TGA

Thermogravimetric Analyzer
General

Thermogravimetry is a technique in which the mass of the sample is TGA 1000

monitored against time or temperature while the temperature of the
sample, in a specified atmosphere, is programmed. This technique ser-
ves the determination of material compositions. It is a common used
analysis method in the chemical and pharmaceutical industry. Thermo-
gravimetric analysis (TGA) is performed on polymers, food, pharmaceu-
ticals as well as many other materials.
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 aca-
demic teaching and day to day laboratory quality control applications.
TGA 1000 HiRes

Unsurpassed performance Research grade TGA equipped with an ultra high resolution sub micro-
gram balance. The low mass design in combination with the ceramic
L - DSC – Combined weight change and differential scanning calori- high speed furnace provides just the right tool for demanding resear-
meter chers. In combination with the 64 position autosampler and the software
Unsurpassed sensitivity – sub microgram balance with thermostatic controlled evacuation and gas dosing option the TGA can tackle deman-
controlled measurement chamber ding sample runs completely unattended.
Benchmark resolution – for detection of
fast weight changes
Reliable Automation – up to 64 position
autosampler
Ultra Fast Heater – Ceramic heater with
up to 200°C/min

2
Software

All LINSEIS thermo analytical instruments are PC controlled. The • Evaluation of mass loss
individual software modules exclusively run under Microsoft ®
• Residue mass evaluation
Windows® operating systems. The complete software consists of
3 modules: temperature control, data acquisition and data evalu- Features-Software:
ation. The 32 bit software incorporates all essential features • Program capable of text editing
for measurement preparation, execution, and evaluation of a • Data security in case of power failure
Thermogravimetric measurement. Thanks to our specialists and ap- • Thermocouple break protection
plication experts, LINSEIS was able to develop comprehensive easy to • Repetition measurements with minimum parameter input
understand user friendly application software. • Evaluation of current measurement
• Curve comparison up to 32 curves
• Storage and export of evaluations
TG – Features: • Export and import of data ASCII
• Mass change as % and mg • Data export to MS Excel
• Rate Controlled Mass Loss • 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 Software packages

3
Unique Features

Measurement system Gas dosing system

The platinum measuring system enables precise TGA measurements. The TGA 1000 HiRes (TGA 1000 optional feature) incorporates an au-
The unique L-Calc DSC sensor attachment permits differential scanning tomatic gas dosing system (MFC Mass Flow Controller) containing two
calorimeter signals. gas channels. The flow rate of the two gases is software controlled.

Options Atmosphere

The following options are available for the TGA: The balance design enables measurements under inert, oxidative, re-
GC, MS or FTIR coupling for evolved gas analysis (EGA) Turbo-molecular ducing and vacuum conditions. Corrosive conditions can be analyzed
pump: for measurements under highest vacuum and cleanest gas-at- with proper precautions. The system is capable of adapting residual gas
mospheres and a vapor generator. analysis systems using an optional heated capillary.

4
Specifications

Heater

Sample

Measuring
system

TGA 1000 TGA 1000 HiRes

Temperature range RT up to 1100°C TR up to 1100°C

Heating and Cooling Rates 0.01 to 150°C/min 0.001 to 200°C/min

Sample Mass 5g 2g

Resolution 0.5µg 0.1µg

Vacuum — Yes (optional)

Sample Carriers TGA TGA-DTA/DSC*

Sample Robot 20 Positions 64 Positions

230/208 VAC 230/208 VAC

Power requirements
50/60 Hz 50/60 Hz

*calculated.: DTA/DSC

5
Applications

Decomposition of Calcium Oxalate monohydrate

CaC2O4 ∙ H2O under Argon Atmosphere
Time [min ]
0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95

28
0 Mass change
35
dM-rel[Ca-Ox-1]
The evolved gases from the decomposition of Calcium Oxalate have
-12.13% 26
-5 30
Mass change 24
-10 -18.69%
25

been fed into the Mass Spectrometer with a heated capillary. The ion
22
-15 20
979.8°C 20
-61.0%
-20 15

currents for mass numbers 18 (water), 28 (carbon monoxide) and 44

18
-25 10 Mass change
-30.05%

Ion Current_18 [E-12 A]

DTA Signal[Ca-Ox-1] 16

DTA Signal [µV]

dM-rel [%]
5
-30

(carbon dioxide) have been imported into the graph.

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
25 0.04
0.0 dM-rel[B_10-1] Mass change
20 -0.26% 0.02

-0.2 15 Mass change 0.00

-0.17%

-0.4
10
5 Mass change
-1.83%
-0.02
-0.04
tri calcium aluminates. After putting on the cement with water different
0 811.1°C -0.06

hydrates slowly form. The absorbed water evaporates first, then hy-
-0.6
145.0°C
-5 751.7°C -0.08
463.0°C
-0.8 -10 -0.10

-15 -0.12

drates of the calcium silicate decompose and at 570°C the hydroxides

dM-rel(derived) [%/min]

-1.0 DTA Signal [B_10-1]

DTA Signal [mV]

-20 -0.14
dM-rel [%]

-25 -0.16
-1.2
-0.18

of calcium, magnesium and aluminum follow. Subsequently, calcium

-30
-1.4 -0.20
-35
-0.22
-1.6 -40

carbonate CO2 splits off.

-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]

Vitriol of Copper

Inorganic salts first set their crystal water free. Vitriol of Copper heated
3.0 DTA Signal smoothed [CUSO-1]
2 Mass change
2.0 -14.08%
0 0.0
-2 1.0

with 10°C/min. results in a first TG stage, which corresponds to 4H2O. -4

-6
0.0
-1.0
1.0

-8 -2.0 2.0

TG and DTA show that the curve is made up of two separate steps, -10
-12
-3.0
-4.0
Mass change
-14.30% 3.0
DTA Signal (smoothed) [µV]

dM-rel(derived) [%/min]

-14 -5.0

one closely behind the other. At around 250°C the most strongly bound
4.0
-16 -6.0
dM-rel [%]

-18 -7.0
5.0
-20 -8.0

water evaporates. -22

-24
-9.0
-10.0
6.0

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]

6
Dehydration of raw gypsum CaSO4 ∙ 2 H2O

The dehydrate is Raw gypsum. There are two molecules of water atta-
5.0
0 45 dM-rel[GIPS1B1] 4.5
4.0
40

ched to a single CaSO4 molecule. By heating up to app. 160°C the semi

-2
3.5

35 3.0
-4
2.5

hydrate gypsum is built. 1,5 molecules of water are released; so two -6

30 2.0

DTA Signal (smoothed) [µV]

1.5
25

DTA Signal(1.Deriv .) [µV/°C]

-8 1.0

CaSO4 molecules are sharing a single water molecule. By heating to

dM-rel [%]
20 0.5
-10
DTA Signal(1.Deriv .) [GIPS1B1] 0.0
15

higher temperatures (400°C) the anhydrate is built. This is the socalled

-0.5
-12
-1.0
10 235.3°C
-14 -2.48µV/°C -1.5

„dead burned gypsum“, also known as alabaster. In this state no water -16
5

0
DTA Signal [GIPS1B1]

199.5°C
-2.0
-2.5
-0.25µV/°C -3.0

at all is attached to the CaSO4 molecules.

-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]

Decomposition of Rubber
1000
950
900
0
dM-rel[rubber]

DTA Signal[rubber]
Mass change -9.27% 5.0
4.5
In the first step of weight loss, the dehydration of the sample takes
-5 4.0

place. The amount of water was 9.27%. In the second reaction step,
850
3.5
800 -10
3.0
750
Dehydration
Mass change
2.5

the volatile components are released by pyrolysis under N2 atmosphere.

-15 -35.99%
700
2.0
650 -20
1.5
DTA Signal(1.Deriv.) [µV/°C]

600

The amount of these components is 35.99%. For the third reaction step,
-25 1.0
Temperature [°C]

550
dM-rel [%]

0.5
500 -30 0.0

the atmosphere is changed to O2 – all organic components are burned

450
-0.5
-35
400
-1.0
350 Mass change
-40 Temperature [rubber] -14.33% -1.5
300
250 -45
Release of volatile parts
-2.0
-2.5
out. The loss in weight is 14.33%. The remaining rest of 40.41% are
200
-50 -3.0
150
100 -55
-3.5
-4.0
inorganic components like ashes, slake or fillers.
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 relea- 0 6

dM-rel[Asp-1] Mass change
-27.03%
1.0

-5 0.0
4

sed, resulting in a weight loss of around 1%. At 140°C the melting point
<< Endo Exo>>

-10 DTA-Signal (smoothed) [Asp-1] Mass change

2
-1.10% -1.0
-15 Dehydration
0
-20

of the Aspirin is reached, resulting in an exothermic reaction, measured Mass change -2.0
-2 -50.85%
-25
-4
DTA-Signal (smoothed) [µV]

-30 -3.0
DTA Signal(1.Deriv.) [µV/°C]

on the DTA trace. At 160°C the decomposition of the melted drug takes -35 -6
-4.0
dM-rel [%]

-40 -8
-45

place in several stages. Since the decomposition products are volatile a

-10 -5.0
-50
-12
-55 -6.0

weight loss of just about 80% occurs.

-14
-60
-7.0
-16
-65

-70 -18 -8.0

Mass change
-75 -20 142.8°C -18.2µV -3.44%
Melting -9.0
-80 -22
-85
-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]

7
 LINSEIS GmbH LINSEIS Inc.
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95100 Selb Robbinsville, NJ 08691
Germany USA
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

Products: DIL, TG, STA, DSC, HDSC, DTA, TMA, MS/FTIR, In-Situ EGA, Laser Flash, Seebeck Effect
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