Operating Instructions

Simultaneous TG-DTA/DSC Apparatus

STA 449 F1 Jupiter®
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Chapter III

System Components

STA 449 F1
STA 449 F1 System Components

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CONTENTS

MEASURING UNIT ........................................................................................1 

FRONT PANEL OF THE MEASURING UNIT ........................................................3 

TFT DISPLAY ................................................................................................... 4 

OPERATING ELEMENTS ...................................................................................... 5 

REAR OF THE MEASURING UNIT ...................................................................7 

GAS OUTLET VALVE ..................................................................................9 

EVACUATION SYSTEM .............................................................................. 10 

VACUUM CONTROL SYSTEM ............................................................................. 11 

EVACUATION PROCEDURE FOR INSTRUMENTS WITHOUT AUTOVAC ...................... 11 

EVACUATION PROCEDURE FOR INSTRUMENTS WITH AUTOVAC ............................ 14 

HIGH-VACUUM MEASUREMENTS ...................................................................... 16 

COOLING SYSTEMS ................................................................................. 17 

CC 300 COOLING SYSTEM ............................................................................... 18 

LN2 COOLING SYSTEM (WITH MAGNETIC VALVE) – 6.351.35 ............................. 19 

SAFE USE OF LIQUID NITROGEN LN2 ................................................................. 20 

SAFETY REGULATIONS FOR LN2 STORAGE VESSELS WITH NETZSCH DEWAR HEAD 

(6.351.35) ................................................................................................... 20 

PRECAUTIONS IN THE EVENT OF OPERATING FAULTS............................................. 21 

FURNACES ............................................................................................. 22 

RHODIUM FURNACE .............................................................................. 22 

PURGING THE HEATING CHAMBER .................................................................. 23 

TEMPERATURES, HEATING RATES AND LIFETIME ............................................... 24 

SILICON CARBIDE FURNACE .................................................................... 25 

TEMPERATURES, HEATING RATES AND LIFETIME ............................................... 26 

PLATINUM FURNACE ............................................................................. 27 

TEMPERATURES, HEATING RATES AND LIFETIME ............................................... 28 

PURGING THE HEATING CHAMBER (OPTION) .................................................... 28 
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HIGH SPEED FURNACE ........................................................................... 29 

TEMPERATURES, HEATING RATES AND LIFETIME ............................................... 30 

PREPARATION ............................................................................................. 31 

ADDITIONAL INFORMATION FOR THE INSTALLATION OF THE RADIATION SHIELD ..... 32 

GRAPHITE FURNACE .............................................................................. 34 

GAS AND VACUUM CONNECTIONS ................................................................. 35 

SAFETY CONTROL SYSTEM (S.C.S.) ................................................................ 36 

FUNCTION ............................................................................................... 36 

GENERAL INFORMATION FOR USING PURGE GASES .......................................... 38 

PRODUCING THE REQUIRED ATMOSPHERE IN THE FURNACE .............................. 40 

PRODUCING THE REQUIRED ATMOSPHERE IN THE SAMPLE CHAMBER .................. 42 

COOLING WATER SUPPLY .......................................................................... 43 

CHANGING THE PROTECTIVE TUBE .................................................................. 45 

LOW TEMPERATURE FURNACES ............................................................... 49 

STEEL FURNACE / SILVER FURNACE ................................................................. 49 

COOLING CONNECTIONS STEEL FURNACE / SILVER FURNACE ............................... 50 

TEMPERATURES, LIFETIME ............................................................................. 50 

ADDITIONAL INFORMATION FOR THE INSTALLATION OF THE RADIATION SHIELD ..... 51 

WATER VAPOUR FURNACE ..................................................................... 53 

SAMPLE CARRIER SYSTEM ........................................................................ 54 

MEASURING HEADS ................................................................................ 55 

THERMOCOUPLE TYPES ............................................................................ 57 

SERVICE SWITCH ..................................................................................... 58 
STA 449 F1 System Components

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Measuring Unit 

Figure 1: measuring unit STA 449 F1 Jupiter (details) 

1 Hoisting Device 

2 Gas Outlet Valve (open) 

3 Furnace 

4 Display and Operating Elements 

5 Safety Button 
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Figure 2: measuring unit STA 449 F1 Jupiter (cross - section)
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Front Panel of the Measuring Unit 

Figure 3: operating elements
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TFT Display 

Figure 4: TFT display

Label Function

1

display for the gas flow and the used gas type for purge 1, purge 2 

and protective 

2

display for the actual vacuum state 

(100% vacuum means minimum pressure) 

3

display for the balance signal 

4

display for the temperature signal

5

display for the type of temperature segment with end temperature 

of the segment 

→ Dynamic segment heating up

→ Isothermal segment 

→ Dynamic segment cooling down 

→ Final emergency temperature

6

display for remaining time of the measurement 
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Operating Elements 

Function Keys 

open the measuring unit 

close the measuring unit 

Control Display 

purge 1 control LED: purge gas 1 (sample chamber) "on/off" 

→ green LED on: purge gas 1 is switched on 

purge 2 control LED: purge gas 2 (sample chamber) "on/off" 

→ green LED on: purge gas 2 is switched on

protective control LED: purge gas (balance system) "on/off" 

→ green LED on: protective gas is switched on

green LED on: instrument is switched on 

orange LED on: measurement is running 
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All electronic valves are proportional valves which open slowly. 

The LEDs on the front panel show the selected function and the 

opening (closing) of the valves. 

Initial state after switching on the power supply:

• all electronic valves are closed 

• vacuum pump is switched off 

• the system is under normal pressure 

the hoisting device is blocked if:

• the system is not under normal pressure (e.g. vacuum) 

• the measuring program is running 
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Rear of the Measuring Unit 

Figure 5: rear of the measuring unit 
STA 449 F1 System Components

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No. label function 

1 USB connection computer system 

2 ASC ASC connection (No. 20) 

3 transportation lock O = Operation 

T = Transport (see page 58 in this chapter) 

4 power connection for furnaces 

connection for 

1 furnace

connection for 

2nd furnace

connection for 

1st furnace

5 external power unit connection for external power unit) 

6 AC input 50/60Hz power connection 230 (115) V 

7 thermoswitch fuse overtemperature 

8 analog digital I/O analog digital input/output 

9 turbo pump connection turbo pump 

10 ext. MFC connection MFC box 

11 valves vacuum 

 external 

outputs CC 300 

 optional 

connection magnetic valve – for AutoVac 

connection gas outlet valve (furnace switch) – 

for AutoVac 

connection LN2

 cooling system CC 300 

optional connection 

12 water outlet connection thermostat outlet 

13 water inlet connection thermostat inlet 

14 pressure-relief valve outlet pressure-relief valve sample chamber 

15 LN2 cooling connection cooling liquid nitrogen 

16 AUX output power output for pumps etc. 

17 vacuum flange connection to the vacuum pump 

18 AC line on/off 

AC input 50/60Hz 

115V/T4A; 230V/T2A 

power switch: instrument "on/off" 

power connection 230 (115) V 

mains fuses 

19 purge 1 

purge 2 

protective 

plug-in connection: purge gas 1 

plug-in connection: purge gas 2 

plug-in connection: protective gas 

20 furnace connection to furnace power connection (No. 4) 

21 ASC connection to ASC (No. 2) 
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Gas Outlet Valve 

Gases evolved from the sample are passed through the gas outlet valve. The function 

"vacuum" can only be used if the gas outlet valve is closed. If the function "AutoVac" is 

used (special equipment), please take care that the gas outlet valve is opened. For dynamic 

measurements the gas outlet valve must also be opened. 

gas outlet valve opened gas outlet valve closed

Figure 6: gas outlet valve 

ATTENTION!

Both for measurements under static atmosphere and under vacuum (without AutoVac), the gas 

outlet valve on the furnace must be closed! 

ATTENTION! 

If a gas hose is connected to the gas outlet valve in order to discharge exhaust gases, the 

gas hose must not be brought into a liquid. Danger of flooding the balance system! 
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Evacuation System 

An evacuation system can be connected to the measuring unit by means of the vacuum 

flange. The sample chamber can be evacuated up to a vacuum of approx. 10-4 mbar. 

The evacuating system consists of following components: 

• vacuum pump (rotary pump or diaphragm pump) 

• shut-off valve 

• pressure gauge (option) 

• connection cables and flanges 

• vacuum hose 

The installation of the evacuating system is described in chapter II!

The recipient is also provided with a safety valve (pressure relief valve), which opens at an 

excess pressure of 0.03 bar. 

Pressure gauge (TFT display - front of the measuring unit) 

 

Figure 7: pressure gauge

normal pressure: no bar is shown in the display 

decreasing pressure: increasing % value is shown in the display 

minimum pressure: 100% vacuum is shown in the display 

overpressure: overpressure is shown in the display 
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Vacuum Control System 

Evacuation procedure for instruments without AutoVac 

• Select Gases and switches in 

the Diagnosis menu and 

switch off all gases (purge 1, 

purge 2 and protective). 

• Close the gas outlet valve. 
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• Check that the shut-off valve 

for refilling is closed (knob 

must show downwards). 

• Switch on the vacuum pump 

(e.g. rotary vane pump or 

diaphragm pump). 

• Open the shut-off valve for 

the vacuum pump slowly. 

Refilling 

• Close the shut-off valve for 

the vacuum pump. 

• Switch off the vacuum pump 

(e.g. rotary vane pump or 

diaphragm pump). 

• Open the shut-off valve for 

refilling slowly (turn the knob 

upwards). 
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• Fill gas into the sample 

chamber up to a slight 

overpressure (see pressure 

gauge on the front display) 

and open the gas outlet valve. 

To create a particularly clean 

gas atmosphere a defined gas 

(purge or protective) must be 

filled at first before the gas 

outlet valve is opened. If the 

outlet valve is opened at first, 

impurities can enter the 

measuring system. 
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Evacuation procedure for instruments with AutoVac 

The evacuation unit AutoVac takes over the automatic evacuation and subsequent refilling 

of the sample chamber. The refilling is carried out via the gas inlet "protective". The 

"AutoVac" mode can be activated during the definition of the temperature program. 

 Installation of the AutoVac - see chapter II! 

• Select Vacuum Controller in the 

Diagnosis menu.

• Set the check mark for Enable. 

 Operating Modes: 

- Evacuate 

At first the sample chamber is 

evacuated via the bypass. After 

reaching a certain threshold, the 

bypass is closed (magnetic valve) 

and the sample chamber is 

evacuated directly via the vacuum 

connection. After reaching a 

further threshold, vacuum is 

reached (Ready is shown in the 

window).

- Evacuate+Fill 

The sample chamber is evacuated 

(as described above) and filled to 

normal pressure. Gas is introduced 

via the gas inlet "protective". 

- Refill 

The sample chamber is refilled 

(after previous evacuation) via gas 

inlet "protective". 

The upper symbols show the state 

of the different vacuum 

components (e.g. valve, pump and 

so on). Green shows the active 

state. 

Principle: 
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The function "AutoVac" can also be selected during the definition of the 

temperature program of the measurement: 

• To activate the AutoVac set the 

check mark for Use AUTOVAC 

Controller.

• Select the number of Evacuation 

+ Fill cycles before starting the 

measurement. 

• If necessary set the check mark 

for Keep Vacuum during 

Measurement.

When using a diaphragm pump with AutoVac it is recommended to increase the 

additional pumping time to approx. 5 to10 minutes: 

• Select Vacuum Setting in the 

Extras menu. 

• For using a diaphragm pump

with AutoVac it is recommended 

to set the value for the 

additional pumping time to 

approx. 5 to 10 minutes. 
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High-Vacuum Measurements 

For measurements under high vacuum the STA 449 F1 Jupiter can be equipped with a high 

vacuum pumping system. 

Measurements under vacuum 

Measurements under vacuum should only be carried out up to maximum 

furnace temperatures of 1400°C. Higher temperatures may cause damages on 

the instrument. 

Hints for the use of the STC in case of measurements under vacuum 

In case of measurements under vacuum with end temperatures up to the 

maximum furnace temperature we recommend to switch off the STC (Sample 

Temperature Controller). As the STC controls the sample temperature by the 

deviation between sample and furnace thermocouple, this can cause problems 

with furnace control (oscillation). In the worst case the furnace can be 

overheated. The STC can be switched on and off in the software (see Help 

system in the Proteus software). 
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Platinum Furnace 

Figure 11: Platinum Furnace 

General Characteristic 

- 25 ... 1500°C 

- Pt-Rh meander heater 

- integrated protective tube for gas flow with stop 

valve 

- air-cooled double shell 
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Temperatures, Heating Rates and Lifetime 

The high-quality heating element of the furnace of a platinum-rhodium alloy allows a 

maximum furnace temperature of 1500°C. However, at high temperatures a physically 

conditioned volatilization of the precious metal alloy is detectable that results in an 

increased wear of the heating element, depending on temperature and time. 

The maximum heating rate in the temperature range to 1200°C is 50 K/min for this furnace. 

In order to reach a possibly high lifetime of the heating element the following 

experimental conditions should only be employed in exceptional case: 

a) heating rates of more than 20 K/min above 1200°C. 

b) longer holds at temperatures > 1350°C due to very low heating rates (<5 K/min) and/or 

longer isothermal phases. 

From the view of lifetime of the heating element the ideal heating rates are between 10 

and 20 K/min; the most favorable temperature program is heating up and switches off at 

the desired admitted maximum temperature. 

Purging the Heating Chamber (option) 

To improve the reproducibility of the baseline the high-quality heating element of the 

Platinum furnace can be optionally purged with an inert gas (preferably N2

). The purge gas 

for the furnace is introduced via a screwing with sintering insert by which the gas flow rate 

is preset (60 ml/min, N2 calibrated, primary pressure 0.5 bar). 

Figure 12: gas connection for purging the heating chamber (Platinum Furnace)
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Sample Carrier System 

Principle 

Figure 28: sample carrier system
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Measuring Heads 

Type thermocouples 

available 

TG (crucible)

S; P 

TG (slip-on plate)

S; P

TG-DTA

E; K; S; W ATTENTION! 

Thermocouple type W is not 

applicable for measurements 

in oxidizing atmospheres! 

Protective gas required! 

TG-DSC

E; K; S; B; P 
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TG 

(for ASC) 

S; P 

TG-DSC 

(for ASC) 

S; K; P 

sample carrier 2000°C / 2400°C 

TG (crucible)

W ATTENTION! 

Thermocouple type W is not 

applicable for measurements 

in oxidizing atmospheres! 

Protective gas required! 

TG-DTA

W ATTENTION! 

Thermocouple type W is not 

applicable for measurements 

in oxidizing atmospheres! 

Protective gas required! 
STA 449 F1 System Components

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Thermocouple Types 

type/temperature range/ 

atmospheres 

Type E (Chromel-Konstantan) 

(-150 to 700°C)

oxidizing to 500°C 

reducing (reduces sensor lifetime) 

inert 

vacuum (reduces sensor lifetime) 

humid to 400°C 

Type K (Chromel-Alumel) 

(-150 to 800°C)

oxidizing to 500°C 

reducing (reduces sensor lifetime) 

inert 

vacuum (reduces sensor lifetime) 

humid to 500°C 

Type S (Pt-10%Rh/Pt) 

(RT to 1650°C)

oxidizing 

reducing (reduces sensor lifetime) 

inert 

vacuum (reduces sensor lifetime) 

humid to 1300°C 

Type B (Pt-30%Rh/Pt-6%Rh) 

(RT to 1700°C)

oxidizing 

reducing (reduces sensor lifetime) 

inert 

vacuum (reduces sensor lifetime) 

Type P (Platinel) 

(-150 to 1000°C)

oxidizing 

reducing (reduces sensor lifetime) 

inert 

vacuum (reduces sensor lifetime) 

humid to 1000°C

Type W (W3%Re-W25%Re) 

(RT to 2400°C)

inert 

reducing 

vacuum 

not for measurements in oxidizing atmospheres
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Service Switch 

• During transport the STA 449 F1 Jupiter is secured with a transport safety 

device – selected via the switch. 

• The switch is placed at the left rear side of the instrument. 

• For setting the switch use a small screw driver. 

Normal operation (O) 

Transport

Operation

• Set the switch to position O (Operation) and 

insert the sample carrier. 

Transport (T) 

Transport

Operation

• For the transport set the switch to position T 

(Transport). The furnace is moved into the 

upper end position. After this remove the 

sample carrier and move the furnace back into 

the lower end position. 
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Chapter IV

Operating the Instrument

STA 449 F1
STA 449 F1 Operating the Instrument

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CONTENTS 

OPERATING THE INSTRUMENT ......................................................................... 1

OPEN THE INSTRUMENT .............................................................................. 1 

INSERTING THE SAMPLE CARRIER ................................................................. 3 

ADJUSTING THE SAMPLE CARRIER SYSTEM .................................................... 5 

ADJUSTING THE FURNACE SYSTEM ............................................................... 6 

PREPARING THE MEASUREMENT................................................................... 7 

WHAT DO YOU NEED FOR THE MEASUREMENT? ..................................................... 7 

CALIBRATION ................................................................................................... 8 

CALIBRATION KITS ............................................................................................ 8 

CALIBRATION OF THE BALANCE ........................................................................... 9 

THERMOSTATIC CONTROL OF THE MEASURING PART ............................................. 10 

SELECTION OF THE SAMPLE CARRIER SYSTEM ........................................................ 10 

PRETREATMENT OF NEW SAMPLE CARRIER SYSTEMS ............................................. 11 

PREPARING THE SAMPLE .................................................................................. 12 

POWDERED SOLIDS ......................................................................................... 12 

COMPACT SOLIDS ........................................................................................... 12 

FILMS ........................................................................................................... 12 

FIBERS .......................................................................................................... 13 

LIQUIDS ........................................................................................................ 13 

UNSTABLE SAMPLES ........................................................................................ 13 

EVAPORATION REACTIONS ............................................................................... 13 

MEASUREMENTS IN DEFINED ATMOSPHERES ........................................................ 14 

SELECT THE SAMPLE CRUCIBLE ........................................................................... 14 

WEIGH THE SAMPLE ........................................................................................ 14 

SELECTION AND PREPARATION OF CRUCIBLES ....................................................... 14 

COMPATIBILITY OF SOME SUBSTANCES AND CRUCIBLE MATERIALS .......................... 18 
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STARTING THE MEASUREMENT - SHORT INSTRUCTION ..................................... 20 

SELECTION OF THE GAS ATMOSPHERE ............................................................... 30 

STATIC CONDITIONS ........................................................................................ 31 

MEASUREMENTS UNDER STATIC CONDITIONS - THE PROS AND CONS ...................... 31 

DYNAMIC CONDITIONS .................................................................................... 32 

DYNAMIC CONDITIONS (DYNAMIC PROTECTIVE GAS ATMOSPHERE) ....................... 32 

DYNAMIC CONDITIONS (DYNAMIC REACTION GAS ATMOSPHERE) ......................... 32 

HINTS FOR USING PURGE GASES ................................................................ 34 

MEASUREMENTS UNDER VACUUM - WHAT SHOULD BE CONSIDERED! ................. 39 

TRANSPORT ........................................................................................... 40 

CLEANING ............................................................................................. 41 
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Preparing the Measurement 

In thermoanalytical investigations the test 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 (chapter V 

"Appendix"). 

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 

need for the 

measurement? 

Assemble the required materials before starting the 

measurement: 

• purge gases (sample chamber and balance) 

• liquid nitrogen (cooling low temperature furnace) 

• sealing tool for pressure-tight crucibles 

• tweezers 
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Calibration • Calibration of the instrument is a prerequisite for 

quantitative analysis of STA measurements. 

• There is a difference between temperature and enthalpy 

calibration. 

ATTENTION! 

• A complete recalibration of the instrument should be 

carried out at least once per year and additionally after the 

exchange of sample carriers, thermocouples or electronic 

components resp. before longer measurement runs. 

• A control of the calibration should be made at least once 

per month or on spec of contamination or explicit changes 

of the test conditions. 

control period reference material 

once per month gold 

Calibration Kits Calibration kits for weight and enthalpy/temperature 

calibration can be supplied with the STA 449 F1. 

A detailed description of the calibration procedure can be 

found in the Software Manual and the enclosed calibration 

reports. 
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Calibration of the 

Balance 

A complete recalibration of the balance should be carried 

out at least once per year and additionally after transport, 

repairs and considerable changes in the test parameters 

(e.g. changing the sample carrier). 

To get a well calibrated balance the following conditions are 

necessary: 

• The balance should be in absolute equilibrium with stable 

TG signal! 

• The instrument with it’s built in electronic should be 

switched on at least one day! 

• Perform the balance calibration under static conditions 

without gas flow! 

• The furnace should be at room temperature! 

• The last measurement with heating should be finished the 

day before, if possible! 

Proceed as follows: 

• Open the NETZSCH measurement software. 

• Select the menu: Diagnosis. 

• Select: Balance Calibration. 

• Start Calibration. 

The complete procedure (step by step) is described when 

starting it. 
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Thermostatic control 

of the measuring 

part 

Switch on the thermostat minimum 2 hours before starting a 

measurement. 

For better thermostatic control switch on the thermostat 

overnight before measurement. 

Do not switch off the thermostat overnight if the equipment is 

to be used the next day. 

Set the thermostat temperature approx. 2°C above ambient 

temperature. 

Selection of the 

sample carrier 

system 

The sample carrier systems can be selected according to the 

application range (TG, DTA/DSC) and working temperature. 

The use of individual thermocouples is restricted to certain 

temperature ranges due to the type of thermocouple material.

The measuring conditions must be selected so that the 

required working temperature can be reached without the 

sample carrier system being damaged. A suitable combination 

of furnace type and sample carrier system must be found. 

Some sample carrier systems can only be used under defined 

gas atmosphere conditions. Detailed instructions for using 

purge and filler gases will be given later in this manual. 
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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. 
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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). 

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. 
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Measurements in 

defined 

atmospheres 

For measurements in defined atmospheres, a needle should be 

used to pierce one to five holes in the lid of the crucible. 

Select the sample 

crucible 

 See page 18: "Compatibility of some substances 

 and crucible materials" in this 

chapter. 

Weigh the sample − Weigh the sample with an analytical balance. 

Accuracy: ± 0.01 mg 

− 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. 

Selection and 

preparation of 

crucibles 

?

− Do not touch the crucibles by hand. Use 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 carrier when heated above 1000°C. 
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− 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 the 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 or Al2O3 liners. 

− Cover the crucibles with a thin layer of platinum 

paint on the outer surface of wall, bottom and lid 

to improve the radiation behaviour. 

− 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 900°C.
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How to insert an Al

2

O3 liner into a Pt crucible

alumina liner

Pt crucible

1

2

1) Pick up the alumina liner with the tweezers. 

2) Hold the platinum crucible with the fingers of the other 

hand (wear clean gloves). 

The platinum crucible should not be 

deformed.

3

3) The dimensions of the alumina liner and the platinum 

crucible are very similar (good thermal contact). 

To insert the liner in the crucible without damaging 

either part rotate them in opposite directions while 

moving the Al2O3 liner into place. 

Remove the alumina liner in the same way. 
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?

If the Al2O3 liner does not fit in the crucible:

• Using the supplied reshaping tool roll the platinum 

crucible on a hard, clean support. 

• Now the Al2O3 liner can be easily inserted.

Use the tool for reshaping deformed or 

dented crucibles as well.

Pt crucible tool for reshaping

support
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Compatibility of some Substances and Crucible Materials 

The table below corresponds to our most current information. No claim is made that it is 

exhaustive. The user should regard it only as a guide. 

Because this is a compilation of data from the literature (H. K. Cammenga et al., 

Thermochimica Acta, 219, 1993) and from our own experience it is not possible to cover all 

possible combinations and measurement conditions. In case of doubt, it is advisable to run 

preliminary tests in a separate furnace. 

For platinum crucibles with Al2O3

 inliners basically the same data like for corundum 

crucibles applies. The only exception is nickel as a calibration substance. The melting point 

of nickel with 1455°C is above the recommended maximum working temperature for Pt 

crucibles on a type S sample carrier. 

substance 

crucible 

material

C5H10 H2O Ga In Sn Pb Zn Li2SO4x 

H2O 

Al Ag Au 

corundum, Al2O3 0 0 + + + + + + + + + 

bornitride, BN 0 0 + + + + + + + ? ? 

graphite, C 0 0 + + + + + + + + - 

silicate glass + + + + + + ? + - x x 

fused silica, SiO2+ + + + + + + + - + + 

aluminium, Al + . - + - + - + x x x 

Al, oxidized + + + + + + + + x x x 

silver, Ag + + - - - - - ? - x x 

gold, Au + + . . - - - + - - x 

nickel, Ni + + . . . . . ? - + - 

iron, Fe + . . + . + - ? - + - 

fine steel + + . + . + - ? - + - 

platinum, Pt + + . . - - - + - - - 

molybdenum, Mo + + . ? . ? . ? ? ? - 

tantalum, Ta + + ? + ? ? ? + - + - 

tungsten, W 0 0 . ? ? . + ? . + + 

 

Source: Die Temperaturkalibrierung dynamischer Kalorimeter 

 II. Kalibriersubstanzen, H. K. Cammenga, PTB-Mitteilungen 102 1/92 

+ no solubility, no influence on the melting temperature 

- melt dissolves the crucible material, significant change of melting temperature 

. partial solution process, change of melting temperature may be ignored 

x crucible melts 

? compatibility unknown 

0 combination cannot be realized 
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Measuring metal samples in noble metal crucibles leads to alloy 

formation. It can cause dissolution of the crucible material and 

destruction of the sample carrier (sensor). 

The following materials are critical for PLATINUM: 

- halogens (Cl2

, F2, Br2), aqua regia 

- Li2CO3, prior to emission of CO2

- SiC from approx. 1000°C 

- PbO, FeCl3

- Be alloys (begin to evaporate just above the melting point) 

- HCl with oxidation agents (e.g. chromic acid, manganates, iron(III) salts, molten 

salts) 

- reducing atmospheres 

- Pb, Zn, metalls such as Pb, Zn, Sn, Ag, Au, Hg, Li, Na, K, Sb, Bi, Ni, Fe, steel, As, Si 

- Se above 320°C (immediate cooling and removal of the sample at the end of the 

measurement recommended to prevent evaporation of selenium) 

- metal oxides with reducing substances such as C, organic compounds or H2

- oxide in an inert gas atmosphere at higher temperatures (reduction) 

- sulfur → roughening the surface 

- alkali hydroxides, alkali carbonates, alkali sulfates, alkali cyanides and alkali 

rhodanides at higher temperatures 

- KHSO4

 at higher temperatures 

- carbon black or free carbon above 1000°C 

- SiO2

 under reducing conditions 

- SiC and Si3N4 at temperatures above 100°C 

- (release of elementary Si) 

- HBr, KCN solution at higher temperatures 

- high-temperature resistant oxides above 1000°C 

no resistance to: 

- mixtures of KNO3

 and NaOH at 700°C under exclusion of air 

- mixtures of KOH and K2S at 700°C under exclusion of air 

- LiCl at 600°C 

- Na2O2 at 500°C under exclusion of air 

- MgCl2, Ba(NO3)

2

 at 700°C 

- HBr, HJ, H2O2 (30%) and HNO3 at 100°C 

- KCl (the decomposition products which form during melting are damaging, 

melting point: 768°C) 

limited resistance to: 

- KHF2

, LiF, NaCl at 900°C 

- mixtures of NaOH and NaNO3

 at 700°C under exclusion of air 
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Starting the Measurement - Short Instruction 

Detailed information on the individual steps can be found in the 

hardware and software manuals. 

Explained below is how to: 

• create a baseline 

• set up a measurement 

• and measure a sample 

1. Switch on the 

thermostat at least 3 

hours before starting 

the measurement.

2. Switch on the 

computer system 

and measuring unit 

approx. 60 min. 

before starting the 

measurement. 
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3. Depending on your 

measurement 

conditions, have the 

required supplies 

available: 

liquid nitrogen, 

purge gases, etc.

4. Open the 

instrument.

a) Press "open button"+"safety button" at the same time 

and move the furnace into the upper end position (green 

LED on the "open button" is shining). 
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b) In the upper end position the furnace can be swung out by 

30° to the left or to the right (parking position). 

5. Insert two empty 

crucibles*. 

*for baseline 

(correction) 

measurements
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6. Close the 

instrument.

a) Swing the furnace back to the normal centered position.

b) Press "close button"+"safety button" at the same time 

and move the furnace into the lower end position (green 

LED on the "close button" is shining).
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7. Start the STA 449F1

measurement 

program. 

8. Proceed as shown to 

create a baseline: 

see separate 

software manual 

New

Measurement Definition

Last Items

- define Filename

Header

- sample Mass = 0!

- select temperature calibration file/

sensitivity calibration file

- define all sample settings (e.g. Identity, Name)

- define gases (purge and protective)

- select measurement type: Correction

Setup

- check the instrument setup

Temperature Program

- define all steps of the temperature program

click - Measure

the program switches to the adjustment window

File Menu
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9. Push Initial Cond. 

ON. Wait for stable 

balance. Start the 

measurement. 

If necessary check 

the Instrument 

Configuration. 

see separate 

software manual 

10. Prepare the sample.

Chapter IV 

 

 

11. Weigh the sample. 

Chapter IV 

 
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12. When the cell has 

cooled, open the 

instrument. 

a) Press "open button"+"safety button" at the same time 

and move the furnace into the upper end position (green 

LED on the "open button" is shining). 

b) In the upper end position the furnace can be swung out by 

30° to the left or to the right (parking position). 
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13. Remove the empty 

crucible (front) and 

place the sample 

crucible on the 

front-hand sample 

support.
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14. Close the 

instrument.

 

a) Swing the furnace back to the normal centered position. )

b) Press "close button"+"safety button" at the same time 

and move the furnace into the lower end position (green 

LED on the "close button" is shining).
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15.Proceed as shown to 

combine the sample 

measurement with 

the correction 

measurement: 

see separate 

 software manual 

Measurement Definition

Fast Definition

- enter the sample mass in mg!

- select measurement type: Correction+Sample

- define sample settings

e.g. to accept the settings from the 

correction measurement (e.g. Identity, Name) set the checkmark for 

Get these properties from just opened measurement

- define Filename

click - Measure

the program switches to the 

(see item 9)

adjustment window

File Menu

Open

use file from correction measurement!

sample mass = x mg!

16.Open the NETZSCH 

Proteus Analysis 

program. 

After the 

measurement is 

finished, you can 

start the evaluation.

see separate 

 software manual 
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Selection of the Gas Atmosphere

In principle the STA 449 F1 Jupiter allows measurements under the following conditions: 

• dynamic gas flow 

• static gas atmosphere 

• vacuum 

Figure 4: gas flow diagram STA 449 F1 Jupiter 
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Static Conditions 

Static conditions mean that the furnace chamber is filled with gas and this filler gas will not 

be exchanged during measurement. The gas outlet valve must be closed. 

 

Measurements under Static Conditions - the Pros and Cons 

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. These deposits impair the stability behaviour of the STA 449 F1 Jupiter. 

Higher problems arise if aggressive gases reach the weighing system. This can lead to a 

damage of the weighing system. 

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. 

If nevertheless you want to do static measurements: 

- switch off the all gas connections 

- close the outlet valve 

Measurements with closed outlet valve lead to a pressure increase inside the system. The 

measuring results are falsified (drift). 

Our recommendation: 

Run the STA 449 F1 Jupiter in dynamic protective gas atmosphere (see page 32 in this 

chapter). 
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Dynamic Conditions 

In dynamic mode the sample chamber is purged with gas during measurement. The gas 

outlet valve must be opened. 

Dynamic Conditions (Dynamic Protective Gas Atmosphere) 

The balance chamber must always be purged with inert protective gas. In case of dynamic 

measurements there is a protection of the weighing system by a continuous inert gas flow. 

The protective gas (pure, inert, dry) must 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 

gases. 

Dynamic Conditions (Dynamic Reaction Gas Atmosphere) 

ATTENTION!

Penetration of corrosive purge gas into the balance chamber must be avoided! 

- The balance chamber must always be purged with inert protective gas. 

- Preadjust the flow rates of inert and reaction gas. 

- Evacuate the measuring part. 

- Introduce protective gas through the valve "protective" until pressure compensation 

has been reached. 

- Wait until the inert gas flow has been stabilised. 

- Introduce the reaction gas through the valve "purge 1/purge2". 
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Recommended purge gas rates: 

Purge 1: approx. 50 ml/min 

Purge 2: approx. 50 ml/min 

Protective: 20 ml/min 

The reaction gas can also be introduced at a defined temperature. 

We recommend introducing the reaction gas during an isothermal 

heating segment (heating rate = constant). The gas flow becomes stable 

after some minutes. 

ATTENTION! 

Do not open the instrument after finishing the measurement until the 

sample temperature has fallen below 300°C. 

Fill the instrument until pressure compensation is reached before 

opening. 
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Hints for using Purge Gases 

Inert gases, air and some reaction gases (non toxic, non flammable) can be used. 

ATTENTION! 

In order to avoid environmental hazards or damage to the instrument, the following instructions must be followed when using filler or purge gas:

• The measuring part is a vacuum tight, sealed construction. It is therefore possible to 

carry out measurements in a controlled sample atmosphere. 

• To ensure safety while measuring at application temperatures above 1000°C it is imperative that ceramic parts are used in the reaction area (sample and furnace chamber). 

These parts are naturally exposed to stress due to permanent temperature changes. 

Thus cracks can develop and leakages occur especially in the hot zone. Due to the 

special properties of ceramic materials these defects cannot be predicted in advance and 

are therefore unavoidable even with regular preventative servicing (exchange of parts). 

• Dry, inert gases are recommended for purging the sample chamber. Prior to the introduction of gas a leakage test should be carried out whilst pre-evacuating the system in 

order to assure the purity of the sample atmosphere. We also recommend that the expelled purge gas be passed into a suitable exhaust hood. Depending on the measuring 

conditions (sample material, atmosphere, temperature range) derivative products can 

also be formed due to thermal reactions when using inert gases. These products (e.g. 

HCN, CO, SO2

, dioxin) even in small amounts are very detrimental to health and must 

not be allowed to pass into the work room. 

• Humid gas mixtures may only be used if condensations inside furnace and balance 

system can be avoided. If a humid gas mixture is cooling down, the water begins to 

condensate at a certain temperature. This temperature is called the dew point. The 

temperature must not fall below this limit. NETZSCH offers special furnace types. 

• The user must decide in advance whether toxic gases might be released during a 

measurement. The safety precautions are absolutely essential if this should be the fact. 
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When the measurement requires special reaction gases to be used in the sample chamber 

then a safety check of the potentially hazardous gas or gas mixture is imperative. In this 

case the following aspects have to be taken into consideration: 

• Do explosive gas mixtures or explosive compounds evolve when the sample has contact 

with oxygen (air)? 

• Is it certain that no toxic compounds can evolve from the gases or gas mixtures when 

using the chosen application temperatures? In this connection possible reactions 

between the purge gas in the weighing chamber and the reaction gas in the sample 

chamber should also be investigated. 

• Can it be ruled out that the gases neither corrode the leads nor the seals which are used 

in either the system or the surrounding equipment (valves, manometer or flow meter)? 

If not, leakages are to be expected. 

• Which side effects do the gases or gas mixtures have on the system's accessories? These 

effects do not result in leakages but would considerably increase wear and tear or could 

lead to a total failure of the system. 

The following rules must definitely be noted and followed: 

ATTENTION! 

Under no circumstances may explosive gas mixtures be used. 

• When using flammable gases which form explosive compounds upon contact with 

oxygen (air) or when using toxic compounds normal installation of the apparatus in an 

exposed part of the laboratory is forbidden. 

• Hazards to the measuring part due to defects in the sample chamber area can be 

avoided by installing a controllable surrounding (glove compartment). When using 

flammable gases the instrument can be placed in an oxygen-free environment; in addition appropriate sensor systems enable the escape of hazardous gases to be easily detected. The latter is also true for toxic gases or compounds. 

As limitations exist for certain parts of the instrument when being used in an oxygen-free 

atmosphere it is recommended that the manufacturer be contacted if necessary. For 

example certain heating elements cannot be used up to the given maximum temperature 

when in an inert atmosphere because they need the oxide forming oxygen atmosphere for 

the preservation of their protective coating. 

Information concerning the possibilities 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. 
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Helium (He) 

Chemically inert (inert gas) 

No technical safety limitations 

Argon (Ar) 

Chemically inert (inert gas) 

Asphyxiating 

No technical safety limitations 

Argon should not be used for low temperature investigations 

Nitrogen N2

Largely inert 

Asphyxiating 

No technical safety limitations but sample reactions are possible in the high temperature 

range. 

Air 

Oxidizing 

No technical safety limitations but sample reactions are possible. Application is possible 

above room temperature (maximum application temperature is determined by furnace material, sample carrier type, crucible material). The oxygen could liquefy if used in the low 

temperature range (LN2). 

Oxygen (O2) 

Increases flammability 

(must not come into contact with fats or oils) 

No technical safety limitations but hefty reactions are possible with the sample. 

Application is possible above room temperature (maximum application temperature is determined by furnace material, sample carrier type, crucible material). Liquefaction could occur in the low temperature range (LN2

). 

Carbon dioxide (CO2) 

Non-toxic 

(MAK value 5000 vpm) 

Non-flammable 

Application is possible above room temperature. 

Hydrogen (H2

) 

The instrument is not destined and suitable for use under hydrogen atmosphere. 

It can happen that explosible mixtures are formed inside the system during the respective 

experiments. 
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Ammonia (NH3) 

Toxic 

(MAK value 50 vpm) 

Flammable 

Danger of explosion when in contact with oxygen. 

For safety reasons it is forbidden to use an instrument that has been installed in the normal 

way. 

Corrosion of seals is possible. 

Carbon monoxide (CO) 

Toxic 

(MAK value 10 vpm) 

Flammable 

Corrosive 

For safety reasons it is forbidden to use an instrument that has been installed in the normal 

way. 

Hydrogen sulphide (H2S) 

Toxic 

(MAK value 10 vpm) 

Flammable, corrosive 

For safety reasons it is forbidden to use an instrument that has been installed in the normal 

way. 

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. 

Chlorine (Cl2) 

Very toxic 

(MAK value 5 vpm) 

Non-flammable, corrosive, caustic 

For safety reasons it is forbidden to use an instrument that has been installed in the normal 

way. 

Hydrogen chloride (HCl) 

Toxic 

(MAK value 5 vpm) 

Non-flammable, corrosive, caustic 

For safety reasons it is forbidden to use an instrument that has been installed in the normal 

way. 
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Sulphur dioxide (SO2) 

Toxic 

(MAK value 2 vpm) 

Non-flammable, corrosive 

For safety reasons it is forbidden to use an instrument that has been installed in the normal 

way. 

Fluorine (F2

) 

Very toxic 

(MAK value 0.1 vpm) 

Encourages burning, corrosive, caustic 

For safety reasons it is forbidden to use an instrument that has been installed in the normal 

way. 

Hydrogen fluoride (HF) 

Very toxic 

(MAK value 3 vpm) 

Very caustic, corrosive 

For safety reasons it is forbidden to use an instrument that has been installed in the normal 

way. 

Gaseous hydrocarbon 

Can form explosive gas mixtures with air 

For safety reasons it is forbidden to use an instrument that has been installed in the normal 

way. 

MAK values 2006 
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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 weighing is pre-programmed. 

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. 

Measurements under vacuum 

Measurements under vacuum should only be carried out up to maximum 

furnace temperatures of 1400°C. Higher temperatures may cause damages on 

the instrument. 

Hints for the use of the STC in case of measurements under vacuum 

In case of measurements under vacuum with end temperatures up to the 

maximum furnace temperature we recommend to switch off the STC (Sample 

Temperature Controller). As the STC controls the sample temperature by the 

deviation between sample and furnace thermocouple, this can cause problems 

with furnace control (oscillation). In the worst case the furnace can be 

overheated. The STC can be switched on and off in the software (see Help 

system in the Proteus software).