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Operating Instructions
Cooling Options
Installation
Measurement
SmartSens Terminal
Maintenance
10
11
Technical Specifications
12
Accessories
13
Index
HP DSC 1
Contents
1.1
1.2
1.3
1.4
1.5
1.5.1
1.5.2
1.6
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1-i
HP DSC 1
1.1
Thank you for choosing the HP DSC 1 from METTLER TOLEDO. The HP DSC 1 module
is part of the METTLER TOLEDO STARe thermal analysis system.
The HP DSC 1 is a highly sensitive measuring instrument for differential scanning
calorimetry (DSC) under pressure. Due to its modular construction, it can be used in
a wide range of applications, from quality assurance and production as well as research and development.
The HP DSC 1 can be fitted with different DSC sensors: the FRS5 sensor or the HSS7
sensor. The choice of the sensor depends on the demands of a user's application.
Measuring principle
Differential scanning calorimetry is based on the well-proven Boersma or heat flux
principle in which the heat flow of a sample and a reference measurement are compared. The highly sensitive ceramic sensor is used to measure the difference between
the heat flows.
The experimental parameters are entered in the PC. The PC then sends the temperature program for the individual segments to the measuring module.
The measurement data is continuously transferred from the HP DSC 1 module to the
PC during a measurement. The data is presented as an online curve in the Module
Control Window.
Address of manufacturer:
METTLER TOLEDO AG, Analytical
Sonnenbergstrasse 74
CH-8603 Schwerzenbach
Switzerland
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1-3
HP DSC 1
1.2
Modularity
Options
The HP DSC 1 has a modular design. Each HP DSC 1 can be individually configured
and adapted to your own particular requirements and applications.
If your requirements change, you can expand the module later on with additional options.
The following options are available:
Power switch
HP DSC Microscopy
HP DSC Chemiluminescence
1.3
The HP DSC 1 only can be operated in conjunction with the STARe Software from
METTLER TOLEDO which is installed on a PC. There is no stand-alone mode of the
HP DSC 1.
You need the STARe Software, version 9.30 or later, to operate the HP DSC 1. References are made to the STARe Software in certain parts of these operating instructions.
1-4
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HP DSC 1
1.4
Typographical conventions
Safety notes are marked with safety triangles: The following warning triangles
draw your attention to points concerning safety and danger. Ignoring this information could endanger the user and result in damage to the instrument and other
malfunctions.
Risk of
electric shock
Risk of
explosion
Risk of
fire
Risk of burns
Risk of injury
Times New Roman is used to mark text that appears on the screen of the PC (for
example, menu items, error messages, etc.).
Caution
Notice
Times New Roman
For example, the string File/Open Curve means: click the menu point File and
select the submenu Open Curve.
Italic is used for cross-references referring to titles and paragraphs within this
document and in other documents.
Italic
Text that appears in the bold Arial Narrow font shows text that appears on the
touch-screen of the SmartSens Terminal.
CAPITALS
Bold numbers (1, 2, 3 and so on) indicate single steps of instructions for the
user. Explanatory text is not numbered. The instructions are often followed by text
of smaller size informing you about the result of the action.
The symbol
context.
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1-5
HP DSC 1
1.5
Safety Notes
The instruments have been tested for the experiments and intended purposes documented in the relevant operating instructions. However, this does not absolve you
from the responsibility of performing your own tests of the products supplied by us
regarding their suitability for the methods and purposes you intend to use them for.
You should therefore observe the following safety measures.
Intended use
The HP DSC 1 is intended for performing high pressure differential scanning calorimetry.
All other use and operation beyond the limits of operation defined by MettlerToledo AG without written consent from Mettler-Toledo AG is considered inappropriate.
The limits of operation can be found in Chapter 11, Technical Specifications.
1.5.1
HP DSC 1 system
Ensure that you plug the power cable supplied into a receptacle outlet that is
grounded! In the absence of grounding, a technical fault could be lethal.
Be aware that the outer parts of the furnace may become very hot! This could
possibly cause flammable gas mixtures to ignite.
HP DSC 1
1-6
Switch off the HP DSC 1 and remove the power cable before you open the housing or replace blown fuses. An electric shock could be lethal.
Do not use gases that could form an explosive gas mixture! Reactive gas mixtures could explode.
Never switch the recirculating cooling off when the temperature of the measuring
cell is above 100 C. The surroundings of the measuring cell could heat up in an
uncontrolled manner.
For sample removal, the temperature should be below 40 C.
0911
HP DSC 1
Never touch the furnace, furnace lid or a sample you have just removed from the
furnace! The furnace can reach a temperature of up to 700 C. Use tweezers to
remove the lid or sample.
Allow the measuring cell of the module to cool down to room temperature before
opening its housing.
If you use toxic and flammable gases, place the pressure measuring cell in a
fume hood! Burners or open flames must never be in the vicinity! Before applying
a flammable gas, fill the pressure system twice with nitrogen to get rid of the oxygen!
Use only gas sources with a pressure regulator and a check valve!
Never set the pressure at the regulator higher than 10 MPa (maximum operating
pressure)! The gas source may become contaminated in the absence of a check
valve.
Always set the pressure buildup via GAS IN with the INLET valve!
Make sure that the AUX needle (for fine regulation) is not closed tightly otherwise
the needle could be damaged.
The cooling device should also be on when the instrument is switched on.
The cooling fluid should not be colder than 15 C, otherwise condensation could
develop.
Never try to carry the HP DSC 1 module alone. The instrument weighs approximately 40 kg. At least two people are needed to carry the instrument. To lift the
module, hold it firmly with both hands on the underside of the instrument.
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1-7
HP DSC 1
Use the pressure measuring cell only for experiments for which it has been
manufactured in regard to maximum working pressure, corrosion resistance and
maximum temperature (see chapter 11, Technical Specifications).
When releasing flammable gases: Make sure that the gas is vented according to
the laboratory safety regulations. Connect gas outlet and safety rupture disc to
lines that lead off the gas for proper disposal! Especially take measures to avoid
that the gas does not flow into the instruments housing.
explosive limits
The HP DSC 1 measuring cell is not designed for the use of flammable and explosive gases and the system is not explosion-proof.
However, if an application requires the use of such gases, the system operator
has to be aware of the risks. METTLER TOLEDO excludes any liability for such
applications, despite of the fact that the measurement cell is considered to be
gas-tight. If hydrogen has to be used to create a reducing atmosphere or to
minimize the oxygen concentration, a non-explosive mixture of 4% H2 in an inert gas is the preferred solution. The explosion limits of hydrogen in air cover a
very broad range from 4% to 77%. (The explosion limits of hydrogen and other
gases are indicated in the table below.)
Flammability limits, also called flammable limits, or explosive limits give the proportion of
combustible gases in a mixture, between which limits this mixture is flammable. Gas mixtures consisting of combustible, oxidizing, and inert gases are only flammable under certain conditions. The lower flammable limit (LFL) (lower explosive limit) describes the leanest mixture that is still flammable, i.e. the mixture with the smallest fraction of combustible
gas, while the upper flammable limit (UFL) (upper explosive limit) gives the richest flammable mixture. Increasing the fraction of inert gases in a mixture raises the LFL and decreases UFL.
These limits depend on temperature and pressure and are given here for initial conditions
of 0.1 MPa and 20 C. (Source: MERCK catalog 1990/91)
1-8
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HP DSC 1
Gas
Corrosive
Flammable
Toxic
Ammonia
15 - 28
Argon
Carbon dioxide
Ethylene
2.7 - 34
Helium
Hydrogen
4.0 - 75.6
Nitrogen
Oxygen
Note: The explosion limits values may vary slightly depending on your source of information.
Safety notes related to hydrogen in a high pressure DSC
Loading and unloading the samples requires opening the furnace so that the surrounding ambient gas (usually air) mixes with the furnace atmosphere. Hence,
an explosive mixture can be created which will be ignited by hot surfaces or
sparks.
Hence, there are two measures to avoid explosive mixtures:
- Put the measuring cell in a glove box to reduce the risk of having oxygen in the
measuring cell or
- Fill the furnace with nitrogen (or other inert gas) before opening the cell (pressurize to 1 MPa with nitrogen and release the gas at least three times or purge
long enough with the inert gas).
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1-9
HP DSC 1
Release of flammable gases: make sure that the gas is vented according to the
laboratory safety regulations. Especially take measures that the gas does not flow
into the instrument housing.
Check the tubing system for leaks before working with the flammable gas. For
example use helium and a corresponding gas leak detector. Check also the
measuring cell.
Before loading the cell with the flammable gas, the air has to be fully replaced by
an inert gas so that the explosive gas/oxygen concentration is avoided (pressurize to 1 MPa with nitrogen and release the gas at least three times or purge long
enough with the inert gas).
Never open the furnace when it is hot, wait until the furnace temperature is below
30 C.
Work in a room especially designed for working with explosive gases (alarm
system, wall thickness and so on).
Put the HP DSC 1 behind safety walls or operate it from a safe place. Make sure
that no other persons are in danger.
Consider the risk that the flammable gas can accumulate in the instrument housing. If needed, purge the housing with inert gases to avoid dangerous explosive
concentrations.
The flammable gas may chemically or physically alter some materials of the
measuring cell, furnace, crucible and the sample itself. This could damage the
sensor or other parts of the DSC by forming alloys or in other ways.
Please note that the above list is not exhaustive; other items and precautions may
have to be considered.
1-10
0911
HP DSC 1
1.5.2
HP DSC 1
Never switch off the PC during power-up. Problems could arise the next time it is
powered up.
Always keep the fan opening and the ventilation grill of the instrument free to assure good cooling! Objects such as paper should not cover these openings.
Check the set operating voltage before you switch on the instrument! The instrument may suffer damage if the operating voltage does not match the line voltage.
Purge the measuring cell with an inert gas if you measure samples which form
corrosive gases during decomposition!
0911
1-11
HP DSC 1
1.6
This equipment has been tested and found to comply with the limits for a Class A
digital device, pursuant to both Part 15 of the FCC Rules and the radio interference
regulations of the Canadian Department of Communications. These limits are designed to provide reasonable protection against harmful interference when the equipment is operated in a commercial environment. This equipment generates uses and
can radiate radio frequency energy and, if not installed and used in accordance with
the instruction manual, may cause harmful interference to radio communications.
Operating this equipment in a residential area is likely to cause harmful interference,
in which case the user will be required to correct the interference at his expense.
Cet appareil a t test et s'est avr conforme aux limites prvues pour les appareils
numriques de classe A et la partie 15 des rglements FCC et la rglementation
des radio - interfrences du Canadian Department of Communications. Ces limites
sont destines fournir une protection adquate contre les interfrences nfastes lorsque I' appareil est utilis dans un environnement commercial. Cet appareil gnre,
utilise et peut radier une nergie frquence radiolectrique; II est en outre susceptible
d'engendrer des interfrences avec les communications radio, s'il n'est pas install et
utilis conformment aux instructions du mode d'emploi. L'utilisation de cet appareil
dans les zones rsidentieIIes peut causer des interfrences nfastes, auquel cas l'exploitant sera amen prendre les dispositions utiles pour palier aux interfrences
ses propres frais.
1-12
0911
HP DSC 1
Contents
2.1
Introduction................................................................................................................................ 2-1
2.2
2.2.1
2.2.2
2.2.3
2.2.4
2.2.5
2.3
2.3.1
Installation.................................................................................................................................. 2-10
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2-i
HP DSC 1
This chapter describes the design and function of the HP DSC 1. It first presents an
overview of the different configurations of the HP DSC 1 and then describes the measuring cell in more detail.
2.1
Introduction
The HP DSC 1 module is a high pressure differential scanning calorimeter and includes a stainless steel pressure cylinder containing the furnace, the DSC measuring
sensor and fittings for the gas inflow and outflow. A pressure gauge shows the pressure and a built-in safety rupture disc protects the cell against excessive pressure.
The pressure cell allows measurements up to a maximum working pressure of 10
MPa (100 bar) from room temperature up to 700 C.
The HP DSC 1 is based on the measurement technique of the DSC 1. The DSC measuring sensor is housed in the high pressure cylinder.
The HP DSC 1 replaces the HP DSC827e and includes the following new features and
improvements:
Communication with the PC and STARe Software is now possible via an Ethernet
TCP/IP connection.
The HP DSC 1 has a higher sampling rate (50 points per seconds), which
makes it possible to run TOPEM experiments.
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2-1
HP DSC 1
2.2
Module electronics
SmartSens terminal
400W furnace supply, used for measurements in the temperature range from
room temperature to 700 C with a maximum heating rate of 100 K/min (at
700 C).
The HP DSC 1 module can be individually expanded for more demanding applications with a number of hardware options. When you place your order, you determine
the actual configuration of your HP DSC 1. You can expand your HP DSC 1 with the
required hardware options to meet new demands at any time in the future.
2-2
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HP DSC 1
2.2.1
Outward appearance
The basic configuration of the module is always the same (see Fig. 1).
SmartSens Terminal
Gas connections
Rupture disc
Lifting bracket
Tube connection
Recess in housing
The module stands on three adjustable leveling screws, 1. You can adjust the height
and level the module horizontally.
0911
leveling screws
2-3
HP DSC 1
measuring cell
The measuring cell is located in the pressure cylinder, 7. The pressure cylinder is
opened and closed manually by removing or installing the pressure cylinder cover.
Never touch the furnace, furnace lid or a sample you have just removed from the furnace! The furnace can reach a temperature of up to 700 C. Use tweezers to remove
the lid or a sample.
Never place the furnace lid on any surface of the instrument when the lid is hot. These
surfaces will be damaged.
SmartSens Terminal
The SmartSens Terminal has a touch screen and can display and call up information
(see Fig. 2). Commands can be entered using the terminal keys and the touch
screen.
2-4
0911
HP DSC 1
All the external connections are located at the rear of the HP DSC 1 module.
external connections
Main switch
10 Instrument ID
11 Serial number
Rating plate
12 Water outlet
13 Water inlet
Connection to synchronize
external devices
0911
GC10
Ethernet connection
2-5
HP DSC 1
2.2.2
AC connections
The power supply inlet socket for the AC power supply cable
The line socket, which is coupled with the main switch. If you switch off the
HP DSC 1, you also switch off the peripheral unit connected to this line socket.
-
You can switch off the power to the furnace supply (Furnace Power Off) at the
end of an experiment.
The HP DSC 1 module is built for either 115 V or 230 V alternating power supply
voltages (50 Hz or 60 Hz) during assembly in the factory. This voltage cannot be
changed afterward.
The fuses are located on the rear panel as shown in Fig 3. There is a fuse for the
power supply outlet and a fuse for the electronics supply.
The voltage and current ratings of the fuses are indicated on rating plate on the back
panel. Please refer to these values to find suitable replacements for any blown fuses.
Switch off the HP DSC 1 and unplug the power cable from the power outlet.
Change the fuses at the rear of the module. Do not open the housing.
For more information on power supply and fuses, see the Chapter 4, Installation.
2-6
0911
HP DSC 1
Ethernet TCP/IP connection: The module is connected via the Ethernet TCP/IP connection to the Ethernet port of the PC.
The gas connections for the gas supply are located at the bottom right side of the
HP DSC 1 module:
2.2.3
Parts supplied
Calibration kit
Operating Instructions
Declaration of conformity
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2-7
HP DSC 1
2.2.4
Measuring cell
The measuring cell essentially consists of the furnace and the DSC sensor. It is explained in detail in the following.
In the measuring cell, you can take advantage of the HSS7 high-sensitivity sensor
with its 120 gold-gold/palladium thermocouples. The measuring cell can also be operated with the full-range FRS5 sensor. With both sensors, the digital resolution of
the measurement signal is less than 0.04 W.
A/D-converter
You can read more than 16 million measuring points with the new 24 bit analog/digital converter.
furnace
The furnace, which is made of pure silver, is pressed against the insulator disk of the
flat heating element by the spring loaded furnace assembly. A Pt100 temperature
sensor measures the temperature signal. The DSC sensor is mounted on a glass ceramic disk that is in direct thermal contact with the heater plate of the silver furnace.
The heat of the furnace is removed over the disc-shaped thermoresistor to the heat
sink See Fig.4).
purge gas
The purge gas inlet supplies the gas (usually about 80 mL/min) to the inlet at the
bottom of the furnace body (AUX). Here it is heated to the cell temperature and then
enters the sample chamber. Finally it escapes through the hole in the furnace lid and
is vented at the gas outlet together with the pressure build up gas.
cooling
An external cooling device must be connected providing a water flow rate of 20 l/h,
with water temperatures between 20 and 30 C. Refer to Chapter 3 Cooling for specific details.
2-8
0911
HP DSC 1
2.2.5
Measurement principle
The DSC measurements are based on the well-proven Boersma or heat flux principle.
The experimental parameters are entered in the PC. The operator then sends the temperature program for the individual segments to the measuring module.
During a measurement, measurement data is continuously transmitted from the module to the PC. The data is presented as an online curve in the Module Control Window.
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2-9
HP DSC 1
2.3
The Switched Line Socket option allows you to switch peripheral units (e.g. a refrigerated circulator) on and off in order to save power. The peripheral unit is switched on
and off via the line socket depending on how you defined it in the experimental
method.
At the end of the experiment, the furnace supply can also be switched off. The module
remains in this power saving mode until it is reactivated for the next experiment.
2.3.1
Installation
51 119 955
51 119 954
A power switch should only be installed by a qualified person who is familiar with
your local installation regulations.
2-10
0911
HP DSC 1
Cooling
Cooling
3.1
We recommend using a refrigerated circulator for cooling the high pressure cylinder.
The following requirements for the cooling system must be fulfilled to ensure that the
high pressure cylinder and the measuring cell are cooled sufficiently and the temperature control system operates properly.
If the temperature monitoring system is operated outside of the permitted range,
measurement errors can occur.
Required cooling power for operation:
Up to 500 C: 200W
Higher than 500 C: 400 W
Constancy of temperature: +/- 1 C
Pump and suction capacities:
Pump capacity: 10 L/min at 0 bar
Suction capacity: 250 mbar at 0 L/min
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3-1
HP DSC 1
Installation
Installation
Contents
4.1
4.1.1
4.1.2
4.1.3
4.2
4.3
4.4
4.5
4.6
4.6.1
4.6.2
4.6.3
Establishing communication between the STARe Software and your HP DSC 1 module ...................... 4-10
4.6.4
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4-i
HP DSC 1
Installation
Installation
4.1
Location
A well-chosen location for the HP DSC 1 is essential to ensure reliable and precise
measurement results.
The HP DSC 1 should only be operated indoors and at an altitude of less than
3000 m above sea level.
The module is designed for operation at room temperatures in the range
+ 10 C to + 31 C and at a relative humidity of 20% to 80% under conditions
where no condensation occurs.
Before switching on the module, allow all its parts to reach a temperature between
+10 C and +31 C. Make sure that the relative humidity is between 20 and 80%
and non-condensing conditions are met at its installation location.
4.1.1
Electromagnetic fields are present everywhere in our environment. These can cause
interference and adversely affect the performance of the HP DSC 1 by creating artifacts, for example.
When choosing the installation location for the HP DSC 1, avoid the following electromagnetic disturbances:
Ensure that no vertical power lines, motors, or similar devices are near the module. Check the neighboring rooms as well.
Ensure that the following minimum distances are kept between the HP DSC 1 and
the following devices:
electromagnetic
disturbances
0.5 m to a PC
1.0 m to a printer or a plotter with a power supply transformer
1.2 m to a refrigerated circulator
1.0 m to any lamp with a fluorescent tube
5.0 m to a refrigerator or a deep freezer
Avoid close proximity to all other electrical instruments. They are possible causes
of noise and should be kept well away from the HP DSC 1.
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4-1
Installation
HP DSC 1
4.1.2
working area
Working area
4.1.3
Room conditions
The module should only be operated indoors and at an altitude of less than 3000 m
above sea level.
room conditions
4-2
0911
HP DSC 1
4.2
Installation
Please refer to chapter 3, Installation Instructions of the STARe Software User Hand-
book.
4.3
Gas supplies
Depending on the application, the following gases can be used as purge gas: O2 or
an inert gas such as N2, Ar or He.
The gas is supplied from gas bottles: A 2-stage pressure reduction valve with a pressure gauge from 0 to 100 bar should be installed for each gas.
Flow meters
To adjust the gas flow rate, flow meters with the following flow ranges should be
used:
Purge gas flow rate:
0911
0 100 mL/min
4-3
Installation
HP DSC 1
4.4
Power supply
To operate the HP DSC 1 you require a stable AC power supply system that complies
with the Emission Standard EN 61326-1:2006 for industrial environments. Additionally, the AC voltage fluctuation must be within a tolerance of 10% of the nominal AC
supply voltage.
If your AC power supply does not meet these requirements, contact your local
METTLER TOLEDO service engineer for the installation of a stabilized power supply
unit.
On the HP DSC 1 module:
Check the operating voltage set for the instrument before switching it on. The instrument can suffer damage if the operating voltage does not match the AC supply voltage.
Use only the fuses specified on the rating plate on the back panel of the
HP DSC 1.
The HP DSC 1 has two electrical power supply systems:
voltage
The HP DSC 1 is manufactured in the factory for alternating voltages of either 115 V
or 230 V (50 or 60 Hz). The voltage is indicated on the rating plate on the rear
panel.
The fuses of the HP DSC 1 are located on the rear panel as shown in 3 in Chapter 2.
There is a fuse for the power supply outlet and a fuse for the electronics supply.
The voltage and current ratings of the fuses are indicated on rating plate on the back
panel of the HP DSC 1. Please refer to these values if you have to replace any blown
fuses.
4-4
0911
HP DSC 1
4.5
Installation
Never try to carry the HP DSC 1 module alone. The instrument weighs about 40 kg. At
least two people are needed to carry the instrument. Hold the module firmly on the
underside with both hands.
Proceed as follows to install the HP DSC 1:
1
The HP DSC 1 module is built for 115 V or 230 V alternating voltages in the factory.
This voltage cannot be changed.
3
Before switching on, check the voltage indicated on the rating plate on the rear
panel. If the voltage is wrong, call a service engineer.
Connect the Ethernet socket on the rear panel to the Ethernet port on the PC with
the Ethernet cable supplied. Use the Cat 5e cable to connect to a switch in an IT
network. Use the crossover cable to directly connect to the PC. You can find more
information on setting up a TCP/IP connections in Chapter 1 of the STARe Software User Handbook.
leveling screws
voltage
On delivery, the instrument is screwed together; the furnace lid, and the alumina
wool mat for the pressure cylinder cover are individually packed.
Remove the 4 nuts (a - d).
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4-5
Installation
HP DSC 1
The gas connections, GAS IN for the pressure buildup and AUX IN for the purge gas
are designed for pipelines with an external diameter of 1/8 inch.
Push the pipeline into the gas connection up to the stop and tighten the nut
by hand.
Tighten the nut by a 1/4 turn.
MPa
10
5
1500
1000
500
2000
psi
2300
15
4
7
5
AUX
OUT
IN
10
Bulkhead union
for purge gas in
Bulkhead union
for pressure gas in
10
4-6
0911
HP DSC 1
Installation
Attach the tube to the gas source and perform the leak test (chapter 6, section
Leak test).
If using the PC 10, make sure that the connections are properly inserted and
tightened. See the diagram below for the connections on the HP DSC 1.
AUX
11 Rupture disc
INLET
12 Tube connection
10 OUTLET
Always use a gas source (bottle or line) that has a relief valve and a check valve! Set
the pressure at the reducing valve to the desired measuring cell pressure.
The tubes that link the gas sources and the pressure cell must match the reduced
pressure requirements of the gas sources.
Decomposition products from samples can be carried out by the purge gas. The
gases are transferred through the gas tubing to the gas outlet at the right side of
the module.
9
0911
4-7
Installation
HP DSC 1
4.6
STARe Software version 9.30 or later is required to run the HP DSC 1. Before you start
up your module you have to make some preparations in the STARe Software. This
section describes the functions of the STARe Software Install Window that are specific
to the HP DSC 1 module. The full description of the Install Window can be found in
the online Help to the Install Window.
Chapter 5, Switching on and switching off, explains how to switch on your HP DSC 1.
4.6.1
Click Functions/Install Window in the main menu bar of the STARe Software.
An Install Window opens and the symbol
4-8
0911
HP DSC 1
4.6.2
Installation
To install your module in the STARe Software, you have to open a data set belonging
to your module in the STARe Software. You can import the data set from the module
CD ROM supplied and open it in the STARe Software. You can also create a new individual data set and perform the installation in the STARe Software step-by-step.
To import the module data set of your STARe module from the module CD ROM supplied:
1
Insert the module CD ROM in the CD ROM drive. In the Install Window, click the
Module tab and then click Import on the File menu.
The Import Module dialog box appears.
Mark the data set of your HP DSC 1 module and click Import.
The data set is imported together with the settings and adjustment data.
Instead of using the supplied CD ROM you can also create a new module data
set in the STARe Software. The module data set created in this way contains only
the default adjustment data. However, if you want to use a module data set created in this way for your measurements, you must first of all adjust your
HP DSC 1 module. You can find instructions on how to adjust your HP DSC 1
module in the chapter Calibration and Adjustment. During the adjustment, the
STARe Software saves the new adjustment data and at the same time overwrites
the previous adjustment data (for example, the default values).
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4-9
Installation
HP DSC 1
4.6.3
If you have opened a data set for your HP DSC 1 module in the STARe Software, you
can establish communication by connecting it to a port on your PC.
To establish communication between the STARe Software and the HP DSC 1 module:
1
connecting to port
Detailed information on how to create a new connection for your HP DSC 1 module is
given in the online Help to the Install Window under "Administering connections".
The HP DSC 1 module is connected to the port and communication is established after a brief
time lag. The activated connection is indicated by a continuous solid red line.
4-10
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HP DSC 1
Installation
0911
4-11
Installation
HP DSC 1
4.6.4
In the Install Window, you can view the current adjustment data of your HP DSC 1
module, but you cannot change the adjustment values. The data corresponds to the
most recent adjustment of your HP DSC 1 module. It is identical to the calibration
data displayed in the information boxes at the end of the individual calibration runs.
You can find instructions on how to calibrate and adjust your HP DSC 1 module in
the Chapter Calibration and adjustment.
Your HP DSC 1 module was adjusted in the factory before delivery. If you have not
performed any adjustments and not imported any adjustment data, the data corresponds to the factory adjustment.
To view the HP DSC 1 module adjustment data:
1
Open the data set of your HP DSC 1 module in the Install Window as follows:
Click the Module tab and then click File/Open.
The Open Module dialog box appears with a list of the modules stored in the database:
Click your HP DSC 1 module data set in the list and then click OK.
The Open Module dialog box is closed and the data set of your module appears on the
Module tabbed page.
The temperature adjustment data is displayed in the upper part of the dialog box (cell temperature and Tau Lag adjustment). The heat flow adjustment data is displayed in the lower
part (the data for the calorimetric sensitivity components E Indium and dE relative).
The dialog box displayed above contains the default data of the STARe database.
The STARe Software uses this data if no other adjustment data for your module is
available.
You can print the adjustment data together with the other module data by clicking
File/Print
4-12
0911
HP DSC 1
Before switching on the HP DSC 1, make sure that all its parts have reached temperatures between +10 C and +31 C and the relative humidity is between 20% and
80% and no condensation can occur.
5.1
Switching on
Switch on the HP DSC 1. The power switch is located on the rear panel. See Fig.
3 in chapter 2. The order in which you switch on the PC and the module is not
important.
If no communication can be established between the module and the PC, check
the following causes:
The connection has not been set up correctly in the STARe Software.
The Ethernet cable is not connected correctly or the wrong cable is being
used.
See chapter 10, Error Messages and Warnings, under List of warnings.
5.2
You can perform an indium check to see if the measurement results of your module
are within the specified tolerances.
Perform an indium check. If the results from the indium check are within the limits of tolerance, you can start your measurements.
5.3
Switching off
Never switch the refrigerated circulator off when the temperature of the measuring cell
is above 100 C. The surroundings of the measuring cell could heat up in an uncontrolled manner.
For sample removal, the temperature should be below 40 C.
1
Always remove the last sample crucible before switching off the instrument.
Switch off the module. The power switch is located on the rear panel. See Fig. 3
in chapter 2. The order in which you switch off the PC and the module is not important.
0911
5-1
HP DSC 1
Measurements
Measurements
Contents
6.1
6.2
6.3
6.4
6.5
6.5.1
6.6
6.6.1
6.7
6.7.2
Performing an experiment without a flow meter, flow controller or pressure controller............................ 6-7
6.7.3
Performing an experiment with a flow meter, flow controller or pressure controller .............................. 6-10
6.7.4
0911
6-i
HP DSC 1
Measurements
Measurements
6.1
The DSC cell including the furnace and furnace lid must be clean and free of any
residue.
0911
6-1
Measurements
HP DSC 1
6.2
Leak test
Before you perform the first measurement under pressure, you should test the cell for
leaks with an inert gas such as nitrogen.
Always use a gas source (bottle or line) that has a check valve and a reducing valve!
Set the pressure at the reducing valve to the desired measuring cell pressure.
1
Attach the gas source to inlet GAS IN (see chapter 4, section 4.5).
3 Set the pressure of the gas source with the reducing valve to 10 MPa and
open the gas source.
4 Open INLET valve: The pressure should increase at a maximum rate of
0.1 MPa/s.
5
7 The pressure drop in the cell should be less than 0.2 MPa/30 min. If this is
not the case, several malfunctions can be the cause (see chapter 9, section 9.2).
8
6.3
Open the OUTLET valve after the test: The gas flows out of the GAS OUT outlet.
The built-in safety rupture disc is intended to prevent an excessive pressure load on
the pressure cell. It ruptures when its response pressure is exceeded.
The nominal bursting pressure of the rupture disc is between 12.4 and 13.8 MPa.
The attainable pressure in dynamic measurements should therefore not be higher
than 10 MPa (see section Pressure not controlled in this chapter).
As soon as a leak has been found at the outlet of the rupture disc, you must change
the rupture disc! (see chapter 9, section Changing the rupture disc).
Install only a rupture disc supplied by METTLER TOLEDO that responds at the required
response pressure! (see chapter 12, Accessories).
A wrong rupture disc may not respond until the pressure is too high: The pressure cell
could explode!
6-2
0911
HP DSC 1
6.4
Measurements
The Pressure Controller PC10 includes the BROOKS control and display unit, which
automatically regulates the pressure and the gas flow within the measuring cell.
1 Connection to AUX
2 Connection to INLET
9 Bridging tube
3 Connection to OUTLET
10 Fitting
4 Diagram of connections
11 Fitting
5 Pressure controller
13 Quick-Vent Valve
7 Gas controller
Align the gas connections of the PC10 and the HP DSC 1 by adjusting the leveling screws at the bottom of the PC10.
These should be aligned properly to avoid bad connections or even damage.
Attach cables for gas flow and pressure from BROOKS control and display unit to
the PC10.
0911
6-3
Measurements
HP DSC 1
Connect the gas to the INLET and tighten the screw. Make sure that the QuickVent Valve is open.
At the end of the experiment remember to open the Quick-Vent Valve to release
the pressure.
10 Check that all pressure has been released. Sometimes pressure can be built up
again unknowingly if the instrument hasnt been completely vented.
*Refer to the operating instructions of the BROOKS control and display unit for further
information.
6-4
0911
HP DSC 1
Measurements
6.5
Preparing an experiment
6.5.1
If you are using the Pressure Controller PC 10, follow the instructions for connecting
this instrument first before continuing with the following procedure (see section 6.4,
Connecting the Pressure Controller PC10).
Proceed as follows to connect the gas sources for the pressure build up and the
purge gas.
1
Attach the gas source for the pressure buildup to the inlet GAS IN.
If necessary, connect a gas supply for purging the measuring cell to inlet AUX IN
(see chapter 4, section Installing the HP DSC 1 Module).
Optional step: Attach the tubing connection to the outlet GAS OUT and connect
the tubing for leading off the gas flowing out (see chapter 12, Accessories).
Optional step: Attach the tubing connection to the safety rupture disc and connect
it to the pressure tubing ( 14 mm). Fasten it with a clamp so that if the rupture
disc bursts the escaping gas at that point will be led off.
6.6
Before you can perform a measurement on the HP DSC 1, you must make the following preparations. Refer to the STARe Software online Help for more information.
1
Check the DSC sensor position. The DSC sensor must be positioned exactly in
the center of the furnace.
If the DSC sensor is not in the center position, adjust the DSC sensor with the
centering gauge.
Perform an indium check (see chapter 8, section Calibration and Adjustment: the
indium check.).
0911
6-5
Measurements
HP DSC 1
6.6.1
Depending on the application, you can work with a crucible without a lid, for example, when measuring oils to determine their oxidative stability.
For enthalpy determinations, you should perforate the crucible lid once using the needle from the crucible set.
For determinations of boiling temperatures, perforate the crucible lid, on a hard surface with a compass point (hole diameter: approx. 50 m) or use the perforated lids
from METTLER TOLEDO.
Dont use a hermetically sealed crucible: It will collapse (under pressure > 1 MPa!)
6.7
Performing an experiment
6-6
If you need a more accurate pressure reading for your measurements, you can
attach a PC 10. For more information, see chapters 6.4 and 6.7.2
The closed cell needs a relatively long time to cool down to room temperature after a measurement. The cooling proceeds faster if the cell is under pressure.
If you need a pure gas atmosphere, fill (up to approx. 2 MPa) and empty (close
INLET valve, open OUTLET valve) the pressure cell three times with gas, before
you fill the cell with gas for the measurement.
0911
HP DSC 1
Measurements
6.7.2 Performing an experiment without a flow meter, flow controller and pressure controller
Proceed as follows to perform the experiment:
1
Open the pressure cell by unscrewing the four nuts on the pressure cylinder cover
and lifting it off. Remove the alumina wool mat.
Never touch the furnace, the furnace lid or a sample that has just been removed from
the furnace. The temperature of the furnace can reach up to 700 C. Always use
tweezers to remove the furnace lid or crucible.
2
Place the sample crucible carefully on the left pan position of the DSC sensor and
place an empty reference crucible on the right.
Replace the furnace lid using tweezers. Make sure that the lid is in the correct
position and the tooth on the furnace top fits into the notch in the side of the lid.
You could otherwise jam it.
Place the alumina wool mat in the pressure cylinder on top of the furnace and
press down. Before mounting the pressure cylinder cover make sure that its Oring is free of alumina wool fibers.
Mount the pressure cylinder cover and tighten the four nuts by hand. This is sufficient to seal the system.
0911
6-7
Measurements
HP DSC 1
Start an experiment on the module. Wait until the measuring cell has reached the
insert temperature.
The module goes to the insert temperature. The request to insert the sample is displayed
on the touch screen and in the Module Control Window.
Open the OUTLET valve slowly to release the pressure at the end of the experiment.
When the pressure gauge shows no pressure, open the valve fully to be certain
that the cell is definitely at atmospheric pressure.
Do not unscrew the nuts until the measuring cell is at atmospheric pressure! Before
removing one nut, unscrew all 4 nuts by one turn.
5
Remove the pressure cylinder cover, the alumina wool mat and the furnace lid.
If you are using an alumina crucible, allow it to cool down first before placing it on a
cold surface. The crucible might otherwise crack due to too rapid cooling. In general,
do not place the crucibles on a cold surface or on the instrument housing.
8
Standby temperature
9
furnace power off
6-8
Click RESET to set the measuring cell to the standby temperature after the measurement.
Click RESET twice in the Module Control Window to switch off the heating power
after the measurement.
0911
HP DSC 1
Measurements
6.5
6.0
5.5
5.0
T [C]
0
100
200
300
400
500
600
If you measure over a small temperature range, the pressure change is correspondingly small. If you require accurate pressure data, we advise plotting a pressuretemperature curve.
0911
6-9
Measurements
HP DSC 1
6.7.3 Performing an experiment with a flow meter, flow controller or pressure controller
Gas connection possibilities with the PC 10
With PC 10 with 1 gas connected
6-10
0911
HP DSC 1
Measurements
Without
AUX IN closed
AUX CONTROL closed
INLET closed
AUX IN
OUTLET closed
isothermal: pressure constant
dynamic: pressure increase
CONTROL
Fig. 1
INLET
OUTLET
AUX IN open
AUX CONTROL open
INLET closed
AUX IN
CONTROL
Fig. 2
INLET
OUTLET
AUX IN open
in isothermal measurements *
Flow rate (for example,50 mL/min)
(Reducing valve of purge gas source
set to same pressure as measuring
cell pressure)
INLET closed
AUX IN
Flow
controller
CONTROL
INLET
OUTLET open
isothermal: pressure constant
dynamic: pressure increase*
OUTLET
Fig. 3
With flow rate control in isothermal
and dynamic measurements.
Flow rate (for example, 50 mL/min)
(Reducing valve of purge gas source
set somewhat higher than measuring
cell pressure)
We recommend BROOKS mass flow controller
AUX IN open
AUX CONTROL open
Flow
controller
INLET closed
AUX IN
CONTROL
INLET
Fig. 4
* In dynamic measurements, the flow supplied by the purge gas cylinder decreases with the volume expansion in the pressure
cylinder. Depending on the heating rate and the temperature range, this can cause the pressure to remain practically constant.
** The volume of the pressure cylinder is approx. 0.9 l. With a flow rate of 50 mL/min (purge gas), the pressure would increase
only by around 0.1 MPa within 18 min with OUTLET closed.
0911
6-11
Measurements
HP DSC 1
Without
AUX IN closed
AUX CONTROL closed
INLET closed
OUTLET open
AUX IN
Pressure
controller
CONTROL
Fig. 5
INLET
AUX IN open
AUX CONTROL: Set flow rate (for
example, 50 mL/min)
INLET closed
AUX IN
Pressure
controller
CONTROL
INLET
OUTLET
OUTLET open
isothermal: pressure and flow rate
constant
dynamic: pressure and flow rate
constant
AUX IN open
AUX CONTROL: Set flow rate (for
example, 50 mL/min)
Flow meter
INLET closed
AUX IN
CONTROL
INLET
Pressure
controller
OUTLET open
isothermal: pressure and flow rate
constant
OUTLET
Fig. 7
AUX IN open
Flow
controller
INLET closed
AUX IN
Control In
Fig. 8
INLET
Pressure
controller
OUTLET
OUTLET open
isothermal: pressure and flow rate
constant
dynamic: pressure and flow rate
constant
*** In isothermal measurements, the display of the flow meter remains constant, in dynamic measurements not.
6-12
0911
HP DSC 1
Measurements
Attach the tubing connection to the pressure controller outlet and connect tubing
to lead off the gas.
Connect the pressure controller to the control and display unit (cable).
Open the pressure cell by unscrewing the four nuts on the pressure cylinder cover
and lifting it off. Remove the alumina wool mat.
Never touch the furnace, the furnace lid or a sample that has just been removed from
the furnace. The temperature of the furnace can reach up to 700 C. Always use
tweezers to remove the furnace lid or crucible.
5
Place the sample crucible carefully on the left pan position of the DSC sensor and
place an empty reference pan on the right.
Replace the furnace lid using tweezers. Make sure that the lid is in the correct
position and the tooth on the furnace top fits into the notch in the side of the lid.
You could otherwise jam it.
10 Place the alumina wool mat in the pressure cylinder on top of the furnace and
press down. Before mounting the pressure cylinder cover make sure that its Oring is free of alumina wool fibers.
11 Mount the pressure cylinder cover and tighten the four nuts by hand. This is sufficient to seal the system.
12 Set the flow rate of the cooling water to approx. 30 l/h.
13 Close the OUTLET, INLET and AUX IN valves.
14 Build up the pressure to somewhat above the target value (inlet GAS IN).
15 Close the INLET valve.
16 Set the target pressure at the control unit and switch on the instrument.
17 Open the OUTLET valve and wait until a constant pressure is shown.
0911
6-13
Measurements
send experiment
start measurement
HP DSC 1
18 Send an experiment.
19 Click OK in the Module Control Window to start the measurement.
The measurement starts. At the end of the experiment the REMOVE SAMPLE request
appears in the Module Control Window
If you start your measurements at a relatively high start temperature, in other words
the measuring cell is heated up rapidly, we advise waiting for a constant pressure
display before starting the experiment (confirm Insert Sample after getting a constant
pressure).
Attach the tubing connection (see Accessories) at outlet GAS OUT and connect to
the flow meter using plastic tubing.
Set the pressure for both gas cylinders (pressure buildup/purging) at the reducing
valve to the same value.
Connect both gas cylinders (GAS IN for pressure buildup, AUX IN for purging)
and open.
Open INLET valve until pressure buildup is complete (if needed, empty and fill
with gas to obtain a pure gas atmosphere). Then close INLET valve.
Open the experiment window and select the method you need. Type in sample
name and weight. Send the experiment and wait until the cell is heated to the insert temperature.
Do not confirm INSERT SAMPLE with OK, but release the pressure (OUTLET
valve).
Set the flow with the OUTLET valve and observe it for a few minutes to ensure the
same OUTLET setting for the measurement. Do not readjust.
10 The gas that escapes is topped up by the purge gas cylinder, the set pressure
remains constant.
11 Close AUX IN valve and make sure the INLET valve is closed.
12 Close the gas cylinder (pressure buildup) and disconnect the gas connection
from GAS IN.
13 Open INLET valve so that the gas is vented via GAS IN and reattach the gas connection (see Note a).
6-14
0911
HP DSC 1
Measurements
Open the pressure cell by unscrewing the four nuts on the pressure cylinder cover
and lifting it off.
Be careful: its heavy.
Never touch the furnace, the furnace lid or a sample that has just been removed from
the furnace. The temperature of the furnace can reach up to 700 C. Always use
tweezers to remove the furnace lid or crucible.
3
Place the sample crucible carefully on the left pan position of the DSC sensor and
place an empty reference crucible on the right.
Replace the furnace lid using tweezers. Make sure that the lid is in the correct
position and the tooth on the furnace top fits into the notch in the side of the lid.
You could otherwise jam it.
Place the alumina wool mat in the pressure cylinder on top of the furnace and
press down. Before mounting the pressure cylinder cover make sure that its Oring is free of alumina wool fibers.
Mount the pressure cylinder cover and tighten the four nuts by hand. This suffices
to seal the system.
Build up the pressure via GAS IN, then close INLET valve and open AUX IN valve
fully. The flow rate set with the OUTLET valve lowers the pressure, but it is compensated by purge gas that is flowing in.
10 Send an experiment.
The module goes to the insert temperature. The INSERT SAMPLE request is displayed in the
Module Control Window.
6-15
Measurements
HP DSC 1
Attach the tubing connection to the pressure controller outlet and connect the tubing to lead off the gas that is flowing out.
Connect the flow controller and pressure controller to the control and display unit
(cable).
Open the pressure cell by unscrewing the four nuts on the pressure cylinder cover
and lifting it off. Remove the alumina wool mat.
Never touch the furnace, the furnace lid or a sample that has just been removed from
the furnace. The temperature of the furnace can reach up to 700 C. Always use
tweezers to remove the furnace lid or crucible.
7
insert sample
Place the sample pan carefully on the left pan position of the DSC sensor. Place
an empty reference pan on the right.
Replace the furnace lid using tweezers. Make sure that the lid is in the correct
position and the tooth on the furnace top fits into the notch in the side of the lid.
You could otherwise jam it.
10 Place the alumina wool mat in the pressure cylinder on top of the furnace and
press down. Before mounting the pressure cylinder cover make sure that its Oring is free of alumina wool fibers.
11 Mount the pressure cylinder cover and tighten the four nuts by hand. This suffices
to seal the system.
12 Switch on the control unit if you have not already done so. Set the target values
of the pressure and gas flow rate on the control unit. Close the Quick-Vent valve.
13 Build up the pressure somewhat above the target value (GAS IN inlet).
14 Close INLET valve.
6-16
0911
HP DSC 1
Measurements
15 Set the pressure of the purge gas with the reducing valve somewhat above the
measuring cell pressure and open the purge gas valve.
16 Open first the AUX IN and CONTROL IN valves then the OUTLET valve fully and
wait until the pressure reading is constant.
17 Send an experiment.
The module goes to the insert temperature.
The INSERT SAMPLE request is displayed in the Module Control Window.
start measurement
The measurement starts. At the end of the experiment the REMOVE SAMPLE request appears in the Module Control Window.
19 Set the pressure on the control unit to 0 to relieve the pressure at the end of the
measurement.
If you start your measurements at a relatively high start temperature (the measuring
cell is heated up rapidly), we advise waiting for a constant pressure display before
confirming INSERT SAMPLE on the HP DSC 1 module display.
If you use the same gas for pressure buildup and purging, you can attach a PC 10.
For more information, see chapters 6.4 and 6.7.2.
0911
6-17
Measurements
HP DSC 1
At the end of the experiment, open the OUTLET valve slowly to release the pressure. If you have a pressure controller connected set the pressure on the control
unit to 0 to relieve the pressure.
When the pressure gauge shows no pressure, open the valve fully to be certain
that the cell is definitely at atmospheric pressure.
Do not unscrew the nuts until the measuring cell is at atmospheric pressure! Before
removing one nut, unscrew all 4 nuts by one turn.
3
Remove the pressure cylinder cover, the alumina wool mat and the furnace lid.
If you are using an alumina crucible, allow it to cool down first before placing it on a
cold surface. The crucible might otherwise crack due to too rapid cooling. In general,
do not place the crucibles on a cold surface or on the instrument housing.
Standby temperature
Confirm the REMOVE SAMPLE request in the Module Control Window with OK.
To set the measuring cell to the standby temperature after the measurement, click
RESET in the Module Control Window.
The cell goes to standby temperature
8
furnace power off
To switch off the heating power after the measurement, click RESET twice in the
Module Control Window.
6.7.4
At elevated pressure, the value of the calorimetric constant Eindium is lowered compared with that at atmospheric pressure: The increasing gas density leads to a
change in the thermal resistance between the measuring cell and the sample crucible.
The decrease amounts to approx. 0.6 %/MPa.
For pressure DSC experiments with maximum calorimetric accuracy, you need to run
a heat flow calibration EIn under the pressure you need, for example, 5 MPa nitrogen.
6-18
0911
SmartSens Terminal
SmartSens Terminal
Contents
7.1
7.1.1
7.2
7.3
7.4
7.4.1
7.4.2
7.4.3
7.4.4
7.4.5
7.5
0909
7-i
SmartSens Terminal
SmartSens Terminal
This chapter contains basic information on how to operate the following modules using the SmartSens Terminal:
TGA/DSC 1
DSC 1
HP DSC 1
7.1
The SmartSens Terminal helps you to operate the TGA/DSC 1, DSC 1and HP DSC 1
modules. The main feature of the SmartSens Terminal is the colored touch screen, a
touch-sensitive monitor. The touch screen not only displays information, it also allows you to enter commands by touching certain areas on its surface. You can
choose the information displayed on the screen, change terminal settings or perform
certain operations on the TGA/DSC 1, DSC 1and HP DSC 1 modules.
The following figure provides an overview of the SmartSens Terminal:
SmartSens sensors
Title bar
State indicator
RESET key
HOME key
Touch screen
FURNACE key
SETUP key
0909
7-1
SmartSens Terminal
There are contact-free infrared sensors in the left and right upper corners, (SmartSens
sensors) that respond to movement. The two SmartSens sensors can be assigned different functions such as opening the furnace or scrolling through the displayed measurement values (see Section 7.5, SmartSens Terminal settings). This allows you to
perform certain operations on the SmartSens Terminal without touching it and possibly disturbing a measurement.
The keys arranged on both sides of the touch screen can be used to enter frequently
used commands.
The monitor displays the user interface of the SmartSens Terminal software. The user
interface consists of various menus and windows which in turn can contain elements
such as menus, buttons or symbols.
The front side of the Smartsens Terminal is protected by a transparent plastic cover
that can easily be removed and, if necessary, replaced.
The SmartSens Terminal is mounted on the TA module. It can be rotated in two ways
to adjust its position as shown in the following figure.
7-2
0909
SmartSens Terminal
Home screen
The home screen appears after the startup procedure of the SmartSens Terminal (and
connection to a TA module has been established). All other parts of the user interface
can be accessed from the home screen. The home screen, in turn, can be accessed
from all other parts of the user interface by pressing the HOME key.
At the top, there is a title bar that displays information about the state of the measuring cell and the stages of an experiment. The title bar also contains the name of the
current user of the module (or the user that last established communication) and displays the current date and time.
The measurement values are displayed in the middle part of the home screen.
The buttons at the bottom of the page serve various purposes: You can, for example
call up windows containing information on the module and the current experiment or
change the display of the measurement values. There is also a button to tare the
measured weight value.
The area between the buttons and the measurement values is used for displaying
messages.
0909
7-3
SmartSens Terminal
7.1.2
An experiment running on the module proceeds through a series of stages which correspond to different states of the measuring cell. The states of the measuring cell are
indicated in the title bar by the state indicator and the text that appears next to it.
state indicator
The state indicator is a square symbol at the left end of the title bar. The background
color and the characters it displays refer to the current stage of the measurements or
the corresponding state of the measuring cell.
The text displayed in the title bar gives you more details about the current state of the
measuring cell of your TA module. The different states are listed and explained in the
following table:
The table gives an overview of the colors and the characters displayed in the state indicator. The title bar texts are also listed and explained.
7-4
Color of
state indicator
blue
OFF
green
green
green
red
red
Settling
The temperature is stabilized in the measuring cell.
red
Measurement
The measurement is in progress.
green
green
green
0909
SmartSens Terminal
A red background of the state indicator indicates that the experiment is either in
the settling or the measurement stage.
A green background indicates that the experiment has not yet reached the settling
stage or that it has passed the measurement stage.
Before the measurement stage, the letter "A" indicates that the measuring cell is
either approaching insertion conditions or ready for sample insertion ("A" stands
for "Active").
After the measurement stage, the letter "A" indicates that the measuring cell is either approaching sample removal conditions or is ready for sample removal.
The letter "M" indicates that the measuring cell is either approaching the start
temperature, settling or measuring.
The letter "S" indicates that the measuring cell is holding the standby temperature
or the final user temperature.
The word "OFF" indicates that no experiment is running on the TA module and
that furnace power has been switched off.
-
"S" and "OFF" refer to the behavior at the end of an experiment, the so called
"temperature end behavior (TEB)", which can be defined in the Module Control Window of the STARe Software.
Switching off the furnace power on the module also switches off the cooling
fan or, if installed, the liquid nitrogen cooling device.
There are two types of standby states: a state in which the measuring cell will assume the standby temperature and a state in which the furnace power is switched
off. The RESET key or the Standby ( ) button, which appears at the bottom
right of the display, can be used to change between these two types of states.
After pressing the RESET key in one of the two standby states, a message will
appear, reminding you that resetting the TA module or changing its standby state
will stop experiments that are pending in the experiment buffer of the Module
Control Window from starting automatically. If you wish to proceed, you can confirm this message by touching OK, or you can stop the operation by touching
Cancel.
In the standby state of the measuring cell, the RESET key or the Standby ( )
button, which appears at the bottom right of the display, can be used to change
between the "Standby Temperature" state and the "Furnace Power Off" state.
0909
7-5
SmartSens Terminal
7.2
The SmartSens Terminal keys arranged on both sides of the touch screen are described below. The keys are assigned to frequently used functions. You can use the
keys independently of the display on the screen, with the exception of the ROTATE
key, which changes the display (see below).
The HOME key takes you back to the home screen from any other window or
menu.
Use the SETUP key to enter the setup menu from which you can access information about the settings of the SmartSens Terminal and your module. The terminal
settings can be changed by any user but the settings of your TA module are
password protected.
The FURNACE key automatically opens and closes the furnace. On the DSC 1,
this key is only available if the Automatic Furnace Lid option is installed.
You can select the measurement value displayed in the second line of the display
with the ROTATE key.
Use the RESET key to stop an experiment that is running and reset the state of
your TA module. Pressing the RESET key once prematurely stops the current experiment and sets the TA module to the standby state.
If you press the RESET key a second time, it switches off the heating power. The
text Standby (furnace power off) appears in the title bar of the display (see also
the remark about changing the standby state at the end of Section 7.1.2).
7-6
0909
SmartSens Terminal
7.3
The most important buttons and symbols in the user interface of the SmartSens Terminal are listed below.
There are other buttons and symbols in the user interface which are not mentioned
here for clarity reasons. They are however mentioned in other sections of this chapter
to explain operating procedures.
Buttons
Name
Description
Standby
Proceed or Skip
Signals
System Info
Experiment
Terminal
Calls up the Terminal Setup menu to change the terminal settings (see
Section 7.5)
Appears on the Setup menu
Gas
Calls up a menu that allows you to make the settings for the gas flow rates with a GC 10 or a GC 20 gas controllers; only available if a gas controller is installed (see Section 7.4.3)
Appears on the Setup menu
Toggle
Diagnostics
Tests the state of the TA module. The result of this test is written into a
log file stored on the PC (see Section 7.4.4)
Appears on the Setup menu
Tare
0909
7-7
SmartSens Terminal
Buttons (continued)
Service
Home
Symbols
Name
Description
Furnace
Furnace open
Furnace closed
Sample robot l
Sample robot
active
Indicates whether the sample robot is active or not. If no symbol is displayed, the sample robot is not installed.
The symbol flashes when the sample robot is performing a task. (see
Section 7.4.4)
Sample robot
inactive
Gas is flowing
Gas controller
(only available when a
gas controller is installed)
7-8
0909
SmartSens Terminal
7.4
Notice
Operating the terminal could cause vibrations and hence disturb a measurement.
7.4.1
Automatically after starting the module, the home screen appears. Measured values
are shown on two lines in the middle part of the home screen. On the DSC 1 and the
HP DSC 1, the cell temperature and the heat flow are displayed by default. On the
TGA/DSC 1, the cell temperature and the weight are displayed.
To return to the home screen from any part of the user interface:
Press the HOME key to the left of the touch screen.
7.4.2
The cell temperature is displayed by default on the first line in the middle of the home
screen. By changing the terminal settings, you can however have a different value
displayed here (see section 7.5 SmartSens Terminal settings).
In the second line in the middle of the home screen you can display the following
measurement values one after another.
On the DSC 1 or HP DSC 1 module:
Heat flow
Flow rate of cell gas (if a gas controller is installed and gas is flowing)
Flow rate of method gas (if a gas controller is installed and gas is flowing)
Heat flow
Flow rate of cell gas (if a gas controller is installed and gas is flowing)
Flow rate of method gas (if a gas controller is installed and gas is flowing)
Sample temperature
0909
7-9
SmartSens Terminal
Apart from only two measured values in the center of the home screen, you can display a complete list of the currently measured values.
display list of
measured values
Cell temperature
Heat flow
Gas flow
Gas flow
Weight
only on TGA/DSC 1
Sample temperature
only on TGA/DSC 1
You can choose which measurement values are displayed and define the order in
which they appear in the terminal settings (see Section 7.5 SmartSens Terminal settings).
7-10
0909
SmartSens Terminal
7.4.3
You can enter a number of commands for your module directly on the SmartSens Terminal. With the help of such commands, you can, for example cause an experiment
that is running to move on to the next stage, prematurely stop a running experiment
or open the furnace.
If your TA module does not use a sample robot, the stages of an experiment at which
the sample is inserted and removed must be confirmed with the Proceed ( ) button
before the next stage can begin. If a sample robot is installed and activated, the experiment will continue automatically through these stages. You cannot use the Proceed button to confirm them in this case.
Proceed button
You can prematurely stop some stages of an experiment and start the next one with
the Skip ( ) button. This applies to all measurement phases except the measurement stage and the stages to insert and remove the sample.
Skip button
Skipping experiment stages can be done for example to shorten the time of an experiment. It can however disturb the continuation of the experiment or even affect
measurement accuracy. For example, the desired measurement results may not be
achieved if the settling stage is skipped. It is therefore entirely the user's responsibility
to decide whether to skip an experiment stage or not.
Notice
The stage of an experiment corresponds to the state of the measuring cell. A text describing the state appears in the title bar of the display. The following table provides
an overview of the experimental stages that must be confirmed with the Proceed ( )
button and those that can be stopped with the Skip button ( ). The second column
contains the states of the measuring cell corresponding to the different stages.
Stage of the experiment
Displayed text
(state of the measuring cell)
Action to continue
Settling
0909
7-11
SmartSens Terminal
RESET key
You can stop an experiment that is running with the RESET key and reset your TA
module to its initial state. Pressing the RESET key once stops the current experiment;
pressing the key a second time switches off the furnace heating.
To stop an experiment that is running:
Press the RESET key to the right of the touch screen.
The TA module approaches the standby temperature and waits in this state until you start
a new experiment or press the RESET key again.
To switch off the furnace heating: Press the RESET key again.
The furnace heating is switched off and the text Standby (furnace power off) is displayed in
the title bar.
FURNACE key
7-12
0909
SmartSens Terminal
By touching the Gas ( ) button in the setup menu, you can call up a menu that allows you to define the settings for the gas flow rates with gas controllers of the types
GC 10, GC 20, TSO800GC and TSO800GC1. With gas controllers of these types, you
must set the gas flows manually by adjusting the needle valves with the knobs on the
front panel of the gas controller. The Gas ( ) button is only available if the installed
gas controller is one of these types. With gas controllers of the types GC 100 and
GC 200 the Gas ( ) button is not available because the gas flow is controlled automatically.
You can open and close the needle valves by pressing the Toggle (
SmartSens Terminal.
) button on the
Gas button
Toggle button
Adjust the gas flow with the relevant knob on the gas controller. You can see how
the flow rate value changes on the display. See the gas controller operating instructions for further details.
To switch between the gas flows, touch the Toggle button ( ). The toggle button opens and closes the electromagnetic valves in the gas controller.
A symbol on the right side of the title bar indicates by its appearance that the gas is
flowing or the electromagnetic valve is closed:
indicates that the gas is flowing
indicates that the gas is not flowing (electromagnetic valve closed)
On the TGA/DSC 1 module, the touch screen features the Tare button, which allows
you to tare a measured weight value to weigh in the sample. Touching the Tare button sets the sample weight value to zero. For more information, refer to Chapter 6,
Weighing In, in the operating instructions of your TGA/DSC 1 module.
Tare button
The Tare button is only available in the standby state of the TGA/DSC 1 module
and in the initial stages of an experiment. It is no longer available after the insert
sample stage.
0909
7-13
SmartSens Terminal
7.4.4
You can display information about the configuration or the state of your module:
TGA/DSC 1
DSC 1
HP DSC 1
Information on configuration includes for example the identification number, the type
of the sensor installed or the version of the module software.
Information about the state of your module is above all useful to your METTLER
TOLEDO service engineer when troubleshooting possible malfunctions.
To display information about your module:
System Info button
A window appears containing information on your TA module. You can scroll through the displayed text using the arrow keys and display the following information.
Sensor type
Furnace
Cooling option
Display
Controller
Balance
You can perform a diagnostics test and generate a report about the state of your TA module.
The information is written to a log file that is stored in the subfolder "log" of the installation
folder of the STARe Software on your PC.
To obtain information about the state of your TA module:
1
7-14
0909
SmartSens Terminal
7.4.5
You can display information about the current experiment. This includes for example
the names of the user, the experiment, the method and the sample.
To display information about the current experiment:
Touch the Experiment (
Experiment button
User
User name
User ID
User identification
Method
Method name
Experiment
Experiment name
Sample
Sample name
0909
7-15
SmartSens Terminal
7.5
This section shows how to adjust the SmartSens Terminal to suit your needs by
changing the terminal settings.
You can change the terminal settings on the Terminal Setup menu.
Terminal Setup
menu
) button.
The Terminal Setup menu to change the terminal settings appears. You can scroll though the
list of parameters using the arrow keys at the bottom.
Touch the button in the list that corresponds to the desired property.
You can define the order of the measured values that appear in list of signals after
touching the Signals button.
To define the order of the measured values displayed:
1
Press each of the six buttons in the list to delete the current order.
Now touch the blank buttons in the desired order. To exclude any measured
value from the list: Leave the corresponding button blank.
7-16
0909
SmartSens Terminal
Touch the button in the SmartSens left or SmartSens right row, respectively.
Touch the button in the list that corresponds to the desired function. The following
functions are available:
None
No function is assigned
Furnace
Open/close furnace
Home
Setup
Tare
Rotate
Standard settings:
Set the brightness to a value between 0% and 100% using the arrow keys (you
can adjust it in steps of 20%). The change of brightness is immediately visible.
contrast
Set the contrast to a value between 20% and 100% using the arrow keys (you
can adjust it in steps of 2%). The change of contrast is immediately visible.
color selection
The color palettes in the left column offer a visually attractive appearance with soft
contrast, while the palettes in the right column offer a display with more contrast for
better readability under poor light conditions.
Default setting: Color palette 1 (blue with soft contrast)
0909
7-17
SmartSens Terminal
beep volume
Set the volume of the beep to a value between 0% and 100% using the arrow
keys (you can adjust it in steps of 10%). The sound is audible while pressing
the arrow keys.
A screen saver can be set to appear after a certain time. When the screen saver is
switched on, the state of the measuring cell is displayed in large letters on the screen.
This can be useful, for example in a large laboratory room for recognizing the state of
the measurement cell from afar.
To set the time after which the screen saver is switched on:
1
Using the virtual keypad, enter the time in minutes after which you want the
screen saver to be switched on. If you enter 0 minutes, the screen saver remains
switched off.
The display can be switched off automatically after a certain time. Switching off the
display can prolong the life time of the touch screen.
To set the time after which the display is switched off:
1
Using the virtual keypad, enter the time in minutes after which you want the display to be switched off. If you enter 0 minutes, the display remains switched on.
If the screen saver is switched on (see above) the display will be switched off at
the specified time after the time the screen saver was switched on.
If you feel that the SmartSens Terminal is no longer reacting correctly when you touch
a specific part of the screen, you can adjust the sensitivity of the touch screen.
To adjust the sensitivity of the touch screen:
7-18
Touch Activate.
Touch the flashing area indicated by the animated hand. Repeat this operation
when you are prompted by the hand. The procedure can be stopped at anytime
by touching C (cancel).
0909
HP DSC 1
Contents
8.1
8.2
8.3
Adjustment................................................................................................................................... 8-4
8.3.1
8.3.2
8.3.3
0911
8-i
HP DSC 1
The terms "adjustment" and "calibration" are used in these operating instructions according to the following definitions:
calibration
For the module in question, the determination of the actual deviation of measured values of reference substances from the standard literature values by means of calibration measurements.
Reference substance: a substance that is suitable for the calibration measurement and whose thermoanalytical property values are well established in the literature
adjustment
Adapting the specific module parameters so that the measured values of the calibration measurements performed afterward are within the limits of permissible error
Limits of permissible error: the specified extreme values for permitted deviations (positive and negative)
from a set value.
8.1
It is good laboratory practice to check the measurement accuracy of laboratory instruments at least once a month. You can check the measurement accuracy of your
HP DSC 1 module by performing calibration measurements with suitable reference
substances, typically indium and zinc. With a calibration measurement, no instrument parameters are changed.
GLP
We recommend that you use the single sample Check methods in the STARe Software
database for version 9.10 to perform calibration measurements. The names of these
methods all begin with the word "Check".
calibration methods
Using a Check method, the onset temperature of fusion and the heat of fusion are
evaluated automatically at the end of an experiment. Additionally, a conformity check
is performed.
No adjustment is necessary if the results of the check are within the tolerance limits
defined by METTLER TOLEDO.
If the results of the check are not within the defined tolerance limits, we recommend
that you repeat the Check with new samples. If the results are still not within the limits, the module must be adjusted.
The tolerance limits are stated in the document "CQ System Test before Delivery"
which is shipped with your HP DSC 1 module.
0911
CQ System Test
8-1
HP DSC 1
The following Check methods are available for indium and zinc checks:
Check DSC Zn exo^
Check DSC In endo^
Check DSC In exo^
Check DSC Zn endo^
The characters "exo^" in the method name indicate that the method is for measurements according to the ICTA sign convention. The characters "end^" indicate that the
method is for measurements according to the Anti-ICTA sign convention
You can display a list of the Check methods in the Method Window of the STARe Software as follows:
To display a list of the Check methods:
1
In the Method Window of the STARe Software, click File/Open to call up the
Open dialog box. Then click Filter to open the Method Filter dialog box.
In the Method Filter dialog box, select DSC as the TA technique and then click
OK.
8-2
To print the information: Click Print. You can also print the information to PDF file
if you have installed a PDF creation tool.
0911
HP DSC 1
8.2
In contrast to the various calibration procedures, the so-called indium check is a normal method with automatic evaluation of the result and conformity check. No instrument parameters are changed.
It is good laboratory practice (GLP) to check the accuracy of the temperature and heat
flow once every month. The indium check is based on measuring the onset temperature of fusion and the heat of fusion of indium.
GLP
Methods defined for control measurements for every type of module are included in
the STARe system database. The control measurements are calibrations and therefore
do not change the instrument parameters.
methods
Notice
Select the method depending on the convention you want to use for the DSC signal.
A If you want to check the measurement accuracy at higher temperatures, you
can also perform a zinc check in the same way.
If necessary, measure a second sample for comparison.
No adjustment is necessary if the results of the check are within the tolerance limits
defined by METTLER TOLEDO:
Indium:
Onset temperature
Heat flow 28.45
Zinc:
156.6 0.3 C
0.6 J/g
If the results of the check are not within the defined limits, the module must be adjusted.
0911
limits
adjustment
8-3
HP DSC 1
8.3
Notice
Adjustment
Adjustments that are not performed properly can result in incorrect temperature and
heat flow scales and lead to inaccurate measurement results. Adjustments should
therefore only be carried out by qualified personnel.
Adjusting your HP DSC 1 requires a certain amount of knowledge about the instrument, in particular the workings of the measuring cell. Before attempting to adjust the
TA module, make sure you are properly trained to do this. METTLER TOLEDO provides
appropriate training courses. Ask your METTLER TOLEDO sales office for more information. To learn more about the different calibrations or adjustments and how they
are performed, see Chapter Calibration and adjustment in the STARe Software User
Manu-al.
We strongly recommend that you ask a METTLER TOLEDO service engineer to adjust
your TA module if you are not sure how to do this yourself.
8.3.1
8.3.2
factory adjustment
The data of the factory adjustment of your module is included in the module dataset
stored on the CD-ROM which is supplied with your HP DSC 1 module.
For the initial installation, please follow the instructions in chapter 4, Installing your
DSC module in the STARe Software or consult the online Help to the Install Window of
the STARe Software under the topic Opening a STARe module dataset.
CQ System Test
8-4
The results of the factory adjustment are stated in the document "CQ System Test before Delivery" which is shipped with your HP DSC 1 module.
0911
HP DSC 1
8.3.3
A number of methods to perform adjustments are available in the STARe Software database. These methods all include the characters "Calib" at the beginning of their
names. The following methods are included in the STARe Software database for version 9.10 to perform adjustments:
Calib DSC Total Indium
Calib DSC Total . . . . . n-C8H18/In
Calib DSC Total . . . . . In/Zn
Calib DSC Temp Single . . Zn
Calib DSC Temp Single . . In
Calib DSC Tau Lag Single . . . . In
Calib DSC Temp Multi . . . . In/Zn
Calib DSC Heat Flow Single Zn
Calib DSC Heat Flow Single In
The following words and characters in the method name also indicate for which purpose a method is intended to be used:
"Multi" indicates a calibration on the basis of a measurement with more than one
substance in the same crucible.
"Temp" indicates that the method is for calibration and adjustment of the cell
temperature.
"Tau Lag" indicated that the method is for calibration and adjustment of the tau
lag.
"Heat Flow" indicated that the method is for calibration and adjustment of the
heat flow.
"Total" indicates a method with which several types of calibration and adjustment
can be performed on the basis of one measurement.
By performing an indium check after an adjustment, you can make sure that the
adjustment at the melting point of indium (156.6 C) has been done properly.
By performing a zinc check after an adjustment, you can make sure that the adjustment at the melting point of zinc (419.5 C) has been done properly.
0911
8-5
HP DSC 1
evaluation of a
calibration measurement
To meet your own demands on accuracy, you can create your own method and perform the adjustment manually. The following procedure explains how you evaluate a
calibration measurement. You can use the results of the evaluation to adjust your TA
module.
To perform a calibration measurement and evaluation:
1
Change the method according to your needs and save it under a new name.
Set up an experiment in the Experiment Window (see the online Help in the Experiment Window for more details on this). Then start the experiment.
Open the measured heat flow curve in the Evaluation Window and display it versus reference temperature by clicking TA/Curve vs. Reference Temp.
8-6
0911
HP DSC 1
Now perform the integration on the melting peak again, this with the result mode
Abscissa Unit:
Click Settings/Result Mode and select Abscissa Unit as the result mode.
Draw a frame around the fusion peak on the curve.
Click TA/Integration (or press CTRL+F6) to perform an integration evaluation on the selected curve section.
Compare the results of the onset temperature and enthalpy of fusion with the values stated in the document "CQ System Test before Delivery" which is shipped
with your HP DSC 1 module.
0911
8-7
HP DSC 1
Maintenance
Maintenance
Contents
9.1
9.2
9.3
9.4
Electrical safety test per DIN VDE 0702 in EU countries ................................................................. 9-7
0911
9-i
HP DSC 1
Maintenance
Maintenance
9.1
In this chapter, maintenance work is described that can be carried out by the operator
(see also section 9.3: Malfunctions).
Faulty gas lines and valves or a faulty pressure gauge may be changed only by
trained service engineers!
If the furnace is dirty, heat the furnace using air as AUX gas.
Use only original spare parts and accessories from METTLER TOLEDO. METTLER
TOLEDO denies any liability for any damage resulting from use of non-original spare
parts and accessories.
9.1.1
NOTICE
If the furnace is dirty, we recommend that you bake it out to clean it using air as AUX
gas as follows.
To clean the furnace:
1
Create a suitable method to run on your module with the following temperature
program:
First segment:
dynamic from 25 to 700 C, heating rate 50 K/min
Second segment:
isothermal, 20 minutes at 700 C
In the Experiment Window, select No Pan in the Select Sample Holder dialog
box and name the method "bake out", for example.
0911
9-1
Maintenance
HP DSC 1
9.1.2
Open rupture disc screw (5) and remove the rupture disk.
Assembly
3
1
5
4
Insert rupture disc (2) with the curvature facing the screw.
Check
Before you start measurements, check the new rupture disc:
1
Build up a pressure of 10 MPa with an inert gas and check for leaks (see chapter
6, section Leak test). 1 MPa 145 PSI.
9.1.3
Pressure cylinder
As soon as you notice a pressure drop in the measuring cell, check the gas inlets and
outlets.
It is not always necessary to replace the O-rings. It is often sufficient to clean the Oring and the groove.
9-2
Change the O-rings of the cylinder cover and base (see chapter 12, Accessories).
Grease new O-rings with a little silicone grease, before inserting them.
METTLER TOLEDO STARe System
0911
HP DSC 1
Maintenance
Cooling cover
If water flows out of the cooling cover, loosen the screws of the cooling cover using a hex key and change the inner and outer O-rings (see chapter 12, Accessories).
9.1.4
Decomposition products of samples can condense in the gas line OUT and block it.
To clean the gas line:
1
Attach tubing to the gas outlet OUT (lay end in a collection vessel).
Remove the fixing screw of the pressure cylinder and lift up the pressure cylinder.
Inject solvent into the opening of the gas line (10) using a syringe (see figure below).
Build up pressure with inert gas via the AUX inlet so that the solvent is forced out
of the gas line OUT. Depending on the solvent, flush the line and dry with gas.
0911
9-3
Maintenance
HP DSC 1
You can clean the gas line IN in a similar manner: close the tubing connection at
the gas inlet GAS IN, open the INLET valve, and close the OUTLET valve and continue with step (3).
5
12
11
10
8
9
9.1.5
Bulkhead union
The gas inlets and outlets IN, AUX and OUT have a two-ferrule tube fitting (Gyrolok).
Be careful not to lose the ferrules.
You can order these as spare parts and replace them (see chapter 12, Accessories)
3
4
First lay the rear ferrule (3) in the unscrewed nut (2), then the front ferrule (4).
(1) is the tube, (5) the valve and (6) the shoulder of the front ferrule.
9-4
0911
HP DSC 1
9.1.6
Maintenance
You may need to clean the sensor if the blank curve is not to your satisfaction. This
could be caused by several events.
9.1.7
A DSC sensor that has not been properly installed and positioned can lead to incorrect measuring results. The replacement of the DSC sensor must therefore be carried
out by a METTLER TOLEDO service engineer.
Only use original spare parts and accessories from METTLER TOLEDO. METTLER
TOLEDO denies any liability for any damage resulting from use of non-original spare
parts and accessories.
If the sensor in your measuring cell is defective it can be replaced by a new sensor. It
is also possible to replace the FRS5 sensor by an HSS7 sensor, or vice versa. The replacement of the DSC sensor must be carried out by a METTLER TOLEDO service engineer.
9.1.8
A DSC sensor that has not been properly positioned can lead to incorrect measuring
results. The centering of the DSC sensor must therefore be carried out by a
METTLER TOLEDO service engineer.
The DSC sensor can be accurately centered with a special centering tool. The sensor
must be centered by a METTLER TOLEDO service engineer.
0911
9-5
Maintenance
HP DSC 1
9.2
Malfunctions
No pressure buildup
Malfunctions
Causes
Inlet valve closed
Measures
Open valve
Tighten nuts
Line blocked
Lines leaking
Valves faulty
Unknown leaks
No pressure drop
Check valve
No or insufficient cooling
O-rings defective
9-6
0911
HP DSC 1
9.3
Maintenance
Disposal
9.4
In EU countries, the HP DSC 1 must be periodically tested for electrical safety in accordance with DIN VDE 0702. The test should be executed by an authorized electrician according to the test report form inserted at the end of this chapter. The form is to
be filled in and stored at the location of the instrument.
METTLER TOLEDO Service gladly offers the service of performing the electrical safety
test. Please ask your METTLER TOLEDO service agent.
0911
9-7
Tested by:
Class of product: Class I
Check by inspection:
No damage on product
Fuse rating
Product has no defects
Components:
Object/Part No.
Manufacturer
Type/Model
Ratings
Evidence
of acceptance
Power cord
Feller (Austria)
--
H05VV-F3G 1.00mm2
HAR
Fuse
Schurter
FST
T2,0L250V
VDE-S+-UR-SEMKOCBcert
Functionality:
Function of product
Testing / Measuring:
Used test equipment:
Impedance of protective
bonding (RSL)
Insulation (RISO)
()
(M)
(mA)
Test point
Enclosure back side
Test sample class I provided with power cord set (Cable and plug)
Accessible parts / enclosure
Test equipment acc EN61557
Black outlet
Test sample:
Main switch ON!
Limits: RSL > 0,3
RISO < 1M
The product is conform with the state of the art and technology.
The product is not conform with the state of the art and technology.
Signatures:
Tested by:
Customer:
___________________________________________
Place
Date
Signature
Place
_______________________________________________
Date
Signature
HP DSC 1
10
10.1
Error messages
error message
In some cases the user can take action and solve the problem. The error code should
however always be reported to METTLER TOLEDO service support.
Every error message is assigned a one to four digit number code. There are main error messages and subordinate error messages. Each subordinate error message is
related to a particular main error message but describes the problem in more detail.
Example: Errors 2301 and 2302 are errors subordinate to error 23.
The following lists contain all the error messages and warnings relevant for the operation of the HP DSC 1.
0911
10-1
HP DSC 1
Check the following list to find out possible causes for the warning and to decide
on possible measures to overcome the problem.
If you cannot overcome the problem or if the warning re-appears, call your local
service engineer.
Cause
Measures
20
21
See ERROR 4
Maximum temperature at 700 C
22
See ERROR 4
Maximum temperature at 700 C
10-2
0911
HP DSC 1
Cause
Measures
23
24
25
See ERROR 23
26
See ERROR 4
27
See ERROR 4
28
29
Hardware error
See ERROR 4
30
31 to 41
Hardware error
See ERROR 4
42
See ERROR 24
43
Hardware error
See ERROR 4
0911
10-3
HP DSC 1
Cause
Measures
128 to999
(except 850,
see below)
850
10.2
List of warnings
Warnings inform you about a deviation from the expected behavior. In some cases
you can just confirm the warning, and in other situations you must take action.
Each warning is assigned a one to two digit number code.
A warning does not interrupt a measurement (exceptions: warnings 10, 12 and 13).
10-4
Check the following list to find out possible causes for the warning and to decide
on possible measures to overcome the problem.
If you cannot overcome the problem or if the warning re-appears, call your local
service engineer.
0911
HP DSC 1
Warning
Cause
Measures
13
14
20 to 54
Click OK.
0911
10-5
HP DSC 1
Cause
Measures
55
56 ff.
Click OK.
58 to 61,
90
10-6
version mismatch
0911
HP DSC 1
11
Specificatons
Specifications
TEMPERATURE DATA
All data applies to ambient
environmental pressure
Temperature range
400 W
Water cooling
22 C to 700 C
Temperature accuracy1
0.2 K
Temperature precision1
0.02 K
Temperature reproducibility
0.1 K
Heating time2
RT to 700 C
0.1 MPa:
5 min
10 MPa:
5 min
0.1 MPa:
10 MPa:
11 min
9 min
CALORIMETRIC DATA
FRS5
HSS7
Sensor type
ceramic
ceramic
56
120
1.7 s
3.9 s
350 mW
160 mW
Resolution
0.04 W
0.01 W
Digital resolution
Measurement range
at 100 C
SAMPLING
Sampling rate
1
maximum 50 points/second
0911
11-1
Specificatons
HP DSC 1
Dimensions
Length / width / height 63 cm x 46 cm x 44 cm
Weight approximately 40 kg
Pressure cell
Pressure range
0 to 10 MPa
ca. 20 L/h
Temperature: 20 to 30 C
Materials of pressure cell
Cylinder jacket:
Guide rods:
Valves (fittings):
Needle valve:
Pressure gauge:
Pressure lines:
Gas connection
1/8 inch
O-rings
Gas connections
1/8 inch
Tube diameter
Outer diameter:
1/8 inch
Stainless steel
Tube adapter
Outer diameter:
15 mm
No corrosive gases
No explosive gas mixtures
AUX gas
No corrosive gases
No gases that can produce an explosive mixture with the pressure build up gas
Crucible types
11-2
0911
HP DSC 1
Specificatons
Measuring cell
Environmental conditions
Suitable locations Only indoors
At altitudes below 3000 m above sea level
Ambient temperature 10 to 31 C
Relative humidity less than 80% for temperatures up to 31 C and non-condensing
Pollution degree 2
Overvoltage category II
Electric power supply
Approvals
Electrical safety: IEC/EN61010-1:2001
IEC/EN61010-2-010:2003
CAN/CSA C22.2 No. 61010-1-04
UL Std No. 61010A-1
Electromagnetic compatibility: EN61326-1:2006 (Class B)
EN61326-1:2006 (industrial environments)
FCC, Part 15, class A
AS/NZS CISPR 22, AS/NZS 61000.4.3
Conformity mark: CE, CB, CSA
Pressure test Approved by Swiss Technical Services AG (Swiss TS)
Wallisellen, Switzerland
A test report is available from Swiss TS
0911
11-3
HP DSC 1
12
Accessories
Accessories
Only use original spare parts and accessories from METTLER TOLEDO. METTLER
TOLEDO denies any liability for any damage resulting from use of non-original spare
parts and accessories
ME order number
Standard accessories
Operating Instructions HP DSC 1, English
51710771
IQ/OQ Logbook
Crucible set
51141439
51142765
Calibration kit
51142760
Tool kit
51142770
119442
119441
27331
87978
Wrench, 14 mm
72059
119360
51191860
51191861
51143110
Glass cover
51142300
51142637
51142638
51140860
51191160
51141544
0911
12-1
Accessories
HP DSC 1
Optional accessories
ME order number
51119682
51119955
51119954
51141348
51141302
51141628
11612
26741
Tweezers **
51191865
29772
119410
709301
119428
51141999
51140879
51141581
51190800
O-ring (69.49x2.01)
51191931
71738
71543
51191263
26735
Nut M14
26753
51191276
51143150
51191743
51191750
51191744
51191751
12-2
0911
HP DSC 1
Accessories
00026947
71752
71745
71746
Silicone grease
71300
51710263
Optics accessories
ME order number
51143089
51143090
51191624
51192064
0911
12-3
Accessories
HP DSC 1
Lid
Volume L
ME order no.
with
20 L
without
100
51119810
with
40 L
with
100
27331
with
40 L
without
100
26763
without
40 L
without
400
51119870
400
51119871
400
51140832
400
51119873
without
100 L
without
400
51119872
with
160 L
with
40
27811
Copper crucible
without
40 L
with
100
51140407
Gold crucible
with
40 L
with
27220
with
30 L
without
51119842
with
70 L
without
51119654
with
150 L
without
24126
with 2)
120 L
with
25
26929
with 2)
120 L
without
25
29990
with
40 L
with
25
26732
with
40 L
without
25
26731
with
30 L
without
51140404
with
30 L
without
51140405
60
51140403
with
270 Ll
with
650072
with
500 L
with
650066
12-4
1)
2)
3)
To seal the disposable high pressure crucibles, you need a Toggle Press with a
closing force of approx. 10 kN. In addition there is the: Tool Kit for the Toggle
Press (female die to fit the crucible, male die to fit the lid)
order no. : 26733
0911
HP DSC 1
Index
13 Index
A
Accessories, 12-1
calibration, 8-1
accuracy, 8-6
Accuracy, 8-3
calibration methods
centering, 6-5
altitude, 4-2
cooling, 2-8
cooling flange, 10-3
Corrosive gases, 1-9
crucible types, 12-4
CQ System Test, 8-1
D
differential scanning calorimetry, 1-1
dimensions, 4-2, 11-2
DSC sensor, 6-1, 9-5
0911
Index
HP DSC 1
EMC, 4-1
HP DSC 1
I
ICTA sign convention, 8-2
indium check, 5-1, 6-1, 6-5, 8-1, 8-3, 8-5
infrared sensor, 7-4
L
leveling screws, 2-3
line socket, 2-6
location, 4-1
0911
HP DSC 1
Index
P (continued)
Maintenance, 9-1
manufacturer, 1-1
module, 4-9
resolution, 2-8
resolution, 11-1
P
plastic cover (SmartSens Terminal, 7-4peripheral
units, 2-10
power saving mode, 2-10
Power supply
0911
Index
HP DSC 1
T (continued)
time constant, 2-2
V
Voltage, 2-6, 4-5, 10-2
startup, 5-1
switched line socket, 2-10
STARe Software, 1-2, 4-7, 4-8
warnings, 10-4
weight, 4-2
Z
zinc check, 8-1, 8-5
T
Tare button, 7-9, 7-15
Tau Lag adjustment, 4-12
temperature accuracy, 11-1
temperature end behavior, 7-7
temperature precision, 11-1
Terminal button, 7-9
terminal settings, 7-18
thermocouples, 2-8
4
0911
*51710771*
Mettler-Toledo AG 2009
ME-51710771A
Printed in Switzerland
Mettler-Toledo AG, Analytical, Sonnenbergstrasse 74, CH-8603 Schwerzenbach, Switzerland, Tel. (044) 806 77 11, Telefax (01) 806 73 50, Internet: http://www.mt.com
0911/2.12