Manual - Notes

LINSEIS STA PT1600
Thermogravimetric Analyzer
Instruction Manual
Linseis Messgerte GmbH

Vielitzer Str. 43
D-95100 Selb
Tel.: 0049 9287 880-0

Fax: 0049 9287 70488
Mail: [email protected]
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. 1400C and 1600 C furnace .............................................................................................................. 25
7.2.2. 1750C furnace .................................................................................................................................. 28
7.3. Change furnace thermocouple......................................................................................................... 30
8. PREPARING A MEASUREMENT ....................................................................................... 32

9. COMPATIBILITY OF CRUCIBLE MATERIALS AND SOME SUBSTANCES ............. 36
10. SELECTION OF THE GAS ATMOSPHERE....................................................................... 37
11. GASES AND THEIR LIMITATIONS .................................................................................. 39
12. GAS FLOW IN THERMOGRAVIMETRIC EXPERIMENTS ........................................... 41
13. LINSEIS STA MEASUREMENT SOFTWARE .................................................................. 42
13.1. Type of Measurement ..................................................................................................................... 42

13.1.1. TG Measurement ............................................................................................................................... 42
13.1.2. DTA/HDSC Measurement .................................................................................................................. 42
13.1.3. TG+DTA/HDSC Measurement ............................................................................................................ 42
13.2. Setup Data Acquisition .................................................................................................................... 43

13.2.1. Example TG Measurement ................................................................................................................ 43
13.2.2. Example DTA Measurement .............................................................................................................. 43
13.2.3. Example TG DTA Measurement ...................................................................................................... 44
13.2.4. Description of the Input Parameter................................................................................................... 44
13.3. Program Controller .......................................................................................................................... 46

13.3.1. Controller Set Values ......................................................................................................................... 46
13.3.2. Program the Controller Set Values .................................................................................................... 46
13.3.3. Graphic Display .................................................................................................................................. 47
13.3.4. Store Controller Set Values................................................................................................................ 47
13.3.5. Load Controller Set Values ................................................................................................................ 47
13.3.6. Delete Controller Set Values.............................................................................................................. 47
13.3.7. Display Current Values ...................................................................................................................... 48
13.3.8. Uncontrolled Preheating ................................................................................................................... 49
13.3.9. Adjust Cold Junction Reference ......................................................................................................... 49
13.3.10. PID-Parameters.................................................................................................................................. 50
13.4. Start and Stop Measurement........................................................................................................... 51

13.5. Real-time graphic ............................................................................................................................ 51
13.6. Balance Setup .................................................................................................................................. 52
13.6.1. Zero Adjustment ................................................................................................................................ 52
13.6.2. Zero Point Definition ......................................................................................................................... 52
13.6.3. Manual Adjustment ........................................................................................................................... 52
13.6.4. Automatic Adjustment ...................................................................................................................... 53
13.7. Relays .............................................................................................................................................. 53
14. PERFORMING A ZERO BASELINE CURVE..................................................................... 54
15. PERFORMING A SAMPLE CURVE .................................................................................... 61

16. LINSEIS STA EVALUATION SOFTWARE ....................................................................... 68
16.1. Introduction .................................................................................................................................... 69

16.1.1. Minimum Hardware + Software Requirements ................................................................................ 69
16.1.2. Recommended Equipment ................................................................................................................ 69
16.1.3. Evaluation of Measurements ............................................................................................................ 69
16.2. Start new Evaluation ....................................................................................................................... 70

16.2.1. Save Evaluation.................................................................................................................................. 71
16.2.2. Open Existing Evaluation ................................................................................................................... 71
16.2.3. Various Evaluations Simultaneously .................................................................................................. 71
16.2.4. Arrange Evaluation Windows ............................................................................................................ 72
16.2.5. Change of Active Evaluation Windows .............................................................................................. 72
16.3. Traces in the Evaluation ................................................................................................................... 73

16.3.1. Defaults for Traces............................................................................................................................. 73
16.3.2. Add Traces ......................................................................................................................................... 73
16.3.3. Select Actual Trace ............................................................................................................................ 73
16.3.4. Select Trace Display ........................................................................................................................... 74
16.3.5. Delete Traces ..................................................................................................................................... 74
16.3.6. Hide and Restore Traces .................................................................................................................... 74
16.3.7. Hide and Restore Trace Names ......................................................................................................... 74
16.4. Evaluation Icon ................................................................................................................................ 75

16.4.1. Function Groups ................................................................................................................................ 75
16.4.2. Temperature profile Icon .................................................................................................................. 76
16.5. Summery of Functions ..................................................................................................................... 77

16.5.1. Correction Procedure ........................................................................................................................ 77
16.5.2. Curve Arithmetic................................................................................................................................ 79
16.5.3. Creation of a Collection File ............................................................................................................... 80
16.6. Program description ........................................................................................................................ 81

16.6.1. Tool box ............................................................................................................................................. 81
16.6.2. Explanation of Tools .......................................................................................................................... 82
16.6.3. Evaluate Traces .................................................................................................................................. 83
16.6.4. Legend ............................................................................................................................................... 84
16.6.5. Lines ................................................................................................................................................... 86
16.6.6. Info Field ............................................................................................................................................ 87
16.6.7. Print ................................................................................................................................................... 88
16.6.8. Miscellaneous .................................................................................................................................... 89
16.6.9. How to perform an ASCII export ....................................................................................................... 90
Data Structures ............................................................................................................................................... 97

16.6.10. Data Formats ..................................................................................................................................... 97
16.6.11. Name and Directory Conventions ..................................................................................................... 97
16.6.12. Created Data ...................................................................................................................................... 98
16.6.13. DSC and HDSC calibration file ............................................................................................................ 99
16.7. Menu and Dialog Sequence ........................................................................................................... 100

16.8. Hints .............................................................................................................................................. 102
16.8.1. Recommended Standard Evaluation ............................................................................................... 102
16.8.2. Problems with Trace Display ........................................................................................................... 102
16.8.3. Limitation of Trace Section .............................................................................................................. 102
16.8.4. Information Field ............................................................................................................................. 102
17. HOW TO CREATE A DSC OR HDSC CALIBRATION FILE ......................................... 103
17.1. (H)DSC Calibration by Measurement of Phase Change Enthalpies ................................................. 104

17.2. (H)DSC Calibration with Heat-Capacity Standard ........................................................................... 108
18. EVALUATION FLOWCHARTS ......................................................................................... 114
18.1. DTA evaluation flowchart .............................................................................................................. 114

18.2. DSC evaluation flowchart .............................................................................................................. 115
18.3. TG evaluation flowchart ................................................................................................................ 116
18.4. Cp evaluation flowchart................................................................................................................. 117
19. ERROR CODES .................................................................................................................... 118
20. LINSEIS STANDARD REFERENCE MATERIAL ........................................................... 119
21. ENTHALPY OF MELTING FOR STANDARDS .............................................................. 127
22. SAPPHIRE SPECIFIC HEAT CAPACITY LITERATURE VALUES............................. 129
23. THERMOGRAVIMETRIC ANALYSIS OF CALZIUMOXALATE ................................. 131
24. CHEMICAL BEHAVIOR OF CRUCIBLES ........................................................................ 132
24.1. Platinum Crucibles ......................................................................................................................... 132

24.2. Important hint for HDSC measuring system ................................................................................... 133
24.3. Aluminumoxid Crucibles ................................................................................................................ 134
24.4. Graphite Crucibles ......................................................................................................................... 135
25. QUICK START MANUAL FOR THERMOBALANCE PT 1600 .................................. 136
25.1. Measurement with sample (1600 C) ............................................................................................. 136

25.2. Measurement zero file (1600 C) ................................................................................................... 137
26. APPENDIX ............................................................................................................................ 138
27. SOME THERMO ANALYTICAL STANDARDS .............................................................. 139

General Information
1. GENERAL INFORMATION
In the design of your Linseis instrument, we try to take individual solutions into account
and to include these in the documentation.
Nevertheless, the keep the range of the instrument documentation at a level which can
be handled, the instrument manual/description has to be limited to common or standard
model.
Electronic or mechanical distribution or duplication of this/these instructions requires

written permission from LINSEIS MESSGERTE GmbH.
All instrument features, 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.
Linseis Messgeraete GmbH welcomes any remarks, suggestions or new ideas regarding
the instrument and these operating instructions. Please send any comments to the
following address:
LINSEIS Messgerte GmbH

Vielitzer Str.43
D-95100SELB
Telephone: (+49) 9287 880-0

Fax: (+49) 9287/70488
E-Mail [email protected]
Internet http://www.linseis.com
Any type of maintenance or service of the instrument must be carried out by LINSEIS
trained customer service personnel.
A service contract for your thermal analyzer is available on request.
This instrument instruction manual is designed to allow proper operation of the
instrument by the customer. LINSEIS Messgerte GmbH will accept no liability for
damage following-on improper use.
1
Basic System Safety Information
2. BASIC SYSTEM SAFETY INFORMATION
Allowed instrument operation
Any operation or misuse of the instrument other than explicitly certified requires
written approval from LINSEIS.
Any use exceeding the (expanded) authorized system operation is considered
unauthorized. The producer cannot be held accountable for any damage follow-on
such unauthorized use of the 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,
commissioning, operation and maintenance.
Training of User Personnel
Your Linseis instrument may only be operated and maintained by authorized,

trained and individually instructed personnel.
Responsibility for Commissioning, Operation and Training
Responsibility for commissioning, operation and maintenance must be clearly

defined and compliance must be ensured. The resulting responsibilities can be
clearly resolved under the aspect of safety.
Instrument Operation Guideline
The operator must make sure that only trained personnel work on the instrument.
Any type of operation of the instrument which reduces the safety of the
instrument user and the operability of the analyzer should be avoided.
Unauthorized changes to the system
Unauthorized modifications and changes which affect the safety of the thermal
analyzer are not permitted.
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.
2
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.
During Maintenance and inspection the instrument must be switched off and
unplugged.
Instruments or parts sent in for maintenance or repair should, to the extent

possible, be free of dangerous or harmful substances (e.g. toxic, radioactive,
etc.). Otherwise, the type of contamination must be declared. 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, a check should be made to ensure that all
protective devices are in place and operate properly. 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. Furthermore, possible dangerous reactions
with the materials used must be considered. At operating temperatures above
50C, protective gloves must be worn. Any industry specific regulations for the
analyzer are always relevant.
Consider possible reactions with the materials.
Warning signs should be hung in the appropriate places in accordance with

national and regional regulations.
Using Gases
Obey the appropriate national or international rules and protective measures

when using gases for a measurement.
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.
Use of the Operating Instructions
Using guidelines from the system Operation Manuals, the operator should arrange
additional internal operating instructions which specify the actions and tasks
required for additional safe operation.
The operating instructions should be easily accessible at the work place of the
instrument.
3
PRECAUTIONS & REQUIREMENTS
3. PRECAUTIONS & REQUIREMENTS
3.1. PROTECTING THE OPERATOR
The following safety precautions must be followed:
1. Plug all instruments into 3-prong receptacles to assure proper grounding

2. Do not remove instrument covers or attempt internal adjustments without unplugging
the instrument.
3. To prevent the possibility of burns, do not handle any items when the furnace is
above room temperature.
4. Use a filter trap on the purge gas outlet when noxious fumes are likely to be
generated.
3.2. PROTECTING THE INSTRUMENT
The following precautions will help protect the instrument:
1. Handle the furnace, thermocouples, measuring systems, and protection tubes with
care.
2. The internal balance parts are very fragile. Do not use any mechanical force when
working with the counter weights or measuring systems.
3. Do not disconnect power if the furnace is above 500oC. It will cause thermal shock to
the alumina components
4. When operating in a vacuum, slowly vent the system back to atmosphere. Opening
vacuum valves quickly will damage the internal balance parts.
4
Required facilities for installation
4. REQUIRED FACILITIES FOR INSTALLATION
1. Space requirement: (W x D x H)
a) Bench space for computer, printer and balance

Balance: 430 wide x 540 deep x 620 (mm) high
Approx. 25 kg
b) Floor space: power supply unit, 444 x 405 x 270 mm, approx. 25 kg
2. AC Voltage requirement:
Qty. 4 receptacle 230 V AC, 16 Amp for computer, printer, STA and power supply
NOTE: Receptacles can be substituted with approved replacements, please notify

Linseis of change.
3. Cooling water:
flow rate minimum: approx. 0,5 l / min, cooling water within 3m from outlet, flexible
hose with 6mm inner diameter supplied.
Stand alone chillers are acceptable, for example Linseis model no. L75/WCU.
4. Bench for STA

Bench for STA must be built in a stable way to insure no vibration and stable
condition for measurements. There should be no interference with heavy machineries
and other type of vibrations.
5
Instrument Description
5. INSTRUMENT DESCRIPTION
5.1. 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. Highly sensitive
optical transducers detect the balance arm displacement. The transducers regulate the
current to the magnetic coils that compensate for the weight changes keeping the
balance arm at a constant zero position. This current is amplified and produces the TGA
signal. The magnetic coils are also used to electronically tare the system.
6
5.2. SPECIFICATIONS
STA PT1600 balance and amplifier
Temperature range: -150 to 1750oC*

Heating rate: 0.1 to 100oC/min. **
Max. Sample weight: (depends on model)
Tare: electronic
Max. Vacuum: 10-5 mbar
Resolution: 0.5/0.1g
Accuracy: + 1% full scale or 10g, whichever is greater
Repeatability: + 0.5% full scale or 10g, whichever is greater
PID control: One or two stage cascade controller

Thermocouples: 6 different thermocouple types
Resolution: 1/20K
Resolution: 0.1s
Temp. Segments: 16 programmable temperature segments
program heating
* Different furnaces
** Different measuring systems
7
5.3. MEASURING SYSTEMS
TG Measuring DSC Measuring DTA Measuring DSC Cp Measuring

System System System System
STA PT1600
Simultaneous Thermal Analyzer
8
5.3.1. Linseis STA and High temperature DSC Measuring Heads
Type Available thermocouple types
DTA
E; K; S; B; C
DSC
E; K; S; B
DSC - Cp
E; K; S; B
9
5.3.2. Type / temperature range / atmospheres
Type Temperature range Atmospheres
Type B (Pt18%/Pt-Rh) RT to 1750C oxidizing

reducing (reduces sensor
lifetime)
inert
vacuum (reduces sensor
lifetime)
Type C (W/W-Rh) RT to 2320C Vacuum
Inert
Not for oxidizing
atmospheres.
Not practical below 400C.
Type E (Chromel / -150 to 700C oxidizing to 500C
Konstantan) reducing (reduces sensor
lifetime)
inert
lifetime)
Type K (Chromel / Alumel) RT to 800C oxidizing to 700C
lifetime)
inert
lifetime)
Type S (Pt10%/Pt-Rh) RT to 1650C oxidizing
lifetime)
inert
lifetime)
10
5.4. FURNACES
The Linseis STA PT1600 can use a large selection of different exchangeable furnaces
listed below.
Depending on the configuration and the required measurement speed, accuracy and
type, the following furnaces can be mounted onto the system.
Type of Furnace L75/264 L75/220 L75/230 L75/240 L75/PT

Temperature
range -150C RT
RT 1000C RT 1400C RT 1600C
(RT = Room 600C 1750C
Temperature)
Cooling medium LN2
Furnace cooling Air Air Air Water
Furnace Inert, Gas,

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
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
5.6. 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
Installation
6. INSTALLATION
6.1. SET UP EQUIPMENT PLACEMENT
The room where the instrument is placed should be free of vibration sources, large
motors, large energizing resistance loads, or capacitor discharges. The room floor should
be stable and not flex when individuals walk around or towards the thermobalance. Place
the thermobalance on a sturdy vibration-free floor with close access to power, cooling
water, and purge gas outlets. The area should be free of drafts and extreme changes in
the room air temperatures.
Place the cabinet on a stable floor out of the high traffic areas.
The Instrument STA PT1600 has to be connected to the PC via the USB cable. The plug
for the USB is indicated on the rear of the instrument.
6.2. 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.
Use only one power outlet (or a power board) for the instrument, the Thyristor power
supply, the computer and other additional Linseis devices if it is possible and permitted.
If this is impossible make sure that the neutral conductor and the ground conductor is
potential-free!
Connect up the control signals first, then the furnace power supply and finally connect
the whole system the mains.
14
Installation
6.3. INSTALLING THE TA-WIN & WIN-STA SOFTWARE
For USB connection
!!!! Before connecting Thermo analytical Devices with your PC, make sure that
the Software installation has been completed!!!!
To perform a correct software installation, follow the points outlined in the appropriate
order, do not leave out any point.
Installation procedure:
1. Place the CD-Rom with the Linseis TAWIN software in the CD-drive.
Normally the installation will now start automatically. In case this does not
happen, start the file setup.exe located on the CD.
2. Follow the instructions displayed on your monitor.
3. After successfully installing the appropriate software for your ordered thermo
analytical device, you should now find the LINSEIS TAWIN software ICONS on
your desktop.
4. Now please switch on your Thermal Analyzer and connect it with the computer via
the USB cable provided from LINSEIS.
5. WINDOWS will tell you that it has found a new hardware device. The displayed
message will indicate that the found device is a Thermal Analyzer.
(The exact Model will be indicated).
6. Windows will now ask how the search for the appropriate driver shall be
performed: automatically or manually. Confirm that the automatic search shall
be performed. Normally Windows will automatically detect and install the driver.
In the event that Windows does not automatically find the correct driver, select
the driver manually. The appropriate driver location is as follows:
C:\tawin\driver
After successfully completing the installation, you can now start to perform
measurements with your Thermal Analyzer.
15
Installation
6.4. INSTALLATION AND CHANGE OF THE MEASURING SYSTEM
6.4.1. Preparation
1. Raise furnace with furnace lift to the upper position.
2. Remove heat shields (if installed).
3. Shut off instrument and computer.
4. Open the device on the left side through loosening the 3 screws.
Screws
5. Open the balance chamber (unlock the screws and remove the cover)
Screws
16
Installation
6.4.2. Disassemble measuring system
1. Loosen the fixing screw (only loosen, do not remove the screw).
2. Take a small screwdriver, snap in the groove below the measuring system and
lever it out. Meanwhile hold the measuring system from the outside.
3. Remove the measuring system upwards and put it in the container.
Measurement system
Groove
End stop
Fixing screw
Balance beam
6.4.3. Assemble measuring system
1. Now insert new measuring system from above into the balance housing. Please
note that the plug of the measuring system has a flat side, which has to fit into
the flat side of the receptacle.
2. When the measuring system locked in place properly, tighten the fixing screw.
3. Place Al2O3 crucibles on the measuring system.
4. Adjust with the knurled screw and additional counterweights on the left side of the
balance beam the balance, so that the balance beam touches just the lower end
stop.
17
Installation
6.4.4. Tare Balance
1. Open screw cap beside the furnace lift.
2. Rough tuning: When device is switched off put weights into the funnel, in order
that the balance beam floats free. To check free movability , touch the funnel or
sample holder slightly, then balance movement slowly die away. If balance
movement stops promtly, the balance beam is not correct tared.
3. Switch on the instrument, but do not start the measurement software.
4. 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.
Alternatively the balance can be tared with the knurled screw and counterweights
in the balance chamber.
5. Remount the cover of the balance housing and tighten the 6 screws and next
remount the left cover with 3 screws.
18
Installation
6.4.5. Correction measurement
1. Start the PC and launch the respective measuring program (Type S, Type K, etc.).
2. Do a correction measurement up to the maximum allowed temperature of

measuring system.
Note:
According to this tutorial the balance is tared for Al2O3 crucibles and a probe weight
(probe material and reference material) about max. 150 mg. For other crucibles or
heavier probes you must repeat the tare procedure.
19
Installation
Manual for change of thermal shield of a cryogenic furnace
1. Remove the platinum cylinder.
2. Remove the thermal shield stack.
20
Installation
3. Fit the flange and fix it with a clamp.
4. Insert the heat shield plates and rotate those with a pair of tweezers (or
something like that) so that the hole becomes minimal.
21
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. Mount the O-ring (metal nose downside) on flange.
22
Installation
7. 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.
8. Make sure that the cryogenic furnace is into the correct position. Bring furnace
carefully to lower position. Please check while lowering, that there isnt contact
between insulation and furnace. Measurement system will be destroyed.
23
Furnace maintanace
7. FURNACE MAINTANACE
7.1. DISMOUNT FURNACE
For dismounting furnace, first raise the furnace lift in the upper position and disconnect
the instrument and the Thyristor power supply from the mains. Then four connections
have to be released as shown in the pictures below. Finally loosen the three fixing screws
and heave the furnace carefully upwards away. Furnace weight amounts roughly 7 kg.
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
Furnace maintanace
7.2. REPLACING THE FURNACE HEATING ELEMENTS
7.2.1. 1400C and 1600 C furnace
Attention: Reparation should only executed by skilled personnel.
1. Switch off the power.

2. Disconnect the power cable from instrument and power supply.
3. Remove the 4 Philips countersunk screws, which securing the top furnace cover.
Carefully lift the cover straight up and set aside.
Countersunk screws
4. Carefully remove the heat insulation parts from the heating element and next to the
power connections. Loosen the electrical connections.
Insulation
Electrical connections
25
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 mustnt 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. 1750C furnace
Hint:
The following example is for the LINSEIS L81/250M MoSi2 furnace. Its temperature range
reaches from RT up to 1750C. 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
Furnace maintanace
1. Disconnect the power connectors.
2. Disconnect the heating element power connectors.

3. Carefully pull out the heating elements.
4. Remove the new heating elements from its package.
5. Place the new heating into the furnace.
6. Reconnect the power connectors.
7. Close the furnace.
8. Connect the furnace power connectors.
29
Furnace maintanace
7.3. CHANGE FURNACE THERMOCOUPLE
Attention: Reparation should only executed by skilled personnel.
1. Disconnect instrument and power supply from mains.

2. Open the furnace and remove the heating element.
3. Disconnect the old thermocouple.
4. Remove the broken thermocouple and insert the new one.
30
Furnace maintanace
5. Connect the thermocouple on the terminal block. Regard the polarity of the
thermocouple. Normally the plus wire is marked with a black mark, and is
connected with the black wire.
6. Remount the heating element. Look to it, that there is no contact between wires
and hot parts.
Very important: After reparation you must check the shown temperature in the
measurement program. Reset the CJR adjustment, and check if there is shown the real
temperature. Start heating with a slow heating rate and check if the temperature rise. If
the temperature doesnt rise, there must a mistake. In this case promptly stop heating.
Cool down the system, and look for troubleshooting.
31
Preparing a measurement
8. PREPARING A MEASUREMENT
Preparing the In thermo analytical investigations, the test

measurement parameters have a significant influence on the
results.
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.
One distinguishes between temperature and enthalpy
calibration.
A new calibration is required any time the instrument
is repaired and when there are significant changes in
the measurement conditions.
Calibration Kit's Calibration kit's for enthalpy/temperature calibration

can be ordered from LINSEIS Messgerte GmbH:
1. DSC/DTA calibration kit (temperature and
enthalpy)
2. DSC/DTA calibration kit (temperature and
enthalpy)
Calibration of the Balance We recommend that the balance be recalibrated

following transport, repairs and considerable changes
in the test parameters (e.g. changing the sample
holder).
32
Preparing the sample When preparing the sample, the effects to be

interpreted and the consistency of the sample must
be considered. Good thermal contact between the
sample and heat-flux sensor is an indispensable
requirement for optimum results.
The methods most frequently used for preparation of
solid and liquid samples are described below.
Powdered solids The sample is evenly distributed in the bottom of the

sample crucible.
Compact solids Compact solids, e.g. rubber or thermoplastic, are cut

into thin slices with a knife, scalpel or razor blade.
For the analysis, 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).
If it is not possible to punch out a suitably sized disc,
the bottom of the crucible is covered with thin slices
of the material.
A sample crucible must always be used. 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 discs should completely cover the
bottom of the crucible.
In order to improve the contact between the sample
and crucible bottom, the lid should be placed on the
crucible, with the convex side down, and sealed.
Fibers The fiber can be cut into small pieces, which are then
spread parallel on the bottom of the crucible.
The fiber is wound around a small rod. The coiled

fiber is then removed from the rod and placed in the
crucible.
A bundle of fibers is wrapped with aluminum foil and

cut at both ends. (The weight of the sample can be
increased with voluminous fiber materials.) The fiber
material with the foil wrapping is then placed in the
crucible.
The significance of the experimental results can be

increased in all cases by adding a drop of silicone oil
(improves the heat transfer).
33
Liquids Depending on the viscosity, liquid samples can be

dropped into the crucible with a thin glass rod, a
micro-pipette or a syringe.
Unstable samples Unstable samples are tested in special pressure-tight

crucibles (optional).
The measuring unit must be recalibrated when
pressure-tight crucibles are used.
Evaporation reactions When investigating evaporation reactions, e.g.

evaporation of water of crystallization, a closed
crucible with a small hole in the center of the lid
should be used.
The hole should be punched prior to sealing to avoid
deformation of the crucible later.
Measurements in defined For measurements in defined atmospheres, a needle

atmospheres should be used to pierce one to five holes in the lid of
the crucible.
Select the sample crucible Select the crucible depending on:

sample carrier system
sample material
purge gas atmosphere
34
Selection and preparation of Do not touch the crucibles by hand. Use

platinum crucibles tweezers!
Always heat up the crucible to the final
working temperature before the first
measurement.
After treating the crucible with acids or
solvents, clean it with distilled water.
Dry the crucible and heat it up again to final
working temperature.
Place PtRh-crucibles with the crucible rim
(facing downwards) on to the sensor plate
before first heating. In this way the crucibles
do not stick to the sensor plate.
PtRh-crucibles also tend to stick to the sensor
plate of the sample holder when heated above
1000C.
Loosen the crucibles carefully (also on
reference side) after every single run.
Lift up the crucibles and replace them.
Take care that the lids do not stick to the
crucible rim.
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.
Heat up a small amount of sample on a piece
of Pt-foil in a separate laboratory furnace.
Traces of reaction will be visible on the surface
of the foil. This indicates that PtRh-crucibles
should not be used.
If samples cannot be measured in PtRh-
crucibles, use Al2O3 crucibles.
Cover the crucibles with a thin layer of
platinum paint on the outer surface of wall,
bottom and lid to improve the radiation
behavior.
Heat up the crucible to final working
temperature to burn out the solvents before
using the crucibles on DSC.
This treatment will have a positive effect on
the Cp-data compared to those measured in
Al2O3-crucibles, especially in the temperature
range above 900C.
Weigh the sample Weigh the sample with an analytical balance.

Accuracy: 0.1 mg or better
Clean the crucible and lid with acetone or

alcohol prior to use.
When filling the crucible, no sample material
may remain on the edge of the crucible.
35
Compatibility of crucible materials and some substances
9. COMPATIBILITY OF CRUCIBLE MATERIALS AND SOME

SUBSTANCES
Measuring in metal crucibles requires special care. Corrosion of the crucible material may
go to destruction of sample carrier and sensor.
substances
Ag, silver
Au, gold
aluminu
Pb, lead
Zn, zinc
gallium
Li2SO4
indium
C5H10
Sn, tin
water
xH2O
H2O,
Ga,
In,
Al,
m
crucible material
Ag, silver
Al, aluminum
Al, oxidized
Al2O3, corundum
Au, gold
BN, bornitride
C, graphite
Fe, iron
fine steel
Mo, molybdenum
Ni, nickel
Pt, platinum
silicate glass
SiO2, fused silica
Ta, tantalum
W, tungsten
No solvability, no variation on the melting temperature

Change of melting temperature, molten mass dissolves the crucible material
Crucible will melt
Change of melting temperature may be ignored (partial solution process)
Compatibility unknown
Combination isnt possible
36
Selection of the gas Atmosphere
10. 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, resolution in the g 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 weighing system - the heart of the STA PT1600 - must be open towards the sample
space. The protective gas (pure, inert, and dry) should continuously purge through the
weighing system into the sample space.
How to create a particularly clean gas atmosphere:
Use a vacuum pump (a diaphragm pump is sufficient) for evacuation. Prior to starting the
measurement the measuring system can be repeatedly evacuated and refilled with purge
gas.
Measurements under static conditions
In case of static measurements there is no protection of the weighing system by a

continuous inert gas flow. This has effects on the function of the weighing system.
In the most positive case only air humidity deposits on the surface of the weighing
system, this deposit impairs the stability behavior of the STA PT1600.
37
Selection of the gas Atmosphere
Higher problems arise, if aggressive gases reach the weighing system. This can lead to a
damage of the weighing system:
1. Measurements in static gas atmosphere are only admitted, if the sample does not
release aggressive or condensable reaction products.
The operator of the instrument is personally responsible that samples releasing
aggressive, reactive or condensable reaction products are not measured under
static conditions.
Therefore static gas operation should be an exceptional case.
2. The weighing system must be protected for all operation modes (static, dynamic).
a) When changing the samples or during a measurement pause keep open the
system only as long as really necessary.
Use a protective gas for the weighing system (dry, inert, pure), being not lighter
than air. In this way you minimize the penetration of air humidity into the STA
PT1600.
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.
If nevertheless you want to do static measurements:
Take care that the weighing system is protected by an inert gas.
Measurements with closed outlet valve lead to a pressure increase inside the system. The
measuring results are falsified (drift).
Gas flow (vacuum) inside the STA PT1600
Measurements under vacuum - what should be considered!

In case of measurements under vacuum a protection of the weighing system by an inert
gas is not possible.
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.
The operator of the instrument is personally responsible (for example by suitable

pretests) that samples releasing aggressive, reactive or condensable reaction products
are not measured under vacuum conditions.
38
Gases and their limitations
11. 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.
The following is a selection of purge gases including their limiting properties. The list
makes no claim on being complete.
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, but sample reactions are
possible in the high temperature range.
Air Oxidizing
possible. Application is possible above room temperature
(maximum application temperature is determined by furnace
material, sample holder, thermocouple).
Oxygen (O2) Increases flammability
(must not come into contact with fats or oils)
possible. Application is possible above room temperature
(maximum application temperature is determined by furnace
material, sample holder, thermocouple).
Carbon dioxide (CO2) Non-toxic
(MAK- value 5000 vpm),
Non-flammable
Application is possible above room temperature.
Hydrogen (H2) Flammable,
Danger of explosion when in contact with oxygen
The use is not allowed for safety reasons.
Ammonia (NH3) Toxic
(MAK value 50 vpm),
Flammable
Danger of explosion when in contact with oxygen.
Corrosion of seals is possible.
Carbon monoxide (CO) Toxic
(MAK-Wert 10 vpm),
Flammable
Corrosive
Hydrogen sulphide Toxic
(H2S) (MAK value 10 vpm),
Flammable, corrosive
39
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. However, 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 manufacturers of gases and gas mixtures can
provide the required information.
Gas Properties
Chlor (Cl2) Very toxic
(MAK value 5 vpm),
Non-flammable, corrosive, caustic
Hydrogen chloride Toxic
(HCl) (MAK value 5 vpm),
Non-flammable, corrosive, caustic
Sulphur dioxide Toxic
(SO2) (MAK value 2 vpm), Non-flammable, corrosive
Fluor (F2) Very toxic
(MAK value 0.1 vpm),
Encourages burning, corrosive, caustic
Hydrogen fluoride Very toxic
(HF) (MAK value 3 vpm),
Very caustic, corrosive
Gaseous Can form explosive gas mixtures with air
hydrocarbon The use is not allowed for safety reasons.
MAK values 1994

MAK-value (Maximum workspace concentration)
We recommend that the expelled purge gas be passed into a suitable exhaust hood. The
measuring part must be sufficiently purged with inert gas once the measurement is
finished.
40
GAS FLOW IN THERMOGRAVIMETRIC EXPERIMENTS
12. 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.
Thermogravimetry is in most cases a dynamic process, in that weight changes are

recorded against precisely controlled heating rates that produce a continuously changing
temperature. Since the sample evolves a gaseous product as the temperature increases,
the concentration of the ambient static atmosphere around the sample will change. As
the rate of decomposition increases, the concentration of the evolved products will
increase. If the reaction is reversible, the reaction rate could decrease. Convection
currents in the balance, could cause a continuously change of the gas concentration
around the sample. Results would not be reproducible. Beside from concentration
considerations, no gas flow produces uneven temperature gradients in the system and
poor temperature repeatability. Back diffusion of air will occur, if the system remains
inert without gas flow. If the system is sealed to avoid back diffusion, pressure build up
will cause buoyancy changes and disturb the weight readings.
Reaction gas can be an inert gas, such as nitrogen or argon, if no reaction within the
sample is the objective. Explosive gases, such as hydrogen or oxygen, should be used
with extreme caution. Generally a blend of a low percentage of hydrogen in an inert gas
is a relatively safe procedure. Air is a safe substitute for oxygen. All corrosive gases
should be used with extreme care. Reaction gases should flow at 5 - 7 l/h, but no slower
than 1 l/h and no faster than 10 l/h. Reaction gas, as all gases, should be at low inlet
pressure (approx. 5-10 psi) to prevent gas from rushing into the system. This rush will
produce instability and could possibly blow sample out of the crucible. This particularly
occurs, when switching from vacuum to gas flow. Precise rotameter control is
recommended in this case.
41
Linseis STA Measurement Software
13. LINSEIS STA MEASUREMENT SOFTWARE
13.1. TYPE OF MEASUREMENT
Before starting an STA measurement the type of measurement must be defined. It can
be either a TG measurement, DTA measurement or one with both DTA/TG. You must also
decide if you want to measure a sample or a zero line. The present type of measurement
is displayed in the title of the program window.
13.1.1. TG Measurement
To start a TG measurement, select Data Acquisition - Type - Sample TG for a sample

measurement.
For a zero line measurement, select Data Acquisition - Type - Zero Line TG.
13.1.2. DTA/HDSC Measurement
Depending on how your system is equipped, you can choose between a DTA or a HDSC
measurement. The difference lies in the measuring head.
To start a DTA/HDSC measurement, select Data Acquisition - Type - Sample DTA (or
HDSC) for a sample measurement. For a zero line measurement, select Data
Acquisition - Type - Zero Line DTA (or HDSC).
13.1.3. TG+DTA/HDSC Measurement
To start a TG and a DTA/HDSC measurement simultaneously, select "Data Acquisition-

Type - Sample" to DTA for a sample measurement. To start a zero line measurement,
select Data Acquisition - Type - Zero Line TG+DTA.
42
13.2. SETUP DATA ACQUISITION
After selecting Data Acquisition - Settings... from the menu bar, a dialog window will be
displayed. 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. The following pictures show examples of
the various dialog windows for different types of measurements,
13.2.1. Example TG Measurement
13.2.2. Example DTA Measurement
43
13.2.3. Example TG DTA Measurement
13.2.4. Description of the Input Parameter
Following is a list and description of all the parameters, even when they are not shown in
all the dialog windows at the same time.
User: This field is for the name of the person, who is doing the measurement. The name
of the user 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.
The name of the laboratory is also displayed in the comment field of the data
evaluation program.
Atmosphere: This field is for the gas atmosphere that is being used in the
measurement. The name of the gas is also displayed in the comment field of the
data evaluation program.
Flow Rate: This field is for the flow rate of the gas. It is displayed together with the
name of the gas in the comment field of the data evaluation program.
Comment: This field is for a short comment about the measurement. It is also displayed
in the comment field of the data evaluation program.
44
Sample File: This input is for the name of the sample tile where measured data is
stored. It is also possible to choose an existent file through the use the symbol on
the right side of this box. The sample files for TO measurements always have the file
extension .GPR". For DTA-HDSC measurements the file extension is ".TPR". The
program will, automatically add the file extensions when they are missing. In a zero
line measurement this field is deactivated. No filename can be entered.
Zero File: This field is for the name of the zero file used in the measurement. In a
sample measurement this entry can be used for later information during a data
evaluation. This entry defines the name of the file where measured data is stored in
a zero Fine measurement. The zero files in TG measurements always have the file
extension ".GNL", in DTA/HDSC measurements the extension is ".TPR". This ending
is automatically added when missing.
Sample: This input field is for a short description of the sample. This description is also
displayed in the comment field of the data evaluation program.
Sample Weight: This input field is for the weight of the sample used in the
measurement. In case the sample weight contains a fraction, it has to be entered
with decimal point (e.g. 10.3). The sample weight is also displayed in the comment
field of the data evaluation program.
Reference: This field is for the reference material in a DTA measurement. It is also
displayed in the comment field of the data evaluation program.
Reference Weight: This field is for the weight of the reference material used in the OTA
measurement. This weight is also displayed in the comment field of the data
evaluation program.
Sampling Interval: This value sets the time intervals in which data is measured and
stored. The smaller this value is, the shorter the time intervals and the higher the
accuracy, especially in measurements with fast changing signals; but on the other
hand, the faster sampling causes large; data files that need a longer time for the
evaluation and more space on the hard disc.
Duration: This field is for the duration of the data acquisition of the measurement. This
duration is independent from the duration of the controller program. It is important,
that these two durations are not mixed up. This time constant controls the time that
data will be stored onto the hard disc. Together with the end temperature, the
duration creates the switch off conditions for the data acquisition. The acquisition
will stop after one of the parameters has reached the entered value (see also End
Temp.).
End Temp.: This field is for the temperature that ends the acquisition. The shut off is
independent from the duration of the controller program (see also Duration).
Together with the duration, the end temperature creates the switch off conditions
for the data acquisition. The acquisition will be slopped after one of the parameters
has reached the entered value.
Range: The range must be chosen from a list of values that depend on the type of
measurement and instrument. This entry is very important, because all the initial
data will be tabulated and stored with it.
In other words: Entering a wrong value for the range causes all measured data to be
stored and displayed incorrectly.
45
13.3. PROGRAM CONTROLLER
The programming of the controller sets the temperature stages of a measurement. The
pre-heat and cool-down periods of a measurement, as well as the regulator behavior are
defined here.
13.3.1. Controller Set Values
13.3.2. 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. Up to 16 different cycles can be programmed. Each will be
processed one after the other. 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. (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. With this feature
it is defined when & which gas shall be used
Number of cycles Defines how often the program shall be repeated
46
13.3.3. Graphic Display
This feature displays on screen, the programmed temperature profile of a measurement

as a function over time. This gives an exceptional optical control and the temperature
profile can be changed if necessary. A special feature is the choice of the starting
temperature. It can be either the actual sample temperature or any other temperature.
The starting temperature must be entered manually.
It is useful to use a different temperature than the actual sample temperature when
creating a new temperature profile, 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.
13.3.4. Store Controller Set Values
If a temperature profile should be needed at a later time for other measurements, it can
be stored by selecting Store" on the screen and entering a name.
13.3.5. Load Controller Set Values
To load a temperature profile the field Load must be selected. Another dialog window
will appear on screen, with stored profiles listed. From this selection you can choose and
activate the desired profile.
13.3.6. 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
13.3.7. Display Current Values
It may be interesting during a measurement to get a view of the current temperature

and control parameter of the system. This is possible by choosing the menu selection
Controller - Current Values...
The following parameters will be displayed:
Temperature Profile: Oven Parameters:
- Cycle number - Target Temp.

- Segment number - Current Temp.
- Heating Rate - Maximum Temp.
- Target Temp. - Thermocouple Type
- Dwell Time
- Remaining Time
- Relay conditions
Sample Parameters: Power Output:
- Target Temp. - State (on/off)

- Current Temp.
- Reference Temp.
- Thermocouple Type
48
13.3.8. Uncontrolled Preheating
The function of uncontrolled preheating is used, when a sample temperature can only be
measured after a certain starting temperature (e.g. with a radiation pyrometer from
400C). The normal controller program would fail in this case because the temperature,
which is necessary for the control, is below the starting temperature and cannot be
determined.
The Parameters of the uncontrolled preheating are displayed as follows:
Target Temp. (in CC)

Max. Power Output (in %)
Ascent (in %/min)
After the target temperature is reached, the uncontrolled preheating is stopped and the
normal controller program
13.3.9. Adjust Cold Junction Reference
The controller board uses a built in reference cold junction to compensate for thermal
voltages in the input connectors. Adjustment of the sample thermocouple can be done
with the cold junction reference. The thermocouple must be inserted into a known
temperature (e.g. CC in ice water).
An adjustment dialog window can be displayed on the screen with Controller - Adjust
CJR...
Here, the actual temperature of the thermocouple is displayed, and the user can now
enter the nominal sample temperature, which was assumed to be measured (e.g. 0C).
By using the field Adjust, the adjustment is made. The accuracy of the adjustment cap
is increased by repeating this step a few times.
If by accident the thermocouple has been adjusted to an incorrect temperature, then the
adjustment can be reset by using the field "Reset" and then started again.
Once the calibration of the sample thermocouple is made the correction value will be
stored, and used for future measurements, even if the program is turned off.
49
13.3.10. PID-Parameters
The PID-Parameters directly change the controlling behavior of the electronic

temperature controller and have to be selected carefully.
The controller works as a cascade controller. It will process the sample as well as the
furnace temperature as controlling parameters.
13.3.10.1. Parameter Definition
The PID-parameters have to be entered as separate P-, I- and D- fractions for controller
1 (sample temperature) as well as controller 2 (furnace temperature). The value range
for each parameter can be between 0 and 32767. The defaults are made according to
known values of Linseis GmbH.
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, then the current value
used for the control loop is only the furnace temperature.
13.3.10.2. Store Parameters
If various sets of parameters should be available for different measurements, they can be
stored after selecting Store and recalled for later measurements.
13.3.10.3. 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.
13.3.10.4. Set Defaults
Sometimes it can happen that unfavorable parameters were set for the controller and the
proper parameters are lost. In this case, we recommend choosing the defaults and
changing the parameters from there until the desired parameters are selected. The
defaults can be entered through selecting the field Reset.
50
13.4. START AND STOP MEASUREMENT
To start and stop a measurement there are two fields marked Start and Stop in the
main menu. After selecting one of these options a dialog window appears on the screen
showing the user his choices. In particular the data acquisition and the controller
program can be started while a measurement is in progress; the lower side of the screen
displays the following important information about the measurement:
- Number of stored data

- Duration of the measurement
- Active controller program
- Active data acquisition TG
- Active data acquisition DTA/HDSC
13.5. REAL-TIME GRAPHIC
The real-time graphic displays the data during a measurement. 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.
The time axis always has, at the start, a scale from 0-10 mm. The y-axis is set at the
start to 10% of the selected range.
The graphic display is equipped with an automatic re-scaling function. This means, that
after one of the measured values (or of the passed by time) leaves the selected range, a
new range will be calculated and displayed on screen which includes the new data. This
procedure can repeat itself in a measurement. The graphic display of the measured
values always starts with the beginning of the measurement. This means that the whole
measurement is visible on screen.
Below the graphic display the measured parameters are shown as digital values.
The graphic display of the measured data remains on the screen after a measurement
until a new measurement is started, or the menu selection Options - Clear Graphic is
chosen to erase the display.
51
13.6. BALANCE SETUP
13.6.1. Zero Adjustment
To adjust the zero point of the thermal balance select the menu Options - Setup Scales.
Depending on the instrument, the zero point can be adjusted either manually or
automatically.
For the adjustment, two gauges are displayed on a dialog window and are used for the
adjustment.
The left gauge shows the total actual range from -100%to +100%. The right gauge
displays the offset from the selected zero point. The zero point does not have to be in the
middle of the physical range, it can be shifted to get a asymmetric measurement.
13.6.2. Zero Point Definition
To define a zero point in an instrument range, the field Zero Point must be activated.
A dialog window will appear on the screen. The user can decide if the zero point must be
in the middle of the range, or if it should be shifted asymmetrical. If asymmetrical, the
position must be entered in % of the actual range.
The advantage of a asymmetric zero point shift results in a wider range on one side. This
requires knowledge of the expansion behavior of the sample to avoid an over-range
situation during the measurement.
13.6.3. Manual Adjustment
The manual adjustment is always used when the instrument has no automatic zero
adjustment. After the position of the zero point is defined (see last section), 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, and the digital display on both gauges
show exactly the %-value of the zero point position.
To exit the zero point adjustment select "Close in the dialog window.
52
13.6.4. Automatic Adjustment
After the position the zero point is defined (see section zero point definition), the
automatic adjustment will be started when selecting the field "Automatic Zero
Adjustment. Then the field disappears and a remark that the zero point of the system is
now adjusting is displayed. After the adjustment is finished, the field appears again and
the dialog window can be left by selecting Close on the screen.
13.7. RELAYS
The controller in the Instrument is equipped with relay outputs. These outputs may
control valves for gas or cooling water supply.
The condition of these outputs can be defined either in the controller set values for every
cycle number (separate for every cycle) or. The active condition is displayed with a little
mark in front of the relay number.
The menu points for the outputs are named by default Relays1. ...Relays4. These names
can be changed to get a more accurate statement, e.g. into Gas Inlet. To do this a few
entries have to be made into the file DIL.INI of the measurement program. In the
section called [RELAYS] it is possible to define under the relay numbers 1-4 the names of
the relay outputs. The character following the &-character is used as a fast-choice with
the keyboard. For instance:
[RELAYS]
1=Relay&1
2=Relay&2
3=&Gas Inlet
4=Relay&4
53
PERFORMING A ZERO BASELINE CURVE
14. PERFORMING A ZERO BASELINE CURVE
In order to perform a zero baseline curve please follow the outlined instructions carefully.
Please do not miss out any points in order to gain a satisfying result and to avoid damage
to the system.
1. Switch the balance to ON
2. Lift the furnace automatically by pressing the lift button located on the front of the
instrument.
Lift button
3. Carefully remove the sample crucible.
Clean the crucible or replace it if the old sample can not be cleaned from the
crucible.
Inspect the Al2O3 reference material. If it is contaminated replace with new Al2O3.
Place equal amounts of Al2O3 in the reference and sample crucibles.
The normal amount is 1/3 full (max. 150 mg for sample and reference).
Note: Sample is right, reference is left.
54
4. Start the software STA data collection software using the desktop icon
Desk top data collection icon
5. Now select in the Software
- DATA ACQUISITION
- TYPE, ZERO LINE TG+DTA
- DATA ACQUISITION
- SETTINGS
55
7. Enter the data collection information:
The data collection termination is control by the Duration and End Temp. value.
Whichever value reaches the stop criteria first, will result in the data collection
being terminated. Always select a time or temperature higher than the final data
point needed. Click OK to complete settings.
56
- CONTROLLER
- TEMPERATURE PROFILE
9. Enter the desired heating rate to the maximum temperature.
Precaution: Do not exceed the heating rate of your selected furnace to prevent
damage of the heating element!
57
- CONTROLLER
- CURRENT VALUES
11. Check the current furnace and sample temperature.
Precaution: The temperature must be a room temperature before starting the

system.
Furnace
Sample
temp.
58
- OPTIONS
- SETUP SCALES,
13. Click to TARA ADJUSTMENT to calibrate the Tara
- OPTIONS
- BASELINE CORRECTION
- SELECT CORRECTION
59
15. Check if ACTUAL CORRECTION is NONE
16. Start the measurement by selecting Start

Check data collection and controller.
Click OK to start the measurement
17. Monitor the run using the real time graphic and current values windows.
18. 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.
19. Create a new baseline correction characteristic
Check if the zero baseline is repeatable for the used measuring system.
Choose OPTIONS
- NEW CORRECTION
Enter an expressive description and choose a zero line file.
60
PERFORMING A SAMPLE CURVE
15. PERFORMING A SAMPLE CURVE
1. Switch the balance to ON.

2. Lift the furnace automatically by pressing the lift button located on the front of the
instrument.
Lift button
3. Carefully remove the sample crucible.
Clean the crucible or replace it if the old sample can not be cleaned from the
crucible.
Inspect the Al2O3 reference material. If it is contaminated replace with new Al2O3.
Place Al2O3 in the reference and your sample in the sample crucibles.
Weigh the reference and the sample before.
The normal amount is 1/3 full (max. 150 mg for sample and reference).
Close the plug-in on the furnace top.
Note: Sample is right, reference is left.
61
4. Start the STA measurement software using the desktop icon.
5. Select in the Software
- DATA ACQUISITION
- TYPE
- ZERO LINE TG+DTA
- OPTIONS
- SELECT CORRECTION
62
7. Select for the mounted measuring system the correct baseline correction.
- DATA ACQUISITION
- SETTINGS
63
9. Enter the data collection information
Text fields:
Operator, Atmosphere,
Laboratory,
Flow Rate,
Sample and Reference name,
Comments
TG Sample File names: *.GPR extension will be automatically inserted.

DTA Sample File name: *.TPR extension will be automatically inserted.
Enter the sample weight.
The data acquisition termination is determined by the Duration OR End Temp. value.
Whichever value first reaches the stop criteria will result in the data collection being
terminated. Always select a time or temperature higher than the final data point needed.
Click OK to complete settings.
64
- CONTROLLER
- TEMPERATURE PROFILE
11. Enter the desired heating rate to the maximum temperature.
65
- CONTROLLER
- CURRENT VALUES
13. Check the current furnace and sample temperature.
Precaution: The temperature must be at room temperature before starting the

system.
Furnace
Temperatur
Sample
e
temp.
66
- OPTIONS
- SETUP SCALES
15. Click to TARA ADJUSTMENT to calibrate the Tara.
16. Start the measurement by selecting Start, Check data collection and controller.
Click OK to start the measurement. Monitor the run using the real time graphic
and current values windows.
17. 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.
67
Linseis STA Evaluation Software
16. LINSEIS STA EVALUATION SOFTWARE
Software
All LINSEIS thermo analytical instruments are PC controlled. The individual software
modules exclusively run under Microsoft Windows operating systems. The complete
software consists of 3 modules: temperature control, data acquisition and data
evaluation. The 32 bit software incorporates all essential features for measurement
preparation, execution, and evaluation of a Thermogravimetric measurement. Thanks to
our specialists and application experts, LINSEIS was able to develop comprehensive easy
to understand user friendly application software.
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, TMA, DIL, etc.)
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
16.1. INTRODUCTION
The present Program module "Thermal Gravimetric Evaluation" is part of the program
package "Thermal Analysis. It is designed specifically for the evaluation of TG values
with the Linseis thermal balances: L81/I, L81/II, STA PT1000 and STA PT1600 which are
controlled trough the Microsoft Windows version of the STA measurement program. It
also includes a convert function of older data formats of the STA DOS version.
16.1.1. Minimum Hardware + Software Requirements
State of the art PC

VGA screen
Mouse
MS-Windows operating system
MS-Windows XP etc.
16.1.2. Recommended Equipment
Windows supported printer or plotter or both, for table and trace printout.
The above listed hardware + software requirements are the minimum. For
efficient operation, 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. If you are new to the Windows system, please refer to the manuals.
It is also required, that the user becomes familiar with all the functions of the TG
evaluation program. The operation of the evaluation program is described in
detail in the manual Display and Evaluation of Measured Data.
16.1.3. Evaluation of Measurements
The ability of displaying the results of one or more measurements that are connected is
called evaluation. All traces and additional information is going to be displayed in an
evaluation window, called evaluation.
69
16.2. START NEW EVALUATION
For every data evaluation an evaluation window has to be used, where the measured
data can be displayed as a trace. To start a new evaluation, you have to choose FILE -
NEW
The File New dialog box is now displayed and the user is being asked to name this
evaluation. This name is used to characterize the evaluation and should be used with an
ending that characterizes the file.
For the name of the file only eight characters are allowed.
The default is NONAME. Added to the name comes a file extension for configuration files
(standardized .CFG).
70
16.2.1. Save Evaluation
To save an existing evaluation you have to choose FILE - SAVE, and the program
saves the evaluation with its current name.
To save a new, unnamed evaluation you have to choose FILE - SAVE AS.... After that
a dialog box will appear, and the user is asked to name the evaluation.
16.2.2. Open Existing Evaluation
Once an evaluation is saved, you can open it with the command FILE - OPEN. And the
traces, legends, etc. will be restored, as far as the matching data files were not deleted
or overwritten.
In case the evaluation program can not find the data file, which was entered as a data
source for a trace definition, you have the following choices:
1. You can enter a new directory, in case the file still exists, but has been copied,
and repeat to load it. The measured curve will then be created in the new sub
directory.
2. In case the referring file does not exist anymore, you can ignore the last
mentioned hint.
The program will go on to load the evaluation without the missing trace.
3. You can stop the evaluation, if you think something is wrong.
16.2.3. Various Evaluations Simultaneously
It is possible to work in different windows on more than one evaluation at the same time.
To do so you have to load more evaluations, or create new ones. The windows, which will
open up, can be changed in their size and can be arranged freely.
Hint: The menu bars as well as the status bar are displayed only once.
All the actions and information relate to the actual window.
71
16.2.4. Arrange Evaluation Windows
The evaluation windows can be arranged automatically by MS-Windows. To arrange the

windows you have to select WINDOW: on the menu bar. Then the windows can be
arranged next to each other (command TILE) or on top of each other (command
CASCADE). In addition windows can be rearranged when they are displayed as icons.
(Command ARRANGE ICONS).
16.2.5. Change of Active Evaluation Windows
The change of the actual evaluation window can either be done through selecting the
requested window with the mouse, or through selecting the evaluation name in the menu
FILE. The last mentioned is useful, when the requested window can not be selected
because it is hidden by other windows.
72
16.3. TRACES IN THE EVALUATION
In a single evaluation window you can load various traces. They will be displayed on top
of each other and in different colors.
16.3.1. Defaults for Traces
In the menu select TRACE. DEFAULTS... you can set the defaults for the parameters,
which should be used as standard settings when loading a new trace.
This makes it possible to pre-select certain ways of scaling or displaying, which are
needed for the co-ordinate axes. This way they do not have to be adjusted for every new
trace.
16.3.2. Add Traces
To add another trace to an evaluation you have to select FILE - LOAD DATA.... A file
option menu will appear on the screen.
Besides the standard boxes of the windows-file selection system a combination field
exists, where the type of the files can be entered which are displayed in the file box.
If a file is selected whose type fits the binary data format of the evaluation program it is
immediately used in the evaluation. In case the type of the file does not fit the format,
then it has to be imported (which means it has to be transformed). The program
recognizes automatically by the file ending which import filter needs to be used.
Depending on the type of source file it is possible to enter various parameters during the
import. When a file was selected where the program does not recognize the ending; a
dialog box appears on the screen, asking the user how the program should proceed with
the file. You have now to select, if the file should be loaded directly, or if it needs to be
imported and with which filter.
Another entry you can make now is to save the (until now unknown) file extension, to be
able to use more files with extensions of the same type later on.
Hint: All the files with measured values have always exact defined extensions,
because they were created through certain types of measurements or
instruments. To get more information about this subject, which files have to
be imported and which files can be loaded directly, please refer to the
additional chapters about the specific types of measurement or instruments,
where the endings and the meanings of the individual files are explained in
detail.
16.3.3. 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.
This trace name creates a trace reference to the applied labels and the axis display.
You can change the actual trace by selecting the arrow on the right side of the name.
That opens up a box with a list of all available traces, where you can select the requested
one with the mouse.
Hint: When you select a trace that is hidden in the moment, then it will be restored
on the screen.
73
16.3.4. Select Trace Display
After selecting TRACE - CHANGE... a dialog box appears, where all the parameters for
the trace display can be seen.
They include: - Global trace parameter: trace color, line type

- Ranges for X and Y: margins of the display
- Axis parameters: visible, position, color, etc.
16.3.5. Delete Traces
With TRACE - DELETE... one or more traces can be deleted.
Hint: Deleting the trace and the stored parameters (labeling, lines, etc.) will result
in a complete loss of the trace. You should decide, if you really want to delete
or only hide the trace (make it invisible).
16.3.6. Hide and Restore Traces
The menu selection TRACE - HIDE... and TRACE - RESTORE... are only valid for
the present display of the traces. Hereby nothing will be deleted, only the trace with its
matching axis and labeling is drawn or is not drawn. The present condition can also be
changed by selecting TRACE - CHANGE.. - GLOBAL TRACE PARAMETER - TRACE
VISIBLE.
16.3.7. Hide and Restore Trace Names
For every trace, which is displayed in the evaluation, a trace name is created in the color
of the trace, and is displayed together with the trace on the screen.
In case a lot of traces are displayed at the same time, the amount of the labeling can be
disturbing. To avoid this, it is possible to hide the trace names temporarily (they are not
deleted!).
To do so, you have to select in the menu bar OPTIONS - TRACE NAME.
The condition between visible/invisible is changed every time you select TRACE NAME.
When the name is visible, a little check mark appears on the left side of TRACE NAME.
Hint: In case you want to delete the whole trace name, please go to section 6.3.
(Change and Delete Single Labeling) and proceed as described.
74
16.4. EVALUATION ICON
16.4.1. Function Groups
This Icon defines the type of data that can be evaluated. Since the program performs
evaluations for all Linseis Thermal Analyzes, the type of instrument providing the
measuring data has to be selected once.
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.
developed for customers.
The selected Evaluation type is displayed in the line following the Function Group Icon.
75
16.4.2. Temperature profile Icon
This box provides information concerning the chosen temperature profile during the
measurement.
The example to the left shows:
Heat up: 10K/min up to 1465C

Cool down: 30K/min down to 700C
76
16.5. SUMMERY OF FUNCTIONS
16.5.1. Correction Procedure
A successful evaluation of raw data requires a correction because of errors, which will
occur during a measurement and resulting noise of the temperature signal.
Incorrect data will not be accented by the program in most steps of the evaluation.
The zero correction and the smoothing of the temperature signal will be described in the
following two sections.
16.5.1.1. Zero Correction
A measurement without a sample creates a signal that will show only the expansion of
the system itself (zero curve). To avoid this error, the zero curve must be subtracted
from the sample curve (measurement with sample). Different zero curves may be
applied, depending on the parameters.
When the change in mass is moderately huh, the zero curve can be neglected and no
zero correction is applied.
16.5.1.2. X Axis Smoothing
The smoothing of the temperature signal (x axis smoothing) requires a steadily

increasing or decreasing temperature signal. In case the signal can not be corrected over
temperature, it must be corrected over time.
16.5.1.3. Y Axis Smoothing
The smoothing of the y axis is performed independent from the x axis smoothing. The y
axis smoothing is important to calculate the derivation.
16.5.1.4. Derivation
It is possible to calculate a derivative of measured curves over time or over temperature

(1st or 2nd derivation).
The algorithm uses a spline function to calculate the derivation.
77
16.5.1.5. Relative Change in Mass
The relative change in mass can be calculated with:
M k
Mrel (k) = * 100 (where k=1.....n)
M k
for every point k.

M0 is the mass of the sample at room temperature. Mk is the change of mass at the
temperature tk. The unit is given in 1%.
16.5.1.6. Mass calculation
The following described procedures are interactive functional for every trace section. The
results are entered as labels into the graphic, so they can be used for a hard copy. In
case you want the results in a printout as a tabulated format, the program offers a
protocol option.
The number of calibrations per curve is practically infinite.
16.5.1.7. Change in Mass
The total change in mass for a marked section is calculated and entered into the graphic
as a label. An optional calculation is the abscissa difference.
The entry into the protocol includes the start and end temperature as well as the relative
and absolute change in mass.
A negative change in mass marks a weight loss.
16.5.1.8. 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. An
optional function is the display of the abscissa. The entry into the protocol for this point
includes the temperature and the relative and absolute change in mass over time.
The ascent calculation is done with a two point differentiation which needs a smoothed
trace.
16.5.1.9. Reaction Stage
To mark a reaction stage, a calculation of the intersections of two tangents on the trace
is needed. The two tangents must be before and after the reaction together with the
turning tangent in the point of the largest ascent. The user enters the position of a
tangent through two points. The tangents are calculated through linear regression and
they are extrapolated with the intersections of the turning tangent.
In the graphic are the two tangents, the turning tangent as well as the coordinates of the
intersection labeled (abscissa display optional).
The entry into the protocol includes the temperature of the intersections as well as the
relative and absolute mass difference between both points.
The ascent calculation is done with a two point differentiation which needs a smoothed
trace.
78
16.5.2. Curve Arithmetic
The following section describes two ways to work with traces. The arithmetic operation of
traces as well as the mean curve.
16.5.2.1. Arithmetic Operation

Several different operations can be applied to correct data files. All traces must have
identical units for X and Y axis.
One trace operations
constant offset
constant factor
reflect through X axis
Two and more traces operations

addition
subtraction
multiplication
division
16.5.2.2. 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). A
confidence interval is also calculated for the mean curve (means for every single data
point).
Usually only a few traces are in use, so that a diffusion function (Student or t diffusion)
for correction must be applied. With the Student or t diffusion a clearly wider confidential
interval can be calculated (when compared to the Gauss or the normal diffusion).
For the sample range of n>30 is the difference between the Student and the Gauss
diffusion negligible (where n<30).
The following equations are given:
The factor z is the so called standardization of the t diffusion. This factor is listed for a
variety of error possibilities (in this program package for 95%, 99% and 99.9% statistical
confidence). The file, created when calculating the mean curve, includes information
about the confidence interval as well as values for its calculation. For further editing of a
mean curve, the curve must be converted into an editing file.
A special situation is the mean of a zero curve. Because of the existing noise, the zero
curve must be smoothed first, which is done automatically with the calculation of the
mean. Then the resulting mean curve can be converted back into a zero curve.
Important:
Zero curves can only be connected with each other and not with sample or edited traces.
79
16.5.3. Creation of a Collection File
Every step of an evaluation needs its own data file (see section Data Structures). For
this reason it is appropriate to collect these files in a collection file. This file holds,
besides the columns of time and temperature, the V columns for various traces. All traces
must be from one evaluation and will be synchronized over the X axis grid of the first
selected trace. In case a trace is added, longer than the first, it will be cut. In the
opposite case, non existing points will be marked as empty entries.
A collection file can be extended by adding new traces, as long as they are from the
same evaluation.
In case you add a new trace with a name that already exists, the program will ask you if
you want to overwrite or add the trace.
The collection file exists as a binary data file. It can be convened with the ASCII export
filter into an easy readable form.
The loading of a collection file happens automatically through a specific import filter. It
creates new files considering empty entries.
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16.6. PROGRAM DESCRIPTION
16.6.1. Tool box
1 2 3 4 5 6 7 8 9 10 11
12 13
1. This function field is used to display and to select the actual trace. In the combo
box the Trace name is displayed in the trace color.
2. This function filed selects the tool used for generation of Text labels. All
subsequent added text labels are always related to the actual trace. The position
of the text label is defined by clicking to the desired position in the graphic
window.
3. This function field selects the tool used for generation of Value labels. All
subsequent added value labels are always related to the actual trace. First the
desired data point is clicked, then the desired position in the graphic window.
4. This function field selects the tool used to Edit text or value labels. After clicking
to a text or value label, it can be moved, edited or deleted.
5. This function field selects the tool used to draw lines. Both end points must be
specified with a click. The line will be assigned to the actual trace.
6. This function field selects the tool used to edit lines. After clicking to one of the
end points of a line, it can be marked, moved, rotated or deleted.
7. This function field is used to determine the pint of intersection, and to add the
related value label. Both lines must have been marked before.
8. This function field selects the tool for magnification (Zoom). With the left mouse
button pressed the desired zoom area is selected. After pressing the right mouse
button the zoom is performed.
9. This function field undoes the last zoom and the previous screen is displayed.
10. This function field turns off all previous zoom actions and restores all traces to
their original appearance.
11. Display or hide X-axis scaling (selecting a trace with tool 1 will allow to hide or
display the corresponding axis)
12. Display or hide Y-axis scaling
13. This tool displays the XY values while scrolling over the actual trace.
Display or hide the tool box

The tool box can be displayed or hidden by selecting "Options" "Toolbar" from menu.
Usually the tool box should be set visible, since some of the operations can't be
performed if it is hidden.
81
16.6.2. Explanation of Tools
Zoom
The internal resolution of a displayed trace is stored with approximately 20,000 data
points. Compared to that, the screen has a much smaller resolution (in most cases 1000
points). For that reason, a display can be magnified in size to a certain degree (up to
about 100 times).
This magnification does not calculate (because of a time reasons) any new points in
between, so that in a file with a high amount of data points (more than 20,000) not all
the points are displayed on the screen.
In this case a new image can be created through the choice of the section (TRACE -
CHANGE - RANGE MARGINS), which now also has a resolution of 20,000 points.
Normally the resolution of the whole trace good is enough to show, even after the
magnification, all the data points.
Magnify New Section (Zoom)
To get a magnification of a certain section of the trace you need the Zoom-Tool. You
can get this tool by selecting the magnifying glass icon in the tool bar, which is
underneath the menu bar.
When this tool is used in the graph, the cursor switches into the shape of a magnifying
glass.
To get a specific section, you can open up a window using your mouse. To open up the
window, you first pick one corner of the desired section, press and hold down the left
mouse button and move to the opposite corner. The requested window is hereby
displayed as a box, which can be changed in size and shape, outlined with a broken line.
After releasing the left mouse button the window stays on the screen.
Pressing the right mouse button quickly will display the selected section on the screen.
To magnify this section even more, you have to create another window by selecting a
new corner and using your mouse. The old window will then be overwritten by the
program.
Undo Last Magnification
Magnifications can be selected as often as needed, until certain resolution limits are
reached. With every new magnification, the old one will be stored in the so called Zoom
Stage. This Zoom Stage is displayed as a number on the right side of the status bar.
The whole trace has the 0, the first zoom #1, the second zoom #2, and so on.
To get the previous magnification, you have to choose the magnification glass icon with
the mark -1in it. This icon in the tool bar makes it possible for you to get step by step
back to previous magnifications.
Display without Magnification
In a lot of situations is it not only needed, to display and label the traces on the screen,
but to edit and evaluate them through specific, numeric procedures.
On the menu bar you will see the selection EVALUATE, which gives you a variety of
functions for processing data files. To get from any zoom # back to the whole trace
(zoom 0); select the crossed magnification glass icon in the tool bar.
82
16.6.3. Evaluate Traces
These function groups suit additional directories, which are available separate from the
source program. This way the function volume of the evaluation program can fit the
needs of the user.
In the first line of the edit menu appears the statement FUNCTION GROUP~, where the
desired function group can be selected and activated. The name of the function appears
in the second line of the menu. The individual functions can then be selected in the
following lines. They are described in the documentation, which comes with every
additional directory.
Evaluation Protocol
In some function directories certain evaluation results are held in a protocol file, which
can be printed out or can be stored. The protocol file has always the same name as the
evaluation window, where it belongs to. The file has always the default ending .TXT.
The protocol file is stored in the ASCII-format and can be viewed and printed out with a
regular editor.
Turn Protocol On/Off
In the menu selection OPTIONS - PROTOCOL can be selected, if the actual function
directory is enabled to protocol evaluation steps. This condition is changed every time
you select PROTOCOL. In some applications a protocol is saved for the records or for
documentation.
Hint: In some function directories the protocol file can start to store parameters as
soon as data are available. Therefore it is recommended to turn on the
function right after opening the evaluation window to get a complete protocol.
Print Protocol
To print out the protocol, you have to select PRINT PROTOCOL. The form, in which
the protocol tile is printed, depends on the actual function directory.
83
16.6.4. Legend
In addition to the display of the traces, it is possible to set labels within an evaluation.
These labels are always related to a trace.
The legend is always related to the actual trace, which is displayed in the box below the
menu bar. The position of the legend can be defined screen oriented, which means
independent from the magnification, as well as trace related, which means it is set with
trace co-ordinates. Besides that, the labeling can be horizontal as well as vertical, it can
be in the color of your choice and can also have several lines.
General Labeling
To get a general labeling of a trace, use the icon named ABC. After selecting it with
your mouse, you will get a mouse cursor in form of a 90-degree angle.
Now you can move the pointer to the desired text position and press the left button.
After that a dialog box appears where the legend can be entered as well as information
about the position, direction and color. After entering OK, the text will be displayed in
the evaluation window.
Labeling of a Data Point
A special legend type exists for marking certain points on the trace. The point on the
trace, which should be labeled, is marked with a cross, and an additional line.
To do this, you have to select the icon marked XY in the tool bar.
Now the mouse cursor will appear in form of a little cross, which you use to select a point
on the trace and confirm this by clicking the left mouse button. In case you did not hit
the trace exactly with the marker, the closest data point will be calculated and marked.
The form of the cursor changes now into the shape of the general labeling, and the
position for the legend can be selected.
The following dialog to enter the text differs (because of the option to enter co-ordinate
values) from the general labeling. It can only be related to a trace.
Change and Delete individual Labels
To change, move or delete a label, you need the tool to change the legend. You can get it
by selecting the icon with the shaded area in the tool bar.
To change the label, you have to move the mouse cursor to the text on the screen and
hit the left button and hold it down. After that a dialog box appears on the screen, which
gives you the choices between MOVE, CHANGE and DELETE. Now you have to
scroll, until the desired action is selected.
The first option is to move the label, which appears on top of the dialog box. After
releasing the mouse button, you can move the label. Another click of the left mouse
button ends the move.
The second option is to change the label. Selecting this option will bring up a dialog box,
like the one when entering a new label, with the difference that the actual parameters
are set (name, color, etc.)
The last option is to delete the label completely. After DELETE is clicked on, a dialog
box is displayed on the screen where you have to confirm the action.
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Delete Groups of Labels
If you want to delete a whole group of labels at one time, rather than every label
individually, you need to select
TRACE - DELETE LABELS....
To delete a complete group of labels, a dialog box appears on the screen, with a list of all
the groups. You can now select one or more groups you want to delete.
Hint: The labels, which have to be deleted, can only be from the
actual trace, which is displayed in the tool bar. All the labels
from other traces will stay unchanged.
Hide and Restore all Labels
In an evaluation with lots of labels on a curve, you might want to make all the labels
invisible, so that you can only see the trace on the screen.
To do so, you have to select in the menu bar OPTIONS - LABELS. The condition
between visible/invisible is changed every time you select LABELS. When the label is
visible, a little check mark appears on the left side of LABELS.
Hiding the labels does not delete them, it makes them only invisible. To hide and restore
the trace names, please refer to chapter 3.7.
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16.6.5. Lines
Similar to labeling a trace, it is possible to draw lines within an evaluation. These lines
are always related to the trace, which means, they are linked to co-ordinates of the trace
display. They are displayed always inverted to the background.
Draw Lines
To draw a line, you need the Line-Tool. You can get this tool, by selecting the line icon
in the tool bar.
To draw a line, you first pick the starting point of the line and click the left mouse button.
Now you can move your cursor in the window, and you see the line like a rubber band,
which is held in one spot.
Hitting the left mouse button again will hold the line in the actual position.
Change Lines
To change lines, you need to pick the line icon with the arrows.
Then you have to go with the cursor to one of the ends of the line, which you would like
to change, and hit the left mouse button and hold it down. A dialog box appears on the
screen, which offers the selection between MARK, ROTATE, MOVE and DELETE.
MARK:
With the command MARK, a line, which needs to be edited (e.g. for line intersections),
has to be selected.
The marking of a line is displayed as little quadrants on both ends of the line.
ROTATE:
To rotate a line, you have to select one end of the line, hit the left mouse button and
hold it down. Go down to ROTATE, and release the button. The line can now be rotated
with the point, which you selected. The other end of the line stays in place.
MOVE:
To move a line parallel, you have to select MOVE in the dialog box.
The length of the line remains the same.
DELETE:
With the option DELETE it is possible to delete a whole line.
Calculate Line Intersection
The icon in the tool bar with the two crossed lines, is used to calculate an intersection.
To calculate an intersection, you have to mark two lines which are related to the same
trace, and select the icon in the tool bar. After that, the intersection will be labeled with a
data point and the line marks will disappear automatically.
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16.6.6. Info Field
The info field is a text window, which is capable of storing additional information about a
measurement or evaluation. It is displayed in a separate window below the trace.
Load and Edit Info Field
If a data file has additional information about a measurement, they can be loaded as a
text file using the commands OFTIONS - INFO FIELD... - LOAD....
The information for the info field will be taken from the same file as the actual trace.
After that, you can change and edit the window with EDIT.... For the text in the info
field, there is a maximum of six lines.
Hint: You can enter a text into the info field, without loading already
existent data. However, if a text is loaded from a file, the actual text
into the field will be overwritten.
Hide and Restore Info Field
To be able to display the traces on the full screen, you have the choice of hiding the info
field. To hide or restore the info field, you need to select OPTIONS - INFO FIELD... -
VISIBLE. Every time you select visible, the condition between visible and invisible
changes.
Hint: Hiding the info field does not delete it; it makes it only invisible on the
screen.
Delete Info Field
With OPTIONS - INFO FIELD... - DELETE the whole window will be deleted. The
(until now) existing text will be lost entirely. After that a new window can be created.
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16.6.7. Print
The results of an evaluation can be printed on every Windows compatible printer or

plotter. For the printout, a large temporary file is installed, so make sure that enough
space is left on the hard disk.
Printer and Interface selection
To select a printer that is already installed under Windows, you do not have to leave the
evaluation program. With PRINT - SELECT PRINTER you get into a dialog box, where
all the installed printers and selected interfaces are listed. These settings can be changed
temporarily as well as stored permanently in the Windows standard settings.
Printer Setup
The commands PRINT - PRINTER SETUP enables to check and, if necessary, change
the settings of the printer. The dialog window is different for every printer and can not be
described in detail. When using a color printer, we recommend to select the option
COLOR to increase the quality of the printout. The print speed of the graphic depends
mostly on the used resolution and the color option. An incorrect input to the paper size
can cause that parts of the print out are missing, or printed inaccurately.
Screen Dump
PRINT - GRAPHIC starts the screen dump on a printer or a plotter. To use the better
resolution of the printer or plotter, a new picture will be built up internal, instead of just
using the screen copy. This procedure and the use of the print manager need a little
time. When the graphic is stored temporarily in the print manager, it is possible to
continue to work with the program, even when the printer is still printing.
Print Evaluation Protocol
For an evaluation where the protocol mode was turned on, a text file is created which
stores information about the evaluation results. This includes the controller parameters of
a DSC file, the actual contents of the info field and the results of the previous peak
evaluations. The protocol can be turned on or off with OPTIONS -PROTOCOL (see
chapter 5.2.).
The created file has the same name as the evaluation, with the difference of the ending
.TXT. It can be edited with a standard text editor.
With OPTIONS - PROTOCOL the protocol file can be printed out in a tabulated format
on the active printer.
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16.6.8. Miscellaneous
Co-ordinate Display
In the status bar two buttons are displayed. One is marked X, the other r.
Respectively next to their right side, the co-ordinate values of the actual trace are
displayed.
This display can be turned on or off by pressing the according button. The condition
between on and off is switched every time you select the button.
To get into a delta mode, the cursor has to be positioned and the left mouse button has
to be pressed down and held down. The actual position is now stored as the zero
position. By moving the cursor, you will see the X and Y deviation from the zero position
displayed. The delta mode is active as long as the left mouse button is pressed down.
Copy Evaluation to Clipboard
With FILE - COPY TO CLIPBOARD it is possible to copy a picture of the actual

evaluation window to the Windows clipboard (temporary storage). The picture can then
be transferred into other Window programs, e.g. Word for Windows or Paintbrush. It will
have the same resolution as the evaluation, which was displayed on the screen.
Hint: To copy the entire screen to the Windows clipboard, you can use the
buttons PRINT or ALT-PRINT. In this case, all the menus and visible
windows are included in the picture.
Hide and Restore Tool Bar
In the menu OPTIONS - TOOL BAR can be determined, if the tool bar below the menu
bar is visible or not.
The tool bar should be turned on all the time, because some functions would be lost
without it.
File Definition
In the menu OPTIONS - FILE the file categories are defined, where the program looks
for certain files.
Editor
The menu selection OPTIONS - EDITOR activates an editor. The editor is hereby
started as an individual Windows application and has to be ended the same way.
Which editor is used, is defined in the file TA.INI. This is usually the Windows note pad.
However, in TA.INI another application can be applied, which is then used as an editor.
DOS-Shell
Sometimes it is required to use certain DOS-commands (e.g. delete, copy, etc.).

In the menu selection OPTIONS - DOS SHELL you can start an application which
makes that possible. The evaluation program uses standardized the DOS-Surface of
Windows 2.1. The File Manager for Windows 3.0 can also be used. Hereby, the name of
the according application has to be entered into the file TA.INI.
For advanced users the command processor of MS-DOS could also be used as a pure
DOS application.
89
16.6.9. How to perform an ASCII export
a) Perform an ASCII export in TAWIN
Open the requested file with the TAWIN Data Evaluation Software.
Select ASCII-Export
Select the data file which shall be exported into ASCII format.
90
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, for example:

Time, Temperature, Delta L, Weight, etc.
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.
Decimal Comma: for USA etc.
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b) Import the .ASC file into EXCEL
Please open Microsoft EXCEL and select the open a new file icon
Now go the folder where the created .ASC (ASCII) file has been stored.
Select all data types in the data type pull down menu.
The created ASCII file will appear, double-click the .ASC file. Now the import filter will
appear on your screen.
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The EXCEL import assistance will appear on your screen.
STEP 1 of the import assistant
a) At first please click the data type
b) Then select the appropriate data source Western European.
Now select next and proceed to step 2 of the import assistant.
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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
Please complete the import procedure by selecting the FINISH button.
The imported data file should now appear in a EXCEL spreadsheet.
95
Successful data import:
Example
96
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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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.
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16.6.13. DSC and HDSC calibration file
The calibration file (*.DCF) has the same structure like a standard WINDOWS profile
(*.INI) file.
Sample calibration-file:
[TEMPCAL]
K2SO4_1=584.0000,25.10,2.07
BaCO3=806.0000,5.80,0.12
[TCORR]
a=-0.086936937
b=75.871171171
m=1.10
s=1.38
[ENTHCAL]
K2SO4_1=584.0000,-5.959226
K2SO4_2=1069.0000,-5.990864
BaCO3=806.0000,-6.536475
SrCO3=929.0000,-11.231469
[HCORR]
a0=-405.115
a1=1.55966
a2=-0.00197059
a3=8.05297e-007
s=1.28502e-011
Description:
In the section [TEMPCAL] the materials used for the temperature calibration are listed. In
the section [TCORR] the related coefficients are stored. The corrected temperature 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. The heat flow is calculated according
the following equation:

H = Heatflow [mJ/s or mW], T = DSC/HDTA Signal [mK or V], T = Temperature [C]
s is the standard deviation for the coefficients calculated.
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16.7. MENU AND DIALOG SEQUENCE
The following will give you a view over the dialog sequence for all TG specific commands
from the menu "Evaluation. All other menus are ignored, because they are described in
the documentation for the evaluation program.
Menu Evaluation
Menu Function Group
TG-Evaluation
....(further evaluations, if enclosed in package)
Signal correction, X-smoothing Signal correction
Zero correction (Temp. 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)
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
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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)
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% 199.9%)
Range (Whole trace(s) / Zoom window / Controller stage)
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)
Select collection file (file name .GSM)
Trace Selection
Controller stage
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16.8. HINTS
16.8.1. Recommended Standard Evaluation
We recommend the following procedure to create a standard evaluation:
1. Create new evaluation window (File - New) I enter name.

2. Load function group (Evaluation - Function Group - TG-Evaluation).
3. Load Data...: File - Load Data... with TG-import <sample> (use
appropriate import filter when importing data.).
4. Signal correction: Evaluation - Signal correction, X-smoothing.
5. Signal smoothing: Y-smoothing.
6. Turn on protocol function: Options - Protocol (The On condition is marked
with a little check mark on the left side.)
7. Mass calculation: Evaluation - Mass calculation ..., selection of coefficients.
8. Protocol printout: Print - Protocol...
16.8.2. Problems with Trace Display
One problem that may occur is that the display becomes unclear when using too many
traces. However, the program is equipped to hide all traces, except the last used trace
(and perhaps directly related traces).
This function is also available in the main menu. Under Trace, you will find commands
such as Hide... - Restore... - Adjust Ranges.
16.8.3. Limitation of Trace Section
When using a full trace with its entire length, the processing time slows down or it is
impossible to process the curve. (E.g. when heat-up and cool down stages exist.)
The use of the zoom function or the selection of a controller stage will give you a range
of the trace to evaluate.
16.8.4. Information Field
The most important information about the trace is shown to the user while loading the
trace. They can be displayed by selecting Options - Info field... - Load....
The information in this field can be changed with the Edit... function.
The window is constantly undated with new results of the evaluation.
With the function Options - Info field... - Load Original... the present information
window can be overwritten by the original.
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How to create a DSC or HDSC calibration file
17. 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.g. Sapphire)
Both Methods have advantages and disadvantages:
At Calibration with Substances (Enthalpy) only a few calibration points are

possible, but also the temperature scale can be calibrated.
Calibration with a Heat Capacity Standard uses one calibration run for the whole
temperature range. In this case a temperature calibration is not possible.
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17.1. (H)DSC CALIBRATION BY MEASUREMENT OF PHASE CHANGE

ENTHALPIES
For signal calibration of DSC/HDSC measurements, a calibration file (*.DCF) is required.

This file usually contains two kind of calibration information:
Coefficients for temperature calibration, related to the used heating rate
Coefficients for enthalpy calibration (mK or V to mW) as a function of the

temperature
For temperature calibration a first order polynomial function (offset and factor), for
enthalpy calibration a polynomial up to a fifth order may be used. The information of the
enthalpy calibration must be contained in the calibration file, the information for
temperature calibration can be included (if it is not present, a temperature calibration of
measurements cant be performed).
To create a calibration file, the following data is required:
A DSCCAL.INI-file, containing the proper values of onset-temperature ([C]) and

enthalpy ([J/g]) of the desired calibration substances.
The data-files of the calibration measurements
The set of calibration substances used should include the desired temperature range for
sample measurements. The following substances are predefined in the DSCCAL.INI file
additional substances may be added by the user:
Indium=156.5985,28.59
Zinn=231.928,60.86
Gallium=29.7646,80.48
Blei=327.462,24.81
Zink=419.527,112.46
BaCO3=806.000,103.66
SrCO3=929.000,149.36
K2SO4_1=584.000,42.91
K2SO4_2=1069.000,210.30
The first column contains the name of the substance used, the second one the onset-
temperature in [C] and the third one the enthalpy in [J/g]. If a substance has more than
one peak, it must be entered several times, once for each peak, using different names
for each peak (see K2SO4, having two peaks).
The calibration measurements should be run with the same crucibles and heating rates
used for the sample measurement also. If it is desired to use the temperature calibration
too, 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 corrected value
of the onset-temperature is extrapolated for heating rate 0K/min).
104
It is useful to create an own subdirectory for all calibration measurements. It is also

suggested to use filenames, corresponding to the used substance and heating rate (e.g.
PB10-1 for: Substance lead, heating rate 10K/min, first run) to avoid confusing during
evaluation of the measurements.
When all calibration measurements are completed, the data-files must be evaluated to
create the protocol-files, containing the information for heating-rate, onset-temperature
and peak-area. The following procedure is suggested:
Start the data-evaluation (if it not running yet).
Create a new evaluation window (FILE-NEW).
Use the name of the calibration substance used as the evaluation window name, this
name must match the MS-DOS naming conventions.
Select the proper function library (EVALUATION-FUNCTION GROUP-DSC or HDSC), if

not already set up.
Switch on the generation of the evaluation protocol (OPTIONS-PROTOCOL). If an

evaluation protocol with the same name exists, you are asked either to append to or
to delete the existing protocol file. If the existing file holds valid information of earlier
evaluations you should select append, if not, you should choose delete and create a
new protocol file.
Load the data file of the calibration measurement (FILE-LOAD).
Optional you can perform a zero-correction if desired (a corresponding zero

measurement must be available).
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, perform smoothing

only, derivation is not required. Use the smoothing factor suggested by the program.
Choose DATA PEAK EVALUATION from menu EVALUATION. Then you are asked for
several options. 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). Partition integration is not
required for single peaks. The enthalpy for calibration purpose should always be set
to grams, not to mol.
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, 4 if the method of increase of
the peak are is used, marking those regions of the trace, the baseline is still identical
to the trace).
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Hide or delete all traces and load the next data-file, created with the same calibration
substance and perform the same procedure described above. So all information of
multiple measurements, using the same calibration substance are written to a single
protocol file. This protocol file has the same name like the evaluation window and the
ending TXT. It is located in the PARAM directory of the related function library (e.g.
C:\TAWIN\DSC\PARAM).
When the evaluation of all data files of one calibration substance is completed, choose
EXIT from the file to close the active evaluation window.
Use the same procedure for all calibration substances measured.
After this, the related PARAM-directory should contain one protocol file for each
calibration substance used. Now you can close the data evaluation program and start the
generation of the calibration file, using DSCCAL or HDSCCAL, depending on the
instrument used.
Select NEW or OPEN from menu CALFILE, depending if you want to create a new
calibration file or to add the new information to an existing one. Next you are asked for
the calibration file name. The default name is CALIB, but you can use any name desired
(the name must match the MS-DOS naming conventions). If you have chosen NEW
before and a calibration file with this name already exists, you are asked whether to over
write it or not.
After this you can create entries for temperature an enthalpy calibration, using the menu
topics TEMPARATURE and ENTHALPY. For temperature calibration, the protocol file(s)
used, must contain at least two measurements of the same substance, measured at
different heating rates. When choosing TEMPERATURE from the menu, you are asked for
the name of the protocol file. Switch to the proper directory containing the protocol files
generated (e.g. C:\TAWIN\DSC\PARAM) and select the protocol file desired. If the
selected protocol file contains only measurements with the same heating rate or a single
measurement only, an error message is displayed. If there are at least two entries with
different heating rates, you are asked to select the desired entries in a list box (for
default all entries are selected). After this, the coefficients for temperature correction
may be calculated (selection Calculate Te (0)). After calculation, you are asked if you
want to store the results in the calibration file. 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. If more than one protocol file is used for temperature
calibration, the average of all results is calculated.
106
For enthalpy calibration, a similar procedure is used. You are also asked for the protocol
file to use, and for selecting the desired entries in the protocol file (for default all entries
are selected). After this, the factor for enthalpy calibration may be calculated (selection
Calculate Factor). After calculation, you are asked if you want to store the results in the
calibration file. If the protocol file contains more than one peak entry, the average will be
calculated. 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. At this
point, the calibration file contains one entry for every substance used, with the onset
temperature and the factor for calculating [mW] from [mK] or [V]. Now the polynomial
coefficients for the enthalpy calibration may be calculated (Selection Approximation
Curve). There are two different ways for calculation:
You can enter the desired correlation. The polynomial order is chosen automatically to
match the entered correlation
You can enter the desired polynomial order and the resulting correlation is calculated.
This is useful to force the use of a lower polynomial order (Suggested: second
degree) to avoid a rough behavior of the calibration function, especially outside of the
definition range (Temperature range of substances used). If the resulting correlation
has a low value (1.0 = best value, < 0.5 = 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).
After this the calibration file is ready to use by the evaluation program. Before leaving
(H)DSCCAL you may view the *.CAL (or protocol *.TXT) file(s) by means of the Notepad
editor (menu topic EDIT). 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). For this purpose, the
desired temperature range and file name must be entered. The generated file (ending
*.DCP) will be stored in the CALIB-directory (e.g. C:\TAWIN\DSC\CALIB), the same
directory the calibration file (ending *.DCF) is stored also.
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17.2. (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.
This table (Text file) must have two columns, Temperature [C] and Head Capacity
[J/gK]. Both columns are delimited with one or more blanks, a dot is used for the decimal
separator. A minimum of 6 entries are necessary, maximum are 100 entries:
Example of a table for Sapphire:

0.0 0.717914
50.0 0.824791
100.0 0.906528
150.0 0.969583
200.0 1.018848
250.0 1.057906
300.0 1.089367
350.0 1.115137
400.0 1.136620
500.0 1.170614
550.0 1.184475
600.0 1.196870
650.0 1.208120
700.0 1.218464
750.0 1.228080
800.0 1.237096
850.0 1.245605
900.0 1.253670
950.0 1.261337
1000.0 1.268635
To create a table the Windows Editor Notepad can be used.

The extension must be .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.
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How to create a Calibration File:
The zero run and the calibration run must be done, than:
- Load the Calibration Standard run into the Evaluation software

- 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
Then the result must be compared with the literature values. The software displays the
available calibration standards tables. 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. Next the corresponding literature temperature value will
be interpolated and divided by this (uncalibrated) calculated value. The result is the
calibration factor. This file has the extension .HCF (Heat flow Calibration File) and will be
saved in the CALIB directory. The name must be given in the following dialog. The
default name is the name of the calibration standard run:
110
In the next diagram the Calibration factor is displayed against Temperature:
The calculation of the calibration file is now finished. This calibration file now can be used
to calibrate sample runs.
Using the Calibration File:
Load a sample run into the evaluation. Do the zero correction.

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. Select the correct FILE TYPE.
.DCF files if using a calibration file which was created with substances
.HCF files if using a calibration file which was created with a Heat Capacity Reference
Sample.
111
Then select the correct file from the list:
The Heat Flow Trace will be calculated [mJ/s]:
112
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.
Also the Heat Flow Trace can be used to calculate the Heat capacity of the sample.
Therefore the point SPECIFIC HEAT CURVE must be selected. This trace gives the heat
capacity of the sample for any temperature value [J/gK]:
113
Evaluation flowcharts
18. EVALUATION FLOWCHARTS
18.1. DTA EVALUATION FLOWCHART
114
18.2. DSC EVALUATION FLOWCHART
115
18.3. TG EVALUATION FLOWCHART
116
18.4. CP EVALUATION FLOWCHART
117
Error Codes
19. ERROR CODES
Internal device errors are shown as error codes in the actual values field in the weight
reading.
The shown error code is composed of the error marker E and a classification number.
In the following spreadsheet are the meanings of the codes explained.
Are several errors present, the shown code is the sum of the particular error codes.
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. Therefore choose
OPTIONS Read error-status.
118
Linseis Standard reference Material
20. LINSEIS STANDARD REFERENCE MATERIAL
Certificate
Standard reference Material
DTA HDSC
Weight loss as a Function of Temperature
Material
Indium In Onset: 156.6 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 220C with 5K/min.
The provided Reference Material BaCO3 was heated up to 1000C with 5K/min.
The provided Reference Material K2SO4 was heated up to 1200C with 5K/min
The provided Reference Material Nickel was heated up to 1550C with 5K/min
Origin of reference Material:
The provided Indium, BaCO3, K2SO4; Nickel has a manufacturer guaranteed purity better 99.99%.
For this please refer to manufacturer certificate.
Selb 95100 / Germany

Dec 04, 2008
Standard reference program
119
Certificate
Thermogravimetry: Copper sulfate

Copper sulfatee: CuSO4 + 5H2O
1. Stage: Decarbonation: CuSO4 + 5H2O CuSO4 + 3H2O

Mass change: -14.43%
2. Stage: Decarbonation: CuSO4+ 3H2O CuSO4 + H2O

Mass change: -28.86% (-43,29% in total)
3. Stage: Decarbonation: CuSO4 + H2O CuSO4

Mass change: -36.08% (-79,37% in total)
The provided Calibration Material copper sulfate was heated up to 310C with 5K/min.
The provided Copper sulfate has a manufacturer guaranteed purity better 99%. For this please refer to
manufacturer certificate.

March 06, 2006
120
121
Certificate
Thermogravimetry: Calcium oxalate

Calcium oxalate: CaC2O4+1H2O
1. Stage: Dehydration: CaC2O4 + 1H2O CaC2O4 + H2O

Mass change: -12.3%
2. Stage: Building carbonate: CaC2O4 CaCO3 + CO
Mass change: -19.2% (-31.5% in total)
3. Stage: Decarbonation: CaCO3 CaO + CO2
Mass change: -30.1% (-61.6% in total)
The provided Calibration Material Calcium Oxalate was heated up to 1000C with 5K/min.
The provided Calcium Oxalate has a manufacturer guaranteed purity of 99.7%. For this please refer to

March 17, 1994
122
Certificate
Thermogravimetry: Al2O3
Aluminum oxide: Al2O3
The provided Reference Material Al2O3 was heated up to 1600C with 5K/min.
The provided Al2O3 has a manufacturer guaranteed purity better 99%. For this please refer to

March 06, 2006
123
124
Certificate
Thermogravimetry: Calcium carbonate

Calcium carbonate: CaCO3
Stage: Decarbonation: CaCO3 CaO + CO2

Mass change: -30.1%
The provided Calibration Material Calcium carbonate was heated up to 1000C with 5K/min.
The provided Calcium carbonate has a manufacturer guaranteed purity better 99%. For this please
refer to manufacturer certificate.

March 06, 2006
125
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. These values may be used for temperature and/or cell constant
calibration of the Linseis DSC or HT-DSC/DTA.
127
Enthalpy of Melting for Standards
128
Sapphire Specific Heat Capacity Literature Values
22. 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. The table below summarizes
specific heat capacity data (literature values) for sapphire as a function of temperature.
These values can be used in the required calculations.
129
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).
The sapphire pieces passed a #10 sieve but were retained by a #40 sieve, and had 99.98
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 units J/gmole are absolute joules per degree per gram mole
(molecular weight - 101.9613) at a constant pressure of 1 atmosphere (100 Pa).
130
Thermogravimetric analysis of Calziumoxalate
23. THERMOGRAVIMETRIC ANALYSIS OF CALZIUMOXALATE
Calziumoxalate: CaC2O4 + 1H2O
1. Stage: Dehydration: CaC2O4 + 1H2O CaC2O4 + H2O

Mass change: -12.3%
2. Stage: Building carboante: CaC2O4 CaCO3 + CO

Mass change: -19.2% (-31.5% total)
3. Stage: Decarbonation: CaCO3 CaO + CO2

Mass change: -30.1% (-61.6% total)
131
Chemical behavior of Crucibles
24. CHEMICAL BEHAVIOR OF CRUCIBLES
24.1. PLATINUM CRUCIBLES
Critical for Platinum is:
Halogens (Cl2, F2, Br2), aqua regia

Li2CO3, already before CO2-release
SiC at app. 1000C
FeCl3
Be composites (evaporate just above melting point)
HCL with oxidizer, for example (chromic acid, manganat, Iron (III)-salts, salt
smelter)
Reducing atmosphere
Pb, Zn, Sn, Ag, Au, Hg, Li, Na, K, Sb, Bi, Ni, Fe, Steel, As, Si (composition
creation)
P, B
Se above 320C (cool down sample immediately after measurement and remove
probe to prevent Selenium evaporation)
Metal oxides with reducing substances such as C, organic compositions or H2
Sulfur, keying the surface
Alkali hydroxide, - carbonates, - sulfates, - cyanides and rhodanides at elevated
temperatures
KHSO4 at elevated temperatures
Carbon black or carbon above 1000C
SiO2 under reducing conditions
HBr, KCN-dilution at elevated temperatures
High temperature resistant oxides above 1000C
Platinum is not resistant against:
Mixtures out of KNO3 and NaOH at 700C sealed from air

Mixtures out of KOH and K2S at 700C sealed from air
LiCL at 600C
Na2O2 at 500C sealed from air
MgCl2, Ba(NO3) at 700C
HBr, HJ, H2O2 (30%) and HNO3 at 100C
KCI (damaging at the decomposition products crated during the melting, melting
point 768C)
Limited durable against:
KHF2, LiF, NaCl at 900C

Mixtures of NaOH and NaNO3 at 700C sealed from air
132
24.2. IMPORTANT HINT FOR HDSC MEASURING SYSTEM
Above app. 1100C direct touching platinum surfaces are welded. So, without special
precautions the platinum crucibles and the measuring system would become welded,
crucibles and measuring system would be destroyed. If the system shall be used above
1100C, the crucibles and the measuring system must be baked separately in oxidizing
atmosphere (air) to create a coating of platinum oxide, preventing welding during
measurement.
To do this, the measuring system and the crucibles must be heated separately up to
1500C (20K/min) and held for a 15min dwell time (cooling should be done with
30K/min). To bake the crucibles, a small disc of alumina (Al2O3) is used as a spacer
between the measuring system and the crucibles. The crucibles must be put bottom up
on the alumina disc. In a second run the measuring system itself must be baked also
(without alumina disc).
After baking, the surfaces of the measuring system must not be touched with fingers or
polluted with other substances.
Not any temperatures above 1500C must be used with platinum crucibles, because the
coating of platinum oxide will be destroyed at these temperatures. So, for measurements
up to 1550C crucibles made of alumina must be used instead.
After heating up above 1500C, the measuring system must be baked at 1500C again.
In spite of baking the platinum parts, the crucibles may stick slightly on the measuring
system, when used above 1200. To remove the crucibles, use a pair of tweezers to tip
over the crucible while holding the measuring system by hand. Do not forget to remove
the crucible for the reference material also after each run, to prevent from becoming
welded on the measurement system due to multiple runs.
133
24.3. ALUMINUMOXID CRUCIBLES
Critical for Aluminumoxid is:
N2 in presence of Carbon: creation of AIN, 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 700C
Sulfur: no reaction with liquid sulfur, if Carbon is present during the gas phase,
creation of sulfides at elevated temperatures
H2S: under heat exposure creation of Al2S up to 3%
C: Creation of Carbides and Al at app. 1400C
HF: quantitative reaction to AIF3 and H2O at elevated temperatures
CuSO4: Diffusion trough crucible surface at app. 1000C
Compositions containing Silica, such as MOSi2: in Inertia lead to contamination of
Al2O3 at app. 1200C; under air reaction at the contact point
Metal fluorides: attacked by smelter, creation of (AIF6)3- anions and cryolite
related salts
Glass: Glass smelter dissolves Al2O3
Hydrogen sulfate of the Alkali- and Alkaliearthoxide
HCI: no reaction until 600C, reaction at elevated temperatures which is
increased when Carbon is present
B2O3 or Borax: Smelter dilutes Al2O3, creation of Aluminaborates and -borides
Alkali- and Alkaliearthoxide and their salts with volatile anions: smelter creates
Aluminates or double oxides, important for Hydroxides, Nitrides, Nitrates,
Carbonates, Peroxides, etc
CaC2: under heat creation of Al4C3
PbO: Reaction at 700C, also important for Lead oxide and Lead salt in
combination with anions of volatile acids
UO3: Reaction start at 450C, analog PbO
MeO: Me = Fe2+, Co2+, Ni2+, etc.
Alcali- Earthalcaliferrites : smelter dissolves Al2O3
Zirconium composites with melting points between 800 and 1200C : slow and
weak reaction
Some metal alloys such as: Fe with 4% Al
134
24.4. GRAPHITE CRUCIBLES
Critical for Graphite is:
O2, reaction above 400C

Melted metals such as: Fe, Co, Ni, Na
N2 reaction starting from 1700C (Creation of small amounts of Cyanides)
Oxides (probable reduction when directly contacting)
Water vapor
F2, Br2, at room temperature
Sulfur
Si at app. 1400C (formation of SiC)
Chromic acid (aqueous)
Cl-SO3H
SiO2 formation of SiC via the intermediate product SiO (technical production of
SiC at temperatures above 1800C, for that the reaction of SiO2 and C certainly
starts earlier)
NO, NO2
Sulfur acid H2SO4 concentrated at arr. 150C
Saltpeter acid HNO3, diluted at arr. 90C
SO3 at arr. 100C
Danger of explosion with HCLO4
NaOCL at arr. 50C
135
QUICK Start manual for Thermobalance PT 1600
25. QUICK START MANUAL FOR THERMOBALANCE PT 1600
25.1. MEASUREMENT WITH SAMPLE (1600 C)
Switch on computer and balance.

Open cooling water (flow >0.5 l/min) if using chiller adjust approx. 24C.
Open furnace using LIFT switch at balance press .
Remove used crucible and clean it toughly.
Insert new sample and weigh before.
Place crucible onto measuring system (reference crucible empty or with Al2O3).
Close furnace using LIFT switch at balance press .
.
Start software STA MEASUREMENT.
Program CONTROLLER, TEMPERATURE PROFILE.
ATTENTION!
Always program one heating rate with 30 C/min down to 700 C as last segment
to cool down controlled, for heating element and alumina tube protection, when
you heat higher than 700C.
Check CONTROLLER, CURRENT VALUE for temperature of sample and furnace

should be room temperature.
Select DATA ACQUISITION, TYPE, SAMPLE TG+DTA.

Program DATA ACQUISITION, SETTINGS.
Sample file name, zero file name, weight of sample, duration, end temperature,
and ranges for TG and DTA (default DTA 250 V), Switch filter to .
Select OPTIONS, SETUP SCALES to find the Tara of the balance.

Press AUTOMATIC ZERO ADJUSTMENT.
Start measurement with START.

It is useful to start the measurement without the controller to see if the TG and
the DTA Signal has no drift anymore. If it is Ok stop measurement and start the
whole experiment.
Monitor measurement with CONTROLLER CURRENT VALUES or real time graphic.
ATTENTION!
Dont switch balance main switch off as long furnace is hot.

Dont close cooling water as long furnace is hot.
Open the furnace, switch cooling water off or switch balance off only if the
temperature value on the display is less than 100C.
136
QUICK Start manual for Thermobalance PT 1600
25.2. MEASUREMENT ZERO FILE (1600 C)
Switch on computer and balance.

Open cooling water (flow >0.5 l/min) if using chiller adjust approx. 24C.
Open furnace using LIFT switch at balance press .
Remove used crucible and clean it toughly.
Place two empty clean crucibles (or two crucibles filled with an equal quantity
Al2O3) onto measurement system.
Close furnace using LIFT switch at balance press .
Start software STA MEASUREMENT.

Program CONTROLLER, TEMPERATURE PROFILE.
One segment to maximum temperature, gas conditions and heating rate like in
the sample run.
ATTENTION!
Always program one heating rate with 30 C/min down to 700 C as last segment
to cool down controlled, for heating element and alumina tube protection, when
you heat higher than 700C.
Check CONTROLLER, CURRENT VALUE for temperature of sample and furnace

should be room temperature.
Select DATA ACQUISITION, TYPE, ZERO TG+DTA.

Program DATA ACQUISITION, SETTINGS.
Zero file name (should follow DOS conventions max. 8 characters or numbers
only), duration, end temperature, and ranges for TG 25mg and DTA 250V,
switch filter to .
Select OPTIONS, SETUP SCALES to find the Tara of the balance.

Press AUTOMATIC ZERO ADJUSTMENT.
Start measurement with START.

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.
Monitor measurement with CONTROLLER, CURRENT VALUES or real time graphic.
ATTENTION!
Dont switch balance main switch off as long furnace is hot.

Dont close cooling water as long furnace is hot.
Open the furnace, switch cooling water off or switch balance off only if the
temperature value on the display is less than 100C.
137
Appendix
26. APPENDIX
J.O.Hill (de.):
For better Thermal Analysis,
Edition III; ICTA 1991
W.WM. Wendlandt:
Thermal Methods of Analysis,
John Wiley & Sons, New York, London, Sidney, Toronto, 1974
B. Wunderlich:
Thermal Analysis,
Academic Press Inc., Boston, San Diego, New York, 1990
A. Blazek:
Thermal Analysis,
Van Norstrand, London, 1972
Peter Haines
Principles of Thermal Analysis and Calorimetry
Royal Society of Chemistry; 1st edition (August 1, 2002)
Adrian Bejan
Advanced Engineering Thermodynamics,
Wiley-Interscience; 2nd edition (October 2, 1997)
T. Hatakeyama, Liu Zhenhai

Handbook of Thermal Analysis
John Wiley & Sons (March 5, 1999)
Randall M. German
Sintering Theory and Practice
John Wiley & Sons (January 19, 1996)
by James S. Reed
Principles of Ceramics Processing, 2nd Edition
Wiley-Interscience; 2 edition (January 9, 1995)
P. Barnes, J. Bensted
Structure & Performance of Cements
Spon Press; 2nd edition (January 15, 2002)
R.C. MacKenzle
Differential Thermal Analysis Fundamental
Academic Pr (June 1, 1970)
Werner Smykatz-Kloss
Differential Thermal Analysis: Application and Results in Mineralogy, (Ecological
Studies,)
Springer-Verlag (December, 1974)
M.I. Pope
Pope Differential Thermal Analysis - A Guide to the Technique and Its Applications,
John Wiley and Sons Ltd (May 6, 1977)
138
Some Thermo Analytical Standards
27. 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, 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
Some Thermo Analytical Standards
Integration Einzelanleitungen,
003 30.07.2009 Griehammer all Inhaltsverzeichnis erstellt, gesamtes
Dokument berarbeitet
Parts list entfernt, heating element change
004 14.09.2010 Griehammer 1600C Abgleich berarbeitet Messysteme
berarbeitet
Chaper
005 27.10.2010 Grie?hammer
19 Kapitel errorcodes eingefgt
006 22.02.2011 Griehammer 6.2 electrical wiring added
anneling moved to chapter chemical
007 02032011 Griehammer
behavior of crucibles
140

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LINSEIS STA PT1600

Linseis Messgerte GmbH

Tel.: 0049 9287 880-0

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

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

3.1. Protecting the Operator..................................................................................................................... 4

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

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

5.1. General information .......................................................................................................................... 6

5.4. Furnaces .......................................................................................................................................... 11

6.1. Set Up Equipment Placement .......................................................................................................... 14

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

7.1. Dismount furnace ............................................................................................................................ 24

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

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

10. SELECTION OF THE GAS ATMOSPHERE....................................................................... 37

11. GASES AND THEIR LIMITATIONS .................................................................................. 39

12. GAS FLOW IN THERMOGRAVIMETRIC EXPERIMENTS ........................................... 41

13. LINSEIS STA MEASUREMENT SOFTWARE .................................................................. 42

13.1. Type of Measurement ..................................................................................................................... 42

13.2. Setup Data Acquisition .................................................................................................................... 43

13.3. Program Controller .......................................................................................................................... 46

13.4. Start and Stop Measurement........................................................................................................... 51

13.7. Relays .............................................................................................................................................. 53

14. PERFORMING A ZERO BASELINE CURVE..................................................................... 54

15. PERFORMING A SAMPLE CURVE .................................................................................... 61

16.1. Introduction .................................................................................................................................... 69

16.2. Start new Evaluation ....................................................................................................................... 70

16.3. Traces in the Evaluation ................................................................................................................... 73

16.4. Evaluation Icon ................................................................................................................................ 75

16.5. Summery of Functions ..................................................................................................................... 77

16.6. Program description ........................................................................................................................ 81

Data Structures ............................................................................................................................................... 97

16.7. Menu and Dialog Sequence ........................................................................................................... 100

17. HOW TO CREATE A DSC OR HDSC CALIBRATION FILE ......................................... 103

17.1. (H)DSC Calibration by Measurement of Phase Change Enthalpies ................................................. 104

18. EVALUATION FLOWCHARTS ......................................................................................... 114

18.1. DTA evaluation flowchart .............................................................................................................. 114

19. ERROR CODES .................................................................................................................... 118

20. LINSEIS STANDARD REFERENCE MATERIAL ........................................................... 119

21. ENTHALPY OF MELTING FOR STANDARDS .............................................................. 127

22. SAPPHIRE SPECIFIC HEAT CAPACITY LITERATURE VALUES............................. 129

23. THERMOGRAVIMETRIC ANALYSIS OF CALZIUMOXALATE ................................. 131

24. CHEMICAL BEHAVIOR OF CRUCIBLES ........................................................................ 132

24.1. Platinum Crucibles ......................................................................................................................... 132

25. QUICK START MANUAL FOR THERMOBALANCE PT 1600 .................................. 136

25.1. Measurement with sample (1600 C) ............................................................................................. 136

26. APPENDIX ............................................................................................................................ 138

27. SOME THERMO ANALYTICAL STANDARDS .............................................................. 139

Electronic or mechanical distribution or duplication of this/these instructions requires

LINSEIS Messgerte GmbH

Telephone: (+49) 9287 880-0

2. BASIC SYSTEM SAFETY INFORMATION

Allowed instrument operation

Manufacturer approved operation of the instrument includes training of personnel

Training of User Personnel

Your Linseis instrument may only be operated and maintained by authorized,

Responsibility for Commissioning, Operation and Training

Responsibility for commissioning, operation and maintenance must be clearly

Instrument Operation Guideline