DSC 131 Manual

G/DSC131-1A
DSC 131
COMMISSIONING
UTILIZATIONS
DSC 131 - Commissioning/Utilizations
CONTENTS
CONTENTS ................................................................................................................ I
REVISIONS TABLE ................................................................................................ I
WARNING TO USERS .................................................................................................1
CHAPTER 1 COMMISSIONING...................................................................................2
1.
2.
3.
4.
5.
6.
PRESENTATION ...........................................................................................................................2
2. INSTALLATION .........................................................................................................................3
2.1. Location .......................................................................................................................................4
2.2. Dimensions and weight................................................................................................................4
2.3. Electrical circuit...........................................................................................................................4
ELECTRICAL AND COMPUTER CONNECTIONS .................................................................................5
3.1. Electrical connections ..................................................................................................................5
3.2. Computer connections .................................................................................................................5
FLUID CONNECTIONS ...................................................................................................................6
4.1. Sweeping gas circuit ....................................................................................................................6
4.2. Cooling circuit .............................................................................................................................8
4.2.1. Air cooling........................................................................................................................8
4.2.2. Cooling accelerator...........................................................................................................9
4.2.3. Cooling with a cryogenic plunging device .....................................................................10
4.2.3.1. Device ___________________________________________________________________10
4.2.3.2. First commissioning _________________________________________________________11
4.2.3.3. Utilization_________________________________________________________________11
4.2.3.4. Stopping the device _________________________________________________________12
4.2.4. Liquid nitrogen cooling device.......................................................................................12
COMMISSIONING OF THE CALORIMETRIC TRANSDUCER................................................................ 13
5.1. Presentation................................................................................................................................13
5.2. Commissioning ..........................................................................................................................14
TECHNICAL CHARACTERISTICS .................................................................................................. 15
6.1. DSC 131.....................................................................................................................................15
6.2. Cryogenic device .......................................................................................................................16
6.3. Materials in contact with the gas ...............................................................................................16
6.4. Conforming to standards............................................................................................................16
CHAPTER 2 - UTILIZATIONS .....................................................................................20

1.
SELECTING THE CRUCIBLE ........................................................................................................ 20

1.1. Low-volume aluminum crucible................................................................................................21
1.1.1. Description .....................................................................................................................21
1.1.2. Crimping.........................................................................................................................21
1.1.3. Utilization .......................................................................................................................22
1.2. Medium-volume aluminum crucible..........................................................................................23
1.2.1. Description .....................................................................................................................23
Contents

1.2.2. Crimping.........................................................................................................................23
1.2.3. Utilization .......................................................................................................................26
1.3. High Pressure crucible 500 bars 600C S60/58186..................................................................27
1.3.1. Description .....................................................................................................................27
1.3.2. Crimping.........................................................................................................................28
1.3.3. Utilization .......................................................................................................................30
1.3.3.1. Instructions for use __________________________________________________________30
2.
PREPARING THE EXPERIMENT.................................................................................................... 31
2.1. Weighing a sample.....................................................................................................................31
2.2. Placing crucibles in the DSC .....................................................................................................32
2.3. Selecting the sweeping gas ........................................................................................................33
2.4. Entering experimental conditions ..............................................................................................33
2.4.1. PID actions .....................................................................................................................34
2.4.2. Safety temperature ..........................................................................................................34
2.4.3. Control valve and fan .....................................................................................................34
2.4.4. Scanning and sequencing ...............................................................................................35
2.4.4.1. Simple cycle _______________________________________________________________36
2.4.4.2. Staged cycle _______________________________________________________________37
2.5. Making use of the test................................................................................................................39
2.5.1. Thermogramme ..............................................................................................................39
2.5.2. Determining transformation temperatures (or times) .....................................................40
2.5.2.1. Endothermic transformation___________________________________________________40
2.5.2.2. Exothermic transformation____________________________________________________41
2.5.2.3. Glass transition_____________________________________________________________42
2.5.3. Temperature correction...................................................................................................43
2.5.3.1. Standard materials __________________________________________________________44
2.5.3.2. Experimenting _____________________________________________________________44
2.5.3.3. Temperature correction for a fixed scanning rate___________________________________46
2.5.3.4. Temperature correction for various scanning rates _________________________________47
2.6. Energy calibration......................................................................................................................48
2.6.1. Measuring the fusion heat of a pure substance...............................................................48
2.6.2. Standard materials ..........................................................................................................49
2.6.3. Experimenting ................................................................................................................50
2.6.4. Calibration with a single standard ..................................................................................50
2.6.5. Calibration with various standards .................................................................................51
APPENDIX A...........................................................................................................52
APPENDIX B...........................................................................................................53
APPENDIX C...........................................................................................................54
ANNEX D .............................................................................................................54
Contents
ii
REVISIONS TABLE
07/07/06 Add electrical scheme G/DSC131-1A
12/06/06
General corrections
J. DENIS
F/DSC131-1A
C. MATHONAT
T. THIMON / C. MATHONAT
A.FOUILLAT
01/06/06
New HP crucibles
21/06/05
Corrections
E/DSC131-1A
C. MATHONAT
D/DSC131-1A C.MATHONAT
C. CARTET
C. MATHONAT
23/02/05 Max N2Temperature
C/DSC131-1A C. MATHONAT
G.BOURDIN
C. MATHONAT
28/07/04 Modification of tight

crucible pressure use
B/DSC131-1A
26/09/03
P35 corrosive and

reducing gases use
caution adding
A/DSC131-1A J. PICOCHE
17/02/03
MODIFICATIONS
21/10/99
LAY OUT
REV
DATE
REVISION PURPOSE
REVISIONS TABLE
S. BENOIT
C.MATHONAT C. MATHONAT
C.MATHONAT/ C.MATHONAT
S.MARTINELLO
C/DSC131A P. FOURNIER
C. CARTET
C. MATHONAT
B/DSC131A
K. DAVAT
JL. DAUDON
DONE BY
APPROVED BY
J.L. DAUDON
BOOKLET REQUIRED BY
REF
WARNING TO USERS
Operating the instrument requires scientific and technical skill providing for
compliance with all the laws of chemistry and physics.
The specifications and applications of our products are always likely to be
modified. SETARAM will respond to any foreseeable damage directly linked to
faults in its instruments, within the limits of the obligatory provisions in the law
applying to the victim's action.
SETARAM is in no way liable for the damage resulting from experiments carried
out with its instruments. Non-compliance with the advice and instructions
contained in the commissioning or operating booklets will always be grounds for
excluding liability, in particular, in case of instruments alterations not expressly
approved by SETARAM.
Before commissioning the instrument, carefully read the instructions and fully
comply with every point. Commissioning of various instruments require strict
compliance with the directions and warnings contained in the various booklets.
To use peripheral instruments together with our apparatus (like for instance,
computer, thermostated bath, pump...), report to specific users manuals, delivered
with each peripheral in order to guarantee a good working order as well as a good
safety level of those equipments for our applications.
The instrument does not have a locking system preventing the access to the
transducer whereas it could be able to stay at a high temperature. It is necessary
to check this temperature thanks to the window Direct Programming (report to
the Setsoft booklet) before opening the instrument.
Safety recommendations:
Carry the instrument with carefulness.
Think that vibrations or a shock may cause damages inside the instrument.
Read carefully safety labels.
Do not remove any label!
Do not switch on the instrument in case it is damaged.
Before getting the instrument repaired, unplug it.
Do not switch on an instrument on which feed cable is damaged.
Once the instrument has been correctly installed, the customer will ensure that
those operating it have the technical and scientific skills. He will make sure that
Warning to users
G/DSC131-1A 07/07/06
the products worked upon, as well as the experimenting conditions, are not likely
to cause damage resulting from non-compliance with the laws of physics and
chemistry. The customer will also ensure, under his public liability, that the
instrument and its connections are not accessible to any operating or maintenance
staff unaware of the operating instructions.
Any use not corresponding exactly to the instrument's general specifications will
require initial contact being made with SETARAM.
The instruction leaflet enumerates other recommendations,
indicated through a triangle with an exclamation mark in it. Read
and follow carefully those recommendations! If you DO NOT, it
could generate serious consequences such as a breakdown,
material damages as well as hurting people badly and even kill
them.
Indicates a high temperature area.
Indicates an electric danger.
Indicates a low temperature area.
Indicates a risk of catching or crushing ones hand.
CHAPTER 1 COMMISSIONING
1. Presentation
Due to its experience in the technology of DSC analyzers, SETARAM has
developed a new analyzer called DSC 131.
Performances such as selectivity, sensitivity, rapidity are the result of the original
measuring principle used for the construction and operation of the DSC 131s
transducer.
This booklet shows the DSC 131 analyzer distinguished by the following features:
Warning to users
G/DSC131-1A 07/07/06
a single structure including the transducer, its cooling system and

microprocessor-controlled controller.
a multitask software package enabling piloting other modules (for instance
modules from the labsysTM line).
a varied range of crucibles available for the various types of experiment.
FIGURE 1: DSC 131
The DSC 131 instrument is designed for ease of operation while offering
robustness and high performance.
This instrument is appropriate for work in laboratories carrying out research and
quality control, in universities and schools, providing that the instructions given at
the beginning of this booklet are followed.
This instruction booklet -which contains various parts (commissioning,
utilization, maintenance, practical applications)- is especially intended for
commissioning the instrument and for describing the main operating modes.
Software operations will be dealt with separately.
2. 2. Installation
When a DSC 131 instrument has been ordered, the various parts
of the instrument are carefully checked and tested before
shipment.
Upon receipt of the equipment, carefully check the various parts
for their condition. Should any be damaged, make the customary
claim against the transport operator.
Check that the material delivered is the one you ordered.
Commissioning
G/DSC131-1A 07/07/06
2.1. Location
The DSC 131 instrument is best installed on a stable table, such as a laboratory
bench.
The instrument must be sheltered from draughts, and, if possible from the suns
rays, especially the rear panel (thermocouple measurement housing and preamplifier housing).
2.2. Dimensions and weight
The DSC 131 instrument has a compact structure including various elements: a
detector, a furnace and a controller.
A series cable connects the instrument to the computer, itself combined with a
printer-plotter.
Weight : 23 kg/56 lb
FIGURE 2: DIMENSIONS OF THE DSC 131
The unit should be carried by two persons and held at the bottom
of the structure.
2.3. Electrical circuit

The instrument is to be used at 230 Volts.
If any other voltage is required, a transformer to be fitted between
the instrument and the mains power point is to be added.
Commissioning
G/DSC131-1A 07/07/06
Do plug the instrument ONLY in a ground connection.
3. Electrical and computer connections

3.1. Electrical connections
A single supply cable on the rear panel is to be connected to the mains 230 V /2A
with ground connection (figure 3).
Refer to the Maintenance chapter in the Practical Work/Maintenance
booklet for any modification on cards.
Secteur
Main
Disjonteur
Circuit breaker
Port srie
Serial port
FIGURE 3: ELECTRICAL CONNECTIONS
3.2. Computer connections

As the computer models undergo frequent changes, instructions for
connecting the computer itself are subject to modifications. Information about
connections for a COMPAQ computer is given in the present chapter.
Note
Therefore, it is necessary to refer to the computers operating

booklet.
The instrument and more precisely the CS332 controller, is linked to the computer
via an RS232-series cable, containing 9-pin connectors at both ends.
Connections are as shown on the figure hereafter:
Commissioning
G/DSC131-1A 07/07/06
FIGURE 4: COMPUTER CONNECTIONS
series-cable between (1) (serial port controller) and (2) (computer)

screen cable between (3) (central unit) and (4) (screen)
printer/plotter cable between (5) (central unit) and (6) (printer/plotter)
connection cable for the mouse on (7)
connection cable for the keyboard on (8)
connection to the mains for the central unit on (9)
connection to the mains for the screen on (10)
If the connector on the computers series cable contains more than
9 pins, an adaptor -which is not supplied- is required.
4. Fluid connections
4.1. Sweeping gas circuit
The sweeping gas circuit aims at:
1. preventing the crucible and the sample from oxidizing,
2. preventing the DSC transducer from oxidizing when the temperature is higher
than 500C in isothermal condition or 600C in scanning condition (up to
5C.min-1).
3. imposing a gas different from the air.
Two possibilities are available according to the option:
1. A single sweeping gas linked to the inlet 1 on the rear panel. A regulation
valve is used to set the rate.
Commissioning
G/DSC131-1A 07/07/06
2. Automatic gas switching: two inlets identified as inlet 1 and inlet 2 are linked
to an electrovalve piloted via the software. A regulation valve to be found on
each inlet is used to set a rate. This option allows either two various gases to be
switched or a single gas to have two different rates (rapid purging to push the
air out before starting an experiment).
For gas connection, see Figure 5 hereafter:
Vanne de rglage
Entre 2
Control valve
Inlet 2
Entre 1
Inlet 1
Sortie
Outlet
Gaz
Gas
FIGURE 5: GAS CONNECTIONS
A gauge pressure with a pressure-relief valve is fixed on the gas bottle. Link the
gauge pressure outlet to the instrument inlet located on the rear panel. Reduce to a
pressure of about 1.5 bars.
Outlet of the experimenting chamber is connected to outlet on the instruments
rear panel.
Inlet and outlet on the instruments rear panel have unions (refer to Chapter 2 - 7 Gas connections on the rear panel in the Practical work/Maintenance booklet
for tightening the connections.)
The loss of mass is pre-adjusted in our workshop. A flowmeter must be used at
the instrument outlet to check or adjust the rate to the experiment. Rates of a few
liters per hour are recommended.
WARNING Fully tighten the unions around the pressure gauge to prevent any leak,
and the bottle from emptying rapidly.

To check the fluid-tightness:
Close the experimenting chamber with a stopper on the gas outlet.
Commissioning
G/DSC131-1A 07/07/06
Open the gas supply bottle and reduce the pressure to about 1.5 bars.
Open the pressure-relief valve.
Use soapy water or any other means of detecting leaks to test the various
connections.
Should there be a leak, further check the flexible hoses, and especially check that
the ends are finless.
WARNING The gas used or released by a sample after a reaction must be
chemically compatible with the various elements of the gas circuit (refer to the
chapter 1-6 in this booklet).
If a gas released by a sample is susceptible to be combustible or
toxic, Outlet, in the rear face of the instrument, must be linked to
a device insuring the safety of persons or goods.
4.2. Cooling circuit
4.2.1. Air cooling
The transducer is surrounded by a pipe (1) guiding the cooling air. A fan placed at
the far end of the pipe ensures the circulation of cooling air (see the figure
hereafter). The fan is controlled by the software on the window direct
programming or sequences.
Erreur ! Des objets ne peuvent pas tre crs partir des codes de champs de mise en forme.
FIGURE 6: AIR COOLING
Cooling the transducer is done via the pipe and provides for various operations:
Cooling the convector to protect the users.
Cooling the furnace support and protection of their various respective seals.
Cooling the instrument rapidly when from a high temperature (after heating
process) down to ambient.
The fan must always be On, unless in sub ambient use.
WARNING A safety thermostat cuts the power when the temperature of the
furnace base is higher than 100C.
Commissioning
G/DSC131-1A 07/07/06

4.2.2. Cooling accelerator
WARNING This device is designed to improve the thermal coupling between the
transducer and the heater and therefore natural cooling is increased at a maximum
speed.
Temperature/ C
500
450
400
350
300
250
200
150
100
50
dTemperature/ K/min
0
-5
-10
-15
-20
-25
-30
-35
-40
-45
-50
-55
Argon
Temperature/ C
5 10 15 20 25 30 35 40 45
Time/ min
dTemperature/ K/min
350
0
-20
-40
-60
-80
-100
-120
-140
-160
300
250
200
Helium
150
100
50
0
10
15
Time/ min
However, a lower increase in temperature and maximum speed will be observed

and especially under a sweeping of helium.
This device is composed of a bulky metal cylinder (1) located in the transducer's
base (2) and covered by the radiator (3).
It is mounted at the very beginning of the experiment and used during the whole
experiment.
1
3
2
FIGURE 7: COOLING ACCELERATOR
Commissioning
G/DSC131-1A 07/07/06
Under air, nitrogen, argon... the maximum temperature is 500C.
Under helium the maximum temperature is 300C and the

maximum speed is 30C/min.
4.2.3. Cooling with a cryogenic plunging device

4.2.3.1. Device
The device is composed of two inseparable subsets linked by an insulated sleeve.

The cold source itself is a mechanical two-stage cold generator. The fluid is
brought to the exchanger via the insulated sleeve.
The convector is replaced by the exchanger on the furnace.
Cold system stand
FIGURE 8: COLD SYSTEM DEVICE
Commissioning
G/DSC131-1A 07/07/06
10

4.2.3.2. First commissioning
1. The cold system must be on the right side of the DSC 131 to have the cold
source naturally positioned and to avoid strength on the transducer. The
system's rear should never be placed against a wall.
The minimum radius of curvature of the sleeve is of 20 cm
2. Installing the base:

Under the base plate, unscrew the last knurled screw on the right side of the
instrument.
Lift the instrument so as to insert the base under the instrument's rear right feet
and retighten the knurled screw to fix the base and the body at the same time.
3. Connecting the safety:
Connect the safety cord from the cooling device on the external safety socket
(see Figure 9). The ghost connector should be removed.
Scurit externe
External safety
FIGURE 9: CONNECTION OF THE SAFETY DEVICE

Note
When the cold system is not in use, it just remains on its base.
Note
Safety can stay constantly connected.
4.2.3.3. Utilization
1. Remove the convector (and cooling accelerator if need be) and replace it by the
exchanger. Access to the sample is possible by the top keeping the exchanger
in place.
2. Start the gas circulation.
The sub ambient mode must be used with a dry gas sweeping.
Commissioning
G/DSC131-1A 07/07/06
11
3. Introduce the crucibles and the sample.

4. Determine a temperature close to the ambient (or lower if the user is not
interested in a decrease in temperature) using the Direct programming
(refer to the Setsoft software booklet).
5. Switch on the switch on the front panel to start the cold system. After a while
temperature within the exchanger will start decreasing down to about -90C.
6. After about 20 minutes the cold system itself will reach its minimum
temperature. This temperature is not checked while the scanning temperature
of the DSC 131 is checked by the furnace heating. The instrument is now ready
for use (refer to Chapter 2 - Utilizations and to the Setsoft software booklet).
Minimum and maximum temperatures depend on the sweeping gas
used:
Argon, dry air, nitrogen: -50C to 400C
Helium: -80C to 200C.
The minimum temperature to be reached directly depends on the
ambient temperature -which will be between 20 and 24C for the
optimum functioning of cold system.
The sample may be changed while the cold system is still on. However, follow the
instructions below:
1. Determine the furnace temperature at 30C via the Direct programming
window.
2. Increase the gas rate (approximately plus one revolution on the rate adjusting
device on the rear panel) to reduce the ambient air inlet when opening the
furnace.
If the gas switching option is available an experiment rate (1.5 l/h) may be
selected on a normally open circuit and a more important rate (about 15 l/h) on the
other circuit.
3. Open the covers and change the sample.
WARNING This must be done rapidly.
4.2.3.4. Stopping the device
1. Stop the cold system using the switch on the front panel.
2. Determine a scanning temperature of 30C.
3. Remove the cold source after about 20 minutes and place it on its base.
4.2.4. Liquid nitrogen cooling device
The cooling device uses liquid nitrogen to cool down the DSC 131 when used
with temperatures lower than ambient.
A container of liquid nitrogen is placed where the convector is located. This
container is of about 1.5 liters.
Commissioning
G/DSC131-1A 07/07/06
12

WARNING The use of subambient mode requires the cooling fan to be switched
off.
When the container is installed fill it up with liquid nitrogen.
The level of liquid nitrogen must always be high enough in order to avoid an
uncontrolled increase in temperature.
Liquid
nitrogen
container
Fan
FIGURE 10: COOLING DEVICE
Liquid nitrogen can burn your skin severely. Therefore, wearing

gloves and glasses is recommended when the container is refilled.
In order to avoid an uncontrolled cooling process, the DSC 131 must be on
regulation at 20C for instance, before being filled with liquid nitrogen.
Note
WARNING Circulation of inert gas (helium) is necessary for the instrument to
work properly at very low temperature. Argon and nitrogen should be avoided at
very low temperature as these two gases partly liquefy.
5. Commissioning of the calorimetric transducer

5.1. Presentation
The furnace-transducer set is hermetically closed either by the convector (1) or by
the container of liquid nitrogen. Tightness is ensured by an o-ring (2).
When the convector or the container is removed, a protecting shutter closes the
hole and only the part of the transducer to be used is displayed.
Commissioning
G/DSC131-1A 07/07/06
13
The transducer is made of:

a machined metallic plate (8) providing for two housings for the measure and
reference crucibles. A thermocouple is welded under each housing to perform
the differential measurement.
a temperature measurement thermocouple in the middle of the plate.
a four-wire shaft receiving the various connecting wires.
The transducer is placed in a silver block (3), centering is ensured by three
adjustable screws (4) supported by the shaft.
A heating element (5) surrounds the block and provides for heating. The
regulation thermocouple (6) provides for temperature control and measurement.
A stopper (7) closes the upper part of the chamber.
The gas is introduced into the lower part of the analysis chamber via a stainless
steel tube (10).
A hole (9) in the cover (7) lets the gas out of the analysis chamber.
9
1
8
5
3
4
6
10
Gas inlet
Gas outlet
FIGURE 11: DSC131 SECTION
5.2. Commissioning
Switch on the supply rack on the rear panel to use the transducer and the
instrument. A green light appears on the front panel.
Switch on the computer and the printer (see corresponding manual).
Start with Collection on the Setsoft. On the Display menu, choose Direct
programming. In this window, furnace and samples temperatures are shown
Commissioning
G/DSC131-1A 07/07/06
14
as well as the Heatflow signal. We can fix a regulation temperature, start the
ventilator and commute a sweeping gas (option).
To accede to experiment chambers:
remove the convector (1)
close the protecting shutter
remove the stopper (7) using laboratory pliers introduced in the two
recessed holes
the "measure" crucible is at the front of the instrument while the "reference"
crucible is at the rear.
The DSC 131 can start carrying out experiments. Refer to the Utilization and
Setsoft booklets.
6. Technical characteristics
6.1. DSC 131
Single-phase electric network
230 V + - 10 % 50/60 HZ
Total power consumed
320 VA
Safety equipment
Programmable safety temperature

through a software
Thermoswitch of safety on the
transducer
Gas inlet pressure
3 bar maximum
Working ambient temperature
From 5C to 40C
Relative humidity
Maxi.
80%
at
ambient
temperatures up to 31C,
decreasing to 50% at 40C.
Dimension W x H x D
DSC
420 x 350 x 530
DSC + cryogenic device
435 x 350 x 530
DSC + Liquid nitrogen tank
420 x 780 x 530
Weight
DSC 23 kgs
Working temperatures range
From 150C up to 700C. Those

values will be entered in relation
to the options, crucibles or
sweeping
gas
used.
Consequently, it is imperative to
refer to the instructions leaflet.
Commissioning
G/DSC131-1A 07/07/06
15
Programming speed
From 0.001 to 50C/minute.

Those values will be entered in
relation to the options or
sweeping gas used. Refer to the
instructions leaflet.
Samples maximum volume
Aluminum crucible
: 30 l
Aluminum crucible
: 100 l
HP crucible: 30 l
Liquid nitrogen tanks filling volume
2 liters
6.2. Cryogenic device

Electric networks power supply
220 V / 50Hz
Total power consumed
1 KVA
Safety equipment
Thermoswitch
Working ambient temperature
22C (optimum)
Working relative humidity
50 % (optimum)
Dimension ( W x H x D )
250 x 480 x 510
Weigh
32 kgs
Range of working temperature
From -70C up to 400C. Those

values will be variable in relation
to the sweeping gas used. Refer
to the booklet.
6.3. Materials in contact with the gas

Tubing
Polyurethane
Connector
Brass
Analysis chamber
Stainless steel, silver, Dural
Sensor
Chromel, Constantan, alumina
Crucible
Aluminum, incoloy
6.4. Conforming to standards

Emission
standard:
EN
EN 61326/A1 (October 1998)
Commissioning
G/DSC131-1A 07/07/06
61326-1
(July
1997)
and
16
Immunity
standard:
EN
EN 61326/A1 (October. 1998)
61326-1
(July
1997)
and
European basic standard: EN 55022 Class B (December 1994)

Harmonized standard: EN 61010-1 (August1993)
(November
Commissioning
G/DSC131-1A 07/07/06
and EN 61010-1/A2
1995)
17
Appendix Table of the Polyurethane chemical compatibility

Substance
Family
Acetone
Ketones
Acetonitrile
Nitriles
Aluminum Salts
Aluminum Compounds
Barium Salts
Barium Compounds
Benzyl Alcohol
Hydroxyl Compounds
Boric Acid
Inorganic Acids
Butanol
Hydroxyl Compounds
Calcium Chlorite
Calcium Compounds
Carbon Disulfide
Sulfur Compounds
Cupric Chloride
Copper Compounds
Cyclohexanone
Ketones
Dichloromethane
Halogen Compounds
Diethylamine
Aliphatic Amines
Diethylformamide
Aliphatic Amines
Ethyl Acetate
Carboxylic Esters
Formaldehyde
Aliphatic Aldehydes
Gasoline
Aromatic Hydrocarbons
Glycol Ether
Ethers
Hexane
Aliphatic Hydrocarbons
Hydrochloric Acid
Inorganic Acids
(37%)
Hydrogen Peroxide
Peroxides
(30%)
Hydroflouric Acid (48%) Inorganic Acids
Jet Fuel (JP-5)
Aliphatic Hydrocarbons
Kerosene
Hydrocarbons
Aliphatic Hydroxylic
Methanol
Compounds
Methyl Ethyl Ketone
Aliphatic Ketones
Aliphatic and Alicyclic
Mineral Oil
Hydrocarbons
Naphtha
Hydrocarbons
Nitrobenzene
Nitro Compounds
Aromatic Hydroxylic
Phenol
Compounds
Propylene Glycol
Hydroxylic Compounds
Sodium Hydroxyde
Inorganic Bases
(50%)
Sulfuric Acid (98%)
Inorganic Acids
Sulfuric Acid (50%)
Inorganic Acids
Tetrachloroethylene
Halogen Compounds (Vinyl
Commissioning
G/DSC131-1A 07/07/06
Compatibility
Not recommended
Weak
Good
Good
Weak
Good
Good
Good
Weak
Good
Not recommended
Not recommended
Weak
Not recommended
Weak
Good
Good
Good
Good
Not recommended
Weak
Not recommended
Good
Good
Good
Not recommended
Good
Good
Not recommended
Not recommended
Good
Good
Not recommended
Not recommended
Good
18
Tetrahydrofuran
Toluene
1,1,1-Trichloroethane
Trichloroethylene
Triethylamine
Turpentine
Water
Halides)
Alicyclic Ethers
Aromatic Hydrocarbons
Aliphatic Halogen Compounds
Halogen Compounds (Vinyl
Halides)
Aliphatic Amines
Hydrocarbons
Misc.
Not recommended
Weak
Weak
Weak
Good
Good
Good
Those indications are provided as information and are not

necessarily reliable for all the conditions for use.
We are not responsible in any way for this table as safety or
guarantee terms towards our instrument.
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DSC 131 - Commissioning/Utilisations
CHAPTER 2 - UTILIZATIONS
1. Selecting the crucible
The crucible selected for the sample analysis very often determines the quality of
the analysis. This is a vital choice that depends on the sample to be analyzed and
the application to be carried out.
Three types of crucibles are available with the DSC 131:
low-volume aluminum crucible (30 mm3)
medium-volume aluminum crucible (100 mm3)
high-pressure crucible (30 mm3)
The crucible depends on the sample to be analyzed. As a general rule:
Use a low-volume aluminum crucible to analyze a small mass of solid sample
so as to have a shorter response time from the DSC transducer.
Use a medium volume aluminum crucible to analyze a larger mass of solid
sample and liquids at a medium temperature.
Use a HP crucible to analyze samples with high vapor pressure and liquids.
Choosing the crucibles volume depends on the mass of sample to be analyzed. As
a general rule, analyze a small mass of sample (about 10 mg) so as to minimize
the effects of a thermal gradient within the product.
However, if a low thermal effect is to be measured, use the largest mass of sample
available.
The various recommendations given above cannot cover all the
instruments applications.
Before analyzing a new product you have to get information
about the risks of corrosion for the crucible during the heating or
one of the possible transformations (fusion, decomposition...).
This is a vital choice as it determines the outcome of the
experiment. Making the wrong choice can lead to damaging the
crucible, and thereby damaging the DSC transducer.
Follow the instructions in force to eliminate the samples which
could be dangerous towards the environment.
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1.1. Low-volume aluminum crucible

WARNING Can be used only up to 550C
1.1.1. Description
The low-volume aluminum crucible is not fluid-tight and is made of (Figure 12):
a 0.2 mm-thick stamped aluminum tray with a flat bottom.
a 0.12 mm-thick stamped aluminum cover to be fitted into the tray.
FIGURE 12: LOW VOLUME ALUMINIUM CRUCIBLE
1.1.2. Crimping
Use a crimping tool composed of a matrix (1) and a punch (2) to close the
crucible (see Figure 13).
FIGURE 13: CRIMPING TOOLS
In practice, once the weight of the sample plus the crucible is known:
1.
2.
3.
4.
5.
Place the crucible in the matrix opening.

Place the cover on the crucible and slightly introduce it.
Fit the punch on the matrix.
Place the whole set on a flat surface and
Press with your hand to drive the punch in the matrix down to the stop.
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6. Remove the crucible.

WARNING The DSC 131 will give the correct measure only if the bottom of the
crucible is perfectly flat so as to provide a good thermal contact with the detector.
Check that the bottom of the crucible is flat after the crimping operation. Change
the crucible if the surface of the bottom is uneven.
1.1.3. Utilization
The low-volume aluminum crucible is recommended for the DSC 131 because the
bottom of the crucible is thin and therefore its low thermal mass ensures a short
response time of the DSC.
This crucible is to be used with small weights of samples (a few mg).
The samples can be:
1. solid such as mineral, organic and metallic samples, as well as powders, films,
grains,....
WARNING Be very careful before starting the analysis:
Make sure that the sample will not corrode the aluminum crucible during heating
at high temperature or after the transformation (fusion for a metal or a mineral
sample for instance).
As the crucible is not fluid-tight, make sure that the sample will not overflow, and
thereby lead to damaging the transducer. If you are not sure about an experiment,
heat the crucible in a small furnace before performing the experiment.
2. liquids at low temperature
As the crucible is not fluid-tight, do not use the low-volume
crucible above 50C when testing liquids because of evaporation.
Indeed, the thermal effect corresponding to evaporation may hide
the effect to be measured.
Make sure that the crucible is not completely filled in order to
prevent the overflowing during the crimping process.
Do not analyze corrosive liquids in this type of crucible.

As for applications, the low-volume aluminum crucible is perfectly adapted to
following measure:
state transformation (fusion, crystallization)
phase transitions, polymorphism
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glass transition
cross-linkage
dehydration
oxidation (when a coverless crucible is used)
The low-volume aluminum crucible cannot be re-used after the
analysis.
1.2. Medium-volume aluminum crucible

WARNING Can be used only up to 550C
1.2.1. Description
The medium-volume aluminum crucible is composed of (Figure 14):

a 0.3 mm-thick and 5.5 mm-high pressed aluminum tray with a flat bottom
an aluminum cover (3 different types are available):
hard aluminum cover (S60/12727)
standard cover (2)
cover with a hole (3)
2
FIGURE 14: MEDIUM VOLUME ALUMINUM CRUCIBLE WITH COVER
1.2.2. Crimping
In case of high vapor-exhibiting reactions, excess pressure may

be produced in the crucible depending on the type of crimping.
The use of a pierced cover is highly recommended so as to avoid
excess pressure and prevent the crucible from exploding.
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Metal crucibles are closed using an appropriate crimping tool (Figure 3).
After weighing the sample in the crucible, proceed as follows:
The template (A) receives the crucible to be crimped and holds it in position
during crimping.
FIGURE 3 : CRUCIBLE CRIMPING TOOL
The punch (B) crimps the lid onto the crucible. After the crimping operation,
make sure that crimping is correct. Check in particular that the lid is not askew.
WARNING The templates act as gauges for checking the diameter of the crucibles,
or more generally of any experimental element or fitting introduced into the

calorimeter. No element or fitting must be introduced into the calorimeter if it
cannot pass through the template.
WARNING Check that the bottom of the crucible is not uneven after the crimping,
as for the low-volume crucible (refer to Warning in paragraph Low-volume

aluminum crucible).
A compact sample in the crucible may be more adapted to some applications or
samples to be analyzed as a better thermal contact is ensured and vapor pressure is
maintained above the sample (e.g. dehydration of gypsum and plaster).
The crucible with a standard cover or a cover with a hole is to be

used for investigations on solids and powders. For liquids, use a
HP crucible.
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Check that the product to be analyzed does not corrode

aluminum.
The crucible cannot be re-used.
Use the HP crucible for investigations under high internal

pressure.
If the sample is a liquid do not entirely fill the crucible so as to
have enough expansion volume for the liquid.
Check the crucible tightness: test the sample before using the
DSC (in a small furnace for instance).
Check that the liquids analyzed do not corrode aluminum.
The crucible cannot be re-used.
1.2.3. Utilization
The aluminum medium volume crucible is used when a quite large mass of
sample is to be analyzed. As the thermal mass is higher the response time from the
DSC 131 is longer when this type of crucible is used.
The standard cover is mostly used when solids, powders, films... are investigated.
The pierced cover is used when products are undergoing dehydration.
The pierced cover is also used when interaction between a reactive gas and the
sample is investigated (e.g. oxidation). For this type of application the sample can
be placed in a coverless crucible.
See the limits in the previous paragraph.
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1.3. High Pressure crucible 500 bars 600C S60/581 86

In many applications, the sample must be placed into a fluid-tight crucible to keep
the vapor inside during the heating, as the thermal effect (vaporization) would
hide the chosen thermal effect (decomposition, polymerization...). The HP
crucible is perfect for this type of application.
1.3.1. Description
In many applications, the sample needs to be isolated in a fluid-tight crucible to

prevent any vapor release during heating, as the thermal effect (vaporization)
would mask the thermal effect under study (decomposition, polymerization, etc.).
In such cases it is possible to use crucibles with non-controlled pressure that meet
the European standard for pressurized containers (CE97/23). They can work at up
to 500 bars and 600C and feature a safety device that allows excess pressure to
be released.
WARNING
The gilded Cell S60/58159 can be used only up to 400C
Their use implies that sometimes the internal pressures in the crucible are very
high and often poorly known. Before using these crucibles, a number of
recommendations must be applied.
A poorly controlled phenomenon can result in serious damage that is
not covered by the manufacturer's warranty (comply with the crucible utilization
limits).
WARNING
WARNING Never undertake an experiment that could produce high pressures

without studying it beforehand by heating one or more crucibles loaded with
samples in the same way in an adjacent furnace, but at a rate and at a temperature
slightly higher than those planned.
WARNING Pay attention to the very rapid rise in the saturation pressure as a
function of the temperature. Leave sufficient volume for the liquids to expand.
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1-cap
2-crucible body
FIGURE 4: FLUID-TIGHT NON-CONTROLLED PRESSURE CRUCIBLES. (THE HEIGHT SHOWN ON THE
DRAWING IS THE SENSYS CELL ONES)
The crucible has a machined body and a tapered cap that screws into the body.
1.3.2. Crimping
The crucible is closed by fitting its screw-in cap and tightening it to the necessary
and sufficient torque. The cap 1-Figure 5 has a top section that enables it to be
screwed into the body of the crucible 2-Figure 5 and which breaks when the
correct tightening torque is applied. This guarantees resistance to a pressure of
500 bar. A 6-mm open-end wrench is used to tighten the cap.
1-cap with breakoff top section
2-crucible body
FIGURE 5 FLUID-TIGHT NON-CONTROLLED PRESSURE CRUCIBLE . (THE HEIGHT SHOWN ON THE

DRAWING IS THE SENSYS CELL ONES)
Tool S60/58163 is used to hold the crucible in position. When the crucible is held
with the tool, tighten the tool with the screw until the crucible is not rotating.
Tighten the cap with the open-end wrench Figure 7. Tighten until the top section
of the cap breaks off Figure 8, indicating that the right tightening torque has been
applied.
Screw
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Positioning of the
tight crucible
SENSYS: S60/58158
or
DSC131: S60/58186
28
Positioning of the
tight crucible
SENSYS: S60/58232
Tool S60/58163
FIGURE 6 TOOL FOR HOLDING THE FLUID-TIGHT CRUCIBLE.
Remarque These crucibles are in accordance with the European standard for containers
under pressure (CE97/23) and they can be used with non-dangerous and
dangerous gases of class 2 and class 1. Be careful gas panel furnished by
SETARAM are only working with non-dangerous gases of class 2
WARNING
The maximum use temperature is of 600C. The pressure must not exceed 500
bars.
A 6-mm open-end wrench is used to tighten the cap as shown on Figure 7. The
wrench is provided with the tool: S60/58305
FIGURE 7 CLOSING OF THE CRUCIBLE

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Figure 8 After breaking
If the sample is a liquid, do not fill the crucible too much. The
level of the liquid must be below the shoulder on which the
stopper lays.
Make sure that the groove is not humid and dry it if necessary.
Humidity can lead to a thermal effect related to water
evaporation.
1.3.3. Utilization
1.3.3.1. Instructions for use
The HP crucible is particularly well adapted to investigate decomposition of

organic products, polymerizations, reactions with a high internal pressure.
The crucible provides for tightness up to very high internal pressures.
However, internal pressure is often not well known and some recommendations
are necessary before starting this type of experiment:
If a crucible explodes in the calorimeter (the stopper is expelled
when pressure is too high), it may cause damages which are not
guaranteed by the manufacturer. It is vital to respect the limits for
the metal seal used.
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Before carrying out an experiment that might lead to high

pressure, heat in a furnace one or several crucibles similarly filled
at a scanning rate and temperature slightly higher than necessary
for the investigation.
As a general rule, a preliminary experiment with a small mass of
sample is recommended especially when decomposition is
investigated (1 to 2 milligrams). Decomposition phenomena are
generally highly exothermic. If the thermal phenomenon is low,
amplify the scanning rate instead of increasing the sample mass.
Enough expansion volume above the sample is necessary, in
order to analyze liquids.
Should the first experiment be dangerous, stay near the
instrument in order to stop the experiment if need be.
When higher than 300C the crucible needs to be atmospheric
corrosion-tight. The transducer must be swept by an inert gas.
The cell can be used only once.
2. Preparing the experiment

Once the crucible is selected (see section Selecting the crucible) and the necessary
precautions are taken, the experiment requires various operations:
1.
2.
3.
4.
5.
6.
Weighing a sample
Arranging crucibles in the DSC
Selecting the sweeping gas
Entering the experiment conditions
Recording signals
Processing data
2.1. Weighing a sample

The sample can be a liquid or a solid (powder, granule, film ...). In both cases, the
sample represents the product to be analyzed and must be carefully used.
Weigh the sample in the crucible, using a balance providing a measurement
accuracy of 0.01 mg.
Note
Use the highest mass of sample is the chosen thermal effect is low.
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If close thermal effects are to be separated, use a small mass of sample so

as to decrease the thermal gradient effect in the sample and to improve the peaks
separation.
Note
If the sample is explosive, weigh only a few milligrams of

sample.
Make sure that the crucibles are not filled up above the space
necessary to the crimping process.
Before closing the crucible, check that the groove is clean.
After the crimping, check that the bottom of the crucible is still
flat and even.
2.2. Placing crucibles in the DSC
1. Remove the convector and close the protecting shutter.
2. Remove the metal stopper protecting the experimental chamber to reach the
actual transducer.
3. Place the crucible with the sample in the right chamber or the sample
chamber of the transducer. Check that the crucible is properly centered and
arranged in the chamber.
4. In the left chamber, place a crucible that is similar to the one in the right
chamber and of the same type.
The crucible could be:
empty, in case of a low mass sample or a high thermal effect
measurement.
filled with an equal mass of alumina (previously calcinated) if the sample
mass is important or the thermal effect to measure is low.
The reference crucible mainly compensates the thermal effect due to the specific
heat of the sample.
In practice, the reference crucible remains empty when the low volume
aluminum crucible is used. When the medium volume crucible is used, it may be
useful to fill it with alumina.
If a liquid is analyzed in a tight crucible it is recommended to use distilled water
as a reference but the instructions for use given in the chapters referring to
crucibles must be taken into account.
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5. Set the metal stopper.

6. Close the instrument with the convector.
2.3. Selecting the sweeping gas
(Connections of the sweeping gas circuit are described in paragraph 4.1. in the
Commissioning chapter).
The DSC 131 offers various possibilities:
Do not use sweeping gas: generally with aluminum crucibles when temperature
is above 0C.
Use an inert sweeping gas (argon, nitrogen, helium): the sweeping gas is used
to prevent the sample from oxidizing (with opened crucible).
WARNING The calibration of the DSC transducer varies with the type of gas used.
See Energy calibration in the present chapter.

Use an active sweeping gas (oxygen, hydrogen): the sweeping gas is used to
investigate the sample/sweeping gas reaction with an opened crucible.
Before investigating a reaction between a sample and a reactive
gas, make sure that the transducer is not likely to corrode or be
damaged due to a violent reaction.
Use an inert gas and then a reactive gas: in some investigations (determination
of induction time for oil for instance), first, the sample must be protected under
inert gas, and then the inert gas is replaced by an oxidizing gas (air, oxygen) in
order to oxidize the sample.
WARNING Use gases having a close density (argon and oxygen for instance).
Indeed, the flow of both gases must be adjusted so as when changing the gas, the
DSC signal is not disturbed. Use the device for automatic commutation of gases
(option) as this operation is performed via the computer.
WARNING It is forbidden to use corrosive and/or reducing gases.
In any case, if the temperature exceeds 500C in isothermal mode

or 60C in programming at speed at a least equal at 5C/min, the
transducer must be protected by a neutral gas.
2.4. Entering experimental conditions
This part of the experiment is also detailed in the software booklet which provides
information related to the test to be carried out from the computer.
In this paragraph, additional instructions on the experiment itself are given:
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Scanning and sequencing

PID actions
Safety temperature
Control of the electrovalve and cooling fan
2.4.1. PID actions
The regulation of the DSC 131s furnace is done via a K thermocouple. PID
coefficients for regulation must be entered in the computer so as to regulate the
furnace.
PID values are expressed in:
C for P (Proportional)
Seconds for I (Integral)
Seconds for D (Derivative).
The values to be used in the software are as follows:
P
50
50
These values apply to the whole temperature range of the DSC 131.
2.4.2. Safety temperature
Entering a safety temperature is vital for protecting the DSC transducer, the
sample and the crucible, depending on the experiments to be carried out.
In general, the following values are to be recommended:
If the work is performed over the whole temperature range set the value for the
safety temperature at the maximum operating temperature plus 20C.
If protection is required for the sample under analysis so as to prevent
decomposition, oxidation, etc or for a crucible as a function of its temperature
capacity, set the value for the safety temperature at the protection temperature
chosen.
Temperature scanning automatically stops at the selected temperature should there
be a problem or previous errors.
2.4.3. Control valve and fan
The valves window is used to control both the fan and the gas automatic
commutation device (option).
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The fan is switched on by activating the second box of the valves window.
In the list of sequences, the Valves column must be following (0100 0000)
Gas 1 is normally on when no specific command is requested. By activating
the first box of the valves window, gas 1 is replaced by gas 2.
In the list of sequences, the Valves column must be following (1000 0000)
Electrovalve
Fan
FIGURE 24: CONTROL ELECTROVALVE AND FAN
2.4.4. Scanning and sequencing
Before starting the experiment, a sample scanning cycle needs to be prepared. To

do this, the software offers a sequence-gathering table which carries out heating
and cooling operations, as well as periods of constant temperature.
In practice, two types of sequence are available: scanning and isothermal
sequences.
1. For a scanning sequence, supply the initial and final temperatures, as well as
the scanning rate during this sequence. The table shows the duration of the
scanning sequence (See figures 25 and 26).
2. For an isothermal sequence, supply the level temperature (C) and the length of
the level (sec.).
An experiment is defined as a collection of scanning and isothermal sequences.
Here are a few examples to understand the functioning:
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2.4.4.1. Simple cycle
The simplest, and often the most common cycle, involves heating a sample
continuously and cooling it.
In that case it is necessary to set:
1. An isothermal level at the start temperature (generally, a few degrees below
ambient temperature) so as to produce stability in the DSC signal before the
start of the heating for 300 seconds.
2. A scanning sequence with the initial and the final temperature in the test, as
well as the selected scanning rate.
3. An isothermal level at the final temperature, to have a stable DSC signals for
300 seconds.
4. A scanning sequence with its initial temperature as the one reached, and the
final temperature as the initial one.
The graph (Figure25) is a means of checking that parameters entered in the
computer are correct.
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FIGURE 25: SIMPLE CYCLE
Refer to the software booklet Setsoft for the cycling operations in such an
experiment. This operation is interesting to plot a base line for a given sample that
does not transform during the second heating.
2.4.4.2. Staged cycle
The staged cycle provides for carrying out heating or cooling in various stages.
For example:
1. An isothermal level at the start temperature for 300 seconds.
2. A scanning sequence with the initial temperature and the intermediate
temperature at an initial scanning rate.
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3. An isothermal level at the intermediate temperature.

4. A scanning sequence from the intermediate temperature to the final
temperature at a second scanning rate.
5. A scanning sequence from the final temperature to the start temperature at a
cooling rate.
FIGURE 26: STAGED CYCLE
Working from these two examples, more complex cycles can be produced
depending on the experiments requirements. 250 sequences are available to
carry out this work.
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The valves window is used if the gas automatic commutation device is used. Gas
1 is normally on when no specific command (0000 0000) is requested. By
activating the electrovalve (1000 0000), gas 1 is replaced by gas 2.
When using the cooling accelerator the maximum temperature is
500C under air, nitrogen, argon ...and 300C at 30C/min under
helium.
WARNING The value for the cooling rate must be provided as positive.
2.5. Making use of the test

After entering the experimental conditions, start scanning the temperature cycle
and record the thermogramme.
2.5.1. Thermogramme
Working from the first recorded thermogramme, replot it as a function of either

time or temperature by optimizing the axes via the Zoom functions.
As a general rule, preference is given to representing as a function of the more
expressive temperature so as to situate the products transformation temperatures.
However, if the cycle contains a succession of scanning sequences and isothermal
levels representing as a function of time provides for an overall display of the
phenomena.
Two types of phenomena are shown on a thermogramme:
1. Endothermic phenomena such as fusion, phase transition, glass transition,
evaporation, etc.
2. Exothermic phenomena such as crystallization, decomposition, oxidation,
polymerization, etc.
Endothermic peaks are commonly directed toward the bottom of the
thermogramme and the exothermic peaks toward the top (see figure hereafter).
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Heat flow
15
EXO
10
5
0
-10
-15
-20
-25
-30
temperature in C
-35
50
100
150
200
250
350
300
FIGURE 27: ENDOTHERMIC AND EXOTHERMIC PEAKS
When making use of the thermogramme, the first operation involves identifying
the various transformations and specifying them as endothermic or exothermic
effects.
2.5.2. Determining transformation temperatures (or times)
In this section, three types of transformation are available:

1. Endothermic transformation such as fusion or phase transition
2. Exothermic transformation such as crystallization or reaction
3. Glass transition
The methods used for determining the transformation temperatures (or times)
comply with the international ISO standards in force or in draft.
2.5.2.1. Endothermic transformation
The endothermic transformation thermogramme is shown below:

heat flow
T im
Teim
Tefm
T fm
Tpm
temperature
FIGURE 28: ENDOTHERMIC TRANSFORMATION THERMOGRAMME
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The following temperatures (or times) are determined:

Temperature Tim (or time tim) at the peak start corresponding with the peaks
take-off in relation to the base line plotted between the start and the end of the
peak.
Temperature Teim (or time teim) corresponding to the onset temperature, i.e.
the intersection between the base line and the tangent at the peak inflexion
point in the increasing phase.
Temperature Tpm (or time tpm) corresponding to the top of the peak.
Temperature Tefm (or time tefm) corresponding to the endset temperature,
i.e. the intersection between the base line and the tangent at the peak inflexion
point in the decreasing phase.
Temperature Tfm (or time tfm) at the peak end corresponding with the peak
returning to the base line.
heat flow
2,5
Teim
0,0
-2,5
temperature
EXO
-5
-7,5
-10
time (s)
1560
1620
1680
1740
1800
FIGURE 29: THERMOGRAMME OF THE FUSION OF A PURE SUBSTANCE
In the particular case of a pure crystalline substance, the fusion temperature is

measured at the onset Teim (Figure 29).
Refer to the Practical Works chapter for additional explanations.
For semi-crystalline substances, like numerous polymers, the fusion (or softening)
temperature is measured at the Tpm temperature on the top of the peak.
2.5.2.2. Exothermic transformation
The exothermic transformation thermogramme is shown hereafter:
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Tpc
heat flow
exo
Tic
Teic
Tefc
Tfc
temperature
FIGURE 30: THERMOGRAMME OF AN EXOTHERMIC TRANSFORMATION
The following temperatures (or times) are determined:

Temperature Tic (or time tic) at peak start corresponding with the peaks takeoff in relation to the base line plotted between the start and the end of the peak.
Temperature Teic (or time teic), corresponding with the onset temperature,
i.e. the intersection between the base line and the tangent at the peaks
inflexion point in the increasing phase.
Temperature Tpc (or time tpc) corresponding with the top of the peak.
Temperature Tefc (or time tefc) corresponding with the endset temperature,
i.e. the intersection between the base line and the tangent at the peaks
inflexion point in the decreasing phase.
Temperature Tfc (or time tfc) at the peak end corresponding with the peak
returning to the base line.
In the same way as for fusion the crystallization temperature in a pure, crystalline
substance is measured at the onset temperature Teic.
For a semi crystalline substance, crystallization is measured at the temperature
Tpc on the top of the peak.
2.5.2.3. Glass transition
Given what we know at the moment, glass transition corresponds with the
progressive change in the properties of a solid to those of a viscoelastic liquid.
As glass transition is a progressive process it is distinguished by three distinct
temperatures (Figure 31):
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Tig
Tg
T eg
FIGURE 31: GLASS TRANSITION WITHOUT RELAXATION TIME
The temperature at the start of transition Tig given by the intersection between
the base line (before the transition) and the tangent at the inflexion point (line
of the largest slope).
The temperature at the end of transition Teg given by the intersection between
the base line (after the transition) and the tangent at the inflexion point.
The conventional temperature for glass transition Tg produced by the
intersection of the curve and the half-way line between the two base lines.
If the sample shows any aspect of relaxation before or after the glass transition,
proceed as described in Figure32:
Tig
Tg
Teg
FIGURE 32: GLASS TRANSITION WITH RELAXATION TIME
2.5.3. Temperature correction
Measuring the samples temperature is performed through a platinum probe in the

calorimetric unit.
Although this measurement is done near the sample, a small difference may be
noted with the samples real temperature due to the thermal gradient and the time
for the heat to cross the crucible wall and detector.
Temperature correction will vary according to:
The scanning rate used
The type of crucible involved
The type and rate of sweeping gas
Standard materials with known fusion or transformation points are required to
carry out this temperature correction.
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2.5.3.1. Standard materials
Metals are preferable for determining temperature calibration of the DSC 131 as
shown in the table below:
Substance
Melting point (C)
Mercury
-38.86
Indium
156.598
Tin
231.94
Lead
327.47
Reference : ENR7-6ET01 (Annex A)

For these metals, choose a purity of 4N (99,99 %) or even better 5N (99,999%).
However, depending on the range of temperature planned for analysis, inorganic
and organic substances may be used for fusion and transition:
Substance
Temperature (C)
Cyclohexane
-86.91
Potassium Nitrate
128
Silver sulfate
424
Quartz
571
Reference : ENR7-6ET01 (Annex A)

When using these substances special attention must be paid to
substances exhibiting high vapor pressures.
In addition, certain substances can break down if heated beyond
their transition or fusion temperature. It is thus VITAL to remain
within the temperature measurement corresponding with the
transformation given in the table.
Some substances can react to the crucible material. A table of
compatibility between substances and crucible materials is
available in Annex C.
2.5.3.2. Experimenting
Choose at least three standard materials comprising the temperature zone to be

used for analyzing the samples.
Set the experimental conditions to be used for analyzing the sample, especially:
Type of crucible
Type and flow rate of the sweeping gas
Temperature scanning rate
Utilizations
G/DSC131-1A 07/07/06
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For each standard material:

Weigh about 50 mg of substance in the crucible.
Arrange the crucible on the sample side of the DSC transducer. Arrange an
identical, empty crucible on the reference side.
Close the furnace and switch on the sweeping gas.
Prepare the scanning cycle so as to get the substance molten.
In practice, scan the furnace temperature rapidly (30C/mn) up to around 30C
before fusion. After an isothermal stabilization level record the fusion at the
chosen rate.
Finally, scan the furnaces cooling.
FIGURE 33: EXAMPLE OF THE CYCLE SCANNING
Utilizations
G/DSC131-1A 07/07/06
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Record the corresponding thermogramme and replot the part corresponding to

the standards fusion as a function of temperature.
Repeat the operation for each material, adjusting each time the temperature
range for measuring the fusion or transition.
Expand the temperature range for analyzing fusion when the scanning rate
increases.
Note
Note A second fusion of the sample is recommended after cooling and the
second thermogramme provides useful information. The first fusion does provide
a compact shape to the sample, which is more helpful for the heat exchange with
the transducer.
2.5.3.3. Temperature correction for a fixed scanning rate
For each fusion peak determine the onset temperature Teim as defined in
paragraph 2.5.2.1.
If:
Teim, the onset temperature measured
Tfi the real fusion temperature for sample i
dTi = Teim - Tfi the temperature correction
Draw up a table (Teim, Tfi, dTi) and plot the variation dTi = f (Teim) (see Figure
below).
Ti
V = 5C mn -1
10
8
pente = a
Ti = Ti + a T i
Tei
162,8
239,5
336,9
430,5
FIGURE 34: TEMPERATURE CORRECTION FOR A FIXED SCANNING RATE
Express this variation in the form of a straight line:

dTi = B0 + B1. Teim
Utilizations
G/DSC131-1A 07/07/06
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Determine B0 and B1 using a regression program.

Enter the values of B0 and B1 on to the softwares Parameter window for
temperature correction.
Reset the values B2 and B3.
This relationship provides for correcting any temperature for the analysis
interval considered and by always using the same scanning rate.
Note
2.5.3.4. Temperature correction for various scanning rates
If analyzing the sample has to be done at various temperature-scanning rates the

fusion of the standard materials needs to be studied at various scanning rates Vi.
In practice, carry out experiments for each standard using at least three different
rates, the values of which encompass the values of the rates to be used for the
sample.
Draw up a table (Teim, Tfi, Vi, dTi).
Determine the coefficients Bo, B1 and B2 for the correction relationship using the
least squares method or a regression program: dTi = B0 + B1. Teim + B2. Vi
In practice, if N is the number of tests carried out, calculate the following sums:
Teim
Vi
dTi
Teim2
Teim. Vi
Teim. dTi
Vi2
Vi. dTi
Here the coefficients are produced by the relationships:

B0 =
J
W
B1 = K
B2 = L
where:
W = N (DG - E2) - A2G + 2ABE - DB2
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G/DSC131-1A 07/07/06
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J = C (DG - E2) - F (AG- EB) + H (AE - DB)

K = N (FG - HE) - A (CG - BH) + B (CE - FB)
L = N (DH - EF) - A (AH - EC) + B (AH - DC)
The temperature correction thus determined applies for any scanning temperature
and rate for the range investigated.
Enter the values B0, B1 and B2 in the softwares Parameter window for
The coefficient B3 is reset for the instrument used.
WARNING During experiments for determining temperature correction, check that
the values B0, B1, B2 and B3 are reset in the software.

2.6. Energy calibration
It is necessary to carry out an energy calibration of the DSC 131.
The DSC transducer can be calibrated by using standards so as to transform the
electrical signal S (in microvolt) into thermal power P (in milliwatt). Then, a
calibration coefficient K is determined:
S = K. P
The calibration coefficient K varies with various parameters:
The temperature of the experiment
The type of crucible
The type and flow of sweeping gas
Paragraph 2.6.1 (hereafter) shows the means of calculating the calibration
coefficient K.
2.6.1. Measuring the fusion heat of a pure substance
The thermogramme representing the fusion of a pure substance is shown in Figure

below (refer also to the Practical Work chapter):
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G/DSC131-1A 07/07/06
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heat flow (mW)
2,5
0,0
-2,5
EXO
-5,0
-7,5
-10
temperature C
TPR
157
158
159
160
161
FIGURE 35: FUSION OF A PURE SUBSTANCE
The heat of fusion for the sample analyzed is produced by integrating the area
under the peak between the peaks start Tim and end Tfm temperatures.
Without initial calibration the ordinate is expressed in V and the abscissa in
seconds, the peak area is expressed in V. s.
Integrating the peak is done via the Integration function on the base software
once the type of base line is selected. For a fusion peak, use a straight base line
between the temperatures Tim et Tfm.
2.6.2. Standard materials
Paragraph 2.5.3.1. provides a table of standard metals for determining the

For energy calibration the same standards may be used as they are thermally
stable and offer the facility of being used for numerous and successive tests
without modifying their specifications.
Their fusion heat contents are used for energy calibration.
Substance
Fusion heat content

(J / g)
Fusion heat content

(C)
Mercury
11,469
-38.86
Indium
28,51
156.598
Tin
60,21
231.94
Lead
23,00
327.47
ENR7-6ET03 (Annex B)
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G/DSC131-1A 07/07/06
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Based on the sample transformation temperature the standard chosen for energy
calibration will be the one with a melting point closest to the transformation
temperature of the sample.
As for determining temperature correction, an inorganic substance may be used
for energy calibration.
Substance
Fusion heat content (J / g)
Melting point (C)
KNO3
53,2
128
ENR7-6ET03 (Annex B)
Note
Certified Reference Materials (CRM)
Note For measurements requiring a higher accuracy, some Certified Reference

Materials for temperature calibration (or temperature and fusion heat calibration)
are available in national laboratories such as the National Institute of Standards
and Technology (NIST-USA) and the Laboratory of the Government Chemist
(LGC-GB). These Certified Reference Materials enable the traceability of the
measurements (Cf. Annex A and B)
2.6.3. Experimenting
Choose one or several standards based on the transformation temperature range

investigated.
The experimenting conditions are similar to those described in paragraph 2.5.3.2.
Plot the fusion curve as a function of time or temperature.
In practice temperature and energy calibrations are carried out with the
same experiment, on the same fusion peak (Reset all coefficients (sensitivity,
temperature) to carry out calibrations) of the metal standard.
Note
2.6.4. Calibration with a single standard
If the transformation takes place within a limited temperature range, a single

coefficient of calibration can be used by choosing the standard with the closest
melting point.
Let H be the fusion heat content for the metal standard chosen (in J / g),
Let m be the mass of the standard analyzed (in g),
Let S be the area of the fusion peak (in V. s),
Then, the calibration coefficient at the standards melting point is given by:
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G/DSC131-1A 07/07/06
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K=
S 1
x ( V / W ) in microvolt per watt
H m
K is better expressed in V/mW.

For any peak area A (in V. s) combined with the corresponding transformation Q
(in Joule), the formula is:
Q=
A
K
2.6.5. Calibration with various standards
As mentioned in the previous paragraph, calibration with a single standard is

recommended for a limited temperature range. However, if the test is carried out
over several hundred degrees, various metal standards are recommended so as to
plot a variation curve of the coefficient of calibration as a function of temperature.
The substances shown in paragraph 2.6.2 can be used.
Choose at least five standards in order to produce correct determining.
Let Hi be the fusion heat content of the standard i (in J / g),
Let mi be the mass of the standard i investigated (in grams),
Let Si be the area of the fusion peak (in V. s),
The coefficient of calibration Ki at the standards melting point Teim is given by:
Ki =
Si 1
x
(in V / W)
Hi mi
Express Ki in V / mW.
Draw up a table (Teim, Ki) and plot the variation K = f (Teim)
This calibration curve reveals the instruments coefficient of calibration at any
temperature (see example hereafter).
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G/DSC131-1A 07/07/06
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K (microV/mW)
2
A0 = 3.0908E+00
A1 = 7.0250E -03
A2 =-4.5361E -05
A3 = 8.8112E -08
A4 =-6.0381E -11
tempratures (C)
0
-50
50
100
150
200
250
300
350
400
450
FIGURE 36: DSC 131 CALIBRATION CURVE
The coefficients A0, A1, A2, A3, A4 thus determined are entered on to the
softwares Parameter page for automatically transforming the DSC signal into
thermal power.
The peak integration directly supplies the transformation heat in Joules.
Utilizations
G/DSC131-1A 07/07/06
52
DSC 131 Annex A
APPENDIX A
STANDARD REFERENCE MATERIALS FOR TEMPERATURE
CALIBRATION
ENR7-6ET01
REV.B
Page 1 / 1
Reference Material
Transition
T (K)
T (C)
Uncertainty (mK)
Ref *
Cyclopentane
s/s
122.38
-150.77
50
Cyclopentane
s/s
138.06
-135.09
50
Cyclopentane
s/l
179.72
-93.43
50
Cyclohexane
s/s
186.24
-86.91
20
Mercury
s/l
234.29
-38.86
30
n-Decane
s/l
243.51
-29.64
Water
s/l
273.15
0.00
Gallium
s/l
302.9146
29.7646
Gallium
s/l
302.930
29.780
10
PTB
Naphtalene
s/l
353.38
80.23
20
LGC 2603
Potassium nitrate
s/s
401
128
5000
Indium
s/l
429.7485
156.5985
46
NIST SRM 2232
Tin
s/l
505.09
231.94
10
NIST SRM 2220
Tin
s/l
505.078
231.928
Bismuth
s/l
544.550
271.400
10
PTB
Lead
s/l
600.62
327.47
20
LGC 2608
Lead
s/l
600.61
327.46
10
Zinc
s/l
692.677
419.527
Zinc
s/l
692.71
419.56
20
Silver sulfate
s/s
697
424
5000
Silver sulfate
s/s
697
424
Quartz
s/s
844
571
Quartz
s/s
844
571
Lithium Sulphate
s/s
851.43
578.28
250
Aluminium
s/l
933.48
660.33
50
LGC 2612
Silver
s/l
1234.930
961.780
NIST SRM 1746
Gold
s/l
1337.33
1064.18
Nickel
s/l
1728
1455
Palladium
s/l
1827
1554
Alumina
s/l
2325
2052
10
CRM
a
NIST SRM 2225
b
c
e
f
NIST SRM 2221A
g
NIST SRM 8759
g
h
7
5000
NIST SRM 8759
6
3
d
d
5000
Remarks **
NIST SRM 742
*References
1.
H.K. Cammenga, W. Eysel, E. Gmelin, W. Hemminger, G.W.H. Hhne and S.M. Sarge
The temperature calibration of scanning calorimeters. Part. 2. Calibration substances
Thermochemica Acta, 219 (1993) 333-342
2.
R. Sabbah, An Xu-wu, J.S. Chickos, M.L. Planas Leitao, M.V. Roux, L.A. Torres
Reference materials for calorimetry and differential thermal analysis
Thermochimica Acta 331 (1999) 93-204
3.
Values from National Institute of Standards and Technology (NIST).[USA]
4.
Finke H.L. ; Gross M.E. ; Waddington G. ; Huffman H.M.
Low temperature thermal data for the nine normal paraffin hydrocarbons from octane to hexadecane
Journal of the American Chemical Society, 1954, 76, 333-341
5.
Values from the Laboratory of the Governement Chemist (LGC).[UK]
Handbook of Thermal Analysis and Calorimetry, Patrick K. Gallagher, Volume 1 Principles and Practise, 1998
Chap 13 Calibration and Standardisation in DSC-M.J. Richardson and E.L. Charsley
6.
Norme ASTM E967-97 Standard Practice for Temperature Calibration of DSC and DTA
(F.D. Rossini, pure applied chemistry, Vol 22, 1970, p 557)
7.
Values from the Physikalisch-Technische Bundesanstalt (PTB).[Germany]
**Remarks
a.
Only in hermetically sealed crucible.
b.
Air-satured, bidistilled water in hermetically closed crucible.
c.
Melt reacts with Al (strong supercooling with Gallium).
d.
Melt reacts with Al, Pt.
e.
Melt reacts with Pt, oxidizes quickly (use protective gas).
f.
Melt (and vapour) react with Al, Pt ; high vapour pressure at melting point (approx 20 Pa).
g.
Use metallic crucible only.
h.
Anhydrate is hygroscopic, thus weigh-in as Li2SO4.H2O, Dehydratation takes place from 100 C, thus turbulent movement
of particles in the crucible and high water-vapour pressure (do not use hermetically sealed crucible), Must not melt (change of
properties).
i.
Melt reacts strongly with Pt.
j.
Melt dissolves oxygen, reacts with Pt.
k.
Use Al2O3 crucible only
Appendix A
G/DSC131-1A 07/07/06
52
DSC 131 Annex B
APPENDIX B
STANDARD REFERENCE MATERIALS FOR
HEAT
CALIBRATION
ENR7-6ET03
Reference Material
Cyclopentane
Cyclopentane
Cyclopentane
Cyclohexane
Mercury
Water
Gallium
Gallium
Naphtalene
Potassium nitrate
Indium
Tin
Bismuth
Lead
Zinc
Lithium Sulphate
Aluminium
Silver
Gold
Nickel
Palladium
Alumina
Transition
s/s
s/s
s/l
s/s
s/l
s/l
s/l
s/l
s/l
s/s
s/l
s/l
s/l
s/l
s/l
s/s
s/l
s/l
s/l
s/l
s/l
s/l
T (C)
-150.77
-135.09
-93.43
-86.91
-38.86
0.00
29.7646
29.780
80.23
128
156.5985
231.94
271.400
327.47
419.56
578.28
660.33
961.780
1064.18
1455
1554
2052
Heat (J/g)
69.60
4.91
8.63
79.8
11.469
333.78
79.88
80.14
147.6
50.5
28.51
60.21
53.14
23.00
107.4
228.1
401.3
104.8
64.5
300
162
1092
REV.
A
Uncertainty
(J/g)
Ref *
0.35
1
0.03
1
0.05
1
0.9
2
0.008
3
4
0.72
1
0.33
5
0.7
6
7
0.19
3
0.19
3
0.22
5
0.06
6
1.3
3
10.5
1
1.6
6
8
1
7
7
9
Page 1 / 1
CRM
Remarks **
a
a
a
a
NIST SRM 2225
PTB
LGC 2603
NIST SRM 2232
NIST SRM 2220
PTB
LGC 2608
NIST SRM 2221A
LGC 2612
b
c
c
a
d
c
e
f
g
h
i
i
j
j
* References
1.
S.M. Sarge, E. Gmelin, G.H. Hhne, H.K. Cammenga, W. Hemminger, W. Eysel.
The caloric calibration of scanning calorimeters.
Thermochemica Acta 247 (1994) 129-168.
2.
R. Sabbah, An Xu-wu, J.S. Chickos, M.L. Planas Leitao, M.V. Roux, L.A. Torres
Reference materials for calorimetry and differential thermal analysis
Thermochimica Acta 331 (1999) 93-204
3.
Values from National Institute of Standards and Technology (NIST).[USA]
4.
DSC Calibration below 0C, G. Hakvoort, Journal of Thermal Analysis, vol 41 (1994)1551-1555.
5.
Values from the Physikalisch-Technische Bundesanstalt (PTB);[Germany}]
6.
Values from the Laboratory of the Governement Chemist (LGC).[UK]
7.
Handbook of Thermal Analysis and Calorimetry, Patrick K. Gallagher, Volume 1 Principles and Practise, 1998
Chap 13 Calibration and Standardisation in DSC-M.J. Richardson and E.L. Charsley
8.
J. Emsley, The elements, 3rd edition, Oxford Press, Oxford 1998.
9.
Handbook of Chemistry and Physics, 83rd edition, D.R. Lide, CRC Press 2002-03.
**Remarks
a.
Only in hermetically sealed crucible.
b.
Air-satured, bidistilled water in hermetically closed crucible.
c.
Melt reacts with Al (strong supercooling with Gallium).
d.
Melt reacts with Al, Pt.
e.
Melt reacts with Pt, oxidizes quickly (use protective gas).
f.
Melt (and vapor) react with Al, Pt ; high vapor pressure at melting point (approx 20 Pa).
g.
Anhydrate is hygroscopic, thus weigh-in as Li2SO4.H2O, Dehydratation takes place from 100 C, thus turbulent movement of particles
in the crucible and high water-vapor pressure (do not use hermetically sealed crucible), Must not melt (change of properties).
h.
Melt reacts strongly with Pt.
i.
Melt dissolves oxygen, reacts with Pt.
j.
Use Al2O3 crucible only
Appendix B
G/DSC131-1A 07/07/06
53
DSC 131 Annex C
APPENDIX C
Compatibility of reference substances / crucibles materials
According to H.K. Commenga et al, The temperature Calibration of scanning calorimeters.
Part2: Calibration substances, Thermochimica acta, 219 (1993), 333-342
0
0
0
+
+
+
+
+
+
+
+
+
+
+
+
0
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
?
+
?
+
+
+
+
+
+
?
?
+
+
+
+
+
+
+
+
+
?
?
+
+
+
?
+
+
?
+
+
+
+
+
+
+
+
?
+
?
?
?
+
?
+
?
+
+
+
+
?
+
+
+
+
?
+
+
Gold
Silver
Aluminium
Zinc
Lead
Tin
Indium
Gallium
water
0
0
0
+
+
+
+
+
+
+
+
+
+
0
Lithium sulphate
Crucible material
Corundum, Al2O3
Boron Nitride, BN
Graphite, C
Silicate glass
Quartz glass, SiO2
Aluminium
Aluminium oxidized
silver, Ag
Gold, Au
Nickel, Ni
Iron, Fe
Stainless steel
Platinum, Pt
Molybdenum, Mo
Tantalum, Ta
Tungsten, W
cyclopentane
Calibration substance
+
?
0 hermetic sealing of crucible not easily possible.

+ no solubility and no influence on the melting temperature to be expected.
- melt dissolves crucible material, greater change in the melting temperature.
partial solution processes are possible with negligible change in the melting temperature.
crucible melts.
? compatibility unknown.
Appendix C
G/DSC131-1A 07/07/06
54
DSC 131 Annex D
ANNEX D
Appendix D
G/DSC131-1A 07/07/06
54
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: low cost series of multi-module thermal analyzers
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DSC, TG/DSC : ambient to 1600C
TMA : ambient to 1000C
SETSYS : top of range in thermal analyzers
DTA, TG/DTA : -150 to 2400C
DSC, TG/DSC : -150 to 1600C
TMA, DLTMA : -150 to 2400C
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micro DSCIII : -20 to 120C ("batch and flow")
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G/DSC131-1A

DSC 131 - Commissioning/Utilizations

CHAPTER 2 - UTILIZATIONS .....................................................................................20

SELECTING THE CRUCIBLE ........................................................................................................ 20

DSC 131 - Commissioning/Utilizations

DSC 131 - Commissioning/Utilizations

07/07/06 Add electrical scheme G/DSC131-1A

23/02/05 Max N2Temperature

28/07/04 Modification of tight

P35 corrosive and

DSC 131 - Commissioning/Utilizations

DSC 131 - Commissioning/Utilizations

Indicates an electric danger.

Indicates a low temperature area.

Indicates a risk of catching or crushing ones hand.

DSC 131 - Commissioning/Utilizations

a single structure including the transducer, its cooling system and

FIGURE 1: DSC 131

DSC 131 - Commissioning/Utilizations

FIGURE 2: DIMENSIONS OF THE DSC 131

2.3. Electrical circuit

DSC 131 - Commissioning/Utilizations

Do plug the instrument ONLY in a ground connection.

3. Electrical and computer connections

FIGURE 3: ELECTRICAL CONNECTIONS

3.2. Computer connections

Therefore, it is necessary to refer to the computers operating

DSC 131 - Commissioning/Utilizations

FIGURE 4: COMPUTER CONNECTIONS

series-cable between (1) (serial port controller) and (2) (computer)

DSC 131 - Commissioning/Utilizations

FIGURE 5: GAS CONNECTIONS

and the bottle from emptying rapidly.

Close the experimenting chamber with a stopper on the gas outlet.

DSC 131 - Commissioning/Utilizations

furnace base is higher than 100C.

DSC 131 - Commissioning/Utilizations

However, a lower increase in temperature and maximum speed will be observed

FIGURE 7: COOLING ACCELERATOR

DSC 131 - Commissioning/Utilizations

Under air, nitrogen, argon... the maximum temperature is 500C.

Under helium the maximum temperature is 300C and the

4.2.3. Cooling with a cryogenic plunging device

The device is composed of two inseparable subsets linked by an insulated sleeve.

Cold system stand

FIGURE 8: COLD SYSTEM DEVICE

DSC 131 - Commissioning/Utilizations

2. Installing the base:

FIGURE 9: CONNECTION OF THE SAFETY DEVICE

Safety can stay constantly connected.

DSC 131 - Commissioning/Utilizations

3. Introduce the crucibles and the sample.

DSC 131 - Commissioning/Utilizations

FIGURE 10: COOLING DEVICE

Liquid nitrogen can burn your skin severely. Therefore, wearing

WARNING Circulation of inert gas (helium) is necessary for the instrument to

5. Commissioning of the calorimetric transducer

DSC 131 - Commissioning/Utilizations