First SIM - WORKSHOP

Thermal analysis (TGA/DSC):

practical aspects
TGA Thermogravimetric Analysis
DSC Differential Scanning Calorimetry

Jacek Chwast
jacek.chwast@ees.kuleuven.be
Geo-Instituut

23.01.2013

Measurement conditions
Netzsch STA 409 PC Luxx:
- T [25 1000 C]
- heating rate 10 C/min
- N2 atmosphere (60 ml/min)
- alumina crucibles
- simultaneous measurement of mass
change (TG) and heat flow (DSC)
- 1 analysis (25100025 C) = 3 hrs

furnace

microbalance

Measurement conditions
furnace

Netzsch STA 409 PC Luxx:

- T [25 1000 C]
- heating rate 10 C/min
- N2 atmosphere (60 ml/min)
- alumina crucibles
- simultaneous measurement of mass
change (TG) and heat flow (DSC)
- 1 analysis (25100025 C) = 3 hrs

sample + reference

microbalance

Thermal analysis (TGA/DSC) in a nutshell

TG analysis mass (T)

DSC analysis heat flow (T)

T
G/m
g

D
T
G/(m
g/m
in
)

0
.0
0
0
[1
]

-0
.5
0
0

[1
]ce
m
I1
A4
d
.dsv
T
G
D
T
G

-1
.0
0
0

0
.0
-0
.1
-0
.1

-1
.5
0
0

O
n
se
t*: 4
2
9
.2C
-0
.2

-2
.0
0
0
-0
.2

-2
.5
0
0
[1]

1
0
0
.0

2
0
0
.0

3
0
0
.0

4
0
0
.0

5
0
0
.0
6
0
0
.0
7
0
0
.0
T
e
m
pe
ra
ture/C

8
0
0
.0

9
0
0
.0

-0
.3

1
0
0
0
.0

Examples of thermal reactions resulting in

mass change, measured by TG analysis:
-loss of free water
-loss of bound water
-decomposition
TG applications:
-identification and quantification of sample
components
-thermal stability studies

Examples of thermal reactions resulting in

heat flow, measured by DSC analysis:
-crystallization
-melting
-glass transitions
DSC applications:
-thermodynamic characterization of pure
substances
-quality control: sample purity
4
-thermal stability studies

Sample compatibility
Requirements:
- no reaction with alumina crucible
- no expansion or creep during thermal decomposition
Compatible materials (KUL expertise):
- clays and other geological materials
- cements
- slags
Limitations:
- polymers can be hazardous, as they can foam at high
temperatures,
- compatibility assessment is necessary for new materials
5

Evaluation of new materials

Compatibility assessment:
by providing a reference to a thermal analysis
or
by burning the sample in a furnace
at the conditions foreseen for the measurement:

sample composition
temperature range (max. 1000 C)
inert atmosphere
alumina crucible

Sample preparation
1) Sample form:

fine powders
compact solids
films, fibers

2) Ensure good thermal contact between

sample and heat flux-sensor:

powders: evenly distributed at the bottom

of the sample crucible, gently tamped

3) Always use the same

sample mass (~ 10-30 mg)

Analysis of results
Software: NETZSCH Proteus (Marsh procedure)
Quantification of portlandite (Ca(OH)2) content in cement
T
G/m
g

~430C: Ca(OH)2 -> CaO + H2O

0
.0
0
0

D
T
G/(m
g/m
in)
[1]

-0
.5
0
0

[1
]ce
m
I1
A4
d
.d
sv
T
G
D
T
G

-1
.0
0
0

0
.0
-0
.1
-0
.1

-1
.5
0
0

O
n
se
t*: 4
2
9
.2C
-0
.2

-2
.0
0
0
-0
.2

-2
.5
0
0
[1]

1
0
0
.0

2
0
0
.0

3
0
0
.0

4
0
0
.0

5
0
0
.0
6
0
0
.0
7
0
0
.0
T
e
m
pe
ra
tu
re/C

8
0
0
.0

9
0
0
.0

-0
.3

1
0
0
0
.0

Analysis of results
Software: NETZSCH Proteus (Marsh procedure)
Quantification of portlandite (Ca(OH)2) content in cement

~430C: Ca(OH)2 -> CaO + H2O

T
G
/m
g

[1
]c
e
m
I1
A4
d
.d
s
v
T
G

-1
.7
0
0
-1
.8
0
0

mass
loss

-1
.9
0
0
-2
.0
0
0

[1
]

-2
.1
0
0
4
0
0
.0

4
2
0
.0

4
4
0
.0

4
6
0
.0
T
e
m
p
e
ra
tu
re/C

4
8
0
.0

5
0
0
.0

Analysis of results
Software: NETZSCH Proteus (Marsh procedure)
Quantification of portlandite (Ca(OH)2) content in cement

~430C: Ca(OH)2 -> CaO + H2O

T
G
/m
g

[1
]c
e
m
I1
A4
d
.d
s
v
T
G

-1
.7
0
0
-1
.8
0
0
-1
.9
0
0
-2
.0
0
0

[1
]

-2
.1
0
0
4
0
0
.0

4
2
0
.0

4
4
0
.0

4
6
0
.0
T
e
m
p
e
ra
tu
re/C

4
8
0
.0

5
0
0
.0

10

Analysis of results
Software: NETZSCH Proteus (Marsh procedure)
Quantification of portlandite (Ca(OH)2) content in cement

~430C: Ca(OH)2 -> CaO + H2O

T
G
/m
g

[1
]c
e
m
I1
A4
d
.d
s
v
T
G

-1
.7
0
0

M
a
s
sL
o
s
s(M
a
rs
h
):
O
n
s
e
t:
4
3
1
.7C
In
fle
c
tio
n
:
4
4
0
.4C
M
a
s
sC
h
a
n
g
e
: -0
.2
5
8m
g

-1
.8
0
0
-1
.9
0
0
-2
.0
0
0

[1
]

-2
.1
0
0
4
0
0
.0

4
2
0
.0

4
4
0
.0

4
6
0
.0
T
e
m
p
e
ra
tu
re/C

4
8
0
.0

5
0
0
.0

11

Contact information and reservations

Contact / Training:
Jacek Chwast
jacek.chwast@ees.kuleuven.be
tel. +32 16 3 27593 or +32 16 3 27580
Responsible professor: Jan Elsen
TG /DSC instrument:
Geo-Instituut
Celestijnenlaan 200c
Room 01.83
Reservations:
- fill in the reservation list in the room 01.83
12

Thank you for your attention

Questions?

13