Mettler Toledo HP DSC 2+ Operating Instructions Manual
Thermal Analysis Excellence
HP DSC 2+
Operating Instructions
Table of Contents
1 Introduction 3
1.1 About this document .................................................................................................... 3
1.2 Software versions required for your instrument................................................................. 3
1.3 Hardware options ........................................................................................................ 4
1.4 METTLER TOLEDO support and service ........................................................................... 4
2 Safety Information 5
2.1 Definition of signal words and warning symbols.............................................................. 5
2.2 General and instrument-specific safety information .......................................................... 5
2.2.1 General safety information.............................................................................. 5
2.2.1.1 Intended use........................................................................................... 5
2.2.1.2 Operating instructions.............................................................................. 6
2.2.1.3 Qualification of personnel......................................................................... 6
2.2.1.4 Protective clothing................................................................................... 6
2.2.1.5 General laboratory safety.......................................................................... 6
2.2.2 Instrument-specific information ....................................................................... 6
2.2.2.1 Safety notes related to operation at high pressure........................................ 6
2.2.2.2 Measures for your protection..................................................................... 7
2.2.2.3 Measures for operational safety................................................................. 9
2.2.2.4 Safety notes related to operation with explosive or flammable gases ............. 10
2.2.2.5 Precautions to minimize risks when using explosive or flammable gases ...... 10
2.2.2.6 Special safety notes on using hydrogen ..................................................... 11
2.2.2.7 Explosive limits....................................................................................... 11
2.2.2.8 FCC rules and the radio interference regulations .......................................... 11
2.2.3 Information on the cryostat............................................................................. 11
2.3 Warning symbol on the instrument ................................................................................ 12
3 Design and Function 13
3.1 Overview of the HP DSC module.................................................................................... 13
3.2 Connections on the rear panel....................................................................................... 14
3.3 The measuring cell....................................................................................................... 15
3.3.1 Cross section of the measuring cell ................................................................. 15
3.3.2 DSC sensors................................................................................................. 16
3.4 The cryostat ................................................................................................................ 16
3.5 SmartSens terminal...................................................................................................... 17
3.5.1 Overview of the SmartSens terminal................................................................. 17
3.5.2 The touch screen........................................................................................... 18
3.5.3 State indicator and experiment stages.............................................................. 20
3.6 Stages of an experiment ............................................................................................... 22
4 Installation and Putting into Operation 25
5 Operation 27
5.1 Workflow for experiments.............................................................................................. 27
5.2 Preparing the HP DSC module for experiments ................................................................ 27
5.2.1 Hints before you start an experiment................................................................ 27
5.2.2 Crucibles – without lid or with perforated lid ..................................................... 28
5.2.3 Performing a leak test.................................................................................... 28
5.3 Performing an experiment............................................................................................. 28
5.3.1 Loading the sample crucible into the measuring cell ......................................... 28
5.3.2 Starting the experiment .................................................................................. 30
5.3.3 Removing the sample and switching off the instrument...................................... 31
5.4 Terminating an experiment............................................................................................ 32
5.5 Using the SmartSens terminal........................................................................................ 33
5.5.1 Using the keys and the SmartSens sensor ........................................................ 33
Table of Contents 1Thermal Analysis Excellence
5.5.2 Entering commands on the DSC module.......................................................... 34
5.5.2.1 Confirming an experiment stage................................................................ 34
5.5.2.2 Skipping an experiment stage................................................................... 34
5.5.2.3 Terminating an experiment ....................................................................... 34
5.5.2.4 Switching between standby and power save states...................................... 35
5.5.2.5 Starting experiments with One Click™ buttons ............................................ 35
6 Maintenance 37
7 Troubleshooting 39
7.1 Malfunctions ............................................................................................................... 39
7.2 Error messages ........................................................................................................... 39
7.3 List of error messages .................................................................................................. 40
8 Technical Data 43
9 Accessories and Spare Parts 45
Index 47
Table of Contents2 Thermal Analysis Excellence
Introduction 3Thermal Analysis Excellence
1 Introduction
Thank you for purchasing this innovative METTLER TOLEDO instrument.
The HP DSC2+ is a measuring instrument for differential scanning calorimetry under pressure. It is part of
the METTLER TOLEDO system.
1.1 About this document
Operating Instructions and Reference Manual
These operating instructions contain the most important operational information for your instrument.
Additional information can be found in the reference manual, which can be downloaded here:
http://swupdateamc.mt.com/
To obtain these operating instructions in other languages, please contact your METLLER TOLEDO represen-
tative.
Product versions
This document refers to the HPDSC2+. This product name is only used where necessary. Where appropriate, the term "HP DSC module" is used for convenience.
Conventions and symbols used in this document
Buttons on the display are indicated by bold text, for example One Click.
Keys on the instrument are indicated by bold text in square brackets, for example [Reset].
The following symbols are used for procedures requiring user interaction:
prerequisites
1, 2, 3 ... steps
results
1.2 Software versions required for your instrument
Software
The HPDSC2+ can only be operated in conjunction with the Software from METTLER TOLEDO which
is installed on a PC. There is no stand-alone mode.
You require version 14.00 or later of the Software to operate the HPDSC2+.
References to the Software are included in certain parts of this document.
Firmware
These operating instructions refer to instruments running version 1.00 of the firmware.
The firmware version of your instrument is displayed in the System info dialog on the SmartSens terminal.
Introduction4 Thermal Analysis Excellence
1.3 Hardware options
The instrument has a modular design. Each instrument 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 hardware options are available:
• PC 10: Used to automatically regulate and display the pressure and the gas flow in the measuring cell.
• Switched Line Socket: Allows the cryostat to be switched on and off under program control.
• Power Switch: Increases the available power for the cryostat.
• Peripheral Options Board: Required for synchronizing and triggering external devices.
• Hardware options for hyphenated techniques
– Microscopy Kit for HPDSC: Useful for visually identifying thermal events.
– Chemiluminescence Kit for HPDSC: Useful for identifying thermal events in the form of light
emission.
Note
For information about the hardware options above, see the Reference Manual, which can be downloaded
here: http://swupdateamc.mt.com/
1.4 METTLER TOLEDO support and service
METTLER TOLEDO offers you valuable support and services that help you optimally use your instruments:
http://www.mt.com/ta-services
Training
• Live Webinars
http://www.mt.com/ta-webinars
• On Demand Webinars
http://www.mt.com/ta-ondemand
• E-learning
http://www.mt.com/ta-etraining
• In-class Training
http://www.mt.com/ta-training
• Technical Videos
http://www.mt.com/ta-videos
Applications
• UserComs
http://www.mt.com/ta-usercoms
• App
http://www.mt.com/ta-app
• Applications Handbooks
http://www.mt.com/ta-handbooks
• Applications Database
http://www.mt.com/ta-applications
Service News
• Service and Support
http://www.mt.com/ta-service
• Good Thermal Analysis Practice™
http://www.mt.com/gtap
• Promotions
http://www.mt.com/ta-promotions
• TA News
http://www.mt.com/ta-news
Safety Information 5Thermal Analysis Excellence
2 Safety Information
2.1 Definition of signal words and warning symbols
Safety notes are indicated by signal words and warning symbols and contain warnings and information
about safety issues. Ignoring safety notes can lead to personal injury, damage to the instrument,
malfunctions and erroneous results.
Signal Words
WARNING
for a hazardous situation with medium risk, possibly resulting in severe
injuries or death if not avoided.
CAUTION
for a hazardous situation with low risk, resulting in damage to the device
or the property or in loss of data or minor or medium injuries if not
avoided.
Attention
(no symbol)
for important information about the product.
Note
(no symbol)
for useful information about the product.
Safety notes are marked with warning triangles. The following symbols depict safety issues and warnings.
Ignoring the safety notes may lead to personal injury, damage to the instrument, malfunctions and false
results.
In general, please follow the lab safety guidelines as prescribed by your facility in order to avoid injury to
yourself or others.
General hazard Risk of electrical shock Heavy load Risk of explosion
Risk of burns Risk of fire Risk of uncontrolled
pressure release
Risk of poisoning
2.2 General and instrument-specific safety information
2.2.1 General safety information
The instrument is state of the art and complies with all recognized safety rules, however certain hazards
could arise. The instrument should only be operated in sound condition according to the operating
instructions. Do not open the instrument. It does not contain any parts which can be maintained, repaired or
replaced by the user. If you ever have problems with your instrument, contact your authorized METTLER
TOLEDO dealer or service representative.
2.2.1.1 Intended use
The HP DSC is intended for performing differential scanning calorimetry under pressure. All other uses are
deemed to be not intended without the written authorization of Mettler-Toledo AG, as is operation above and
beyond the limits of use stipulated by Mettler-Toledo AG.
For the limits of operation, see Technical Data.
Safety Information6 Thermal Analysis Excellence
2.2.1.2 Operating instructions
The operating instructions must be read and understood. If the instrument is not used according to these
operating instructions, protection of the instrument may be impaired and METTLER TOLEDO assumes no
liability.
2.2.1.3 Qualification of personnel
The instrument should only be operated by qualified personnel. METTLER TOLEDO recommends appropriate
training and offers the respective seminars. The instrument must not be modified by reconstructive
measures compared to the factory original.
2.2.1.4 Protective clothing
It is advisable to wear protective clothing in the laboratory when working with the instrument.
A lab coat and suitable eye protection, such as safety spectacles, goggles or a face
shield should be worn.
Use appropriate gloves when handling chemicals or hazardous substances,
checking their integrity before use.
2.2.1.5 General laboratory safety
In general, the lab safety guidelines as prescribed by your facility must be followed in order to avoid injury
to yourself or others.
When using chemicals and solvents, the instructions of the manufacturer and the general lab safety rules
must be followed.
The responsible body has the responsibility for carrying out appropriate decontamination if hazardous
liquids are spilled on or inside the equipment.
2.2.2 Instrument-specific information
2.2.2.1 Safety notes related to operation at high pressure
CAUTION
Risk of uncontrolled pressure release.
You could be seriously injured by expelled parts.
− Never open the pressure cylinder when the system is under pressure.
Safety Information 7Thermal Analysis Excellence
CAUTION
Risk of personnel injury or damage to the instrument due to operation at high
pressure.
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.
2 Make sure that the maximum working pressure of 10 MPa is not exceeded. The built-
in rupture disk responds at a pressure of 12.4 to 13.8 MPa.
3 When releasing flammable gases, make sure that the gas is vented according to the
laboratory safety regulations. Connect gas outlet and rupture disc to lines that lead off
the gas for proper disposal. Especially take measures to prevent the gas from flowing
into the instrument’s housing.
4 Never use corrosive gases for the pressure buildup or purging.
With time, corrosive gases attack and weaken the materials of the parts under
pressure. Material weakness can lead to an explosion or to leaks in the pressurized
measuring cell.
2.2.2.2 Measures for your protection
WARNING
Risk of electrical shock.
An electrical shock can be lethal.
1 Only use the original power supply cable provided with your instrument and plug it
into a grounded outlet.
2 Never open the instrument housing.
3 The power plug must be easily accessible.
WARNING
Risk of explosion if the instrument is used in an explosive atmosphere.
The housing of the instrument is not gas tight. An explosion caused by a spark can be
lethal.
− Never work in an environment subject to explosion hazards.
CAUTION
Risk of surfaces on the instrument heating up unduly after switching off the
cooling device prematurely.
You can burn yourself on hot surfaces on the measuring cell and in its surroundings.
Hot surfaces on the instrument can cause a fire.
− Never switch off the instrument or the cooling device when the temperature in the
furnace is above 100 °C.
CAUTION
Risk of damage from flammable samples.
Using flammable samples can cause damage to the instrument and in its vicinity.
− Take suitable measures to minimize any risk. See chapter "Operation" for more infor-
mation.
Safety Information8 Thermal Analysis Excellence
CAUTION
Risk of explosion or fire due to explosive or flammable gas mixtures.
Explosion or fire from gas mixtures produced in the sample chamber can seriously injure
you.
1 Never use gases which may result in an explosive or a flammable gas mixture.
2 Never use explosive or flammable gases or gas mixtures to purge the measuring cell.
CAUTION
Risk of toxic or corrosive gases from samples that react or decompose.
You can be poisoned if you inhale toxic gases. Corrosive gases can damage the
measuring cell.
1 Place the instrument in a fume hood if you measure substances which form toxic
gases.
2 Purge the furnace and sample chamber with an inert gas after experiments in which
toxic or corrosive gases may have been produced. Do not use toxic or corrosive or
gas mixtures to purge the measuring cell.
CAUTION
Risk of injury due to heavy load.
You can injure yourself by carrying the instrument alone.
− Never try to carry the instrument alone. At least two people are needed to carry the
instrument.
CAUTION
Risk of hot surfaces.
You can burn yourself by touching parts of the measuring cell, furnace or the crucibles.
1 Always ensure cooling water flow (20 to 30 °C). The pressure cylinder and cover
would otherwise become so hot that you could burn yourself.
2 Allow the measuring cell to cool down to room temperature before performing any task
on the furnace.
3 Never place your fingers on or inside the furnace after an experiment.
4 Use tweezers to remove the furnace lid and crucibles.
Safety Information 9Thermal Analysis Excellence
2.2.2.3 Measures for operational safety
CAUTION
Risk of false operation.
False operation can cause damage to or failure of the instrument.
1 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.
2 Never remove the pressure cylinder for measurements at ambient pressure.
3 Always set the pressure buildup using with the INLET valve.
4 Make sure that the CONTROL IN needle valve (for fine regulation) is not closed tightly
otherwise the needle valve could be damaged.
5 When using chemicals and solvents, comply with the instructions of the manufacturer
and the general lab safety rules.
6 The cooling device should also be on when the instrument is switched on.
7 The cooling fluid should not be colder than 15 ºC, otherwise condensation could
develop.
8 Use the instrument only indoors in a well-ventilated area, at altitudes of less than
3000m above sea level.
9 Avoid the following environmental influences:
- Powerful vibrations
- Direct sunlight
- Atmospheric humidity greater than 80% (non-condensing)
- Corrosive gas atmosphere
- Temperatures below 10 °C and above 31 °C
- Powerful electric or magnetic fields
10 Have the instrument serviced only by METTLER TOLEDO Service.
Note
The above list is not exhaustive; other items and precautions may have to be considered.
Safety Information10 Thermal Analysis Excellence
2.2.2.4 Safety notes related to operation with explosive or flammable gases
CAUTION
Risk of explosion or fire if explosive or flammable gases are used.
You can be injured and the instrument can suffer damaged.
− If an application requires the use of explosive or flammable gases, you must be aware
of the risks and take appropriate safety precautions.
The HP DSC module is not designed for the use of explosive and flammable gases and the system is not
explosion-proof. METTLERTOLEDO excludes liability for all personal injury or damage resulting from using
explosive or flammable gases on the instrument.
See [Precautions to minimize risks when using explosive or flammable gases}10].
2.2.2.5 Precautions to minimize risks when using explosive or flammable gases
− Work in a room especially designed for working with explosive gases (alarm system, wall thickness
and so on).
− Put the instrument 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.
− To release 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 the measuring cell as well.
− Take measures to vent explosive and hot gas in case the rupture disk bursts. The instrument is fitted
with a rupture disk as a protection against overpressure. This disk may burst during the measurement
and release the explosive and hot gas.
− Before loading the cell with the flammable gas, fully replace the air by an inert gas so that explosive gas
or 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.
Note
The above list is not exhaustive; other items and precautions may have to be considered.
Avoiding explosive mixtures
Loading and unloading the samples requires opening the pressure cylinder so that the surrounding ambient
gas, usually air, mixes with the furnace atmosphere: An explosive mixture can be created which will be
ignited by hot surfaces or sparks.
− Put the measuring cell in a glove box with an inert atmosphere 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).
Risk of damaging the instrument
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 instrument by forming
alloys or in other ways.
Safety Information 11Thermal Analysis Excellence
2.2.2.6 Special safety notes on using hydrogen
If hydrogen has to be used to create a reducing atmosphere or to minimize the oxygen concentration, a
non-explosive mixture of ≤4% hydrogen 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.)
The thermal conductivity of hydrogen is much higher than that of nitrogen. Hence, the surroundings of the
furnace may get much hotter than usual and the furnace may not reach the highest end temperatures
2.2.2.7 Explosive limits
Explosive limits, also called flammable or flammability 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).
Gas Explosion limits
(LEL to UEL) in vol
%
Corrosive Flammable Toxic
Ammonia 15 - 28 x x x
Argon – – – –
Carbon dioxide – – – –
Ethylene 2.7 - 34 – x –
Helium – – – –
Hydrogen 4.0 - 75.6 – x –
Nitrogen – – – –
Oxygen – – – –
Note
The explosive limits values may vary slightly depending on your source of information.
2.2.2.8 FCC rules and the radio interference regulations
This equipment has been tested and found to comply with the limits for a Class A digital device, pursuant to
Part 15 of the FCC Rules. 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. Operation of 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
own expense.
2.2.3 Information on the cryostat
WARNING
Risk of electrical shock.
An electrical shock can be lethal.
1 Always use a grounded power supply cable and plug it into a grounded outlet to
provide the cooling device with a grounded connection.
2 Never open the instrument housing.
Safety Information12 Thermal Analysis Excellence
CAUTION
Risk of poisoning by toxic coolant liquids.
− When handling coolant liquids, comply with the instructions of the manufacturer of
these products and the general lab safety rules.
CAUTION
Risk of injury due to improperly secured coolant tube connections.
You could injure yourself if the coolant tubes slip off and the coolant used is toxic or
irritating to eyes and skin.
− Secure the tube connections on the cryostat with hose clamps.
2.3 Warning symbol on the instrument
The following warning symbol is applied on the instrument housing or components to warn users of
possible hazards.
This symbol warns that exposed surfaces can be hot to
the touch and can cause a skin burn.
Design and Function 13Thermal Analysis Excellence
3 Design and Function
3.1 Overview of the HP DSC module
The figure below shows the basic configuration of the instrument.
1
Pressure cylinder with measuring cell
6
Rupture disc
2
Glass cover with note paper underneath
7
Gas connections
3
Pressure gauge
8
Screw feet (3 in total)
4
SmartSens terminal with touch screen
9
Control knobs for valves
5
Tube connection for venting toxic gases
10
Lifting bracket
The HP DSC module is a high pressure differential scanning calorimeter featuring a stainless steel pressure
cylinder which contains the DSC measuring cell. The pressure cylinder allows measurements up to a
maximum working pressure of 10 MPa and from room temperature up to 700°C.
The gas for building up pressure and purge and reactive gases for the measurement are connected to the
gas connections on the right side of the instrument. The gas flow is controlled by the control knobs on the
front side. A pressure gauge shows the pressure and a built-in rupture disc protects the cell against
excessive pressure.
The tube connection can be installed in place of the perforated bolt on the discharge valve if the gas needs
to be expelled in a controlled manner.
The pressure cylinder is opened and closed manually by removing or installing the pressure cylinder cover.
Design and Function14 Thermal Analysis Excellence
3.2 Connections on the rear panel
1
Main power switch
2
Fuse for electronics supply
3
unused
4
Connection for triggering and synchronization external devices
5
Rating plate
6
Power supply inlet socket
7
Line output socket
8
Fuse for line output socket
9
Connection for Power Switch option
10
Ethernet connection
11
Coolant outlet
12
Coolant inlet
Notes
• The line output socket is connected to the main power switch. If you switch off the instrument, you also
switch off any external device connected to the socket, for example the cooling device.
• The instrument is connected via the Ethernet connection to the Software PC.
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