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THERMO-GRAVIMETRIC
ANALYZER
TGA 1000
T H E R M A L A N A L Y S I S
2
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.
Customer satisfaction, innovation, flexibility
and high quality are what LINSEIS represents.
Thanks to these fundamentals, our company
enjoys an exceptional reputation among the
leading scientific and industrial organizations.
LINSEIS has been offering highly innovative
benchmark products for many years.
The LINSEIS business unit of thermal analysis
is involved in the complete range of thermo
analytical equipment for R&D as well as qual-
ity control. We support applications in sectors
such as polymers, chemical industry, inorganic
building materials and environmental analytics.
In addition, thermo physical properties of solids,
liquids and melts can be analyzed.
LINSEIS provides technological leadership. We
develop and manufacture thermo analytic and
thermo physical testing equipment to the high-
est standards and precision. Due to our innova-
tive drive and precision, we are a leading manu-
facturer of thermal Analysis equipment.
The development of thermo analytical testing
machines requires significant research and a
high degree of precision. LINSEIS Corp. invests
in this research to the benefit of our customers.
Claus Linseis Managing Director
3
InnovationWe want to deliver the latest and best tech-
nology for our customers. LINSEIS continues
to innovate and enhance our existing thermal
analyzers. Our goal is constantly develop new
technologies to enable continued discovery in
science.
German engineeringThe strive for the best due diligence and ac-
countability is part of our DNA. Our history is af-
fected by German engineering and strict quality
control.
4
GENERAL
5
Thermogravimetry is a technique in which the
mass of the sample is monitored against time or
temperature while the temperature of the sam-
ple, in a specified atmosphere, is programmed.
This technique serves the determination of ma-
terial compositions. It is a common used analy-
sis method in the chemical and pharmaceutical
industry. Thermogravimetric analysis (TGA) is
performed on polymers, food, pharmaceuticals
as well as many other materials.
Unsurpassed performance L - DSC – Combined weight change and diffe-
rential scanning calorimeter
Unsurpassed sensitivity – sub microgram ba-
lance with thermostatic controlled measure-
ment chamber
Benchmark resolution – for detection of fast
weight changes
Reliable Automation – up to 64 position au-
tosampler
Ultra Fast Heater – Ceramic heater with up to
200°C/min
TGA 1000The LINSEIS TGA 1000 is a robust and reliable
TGA outperforming most competition high end
models. The sub microgram balance offers high-
est sensitivity and resolution. The instrument is
perfectly suited for academic teaching and day
to day laboratory quality control applications.
TGA 1000 HiResResearch grade TGA equipped with an ultra
high resolution sub microgram balance. The
low mass design in combination with the cera-
mic high speed furnace provides just the right
tool for demanding researchers. In combination
with the 42/82 position autosampler and the
software controlled evacuation and gas dosing
option the TGA can tackle demanding sample
runs completely unattended.
6
SOFTWARE
7
All LINSEIS thermo analytical instruments
are PC controlled. The individual software
modules exclusively run under Microsoft®
Windows® operating systems. The com-
plete software consists of 3 modules: tem-
perature control, data acquisition and data
evaluation. The 32 bit software incorpo-
rates 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 un-
derstand user friendly application software.
TG – Features:• Mass Change as % and mg
• Rate Controlled Mass Loss
• Evaluation of Mass Loss
• Residue Mass Evaluation
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
• Data export to MS Excel
• Multi-methods analysis (DSC TG, TMA, DIL,
etc.)
• Zoom function
• 1 and 2 derivation
• Programmable gas control
• Statistical evaluation package
• Free scaling
• Optional Kinetic and Lifetime Prediction Soft-
ware packages
8
UNIQUE FEATURESMeasurement systemThe platinum measuring system enables pre-
cise TGA measurements. The unique L-Calc DSC
sensor attachment permits differential scanning
calorimeter signals.
OptionsThe following options are available for the TGA:
GC, MS or FTIR coupling for evolved gas analy-
sis (EGA) Turbo-molecular pump: for measure-
ments under highest vacuum and cleanest gas-
atmospheres and a vapor generator.
Gas dosing systemThe TGA 1000 HiRes (TGA 1000 optional feature)
incorporates an automatic gas dosing system
(MFC Mass Flow Controller) containing two gas
channels. The flow rate of the two gases is soft-
ware controlled.
AtmosphereThe balance design enables measurements un-
der inert, oxidative, reducing and vacuum con-
ditions. Corrosive conditions can be analyzed
with proper precautions. The system is capable
of adapting residual gas analysis systems using
an optional heated capillary.
9
Sample
Heater
Measuringsystem
10
SPECIFICATIONS
TGA 1000
Temperature range RT up to 1100°C
Heating and Cooling Rates 0.01 to 150°C/min
Sample Mass 5g
Resolution 0.1µg
Vacuum —
Sample Carriers TGA
Sample Robot 42 Positions
Power requirements 230/208 VAC50/60 Hz
TGA 1000 HiRes
Temperature range RT up to 1100°C
Heating and Cooling Rates 0.001 to 200°C/min
Cool down time from 1000°C to100°C in under 10min
Sample Mass 2g
Resolution 0.1µg
Vacuum Yes (optional)
Sample Carriers TGA-DTA/DSC*
Sample Robot 84 Positions
Power requirements 230/208 VAC50/60 Hz
*calculated: DTA/DSC
11
APPLICATIONS
Dehydration of raw gypsum
45
40
35
30
25
20
15
10
5
0
-5
-10
0 20 40 60 80 100 120 140 160 180 200 220 240 260 280 300 320 340 360 380 400
5.0
4.5
4.0
3.5
3.0
2.5
2.0
1.5
1.0
0.5
0.0
-0.5
-1.0
-1.5
-2.0
-2.5
-3.0
-3.5
-4.0
-4.5
-5.0
dM-rel[GIPS1B1]0
-2
-4
-6
-8
-10
-12
-14
-16
-18
-20
-22
dM-r
el [%
]
DTA
Sign
al (s
moo
thed
) [µV
]
Temperature (smoothed) [°C]
DTA
Sign
al(1
.Der
iv.)
[µV/
°C]
DTA Signal [GIPS1B1]
DTA Signal(1.Deriv .) [GIPS1B1]
199.5°C-0.25µV/°C
210.0°C-15.8%
235.3°C-2.48µV/°C
368.0°C20.9%
The dehydrate is raw gypsum. There are two molecules of wa-ter attached to a single CaSO4 molecule. By heating up to app. 160°C the semi hydrate gypsum is built. 1,5 molecules of wa-ter are released; so two CaSO4 molecules are sharing a single water molecule. By heating to higher temperatures (400°C) the anhydrate is built. This is the socalled „dead burned gyp-sum“, also known as alabaster. In this state no water at all is at-tached to the CaSO4 molecules.
Inorganic salts first set their cry-stal water free. Vitriol of Copper heated with 10°C/min. results in a first TG stage, which cor-responds to 4H2O. TG and DTA show that the curve is made up of two separate steps, one closely behind the other. At around 250°C the most strongly bound water evaporates.
Vitriol of copper
3.0
2.0
1.0
0.0
-1.0
-2.0
-3.0
-4.0
-5.0
-6.0
-7.0
-8.0
-9.0
-10.0
-11.0
-12.0
-13.0
-14.0
-15.0
-16.0
-17.0
40 60 80 100 120 140 160 180 200 220 240 260 280 300
0.0
1.0
2.0
3.0
4.0
5.0
6.0
7.0
8.0
9.0
10.0
dM-rel[CUSO-1]
Mass change-14.08%
Mass change-14.30%
Mass change-7.25%
2
0
-2
-4
-6
-8
-10
-12
-14
-16
-18
-20
-22
-24
-26
-28
-30
-32
-34
-36
-38
-40
dM-r
el [%
]
DTA
Sig
nal (
smoo
thed
) [µV
]
Temperature (smoothed) [°C]
dM-r
el(d
eriv
ed) [
%/m
in]
DTA Signal smoothed [CUSO-1]
12
35
30
25
20
15
10
5
0
-5
-10
-15
-20
-25
-30
0 100 200 300 400 500 600 700 800 900 1000
28
26
24
22
20
18
16
14
12
10
8
6
4
2
0
0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95
dM-rel[Ca-Ox-1]Mass change-12.13%
Mass change-18.69%
Mass change-30.05%
Ion Current_18[Ca-Ox]
DTA-Signal[Ca-Ox-1]
Ion Current_28[Ca-Ox]
Ion Current_44[Ca-Ox]
0
-5
-10
-15
-20
-25
-30
-35
-40
-45
-50
-55
-60
dM
-rel
[%]
DTA
-Sig
nal
[µV
]
Temperature (smoothed) [°C]
Ion
Cu
rren
t_1
8 [E
-12
A]
Time [min]
979.8°C-61.0%
25
20
15
10
5
0
-5
-10
-15
-20
-25
-30
-35
-40
-45
-50
-55
-60
-65
-70
-75
0 100 200 300 400 500 600 700 800 900 1000
0.04
0.02
0.00
-0.02
-0.04
-0.06
-0.08
-0.10
-0.12
-0.14
-0.16
-0.18
-0.20
-0.22
-0.24
-0.26
-0.28
-0.30
-0.32
-0.34
-0.36
dM-rel[B_10-1] Mass change-0.26%
Mass change-0.17%
Mass change-1.83%
0.0
-0.2
-0.4
-0.6
-0.8
-1.0
-1.2
-1.4
-1.6
-1.8
-2.0
-2.2
-2.4
dM
-rel
[%]
DTA
Sig
nal
[mV
]
Temperature (smoothed) [°C]
dM
-rel
(der
ived
) [%
/min
]
DTA Signal [B_10-1]
145.0°C463.0°C
751.7°C811.1°C
Cement
The evolved gases from the decomposition of calcium oxa-late has been fed into the mass spectrometer with a heated capillary. The ion currents for mass numbers 18 (water), 28 (carbon monoxide) and 44 (car-bon dioxide) have been impor-ted into the graph.
Decomposition of CaC2O4 • H2O
The main parts of cement are tri calcium silicate, di calcium silicate and tri calcium alumi-nates. Hydrates slowly form af-ter mixing cement with water. The absorbed water evaporates first. Hydrates of the calcium silicate decompose at 570°C. The hydroxides of calcium, ma-gnesium and aluminum follow. Subsequently, CO2 splits off from calcium carbonate.
13
0
-5
-10
-15
-20
-25
-30
-35
-40
-45
-50
-55
-60
0 5 10 15 20 25 30 35 40 45 50 55 60
5.0
4.5
4.0
3.5
3.0
2.5
2.0
1.5
1.0
0.5
0.0
-0.5
-1.0
-1.5
-2.0
-2.5
-3.0
-3.5
-4.0
-4.5
-5.0
1000
950
900
850
800
750
700
650
600
550
500
450
400
350
300
250
200
150
100
50
0
Tem
pera
ture
[°C]
dM-r
el [%
]
Time [min]
DTA
Sig
nal(1
.Der
iv.)
[µV/
°C]
Dehydration
DTA Signal[Rubber 2]
Release of volatile parts
Burn out of organic parts
dM-rel[Rubber 2] Mass change -9.27%
Mass change-35.99%
Mass change-14.33%Temperature [Rubber 2]
Atmosphere: N2 Atmosphere: O2
In the first step of weight loss, the dehydration of the sam-ple takes place. The amount of water was 9.27%. In the se-cond reaction step, the volatile components are released by pyrolysis under N2 atmosphere. The amount of these compo-nents is 35.99%. For the third reaction step, the atmosphere is changed to O2 – all organic components are burned out. The loss in weight is 14.33%. The remaining rest of 40.41% are inorganic components like ashes, slake or fillers.
Aspirin
6
4
2
0
-2
-4
-6
-8
-10
-12
-14
-16
-18
-20
-22
-24
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
1.0
0.0
-1.0
-2.0
-3.0
-4.0
-5.0
-6.0
-7.0
-8.0
-9.0
-10.0
∆M
rel [
%]
DTA-
Sign
al (s
moo
thed
) [µV
]
Temperature (smoothed) [°C]
DTA
Sign
al(1
.Der
iv.)
[µV/
°C]
DTA-Signal (smoothed) [Asp-1]
<< E
ndo
Exo>
>
Mas
s ch
ange
-3.4
6%
∆Mrel[Asp-1]
Mas
s ch
ange
-51.
21%
Mas
s ch
ange
-28.
03%
Mass change -1.12% Dehydration
143.5°C -18.2µVMelting
0
-10
-20
-30
-40
-50
-60
-70
-80
-90
At the beginning of the heating process some adsorbed water is released, resulting in a weight loss of around 1%. At 140°C the melting point of the Aspirin is reached, resulting in an exo-thermic reaction, measured on the DTA trace. At 160°C the de-composition of the melted drug takes place in several stages. Since the decomposition pro-ducts are volatile a weight loss of just about 80% occurs.
Decomposition of rubber
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Products: DIL, TG, STA, DSC, HDSC, DTA, TMA, MS/FTIR, In-Situ EGA, Laser Flash, Seebeck Effect, Thin Film Analyzer, Hall-Effect
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11/18
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