T H E R M A L A N A L Y S I S

THERMO- TGA 1000

GRAVIMETRIC
ANALYZER
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
Claus Linseis
analytical equipment for R&D as well as qual- Managing Director
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.

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
GENERAL

4
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 1000
The 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.

5
SOFTWARE

6
All LINSEIS thermo analytical instruments Features-Software:
are PC controlled. The individual software • Program capable of text editing
modules exclusively run under Microsoft ®
• Data security in case of power failure
Windows® operating systems. The com- • Thermocouple break protection
plete software consists of 3 modules: tem- • Repetition measurements with minimum
perature control, data acquisition and data parameter input
evaluation. The 32 bit software incorpo- • Evaluation of current measurement
rates all essential features for measurement • Curve comparison up to 32 curves
preparation, execution, and evaluation of a • Storage and export of evaluations
Thermogravimetric measurement. Thanks to • Export and import of data ASCII
our specialists and application experts, LINSEIS • Data export to MS Excel
was able to develop comprehensive easy to un- • Multi-methods analysis (DSC TG, TMA, DIL,
derstand user friendly application software. etc.)
• Zoom function
TG – Features: • 1 and 2 derivation
• Mass Change as % and mg • Programmable gas control
• Rate Controlled Mass Loss • Statistical evaluation package
• Evaluation of Mass Loss • Free scaling
• Residue Mass Evaluation • Automatic calibration
• Optional Kinetic and Lifetime Prediction Soft-
ware packages

7
UNIQUE FEATURES
Measurement system
The platinum measuring system enables pre-
cise TGA measurements. The unique L-Calc DSC
sensor attachment permits differential scanning
calorimeter signals.

Options
The 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 system

The 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 software controlled.

Atmosphere
The 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.

Automatic calibration
We offer an automatic calibration function in
the software and hardware. With this function,
our TGA automatically calculates a calibration
factor, which is also displayed.

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Heater

Sample

Measuring
system

9
SPECIFICATIONS
TGA 1000

Design Top-loading

Temperature range (10°C) RT up to 1100°C

Heat and Cooling rates 0.001 up to 250°C/min

Sample mass max. 5g

Resolution 0.1µg

Gas atmosphere Inert, ocid, red., vaccum

Vacuum up to 10E-2mbar

Gas Dosing built-in MFC block with 3 gases

(one Purge gas and two reactive gases)

Cool down speed <12min (1100°C - 100°C)

Sample Carriers TGA

Sample robot 42 positions

Crucible Pt, Al2O3, Au, Al, Ag etc. others on request

EGA Couplings Optional FTIR and/or MS or GC-MS

Interface USB

10
APPLICATIONS
Vitriol of copper
Inorganic salts first set their cry-
stal water free. Vitriol of Copper
3.0 DTA Signal smoothed [CUSO-1]
heated with 10°C/min. results
2 Mass change
0 2.0 -14.08%
0.0 in a first TG stage, which cor-
-2 1.0
responds to 4H2O. TG and DTA
-4 0.0 1.0
-6 -1.0
show that the curve is made
-8 -2.0 2.0 up of two separate steps, one
-10 -3.0
Mass change
3.0
closely behind the other. At
-12 -4.0 -14.30%
around 250°C the most strongly
DTA Signal (smoothed) [µV]

dM-rel(derived) [%/min]
-14 -5.0
4.0
-16 -6.0 bound water evaporates.
dM-rel [%]

-18 -7.0
5.0
-20 -8.0
-22
-9.0 6.0
-24
-10.0
Mass change
-26 -7.25%
-1
1.0 7.0
-28
-12.0
-30 dM-rel[CUSO-1] 8.0
-13.0
-32
-14.0
-34 9.0
-15.0
-36
-16.0
-38 10.0
-17.0
-40
40 60 80 100 120 140 160 180 200 220 240 260 280 300
Temperature (smoothed) [°C]

Dehydration of raw gypsum

The dehydrate is raw gypsum.
There are two molecules of wa-
ter attached to a single CaSO4
5.0
molecule. By heating up to app.
0 45 dM-rel[GIPS1B1] 4.5
4.0
160°C the semi hydrate gypsum
40
-2
3.5 is built. 1,5 molecules of wa-
3.0
-4 35 ter are released; so two CaSO4
2.5

-6
30 2.0
molecules are sharing a single
water molecule. By heating to
DTA Signal (smoothed) [µV]

1.5
25
DTA Signal(1.Deriv .) [µV/°C]

-8 1.0
higher temperatures (400°C)
dM-rel [%]

20 0.5
-10
DTA Signal(1.Deriv .) [GIPS1B1] 0.0
the anhydrate is built. This is
-12
15 -0.5 the socalled „dead burned gyp-
10 235.3°C
-1.0
sum“, also known as alabaster.
-14 -2.48µV/°C -1.5

5 DTA Signal [GIPS1B1] -2.0

In this state no water at all is at-
-16
199.5°C -2.5 tached to the CaSO4 molecules.
0
-0.25µV/°C -3.0
-18
210.0°C -3.5
-5 368.0°C
-15.8%
-20 20.9% -4.0
-10 -4.5
-22 -5.0
0 20 40 60 80 100 120 140 160 180 200 220 240 260 280 300 320 340 360 380 400
Temperature (smoothed) [°C]

11
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]

Ion Current_18 [E-12A]

-25 10 Mass change
-30.05% 16
DTA-Signal[Ca-Ox-1]
dM-rel [%]

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]

-1.0 DTA Signal [B_10-1]

-0.14 gnesium and aluminum follow.
dM-rel [%]

-20

-1.2 -25 -0.16 Subsequently, CO2 splits off

-0.18
-1.4
-30 from calcium carbonate.
-0.20
-35
-0.22
-1.6 -40
-0.24
-45
-1.8 -0.26
-50
-0.28
-55
-2.0 -0.30
-60
-0.32
-2.2 -65
-0.34
-70
-2.4 -0.36
-75
0 100 200 300 400 500 600 700 800 900 1000
Temperature (smoothed) [°C]

12
Decomposition of rubber
In the first step of weight loss,
the dehydration of the sam-
ple takes place. The amount
1000
dM-rel[Rubber 2] Mass change -9.27% 5.0 of water was 9.27%. In the se-
950 0

900
DTA Signal[Rubber 2] 4.5 cond reaction step, the volatile
-5 4.0
850
3.5
components are released by
800 -10
Dehydration
3.0 pyrolysis under N2 atmosphere.
750 Mass change
2.5
700
-15 -35.99% The amount of these compo-
2.0
650 -20
1.5 nents is 35.99%. For the third

DTA Signal(1.Deriv.) [µV/°C]

600
-25 1.0 reaction step, the atmosphere
Temperature [°C]

550
dM-rel [%]

0.5
500 -30 0.0
is changed to O2 – all organic
450
-35
-0.5 components are burned out.
400
-1.0
350 -40
Mass change The loss in weight is 14.33%.
Temperature [Rubber 2] -14.33% -1.5
300
-2.0 The remaining rest of 40.41%
250 -45

200
Release of volatile parts -2.5 are inorganic components like
-50 -3.0
150
-3.5
ashes, slake or fillers.
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
∆Mrel[Asp-1]
1.0 loss of around 1%. At 140°C the
0 6 Mass change -1.12% Dehydration

0.0
melting point of the Aspirin is
4
reached, resulting in an exo-
<< Endo Exo>>

-10
Mass change

DTA-Signal (smoothed) [Asp-1]

2
-1.0
-28.03%

0
thermic reaction, measured on
-20

-2
-2.0 the DTA trace. At 160°C the de-
-30
-4 composition of the melted drug
DTA-Signal (smoothed) [µV]

-3.0
DTA Signal(1.Deriv.) [µV/°C]

-40
-6 takes place in several stages.
-4.0
-8 Since the decomposition pro-
∆Mrel [%]

-50 -10 -5.0 ducts are volatile a weight loss

Mass change

-12 of just about 80% occurs.

-51.21%

-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]

13
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01/23