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Operating Instructions

DSC Apparatus

DSC 204 F1 Phoenix®


CONFORMITY DECLARATION
according to ISO/IEC Guide 22 and EN 45014

Manufacturer’s name: NETZSCH-Gerätebau GmbH


Manufacturer’s address: Wittelsbacherstraße 42
D-95100 Selb

declares that the product:

product name: DSC-Apparatus

model number: DSC 204 F1 Phoenix

conforms to the following product specifications:

EN 61326:1997+A1:1998+A2:2001
EN 61326 :1997 table 3
EN 61000-3-2:2000
EN 61000-3-3:1995
EN 61000-4-2:1995
EN 61000-4-3:1996
EN 61000-4-4:1995
EN 61000-4-5:1995
EN 61000-4-6:1996
EN 61000-4-8:1993
EN 61000-4-11:1994
EN 61010-1:2002+Corrigendum 1:2002+2:2004

We hereby certify that the product is in accordance with the EU Electromagnetic Compatibility
Directive 2004/108/EC and the EU Low Voltage Directive 2006/95/EC.

Selb, January 2011

NETZSCH
Gerätebau GmbH

(Dr. T. Denner)
Managing Director
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DSC 204 F1 Operating Instructions

Operating Instructions DSC 204 F1 Phoenix

Contents

Chapter I General Information

Chapter II Installation

Chapter III System Components

Chapter IV Operating the Instrument

Chapter V Appendix

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DSC 204 F1 Chapter I

General Informationen

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DSC 204 F1 General Informationen

Information

In the design of your instrument, we endeavor to take individual


solutions into account and to include these in the documentation.

However, in order to keep the scope of the technical documentation at


a reasonable level, we must limit the description to a standard model.

We ask for your understanding, if additional information particular to


your instrument is not included within the scope of the standard
instructions.
This additional information can always be found on the corresponding
information sheets.

Prior written permission from NETZSCH-Gerätebau GmbH is required


for electronic or mechanical duplication and distribution of these
instructions.

All technical data, instrument features and other information described


in these operating instructions are presented to the best of our
knowledge and in accordance with the technical standards of the
instrument at the time of printing.

We welcome any comments, suggestions or new ideas concerning the


instrument and these operating instructions. Please address them to:

NETZSCH-Gerätebau GmbH
Wittelsbacherstraße 42
D - 95100 SELB
Telephone: 09287/881- 0
Telefax: 09287/881- 144
E-Mail: at@netzsch.com
Internet: http://www.netzsch-thermal-analysis.com

Maintenance and service must be carried out by NETZSCH Customer


Service personnel.

A service contract is available for our customers.

This instruction manual is provided to give the customer information


on proper operation of the instrument. NETZSCH-Gerätebau GmbH
will accept no liability for damage resulting from improper use.

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DSC 204 F1 General Informationen

Notes on the Use of this Manual

In this manual, the symbols described below are used to simplify orientation.

NOTE

This sets particularly important information apart from the


rest of the text.

ATTENTION!

These instructions must be followed exactly to avoid injury


to the user and damage to the instrument.

This symbol refers to more detailed information which can


be found elsewhere, e.g. in the Software Manual.

The tools listed after this symbol are required for the
installation or modification of your instrument.

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DSC 204 F1 General Informationen

Basic Safety Information

State-of-the-Art Your instrument has been produced with state-of-the-art


technology and is safe to operate.

Authorized Any operation of the instrument other than as authorized


Operation requires consultation with NETZSCH.

Any use exceeding the (expanded) authorized operation is


considered unauthorized. The manufacturer will not be liable
for any damage resulting from such use.

Manufacturer's Authorized operation of the instrument includes compliance


Requirements with manufacturer's requirements regarding installation,
commissioning, operation and maintenance.

Training of Your instrument may only be operated and maintained by


Personnel authorized, trained and individually instructed personnel who
have been informed of possible sources of danger.

Responsibility Responsibility for commissioning, operation and maintenance


must be clearly defined and compliance must be ensured. The
resulting responsibilities can be clearly resolved under the
aspect of safety.

Unauthorized Access The operator must make sure that only trained personnel work
on the instrument.

Improper Operation Any type of operation which reduces the safety of the user
and the operability of the instrument should be avoided.

Unauthorized Unauthorized modifications and changes which effect the


Changes to the safety of the instrument are not permitted.
System

Obligation to Report The user is obligated to immediately report to the operator in


Changes to the charge any changes to the instrument which effect the safety
System of the system.

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DSC 204 F1 General Informationen

Maintenance The operator of the system must ensure that the instrument is
Obligation operated in perfect condition at all times.

Proper Set-up of the The operator must guarantee the openness and cleanliness of
Work Stations the work stations at the instrument through appropriate
instruction and inspections.

Shut-down For all maintenance work, the instrument must be switched off
and unplugged.

Removal of Protective devices may only be removed when the instrument


Protective Devices is switched off and unplugged. It is imperative that the
protective devices be replaced before starting the instrument.

Checks following After maintenance or repair work, a check should be made to


Maintenance or ensure that all protective devices are in place and operate
Repair Work properly. Only then should the instrument be started.

Industry-specific The operator must observe the relevant regulations and


Accident Prevention protective measures when handling the required gases. In
Regulations addition, possible reactions with the materials used must be
considered. At operating temperatures above 55°C, protective
gloves must be worn. In any case, the industry-specific and
local accident prevention regulations are also valid for the
instrument.

Disposal of Production materials are to be disposed of according to local


Production Materials regulations.

Maintenance or Products sent in for maintenance or repair should, to the


Repair extent possible, be free of harmful substances (e.g. radioactive,
toxic, caustic or microbiological materials). Otherwise, the
type of contamination must be declared. Products not
explicitly declared to be "free of harmful substances" will be
decontaminated at the expense of the sender.

Electrical Energy The unit may only be opened by qualified personnel, and only
Danger when it is turned off and disconnected from the power supply!
Any work on the electrical supply, electrical lines and electrical
components may only be carried out by qualified personnel
(electrical professionals).

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DSC 204 F1 General Informationen

Operating Using the Operation Manual, the operator should prepare


Instructions operating instructions which specify the actions and tasks
required for safe operation.

The operating instructions should be placed in a suitable


location in the work place and complied with by the
employees.

Gases Observe the relevant regulations and protective measures


when handling the required gases.

Consider possible reactions with the materials.

Warning signs should be hung in the appropriate places in


accordance with national and regional regulations.

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DSC 204 F1 General Informationen

Safety Regulations for Handling Liquid Nitrogen LN2

It is imperative that you observe the safety regulations for


handling nitrogen.

FIRE AND EXPLOSION HAZARDS


Neither gaseous nor liquid nitrogen are flammable and do not in
themselves constitute a fire or explosion risk. However, both
gaseous and liquid nitrogen are normally stored under pressure
and the storage vessels, whether gas containers or liquid tanks,
should not be located in areas where there is a high risk of fire or
where they may normally be exposed to excessive heat. Vessels
containing compressed gaseous nitrogen may rupture violently if
overheated as a result of exposure to fire.

Oil-lubricated compressors operated continuously on nitrogen


supply for a prolonged period should not be switched to air supply
without thorough cleaning. Otherwise there is a danger that
unoxidized pyrophoric deposits which may have formed in the
machine will explode violently on contact with compressed air.

At equal pressures, the boiling point of liquid nitrogen is lower


than that of liquid air. Air will condense on the external surfaces
of vessels or pipework containing liquid nitrogen at an equilibrium
pressure less than 1.5 bars absolute if the vessels are either not
lagged, or are lagged with a porous cellular-type insulator. The
liquid air produced can result in oxygen enrichment of the
atmosphere local to the equipment. Special precautions must
therefore be taken with regard to the insulation of the vessel
before any maintenance or repair work is started, particularly
where the use of open flames or other potential sources of
ignition is intended.

MATERIAL HAZARDS
Certain steels, such as carbon steel, and some other materials are
unsuitable for use at sub-zero temperatures because they lose
impact strength and become extremely brittle. Carbon steel
cannot be used safely at temperatures below -30°C (-20°F) and is
obviously unsuitable for use with liquid nitrogen. Materials
normally suitable for use at low temperatures are the austenitic
stainless steels, aluminum and copper and its alloys. In an area
where liquid nitrogen spillage can occur, care should be taken to
ensure that the liquid does not come into contact with vulnerable
steel structures and vehicle tires.

Care should be taken to ensure that liquid nitrogen and cold


nitrogen vapor are not trapped in a closed system without any
form of automatic pressure relief. Otherwise, pressures well in
excess of the equipment working pressure will be generated as the
system warms up, thus creating a possible rupture hazard.

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DSC 204 F1 General Informationen

HEALTH HAZARDS

Asphyxia
Nitrogen, although non-toxic, can constitute an asphyxation
hazard through the displacement of the oxygen in the
atmosphere. The potential for this type of hazard is significant
because of the widespread use of nitrogen as a purging or
blanketing gas in chemical, metallurgical, and other industrial
operations and because neither nitrogen gas nor oxygen depletion
are detectable by the normal human senses. Unless adequate
precautions are taken, persons can be exposed to oxygen-deficient
atmospheres if they enter equipment or areas which have
contained or have been purged with nitrogen.

Oxygen is required to support life and its volume concentration in


the atmosphere is normally 21%. At normal atmospheric pressure
(760 mm Hg), persons may be exposed to oxygen concentrations
of 18% by volume (equivalent to a partial pressure of 135 mm Hg),
or even less, without adverse effects. However, the response of
individuals to oxygen deprivation varies considerably. The
minimum oxygen content of breathing atmosphere should be 18%
by volume (at normal atmospheric pressure), but to ensure a wider
margin of operational safety, it is recommended that persons not
be exposed to atmospheres in which the oxygen concentration is,
or may become, less than 20% by volume.

Symptoms of oxygen deprivation, such as increased pulse and


breathing rate, fatigue and abnormal perceptions or responses,
may be apparent at an oxygen concentration of 16%.

Permanent brain damage or death may result from breathing


atmospheres containing less than 10% oxygen. Initial symptoms
include nausea, vomiting and gasping respiration. Persons
exposed to such atmospheres may be unable to help themselves or
warn others of their predicament. The symptoms are an
inadequate warning of the hazard.

BREATHING A PURE NITROGEN ATMOSPHERE WILL PRODUCE


IMMEDIATE LOSS OF CONSCIOUSNESS AND ALMOST IMMEDIATE
DEATH.

Cold burns
Liquid nitrogen and cold nitrogen vapors or gases can produce
effects on the skin similar to a burn. Unprotected parts of the
body coming into contact with uninsulated parts of the equipment
may also stick fast (because all available moisture is frozen) and
the flesh may be torn on separation.

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DSC 204 F1 General Informationen

Frostbite
Severe or prolonged exposure to cold nitrogen vapor and gas can
cause frostbite. Local pain usually gives warning of freezing, but
sometimes no pain is experienced. Frozen tissues are pain-free
and appear waxy with a pallid yellowish color. Thawing of the
frozen tissues can cause intense pain. Shock may also occur if the
frostbite is at all extensive.

Effects of cold on lungs


Prolonged breathing of extremely cold atmospheres may damage
the lungs.

Hypothermia
Low environmental temperatures can cause hypothermia and all
persons at risk should wear warm clothing. Hypothermia is
possible in any environmental temperature below 10°C (50°F), but
susceptibility depends on time, temperature and the individual.
Older persons are more likely to be affected. Individuals suffering
from hypothermia may find their physical and mental reactions are
adversely affected.

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DSC 204 F1 General Informationen

PRECAUTIONS

Operations and maintenance


It is essential that operations involving the use of gaseous or liquid
nitrogen, particularly where large quantities are used, are
conducted in well-ventilated areas to prevent the formation of
oxygen-deficient atmospheres.

Ideally, nitrogen should be vented into the open air well away
from areas frequented by personnel. Nitrogen should NEVER be
released or vented in enclosed areas or buildings where the
ventilation is inadequate.

Before entering areas, vessels or other equipment for maintenance


or other purposes in which the atmosphere is, or may become
deficient in oxygen, action should be taken to make the
equipment safe. Preparatory work will include equipment
isolation from hazardous processes, purging and continued
ventilation with air as appropriate. Equipment in service with
flammable gases should be purged with nitrogen prior to purging
with air to avoid the formation of flammable mixtures.
NEVER USE OXYGEN AS A SUBSTITUTE FOR AIR AS A PURGING
MEDIUM. Prior to entry, the atmospheres should be tested with a
portable oxygen analyzer (calibrated before use) to ensure that
the oxygen lies between 20% and 22% by volume. The use of a
safety work permit system is strongly recommended (Note: The
latter two recommendations need not apply when entering a
Cryo-Guard vehicle for normal loading or unloading purposes. For
details see Cryo-Guard Drivers Instruction Manual).

It should be recognized that although nitrogen is slightly lighter


than air at equal temperatures, liquid nitrogen and cold nitrogen
vapor are denser than air and can accumulate in low-lying areas
such as pits and trenches. Where large spills of liquid nitrogen
occur, a fog is formed in the vicinity of the spill caused by the
condensation of water vapor in the surrounding air. The fog, in
addition to severely reducing visibility, may contain oxygen
concentrations appreciably lower than those of air, thus
presenting a local asphyxation hazard.

IF IT IS NECESSARY FOR A PERSON TO ENTER AN OXYGEN-


DEFICIENT ATMOSPHERE FOR MAINTENANCE OR OTHER
PURPOSES, IT IS ESSENTIAL THAT HE/SHE WEAR, AND BE TRAINED
IN THE USE OF, A SELF-CONTAINED BREATHING APPARATUS.

Persons entering an oxygen-deficient area are advised to wear a


safety belt with a manned safety line attached. Standby personnel
should have ready access to self-contained breathing apparatus
should emergency assistance be required.

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DSC 204 F1 General Informationen

Personnel protection
It is recommended that persons handling gas containers wear
safety glasses, safety footwear and clean, sturdy gloves.

Persons handling equipment in service with liquid nitrogen should


wear protective face shields, loose fitting leather or insulated
gauntlets.

EMERGENCIES
In the event of accident or emergency, the instructions below
should be implemented without delay. After emergency action
has been taken, contact your nearest Air Products PLC Sales Office
(see list at the back) for further advice.

Asphyxiation
Persons showing symptoms of oxygen deprivation should be
moved immediately to a normal atmosphere. Persons who are
unconscious or not breathing must receive immediate first aid.
Medical assistance should be summoned without delay and first
aid measures include inspection of the victim's airway for
obstruction, artificial respiration and simultaneous administration
of oxygen. The victim should be kept warm and quiet.

It is important to note that personnel carrying out rescue


operations must minimize the risk to themselves. A RESCUER
SHOULD NOT ATTEMPT TO ENTER AN OXYGEN-DEFICIENT
ATMOSPHERE WITHOUT USING SUITABLE SELF-CONTAINED
BREATHING APPARATUS; OTHERWISE HE MAY HIMSELF BE
OVERCOME. Many double fatalities have occurred in industry as a
result of personnel who, with the best intentions but without
proper breathing apparatus and equipment, have entered an
oxygen-deficient atmosphere in an attempt to rescue a colleague.
Treatment of cold burns and frostbite
Cold burns should receive medical attention as quickly as possible.
However, such injuries are not an everyday occurrence and
doctors, hospital staff or on-site first aid personnel may not be
aware of the basic methods of treatment. The following notes
describe the first aid treatment and recommended advice for
further treatment to be given by a medical practitioner or a
hospital.
First Aid
In severe cases, summon medical attention at once. Flush affected
areas of skin with copious quantities of tepid water to reduce
freezing of tissue. Loosen any clothing that may restrict blood
circulation. Move the victim to a warm place but not to a hot
environment and do not apply direct heat to the affected areas.
Every effort should be made to protect the frozen areas from
infection and further injury. Dry, sterile bulky dressings may be
used but should not be applied so tightly that blood circulation is
restricted.

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DSC 204 F1 General Informationen

Treatment by medical practitioner or hospital


a) Remove any clothing that may constrict the circulation to the
frozen area. Remove patient to sick bay or hospital.
b) Immediately place the part of the body exposed to the
cryogenic material in a water bath which has a temperature of not
less than 40°C (104°F) but not more than 45°C (113°F). (See below
for exceptions to this recommendation.) NEVER USE DRY HEAT OR
HOT WATER. Temperatures in excess of 45°C will superimpose a
burn upon the frozen tissue.
c) If there has been massive exposure to the super-cooled material
so that the general body temperature is lowered, the patient must
be re-warmed gradually. Shock may occur during rewarming,
especially if this is rapid.
d) Frozen tissues are pain-free and appear waxy with a pallid
yellowish color. They become painful, swollen and very prone to
infection when thawed. Therefore, do not re-warm rapidly if the
accident occurs in the field and the patient cannot be transported
to a hospital immediately. Thawing may take from 15 to 60
minutes and should be continued until the blue, pale color of the
skin turns to pink or red. Morphine or some other potent
analgesic is required to control the pain during thawing and
should be administered under professional medical supervision.
e) If the frozen part of the body has thawed by the time medical
attention has been obtained, do not re-warm. Under these
circumstances, cover the area with dry sterile dressings with a large
bulky protective covering.
Administer a tetanus booster after hospitalization.
Hypothermia
Persons suspected to be suffering from hypothermia should be
wrapped in blankets and moved to a warm place. Slow
restoration of temperature is necessary and forms of locally
applied heat should not be used. Summon medical attention.
Fire fighting
Nitrogen is not flammable and no special fire fighting precautions
or equipment are needed. If an outbreak of fire occurs in the
vicinity of nitrogen storage equipment, the local fire department
should be summoned at once. Unless vessels containing
compressed gaseous nitrogen can be removed safely to an
unaffected area, every effort should be made to keep them cool
by spraying them with large quantities of water.

Liquid nitrogen spillage


If large spills of liquid nitrogen occur, large quantities of water
should be used to increase the rate of liquid vaporization.

Vehicles involved in a heavy liquid spillage should not be moved as


the tires may be frozen to the ground and the rubber will be
brittle.

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DSC 204 F1 General Informationen

GAS CONTAINERS
The content of the container is primarily identified by a label
attached to the container shoulder and secondarily by the color of
the container. The Air Products identification colors for containers
containing nitrogen are:
Body: French gray; shoulder and guard: black (BS 349: 1973)

The following practices are recommended for safe handling and


storage of high-pressure gases including nitrogen containers.

General
− Only trained persons should handle compressed gases.

− Observe all regulations and local requirements regarding the


storage of containers.

− Do not remove or deface labels provided by the supplier for the


identification of the container contents.

− Ascertain the identity of the gas before using it.

− Know and understand the properties and hazards associated


with each gas before using it.

− Establish and implement plans to cover any emergency


situations that might arise.

− When doubt exists as to the correct handling procedure for a


particular gas, contact the supplier.

Handling and Use


− Wear stout gloves.

− Never lift a container by the cap or guard unless the supplier


states it is designed for that purpose.

− Use a trolley or other suitable device or technique for


transporting heavy containers, even for a short distance.

− Leave valve protection caps or guards (where provided) in place


until the container has been secured against a wall or bench or
placed in a stand and is ready for use.

− Where necessary, wear suitable eye and face protection. The


choice between safety glasses, chemical goggles, or full face
shield will depend on the pressure and nature of the gas being
used.

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Storage and handling


− Where necessary for toxic gases, see that self-contained positive
pressure breathing apparatus or a full face air line respirator is
available in the vicinity of the working area.

− Check for gas leaks using a suitable method. Flammable and


toxic gas monitors are available. Where a gas is toxic, check
special procedures specified by the supplier.

− Ascertain that an adequate supply of water is available for first


aid, fire fighting, or dilution of corrosive material in the event
of leakage.

− Employ suitable pressure regulating devices on all containers


when the gas is being emitted to systems with a lower pressure
rating than that of the container.

− Before connecting the container for use, ensure that back feed
from the system into the container is prevented.

− Ascertain that all electrical systems in the area are suitable for
service with each gas.

− Never use direct flame or electrical heating devices to raise the


pressure of a container. Containers should not be subjected to
temperatures above 45°C.

− Never re-compress a gas or a gas mixture from a container


without consulting the supplier.

− Never attempt to transfer gases from one container to another


unless expressly agreed beforehand with the supplier.

− Do not attempt to increase liquid draw-off rate by pressurizing


the container without first checking with the supplier.

− Do not use containers as rollers or supports, or for any other


purpose than to contain the gas as supplied.

− Never permit oil, grease or other readily combustible substances


to come into contact with valves of containers containing
oxygen or other oxidants.

− Keep container valve outlets clean and free of contaminants,


particularly oil and water.

− Do not subject containers to abnormal mechanical shocks which


may cause damage to their valves or safety relief devices.

− Never attempt to repair or modify container valves or safety


relief devices. Damaged valves should be reported immediately
to the supplier.
− Close the container valve whenever gas is not required, even if
container is still connected to equipment.

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DSC 204 F1 General Informationen

− Replace outlet caps or plugs and container caps (where


provided) as soon as container is disconnected from equipment.
Storage
− Containers should be stored in a well-ventilated area. Some
gases will require a specially built area.
− Store containers in a location free of fire risk and away from
sources of heat and ignition. Designation as a "No smoking"
area may be desirable.
− The storage area should be kept clear and access should be
restricted to authorized personnel only. The area should be
clearly marked as a storage area and appropriate hazard
warning signs displayed (flammable, toxic, radio active etc.).
− Containers in storage should be properly secured to prevent
toppling or rolling.
− Vertical storage is recommended where the container is so
designed.
− Container valves should be tightly closed and, where
appropriate, valve outlets should be capped or plugged.
− Container valve protection guard or cap should be in place and
properly secured.
− Protect containers stored in the open against rusting and
weather extremes. Containers should not be stored in
conditions likely to encourage corrosion.
− Store full and empty containers separately and arrange full
containers so that the oldest stock is used first.
− Gas containers should be segregated in the storage area
according to the various categories (toxic, flammable, oxidant,
etc.).
− The amounts of flammable or toxic gases in storage should be
kept to a minimum.
− Flammable gases should be stored away from other
combustible materials.
− Containers held in storage should be periodically checked for
general condition and leakage.

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LIQUID STORAGE CONTAINERS


− Liquid nitrogen is stored and transported either in purpose
built storage tanks or dewar flasks. Storage quantities vary
from a few liters for dewar flasks to several thousands of liters
for storage tanks. The storage tanks are pressurized, insulated
containers which are installed in accordance with established
codes of practice. All liquid storage areas should be kept clean
and free of flammable materials.
− Unlike a liquid nitrogen tank, a vaccum-jacketed dewar flask is
essentially a non-pressurized container.
− Recommendations for handling and storage are as follows:
− The protective caps on dewar flask fill/ drain outlets should be
kept closed when not in use to prevent contamination and
ensure that blockage by frost does not occur. Check caps
regularly to ensure that they have not become sealed by frost
accumulating on the surface. Formation of frost may be
removed by warming gently with air.
− DO NOT USE SOURCES OF EXCESSIVE HEAT SUCH AS STEAM OR
OPEN FLAMES.
− Dewar flasks should be stored in well-ventilated areas where
they are protected against weather extremes, particularly heavy
rain.

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DSC 204 F1 Chapter II

Installation

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DSC 204 F1 Installation

Contents

INSTALLATION .............................................................................................1
PACKING AND DELIVERY ............................................................................1
LOCATION REQUIREMENTS ..........................................................................2
INSTALLATION SCHEMATIC ..........................................................................3
CONNECTING THE SYSTEM COMPONENTS ........................................................6
CONNECTING THE COMPUTER SYSTEM .................................................................. 6
IMPORTANT NOTES FOR SOFTWARE INSTALLATION .............................................. 7
CONNECTING THE CC 200 F1 ............................................................................. 8
CONNECTING THE CC 300 F1 ............................................................................. 9
CONNECTING THE LN2 COOLER (MAGNETIC VALVE CONTROLLED) 6.351.24 OR 25 .. 10
CONNECTING THE LINEAR SMALL COMPRESSOR .................................................... 11
CONNECTING THE ON-OFF VALVE KIT FOR COMPRESSED AIR COOLING ...................... 12
CONNECTING THE COOLING DEVICE FOR PRESSURIZED AIR ...................................... 13
CONNECTING THE INTRACOOLER ....................................................................... 14
CONNECTING THE GAS SUPPLY .......................................................................... 15

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DSC 204 F1 Installation

Installation

In most cases, your DSC 204 F1 is set up and commissioned by


one of our customer service engineers.

If you would like to set up your instrument yourself, please read


the following sections.

Packing and Delivery

We deliver all components in separate cartons. The


measuring unit, electronics, computer system etc. are packed
in form-molded foam to protect against damage during
transport.

We recommend keeping the original cartons. Should repairs


or an extension of the system become necessary, the cartons
can be reused, thus ensuring a relatively safe return to the
manufacturer.

Prior to shipping, we carefully test all components of the


system for mechanical and electrical operability.

After unpacking, please check all delivered components for


possible transport damage and compare the individual items
against the delivery note supplied.

Should an item be missing, please contact us immediately.

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DSC 204 F1 Installation

Location requirements

Select the optimal component arrangement for the space


you have available.

The location of your instrument must meet the


following requirements:

constant temperature conditions (room temperature) to the


extent possible
no direct sunlight on the instruments
dust-free environment to the extent possible

measuring system A stable, shock-absorbent table with a working surface of


approx. 2 m x 1 m is required for the measuring device
(measuring cell, computer, printer).

LN2 cooling system The LN2 cooling system requires 0.5 m x 0.5 m space. The
cooling system should be placed beside the table.

An installation schematic of the measuring system follows


on the next page.

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DSC 204 F1 Installation

Installation schematic

580 250 470 460


depth 530 depth 540 depth 450 depth 400

520
360
250

300

measuring part DSC 204 F1 balance CP2P computer printer table

electrical. connections:
230V, 5A
electrical. connections:
230V, 6A
measures in "mm"

580 150
depth 530 depth 350

230
250

de war pre ssur e

pre ssu re re lie f


CC 200 F1
powe r

de w ar pr es sur e
measuring part DSC 204 F1 Controller table
pre ssu re re lie f
CC 200 F1
powe r CC 200 F1

measures in "mm"
1030

825

Ø 520 Ø 390

storage vessel 60L (LN2) storage vessel 26L (LN2)


with coolant supply device with coolant supply device

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DSC 204 F1 Installation

580
depth 530

250
measuring part DSC 204 F1 table

measures in "mm"
1050

900

Ø 520 Ø 390

storage vessel 60L (LN2) storage vessel 26L (LN2)


with coolant supply device with coolant supply device

580
depth 530
250

measuring part DSC 204 F1 table

measures in "mm"
600

floor
500
depth 700

compressor cooling device


electrical connection:
1 x 230V, 16 A

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DSC 204 F1 Installation

580
depth 530 measures in "mm"

250

measuring part DSC 204 F1


table

260
depth 180
200

linear small compressor


floor

Figure 1: Installation schematics DSC 204 F1

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DSC 204 F1 Installation

Connecting the system components

Requirements
The detailed requirements for installation are given in the enclosed installation schematic.

Connecting the computer system

PC
USB

115V/T6,3A purge 1
230V/T4A

AC line
on/off purge 2

AC input
USB
50/60Hz
protective

optional
fuse LN 2 cooling
115V/T4A
230V/T2A CC 300

mechanical cooling

air cooling
LN 2 cooling

measuring part DSC 204 F1 (rear)

power supply

Figure 2: connecting computer system

For connecting the computer system, see also the technical documentation
of the computer manufacturer.

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DSC 204 F1 Installation

Important notes for Software installation

Your DSC 204 F1 instrument communicates with the PC using the USB interface of the PC.
This requires the installation of suitable drivers delivered together with the Proteus
Software.

→ Before initially connecting the DSC 204 F1 the Proteus Software must be installed first.
For details of installation, please read chapter 3 and chapter 4.2 in the document
“NETZSCH Proteus Software”.

Notes:

Do not use USB hubs (connect your DSC 204 F1 directly to the PC).

Use the original USB cable delivered from NETZSCH.

If you accidentally change the USB interface on the PC the Plug&Play procedure will
start again to install the drivers for this interface. Please note that this procedure has
to be done for any “not yet” connected USB interface.

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Dewar Head

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DSC 204 F1
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GN2/LN2 pressure relief

Figure 3: connecting CC 200 F1


115V/T6,3A purge 1
230V/T4A

dewar heater

J:\DSC204F1\doc-files\englisch\CHAPTER2.DOC
AC line
on/off
Connecting the CC 200 F1

purge 2
Dewargefäß
AC input
50/60Hz USB
cooling gas
AC line controller protective
230V/115V
3,15AT optional
6,3AT
fuse LN 2 cooling
115V/T4A
dewar head 230V/T2A CC 300

mechanical cooling

(see chapter I and chapter III)!


air cooling
LN2 cooling
Installation

LN2 inlet

control electronis measuring part DSC 204 F1 (rear)


CC 200 F1 (rear)

power
supply

LN2 outlet
LN2 inlet

Please pay attention to all safety regulations for handling liquid nitrogen

8
Dewar Head

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DSC 204 F1

GN2/LN2 pressure relief


R

power
supply

Figure 4: connecting CC 300 F1


115V/T6,3A purge 1
230V/T4A

J:\DSC204F1\doc-files\englisch\CHAPTER2.DOC
AC line
on/off
purge 2
Connecting the CC 300 F1

AC input
Dewargefäß
50/60Hz USB
protective

optional
fuse LN 2 cooling
115V/T4A
230V/T2A CC 300

mechanical cooling

(see chapter I and chapter III)!


air cooling
LN2 cooling
Installation

LN2 inlet

measuring part DSC 204 F1 (rear)

LN2 outlet
LN2 inlet

Please pay attention to all safety regulations for handling liquid nitrogen

9
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DSC 204 F1 Installation

Connecting the LN2 cooler (magnetic valve controlled)


6.351.24 or 25

LN2 inlet

LN2 inlet
LN2 outlet
protective
purge 1

purge 2

measuring part DSC 204 F1 (rear)


USB

optional

mechanical cooling

LN2 cooling
CC 300

(forced N2, 0.5 bar)


gas supply
LN2 cooling

air cooling
115V/T6,3A

115V/T4A
230V/T2A
230V/T4A

AC input
50/60Hz
AC line
on/off

fuse

Figure 5: connecting the LN2 cooler with magnetic valve

Please pay attention to all safety regulations for handling liquid nitrogen
(see chapter I and chapter III)!

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115V/T6,3A purge 1
230V/T4A
DSC 204 F1
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AC line
on/off purge 2

AC input
USB
50/60Hz
protective

optional
fuse LN2 cooling
115V/T4A
CC 300
230V/T2A

mechanical cooling hose connection (air)


air cooling
LN2 cooling

J:\DSC204F1\doc-files\englisch\CHAPTER2.DOC
measuring part DSC 204 F1 (rear)
power supply

Figure 6: connecting the linear small compressor


linear small
Installation

compressor
Connecting the linear small compressor

outlet
inlet

11
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DSC 204 F1 Installation

Connecting the on-off valve kit for compressed air cooling

input pressure max. 2 bar absolute (1 bar overpressure)

(compressed air)
hose connection

inlet
outlet
protective
purge 1

purge 2

measuring part DSC 204 F1 (rear)


USB

optional

mechanical cooling

LN 2 cooling
CC 300

power supply
LN 2 cooling

air cooling
115V/T6,3A

115V/T4A
230V/T2A
230V/T4A

AC input
50/60Hz
AC line
on/off

fuse

Figure 7: connecting the on-off valve kit for compressed air cooling

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DSC 204 F1 Installation

Connecting the cooling device for pressurized air

For minimum temperature of 0°C or below (dependent on air pressure). Includes cold air
generator and software controlled magnetic valve.

Requirements at customers site:


Pressurized air, throughput approx. 200 l/min, min. pressure 6 bar, max. pressure 10 bar,
oil-free, dry (pressure dew point <5 °C), filtered (25 µm or better)
hot air
outlet

pressurized
air inlet
cooling air
outlet

inlet
outlet
protective
purge 1

purge 2

The outlet must always be open!


ATTENTION!
measuring part DSC 204 F1 (rear)
USB

optional

mechanical cooling

LN2 cooling
CC 300

!
power supply
LN2 cooling

air cooling
115V/T6,3A

115V/T4A
230V/T2A
230V/T4A

AC input
50/60Hz
AC line
on/off

fuse

Figure 8: connecting the cooling device for pressurized air

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DSC 204 F1 Installation

Connecting the Intracooler

Intracooler (rear)

power supply
protective
purge 1

purge 2

measuring part DSC 204 F1 (rear)


USB

optional

mechanical cooling

LN2 cooling
CC 300
LN 2 cooling

air cooling
115V/T6,3A

115V/T4A
230V/T2A
230V/T4A

AC input
50/60Hz
AC line
on/off

fuse

Figure 9: connecting the intracooler

For connecting the cooling compressor (intracooler), see also the technical
documentation of the NETZSCH cooling compressor.

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DSC 204 F1 Installation

Connecting the gas supply

Figure 10: connecting the gas supply

The gas supply unit (e.g. gas bottle) should be equipped with a gas pressure reducer.
The recommended input pressure at the gas inlet of the instrument is 0.5 bar overpressure.

Max. input pressure 1.0 bar overpressure!


A higher input pressure than 1.0 bar overpressure might damage the MFC.
Therefore, the input pressure should be adjusted at an appropriate gas
pressure reducer of the gas supply unit before the gas hoses are connected.
The gas hoses should be disconnected when the maximum pressure might be
exceeded, for example after an exchange of the gas bottle and reinstallation
of the gas pressure reducer.
The mass flow controllers are not designed for the use of corrosive,
flammable or reducing gases!
See also all recommendations for the use of reactive purge gases (chapter IV)!

After setting the gas pressure reducer to the recommended value of 0.5 bar overpressure
connect the gas hoses for purge 1, purge 2, and protective at the rear of the instrument.
The gas flow for all gases can be adjusted by means of MFCs via the software.

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DSC 204 F1 Chapter III

System Components

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DSC 204 F1 System Components

Contents

MEASURING UNIT ........................................................................................ 1


MEASURING UNIT (WITH AUTOMATIC COVER HOIST) ............................................ 1
OPERATING PRINCIPLE .................................................................................. 2
FRONT PANEL OF THE MEASURING UNIT.......................................................... 4
OPERATING ELEMENTS (ONLY INSTRUMENTS WITH AUTOMATIC COVER HOIST) ............. 4

CONTROL DISPLAY............................................................................................. 4

REAR OF THE MEASURING UNIT .................................................................... 5


COOLING SYSTEMS....................................................................................... 6
NITROGEN COOLING - CC 200 F1 ................................................................ 6
DEWAR HEAD ............................................................................................... 8
FRONT PANEL ............................................................................................. 8

BACK PANEL............................................................................................... 9

NITROGEN COOLING - CC 300 F1 .............................................................. 10


DEWAR HEAD ............................................................................................. 11
FRONT PANEL ........................................................................................... 11

BACK PANEL............................................................................................. 12

LN2 COOLER (MAGNETIC VALVE CONTROLLED) 6.351.24 OR 25 ..................... 13


SAFE USE OF LIQUID NITROGEN LN2 .......................................................... 14
SAFETY REGULATIONS FOR LN2 DEWAR VESSELS WITH NETZSCH DEWAR
HEAD ................................................................................................... 14
PRECAUTIONS IN THE EVENT OF OPERATING FAULTS....................................... 15
AIR COOLING ......................................................................................... 16
LINEAR SMALL COMPRESSOR ............................................................................. 16
ON-OFF VALVE KIT FOR COMPRESSED AIR COOLING .............................................. 17
COOLING DEVICE FOR PRESSURIZED AIR............................................................... 17
MECHANICAL COOLING – INTRACOOLER....................................................... 17
ACCESSORIES ........................................................................................... 18
SEALING PRESS ...................................................................................... 18

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DSC 204 F1 System Components

Measuring unit

height
250

depth
530
width
580

Measuring unit (with automatic cover hoist)

height
300

depth
530
width
580

Figure 1: DSC 204 F1 measuring units

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DSC 204 F1 System Components

Operating principle

gas outlet

cooling air

protective gas

reference
sample
heat flux sensor
furnace block

purge gas

circulating cooling

LN2-/GN2-cooling

Figure 2: DSC 204 F1 measuring cell (schematic)

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DSC 204 F1 System Components

Furnace • silver block

• miniature jacketed heater

• furnace temperature is measured by a thermocouple which is


integrated into the furnace wall

Sample • closed with two silver lids


chamber
• the measuring cell is sealed with the instrument lid

Cooling • nitrogen cooling (liquid or gaseous)

• air cooling - linear small compressor


- on-off valve kit for compressed air cooling
- cooling device for pressurized air

• cooling compressor (intracooler)

Sensor • Measurement of the temperature difference between sample and


reference by heat flux sensor.

• Heat flux sensor with support plate for sample and reference
crucible.

• Measurement of the sample temperature underside the heat flux


sensor.

Purge gas • two separate purge gas inlets (sample chamber),


connected via a tee piece

• gas change during measurement possible

• protective gas (furnace jacket)

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DSC 204 F1 System Components

Front panel of the measuring unit

operating elements

measuring unit

control display safety key

Figure 3: front panel

operating elements (only instruments with automatic cover hoist)


label function
"open"+"safety key" opens the cover of the measuring unit
"close"+"safety key" closes the cover of the measuring unit

control display
label function
purge 1 control LED: purge gas 1 (sample chamber) "on/off"
purge 2 control LED: purge gas 2 (sample chamber) "on/off"
protective control LED: protective gas purging "on/off"
power green LED on: instrument is switched on
orange LED on: measurement is running
The gases "protective", "purge 1" und "purge 2" can be activated
via the software (see Help system Software).

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DSC 204 F1 System Components

Rear of the measuring unit

115V/T6,3A
230V/T4A
purge 1 13
AC line
2 on/off purge 2

AC input
USB
50/60Hz
protective

optional
fuse LN2 cooling
115V/T4A
230V/T2A CC 300

mechanical cooling
12
air cooling
LN2 cooling

3 4 5 6 7 8 9 10 11

Figure 4: rear of the measuring unit

No. label function

1 115V/T4A; 230V/T2A mains fuses

2 AC line on/off power switch: instrument "on/off"

3 AC input 50/60Hz power connection 230 (115) V

4 air cooling plug connection for air cooling

5 LN2 cooling connection: magnetic valve LN2 cooling system

6 USB plug connection: computer system

7 mechanical cooling plug connection: Intracooler

8 LN2 cooling plug connection: CC 200 F1

9 CC 300 plug connection: CC 300 F1

10 optional plug connection: UV lamp

11 purge1 plug-in connection: purge gas 1 (sample chamber)

11 purge 2 plug-in connection: purge gas 2 (sample chamber)

11 protective plug-in connection: protective gas 1 (jacket)

12 connection: cooling agent outlet (rear connection)

13 connection: cooling agent inlet (front connection)

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DSC 204 F1 System Components

Cooling systems

®
The DSC 204 F1 Phoenix can be used with different cooling possibilities:

- nitrogen cooling (liquid or gaseous)


- air cooling: air compressor or electrovalve (pressure air)
- mechanical cooling (intracooler)

Operations on the cooling device requires instructed NETZSCH staff.

Nitrogen Cooling - CC 200 F1

liquid nitrogen
temperature range: 700°C to -180°C
quickest possible cooling time from 600°C to -170°C: >15 min
linear cooling: - with 100 K/min to 380°C
- with 40 K/min to -60°C
- with 20 K/min to -100°C
- with 10 K/min to -150°C

gaseous nitrogen (gaseous nitrogen)


temperature range: 700°C to -100°C
quickest possible cooling time from 600°C to -100°C: 24 min
linear cooling: - with 20 K/min to -20°C
- with 10 K/min to -65°C
- with 5 K/min to -90°C

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DSC 204 F1 System Components

Dewar vessel with centering and


clamping rings (optional)
TR 60:
volume: 60 l
height: 1030 mm
outer diameter: 520 mm
TR 26:
volume: 26 l
Dewar head with supply system height: 825 mm
outer diameter: 390 mm

CC 200 F1 control electronics

For connecting the components see chapter II "Installation"!

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DSC 204 F1 System Components

Dewar head

front panel

working pressure:
0.5 bar

Figure 5: front panel dewar head CC 200 F1

dewar pressure Manometer, indicates the pressure in the Dewar vessel.

pressure relief When actuated, the outlet valve is opened.


The pressure in the Dewar vessel is reduced.
Can only be used when the supply system is connected to the
control electronics.

power green LED on: dewar head is connected to the control electronics

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DSC 204 F1 System Components

back panel

1 2

Figure 6: back panel dewar head CC 200 F1

connection for dewar heater to the control electronics


1
(see chapter II)

connection for dewar head to the control electronics


2
(see chapter II)

GN2/LN2 Nitrogen outlet, connect to the measuring unit

pressure relief outlet for pressure reduction

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DSC 204 F1 System Components

Nitrogen Cooling - CC 300 F1

dewar vessel with centering and


clamping rings (optional)

TR 60:
volume: 60 l
height: 1050 mm
outer diameter: 520 mm
TR 26:
volume: 26 l
height: 900 mm
outer diameter: 390 mm

dewar head with supply system

For connecting the components see chapter II "Installation"!

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DSC 204 F1 System Components

Dewar head

front panel

working pressure:
0.5 bar

Figure 7: front panel dewar head CC 300 F1

pressure relief When actuated, the outlet valve is opened.


The pressure in the dewar vessel is reduced.
Can only be used when the dewar head is switched on.

power green LED on: dewar head is switched on

dewar pressure Manometer, indicates the pressure in the dewar vessel.

working pressure: 0.5 bar

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DSC 204 F1 System Components

back panel

1
2

Figure 8: back panel dewar head CC 300 F1

connection to the DSC instrument: CC 300


1
(see chapter II)

power switch (instrument "on/off")/power supply (AC input)/


2 mains fuses

(see chapter II)

3 pressure relief valve

GN2/LN2 nitrogen outlet, connect to the measuring unit

pressure relief outlet for pressure reduction

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DSC 204 F1 System Components

LN2 cooler (magnetic valve controlled) 6.351.24 or 25

How to connect the LN2 cooler? See chapter II – Installation

front view

2
3
1
4

LN2 cooler; manually controlled supply system, 1 - gas supply (forced N2, 0.5 bar)
operated with compressed gas (N2), 2 - manometer
software-controlled magnetic valve for 3 - magnetic valve
switching the LN2 supply, 4 - gas inlet to measuring unit
with LN2 storage vessel, content 26 l 5 - dewar vessel
6 - shut-off valve (pressure generation)
7 - shut off valve (pressure release)

top view
6 7

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DSC 204 F1 System Components

Safe Use of Liquid Nitrogen LN2

The temperature of liquid nitrogen is -196°C.

You must never touch objects which have been in contact with
liquid nitrogen with your bare hands.
Always wear special gloves and visors when handling liquid
nitrogen.

Please pay attention to all information for handling of LN2


described in chapter I.

Safety Regulations for LN2 Dewar Vessels with NETZSCH Dewar Head

The low pressure vessels are limited to a maximum working pressure of 0.5 bar according
to the pressure equipment directive.

The low pressure vessels with dewar head are designed in such a way that a multilevel
safety circuit prevents possible hazards for the operator when using LN2.
These safety features are:

1. Dewar heating for a controlled pressurization of the vessel incl. pressure relief valve
(opening pressure 0.5 bar) to reduce overpressure inside the vessel.

2. Sufficient big outlet on the pressure relief valve to reduce an overpressure for the case
that the dewar heating control is out of operation and the heating is permanently on.

ATTENTION!
• In order to avoid damages to the dewar head it is forbidden to use hot air instruments
for deicing the components!
• Under no circumstances should the dewar vessel be opened until the pressure has
completely dissipated! Monitor the pressure reduction.
• Escaping liquid nitrogen can lead to serious injuries!
• When removing the supply system from the dewar vessel it can be extremely cold or
extremely hot after switching on by a mistake. Danger of burning! Really wait until the
supply system has cooled down to room temperature.
• If it is not possible to let the cooling head outside the dewar vessel completely dry,
water is collected by time inside the dewar vessel. This water must be regularly removed
by emptying the dewar completely, dumping the ice (water) and drying out the dewar.

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DSC 204 F1 System Components

• Liquid nitrogen used in storage tanks (e.g. dewar vessel) evaporates into the air; 1 litre
of liquid nitrogen releases around 700 litres of nitrogen in the gaseous state. Nitrogen is
an inert, non-toxic gas, but displaces oxygen when released into the atmosphere. Once
the atmospheric oxygen content falls below 19% the human organism is at risk.
• All rooms and areas housing vessels containing liquid nitrogen should be well ventilated
at all times and equipped with at least one oxygen gauge. All personnel should be
informed of the risks associated with the use of nitrogen.
• The dewar vessel is designed for use with liquid nitrogen only.
• The dewar vessel must not be moved with its control head fitted. It must only be moved
when the neck is open.
• Never seal the neck of the dewar vessel hermetically. Use only the stopper provided or
the NETZSCH dewar heads.
• The dewar vessel must always be kept vertical.
• The dewar vessel must always be transported empty, in its original packaging and in
compliance with the current national and international regulations. Never stack vessels
on top of each other.

Precautions in the Event of Operating Faults

If you suspect that the integrity of the equipment has been compromised (for example as a
result of damage sustained during transit or during use), it should be withdrawn from
service. Make sure that the withdrawn equipment cannot be accidentally used by others.
The defective equipment should be handed over to authorized technicians for inspection.

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DSC 204 F1 System Components

Air cooling

Linear small compressor

temperature range: 700°C to 40°C


quickest possible cooling time from 600°C to 40°C: 20 min
linear cooling with 20K/min to 160°C / with 10K/min to 100°C

Technical data

Voltage, alternating current: 230 V, 50/60 Hz / alternative 115 V, 60 Hz


Type of motor protection: IP 20

Pressure, suction side: 1 bar abs.


Pressure, pressure side: 1 bar abs.
Delivery efficiency at atm. pressure: approx. 39 l/min
(measured with air at 20°C)

max. allowable temperature of the medium: +5°C to 40°C


max. allowable temperature of the +5°C to 40°C
environment:

Gas connection: hose, inside diameter 6 mm


outside diameter 8 mm
Flow medium: air
Weight: 6.6 kg

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DSC 204 F1 System Components

On-Off valve kit for compressed air cooling


®
A stationary compressed air supply can be connected to the DSC 204 F1 Phoenix via the
on-off valve kit (see chapter II "Installation").
gas supply:
compressed air, max. 1 bar (impact pressure*)
dry, free of oil and dirt

* Impact pressure is adjusted on the pressure reducer of the compressed air supply without
consumption.

Cooling device for pressurized air


For minimum temperature of 0°C or below (dependent on air pressure). Includes cold air
generator and software controlled magnetic valve (see chapter II "Installation").

Requirements at customers site:


Pressurized air, throughput approx. 200 l/min, min. pressure 6 bar, max. pressure 10 bar,
oil-free, dry (pressure dew point <5 °C), filtered (25 µm or better)

Mechanical cooling – Intracooler

temperature range: 600°C to -85°C

See operating instructions Intracooler.

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DSC 204 F1 System Components

Accessories

Sealing Press

sealing press for cold-welding sample pans:


6.240.10-80

The operation of the sealing press is


described in a separate manual!

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DSC 204 F1 Chapter IV

Operating the Instrument

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DSC 204 F1 Operating the Instrument

Contents

OPERATING THE INSTRUMENT ......................................................................1


PREPARING THE MEASUREMENT ...................................................................2
WHAT DO YOU NEED FOR THE MEASUREMENT? ...............................................2

CALIBRATION ................................................................................................... 3
CALIBRATION KIT ............................................................................................. 3
PREPARING THE SAMPLE .............................................................................4
POWDERED SOLIDS ........................................................................................... 4
COMPACT SOLIDS ............................................................................................. 4
FILMS ............................................................................................................. 4
FIBERS ............................................................................................................ 5
LIQUIDS .......................................................................................................... 5
UNSTABLE SAMPLES .......................................................................................... 5
EVAPORATION REACTIONS ................................................................................. 5
MEASUREMENTS IN DEFINED ATMOSPHERES .......................................................... 5
SELECT THE SAMPLE CRUCIBLE ............................................................................. 6
WEIGH THE SAMPLE .......................................................................................... 6
SEAL THE CRUCIBLE ........................................................................................... 6
INSERT THE CRUCIBLES ...............................................................................7
SAMPLE CRUCIBLE ............................................................................................. 7
REFERENCE CRUCIBLE ........................................................................................ 9
PLACE THE COVERS ......................................................................................... 10

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DSC 204 F1 Operating the Instrument

GENERATE PURGE GAS ATMOSPHERE ...........................................................12


ADJUSTING THE GAS FLOW ............................................................................... 13
SET THE START TEMPERATURE FOR THE MEASUREMENT ....................................13
COOL WITH LIQUID NITROGEN ....................................................................14
GENERAL INFORMATION .................................................................................. 14
COOLING WITH THE CC 200 F1/CC 300 F1 COOLING CONTROLLER ........................ 15
SELECT THE COOLING PROGRAM ........................................................................ 15
COOLING WITH THE LN2 COOLER (MAGNETIC VALVE CONTROLLED) ...................16
HANDLING .................................................................................................... 16
REMOVING THE LN2 COOLER FROM THE DEWAR VESSEL........................................ 16
AIR-COOL (LINEAR SMALL COMPRESSOR) .....................................................17
ON-OFF VALVE KIT FOR COMPRESSED AIR COOLING ........................................17
HANDLING .................................................................................................... 17
COOLING DEVICE FOR PRESSURIZED AIR .......................................................17
HANDLING .................................................................................................... 17
COOL WITH THE COOLING COMPRESSOR (INTRACOOLER)..................................18
MAINTENANCE .......................................................................................19
HINTS FOR USING PURGE GASES .................................................................21

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DSC 204 F1 Operating the Instrument

Operating the instrument

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DSC 204 F1 Operating the Instrument

Preparing the In thermoanalytical investigations, the test parameters have a


measurement significant influence on the results.

Information regarding the specific effects of the individual


test parameters on the results of DSC measurements can be
found in the technical literature.

The following parameters should be considered when


preparing the measurement:

• calibration
• sample preparation
• sample weight
• reference material
• sample chamber temperature
• temperature program
• atmosphere

What do you Assemble the required materials before starting the


need for the measurement:
measurement?
• purge gases (sample chamber and furnace jacket)
liquid nitrogen (cooling)

• sealing press for cold sealing of Al crucibles

• sealing tool for pressure-tight crucibles

• tweezers (pointed for crucibles, offset for lids)

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DSC 204 F1 Operating the Instrument

Calibration • Calibration of the instrument is a prerequisite for


quantitative analysis of DSC measurements.

• There is a difference between temperature and enthalpy


calibration.

ATTENTION!
• A complete recalibration of the instrument should be carried
out at least once per year and additionally after the
exchange of sensors, thermocouples or electronic
components resp. before longer measurement runs.
• A control of the calibration should be made at least once per
month or on spec of contamination or explicit changes of
the test conditions.

control period reference material


once per month indium

®
Calibration Kit A calibration kit is supplied with the DSC 204 F1 Phoenix .
We calibrate your instrument prior to delivery.
A detailed description of the calibration procedure can be
found in the Help system of the Software.

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DSC 204 F1 Operating the Instrument

Preparing the sample

When preparing the sample, the effects to be interpreted and


the consistency of the sample must be considered. Good
thermal contact between the sample and heat-flux sensor is
an indispensable requirement for optimum results.

The methods most frequently used for preparation of solid


and liquid samples are described below.

Powdered solids The sample is evenly distributed in the bottom of the sample
crucible.

Compact solids, e.g. rubber or thermoplastic, are cut into thin


Compact solids
slices with a knife, scalpel or razor blade.

For the analysis, a hollow drill is used to punch out a sample


disc of a suitable size from this larger disc (taken from the
center of the whole sample).

If it is not possible to punch out a suitably sized disc, the


bottom of the crucible is covered with thin slices of the
material.
A sample crucible must always be used. Direct
application of the sample material increases the
danger of contaminating the heat-flux sensor!

PVC
PVC samples should only be heated in inert gas
atmospheres (N2) to a maximum of 220°C.
Otherwise, HCl can evolve and cause serious
damage to the sensor.

Films Discs are punched from films with a hollow drill or punch
pliers. The discs should completely cover the bottom of the
crucible.
In order to improve the contact between the sample and
crucible bottom, the lid should be placed on the crucible, with
the convex side down, and sealed.

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DSC 204 F1 Operating the Instrument

Fibers The fiber can be cut into small pieces, which are then spread
parallel on the bottom of the crucible.

The fiber is wound around a small rod. The coiled fiber is then
removed from the rod and placed in the crucible.

A bundle of fibers is wrapped with aluminum foil and cut at


both ends. (The weight of the sample can be increased with
voluminous fiber materials.) The fiber material with the foil
wrapping is then placed in the crucible.

The significance of the experimental results can be increased


in all cases by adding a drop of silicone oil (improves the heat
transfer).

Liquids Depending on the viscosity, liquid samples can be dropped


into the crucible with a thin glass rod, a micro-pipette or a
syringe.

Unstable samples Unstable samples are tested in special pressure-tight crucibles


(optional).

The measuring cell must be recalibrated when pressure-tight


crucibles are used.

Evaporation When investigating evaporation reactions, e.g. evaporation of


reactions water of crystallization, a closed crucible with a small hole in
the center of the lid should be used.
The hole should be punched prior to sealing to avoid
deformation of the crucible later.

Measurements in For measurements in defined atmospheres, a needle should be


defined used to pierce one to five holes in the lid of the crucible.
atmospheres
The holes should be made prior to sealing to avoid
deformation of the crucible later. It is also an option to run
the measurement without a lid on the crucible.

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DSC 204 F1 Operating the Instrument

Select the sample


crucible

See chapter V: crucibles

Weigh the sample • Weigh the sample with an analytical balance.


Accuracy: ± 0.01 mg

• Clean the crucible and lid with acetone or alcohol


prior to use.
• When filling the crucible, no sample material may
remain on the edge of the crucible. Otherwise,
when cold-sealed, the bond between the crucible
and lid may not be tight.
• After crimping, the bottom of the crucible must be
plane and free of scratches. If the bottom of the
crucible is uneven, the heat transfer between the
heat-flux sensor and the sample is impaired!

Seal the crucible Certain types of crucibles (see chapter V: crucibles) can be cold-
sealed with a special sealing press.

The operation of the sealing press is described in a


separate manual!

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DSC 204 F1 Operating the Instrument

Insert the crucibles

Sample crucible

The lids could still be hot. Danger of burns!


If possible, lay the lid on the metal plate of the
measuring cell.

a) Instrument without automatic cover hoist

• Remove the cell lid and both interior lids.

Use the tweezers for lid for removing the separate


cell lids.

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DSC 204 F1 Operating the Instrument

Insert the crucibles

Sample crucible b) Instrument with automatic cover hoist

• Press "open"+"safety key" at the same time and


move the cover into the upper end position (green LED
on the "open key" is shining).

• Pick up the sample crucible from the top with the


tweezers and place it exactly in the center of the right-
hand support of the heat-flux sensor.

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DSC 204 F1 Operating the Instrument

Reference crucible

The heat-flux resistance is primarily determined by


the crucible and not by the relatively small sample
weight. In general, an empty crucible is used as the
reference.

If a strong baseline drift occurs with samples with a


high specific heat, this asymmetry can be
compensated by using an inert reference material.

The properties of the reference material (thermal


conductivity, specific heat, etc.) should be similar to
those of the sample.

• Pick up the reference crucible from the top with


the tweezers and place in the center of the left-
hand support of the heat-flux sensor.

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DSC 204 F1 Operating the Instrument

Place the covers a) Instrument without automatic cover hoist

• Replace both interior lids (2x) and the exterior lid.

Prior to inserting the lid wait until the furnace has


cooled down to at least 100°C. If the lids are installed
at higher temperatures and eventually canted, a kind
of welding between the surfaces (furnace and cover)
can occur, caused by the fast warming of the silver
cover. Then the only way is to loosen the lid
violently, that can involve a damage of the furnace
and cover.

Use the tweezers for lid for inserting the separate


cell lids.

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DSC 204 F1 Operating the Instrument

Place the covers b) Instrument with automatic cover hoist

• Press "close"+"safety key" at the same time and


move the cover into the lower end position (green
LED on the "close key" is shining).

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DSC 204 F1 Operating the Instrument

Generate purge gas atmosphere

Measurements can be run in static or dynamic


atmospheres.

Conducting measurements in a protective gas


atmosphere has a positive influence on the service
life of the measuring cell.

Recommended:
Use a dry, inert purge gas in the sample chamber
above 500°C.
Required:
The use of a dry, inert purge gas in the sample
chamber above 600°C is absolutely necessary.

The purge gas inlets purge 1 and purge 2 are


connected to one another with a tee inside the
measuring cell. This allows a gas change during the
measurement.
If possible, carry out the gas change within a short,
isothermal program step. You will thus achieve a
clean separation of the atmospheres.

Recommended purge gas rates:


purge 1 approx. 15 - 20 ml/min
purge 2 approx. 15 - 20 ml/min
protective approx. 70 ml/min

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DSC 204 F1 Operating the Instrument

Adjusting the gas flow

Yor instrument is equipped with electronic mass flow


controllers.
The flow rates for the individual gases (purge and
protective) can be adjusted via the software.

The mass flow controller are not designed for the use of
corrosive, flammable or reducing gases!

Set the start temperature for the measurement

The start temperature for the measurement is entered via


the software.

It is frequently the case that the temperature in the


sample chamber is higher than the start temperature for
the measurement.

In order to reach the required start temperature, there


are several cooling options available.

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DSC 204 F1 Operating the Instrument

Cool with liquid nitrogen

General information Cooling with liquid nitrogen is required, if:


cooling processes are being investigated, i.e. if the start
temperature is higher than the end temperature.

To prevent icing of the measuring cell:

• Feed a dry protective gas, e.g. N2 (about 70 ml/min)


into the furnace jacket (use gas inlet "protective").

• Purge the sample chamber (N2, about 20 ml/min, use


gas inlet "purge 1" or "purge 2").

• Due to the good heat transfer, helium can also be


used as a purge gas at very low temperatures. Note
that helium decreases the sensitivity of the sensor.

• Do not change the gas flow rate (protective, purge)


during the measurement. This will eliminate effects on
the sensitivity of the measuring cell.

ATTENTION!
Please pay attention to all safety regulations for
handling liquid nitrogen (see chapter I and chapter III)
and purge gases (see chapter IV).

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DSC 204 F1 Operating the Instrument

Cooling with the CC 200 F1/CC 300 F1 cooling controller

• Use the CC 200 F1/CC 300 F1 cooling controller for


measurements in the temperature range from -180°C
to 700°C.

CC 300 F1 CC 200 F1

Select the cooling


• Select your cooling program according to the
program measurement conditions.
• Establish meaningful cooling rates for the
corresponding applications
(DSC measurements 10-20 K/min).

• For linear cooling at a defined cooling rate, an


isothermal segment must be defined before the
cooling phase begins.

• If starting from a defined end temperature, an


isothermal segment should also be defined after this
temperature has been reached.

• This isothermal segment should be at least 10 minutes


long.

• For certain applications, it may be necessary to


extend the duration of the isothermal segment beyond
10 minutes.

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DSC 204 F1 Operating the Instrument

Cooling with the LN2 cooler (magnetic valve controlled) 6.351.24 or 25

A B

from gas supply


forced N2, 0.5 bar

DSC 204 F1

E D

Handling Be sure that the LN2 cooler is connected to the measuring


unit (see: chapter II – "Installation")
It is possible to use a dry, inert gas for pressure
generation.
In that case open your gas supply.
Open the shut-off valve (A).
Wait until the pressure in the dewar vessel reaches 0.3 bar.
Pressure generation is enhanced when the dewar is not
completely filled. It is not necessary to keep shut-off valve
(A) open when the content of the dewar is less than 50%.
The magnetic valve opens and closes the nitrogen cooling
depending on the software presettings.

Be sure that shut-off valve (A) is closed when dewar is


empty.

Removing the LN2 cooler Close your gas supply.


from the dewar vessel Close the shut-off valve (A).
Open the shut-off valve (B) to reduce pressure in the
dewar vessel. Watch the manometer.
If normal pressure has been reached:
Loosen the butterfly nut (D).
Remove the clamping ring (E).

Draw out the LN2 cooler.

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DSC 204 F1 Operating the Instrument

Air-cool (linear small compressor)

The measuring cell can be cooled to above room


temperature through the introduction of air (linear
small compressor).

Use air-cooling to effectively cool the cell to approx.


100°C.

Air-cooling can be switched on via the software.

On-off valve kit for compressed air cooling

Handling Be sure that the on-off valve kit for compressed air
cooling is connected to the measuring unit (see:
chapter II – "Installation").

The air cooling is switched on and off depending on


the software presettings.

The compressed air leaves the outlet of the cooling


channel with high speed. Depending on the furnace
temperature it might be hot. Please ensure that no
damage can be caused for these reasons.

If liquid nitrogen cooling (6.351.24 or 25) is installed


the highest allowed air pressure is 1 bar overpressure.
If liquid nitrogen cooling (6.351.24 or 25) is not
installed the highest allowed air pressure is 2 bar
overpressure.

Cooling device for pressurized air

Handling Be sure that the cooling device for pressurized air is


connected to the measuring unit (see: chapter II –
"Installation").

The air cooling is switched on and off depending on


the software presettings.

The compressed air leaves the outlet of the cooling


channel with high speed. Depending on the furnace
temperature it might be hot. Please ensure that no
damage can be caused for these reasons.

It is not possible to use the cooling device for


pressurized air with simultaneous connected
liquid nitrogen cooling!

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DSC 204 F1 Operating the Instrument

Cool with the cooling compressor (Intracooler)

Use the Intracooler for measurements in the


temperature range of - 80°C to 600°C.

Do not use the refrigerated bath circulator


out of the upper temperature range.

Read the operating instructions of the Intracooler


- 80°C ... +600°C
prior using the instrument.

For low-temperature application (RT…-180)


it could be necessary to adjust the control
parameters Xp, Tn und Tv of the furnace and
the sample in the Proteus-Software to get an
optimal trend of the temperature. The
following control parameters are
recommended:

Xp Tn Tv

furnace 2 5 4

sample 6 3 4

The basic power for automatical cooling with


gaseous nitrogen (GN2) and liquid nitrogen (LN2)
should be selected to the value 3 for the low
temperature range (see Help-system in the
software).

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DSC 204 F1 Operating the Instrument

Maintenance

• Make absolutely sure before every measurement that


the measuring cell is clean.

• To cleaning the sensor surface, first insert the cover


ring (included in delivery) into the furnace so that the
slot between sensor and furnace wall is covered (this
will ensure that no particles can fall into the slot when
cleaning the sensor).

cover ring

furnace
wall

slot

sensor

• Clean the measuring cell with an organic solvent


(acetone, alcohol), using a lint-free cloth or paper
towel.

• Carefully remove heavy soil from the surface with a


glass fiber brush or a fine diamond sponge.

Extreme caution should be exercised when using a


diamond sponge or glass fiber brush to remove soil.

Do not apply pressure.

• After cleaning remove all particles (vacuuming).

• Afterwards, the cell must be cleaned with acetone and


baked out.

• If not absolutely required to achieve the goal of the


investigation, the measurement should not be run to
the maximum temperature of the cell.

• Do not operate the instrument at temperatures above


600°C for long time measurements.

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DSC 204 F1 Operating the Instrument

• Begin cooling just above the sample reaction


(e.g. 20 - 30 K above the melting point).

• By setting a reasonable temperature program, you


minimize the danger of contaminating the cell.

• Whenever possible, use a protective gas in the sample


chamber.

• Bake out the sample chamber if it is necessary due to


contaminations.
procedure:
Heat the cell to 600°C and hold the temperature
constant for about 30 minutes.

• If possible, avoid measurements with samples that


create heavy soot or soil.

• It is imperative that the sensor surfaces remain scratch-


free.

• Do not introduce LN2 into the system when


temperatures are above 450°C.

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DSC 204 F1 Operating the Instrument

Hints for using purge gases

In dynamic mode the sample chamber is purged with gas during measurement.

Inert gases, air and some reaction gases (non toxic, non flammable) can be used.

In order to avoid environmental hazards or damage to the instrument, the


following instructions must be followed when using purge gas.

Dry, inert gases are recommended for purging the sample chamber. Prior to the intro-
duction of gas, a leakage test should be carried out whilst pre-evacuating the system in
order to assure the purity of the sample atmosphere. We also recommend that the ex-
pelled purge gas be passed into a suitable exhaust hood. Depending on the measuring
conditions (sample material, atmosphere, temperature range), derivative products can also
be formed due to thermal reactions when using inert gases. These products (e.g. HCN, CO,
SO2, dioxine), even in small amounts, are very detrimental to health and must not be
allowed to pass into the work room.

The user must decide in advance whether toxic gases might be released during a measure-
ment. Should this be so, then safety precautions are absolutely essential.

When the measurement requires special reaction gases to be used in the sample chamber,
then a safety check of the potentially hazardous gas or gas mixture is imperative. In this
case the following aspects have to be taken into consideration:

Do explosive gas mixtures or explosive compounds evolve when the sample has contact
with oxygen (air)?

Is it certain that no toxic compounds can evolve from the gases or gas mixtures when using
the chosen application temperatures? In this connection, possible reactions between the
purge gas in the weighing chamber and the reaction gas in the sample chamber should
also be investigated.

Can it be ruled out that the gases neither corrode the leads nor the seals which are used in
either the system or the surrounding equipment (valves, manometer or flow meter)? If not,
then leakages are to be expected.

What side effects do the gases or gas mixtures have on the system's accessories? These ef-
fects do not result in leakages but would considerably increase wear and tear or could lead
to a total failure of the system.

Under no circumstances may explosive gas mixtures be used. The mass flow
controllers are not designed for the use of corrosive, flammable or reducing
gases!

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DSC 204 F1 Operating the Instrument

Information concerning the possibilities of using various gases can be found in the appro-
priate technical literature or can be requested from the manufacturer or retailer of gases.

The following is a selection of purge gases including their limiting properties. The list
makes no claim on being complete.

Helium (He) Chemically inert (inert gas)


No technical safety limitations

Argon (Ar) Chemically inert (inert gas)


Asphyxiating
No technical safety limitations
Argon should not be used for low temperature investigations
Nitrogen N2 Largely inert
Asphyxiating
No technical safety limitations, but sample reactions are possible in
the high temperature range.

Air Oxidizing
No technical safety limitations, but sample reactions are possible.
Application is possible above room temperature (maximum
application temperature is determined by furnace material, sample
holder type, crucible material). The oxygen could liquefy if used in
the low temperature range (LN2).

Oxygen (O2) Increases flammability


(must not come into contact with fats or oils)
No technical safety limitations, but hefty reactions are possible
with the sample.
Application is possible above room temperature (maximum
application temperature is determined by furnace material, sample
holder type, crucible material). Liquefaction could occur in the low
temperature range (LN2).

Carbon dioxide Non-toxic


(CO2) (MAK value 5000 vpm),
Non-flammable
Application is possible above room temperature.

Hydrogen (H2) The instrument is not destined and suitable for use under
hydrogen atmosphere.
It can happen that explosible mixtures are formed inside the
system during the respective experiments.

Ammonia (NH3) Toxic


(MAK value 50 vpm),
Flammable
Danger of explosion when in contact with oxygen.
For safety reasons it is forbidden to use an instrument that has
been installed in the normal way.
Corrosion of seals is possible.

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DSC 204 F1 Operating the Instrument

Carbon monoxide Toxic


(CO) (MAK value 10 vpm),
Flammable
Corrosive
For safety reasons it is forbidden to use an instrument that has
been installed in the normal way.

Hydrogen sulphide Toxic


(H2S) (MAK value 10 vpm),
Flammable, corrosive
For safety reasons it is forbidden to use an instrument that has
been installed in the normal way.

Other reducing For safety reasons it is not possible to use these gases as contact
gases or gas with oxygen or air could result in an explosive compound.
mixtures However, certain gas compounds with inert gases are possible
where the mixture ratio excludes all technical safety doubts while
complying with the required analytical conditions. The
manufacturers of gases and gas mixtures can provide the required
information.

Chlorine (Cl2) Very toxic


(MAK value 5 vpm),
Non-flammable, corrosive, caustic
For safety reasons it is forbidden to use an instrument that has
been installed in the normal way.

Hydrogen chloride Toxic


(HCl) (MAK value 5 vpm),
Non-flammable, corrosive, caustic
For safety reasons it is forbidden to use an instrument that has
been installed in the normal way.

Sulphur dioxide Toxic


(SO2) (MAK value 2 vpm),
Non-flammable, corrosive
For safety reasons it is forbidden to use an instrument that has
been installed in the normal way.

Fluorine (F2) Very toxic


(MAK value 0.1 vpm),
Encourages burning, corrosive, caustic
For safety reasons it is forbidden to use an instrument that has
been installed in the normal way.

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DSC 204 F1 Operating the Instrument

Hydrogen fluoride Very toxic


(HF) (MAK value 3 vpm),
Very caustic, corrosive
For safety reasons it is forbidden to use an instrument that has
been installed in the normal way.

Gaseous Can form explosive gas mixtures with air


hydrocarbon For safety reasons it is forbidden to use an instrument that has
been installed in the normal way.

MAK values 2006

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DSC 204 F1 Chapter V

Appendix

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DSC 204 F1 Appendix

Contents

TECHNICAL DATA ........................................................................................1

ADAPTER FOR COUPLING SYSTEMS ..................................................................3

QMS-COUPLING ................................................................................................. 3
FT-IR-COUPLING ................................................................................................. 4
SPARE PARTS ...................................................................................................... 5

CRUCIBLES .................................................................................................6

SEALING TOOL 6.239.2-92.4 .......................................................................7

MOUNTING ........................................................................................................ 7
HANDLING THE DYNAMOMETRIC KEY .................................................................... 8
SPARE PARTS LIST (SEALING TOOL 6.239.2-92.4) .................................................... 9

LITERATURE ..............................................................................................10

BROCHURES ...................................................................................................... 11
STANDARDS FOR THERMAL ANALYSIS ................................................................... 11

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DSC 204 F1 Appendix

Technical data

Heating System
Temperature range: -180°C ... 700°C (depending on sensor)
τ sensor: -180 ... +700°C
µ sensor: -150 ... +375°C
(max. working temperature +400°C)
Heating rates: 0.001 to 100 (200*) K/min
(*depending on temperature range
and cooling system)
Cooling System
liquid nitrogen: 700°C to -180°C
cold gas: 700°C to -100°C
compressor (Intracooler): 600°C to -85°
linear small compressor: 700°C to 40°C
cooling time: from 600°C to -170°C : >15min (liquid nitrogen)
Measuring System
digital resolution: 24-Bit converter
signal noise: < 60 nV peak to peak
signal time constant: measurement with laserpulse (only verifiable by
manufacturer):
about 0.6 s (τ-Sensor)
experimental (aluminium-crucible):
about 3.6 s (τ-Sensor, Indium)
reproducibility onset-temperature: < 0.2 K (Indium-peak, aluminium-crucible)

reproducibility of peak areas: ± 1% (Indium-peak, aluminium-crucible)

Computer System
Operating system MS-WINDOWS XP Professional,
MS-WINDOWS Vista Business/Enterprise,
MS-WINDOWS 7 Professional/Enterprise/Ultimate
USB Interface,
Windows-compatible printer

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DSC 204 F1 Appendix

Dimensions in mm (w x d x h) /Weight (net) in kg


580 x 530 x 250 / 33
Power Supply
230 V (115 V); 50 Hz or 60 Hz; < 1000 W
Operational Conditions
Ambient temperature 20°C +/- 5°C
Relative air humidity 60% +/- 20%
Atmospheric pressure 1013 hPa +/- 30 hPa

Technical data subject to change

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DSC 204 F1 Appendix

Adapter for coupling systems

Appropriateness
coupling of the DSC 204 F1 with FT-IR Tensor and/or QMS Aëolos.

General
Before starting FT-IR or MS measurements the measuring cell must be purged with
protective gas for approx. 10 minutes since the measuring cell can not be evacuated.

Order number: 6.240.10-43


The adapter can simultaneously be used for FT-IR and QMS coupling.

QMS-coupling

1 5

open

close

2 3

The adapter head (1) is attached by the screwings (2) on the cover of the DSC 204 F1. The
gas tube (3) can be unscrewed for cleaning. The transfer line (4) is fixed upright to the gas
flow on the adapter head. The excess gas is dissipated via the gas outlet tube (6). The
length of the gas outlet tube (PTFE tube) is about 1 m. The protective outlet valve (5) must
be opened for measurements in QM-mode. The adapter can be heated up to 300°C.

During normal measurements without active adapter heating and active QMS, the
protective outlet valve (5) must be opened.

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DSC 204 F1 Appendix

FT-IR-coupling

4 1 6 5

open

close

2
3

The adapter head (1) is attached by the screwings (2) on the cover of the DSC 204 F1. The
gas tube (3) can be unscrewed for cleaning. The transfer line (4) is screwed on the end of
the adapter head. The connection to the QMS is closed with a cover (6). The protective
outlet valve (5) must be closed for measurements in FT-IR-mode.

During normal measurements without active adapter heating and active FT-IR the
protective outlet valve (5) must be opened.

Attention!

The adapter may be heated only up to 230°C because of the FT-IR transfer
line.

FT-IR and QMS-coupling (simultaneous mode)

Additionally to the FT-IR configuration the transfer line to the QMS is mounted.
At simultaneous mode the FT-IR transfer line is used as a bypass for the QMS.
The protective outlet valve (5) must be opened for simultaneous measurements in FT-IR
and QM-mode.

Attention!

The adapter may be heated only up to 230°C because of the FT-IR transfer
line.

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DSC 204 F1 Appendix

Spare parts

3
2

4
open

5
close

6
7
8

no. label order no.


1 copper sealing M5 801.759
2 graphite foil sealing 802.859
3 O-ring 517.004
4 O-ring 516.716
5 V-seal-ring 800.925
6 cell cover 6.240.10-43.3
7 cell cover (small) with gas outlet tube 6.240.10-43.2
heating cartridge 396.908
thermocouple 396.023
teflon tube 3/2 mm 396.698
support sleeve 3/2 mm 398.808
collet 3 mm 396.135

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DSC 204 F1 Appendix

Crucibles

Material Tmax in °C ∅ in mm Capacity Remark Order No.

DSC 200 F3 / DSC 204 F1


Al 600 6.0 25/40 µl set pans / lids, cold-weldable, 100 pcs. 6.239.2-64.5.00

Al 600 6.0 25/40 µl set pans / lids, cold-weldable, 500 pcs. 6.239.2-64.51.00

Al 600 6.0 40 µl set pans / lids, punched, cold-weldable, 100 pcs. 6.239.2-64.8.00

Al 600 6.0 40 µl set pans / lids, punched, cold-weldable, 500 pcs. 6.239.2-64.81.00

sealing press: 6.240.10-80.0.00A with tool set 6.240.10-81.0.00

Al 600 6.0 35 µl set pans / lids, cold-weldable, 100 pcs. 6.240.10-65.1.00

Al 600 6.0 35 µl set pans / lids, cold-weldable, 500 pcs. 6.240.10-65.10.00

sealing press: 6.240.10-80.0.00A with tool set 6.240.10-82.0.00

Al (99.5) 600 6.7 85 µl pan (lid: NGB810406) NGB810405

Ag 700 6.7 85 µl pan (lid: GB398193) GB398192

Al2O3 700 6.8 85 µl pan (lid: GB399973) GB399972

ZrO2 700 6.7 85 µl pan (lid: GB397052) GB397053

quartz glass 700 6.7 85 µl pan (lid: GB399975) GB399974

duran glass 530 80 µl ampoule, 100 pcs. 6.240.1-93.2.00

Pt/Rh 700 6.8 85 µl pan (lid: GB399860) GB399205

Pt/Rh 700 6.8 190 µl pan (lid: GB399860) GB801556

Au 700 6.7 85 µl pan (lid: GB398191) GB398190

Cu 600 6.0 40 µl pan for OIT measurement 6.239.2-64.6.00

pressure-tight crucibles with Au sealing discs:

CrNi steel, gold-plated 500 27 µl re-usable, max. 100 bar, set: 1 crucible/5 sealings 6.239.2-92.3.00

CrNi steel, gold-plated 500 27 µl re-usable, max. 100 bar, set: 10 crucible/50 sealings 6.239.2-92.31.00

CrNi steel, gold-plated 500 100 µl re-usable, max. 100 bar, set: 1 crucible/5 sealings 6.239.2-92.8.00

CrNi steel 500 27 µl re-usable, max. 100 bar, set: 1 crucible/5 sealings 6.239.2-93.3.00

CrNi steel 500 27 µl re-usable, max. 100 bar, set: 10 crucible/50 sealings 6.239.2-93.31.00

CrNi steel 500 100 µl re-usable, max. 100 bar, set: 1 crucible/5 sealings 6.239.2-93.4.00

Titanium 500 27 µl re-usable, max. 100 bar, set: 1 crucible/5 sealings 6.239.2-92.6.00

Titanium 500 90 µl re-usable, max. 100 bar, set: 1 crucible/5 sealings 6.239.2-92.2.00

Titanium 500 100 µl re-usable, max. 100 bar, set: 1 crucible/5 sealings 6.239.2-92.9.00

Au sealings package with 100 pcs. 6.240.1-91.1.00

complete sealing tool for crucibles 6.239.2/.3/.6/.8/.9 and -93.3/.4: 6.239.2-92.4.00

further pressure-tight crucibles:

special steel 200 120 µl max. 20 bar, set: 25 crucible/25 lids/25 sealings 6.240.1-68.1.00

sealing press: 6.240.10-80.0.00A with tool set 6.240.10-83.0.00

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DSC 204 F1 Appendix

Sealing tool 6.239.2-92.4

Mounting

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Handling the dynamometric key

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DSC 204 F1 Appendix

Spare parts list (Sealing Tool 6.239.2-92.4)

Quantity Description Order No.:


1 Phillips screwdriver 802 622
1 Guide 400 01 02
1 Lid support 802 623
1 Plate 803 373
2 Countersunk screw M4 x 16 400 01 05
1 Foundation 400 01 06
2 O-ring 8 x 1.5 800 590
1 Base 400 01 08
2 Countersunk screw M4 x 10 400 01 09
2 Countersunk screw M6 x 16 400 01 10
2 Setscrew No. 6 400 01 11
1 O-ring 47 x 4 400 01 12

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DSC 204 F1 Appendix

Literature

Kaisersberger E.; Möhler H.


NETZSCH Annual for Science and Industry, Volume 1
DSC on Polymeric Materials
Würzburg, Selb 1991

Kaisersberger E.; Knappe S.; Möhler H.


NETZSCH Annual for Science and Industry, Volume 2
TA for Polymers and Additives DSC-TG-DMA
Selb, Würzburg 1993

Kaisersberger E.; Knappe S.; Möhler H.; Rahner S.


NETZSCH Annual for Science and Industry, Volume 3
TA for Polymers and Additives DSC-TG-DMA-TMA
Selb, Würzburg 1994

Brown
Introduction to Thermal Analysis
Chapman and Hall, London, New York, 1988

DIN 51005
Thermische Analyse [TA] Begriffe
Beuth-Verlag GmbH, Berlin, 1983

Hill [ICTA]
For Better Thermal Analysis and Calorimetry
ICTA, 1991

Mackenzie
Differential Thermal Analysis
[Vol. 1, Fundamental Aspects]
Academic Press, 1970

Mackenzie
Differential Thermal Analysis
[Vol. 2, Applications]
Academic Press, 1972

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DSC 204 F1 Appendix

Hemminger, H.K. Cammenga


Methoden der Thermischen Analyse
Springer-Verlag, Berlin/Heidelberg/New York/
London/Paris/Tokyo, 1989

Turi
Thermal Analysis in Polymer Characterization
Heyden & Son, Philadelphia, London, Rheine, 1996

Wendlandt
Thermal Analysis
Vol.19, 3rd edition
John Wiley & Sons, New York/London/Sydney/Toronto, 1986

Brochures

Thermochimia Acta
Elsevier Science Publishers B.V.

Journal of Thermal Analysis


John Wiley & Sons, Chichester
Academiai Kiado, Budapest

Standards for Thermal Analysis

DIN 51 005 Thermal Analysis (TA) terms


DIN 51 006 Thermal Analysis (TA); Thermogravimetry (TG) principles
DIN 13346 Temperature, temperature difference, basic concept and units
DIN 43760 Basic values for measuring resistors
ASTM D3418 Transition temperature of polymers by Thermal Analysis
ASTM E473 Standard definitions of terms relating to Thermal Analysis
ASTM E793 Heats of fusion and crystallization by DSC
ASTM E472 Standard practice for reporting Thermoanalytical Data

ASTM = American Society for Testing and Materials


DIN = Deutsches Institut für Normung e.V.

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