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STARe System

Operating Instructions

Thermal Analysis Excellence


HP DSC 1

Introduction and Safety Notes

Design and Function

Cooling Options

Installation

Switching On and Off

Measurement

SmartSens Terminal

Calibration and Adjustment

Maintenance

10

Errors, Warnings and Malfunctions

11

Technical Specifications

12

Accessories

13

Index

HP DSC 1

Introduction and Safety Notes

Introduction and Safety Notes

Contents
1.1

The HP DSC 1 Module in the STARe system ................................................................................... 1-3

1.2

Options ........................................................................................................................................ 1-4

1.3

The STARe Software...................................................................................................................... 1-4

1.4

Typographical conventions............................................................................................................ 1-5

1.5

Safety Notes................................................................................................................................. 1-6

1.5.1

Measures for your protection........................................................................................................... 1-6

1.5.2

Measures for operational safety..................................................................................................... 1-11

1.6

FCC rules and the radio interference regulations ......................................................................... 1-12

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1-i

HP DSC 1

Introduction and Safety Notes

Introduction and Safety Notes

1.1

The HP DSC 1 Module in the STARe system

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

Introduction and Safety Notes

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:

FRS5 or HSS7 Sensor

Switched Line Socket

Pressure Controller 10 (PC10)

Power switch

Peripheral Option board

HP DSC Microscopy

HP DSC Chemiluminescence

1.3

The STARe Software

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.

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HP DSC 1

1.4

Introduction and Safety Notes

Typographical conventions

The following typographic conventions are used in these operating instructions:

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

The NOTICE sign indicates important information concerning data recording.

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.

Arial Narrow bold

CAPITAL LETTERS indicate keys to be pressed on the PC or on 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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marks a note containing additional information in a particular

METTLER TOLEDO STARe System

1-5

Introduction and Safety Notes

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

Measures for your protection

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.

Never work in an environment subject to explosion hazards! The housing of the


instrument is not gas tight (explosion hazard due to spark formation, corrosion
caused by the entry of gases).

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.

METTLER TOLEDO STARe System

0911

HP DSC 1

Introduction and Safety Notes

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!

Always ensure cooling water flow (20 to 30 C)!


The pressure cylinder and cover would otherwise become so hot that you could
burn yourself!

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.

Never remove the pressure cylinder for measurements at ambient pressure!

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.

Gas controllers should not be connected.

Protective discs for the ceramic sensor


For certain lubricating oils that have to be measured under oxygen (OIT), the oxidation reaction can be explosive. The ceramic sensor may then possibly break as a result of the extremely rapid increase in sample temperature.
If a protective disk (see chapter 12, Accessories) is inserted between the sensor and
the crucible on both the sample and on the reference sides, the heat that is suddenly
liberated reaches the sensor somewhat slower. As a result, there is a smaller temperature gradient and less mechanical stress in the ceramic sensor.

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1-7

Introduction and Safety Notes

HP DSC 1

Safety notes related to operation at high pressure

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).

The maximum working pressure must not be higher than 10 MPa!


The built-in safety rupture disc responds at a pressure of 12.4 to 13.8 MPa.

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.

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 pressure
measuring cell.

Safety notes related specially to operation with flammable or explosive gases


METTLER TOLEDO excludes liability for all damages or losses if the operator uses the
product in connection with explosive or flammable gases. The operator itself is responsible to fulfill all local and internal safety regulations and to follow the limitations
defined in the instructions of the corresponding instrument.

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)

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HP DSC 1

Introduction and Safety Notes

Gas

Explosion limits (LEL


to UEL)in vol %

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

Introduction and Safety Notes

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.

The measurement system is fitted with a rupture disk as a protection against


overpressure. This disk may burst during the measurement and relief the explosive and hot gas: take measures for safe venting.

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 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.

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.

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HP DSC 1

1.5.2

Introduction and Safety Notes

Measures for operational safety

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.

Exclude the following environmental influences:


Vibrations
Direct sunlight
Atmospheric humidity greater than 80% as well as condensing humidity
Temperatures below 10 C and above 31 C
Powerful electric or magnetic fields

Use the instrument only


Indoors
At altitudes below 3000 m above sea level.

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.

Use only fuses of the type specified in the operating instructions!

Never purge the measuring cell with corrosive gases!.

Purge the measuring cell with an inert gas if you measure samples which form
corrosive gases during decomposition!

Have the instrument serviced only by METTLER TOLEDO service staff!

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1-11

Introduction and Safety Notes

HP DSC 1

1.6

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 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.

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HP DSC 1

Design and Function

Design and Function

Contents
2.1

Introduction................................................................................................................................ 2-1

2.2

Configuring the HP DSC 1............................................................................................................ 2-2

2.2.1

Outward appearance...................................................................................................................... 2-3

2.2.2

Power supply connections.............................................................................................................. 2-6

2.2.3

Parts supplied ............................................................................................................................... 2-7

2.2.4

Measuring cell............................................................................................................................... 2-8

2.2.5

Measurement principle ................................................................................................................... 2-9

2.3

Optional switched line socket ..................................................................................................... 2-10

2.3.1

Installation.................................................................................................................................. 2-10

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2-i

HP DSC 1

Design and Function

Design and Function

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:

The HP DSC 1 is fitted with a touch-screen terminal: the SmartSens terminal. It is


possible to display information about the measurement or the HP DSC 1 module
and to enter commands in a much more user friendly way.

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.

The housing of the HP DSC 1 features a new design.

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METTLER TOLEDO STARe System

2-1

Design and Function

HP DSC 1

2.2

Configuring the HP DSC 1

The basic configuration includes the following components:

Measuring cell with ceramic sensor (time constant = 3 s)

High pressure cylinder

Module electronics

Manual furnace lid

Operating state indicator

SmartSens terminal

400 W Power amplifier

Recirculating cooling an instrument must be available for water cooling.

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.

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HP DSC 1

2.2.1

Design and Function

Outward appearance

The basic configuration of the module is always the same (see Fig. 1).

Fig. 1. The HP DSC 1 basic module


1

Leveling screw (3 in total)

SmartSens Terminal

Gas connections

Pressure cylinder with measuring cell

Rupture disc

Lifting bracket

Tube connection

Area for notes with pressure gauge

Recess in housing

10 Control knobs for valves

The module stands on three adjustable leveling screws, 1. You can adjust the height
and level the module horizontally.

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METTLER TOLEDO STARe System

leveling screws

2-3

Design and Function

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.

Fig. 2. The HP DSC 1 module equipped with the Smartsens terminal

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HP DSC 1

Design and Function

All the external connections are located at the rear of the HP DSC 1 module.

external connections

Fig. 3. View of the rear panel of the HP DSC 1 module

Main switch

8 Valve control connection for


and GC20 (unused)

Power supply inlet socket

Line output socket

10 Instrument ID

Fuse for the line output socket

11 Serial number

Rating plate

12 Water outlet

Fuse for the electronics power


supply

13 Water inlet

Connection to synchronize
external devices

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GC10

Ethernet connection

METTLER TOLEDO STARe System

2-5

Design and Function

HP DSC 1

2.2.2
AC connections

Power supply connections

The HP DSC 1 has the following power supply 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.

You can switch a peripheral device (such as a refrigerated circulator) on and


off under method control in conjunction with the Switched Line Socket option.

Power supply line voltage


voltage

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.

To replace blown fuses:


1

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.

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HP DSC 1

Design and Function

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:

Connection GAS IN for the pressure buildup.

Connection AUX IN for the purge gas.

Connection GAS OUT for gas outlet.

2.2.3

gas inlets and outlets

Parts supplied

HP DSC 1 module with built-in DSC sensor, configured according to order

Crucible handling set

Sample preparation kit

Calibration kit

Ethernet Cat 5e cable

Ethernet crossover cable

Centering aid for the DSC sensor

AC cable (country specific)

Operating Instructions

Declaration of conformity

See also Chapter 11, Accessories.

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2-7

Design and Function

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.

Design of the measuring cell


High Sensitivity Sensor

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.

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HP DSC 1

Design and Function

Fig. 4. Cross-section of the HP DSC 1 measuring cell and high pressure


cylinder
In the DSC measuring cell, the FRS5 sensor can be replaced by an HSS7 sensor, or
vice versa. This allows the performance features of the measuring cell to be optimally
adapted to the application. The replacement of the DSC sensor must be carried out by
a METTLER TOLEDO service engineer.

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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METTLER TOLEDO STARe System

2-9

Design and Function

HP DSC 1

2.3

Optional switched line socket

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

The installation of the Switched Line Socket must be performed by a METTLER


TOLEDO service engineer.

Power consumption of external devices


The maximum power available for an external device is limited to 600 W. If necessary, more power can be provided by installing the following external power switches.
Power Switch 115 V

51 119 955

Power Switch 230 V

51 119 954

The Switched Line Socket hardware option must also be installed.

A power switch should only be installed by a qualified person who is familiar with
your local installation regulations.

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HP DSC 1

Cooling

Cooling

3.1

Cooling with refrigerated circulators

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

Location ....................................................................................................................................... 4-1

4.1.1

Electromagnetic compatibility (EMC) ............................................................................................... 4-1

4.1.2

Working area ................................................................................................................................ 4-2

4.1.3

Room conditions ........................................................................................................................... 4-2

4.2

Minimum requirements for the PC................................................................................................. 4-3

4.3

Gas supplies ................................................................................................................................ 4-3

4.4

Power supply ............................................................................................................................... 4-4

4.5

Installing the HP DSC 1 Module .................................................................................................... 4-5

4.6

Installing your HP DSC 1 module in the STARe Software ................................................................ 4-8

4.6.1

Opening the Install Window ............................................................................................................ 4-8

4.6.2

Installing the STARe module in the STARe Software............................................................................ 4-9

4.6.3

Establishing communication between the STARe Software and your HP DSC 1 module ...................... 4-10

4.6.4

Adjustment data in the Install Window ........................................................................................... 4-12

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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 compatibility (EMC)

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.

Do not use a mobile phone, radio transmission equipment or similar devices


during measurements.

0911

METTLER TOLEDO STARe System

4-1

Installation

HP DSC 1

4.1.2
working area

Working area

The HP DSC 1 is a very sensitive high resolution calorimeter. To eliminate or reduce


any possible vibrations during the measurement, it is advisable to install the
HP DSC 1 on a stable bench or table. The ideal solution is a weighing table. A robust
work table is also suitable. Table boards mounted on sturdy L-shaped supports that
are fixed to a solid wall can also be used.
The table (dimensions, material, etc.) must be adequate to provide a stable support
for the weight of the module and the PC:
Weight: approximately 40 kg.
Dimensions: L 63 cm x W 46 cm x H 44 cm
There should be at least 15 cm clearance behind the module for cables and tubing.
If the HP DSC 1 and the PC are to be placed on the same table, we recommend the
following dimensions for the table:
Dimensions: L 150 cm x W 90 cm x H 90 cm
Place the measuring module in a fume hood if you measure substances which form
toxic gases through decomposition!

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

It is designed to operate trouble-free at room temperatures between +10 C and


+31 C with relative humidity of less than 80% under non-condensing conditions.
Direct exposure of the instrument to sunlight should be avoided.

4-2

METTLER TOLEDO STARe System

0911

HP DSC 1

4.2

Installation

Minimum requirements for the PC

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

METTLER TOLEDO STARe System

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

Electronics power supply

Furnace power supply

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

METTLER TOLEDO STARe System

0911

HP DSC 1

4.5

Installation

Installing the HP DSC 1 Module

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

Choose an appropriate location.

Use the leveling screws to adjust the module horizontally.

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 power supply cable.

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.

To set up the pressure cylinder:

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).

Lift up bracket (2) and remove pressure cylinder cover (3).


Place the alumina wool insulation in the pressure cylinder cover and press
down. Make sure that the O-rings groove is free from the wool insulation.
Mount the pressure cylinder cover and tighten the four nuts by hand. This is
sufficient to seal the system.
Attach tubes at the connections for water inlet and outlet at the back of the
module (see Fig. 3 in chapter 2).
Attach the other end of the tubes to the water source, for example, to a refrigerated circulator.

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METTLER TOLEDO STARe System

4-5

Installation

HP DSC 1

To connect the gas sources (see the schematic below):

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

Purge gas inlet

Valve for pressure build up

Pressure gas inlet

Valve for pressure reduction

Safety rupture disc

Needle valve for fine


regulation of purge gas

Bulkhead union
for purge gas in

Bulkhead union
for pressure gas in

10

Bulkhead union for


pressure gas reduction

Valve for purge gas inlet

You can always remove and reattach the tubes.

4-6

METTLER TOLEDO STARe System

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

Prepare the PC for the HP DSC 1:


Make sure that the STARe software is properly installed and install the data set of
your HP DSC 1 module in the STARe software. For the initial installation, please
see the section Installing your HP DSC 1module in the STARe Software or consult
the online Help to the STARe Software Install Window.
Please note that the STARe Software can only communicate with a HP DSC 1
module by using an HP DSC 1 data set. It is not possible, for example, to communicate with an HP DSC 1 using a DSC827e module data set.

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METTLER TOLEDO STARe System

4-7

Installation

HP DSC 1

4.6

Installing your HP DSC 1 module in the STARe


Software

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

Opening the Install Window

Click Functions/Install Window in the main menu bar of the STARe Software.
An Install Window opens and the symbol

4-8

METTLER TOLEDO STARe System

appears in the Windows task bar.

0911

HP DSC 1

4.6.2

Installation

Installing the STARe module in the STARe Software

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

installation with the module


CD-ROM

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.

Enter the path in the Folder box, for example, D:\


The name of your HP DSC 1 module data set appears in the list. This data set was created
during adjustment in the factory and contains the default settings.

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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METTLER TOLEDO STARe System

4-9

Installation

HP DSC 1

4.6.3

Establishing communication between the STARe Software


and your HP DSC 1 module

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

In the Install Window, click the Connections tab.


The Connections tabbed page appears.

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".

Connect your module to the desired port as follows:

Click on the module in the list.

Then click Activate.

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

METTLER TOLEDO STARe System

0911

HP DSC 1

Installation

To disconnect a HP DSC 1 module from the port:


1
2

In the Install Window, click the Connections tab.

disconnecting from port

Double-click the entry of the corresponding module you want to disconnect.


The question Do you want to deactivate the connection to the device ? appears.

Click Yes to disconnect the module from the port.

The HP DSC 1 module is disconnected from the port.

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METTLER TOLEDO STARe System

4-11

Installation

HP DSC 1

4.6.4

Adjustment data in the Install Window

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.

Click the Adjustment Overview button.


The Adjustment Overview dialog box appears.

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

METTLER TOLEDO STARe System

0911

HP DSC 1

Switching the Instrument On and Off

Switching the Instrument On and Off

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.

Establish communication between STARe Software and the PC as described in


Chapter 4, Establishing communication between the STARe Software and your
HP DSC 1 module. It takes approximately one minute until communication between the module and the PC is established.

If no communication can be established between the module and the PC, check
the following causes:

The PC is not switched on.

The module is not switched on.

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.

The IP address is not correct.

See chapter 10, Error Messages and Warnings, under List of warnings.

5.2

Performing an indium check

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.

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METTLER TOLEDO STARe System

5-1

HP DSC 1

Measurements

Measurements

Contents
6.1

Preparing the HP DSC 1 for experiments....................................................................................... 6-1

6.2

Leak test ...................................................................................................................................... 6-2

6.3

The safety rupture disc ................................................................................................................. 6-2

6.4

Connecting the Pressure Controller PC10...................................................................................... 6-3

6.5

Preparing an experiment .............................................................................................................. 6-5

6.5.1

Connecting the gas sources............................................................................................................ 6-5

6.6

Preparing the HP DSC 1 measuring cell for experiments................................................................ 6-5

6.6.1

Crucibles without lid or with perforated lid ..................................................................................... 6-6

6.7

Performing an experiment ............................................................................................................ 6-6

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

The calorimetric sensitivity E ......................................................................................................... 6-18

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METTLER TOLEDO STARe System

6-i

HP DSC 1

Measurements

Measurements

6.1

Preparing the HP DSC 1 for experiments

To avoid inaccurate measurement results or artifacts, the following points must be


observed:

The DSC sensor must be centered properly.

The DSC cell including the furnace and furnace lid must be clean and free of any
residue.

We recommend that you perform an indium check regularly (approximately once


a month). See chapter 8, section Calibration and Adjustment: the indium check.

Refer to chapter 9, Maintenance to learn more about the corresponding maintenance


tasks.

0911

METTLER TOLEDO STARe System

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

Close the valves OUTLET, INLET and AUX.

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

Build up a pressure of 10 MPa.

Close INLET valve and observe pressure gauge.

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 safety rupture disc

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

METTLER TOLEDO STARe System

0911

HP DSC 1

6.4

Measurements

Connecting the Pressure Controller PC10

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

8 Connection for gas controller

2 Connection to INLET

9 Bridging tube

3 Connection to OUTLET

10 Fitting

4 Diagram of connections

11 Fitting

5 Pressure controller

12 Connection from gas supply

6 Connection for pressure controller

13 Quick-Vent Valve

7 Gas controller

14 Leveling screw (3 in total)

Close the Quick-Vent Valve on the PC10.

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.

Slide the gas connections from the two instruments together.


The gray cover panel at the side of the housing is set diagonal to the housing,
which makes the extensions for the gas connections appear different in length.
They are, however, the same length.

Tighten the screws.

Attach cables for gas flow and pressure from BROOKS control and display unit to
the PC10.

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METTLER TOLEDO STARe System

6-3

Measurements

HP DSC 1

Turn on all instruments: HP DSC 1, *BROOKS control and display unit.

Connect the gas to the INLET and tighten the screw. Make sure that the QuickVent Valve is open.

To perform an experiment: Follow steps 6 to 19 under Controlling the flow and


pressure with a special controller on pages 6-16 and 6-17.

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

METTLER TOLEDO STARe System

0911

HP DSC 1

Measurements

6.5

Preparing an experiment

6.5.1

Connecting the gas sources

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

Preparing the HP DSC 1 measuring cell for experiments

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.

Create a method with the following temperature program:


First segment: Dynamic from 25 C to 700 C with a heating rate of 20
K/min
Second segment: Isothermal: 20 minutes at 700 C
Select No pan as the crucible type and name the method heat.

Perform an experiment without a crucible using the method heat.

Perform an indium check (see chapter 8, section Calibration and Adjustment: the
indium check.).

Before the first measurement, run a temperature program without a sample to


precondition the HP DSC 1 cell.

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METTLER TOLEDO STARe System

6-5

Measurements

HP DSC 1

6.6.1

Crucibles without lid or with perforated lid

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

Hints before you start the measurement


Apply this procedure only if you are not working according to a specified norm. The
instructions may differ significantly.

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.

METTLER TOLEDO STARe System

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

Remove the furnace lid with tweezers.


The measuring cell is now open.

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.

Set the flow rate of the cooling water to approx. 30 l/h.

Close the OUTLET, INLET and AUX IN valves.

Open the gas inlet for the pressure buildup.

10 Open the INLET valve slowly.


11 Close the INLET valve when the pressure is reached.

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METTLER TOLEDO STARe System

6-7

Measurements

HP DSC 1

To perform an experiment on the HP DSC 1:


Start experiment

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.

Click OK in the Module Control Window.


The measurement starts. At the end of the experiment the REMOVE SAMPLE request appears 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

Unscrew the nuts.

Remove the pressure cylinder cover, the alumina wool mat and the furnace lid.

Open the furnace chamber and remove the sample.

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

The cell goes to 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.

The heating power is switched off (Furnace Power Off).

METTLER TOLEDO STARe System

0911

HP DSC 1

Measurements

Pressure not controlled


When you perform isothermal measurements, you can set the required pressure at the
desired temperature. The pressure does not change during the measurement.
In dynamic measurements, the pressure increases with the temperature in a manner
which depends on the cooling of the pressure cylinder.
Pressure-temperature curve:
(Heating rate: 10 C/min, gas: nitrogen, cooling water: T 20 C, flow rate 30 l/h)
P [MPa]

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

METTLER TOLEDO STARe System

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

With PC 10 with 2 gases connected

PRC: Pressure controller


MFC: Mass flow controller
Advantage: PC10 offers the Quick-Vent Valve.
See also Fig. 8 below

6-10

METTLER TOLEDO STARe System

0911

HP DSC 1

Measurements

Table 1: Overview of connection possibilities


The following scenarios bear limitations
Purge gas

Without pressure control

Without

AUX IN closed
AUX CONTROL closed
INLET closed
AUX IN

OUTLET closed
isothermal: pressure constant
dynamic: pressure increase

CONTROL

Fig. 1

INLET

OUTLET

With flow rate measurement in isothermal measurements *

AUX IN open
AUX CONTROL open

Flow rate (for example, 50 mL/min)

INLET closed
AUX IN

OUTLET open: flow of e.g. 50 mL/min


isothermal: pressure constant
dynamic: pressure increase*

CONTROL

Fig. 2

INLET

OUTLET

With flow rate control

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)

AUX CONTROL open

We recommend BROOKS mass flow controller

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

OUTLET open: flow rate, for example,


50 mL/min

CONTROL

INLET

isothermal: pressure constant **


dynamic: pressure increase
OUTLET

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.

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6-11

Measurements

HP DSC 1

Table 1: Overview of connection possibilities (continued)


The following scenarios bear limitations
Purge gas

With pressure control

Without

AUX IN closed
AUX CONTROL closed
INLET closed
OUTLET open

AUX IN
Pressure
controller

CONTROL

Fig. 5

INLET

dynamic: pressure constant


OUTLET

With flow rate setting in isothermal


and dynamic measurements ***

AUX IN open
AUX CONTROL: Set flow rate (for
example, 50 mL/min)

Flow rate (for example,


50 mL/min)
(Reducing valve of purge gas source
set somewhat higher than measuring
cell pressure)
Fig. 6

INLET closed

AUX IN
Pressure
controller

CONTROL
INLET

OUTLET

(Reducing valve of purge gas source


set somewhat higher than measuring
cell pressure)

OUTLET open
isothermal: pressure and flow rate
constant
dynamic: pressure and flow rate
constant

With flow rate measurement


Flow meter with operating pressure of
10 MPa, e.g. from BROOKS

isothermal: pressure 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

dynamic: pressure and flow rate


constant

With flow rate control

AUX IN open

(Reducing valve of purge gas source


set somewhat higher than measuring
cell pressure)

AUX CONTROL 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.

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0911

HP DSC 1

Measurements

Pressure controlled with a special controller


To control the pressure in dynamic measurements, you can attach a pressure controller to the outlet GAS OUT (see also Table 1, Fig. 5, 6 with flow meter).
We work with the pressure controller PC 10, which includes the BROOKS control and
display unit.
Proceed as follows for controlled pressure measurements:
1

Connect the pressure controller input to the GAS OUT outlet.

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

Remove the furnace lid with tweezers.

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.
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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).

Setting the flow with a flow meter in isothermal measurements


To set the flow rate (approx. 50 mL/min) of the purge gas and to keep the gas pressure constant in isothermal measurements, you can attach a flow meter at the outlet
GAS OUT (see Table 1, Fig. 2 and chapter 12, Accessories).
We recommend first performing a blank experiment at the desired pressure to determine the setting of the OUTLET valve. This saves time during the actual measurement.
No gas distributor is connected at outlet GAS OUT in the following procedure:
1

Attach the tubing connection (see Accessories) at outlet GAS OUT and connect to
the flow meter using plastic tubing.

Open the needle valve of the flow meter fully.

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).

Open AUX IN and AUX CONTROL valves fully.


Since the pressure from the purge gas cylinder (after the reducing valve) is exactly the same as that of the measuring cell, there is no additional pressure
buildup. If it should be somewhat lower, the check valve prevents the entry of the
pressurizing gas.

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).

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0911

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Measurements

To perform the experiment with the flow meter:


1

Open the pressure cell by unscrewing the four nuts on the pressure cylinder cover
and lifting it off.
Be careful: its heavy.

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.
3

Remove the furnace lid with tweezers.


The measuring cell is now open.

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.

Set the flow rate of the cooling water to approx. 30 l/h.

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.

Experiments at ambient pressure


For measurements at ambient pressure, you can connect a flow meter before the gas
is led to the measuring cell.
Connect the flow meter between gas source and AUX IN and open the AUX IN and
OUTLET valves fully.
By adjusting the AUX CONTROL valve, set a gas flow of 50 mL/min with the flow
meter.
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6-15

Measurements

HP DSC 1

Controlling the flow and pressure with a special controller


To control the flow rate of the purge gas and the pressure in dynamic measurements,
you can attach a flow meter and a pressure controller.
We work with the pressure controller PC, which includes the
BROOKS control and display unit.
1

Connect the pressure controller input to the GAS OUT


outlet.

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 output to the AUX IN inlet.

Connect the flow controller inlet to the purge gas line.

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

Remove the furnace lid with tweezers.


The measuring cell is now open.

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.
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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.

18 Click OK 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.

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Measurements

HP DSC 1

Removing the sample and switching off the instrument


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

Make sure the pressure is completely relieved. Unscrew the nuts.

Remove the pressure cylinder cover, the alumina wool mat and the furnace lid.

Open the furnace lid and remove the sample.

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.

The heating power is switched off (Furnace Power Off).

Purging the measuring cell


The HP DSC 1 offers the possibility of purging the measuring cell with the same gas
that you use for pressure buildup or with another gas. A reactive gas, such as oxygen
is used for the oxidation of the sample, an inert gas for purging gases that are
evolved by the sample.
Never use a purge gas that can react with the pressurizing gas (see Safety Notes)!
Never build up the pressure of the measuring cell via the inlet AUX IN! This can raise
the furnace lid.
The second gas source must also have a check valve to avoid contamination with the
pressurizing gas (see Safety Notes).
For temperatures above 400 C, the oven lid could become fixated while cooling
down. To loosen the oven lid, you can heat the cell to 600 C and lift it off while it is
still hot. Be careful not to burn yourself!

6.7.4

The calorimetric sensitivity E

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.

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SmartSens Terminal

SmartSens Terminal

Contents
7.1

Overview of the SmartSens Terminal ............................................................................................. 7-1

7.1.1

Measuring cell state indicator and stages of a measurement ............................................................. 7-4

7.2

Keys on the SmartSens Terminal................................................................................................... 7-6

7.3

Buttons and symbols on the display............................................................................................... 7-7

7.4

Operating the SmartSens Terminal................................................................................................ 7-9

7.4.1

Displaying the home screen............................................................................................................ 7-9

7.4.2

Displaying the current measured values ........................................................................................... 7-9

7.4.3

Entering commands on the SmartSens Terminal ............................................................................. 7-11

7.4.4

Displaying information about the TA module................................................................................... 7-14

7.4.5

Displaying information about the experiment .................................................................................. 7-15

7.5

SmartSens Terminal settings ...................................................................................................... 7-16

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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

Overview of the SmartSens Terminal

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

OUTLET ROTATE key

Touch screen

FURNACE key

SETUP key

10 Area for messages

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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.

The friction of the tipping movement () can be adjusted by tightening or loosening


the two screws on the back. See photo below. The vertical rotational movement ()
cannot be adjusted.

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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.

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SmartSens Terminal

7.1.2

Measuring cell state indicator and stages of a


measurement

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.

title bar text

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

Characters in Text in title bar and its meaning


state indicator

blue

OFF

Standby (furnace power off)


The furnace is switched off. There is no experiment running on the TA module.

green

Standby (standby temperature)


The furnace is switched on and the measuring cell is at
the defined standby temperature. There is no experiment running on the TA module.

green

Going to insert temperature


The measuring cell is approaching the temperature at
which the sample can be inserted.

green

Wait for insert sample


The measuring cell is ready for sample insertion.

red

Going to start temperature


The measuring cell is approaching the start temperature.

red

Settling
The temperature is stabilized in the measuring cell.

red

Measurement
The measurement is in progress.

green

Going to remove temperature


The measuring cell is approaching the temperature at
which the sample can be removed.

green

Wait for remove sample


The measuring cell is ready for sample removal.

green

Final user temperature


The measuring cell has reached or is approaching the
temperature defined in the temperature end behavior
setting.

METTLER TOLEDO STARe System

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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.

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SmartSens Terminal

7.2

Keys on the SmartSens Terminal

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.

If you have connected a gas controller to your TGA/DSC 1 or DSC 1 (not


HP DSC 1!), you can display the gas flow rates by pressing the GAS key. For
more information, refer to the Operating Instructions for your TA module: Hardware Options.

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).

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7.3

Buttons and symbols on the display

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

Toggles between the two types of standby state


Appears on the home screen

Proceed or Skip

Confirms or skips the stage of an experiment


(see Section 7.4.3)
Appears on the home screen

Signals

Displays a list of the current measurement values (see Section 7.4.2)


Appears on the home screen

System Info

Displays information about the TA module (see Section 7.4.4)


Appears on the Setup menu

Experiment

Displays information about the experiment (see Section 7.4.5)


Appears on the Setup menu

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

Opens and closes the electromagnetic valves of a gas controller to switch


between the gases so that the flow of each gas can be manually adjusted
(see Section 7.4.3)
Appears on the screen after pressing the Gas button

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

Tares the measured weight value. This button is only available on a


TGA/DSC 1. (see Section 7.4.3)
Appears on the home screen

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SmartSens Terminal

Buttons (continued)
Service

Enters the service and maintenance mode of the SmartSens Terminal.


This mode should be entered by a METTLER TOLEDO service engineer
only. It is password-protected.
Appears on the Setup menu.

Home

Changes the display to the home screen


Appears only with list of current measurement values which can be
viewed by touching the Signals button.

Symbols
Name

Description

Furnace

Indicates whether the furnace is open or closed (see Section 7.4.3).

Furnace open

Available on DSC 1 only if the hardware option "Automatic Furnace Lid"


is installed.

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)

Indicates whether the gas is flowing or not (see Section 7.4.3)

Gas is not flowing

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SmartSens Terminal

7.4

Operating the SmartSens Terminal

This section describes how to operate the SmartSens Terminal.


The SmartSens Terminal helps you to operate the TGA/DSC 1, DSC 1 or HP DSC 1.
You can display information about a measurement or perform certain operations on
the module.
Be careful when operating the SmartSens Terminal during a measurement.

Notice

Operating the terminal could cause vibrations and hence disturb a measurement.

7.4.1

Displaying the home screen

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

Displaying the current measured values

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:

Current cell temperature

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)

On the TGA/DSC 1 module:

Current cell temperature

Current weight value

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

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SmartSens Terminal

scroll through the displayed


measurement values

enlarge the display of


measurement values

To scroll through the measurement values displayed in the second line:


Press the ROTATE key several times until the desired measurement value is displayed.
You can enlarge the display of measurement values in the center of the home screen
in order to be able to read the values from a greater distance.
To enlarge the display of the measurement values:
Touch the measurement value displayed.
To scroll through the measurement values, press the ROTATE key several times
until the desired measurement value is displayed.
The measurement value appears enlarged.

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

To display a list of the currently measured values:


Touch the Signals (

) button in the home screen.

The following information is displayed:

Cell temperature

Temperature of the measuring cell

Heat flow

Measured heat flow

Gas flow

Flow rate of cell gas (if installed)

Gas flow

Flow rate of segment gas (if installed)

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).

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7.4.3

Entering commands on the SmartSens Terminal

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

Approaching insert temperature

Going to insertion conditions

Must be confirmed with


without sample robot

Insert sample with crucible

Waiting for sample insertion

Can be skipped with

Approaching start temperature Going to start temperature

Can be skipped with

Stabilizing start temperature

Settling

Can be skipped with

Approaching removal conditions

Going to remove conditions

Can be skipped with

Remove sample crucible

Waiting for sample removal

Must be confirmed with


(without sample robot)

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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

The FURNACE key is a standard feature on the TGA/DSC 1.


On the DSC 1, the FURNACE key is only available if the hardware option "Automatic
furnace lid" is installed. You can remove the automatic furnace lid from or place it on
the furnace by pressing the FURNACE key.
On the TGA/DSC 1 and HP DSC 1 you can open and close the furnace by pressing
the FURNACE key. The furnace symbol indicates that the furnace is open or closed
( , ). The symbols will blink during the opening or closing action of the furnace or
furnace lid.
The furnace or furnace lid must be closed with the FURNACE key before touching
the Proceed ( ) button on the SmartSens Terminal to continue the experiment. If you
touch the Proceed ( ) button before pressing the FURNACE key, a message will
appear requesting you to close the furnace.
Please note that the furnace or furnace lid can only be opened in the settling and the
measurement phase if you have been given furnace open permission (FOP) for your
experiment. Refer to the online Help of the STARe Software for more information.
You can find more detailed information on the automatic furnace lid on the DSC 1 in
the operating instructions of the DSC 1.

7-12

METTLER TOLEDO STARe System

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

To adjust the gas flow when using a gas controller:


1

Press the SETUP key to enter the Setup menu.

Touch the Gas 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.

Touch the Done button (

) to display the gas flow rates.

) when the gas flow rates are as wanted.

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.

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7-13

SmartSens Terminal

7.4.4

Displaying information about the TA module

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

Press the SETUP key to enter the Setup menu.


Touch the System Info (

) button on the Setup menu.

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.

diagnostics test with


Diagnostics button

Module identification number

Unique identification number of your module

Module software version

Name of the current module software version

Module serial number

Serial number of TA module

Sensor type

Type of sensor installed

Furnace

Type of furnace installed in the TGA/DSC 1

Cooling option

Type of cooling option installed

Display

Version name of the SmartSens Terminal software

Controller

Type of controller board installed

Balance

Type of balance installed in the TGA/DSC 1

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

Touch the Diagnostics ( ) button on the Setup menu.


The Diagnostics menu appears. There is also a Home ( ) button, which returns you to
the home screen.

7-14

Touch the Full Test ( ) button to start the diagnostics test.


The text Full test is running appears to indicate that the diagnostics test is running. As
soon as the test is completed, the text Full test finished appears.

Press the Home (

) button to return to the home screen.

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SmartSens Terminal

7.4.5

Displaying information about the experiment

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 (

) button on the home screen.

Experiment button

A window containing information about the current experiment appears.

User

User name

User ID

User identification

Method

Method name

Experiment

Experiment name

Sample

Sample name

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SmartSens Terminal

7.5

SmartSens Terminal settings

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

To access the "Terminal Setup" menu:


Press the SETUP key to the left of the touch screen.
Touch the Terminal Setup (

) 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.

This applies to all settings described below.


property displayed
in first line

To select the property displayed in the first line of the display:


1

Touch the button in the Upper display line row.

Touch the button in the list that corresponds to the desired property.

Default setting: Tc (cell temperature)


define order of
measured values
in list

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

Touch the Setup button in the Signals view configuration row.


The buttons in the list that now appears correspond to the measured values that can be
displayed. The corresponding measured values are indicated in each line of the list.

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.

The buttons are now numbered in the desired order.

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0909

SmartSens Terminal

To assign functions to the left and right SmartSens sensors:


1

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

Back to home screen

Setup

Display setup menu

Tare

Tare measured weight value (TGA/DSC 1 only)

Rotate

Scroll values in the second line of the display

left and right


SmartSens sensors

Standard settings:

"None" is assigned to the right SmartSens sensor

"Rotate" is assigned to the right SmartSens sensor


brightness

To adjust the brightness of the display:


1

Touch the button in the Brightness row.

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.

Default setting: 80%


If the SmartSens Terminal is not used for 15 minutes, the display is dimmed. This extends the life cycle of the backlighting. As soon as you press a key or a different
measured value is displayed, the display resumes at the brightness set.
To adjust the contrast of the display:

contrast

Touch the button in the Contrast row.

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.

Default setting: 50%


To change the colors of the display:

color selection

Touch the button in the Color selection row.

Touch the color palette of choice in the list.

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)

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SmartSens Terminal

beep volume

To change the beep volume:


1

Touch the button in the Sound row.

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.

Default setting: 70%


screen saver

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

Touch the button in the Screen saver timeout row.


The animated calculator appears. You can use it to enter numbers.

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.

Default setting: 0 minutes (screen saver is switched off)


To return to the previous display after the screen saver has been switched on:
Touch the screen.
display off timeout

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

Touch the button in the Display off timeout (minutes) row.


The animated calculator appears. You can use it to enter numbers.

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.

Default setting: 0 minutes (display remains switched on)


To return to the previous display after it has been switched off: Touch the screen.
touch adjustment

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).

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HP DSC 1

Calibration and Adjustment

Calibration and Adjustment

Contents
8.1

Calibration measurement and evaluation ...................................................................................... 8-1

8.2

Calibration: the indium check ....................................................................................................... 8-3

8.3

Adjustment................................................................................................................................... 8-4

8.3.1

Adjustments at elevated pressure..................................................................................................... 8-4

8.3.2

The factory adjustment ................................................................................................................... 8-4

8.3.3

Adjusting the HP DSC 1.................................................................................................................. 8-5

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HP DSC 1

Calibration and Adjustment

Calibration and Adjustment

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

Calibration measurement and evaluation

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.

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CQ System Test

8-1

Calibration and Adjustment

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.

A list of the methods is displayed.


You can obtain information on the method and the automatic evaluation linked to it
by previewing the Check method in the Method Window.
To preview or print information on the Check method:

8-2

Click File/Print Preview.

To print the information: Click Print. You can also print the information to PDF file
if you have installed a PDF creation tool.

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HP DSC 1

8.2

Calibration and Adjustment

Calibration: the indium check

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

Advice on sample preparation (indium check or calibration) is given in the


chapter Calibration in the STARe Software Operating Instructions

Notice

To perform a control measurement


Use one of the following methods:

Check DSC ^exo In

Check DSC ^endo In

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:

Onset temperature 419.6 0.7 C


Heat flow 107.5 3.2 J/g

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.

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adjustment

8-3

Calibration and Adjustment

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

Adjustments at elevated pressure

We recommend carrying out the adjustments at the particular operating pressure at


which the HP DSC 1 measurements will be performed, since the sensitivity E of the
DSC sensor is slightly dependent on pressure.

8.3.2
factory adjustment

The 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.

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HP DSC 1

8.3.3

Calibration and Adjustment

Adjusting the HP DSC 1

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:

"Single" indicates a calibration on the basis of a single sample measurement.

"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.

Example: Calib DSC Temp Single . . In


This is a method for calibration and adjustment of the cell temperature using a single
indium sample.
Checks after an adjustment:

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.

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8-5

Calibration and Adjustment

HP DSC 1

It is possible to improve the measurement accuracy of your HP DSC 1 by adjusting it


in a special way. The methods provided in the STARe Software database may not be
sufficient for this. For example, you may wish to perform a two or three-point adjustment within a particular temperature range.
manual adjustment

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

Select or create a suitable calibration method in Method Window of the STARe


Software to measure the fusion point of the substance of interest. We recommend
a heating rate of 10 K/min.
The calibration method is opened in the Method Window.

Change the method according to your needs and save it under a new name.

Prepare the sample crucible.

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.

Make the following evaluation settings on the Settings menu:


Click Settings/Result Mode and select Sample Temp as the result mode.
Click Settings/Optional Results and select the optional results Heating
Rate, Onset, Norm. Value, Result Mode and Tangents.

Click Settings/Baselines/Spline on the Settings menu to select the baseline


type spline.

8-6

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0911

HP DSC 1

Calibration and Adjustment

Perform an integration evaluation on the fusion peak as follows


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.
The results of the integration are displayed in a text block.

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.

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8-7

HP DSC 1

Maintenance

Maintenance

Contents
9.1

General advice on maintenance .................................................................................................... 9-1

9.2

Malfunctions ................................................................................................................................ 9-6

9.3

Disposal ...................................................................................................................................... 9-7

9.4

Electrical safety test per DIN VDE 0702 in EU countries ................................................................. 9-7

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Maintenance

Maintenance

9.1

General advice on maintenance

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

Cleaning the furnace

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.

Perform an indium check after this experiment is completed.

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9-1

Maintenance

HP DSC 1

9.1.2

Changing the safety rupture disc

Disassemble and reassemble the safety rupture disc as described below.


Disassembly
1

Open rupture disc screw (5) and remove the rupture disk.

Clean contaminated parts with acetone or ethanol.

Grease thread with a little silicone grease.

Assembly

3
1

5
4

Insert the gasket (1).

Insert rupture disc (2) with the curvature facing the screw.

Insert slip ring (3).

Lay safety screen (4) in the rupture disc screw (5).

Screw in rupture disc screw.

Check
Before you start measurements, check the new rupture disc:
1

Attach tubing connection to the safety rupture disc screw.

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.

Changing the alumina wool insulation of the pressure cylinder cover


The alumina wool lining serves to stabilize the pressurizing gas circulation. It must be
replaced from time to time, after approx. 30 measurements. (see chapter 12, Accessories).

9.1.3

Changing the O-rings

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

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HP DSC 1

Maintenance

Access to cylinder base (see figure on page 9-4)


3

Remove bracket and lift up jacket tube.

Unscrew holding-down device of pressure cylinder and lift up pressure cylinder.

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

Cleaning Gas line OUT

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).

Close the INLET valve, open the OUTLET valve.

Lift up the bracket and remove the pressure cylinder cover.

Remove the bracket and lift up the jacket tube.

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).

Mount the pressure cylinder and close.

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.

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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).

1 Heating connection (left)


2 Pt100 connection (left)
1

3 Pt100 connection (right)


4 Heating connection (right)
5 Spacer column

5
12

6 Connection for short sensor wire

7 Connection for long sensor wire

11

8 Feedthrough for purge gas


9 Spacer column

10

10 Feedthrough for gas inlet and


outlet (pressure)

8
9

11 Spring support for tension spring


12 Spacer column

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

METTLER TOLEDO STARe System

0911

HP DSC 1

9.1.6

Maintenance

Cleaning the sensor

You may need to clean the sensor if the blank curve is not to your satisfaction. This
could be caused by several events.

Particles on the sensor

The crucible is stuck to the sensor

The sensor position has shifted

Clean the sensor surface with a cotton swab dipped in alcohol


or
Heat the open measuring cell for 15 min at 500 C.

9.1.7

Replacing the DSC Sensor

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

Centering the DSC sensor

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

METTLER TOLEDO STARe System

9-5

Maintenance

HP DSC 1

9.2
Malfunctions
No pressure buildup

Malfunctions

Causes
Inlet valve closed

Measures
Open valve

Outlet valve open

Close outlet valve

Gas source with insufficient pressure

Check gas source

Expansion of the gas: leads to internal ice


formation

Always pre-flush lines with dry inert gas

Pressure cylinder cover not screwed on


tightly

Tighten nuts

Line blocked

Clean line (see section 9.1.3)

Lines leaking

Call METTLER TOLEDO service

Valves faulty

Check bulkhead union (see section 9.1.3),


otherwise call METTLER TOLEDO service

Safety rupture disc faulty

Replace rupture disc


(see section 9.1.1)

Pressure gauge faulty

Call METTLER TOLEDO service

O-rings of pressure cylinder faulty

Change O-rings (see section 9.1.2)

Unknown leaks

Call METTLER TOLEDO service

Too much pressure buildup

Pressure regulator of gas source faulty or


set too high

Check reducing valve, set pressure buildup


with INLET valve

No pressure drop

Outlet valve closed

Check valve

Pressure drop too small

GAS OUT line blocked

Clean line (see section 9.1.3)

Rapid pressure change

Abrupt opening or closing of gas source

Close INLET valve beforehand

Pressure cylinder too hot

No or insufficient cooling

Check water flow and temperature: 30 l/h


and 20 C

Water flows out of cooling


cover

O-rings defective

Change O-rings (see section 9.1.2)

Too little pressure buildup

9-6

METTLER TOLEDO STARe System

0911

HP DSC 1

9.3

Maintenance

Disposal

In conformance with the European Directive 2002/96/EC on Waste Electrical and


Electronic Equipment (WEEE) this device may not be disposed of in domestic waste.
This also applies to countries outside the EU, per their specific requirements.
Please dispose of this product in accordance with local regulations at the collecting
point specified for electrical and electronic equipment.
If you have any questions, please contact the responsible authority or the distributor
from which you purchased this device.
Should this device be passed on to other parties (for private or professional use), the
content of this regulation must also be related.
Thank you for your contribution to environmental protection.

9.4

Electrical safety test per DIN VDE 0702 in EU


countries

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

METTLER TOLEDO STARe System

9-7

Routine electrical safety test DIN VDE 0702


Test report
Customer-Id.:
Applicant:

Test report no.:


Agent:

Product / Serial number:


Test according: DIN VDE 0702; Routine electrical safety test
Mains supply:
230V, 50Hz, 6A

Tested by:
Class of product: Class I

Check by inspection:

No damage on product

Accessible parts of product are not hazardous live


Warning markings:

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

Function of protection devices

Testing / Measuring:
Used test equipment:
Impedance of protective
bonding (RSL)

Insulation (RISO)

Leakage current (IEA)

()

(M)

(mA)

Protective conductor / Equipotentiality

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

IEA > 3,5mA

Routine test pass

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.

Test label affix on product

Signatures:
Tested by:

Customer:

___________________________________________
Place
Date
Signature

Place

Next test date: ..

_______________________________________________

Date

Signature

HP DSC 1

10

Error Messages and Warnings

Error Messages and Warnings

If a malfunction or a disturbance occurs, an error message or a warning will appear


on the PC screen describing the problem and possible measures to overcome it. The
corresponding error message or a warning will also appear on display of the SmartSens Terminal.

10.1

Error messages

Error messages indicate a serious malfunction. A measurement is always interrupted


when an error message occurs. In some cases, the problem can be overcome by the
operator. In most cases a METTLER TOLEDO service engineer must be called.

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

METTLER TOLEDO STARe System

10-1

Error Messages and Warnings

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.

Follow the instructions in the column Measures.

If you cannot overcome the problem or if the warning re-appears, call your local
service engineer.

List of error messages


Error

Cause

Measures

Problems with the Pt100 temperature sensor (DSC cell)


or with the electronics.

Switch off the HP DSC 1 module for at least five


seconds and then re-start the module. During the
power up, the module performs an internal selftest.

Inform your local service engineer and report the


error number code and the problem. Your feedback helps us to eliminate problems in later versions.

If the error occurs again, call your local service engineer.

AC supply voltage outside the acceptable range.

Check the current voltage and compare it with the


voltage selector setting at the rear panel. The voltages must match.

The software version and the hardware version of the


HP DSC 1 module do not correspond.

Check versions. Call a service engineer and report


code and problem.

20

Furnace lid blocked (or frozen on when using one of the


low temperature cooling options)

Check the furnace lid.


If the furnace lid is frozen on, heat the measuring
cell until the furnace lid can be moved again.

21

Furnace lid position detection defective

See ERROR 4
Maximum temperature at 700 C

22

Furnace temperature is out of acceptable range

See ERROR 4
Maximum temperature at 700 C

10-2

METTLER TOLEDO STARe System

0911

HP DSC 1

Error Messages and Warnings

List of error messages (continued)


Error

Cause

Measures

23

Problems with the Pt100 temperature sensor in the


furnace (DSC cell) or with the electronics.

Report code and problem to your local service engineer.


Maximum temperature at 808 C

24

The temperature of the cooling flange is above the


specified value; heat dissipation is no longer effective.

With a refrigerated circulator, check the coolant flow


and temperature.
Maximum temperature at 180 C.

25

Problems with the Pt100 temperature sensor in the


heat sink (DSC cell) or with the electronics.

See ERROR 23

26

Cooler temperature calibration defective

See ERROR 4

27

Electronics power supply defective

See ERROR 4

28

DSC sensor defective or measuring channel defective

Report code and problem to your local service engineer.

29

Hardware error

See ERROR 4

30

Module identification not available

Call your local service engineer and report code


and problem.

31 to 41

Hardware error

See ERROR 4

42

Cold junction temperature is outside specified value

See ERROR 24

43

Hardware error

See ERROR 4

0911

METTLER TOLEDO STARe System

10-3

Error Messages and Warnings

HP DSC 1

List of error messages (continued)


Error

Cause

Measures

128 to999

Internal software error

(except 850,
see below)

exceptions: ERROR 400 and 401

Switch off the module for at least five seconds and


then re-start the module. During the power up, the
module performs an internal self test.

Inform your local service engineer. If possible, inform


the service engineer about the circumstances that
led to the error. Your feedback helps us to eliminate
problems in later versions.

If you cannot overcome the problem, call your local


service engineer and report code and problem.

850

Software or hardware problems

SmartSens Terminal defective

10.2

Call your local service engineer and report code and


problem.

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.

Follow the instructions in the column Measures.

If you cannot overcome the problem or if the warning re-appears, call your local
service engineer.

METTLER TOLEDO STARe System

0911

HP DSC 1

Error Messages and Warnings

Warning

Cause

Measures

13

SmartSens Terminal disabled

Call your local service engineer and report code and


problem.
During power up, do not press a key or button,
otherwise warning 13 will appear.

14

Insert, start- or remove temperature of the sample


could not be reached or held constant.

Click OK or Reset on the PC or, press Skip or


RESET on the SmartSens Terminal.

20 to 54

Internal software error was detected and eliminated.

Click OK.

0911

METTLER TOLEDO STARe System

10-5

Error Messages and Warnings

HP DSC 1

List of warnings (continued)


Warning

Cause

Measures

55

The module identification number is wrong.

Check the number.


The identification number must match the number you
find in the Identification box in the Module tab of the
Install Window.

56 ff.

Internal software error

Click OK.

Inform your local service engineer. If possible: inform


the service engineer about the circumstances that
led to the error. Your feedback helps us to eliminate
problems in later versions.

If you cannot overcome the problem, call your local


service engineer.

58 to 61,
90

10-6

version mismatch

Problems with communication

Check the connections between the module and the


PC.
If you cannot overcome the problem, call your local
service engineer.

METTLER TOLEDO STARe System

0911

HP DSC 1

11

Specificatons

Specifications

TEMPERATURE DATA
All data applies to ambient
environmental pressure
Temperature range

Cooling system: double-walled jacket with water


cooling (22 C)
Furnace power

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

Possible heating rates


Cooling time

0.1 MPa:

5 min

10 MPa:

5 min

0 to 100 K/min (at 700 C)


smallest increment 0.01 K/min
water cooling
from 700 C to 100 C

0.1 MPa:
10 MPa:

11 min
9 min

CALORIMETRIC DATA

FRS5

HSS7

Sensor type

ceramic

ceramic

Number of thermo couples

56

120

Signal time constant

1.7 s

3.9 s

350 mW

160 mW

Resolution

0.04 W

0.01 W

Digital resolution

16.8 million points

Measurement range

at 100 C

SAMPLING
Sampling rate
1

maximum 50 points/second

based on metal standards

0911

METTLER TOLEDO STARe System

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

Pressure limit of rupture disk

12.4 to 13.8 MPa

Cooling of pressure cylinder

Cooling agent: water


Flow rate:

ca. 20 L/h

Temperature: 20 to 30 C
Materials of pressure cell

Cylinder jacket:

Stainless steel 1.4435 (AISI 316)

Bottom and cover:

Stainless steel 1.4435 (AISI 316)

Guide rods:

Stainless steel 1.4435 (AISI 316)

Screws and nuts:

Stainless steel 1.4435 (AISI 316))

Valves (fittings):

Stainless steel 1.4435 (AISI 316)

Needle valve:

Stainless steel 1.4435 (AISI 316)

Pressure gauge:

Stainless steel 1.4435 (AISI 316)

Pressure lines:

Stainless steel 1.4435 (AISI 316)

Gas connection

1/8 inch

O-rings

O-ring for cylinder cover


O-Ring 69.49x2.01 KALREZ for use with CO2

Gas connections

Gyrolok, outer diameter:

1/8 inch

Tube diameter

Outer diameter:

1/8 inch

Safety rupture disk

Stainless steel

1.4435 (AISI 316)

Tube adapter

Outer diameter:

15 mm

Gas for pressure build up

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

with tall furnace lid (standard):


20 l and 40 l aluminum crucible
30 l alumina and platinum crucible
40 l copper and gold crucible
with flat furnace lid (optional):
20 l, 40 l, 100 l and 160 l aluminum crucible
30 l alumina and platinum crucible
40 l copper and gold crucible
70 l sapphire and platinum crucible
150 l alumina and platinum crucible

11-2

METTLER TOLEDO STARe System

0911

HP DSC 1

Specificatons

Measuring cell

Furnace made of silver

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

230 V, 60Hz, 6 A or 115 V, 50 Hz, 12 A


The tolerance of the AC voltage fluctuation is 10% of the nominal AC supply
voltage.

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

METTLER TOLEDO STARe System

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

Crucible handling set

51142765

Calibration kit

51142760

Tool kit

51142770

Indium pellets for temperature calibration

119442

Zinc pellets for temperature calibration

119441

Set of 40 l Al crucibles without centering pins, with lids (100 pcs)

27331

Plug (2P + G) for the Switched Line Socket

87978

Wrench, 14 mm

72059

DSC sensor centering aid

119360

Ethernet Cat 5e connection cable

51191860

Ethernet crossover connection cable

51191861

Cable (country specific)


Note paper insert (set of 10 sheets)

51143110

Glass cover

51142300

"Do not touch" warning plate

51142637

Blank warning plate

51142638

EPDM rubber tubing, 6 m

51140860

Cobra 15/8 hose clamp (4 pcs)

51191160

Tall furnace lid

51141544

0911

METTLER TOLEDO STARe System

12-1

Accessories

HP DSC 1

Optional accessories

ME order number

Switched Line Socket *

51119682

Power Switch 115 V *

51119955

Power Switch 230 V *

51119954

Small furnace lid

51141348

DSC FRS5 sensor (installed before delivery)

51141302

DSC HSS7 sensor (installed before delivery)

51141628

Tension spring for DSC sensor (installed before delivery) *

11612

Ceramic disc for DSC sensor (installed before delivery) *

26741

Tweezers **

51191865

Needle to pierce crucible lids **

29772

Crucible Sealing Press, with:

119410

Operating instructions (Eng./Ger.) for the crucible sealing press


Tool kit to adapt the crucible sealing press (ME-119410) with the round base to medium
pressure crucibles

709301
119428

Flow meter for gas flow rates up to 266 mL/min air

51141999

Tutorial Sample Kit, with 14 substances

51140879

Alumina wool mat

51141581

O-ring (cylinder cover/cylinder base)

51190800

O-ring (69.49x2.01)

51191931

O-ring (cooling cover, 68 mm)

71738

O-ring (cooling cover, 32 mm)

71543

O-ring (cooling jacket)

51191263

Tube connection (safety rupture disk), external diameter 15 mm

26735

Nut M14

26753

Safety rupture disk kit*

51191276

Pressure controller PC 10*

51143150

Huber Ministat 125 (300W, 230VAC)

51191743

Huber Ministat 125 (300W, 115VAC)

51191750

Huber Ministat 230 (400W, 230VAC)

51191744

Huber Ministat 230 (400W, 115VAC)

51191751

12-2

METTLER TOLEDO STARe System

0911

HP DSC 1

Accessories

Sensor protection disk (2 pcs)

00026947

Screw collar (for ports)

71752

Ferrule, front (for ports)

71745

Ferrule, rear (for ports)

71746

Silicone grease

71300

STARe Software User Handbook, English

51710263

Different types of crucibles according to Table 1

Optics accessories

ME order number

Microscopy kit HP DSC

51143089

Chemiluminescence kit HP DSC

51143090

HP DSC CL Bundle (240 V)

51191624

HP DSC CL Bundle (115 V)

51192064

* These options have to be installed by a METTLER TOLEDO service engineer.


** Included in Crucible Handling Set ME 51142765

0911

METTLER TOLEDO STARe System

12-3

Accessories

HP DSC 1

Table 1. Crucible types


Crucible Type

Lid

Volume L

Centering pin No. of pieces

ME order no.

Light aluminum crucible

with

20 L

without

100

51119810

Standard aluminum crucible

with

40 L

with

100

27331

Standard aluminum crucible

with

40 L

without

100

26763

Standard aluminum crucible

without

40 L

without

400

51119870

Standard aluminium lid

400

51119871

Pierced aluminium lid 50 l

400

51140832

Aluminium lid for piercing

400

51119873

Medium aluminum crucible

without

100 L

without

400

51119872

Tall aluminum crucible

with

160 L

with

40

27811

Copper crucible

without

40 L

with

100

51140407

Gold crucible

with

40 L

with

27220

Small platinum crucible

with

30 L

without

51119842

Medium platinum crucible

with

70 L

without

51119654

Large platinum crucible

with

150 L

without

24126

Medium Pressure crucible 1)

with 2)

120 L

with

25

26929

Medium Pressure crucible 1)

with 2)

120 L

without

25

29990

Disposable High Pressure crucible 3)

with

40 L

with

25

26732

Disposable High Pressure crucible 3)

with

40 L

without

25

26731

High pressure crucible

with

30 L

without

51140404

High pressure gold plated crucible

with

30 L

without

51140405

60

51140403

Seal for gold plated crucible


High Pressure crucible)

with

270 Ll

with

650072

High Pressure crucible)

with

500 L

with

650066

12-4

1)

PCTFE Sealing Ring, for samples dissolved in water, 30 pieces


order no. : 26933

2)

With lid and Viton O-Rings

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

METTLER TOLEDO STARe System

0911

HP DSC 1

Index

13 Index
A

Accessories, 12-1

calibration, 8-1

accuracy, 8-6

calibration method, 8-6

Accuracy, 8-3

calibration methods

A/D converter, 2-8


adjustment, 8-1
Adjustment, 8-4

total calibration, 8-5


calibration methods
Single calibration, 8-5

factory adjustment, 8-4

Calibration methods, 8-3

adjustment data, 4-9, 4-12

calorimetric data, 11-1

adjustment overview, 4-12

centering, 6-5

air cooling, 2-2

Centering the sensor, 9-5

altitude, 4-2

Check methods, 8-1, 8-2

analog/digital convertor, 2-8

cold junction temperature, 10-3

artifacts, 4-1, 6-1

communication, 4-7, 4-10, 5-1


communication problem, 5-1

Control measurement, 8-3


connecting ports, 4-10

basic module, 2-3

Connections tab, 4-10

Boersma principle, 2-9

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

METTLER TOLEDO STARe System

Index

HP DSC 1

electrical safety, 9-7, 11-3

hardware options, 1-2

Electromagnetic compatibility (EMC), 4-1, 11-3

heat flow adjustment data, 4-12

electromagnetic disturbances, 4-1

heat flux principle, 2-9

electromagnetic fields, 4-1

heating rates, 11-1

EMC, 4-1

heating time, 11-1

environmental conditions, 11-3

High Sensitivity Sensor, 2-8

error code, 10-1

HP DSC 1

error message, 10-1


Ethernet
Ethernet cable, 2-7

rear panel, 2-5


HSS7, 2-8
HSS7 sensor, 9-5

Ethernet port, 4-5


Ethernet socket, 4-5
Ethernet TCP/IP connection, 2-2, 2-7
external connections, 2-5

I
ICTA sign convention, 8-2
indium check, 5-1, 6-1, 6-5, 8-1, 8-3, 8-5
infrared sensor, 7-4

insert sample, 6-16, 7-6


INSERT SAMPLE, 6-15, 6-17

factory adjustment, 8-4


fan, 2-2
FCC rules, 1-10
FRS5 sensor, 9-5

insert temperature, 7-6


Install Window, 4-8
installation, 4-1
intended use, 1-4

furnace lid, 10-2


furnace power, 11-1
Furnace Power Off, 2-6
fuses, 2-6, 4-4

L
leveling screws, 2-3
line socket, 2-6

location, 4-1

gas bottles, 4-3


Gas button, 7-9, 7-15
gas controller, 7-15
gas controller symbol, 7-10
Gas flow rate, 4-3
gas supplies, 4-3
GLP, 8-1, 8-3

METTLER TOLEDO STARe System

0911

HP DSC 1

Index

P (continued)

power supply, 4-4, 11-3


mains connections, 2-6

Power supply connections, 2-6

mains supply voltage, 4-4

Power supply system, 4-4

Maintenance, 9-1

power supply switch, 5-1

manufacturer, 1-1

power switch, 2-10

manual adjustment, 8-6

preparing experiments 6-1

Manual furnace lid, 2-4

pressure cell, 11-2

measurement principle, 2-9

pressure reduction valve, 4-3

measurement preparation 6-5

Proceed button, 7-9, 7-13, 7-14

measuring cell, 2-8, 2-9

Pt100 temperature, 10-3

Measuring cell, 2-4

Pt100 temperature sensor, 2-8, 10-2

mobile phone, 4-1

purge gas, 2-8, 4-3

modular design, 1-2

Purge gas flow rate, 4-3

module, 4-9

protective gas, 4-3

module data set, 4-9

Pt100 temperature sensor, 2-9, 10-2, 10-3

Import Module, 4-9

purge gas inlet, 2-9

module (in STARe Software), 4-9

purge gas, 4-3, 2-9

module identification, 10-3


Module Control Window, 2-9

module dataset, 8-4

radio interference regulations, 1-10

multiple sample pan, 8-5

rating plate, 4-4


refrigerated circulator, 2-10, 3-1, 4-1

removing a module from a port, 4-11

needle valve, 13-229

resolution, 2-8

number code, 10-1

room conditions, 4-2


REMOVE SAMPLE, 6-8, 6-14, 6-17, 6-18

RESET, 6-8, 6-18


Operational safety, 1-9

resolution, 11-1

operating state, 2-5


Optics, 12-3
Optional accessories, 12-3
Options, 12-2

P
plastic cover (SmartSens Terminal, 7-4peripheral
units, 2-10
power saving mode, 2-10
Power supply
0911

METTLER TOLEDO STARe System

Index

HP DSC 1

T (continued)
time constant, 2-2

Safety Notes, 1-4


sampling rate, 11-1
Send experiment, 6-14
Sensor
replace sensor, 9-5
shutdown, 5-1
silver furnace, 2-8
SmartSens sensors, 7-4
SmartSens Terminal, 2-4, 10-1, 10-4
specifications, 11-1
spring loaded furnace assembly, 2-8
standard accessories, 12-1

Title bar, 7-3


Toggle button, 7-9, 7-15
Tolerance limits, 8-1, 8-3
total calibration, 8-5
touch screen
brightness of display, 7-19
colors of display, 7-19
contrast of display, 7-19
screen saver, 7-20
touch adjustment, 7-20
volume of the beep, 7-20
typographic conventions, 1-3

Standby temperature, 6-8, 6-18


Start experiment, 6-8
start measurement, 6-14, 6-17

V
Voltage, 2-6, 4-5, 10-2

startup, 5-1
switched line socket, 2-10
STARe Software, 1-2, 4-7, 4-8

stabilized power supply unit, 4-4

warning number code, 10-4

start temperature, 7-6

warnings, 10-4

state indicator, 7-6

weighing table, 4-2

State indicator, 7-3

weight, 4-2

state of TA module, 7-16

working area, 4-2

states of the measuring, 7-6


System Info button, 7-9
system information, 7-16

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

METTLER TOLEDO STARe System

0911

To protect your METTLER TOLEDO products future:


METTLER TOLEDO Service assures the quality, measuring accuracy and
preservation of value of all METTLER TOLEDO products for years to
come. Please send for full details about our attractive terms of service.
Thank you.

STARe thermal analysis system, operating instructions to the HP DSC 1


Subject to technical changes and to the availability
of the accessories supplied with the instruments.

*51710771*
Mettler-Toledo AG 2009

Printed on 100% Chlorine-free paper

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

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