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Simultaneous Thermal Analysis
Simultaneous Thermal Analysis
Simultaneous Thermal Analysis
ANALYSIS
Since 1957 LINSEIS Corporation has been deliv-
ering outstanding service, know how and lead-
ing innovative products in the field of thermal
analysis and thermo physical properties.
2
German engineering Innovation
The strive for the best due diligence and ac- We want to deliver the latest and best tech-
countability is part of our DNA. Our history is af- nology for our customers. LINSEIS continues
fected by German engineering and strict quality to innovate and enhance our existing thermal
control. analyzers. Our goal is constantly develop new
technologies to enable continued discovery in
Science.
3
SIMULTANEOUS
THERMAL ANALYSIS
Simultaneous TGA-DTA/DSC measures both, of the results. The complimentary information
heat flow and weight change of a sample as a obtained allows differentiation between endo-
function of temperature or time under control- thermic and exothermic events which have no
led atmosphere. Simultaneous measurement of associated weight change (e.g., melting and cry-
these two material properties not only improves stallization) and those which involve a weight
productivity but also simplifies interpretation change (e.g., degradation).
Sample holder
Beam
Counter
weight
Our different microbalances are specifically de- Providing ultra light weight design to follow fast
signed to accomplish thermal analysis tasks in weight changes and symmetric construction for
the best possible way. ultra low drift long term measurements.
4
DSC- True Heat Flow measurement
Quantitative DSC-signal
Sample Reference
∆TS=T±x ∆TS=T±0 Reference signal
TM Sample signal
T M melting temperature
Time (s)
Peak area A
~ heat of melting (J/g)
ΔT = T r -T s
Time (s)
Ts = sample temperature
Tr = reference temperature
∆T=TS–TR
Measurable Properties
5
SENSORS
Our STA can be equipped with an unmatched Each sensor is available with different thermo-
amount of different user exchangeable TG-DSC, couples to provide the highest sensitivty for
TG-DTA or TG sensors. your desired temperature range.
TG-DSC Al2O3
Platinum
Aluminium
others
custom volume
0.12ml 0.12ml
TG-DTA
Cap
0.3ml or
custom volume
Crucible
DTA-sensor
6
TGA
custom volume
0.14 ml 0.12 ml
TG-hang- down wire Wheel TG-sample holders for many different applications
60
Type K
Thermoelectric Voltage [mV]
40 Type C
20 Type S
Type B
0
-20
-500 0 500 1000 1500 2000 2500
Temperature [°C]
All sensors available with the thermocouples illustrated. LINSEIS Senosor combinations
cover the broadest temeprature range in the market (-180 up to 2400°C).
7
UNIQUE FEATURES
Vacuum and controlled
atmosphere
The balance design provide for high vacuum,
inert, reducing, oxidiz ing or humidified atmos-
phere. Furthermore, the instrument can be pres-
surized up to 5 bar overpressure (option). Cer-
tain corrosive conditions can be analyzed with
proper precautions. The system is capable of
adapting residual gas analysis systems using an
optional heated capillary.
Sample robot
Our STA PT 1000 and 1600 can be equiped with
a proven sample robot for unattended sample
measurements.
8
of the sample gas capillary. It is used to getter
smallest traces of residual oxygen in the sample
chamber by offering a stronger oxygen affinity
than sample materials, combined with a high ef-
fective surface to ensure the oxygen molecules
react with the getter before they have a chance
to get in touch with the sample. Especially for
Starter kit oxidation sensitive samples, where hydrogen
The starter kit includes a variety of tools such gas mixtures can’t be used or very small enthal-
as scissors, cutting tools, anti electrostatic py signals are expected, the OGM is a very effec-
tweezers, magnifier, crucible holder, pipette, tive and easy to use solution. With its modular
rasps, spatula etc. character, it can be used for special experiments
and can be easily removed for measurements
Oxygen Getter Material OGM under air or where the oxygen content is less
The LINSEIS oxygen getter system (OGM) can be important.
placed in any LINSEIS system as a modification
Furnace Programm
Temperature Type Element Atmosphere TC-Type
-150 – -500°C L81/264 Kanthal inert, oxid., red., vac. K
-150 – 1000°C L81/264ER Kanthal inert, oxid., red., vac. K
RT – 1000°C L81/220 Kanthal inert, oxid., red., vac. K
RT – 1200°C L81/IR IR Heater inert, oxid., red., vac. S
RT – 1500°C L81/230Pt Precious Metal inert, oxid., red., vac. S
RT – 1600°C L81/240 SiC inert, oxid., red., vac. S
RT – 1650°C L81/240Rh Precious Metal inert, oxid., red., vac. B
RT – 1750°C L81/250 MoSi2 inert, oxid., red., vac. B
RT – 2000°C L81/260 Graphite inert., red., (oxid. up to 1750°C) C
RT – 2400°C L81/260 Graphite inert., red., (oxid. up to 1750°C) C
Special Furnaces
RT – 1600/1750°C L81/240/250 WV SiC/MoSi2 water vapor furnace
high speed furnaces up to
RT – 1100/1600°C L81/IR/HF IR/HF
100°C/s
9
optional
EGA
(FTIR/MS/GC-MS)
Heater
Sample
Reference
Gas flow
Vacuum
MFC
Gas
Purge
gas
Balance
10
Benefits of the vertical top
loading design
The vertical “sample on top” design of the ble accuracy due to a stable position of the sam-
LINSEIS thermobalance provides highest possi- ple and easy sample handling.
Advantages:
• Easy sample handling
• Easy exchange of sample holder
• Stable position of the sample in the furnace
(critical for good DTA/DSC and Cp results)
Disadvantage:
• Complicated construction
Horizontal system
Advantages:
• Small buoyancy effects
Disadvantages:
• Sensor exchange very difficult
• Sample handling difficult
• Very high purge gas rate required
• Problems due to sensor expansion during
heating/cooling
Advantage:
• Stable position within furnace
Disadvantages:
• Difficult sensor exchange
• “Dangerous” gas flow within balance housing (sample gets blown out)
• Sensor position depends on sample weight
11
STA PT 1000
Compact fully integrated TG- shortly after each other or almost similar. The
DSC/DTA for organic materi- LINSEIS STA PT 1000 has an integrated furnace
als control cycle that enables the system to stop
The STA PT1000 is dedicated to analysis of or- heating and perform heating rates with a mi-
ganic materials in a relatively low temperature nimum of overshooting so that a broad range
range up to 1000°C. of applications can be covered with the HiRes
The LINSEIS HiRes option for TGA allows ana- software option.
lyzing mass change effects with highest pos-
sible accuracy by effective trigger heating rate Design
changes. The software can detect a mass chan- build in furnace and gas control
ge that could be due to oxidation or decom- furnace with low thermal mass for unmatched
position. As a result the unit can automatically heating and cooling speed
adjust the heating rate or stop heating. After the
mass change is over, the system continues he- Sample robot
ating according to the set profile. This allows a optional 42 or 84 position sample robot is
better separation of effects that are taking place available
12
STA PT 1600
STA PT 1600/1 STA PT 1600/3
The highest resolution 0.025 µg balance for The high mass variant allows measuring samp-
small sample quantities allows the detection of les with big volumes or weight 35/50g to deter-
very small effects with highest accuracy. mine even small effects within a big amount of
inhomogeneous material.
STA PT 1600/2
The standard model covers a broad application
TG - DSC/DTA + Pressure
range with excellent resolution 0.1 µg and accu-
racy.
13
STA HIGH PRESSURE
14
High pressure & high temperature
Taylor made STA product for challenging cu-
stom applications
On Request
Achievable Pressure
350 bar
150 bar
100 bar
50 bar
15
SOFTWARE
All LINSEIS thermo analytical instruments are • Optional Kinetic and Lifetime Prediction
software controlled. The individual software • Software packages
modules run exclusively under Microsoft ®
16
Thermal Library
The LINSEIS Thermal Library software package The Thermal Library allows you the comparison
comes as an option for the well-known, user of the complete curves with a data base provi-
friendly LINSEIS Platinum evaluation software ding thousands of references and standard ma-
that is integrated in almost all our instruments. terials within only 1-2 seconds.
n
t i fi catio
rial Iden
Mate
and
g n i tion
co
u r ve re ystem
c s
DSC retation
p
inter
Measured and matching reference curves (green) and reference curves with poor fit (red).
Multi-Instrument Multi-Lingual
All LINSEIS instruments DSC, DIL, STA, HFM, LFA, Our software is available in many different
etc. can be controlled from one software tem- user exchangable languages, such as: English,
plate. Spanish, French, German, Chinese, Korean,
Japanese, etc.
Report Generator
Convenient template selection to generate cu- Multi-User
stomized measurement reports. The administrator can generate different user
levels providing different rights to operate the
instrument. A optional Log file is available, too.
Data Base
State of the art data base design enables easy Kinetic software
data handling. Kinetic analysis of DSC, DTA, TGA, EGA (TG-MS,
TG-FTIR) data for the study of the thermal beha-
vior of raw materials and products.
17
OTS OXYGEN GETTER
18
TECHNICAL SPECIFICATIONS
STA PT 1000 STA PT 1600 STA HP/2
RT up to 1100/
Temperature range RT up to 1000°C -150 up to 2400°C
1400°C/1600°C/1800°C
up to 150 bar
Pressure up to 5 bar (optional)
custom solution on request
TG 1 2 3
Sample weight 5g 5g 25 g 35 / 50 g 15 / 25 g 35 / 50 g
25 / 2500 25 / 2500
Measuring range 25 / 2500 mg 35000 mg 25 / 2500 mg 35000 mg
mg mg
DSC
DSC resolution 0.3 / 0.4 / 1µW 0.3 / 0.4 / 1 / 1.2 µW 0.3 / 0.4 / 1 / 1.2 µW
Calorimetric sensitivity approx. 4 / 6 / 17.6 µW approx. 4 / 6 / 17.6 / 22.5 µW approx. 4 / 6 / 17.6 / 22.5 µW
DTA
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APPLICATIONS STA PT 1000
Decomposition of rubber
In the first step of weight loss,
the dehydration of the sam-
1000 ple takes place. The amount of
dM-rel[Rubber 2] Mass change -9.27% 5.0
0
950
DTA Signal[Rubber 2] 4.5 water was 9.27%. In the second
900
-5 4.0 reaction step, the volatile com-
850
3.5
800 -10 ponents are released by pyro-
3.0
Dehydration
750 Mass change
2.5
lysis under N2 atmosphere. The
-15 -35.99%
700
2.0 amount of these components
650 -20
1.5 is 35.99%. For the third reaction
550
dM-rel [%]
0.5
500 -30 0.0
ged to O2 – all organic com-
450
-35
-0.5 ponents are burned out. The
400
350 Mass change
-1.0
loss in weight is 14.33%. The
-40 Temperature [Rubber 2] -14.33% -1.5
300 remaining 40.41% are inorganic
-2.0
-45
250
Release of volatile parts -2.5 components like ashes, slake or
200
-50 -3.0 fillers.
150
-3.5
100 -55
-4.0
50 Burn out of organic parts
-60 -4.5
0 Atmosphere: N2 Atmosphere: O2
-5.0
0 5 10 15 20 25 30 35 40 45 50 55 60
Time [min]
Aspirin
At the beginning of the heating
process some adsorbed water
is released, resulting in a weight
1.0
∆Mrel[Asp-1]
0 6 Mass change -1.12% Dehydration loss of around 1%. At 140°C the
4 0.0 melting point of the Aspirin is
<< Endo Exo>>
-10
Mass change
-3.0
DTA Signal(1.Deriv.) [µV/°C]
-40
-6 takes place in several stages.
-4.0
-8 The decomposition products
∆Mrel [%]
-60 -6.0
-14
-7.0
-70 -16
-18 -8.0
-80
-20
Mass change
-9.0
-22 143.5°C -18.2µV
-3.46%
-90 Melting
-24 -10.0
20 40 60 80 100 120 140 160 180 200 220 240 260 280 300 320 340 360 380 400 420 440 460 480 500 520
Temperature (smoothed) [°C]
20
STA HP
Hydrogen Adsorption on Titanium at 700°C
Activated, porous titanium sur-
face was heated to 700°C under
vacuum. At target temperature,
3.5
hydrogen was added and the
pressure was increased in an
3.0 isothermal stage. The weight
increase of the sample gives the
2.5 amount of hydrogen that is ad-
Adsorped Hydrogen [%]
1.5
1.0
0.5
0
0 0.05 0.1 0.5 5
Pressure [bar]
Coal gasification
Coal was heated under nitro-
gen atmosphere at 50bar pres-
sure. The mass signal shows the
50.0
CO + H2 Pressure: 50.0 bar
H2O [sccm/min]
48.0
Pressure [bar]
0.5
N2 [l/min]
–250 47.5
0
–300 47.0
–0.5 –2.0
–350 46.5
–1.0
–400 100% –3.0
coal 46.0
–1.5 gasified
–450
–4.0 45.5
21
STA PT 1600
Decomposition of CaC2O4 • H2O
The evolved gases from the
decomposition of calcium oxa-
Time [min] late has been fed into the mass
0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95
spectrometer with a heated
28
0
35 Mass change capillary. The ion currents for
dM-rel[Ca-Ox-1] -12.13% 26
-5 30
mass numbers 18 (water), 28
Mass change 24
-10 25
-18.69% (carbon monoxide) and 44 (car-
-15 20
22
bon dioxide) have been impor-
979.8°C
-61.0%
20
ted into the graph.
-20 15
18
DTA-Signal [µV]
5
-30 14
0
-35 Ion Current_18[Ca-Ox] 12
-5
-40 10
-10
-45 8
-15
-50 6
-20
4
-55 Ion Current_28[Ca-Ox]
-25
2
-60
-30 Ion Current_44[Ca-Ox]
0
0 100 200 300 400 500 600 700 800 900 1000
Temperature (smoothed) [°C]
Cement
The main parts of cement are
tri calcium silicate, di calcium
silicate and tri calcium alumi-
25 0.04
0.0
20
dM-rel[B_10-1] Mass change
-0.26% 0.02
nates. Hydrates slowly form af-
-0.2 15 Mass change
-0.17%
0.00 ter mixing cement with water.
-0.4
10 -0.02
The absorbed water evaporates
5 Mass change -0.04
0
-1.83%
-0.06
first. Hydrates of the calcium
-0.6 811.1°C
145.0°C
-5 463.0°C
751.7°C -0.08 silicate decompose at 570°C.
-0.8 -0.10
-10
The hydroxides of calcium, ma-
dM-rel(derived) [%/min]
-15 -0.12
DTA Signal [mV]
-20
22
Long term baseline stability
The average baseline stabili-
ty during linear heating up to
50 1600°C is within a range of 5µg.
This allows highest accuracy
40 and repeatability during the
30 most demanding applications
on STA.
20
10
Delta m [µg]
-10
-20
-30
-40
-50
0 200 400 600 800 1000 1200 1400 1600
Temperature [°C]
Modulated cp determination
For highest possible accuracy
of Cp, the LINSEIS STA and DSC
allow the usage of modula-
ted temperature profiles. This
5.0 800 1.70 technique causes a continuous
1.60 change in heat flow of the sam-
700 ple and the system can monitor
1.50
the heat uptake much better
0 600 1.40
Temperature [°C]
Cp mode Saph raw data (HDSC) then with a linear heating pro-
HDSC [µV]
Cp [J/(gK)]
23
LINSEIS GmbH Germany LINSEIS Inc. USA
Vielitzerstr. 43 109 North Gold Drive
95100 Selb Robbinsville, NJ 08691
Tel.: (+49) 9287–880 - 0 Tel.: (+1) 609 223 2070
Fax: (+49) 9287–70488 Fax: (+1) 609 223 2074
E-mail: info@linseis.de E-mail: info@linseis.com
LINSEIS Poland
ul. Dabrowskiego 1
05-800 Pruszków
Tel.: (+48) 692-773-795
www.linseis.com
Products: DIL, TG, STA, DSC, HDSC, DTA, TMA, MS/FTIR, In-Situ EGA, Laser Flash, Seebeck Effect, Thin Film Analyzer, Hall-Effect
Services: Service Lab, Calibration Service
03/18