperature and the factor for calculating [mW] from [mK] or [µV]. You can also create a polynomial curve (a data file which can be loaded by means of the evaluation program) for visual control of the behavior of the calibration factor over temperature (menu topic polynome curve). the average will be calculated.g. The generated file (ending *. < 0. Now the polynomial coefficients for the enthalpy calibration may be calculated (Selection Approximation Curve). This is useful to force the use of a lower polynomial order (Suggested: second degree) to avoid a rough behavior of the calibration function.CAL (or protocol *.

208120 700. The extension must be .261337 1000.0 1.0 1.0 0. A minimum of 6 entries are necessary. 108 .0 1.HRF (Heat flow Reference File) This file should be stored to the CALIB directory C:\TAWIN\DSC\CALIB for DSC or C:\TAWIN\STA\CALIB for HDSC This file is supplied by Linseis if a Calibration Standard is ordered.717914 50.0 1.237096 850.969583 200.245605 900.136620 500.0 1. Temperature [°C] and Head Capacity [J/gK].218464 750.228080 800.824791 100. a dot is used for the decimal separator.115137 400.018848 250.0 1.057906 300.0 1.0 0.0 0.0 1.How to create a DSC or HDSC calibration file 17.0 0.253670 950.184475 600.0 1.089367 350.268635 To create a table the Windows Editor “Notepad” can be used.196870 650.0 1.0 1.0 1.0 1.0 1. Both columns are delimited with one or more blanks. maximum are 100 entries: Example of a table for Sapphire: 0.170614 550.2. (H)DSC CALIBRATION WITH HEAT-CAPACITY STANDARD The following files are needed to create a calibration File: • Zero Curves (run with empty crucible) • Sample run with Calibration Standard in the Sample crucible • Literature values of the used Calibration Standard From the Literature values of the used Heat Capacity Standards a table must be created.0 1.0 1. This table (Text file) must have two columns.906528 150.

than: .How to create a DSC or HDSC calibration file How to create a Calibration File: The zero run and the calibration run must be done. Do the zero correction to subtract the empty run: Next select in the menu EVALUATION the entry ´CREATE CALIBRATION FILE´ A dialog will appear. Select the second trace (the trace which appeared on the screen as the result of the subtraction). 109 . Load the Calibration Standard run into the Evaluation software .

The name must be given in the following dialog. Select the one which matches the calibration run: The software will now calculate according to the used heating rate and the standard mass the (uncalibrated) heat capacity. The result is the calibration factor.How to create a DSC or HDSC calibration file Then the result must be compared with the literature values. The default name is the name of the calibration standard run: 110 .HCF (Heat flow Calibration File) and will be saved in the CALIB directory. The software displays the available calibration standards tables. This file has the extension . Next the corresponding literature temperature value will be interpolated and divided by this (uncalibrated) calculated value.

This calibration file now can be used to calibrate sample runs. Do the zero correction. 111 . Using the Calibration File: Load a sample run into the evaluation.How to create a DSC or HDSC calibration file In the next diagram the Calibration factor is displayed against Temperature: The calculation of the calibration file is now finished. .HCF files if using a calibration file which was created with a Heat Capacity Reference Sample. Select the correct FILE TYPE. Next select in the menu the point ´SIGNAL CALIBRATION´ In the dialog ´CALIBRATION FILE´ select the folder icon to display another windows like the one below.DCF files if using a calibration file which was created with substances .

How to create a DSC or HDSC calibration file Then select the correct file from the list: The Heat Flow Trace will be calculated [mJ/s]: 112 .

Therefore the point ´SPECIFIC HEAT CURVE´ must be selected.How to create a DSC or HDSC calibration file This Heat Flow Trace can be used for further evaluation like smoothing and then Data Peak Evaluation for Enthalpy calculations [J/g] or the Glass Transition point. This trace gives the heat capacity of the sample for any temperature value [J/gK]: 113 . Also the Heat Flow Trace can be used to calculate the Heat capacity of the sample.

1.Evaluation flowcharts 18. EVALUATION FLOWCHARTS 18. DTA EVALUATION FLOWCHART 114 .

Evaluation flowcharts 18.2. DSC EVALUATION FLOWCHART 115 .

TG EVALUATION FLOWCHART 116 .Evaluation flowcharts 18.3.

Evaluation flowcharts 18.4. CP EVALUATION FLOWCHART 117 .

Therefore choose OPTIONS – Read error-status.Error Codes 19. ERROR CODES Internal device errors are shown as error codes in the actual values field in the weight reading. 118 . In the following spreadsheet are the meanings of the codes explained. The shown error code is composed of the error marker E and a classification number. Example: If there is no cooling water flow (E010) and no sample thermocouple mounted (E001) in the reading will shown E011. Error Code Description 001 Sample thermocouple open 002 Furnace thermocouple open 004 Maximum temperature overrun 010 No cooling water flow 020 Tara initalization error 040 Tara error 080 Controller error 100 FIFO Buffer overflow 200 Flash error 800 Internal error Actual error codes can also be shown in the measurement software. the shown code is the sum of the particular error codes. Are several errors present.

2008 Standard reference program 119 . LINSEIS STANDARD REFERENCE MATERIAL Certificate Standard reference Material DTA – HDSC Weight loss as a Function of Temperature Material Indium In Onset: 156. For this please refer to manufacturer certificate. K2SO4. BaCO3.99%. The provided Reference Material “BaCO3” was heated up to 1000°C with 5K/min.Linseis Standard reference Material 20. Nickel has a manufacturer guaranteed purity better 99. The provided Reference Material “K2SO4” was heated up to 1200°C with 5K/min The provided Reference Material “Nickel” was heated up to 1550°C with 5K/min Origin of reference Material: The provided Indium. Selb – 95100 / Germany Dec 04.6 °C Barium Carbonate BaC03 Onset: 806 °C Potassium Sulfate K2SO4 Onset Stage 1: 584 °C Onset Stage 2: 1069 °C Nickel Ni Onset: 1453 °C Procedure of Calibration: The provided Reference Material “Indium” was heated up to 220°C with 5K/min.

29% in total) 3.43% 2. Origin of reference Material: The provided Copper sulfate has a manufacturer guaranteed purity better 99%.08% (-79.86% (-43. 2006 Standard reference program 120 . Stage: Decarbonation: CuSO4 + 5H2O ⇒ CuSO4 + 3H2O ↑ Mass change: -14.37% in total) Procedure of Calibration: The provided Calibration Material “copper sulfate” was heated up to 310°C with 5K/min. For this please refer to manufacturer certificate. Stage: Decarbonation: CuSO4 + H2O ⇒ CuSO4 ↑ Mass change: -36. Stage: Decarbonation: CuSO4+ 3H2O ⇒ CuSO4 + H2O ↑ Mass change: -28. Selb – 95100 / Germany March 06.Linseis Standard reference Material Linseis Standard reference Material Certificate Standard reference Material Thermogravimetry: Copper sulfate Weight loss as a Function of Temperature Copper sulfatee: CuSO4 + 5H2O 1.

Linseis Standard reference Material 121 .

Stage: Decarbonation: CaCO3 ⇒ CaO + CO2↑ Mass change: -30. 1994 Standard reference program 122 .2% (-31.7%.1% (-61.3% 2. Selb – 95100 / Germany March 17. Origin of reference Material: The provided Calcium Oxalate has a manufacturer guaranteed purity of 99. Stage: Dehydration: CaC2O4 + 1H2O ⇒ CaC2O4 + H2O↑ Mass change: -12. Stage: Building carbonate: CaC2O4 ⇒ CaCO3 + CO↑ Mass change: -19.Linseis Standard reference Material Linseis Standard reference Material Certificate Standard reference Material Thermogravimetry: Calcium oxalate Weight loss as a Function of Temperature Calcium oxalate: CaC2O4+1H2O 1.5% in total) 3. For this please refer to manufacturer certificate.6% in total) Procedure of Calibration: The provided Calibration Material “Calcium Oxalate” was heated up to 1000°C with 5K/min.

For this please refer to manufacturer certificate. Origin of reference Material: The provided Al2O3 has a manufacturer guaranteed purity better 99%. Selb – 95100 / Germany March 06.Linseis Standard reference Material Linseis Standard reference Material Certificate Standard reference Material Thermogravimetry: Al2O3 Weight loss as a Function of Temperature Aluminum oxide: Al2O3 Procedure of Calibration: The provided Reference Material “Al2O3” was heated up to 1600°C with 5K/min. 2006 Standard reference program 123 .

Linseis Standard reference Material 124 .

2006 Standard reference program 125 . Origin of reference Material: The provided Calcium carbonate has a manufacturer guaranteed purity better 99%.1% Procedure of Calibration: The provided Calibration Material “Calcium carbonate” was heated up to 1000°C with 5K/min.Linseis Standard reference Material Linseis Standard reference Material Certificate Standard reference Material Thermogravimetry: Calcium carbonate Weight loss as a Function of Temperature Calcium carbonate: CaCO3 Stage: Decarbonation: CaCO3 ⇒ CaO + CO2↑ Mass change: -30. For this please refer to manufacturer certificate. Selb – 95100 / Germany March 06.

Linseis Standard reference Material 126 .

Enthalpy of Melting for Standards 21. ENTHALPY OF MELTING FOR STANDARDS The following table summarizes the best known temperatures and heats of melting for many standard materials. 127 . These values may be used for temperature and/or cell constant calibration of the Linseis DSC or HT-DSC/DTA.

Enthalpy of Melting for Standards 128 .

The table below summarizes specific heat capacity data (literature values) for sapphire as a function of temperature. SAPPHIRE SPECIFIC HEAT CAPACITY LITERATURE VALUES Specific heat capacity measurements by DSC require the use of a well-characterized reference material (usually sapphire) to obtain results. These values can be used in the required calculations.Sapphire Specific Heat Capacity Literature Values 22. 129 .

130 . The units J/gmole are absolute joules per degree per gram mole (molecular weight .101.98 to 99.99 % purities by weight. Heat capacity values below the experimental range were obtained by extrapolation of the Debye equation fitted to the experimental value at the lowest temperature. The sapphire pieces passed a #10 sieve but were retained by a #40 sieve.Sapphire Specific Heat Capacity Literature Values The values in the table were determined by Ginnings and Furukawa of the National Bureau of Standards on aluminum oxide in the form of synthetic sapphire (corundum).9613) at a constant pressure of 1 atmosphere (100 Pa). and had 99.

THERMOGRAVIMETRIC ANALYSIS OF CALZIUMOXALATE Calziumoxalate: CaC2O4 + 1H2O 1.3% 2.1% (-61.Thermogravimetric analysis of Calziumoxalate 23.5% total) 3.2% (-31. Stage: Dehydration: CaC2O4 + 1H2O ⇒ CaC2O4 + H2O↑ Mass change: -12. Stage: Building carboante: CaC2O4 ⇒ CaCO3 + CO↑ Mass change: -19. Stage: Decarbonation: CaCO3 ⇒ CaO + CO2↑ Mass change: -30.6% total) 131 .

KCN-dilution at elevated temperatures • High temperature resistant oxides above 1000°C Platinum is not resistant against: • Mixtures out of KNO3 and NaOH at 700°C sealed from air • Mixtures out of KOH and K2S at 700°C sealed from air • LiCL at 600°C • Na2O2 at 500°C sealed from air • MgCl2.Chemical behavior of Crucibles 24. . F2. keying the surface • Alkali hydroxide. H2O2 (30%) and HNO3 at 100°C • KCI (damaging at the decomposition products crated during the melting. Ni. HJ. for example (chromic acid.1. B • Se above 320°C (cool down sample immediately after measurement and remove probe to prevent Selenium evaporation) • Metal oxides with reducing substances such as C. 1000°C • FeCl3 • Be composites (evaporate just above melting point) • HCL with oxidizer. K. LiF. CHEMICAL BEHAVIOR OF CRUCIBLES 24. Hg. Iron (III)-salts. salt smelter) • Reducing atmosphere • Pb. . Zn. Ba(NO3) at 700°C • HBr. already before CO2-release • SiC at app. Fe.cyanides and – rhodanides at elevated temperatures • KHSO4 at elevated temperatures • Carbon black or carbon above 1000°C • SiO2 under reducing conditions • HBr. As. aqua regia • Li2CO3. manganat. Na. Bi. Sb.carbonates. Au. Li. Si (composition creation) • P. Br2). melting point 768°C) Limited durable against: • KHF2. Sn. Steel. . Ag. organic compositions or H2 • Sulfur.sulfates. NaCl at 900°C • Mixtures of NaOH and NaNO3 at 700°C sealed from air 132 . PLATINUM CRUCIBLES Critical for Platinum is: • Halogens (Cl2.

To do this. After heating up above 1500°C. So. a small disc of alumina (Al2O3) is used as a spacer between the measuring system and the crucibles. to prevent from becoming welded on the measurement system due to multiple runs. After baking.Chemical behavior of Crucibles 24. The crucibles must be put bottom up on the alumina disc. To bake the crucibles. So. 1100°C direct touching platinum surfaces are welded. To remove the crucibles. Do not forget to remove the crucible for the reference material also after each run. when used above 1200°. for measurements up to 1550°C crucibles made of alumina must be used instead. Not any temperatures above 1500°C must be used with platinum crucibles. because the coating of platinum oxide will be destroyed at these temperatures. 133 . the crucibles may stick slightly on the measuring system. In a second run the measuring system itself must be baked also (without alumina disc). crucibles and measuring system would be destroyed. use a pair of tweezers to tip over the crucible while holding the measuring system by hand. the surfaces of the measuring system must not be touched with fingers or polluted with other substances.2. If the system shall be used above 1100°C. the measuring system must be baked at 1500°C again. without special precautions the platinum crucibles and the measuring system would become welded. preventing welding during measurement. IMPORTANT HINT FOR HDSC MEASURING SYSTEM Above app. the measuring system and the crucibles must be heated separately up to 1500°C (20K/min) and held for a 15min dwell time (cooling should be done with 30K/min). In spite of baking the platinum parts. the crucibles and the measuring system must be baked separately in oxidizing atmosphere (air) to create a coating of platinum oxide.

analog PbO • MeO: Me = Fe2+. important for Hydroxides. Nitrates. Co2+. creation of Aluminaborates and -borides • Alkali. • Alcali. Nitrides. also important for Lead oxide and Lead salt in combination with anions of volatile acids • UO3: Reaction start at 450°C.anions and cryolite related salts • Glass: Glass smelter dissolves Al2O3 • Hydrogen sulfate of the Alkali. Carbonates.Chemical behavior of Crucibles 24. reaction at elevated temperatures which is increased when Carbon is present • B2O3 or Borax: Smelter dilutes Al2O3. for this reason measurements with Carbon at elevated temperatures under nitrogen atmosphere are critical • F2: creation of AIF3 and O2 • Cl2: creation of AlCl3 above 700°C • Sulfur: no reaction with liquid sulfur.Earthalcaliferrites : smelter dissolves Al2O3 • Zirconium composites with melting points between 800 and 1200°C : slow and weak reaction • Some metal alloys such as: Fe with 4% Al 134 . 1000°C • Compositions containing Silica. 1400°C • HF: quantitative reaction to AIF3 and H2O at elevated temperatures • CuSO4: Diffusion trough crucible surface at app. Peroxides.and Alkaliearthoxide • HCI: no reaction until 600°C. etc. under air reaction at the contact point • Metal fluorides: attacked by smelter. ALUMINUMOXID CRUCIBLES Critical for Aluminumoxid is: • N2 in presence of Carbon: creation of AIN. Ni2+. such as MOSi2: in Inertia lead to contamination of Al2O3 at app. creation of (AIF6)3. creation of sulfides at elevated temperatures • H2S: under heat exposure creation of Al2S up to 3% • C: Creation of Carbides and Al at app. 1200°C.3.and Alkaliearthoxide and their salts with volatile anions: smelter creates Aluminates or double oxides. if Carbon is present during the gas phase. etc • CaC2: under heat creation of Al4C3 • PbO: Reaction at 700°C.

for that the reaction of SiO2 and C certainly starts earlier) • NO.Chemical behavior of Crucibles 24. 1400°C (formation of SiC) • Chromic acid (aqueous) • Cl-SO3H • SiO2 → formation of SiC via the intermediate product SiO (technical production of SiC at temperatures above 1800°C. Ni. Co. reaction above 400°C • Melted metals such as: Fe. 150°C • Saltpeter acid HNO3. Br2. GRAPHITE CRUCIBLES Critical for Graphite is: • O2. Na • N2 reaction starting from 1700°C (Creation of small amounts of Cyanides) • Oxides (probable reduction when directly contacting) • Water vapor • F2. 90°C • SO3 at arr. 100°C • Danger of explosion with HCLO4 • NaOCL at arr. diluted at arr. NO2 • Sulfur acid H2SO4 concentrated at arr. 50°C 135 . at room temperature • Sulfur • Si at app.4.

• Program CONTROLLER. • Start measurement with START. zero file name. • Open furnace using LIFT switch at balance press ↑. SETTINGS. SETUP SCALES to find the Tara of the balance. • Close furnace using LIFT switch at balance press ↓. weight of sample. Switch filter to √. • Start software STA MEASUREMENT.1. 136 . and ranges for TG and DTA (default DTA 250 µV). end temperature. QUICK Start manual for Thermobalance PT 1600 25. • Place crucible onto measuring system (reference crucible empty or with Al2O3). when you heat higher than 700°C. • Open cooling water (flow >0. duration. ATTENTION! • Don’t switch balance main switch off as long furnace is hot. SAMPLE TG+DTA. . for heating element and alumina tube protection. QUICK START MANUAL FOR THERMOBALANCE PT 1600 25. TEMPERATURE PROFILE. It is useful to start the measurement without the controller to see if the TG and the DTA Signal has no drift anymore.5 l/min) if using chiller adjust approx. • Press AUTOMATIC ZERO ADJUSTMENT. switch cooling water off or switch balance off only if the temperature value on the display is less than 100°C. • Sample file name. CURRENT VALUE for temperature of sample and furnace should be room temperature. • Remove used crucible and clean it toughly. 24°C. • Check CONTROLLER. • Don’t close cooling water as long furnace is hot. • Select OPTIONS. • Monitor measurement with CONTROLLER CURRENT VALUES or real time graphic. MEASUREMENT WITH SAMPLE (1600 °C) • Switch on computer and balance. • Open the furnace. • Program DATA ACQUISITION. • Insert new sample and weigh before. TYPE. ATTENTION! • Always program one heating rate with 30 °C/min down to 700 °C as last segment to cool down controlled. • Select DATA ACQUISITION. If it is Ok stop measurement and start the whole experiment.

ZERO TG+DTA. • One segment to maximum temperature. • Remove used crucible and clean it toughly. • Monitor measurement with CONTROLLER. • Open cooling water (flow >0. TEMPERATURE PROFILE.QUICK Start manual for Thermobalance PT 1600 25. end temperature. SETUP SCALES to find the Tara of the balance.5 l/min) if using chiller adjust approx. switch filter to √. • Select DATA ACQUISITION. duration. MEASUREMENT ZERO FILE (1600 °C) • Switch on computer and balance. • Program CONTROLLER. switch cooling water off or switch balance off only if the temperature value on the display is less than 100°C. • Program DATA ACQUISITION.2. gas conditions and heating rate like in the sample run. • Don’t close cooling water as long furnace is hot. • Check CONTROLLER. 24°C. • Press AUTOMATIC ZERO ADJUSTMENT. • Place two empty clean crucibles (or two crucibles filled with an equal quantity Al2O3) onto measurement system. and ranges for TG ±25mg and DTA 250µV. TYPE. ATTENTION! • Always program one heating rate with 30 °C/min down to 700 °C as last segment to cool down controlled. • Open furnace using LIFT switch at balance press ↑. CURRENT VALUES or real time graphic. • Select OPTIONS. for heating element and alumina tube protection. • Zero file name (should follow DOS conventions max. It is useful to start the measurement without the controller to see if the TG and the DTA signal have no drift anymore. If it is Ok stop measurement and start the whole experiment. 8 characters or numbers only). SETTINGS. • Open the furnace. • Start measurement with START. 137 . • Close furnace using LIFT switch at balance press ↓. CURRENT VALUE for temperature of sample and furnace should be room temperature. ATTENTION! • Don’t switch balance main switch off as long furnace is hot. • Start software STA MEASUREMENT. when you heat higher than 700°C.

San Diego. 1995) P. 1977) 138 . John Wiley & Sons.Appendix 26. 1972 Peter Haines “Principles of Thermal Analysis and Calorimetry” Royal Society of Chemistry. John Wiley and Sons Ltd (May 6. 1st edition (August 1. Bensted “Structure & Performance of Cements” Spon Press. Wunderlich: “Thermal Analysis”. Barnes. Van Norstrand. 2nd edition (October 2. Toronto..) Springer-Verlag (December. Wiley-Interscience. MacKenzle “Differential Thermal Analysis Fundamental” Academic Pr (June 1.WM.I. J. 1999) Randall M. 1997) T.Hill (de. 1996) by James S. Blazek: “Thermal Analysis”. Reed “Principles of Ceramics Processing”. London. Pope “Pope Differential Thermal Analysis . Edition III. Wendlandt: „Thermal Methods of Analysis“. German “Sintering Theory and Practice” John Wiley & Sons (January 19. 2nd edition (January 15. New York. Boston. (Ecological Studies. Academic Press Inc. 2002) R.O. Hatakeyama. 2nd Edition Wiley-Interscience. 1970) Werner Smykatz-Kloss “Differential Thermal Analysis: Application and Results in Mineralogy”. Sidney. 1974) M. New York.): “For better Thermal Analysis”. 2002) Adrian Bejan “Advanced Engineering Thermodynamics”. London.C. APPENDIX J. ICTA 1991 W.A Guide to the Technique and Its Applications”. 1974 B. Liu Zhenhai “Handbook of Thermal Analysis” John Wiley & Sons (March 5. 1990 A. 2 edition (January 9.

SOME THERMO ANALYTICAL STANDARDS DIN 51 005 Thermal Analysis (TA) terms DIN 51 006 Thermal Analysis (TA). Thermogravimetry (TG) principles DIN 13346 Temperature. temperature difference.Some Thermo Analytical Standards 27. basic concept and units DIN 1610 Temperature measurement DIN 43760 Basic values for measuring resistors ASTM D3418 Transition temperature of polymers by Thermal Analysis ASTM E473 Standard definitions of terms relating to Thermal Analysis ASTM E793 Heats of fusion and crystallization by DSC ASTM E472 Standard practice for reporting Thermo analytical Data ASTM= American Society for Testing and Materials DIN= Deutsche Industrie Norm (German Industrial Standard) 139 .

2010 Grie?hammer 19 Kapitel errorcodes eingefügt 006 22. heating element change 004 14.07. gesamtes Dokument überarbeitet Parts list entfernt.10.2011 Grießhammer 6. 003 30.2010 Grießhammer 1600°C Abgleich überarbeitet Messysteme überarbeitet Chaper 005 27.09.2 electrical wiring added anneling moved to chapter chemical 007 02032011 Grießhammer behavior of crucibles 140 .2009 Grießhammer all Inhaltsverzeichnis erstellt.02.Some Thermo Analytical Standards Integration Einzelanleitungen.