HPDSC1

STARe System

Operating Instructions

Thermal Analysis Excellence HP DSC 1

1 Introduction and Safety Notes

2 Design and Function

3 Cooling Options

4 Installation

5 Switching On and Off

6 Measurement

7 SmartSens Terminal

8 Calibration and Adjustment

9 Maintenance

10 Errors, Warnings and Malfunctions

11 Technical Specifications

12 Accessories

13 Index

HP DSC 1 Introduction and Safety Notes

0911 METTLER TOLEDO STARe System 1-i


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


0911 METTLER TOLEDO STARe System 1-3


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 re-search 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 com-pared. 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 tempera-ture 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

Introduction and Safety Notes HP DSC 1

1-4 METTLER TOLEDO STARe System 0911

1.2 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 op-tions.

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. Refer-ences are made to the STARe Software in certain parts of these operating instructions.

Modularity



1.4 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 infor-mation 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 Caution

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.).

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.

Text that appears in the bold Arial Narrow font shows text that appears on the touch-screen of the SmartSens Terminal.

CAPITAL LETTERS indicate keys to be pressed on the PC or on the SmartSens Terminal.

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 marks a note containing additional information in a particular context.

Notice

Times New Roman

Italic

Arial Narrow bold

CAPITALS



1.5 Safety Notes

The instruments have been tested for the experiments and intended purposes docu-mented 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 calo-rimetry.

All other use and operation beyond the limits of operation defined by Mettler-Toledo 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

Switch off the HP DSC 1 and remove the power cable before you open the hous-ing or replace blown fuses. An electric shock could be lethal.

Do not use gases that could form an explosive gas mixture! Reactive gas mix-tures 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.



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 oxy-gen!

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 ºC, otherwise condensation could develop.

Never try to carry the HP DSC 1 module alone. The instrument weighs approxi-mately 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 oxida-tion reaction can be explosive. The ceramic sensor may then possibly break as a re-sult 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 tem-perature gradient and less mechanical stress in the ceramic sensor.



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 instrument’s 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 re-sponsible to fulfill all local and internal safety regulations and to follow the limitations defined in the instructions of the corresponding instrument.

The HP DSC 1 measuring cell is not designed for the use of flammable and ex-plosive 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 in-ert 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 mix-tures consisting of combustible, oxidizing, and inert gases are only flammable under cer-tain conditions. The lower flammable limit (LFL) (lower explosive limit) describes the lean-est 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 flam-mable mixture. Increasing the fraction of inert gases in a mixture raises the LFL and de-creases 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)

explosive limits



Gas Explosion limits (LEL to UEL)in vol %

Corrosive Flammable Toxic

Ammonia 15 - 28 x x x

Argon – – – –

Carbon dioxide – – – –

Ethylene 2.7 - 34 – x –

Helium – – – –

Hydrogen 4.0 - 75.6 – x –

Nitrogen – – – –

Oxygen – – – –

Note: The explosion limits values may vary slightly depending on your source of in-formation.

Safety notes related to hydrogen in a high pressure DSC

Loading and unloading the samples requires opening the furnace so that the sur-rounding 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 (pres-surize to 1 MPa with nitrogen and release the gas at least three times or purge long enough with the inert gas).



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 explo-sive 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 (pressur-ize 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 hous-ing. 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.



1.5.2 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 as-sure 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 instru-ment 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!



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 de-signed to provide reasonable protection against harmful interference when the equip-ment 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 été testé et s'est avéré conforme aux limites prévues pour les appareils numériques de classe A et à la partie 15 des règlements FCC et à la réglementation des radio - interférences du Canadian Department of Communications. Ces limites sont destinées à fournir une protection adéquate contre les interférences néfastes lors-que I' appareil est utilisé dans un environnement commercial. Cet appareil génère, utilise et peut radier une énergie à fréquence radioélectrique; II est en outre susceptible d'engendrer des interférences avec les communications radio, s'il n'est pas installé et utilisé conformément aux instructions du mode d'emploi. L'utilisation de cet appareil dans les zones résidentieIIes peut causer des interférences néfastes, auquel cas l'ex-ploitant sera amené à prendre les dispositions utiles pour palier aux interférences à ses propres frais.

HP DSC 1 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




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 meas-uring cell in more detail.

2.1 Introduction

The HP DSC 1 module is a high pressure differential scanning calorimeter and in-cludes 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 pres-sure 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 meas-uring 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.

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 applica-tions with a number of hardware options. When you place your order, you determine the actual configuration of your HP DSC 1. You can expand your HP DSC 1 with the required hardware options to meet new demands at any time in the future.



2.2.1 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) 6 SmartSens Terminal

2 Gas connections 7 Pressure cylinder with measuring cell

3 Rupture disc 8 Lifting bracket

4 Tube connection 9 Area for notes with pressure gauge

5 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.

leveling screws



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 fur-nace! 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.

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

measuring cell

SmartSens Terminal



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

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

1 Main switch 8 Valve control connection for GC10

and GC20 (unused)

2 Power supply inlet socket 9 Ethernet connection

3 Line output socket 10 Instrument ID

4 Fuse for the line output socket 11 Serial number

5 Rating plate 12 Water outlet

6 Fuse for the electronics power supply

13 Water inlet

7 Connection to synchronize external devices

external connections



2.2.2 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

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.

2 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.

AC connections

voltage



Ethernet TCP/IP connection: The module is connected via the Ethernet TCP/IP connec-tion 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 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.

gas inlets and outlets



2.2.4 Measuring cell

The measuring cell essentially consists of the furnace and the DSC sensor. It is ex-plained in detail in the following.

Design of the measuring cell

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 op-erated with the full-range FRS5 sensor. With both sensors, the digital resolution of the measurement signal is less than 0.04 W.

You can read more than 16 million measuring points with the new 24 bit ana-log/digital converter.

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 ce-ramic 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).

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.

An external cooling device must be connected providing a water flow rate of 20 l/h, with water temperatures between 20 and 30 ºC. Refer to Chapter 3 Cooling for spe-cific details.

High Sensitivity Sensor

A/D-converter

furnace

purge gas

cooling



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 tem-perature program for the individual segments to the measuring module.

During a measurement, measurement data is continuously transmitted from the mod-ule to the PC. The data is presented as an online curve in the Module Control Win-dow.



2.3 Optional switched line socket

The Switched Line Socket option allows you to switch peripheral units (e.g. a refriger-ated 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 neces-sary, 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.

HP DSC 1 Cooling


3 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 tempera-ture 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

HP DSC 1 Installation


4 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



4 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 arti-facts, for example.

When choosing the installation location for the HP DSC 1, avoid the following elec-tromagnetic disturbances:

Ensure that no vertical power lines, motors, or similar devices are near the mod-ule. Check the neighboring rooms as well.

Ensure that the following minimum distances are kept between the HP DSC 1 and the following devices:

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.

electromagnetic disturbances

Installation HP DSC 1


4.1.2 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.

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.

working area

room conditions



4.2 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 pres-sure 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: 0 – 100 mL/min



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. Addition-ally, 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 in-strument can suffer damage if the operating voltage does not match the AC sup-ply 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:

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.

voltage



4.5 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.

2 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.

4 Connect the power supply cable.

5 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 Soft-ware User Handbook.

6 To set up the pressure cylinder:

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).

a b

cd

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-ring’s 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 refrig-erated circulator.

leveling screws

voltage



7 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.

0

5

10

15

500

1000 1500

2000

23000psi

MPa

AUX IN OUT

2 3

1

4

5

7

Valve for pressure build up

Valve for pressure reduction

Bulkhead union for purge gas in

Valve for purge gas inlet

Needle valve for fine regulation of purge gas

Safety rupture disc

Pressure gas inlet

Purge gas inlet

Bulkhead union for pressure gas in

Bulkhead union for pressure gas reduction

8 9 10

1

2

3

4

5

6

7

8

9

10

6

You can always remove and reattach the tubes.



8 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.

8 AUX 11 Rupture disc

9 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 com-municate with an HP DSC 1 using a DSC827e module data set.



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 appears in the Windows task bar.



4.6.2 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 indi-

vidual 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 sup-plied:

1 Insert the module CD ROM in the CD ROM drive. In the Install Window, click the Module tab and then click Import on the File menu.

The Import Module dialog box appears.

2 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.

3 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 cre-ated 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).

installation with the module CD-ROM



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 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".

2 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.

connecting to port



To disconnect a HP DSC 1 module from the port:

1 In the Install Window, click the Connections tab.

2 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.

3 Click Yes to disconnect the module from the port.

The HP DSC 1 module is disconnected from the port.

disconnecting from port



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 corre-sponds 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 data-base:

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.

2 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 tem-perature 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…

HP DSC 1 Switching the Instrument On and Off


5 Switching the Instrument On and Off

Before switching on the HP DSC 1, make sure that all its parts have reached tempera-tures between +10 °C and +31 °C and the relative humidity is between 20% and 80% and no condensation can occur.

5.1 Switching on

1 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.

2 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 be-tween the module and the PC is established.

3 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 lim-its 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 uncon-trolled manner.

For sample removal, the temperature should be below 40 °C.

1 Always remove the last sample crucible before switching off the instrument.

2 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 im-portant.

HP DSC 1 Measurements


6 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



6 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.

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.

2 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.

6 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 Open the OUTLET valve after the test: The gas flows out of the GAS OUT outlet.

6.3 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!



6.4 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)

1 Close the Quick-Vent Valve on the PC10.

2 Align the gas connections of the PC10 and the HP DSC 1 by adjusting the level-ing screws at the bottom of the PC10. These should be aligned properly to avoid bad connections or even damage.

3 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.

4 Tighten the screws.

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



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

7 Connect the gas to the INLET and tighten the screw. Make sure that the Quick-Vent Valve is open.

8 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.

9 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 hasn’t been completely vented.

*Refer to the operating instructions of the BROOKS control and display unit for further information.



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.

2 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).

3 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).

4 Optional step: Attach the tubing connection to the safety rupture disc and connect it to the pressure tubing (Ø 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 ex-periments

Before you can perform a measurement on the HP DSC 1, you must make the follow-ing 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.

2 If the DSC sensor is not in the center position, adjust the DSC sensor with the centering gauge.

3 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”.

4 Perform an experiment without a crucible using the method “heat”.

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

6 Before the first measurement, run a temperature program without a sample to precondition the HP DSC 1 cell.



6.6.1 Crucibles – without lid or with perforated lid

Depending on the application, you can work with a crucible without a lid, for exam-ple, when measuring oils to determine their oxidative stability.

For enthalpy determinations, you should perforate the crucible lid once using the nee-dle from the crucible set.

For determinations of boiling temperatures, perforate the crucible lid, on a hard sur-face with a compass point (hole diameter: approx. 50 μm) or use the perforated lids from METTLER TOLEDO.

Don’t 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.

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 af-ter 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.



6.7.2 Performing an experiment without a flow meter, flow con-troller 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.

3 Place the sample crucible carefully on the left pan position of the DSC sensor and place an empty reference crucible on the right.

4 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.

5 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 O-ring is free of alumina wool fibers.

6 Mount the pressure cylinder cover and tighten the four nuts by hand. This is suffi-cient to seal the system.

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

8 Close the OUTLET, INLET and AUX IN valves.

9 Open the gas inlet for the pressure buildup.

10 Open the INLET valve slowly.

11 Close the INLET valve when the pressure is reached.



To perform an experiment on the HP DSC 1:

1 Start an experiment on the module. Wait until the measuring cell has reached the insert temperature.

The module goes to the insert temperature. The request to insert the sample is displayed on the touch screen and in the Module Control Window.

2 Click OK in the Module Control Window.

The measurement starts. At the end of the experiment the REMOVE SAMPLE request ap-pears in the Module Control Window.

3 Open the OUTLET valve slowly to release the pressure at the end of the experi-ment.

4 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.

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

7 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 Click RESET to set the measuring cell to the standby temperature after the meas-urement.

The cell goes to standby temperature.

9 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).

Start experiment

Standby temperature

furnace power off



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]

T [°C]

0 100 200 300 400 500 600

5.0

5.5

6.0

6.5

If you measure over a small temperature range, the pressure change is correspond-ingly small. If you require accurate pressure data, we advise plotting a pressure-temperature curve.



6.7.3 Performing an experiment with a flow meter, flow control-ler 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



Table 1: Overview of connection possibilities

The following scenarios bear limitations

Purge gas Without pressure control

Without

Fig. 1 INLET OUTLET

AUX IN

CONTROL

AUX IN closed

AUX CONTROL closed

INLET closed

OUTLET closed

isothermal: pressure constant dynamic: pressure increase

With flow rate measurement in iso-thermal measurements *

Flow rate (for example, 50 mL/min)

Fig. 2

INLET OUTLET

AUX IN

CONTROL

AUX IN open

AUX CONTROL open

INLET closed

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

isothermal: pressure constant dynamic: pressure increase*

With flow rate control

in isothermal measurements * Flow rate (for example,50 mL/min) (Reducing valve of purge gas source set to same pressure as measuring cell pressure)

We recommend BROOKS mass flow control-ler

Fig. 3

AUX IN

CONTROL

INLET OUTLET

Flow controller

AUX IN open

AUX CONTROL open

INLET closed

OUTLET open

isothermal: pressure constant dynamic: pressure increase*

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 control-ler

Fig. 4

INLET OUTLET

CONTROL

AUX IN

Flow controller

AUX IN open

AUX CONTROL open

INLET closed

OUTLET open: flow rate, for example, 50 mL/min

isothermal: pressure constant ** dynamic: pressure increase

* 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.



Table 1: Overview of connection possibilities (continued)

The following scenarios bear limitations

Purge gas With pressure control

Without

Fig. 5

INLET OUTLET

Pressure controller

AUX IN

CONTROL

AUX IN closed

AUX CONTROL closed

INLET closed

OUTLET open

isothermal: pressure constant

dynamic: pressure constant

With flow rate setting 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)

Fig. 6

INLET OUTLET

Pressure controller

AUX IN

CONTROL

AUX IN open

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

INLET closed

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


Fig. 7

INLET OUTLET

Flow meter

AUX IN

CONTROL

Pressure controller

AUX IN open

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

INLET closed

OUTLET open



With flow rate control


Fig. 8

Control In

INLET OUTLET

Flow controller

AUX IN Pressure controller

AUX IN open

AUX CONTROL open

INLET closed

OUTLET open



*** In isothermal measurements, the display of the flow meter remains constant, in dynamic measurements not.



Pressure controlled with a special controller

To control the pressure in dynamic measurements, you can attach a pressure control-ler 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.

2 Attach the tubing connection to the pressure controller outlet and connect tubing to lead off the gas.

3 Connect the pressure controller to the control and display unit (cable).




6 Place the sample crucible carefully on the left pan position of the DSC sensor and place an empty reference pan on the right.



11 Mount the pressure cylinder cover and tighten the four nuts by hand. This is suffi-cient to seal the system.


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.



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 pres-sure 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 deter-mine 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.

2 Open the needle valve of the flow meter fully.

3 Set the pressure for both gas cylinders (pressure buildup/purging) at the reducing valve to the same value.

4 Connect both gas cylinders (GAS IN for pressure buildup, AUX IN for purging) and open.

5 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.

6 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 in-sert temperature.

7 Do not confirm INSERT SAMPLE with OK, but release the pressure (OUTLET valve).

8 Open AUX IN and AUX CONTROL valves fully. Since the pressure from the purge gas cylinder (after the reducing valve) is ex-actly 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.

9 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 con-nection (see Note a).

send experiment

start measurement



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: it’s heavy.

2 Remove the alumina wool mat.




4 Place the sample crucible carefully on the left pan position of the DSC sensor and place an empty reference crucible on the right.



7 Mount the pressure cylinder cover and tighten the four nuts by hand. This suffices to seal the system.


9 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 com-pensated by purge gas that is flowing in.


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.



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.

2 Attach the tubing connection to the pressure controller outlet and connect the tub-ing to lead off the gas that is flowing out.

3 Connect the flow controller output to the AUX IN inlet.

4 Connect the flow controller inlet to the purge gas line.

5 Connect the flow controller and pressure controller to the control and display unit (cable).





8 Place the sample pan carefully on the left pan position of the DSC sensor. Place an empty reference pan on the right.



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.

insert sample



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.


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.

The measurement starts. At the end of the experiment the REMOVE SAMPLE request ap-pears 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.

start measurement



Removing the sample and switching off the instrument

1 At the end of the experiment, open the OUTLET valve slowly to release the pres-sure. If you have a pressure controller connected set the pressure on the control unit to 0 to relieve the pressure.

2 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.

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

5 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.

6 Confirm the REMOVE SAMPLE request in the Module Control Window with OK.

7 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 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 com-

pared 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.

Standby temperature

furnace power off

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

SmartSens Terminal



This chapter contains basic information on how to operate the following modules us-ing 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 al-lows 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:

1 SmartSens sensors 6 Title bar

2 State indicator 7 RESET key

3 HOME key 8 OUTLET ROTATE key

4 Touch screen 9 FURNACE key

5 SETUP key 10 Area for messages

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 dif-ferent functions such as opening the furnace or scrolling through the displayed meas-urement values (see Section 7.5, SmartSens Terminal settings). This allows you to perform certain operations on the SmartSens Terminal without touching it and possi-bly 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.

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 measur-ing 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 dis-plays 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.

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 cor-respond 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.

The state indicator is a square symbol at the left end of the title bar. The background color and the characters it displays refer to the current stage of the measurements or the corresponding state of the measuring cell.

The text displayed in the title bar gives you more details about the current state of the measuring cell of your TA module. The different states are listed and explained in the following table:

The table gives an overview of the colors and the characters displayed in the state in-dicator. The title bar texts are also listed and explained.

Color of state indicator

Characters in state indicator

Text in title bar and its meaning

blue OFF Standby (furnace power off)

The furnace is switched off. There is no experiment run-ning on the TA module.

green S Standby (standby temperature)

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

green A Going to insert temperature

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

green A Wait for insert sample

The measuring cell is ready for sample insertion.

red M Going to start temperature

The measuring cell is approaching the start tempera-ture.

red M Settling

The temperature is stabilized in the measuring cell.

red M Measurement

The measurement is in progress.

green A Going to remove temperature

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

green A Wait for remove sample

The measuring cell is ready for sample removal.

green S Final user temperature

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

state indicator

title bar text

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 ei-ther 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 Con-trol 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 as-sume 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 con-firm 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.

SmartSens Terminal


7.2 Keys on the SmartSens Terminal

The SmartSens Terminal keys arranged on both sides of the touch screen are de-scribed 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 informa-tion 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: Hard-ware 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 ex-periment 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).

SmartSens Terminal


7.3 Buttons and symbols on the display

The most important buttons and symbols in the user interface of the SmartSens Ter-minal 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)


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


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)


Terminal Calls up the Terminal Setup menu to change the terminal settings (see Section 7.5)


Gas Calls up a menu that allows you to make the settings for the gas flow ra-tes with a GC 10 or a GC 20 gas controllers; only available if a gas con-troller is installed (see Section 7.4.3)


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)


Tare Tares the measured weight value. This button is only available on a TGA/DSC 1. (see Section 7.4.3)


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 open

Furnace closed

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

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

Sample robot active

Sample robot inactive

Sample robot l Indicates whether the sample robot is active or not. If no symbol is dis-played, the sample robot is not installed.

The symbol flashes when the sample robot is performing a task. (see Section 7.4.4)

Gas is flowing

Gas is not flowing

Gas controller (only available when a gas controller is installed)

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

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.

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

Notice

SmartSens Terminal


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

Press the ROTATE key several times until the desired measurement value is dis-played.

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 dis-play a complete list of the currently 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 tempera-ture

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 set-tings).

scroll through the displayed measurement values

enlarge the display of measurement values

display list of measured values

SmartSens Terminal


7.4.3 Entering commands on the SmartSens Terminal

You can enter a number of commands for your module directly on the SmartSens Ter-minal. 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 ex-periment will continue automatically through these stages. You cannot use the Pro-ceed button to confirm them in this case.

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 measure-ment stage and the stages to insert and remove the sample.

Skipping experiment stages can be done for example to shorten the time of an ex-periment. 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.

The stage of an experiment corresponds to the state of the measuring cell. A text de-scribing 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 tempera-ture

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 condi-tions

Going to remove conditions Can be skipped with

Remove sample crucible Waiting for sample removal Must be confirmed with (without sample robot)

Proceed button

Skip button

Notice

SmartSens Terminal


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.

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.

RESET key

FURNACE key

SmartSens Terminal


By touching the Gas ( ) button in the setup menu, you can call up a menu that al-lows 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 auto-matically.

You can open and close the needle valves by pressing the Toggle ( ) button on the SmartSens Terminal.

To adjust the gas flow when using a gas controller:

1 Press the SETUP key to enter the Setup menu.

2 Touch the Gas button ( ) to display the gas flow rates.

3 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 in-structions for further details.

4 To switch between the gas flows, touch the Toggle button ( ). The toggle but-ton opens and closes the electromagnetic valves in the gas controller.

5 Touch the Done button ( ) 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 but-ton 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.

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.

Gas button

Toggle button

Tare button

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:

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 dis-played text using the arrow keys and display the following information.

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.

2 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.

3 Press the Home ( ) button to return to the home screen.

System Info button

diagnostics test with Diagnostics button

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.

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

Experiment button

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.

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.

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

1 Touch the button in the Upper display line row.

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

Default setting: Tc (cell temperature)

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.

2 Press each of the six buttons in the list to delete the current order.

3 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.

Terminal Setup menu

property displayed in first line

define order of measured values

in list

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.

2 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

Standard settings:

"None" is assigned to the right SmartSens sensor

"Rotate" is assigned to the right SmartSens sensor

To adjust the brightness of the display:

1 Touch the button in the Brightness row.

2 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 ex-tends 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:

1 Touch the button in the Contrast row.

2 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.


To change the colors of the display:

1 Touch the button in the Color selection row.

2 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)

left and right SmartSens sensors

brightness

contrast

color selection

SmartSens Terminal


To change the beep volume:

1 Touch the button in the Sound row.

2 Set the volume of the beep to a value between 0% and 100% using the arrow keys (you can adjust it in steps of 10%). The sound is audible while pressing the arrow keys.


A screen saver can be set to appear after a certain time. When the screen saver is switched on, the state of the measuring cell is displayed in large letters on the screen. This can be useful, for example in a large laboratory room for recognizing the state of the measurement cell from afar.

To set the time after which the screen saver is switched on:

1 Touch the button in the Screen saver timeout row.

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

2 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.

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.

2 Using the virtual keypad, enter the time in minutes after which you want the dis-play 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.

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:

1 Touch Activate.

2 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).

beep volume

screen saver

display off timeout

touch adjustment

HP DSC 1 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




The terms "adjustment" and "calibration" are used in these operating instructions ac-cording to the following definitions:

calibration For the module in question, the determination of the actual deviation of measured values of reference sub-stances from the standard literature values by means of calibration measurements.

Reference substance: a substance that is suitable for the calibration measurement and whose thermoana-lytical property values are well established in the literature

adjustment Adapting the specific module parameters so that the measured values of the calibration measurements per-formed 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 in-struments 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 instru-ment parameters are changed.

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".

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 lim-its, 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.

GLP

calibration methods

CQ System Test

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 measure-ments 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 Soft-ware 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.

2 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:

3 Click File/Print Preview.

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



8.2 Calibration: the indium check

In contrast to the various calibration procedures, the so-called indium check is a nor-mal method with automatic evaluation of the result and conformity check. No instru-ment 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 tempera-ture of fusion and the heat of fusion of indium.

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.

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

chapter “Calibration” in the STARe Software Operating Instructions

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 sig-nal.

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 156.6 ±0.3 °C Heat flow 28.45 ±0.6 J/g

Zinc: Onset temperature 419.6 ±0.7 °C Heat flow 107.5 ±3.2 J/g

If the results of the check are not within the defined limits, the module must be ad-justed.

GLP

methods

Notice

limits

adjustment



8.3 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 instru-ment, 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 infor-mation. 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 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.

The results of the factory adjustment are stated in the document "CQ System Test be-fore Delivery" which is shipped with your HP DSC 1 module.

Notice

factory adjustment

CQ System Test



8.3.3 Adjusting the HP DSC 1

A number of methods to perform adjustments are available in the STARe Software da-tabase. These methods all include the characters "Calib" at the beginning of their names. The following methods are included in the STARe Software database for ver-sion 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 pur-pose 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 ad-justment at the melting point of zinc (419.5 °C) has been done properly.



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 adjust-ment within a particular temperature range.

To meet your own demands on accuracy, you can create your own method and per-form 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.

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

3 Prepare the sample crucible.

4 Set up an experiment in the Experiment Window (see the online Help in the Ex-periment Window for more details on this). Then start the experiment.

5 Open the measured heat flow curve in the Evaluation Window and display it ver-sus reference temperature by clicking TA/Curve vs. Reference Temp.

6 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.

manual adjustment

evaluation of a calibration measurement



7 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 evalua-tion on the selected curve section.

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

8 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 evalua-tion on the selected curve section.

9 Compare the results of the onset temperature and enthalpy of fusion with the val-ues stated in the document "CQ System Test before Delivery" which is shipped with your HP DSC 1 module.

HP DSC 1 Maintenance

0911 METTLER TOLEDO STARe-System 9-i

9 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



9 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 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

2 In the Experiment Window, select No Pan in the Select Sample Holder dialog box and name the method "bake out", for example.

3 Perform an indium check after this experiment is completed.

NOTICE

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.

2 Clean contaminated parts with acetone or ethanol.

3 Grease thread with a little silicone grease.

Assembly

5

4

3

2

1

1 Insert the gasket (1).

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

3 Insert slip ring (3).

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

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.

2 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, Acces-sories).

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 O-ring and the groove.

1 Change the O-rings of the cylinder cover and base (see chapter 12, Accessories).

2 Grease new O-rings with a little silicone grease, before inserting them.



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

3 Remove bracket and lift up jacket tube.

4 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 us-ing a hex key and change the inner and outer O-rings (see chapter 12, Accesso-ries).

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).

2 Close the INLET valve, open the OUTLET valve.

3 Lift up the bracket and remove the pressure cylinder cover.

4 Remove the bracket and lift up the jacket tube.

5 Remove the fixing screw of the pressure cylinder and lift up the pressure cylinder.

6 Inject solvent into the opening of the gas line (10) using a syringe (see figure be-low).

7 Mount the pressure cylinder and close.

8 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.



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 con-tinue with step (3).

1 2 3 4

5

6

7

8

9

10

11

12

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)

1

2

3

4 5

6

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.

1 Heating connection (left)

2 Pt100 connection (left)

3 Pt100 connection (right)

4 Heating connection (right)

5 Spacer column

6 Connection for short sensor wire

7 Connection for long sensor wire

8 Feedthrough for purge gas

9 Spacer column

10 Feedthrough for gas inlet and outlet (pressure)

11 Spring support for tension spring

12 Spacer column



9.1.6 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 incor-rect 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 re-placement of the DSC sensor must be carried out by a METTLER TOLEDO service en-gineer.

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.



9.2 Malfunctions

Malfunctions Causes Measures

No pressure buildup Inlet valve closed

Outlet valve open

Open valve

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)

Too little pressure buildup

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)



9.3 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 ac-cordance with DIN VDE 0702. The test should be executed by an authorized electri-cian 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.

Routine electrical safety test DIN VDE 0702 Test report Customer-Id.: Test report no.: Applicant: Agent:

Product / Serial number: Tested by: Test according: DIN VDE 0702; Routine electrical safety test Mains supply: 230V, 50Hz, 6A Class of product: Class I

Check by inspection: No damage on product Fuse rating Accessible parts of product are not hazardous live Product has no defects

Warning markings: 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-SEMKO-CBcert

Functionality:

Function of product

Function of protection devices ……………………………………………………….

……………………………………………………………

Testing / Measuring: Used test equipment:

Test point

Impedance of protective bonding (RSL)

Protective conductor / Equipotentiality (Ω)

Insulation (RISO)

(MΩ)

Leakage current (IEA)

(mA) Enclosure back side Test sample class I provided with power cord set (Cable and plug)

Limits: RSL > 0,3Ω RISO < 1MΩ IEA > 3,5mA

Routine test pass Test label affix on product Next test date: …………………..

The product is conform with the state of the art and technology.

The product is not conform with the state of the art and technology. Signatures: Tested by: Customer: ___________________________________________ _______________________________________________ Place Date Signature Place Date Signature

Test sample: Main switch ON!

Accessible parts / enclosure

Black outlet

Test equipment acc EN61557

HP DSC 1 Error Messages and Warnings


10 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 Smart-Sens 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.

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 er-ror 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 opera-tion of the HP DSC 1.

error message

Error Messages and Warnings HP DSC 1


1 Check the following list to find out possible causes for the warning and to decide on possible measures to overcome the problem.

2 Follow the instructions in the column “Measures”.

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

List of error messages

Error Cause Measures

4 Problems with the Pt100 temperature sensor (DSC cell) or with the electronics.

1 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 self-test.

2 Inform your local service engineer and report the error number code and the problem. Your feed-back helps us to eliminate problems in later ver-sions.

3 If the error occurs again, call your local service en-gineer.

5 AC supply voltage outside the acceptable range. Check the current voltage and compare it with the voltage selector setting at the rear panel. The volt-ages must match.

7 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 ºC

22 Furnace temperature is out of acceptable range See ERROR 4 Maximum temperature at 700 ºC



List of error messages (continued)


23 Problems with the Pt100 temperature sensor in the furnace (DSC cell) or with the electronics.

Report code and problem to your local service en-gineer. Maximum temperature at 808 ºC

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 ºC.

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 en-gineer.

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



List of error messages (continued)


128 to999 (except 850, see below)

Internal software error

exceptions: ERROR 400 and 401

- Software or hardware problems

1 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.

2 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.

3 If you cannot overcome the problem, call your local service engineer and report code and problem.

850 SmartSens Terminal defective Call your local service engineer and report code and problem.

10.2 List of warnings

Warnings inform you about a deviation from the expected behavior. In some cases you can just confirm the warning, and in other situations you must take action.

Each warning is assigned a one to two digit number code.

A warning does not interrupt a measurement (exceptions: warnings 10, 12 and 13).

1 Check the following list to find out possible causes for the warning and to decide on possible measures to overcome the problem.

2 Follow the instructions in the column “Measures”.

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



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.



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

- version mismatch

1 Click OK.

2 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.

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

58 to 61, 90

Problems with communication Check the connections between the module and the PC.

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

HP DSC 1 Specificatons


11 Specifications

TEMPERATURE DATA

All data applies to ambient environmental pressure

Cooling system: double-walled jacket with water cooling (22 °C)

Furnace power 400 W

Temperature range Water cooling 22 °C to 700 °C

Temperature accuracy1 ±0.2 K

Temperature precision1 ±0.02 K

Temperature reproducibility ±0.1 K

Heating time2 RT to 700 °C 0.1 MPa: 5 min

10 MPa: 5 min

Possible heating rates 0 to 100 K/min (at 700 °C) smallest increment 0.01 K/min

Cooling time water cooling from 700 °C to 100 °C

0.1 MPa: 11 min 10 MPa: 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

Measurement range at 100 °C ±350 mW ±160 mW

Resolution 0.04 µW 0.01 µW

Digital resolution 16.8 million points

SAMPLING

Sampling rate maximum 50 points/second

1 based on metal standards

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

Tube diameter

Safety rupture disk

Tube adapter

Gyrolok, outer diameter: 1/8 inch

Outer diameter: 1/8 inch

Stainless steel 1.4435 (AISI 316)

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

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

HP DSC 1 Accessories


12 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

Standard accessories ME order number

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

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 709301

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

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




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

Accessories HP DSC 1


Table 1. Crucible types

Crucible Type Lid Volume µL Centering pin No. of pieces ME order no.

Light aluminum crucible with 20 µL without 100 51119810

Standard aluminum crucible with 40 µL with 100 27331

Standard aluminum crucible with 40 µL without 100 26763

Standard aluminum crucible without 40 µL without 400 51119870

Standard aluminium lid 400 51119871

Pierced aluminium lid 50 µl 400 51140832

Aluminium lid for piercing 400 51119873

Medium aluminum crucible without 100 µL without 400 51119872

Tall aluminum crucible with 160 µL with 40 27811

Copper crucible without 40 µL with 100 51140407

Gold crucible with 40 µL with 6 27220

Small platinum crucible with 30 µL without 4 51119842

Medium platinum crucible with 70 µL without 4 51119654

Large platinum crucible with 150 µL without 4 24126

Medium Pressure crucible 1) with 2) 120 µL with 25 26929

Medium Pressure crucible 1) with 2) 120 µL without 25 29990

Disposable High Pressure crucible 3) with 40 µL with 25 26732

Disposable High Pressure crucible 3) with 40 µL without 25 26731

High pressure crucible with 30 µL without 3 51140404

High pressure gold plated crucible with 30 µL without 3 51140405

Seal for gold plated crucible 60 51140403

High Pressure crucible) with 270 µLl with 1 650072

High Pressure crucible) with 500 µL with 1 650066

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

HP DSC 1 Index

0911 METTLER TOLEDO STARe System 1

13 Index

A

Accessories, 12-1

accuracy, 8-6

Accuracy, 8-3

A/D converter, 2-8

adjustment, 8-1

Adjustment, 8-4

factory adjustment, 8-4

adjustment data, 4-9, 4-12

adjustment overview, 4-12

air cooling, 2-2

altitude, 4-2

analog/digital convertor, 2-8

artifacts, 4-1, 6-1

B

basic module, 2-3

Boersma principle, 2-9

C

calibration, 8-1

calibration method, 8-6

calibration methods

total calibration, 8-5

calibration methods

Single calibration, 8-5

Calibration methods, 8-3

calorimetric data, 11-1

centering, 6-5

Centering the sensor, 9-5

Check methods, 8-1, 8-2

cold junction temperature, 10-3

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

communication problem, 5-1

Control measurement, 8-3

connecting ports, 4-10

Connections tab, 4-10

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

Index HP DSC 1


E

electrical safety, 9-7, 11-3

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

electromagnetic disturbances, 4-1

electromagnetic fields, 4-1

EMC, 4-1

environmental conditions, 11-3

error code, 10-1

error message, 10-1

Ethernet

Ethernet cable, 2-7

Ethernet port, 4-5

Ethernet socket, 4-5

Ethernet TCP/IP connection, 2-2, 2-7

external connections, 2-5

F

factory adjustment, 8-4

fan, 2-2

FCC rules, 1-10

FRS5 sensor, 9-5

furnace lid, 10-2

furnace power, 11-1

Furnace Power Off, 2-6

fuses, 2-6, 4-4

G

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

H

hardware options, 1-2

heat flow adjustment data, 4-12

heat flux principle, 2-9

heating rates, 11-1

heating time, 11-1

High Sensitivity Sensor, 2-8

HP DSC 1

rear panel, 2-5

HSS7, 2-8

HSS7 sensor, 9-5

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

insert temperature, 7-6

Install Window, 4-8

installation, 4-1

intended use, 1-4

L

leveling screws, 2-3

line socket, 2-6

location, 4-1

HP DSC 1 Index


M

mains connections, 2-6

mains supply voltage, 4-4

Maintenance, 9-1

manufacturer, 1-1

manual adjustment, 8-6

Manual furnace lid, 2-4

measurement principle, 2-9

measurement preparation 6-5

measuring cell, 2-8, 2-9

Measuring cell, 2-4

mobile phone, 4-1

modular design, 1-2

module, 4-9

module data set, 4-9

Import Module, 4-9

module (in STARe Software), 4-9

module identification, 10-3

Module Control Window, 2-9

module dataset, 8-4

multiple sample pan, 8-5

N

needle valve, 13-229

number code, 10-1

O

Operational safety, 1-9

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

P (continued)

power supply, 4-4, 11-3

Power supply connections, 2-6

Power supply system, 4-4

power supply switch, 5-1

power switch, 2-10

preparing experiments 6-1

pressure cell, 11-2

pressure reduction valve, 4-3

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

Pt100 temperature, 10-3

Pt100 temperature sensor, 2-8, 10-2

purge gas, 2-8, 4-3

Purge gas flow rate, 4-3

protective gas, 4-3

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

purge gas inlet, 2-9

purge gas, 4-3, 2-9

R

radio interference regulations, 1-10

rating plate, 4-4

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

removing a module from a port, 4-11

resolution, 2-8

room conditions, 4-2

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

RESET, 6-8, 6-18

resolution, 11-1

Index HP DSC 1


S

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

Standby temperature, 6-8, 6-18

Start experiment, 6-8

start measurement, 6-14, 6-17

startup, 5-1

switched line socket, 2-10

STARe Software, 1-2, 4-7, 4-8

stabilized power supply unit, 4-4

start temperature, 7-6

state indicator, 7-6

State indicator, 7-3

state of TA module, 7-16

states of the measuring, 7-6

System Info button, 7-9

system information, 7-16

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

T (continued)

time constant, 2-2

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

V

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

W

warning number code, 10-4

warnings, 10-4

weighing table, 4-2

weight, 4-2

working area, 4-2

Z

zinc check, 8-1, 8-5

To protect your METTLER TOLEDO product’s 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.

© Mettler-Toledo AG 2009 ME-51710771A Printed in Switzerland 0911/2.12

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

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

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

*51710771* Printed on 100% Chlorine-free paper

Documents

HPDSC1