Operating Manual: DSC 3500 Sirius

Operating Manual
DSC 3500 Sirius®
36098 / Version 2.1 / January 2019

Sirius
DSC 3500 Contents
CONTENTS
CHAPTER I – GENERAL INFORMATION & SAFETY INSTRUCTION ................................................ 1
INFORMATION ......................................................................................................................... 2
SAFETY INSTRUCTIONS .............................................................................................................. 3
SAFETY SYMBOLS ..................................................................................................................... 6
INFORMATION FOR THE USAGE OF PURGE GASES ......................................................................... 8
OTHER REDUCING GASES OR GAS MIXTURES .......................................................................................... 11
SAFETY REGULATIONS FOR HANDLING NITROGEN/ LIQUID NITROGEN LN2 ................................... 12
SAFETY REGULATIONS FOR LN2 DEWAR VESSELS .................................................................................. 14
HANDLING OF FUSED SILICA PARTS AND AL2O3-PARTS ............................................................... 16
FUSED SILICA .................................................................................................................................... 16
AL2O3.............................................................................................................................................. 16
CHAPTER II - INSTALLATION ............................................................................................. 17
WASTE DISPOSAL ................................................................................................................... 18
INSTALLATION ........................................................................................................................ 18
PACKAGING ........................................................................................................................... 19
PLACEMENT REQUIREMENTS .................................................................................................... 20
INSTALLATION SCHEMATICS ..................................................................................................... 20
CONNECTING THE SYSTEM COMPONENTS .................................................................................. 21
CONNECTING THE COMPUTER SYSTEM ................................................................................................. 21
IMPORTANT NOTES FOR SOFTWARE INSTALLATION ................................................................................. 22
CONNECTING THE LINEAR SMALL COMPRESSOR .................................................................................... 23
CONNECTING THE ON-OFF VALVE KIT FOR COMPRESSED AIR COOLING ................................................... 24
CONNECTING THE COOLING DEVICE FOR PRESSURIZED AIR ...................................................................... 25
CONNECTING THE INTRACOOLER 40 .................................................................................................... 26
CONNECTING THE INTRACOOLER 70 (230 V / 50 HZ) ............................................................................ 27
CONNECTING THE INTRACOOLER 70 (115 V / 60 HZ) ............................................................................ 28
CONNECTING THE LN2 COOLER CC 200 F3 ......................................................................................... 29
CONNECTING THE LN2 COOLER CC 300 .............................................................................................. 30
CONNECTING THE GAS SUPPLY ........................................................................................................... 31
CONNECTING THE GAS SWITCHES WITH SINTERING INSERTS ................................................................. 31
CONNECTING THE MASS FLOW CONTROLLERS (MFCS) ..................................................................... 32
CONNECTING THE GAS FLOW CONTROL DEVICE (OPTIONAL) TO THE GAS SWITCHES .............................. 33
REMOVING THE SINTERING INSERTS ................................................................................................ 33
CHAPTER III – SPECIFIC INFORMATION OF THE INSTRUMENT .................................................. 35
APPROPRIATE USE .................................................................................................................. 36
REASONABLE FORESEEABLE MISUSE ..................................................................................... 36
SAFETY INFORMATION FOR OPERATING THE INSTRUMENT ...................................................... 36
MEASURING UNIT .................................................................................................................. 39
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OPERATING PRINCIPLE ............................................................................................................ 40

OPEN THE MEASURING CELL.................................................................................................... 41
FRONT PANEL OF THE MEASURING UNIT ................................................................................... 42
REAR OF THE MEASURING UNIT ............................................................................................... 43
COOLING DEVICES .................................................................................................................. 45
LINEAR SMALL COMPRESSOR ............................................................................................................... 45
COOLING DEVICE FOR COMPRESSED AIR COOLING ................................................................................ 46
COOLING DEVICE FOR PRESSURIZED AIR (VORTEX) ................................................................................ 47
LN2 COOLING SYSTEM CC 200 F3 ..................................................................................................... 48
LN2 COOLING SYSTEM CC 300 .......................................................................................................... 49
INTRACOOLER 40 .............................................................................................................................. 50
INTRACOOLER 70 .............................................................................................................................. 51
ALUMINUM COOLING BODY............................................................................................................... 52
GAS FLOW CONTROL DEVICE................................................................................................... 53
SEALING PRESS ....................................................................................................................... 54
UNIT ............................................................................................................................................... 54
AVAILABLE TOOLKITS: ....................................................................................................................... 55
CHAPTER IV – OPERATE THE INSTRUMENT .......................................................................... 56
OPERATING THE INSTRUMENT .................................................................................................. 57
SHORT INSTRUCTIONS – HOW TO START A MEASUREMENT ......................................................... 58
PREPARING THE MEASUREMENT .............................................................................................. 66
CALIBRATION.................................................................................................................................... 66
CALIBRATION KIT .............................................................................................................................. 67
PREPARING THE SAMPLE ..................................................................................................................... 67
POWDERED SOLIDS ....................................................................................................................... 67
COMPACT SOLIDS ......................................................................................................................... 67
FILMS ......................................................................................................................................... 67
FIBERS ........................................................................................................................................ 67
LIQUIDS ...................................................................................................................................... 68
UNSTABLE SAMPLES ..................................................................................................................... 68
EVAPORATION REACTIONS............................................................................................................. 68
MEASUREMENTS IN DEFINED ATMOSPHERES .................................................................................... 68
SELECT THE SAMPLE CRUCIBLE ........................................................................................................ 68
WEIGH THE SAMPLE ..................................................................................................................... 68
SEAL THE CRUCIBLE ...................................................................................................................... 69
INSERT THE SAMPLE CRUCIBLES ...................................................................................................... 69
REFERENCE CRUCIBLE ......................................................................................................................... 70
PLACE THE CELL LIDS .......................................................................................................................... 71
GENERATE PURGE GAS ATMOSPHERE ....................................................................................... 72
ADJUSTING THE GAS FLOW ................................................................................................................. 73
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HINTS FOR SPECIAL GASES BY USING SINTERING INSERTS .......................................................................... 73

PURGE GAS SWITCHING (O.I.T. EXTENSION) .......................................................................................... 74
SET THE START TEMPERATURE FOR THE MEASUREMENT ............................................................... 74
COOLING WITH THE LINEAR SMALL COMPRESSOR ...................................................................... 75
HANDLING ....................................................................................................................................... 75
COOLING WITH LIQUID NITROGEN ............................................................................................ 76
GENERAL INFORMATION .................................................................................................................... 76
COOLING WITH THE LN2 COOLER CC 200 F3 (MAGNETIC VALVE CONTROLLED) ............................ 77
HANDLING ....................................................................................................................................... 77
REMOVING THE LN2 COOLER FROM THE DEWAR VESSEL ......................................................................... 77
ON-OFF VALVE KIT FOR COMPRESSED AIR COOLING .................................................................. 78
HANDLING ....................................................................................................................................... 78
COOLING DEVICE FOR PRESSURIZED AIR .................................................................................... 78
HANDLING ....................................................................................................................................... 78
INTRACOOLER 40 ................................................................................................................... 79
INTRACOOLER 70 ................................................................................................................... 79
MAINTENANCE ...................................................................................................................... 79
DSC 3500 SIRIUS WITH AUTOMATIC SAMPLE CHANGER (ASC) ................................................... 81
MEASURING PART ............................................................................................................................. 82
MAGAZINE ....................................................................................................................................... 83
CONTROL PANEL ASC ....................................................................................................................... 84
DSC 3500 SIRIUS WITH UV-EXTENSION ................................................................................... 86
MEASURING PART WITH UV-EXTENSION .............................................................................................. 86
COMPONENTS ............................................................................................................................. 87
TRANSPORT ........................................................................................................................... 89
CLEANING ............................................................................................................................. 89
CHAPTER V - APPENDIX ................................................................................................... 90
SEALING TOOL ....................................................................................................................... 91
GENERAL INFORMATION .................................................................................................................... 91
INTENDED USE .................................................................................................................................. 92
MOUNTING THE SUPPORT FIXTURE FOR HIGH-PRESSURE CRUCIBLES ........................................................ 93
ADJUSTING THE TORQUE WRENCH ...................................................................................................... 94
USING THE SEALING PRESS SET WITH A HIGH-PRESSURE CRUCIBLE ........................................................... 95
SPARE PARTS LIST ............................................................................................................................. 99
TECHNICAL SPECIFICATIONS ................................................................................................... 100
LITERATURE ......................................................................................................................... 102
BROCHURES ......................................................................................................................... 103
STANDARDS FOR THERMAL ANALYSIS ..................................................................................... 103
36098 / Version 2.1 / January 2019 Contents / Page III

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Chapter I –
General Information &
Safety Instruction
36098 / Version 2.1 / January 2019 Chapter I / Page 1

Sirius
DSC 3500 General Information & Safety Instruction
Information
Prior to installation and operation of your measuring system or individual components, intently
read this generally admitted chapter. The content of this chapter may exceed the information re-
quired for your instrument.
Used notes, information and symbols in the following chapters vary corresponding to your instru-
ment configuration.
Duplication Any duplication or transmission of this document, both electronic and

mechanical, requires a written prior permission of NETZSCH-Gerätebau
GmbH.
Technical Data All technical data, instrument features and other information described
in these operating instructions are compiled with great diligence, elab-
orated to the best of our knowledge and corresponding to the instru-
ments’ technical standards at the time of printing.
We reserve the right of technical modifications.
Proposals We welcome any comments, suggestions or new ideas con-

cerning the instrument, its operating instructions as well as
software or service:
NETZSCH-Gerätebau GmbH
Wittelsbacherstraße 42
D - 95100 SELB
Phone: 09287/881- 0
Fax: 09287/881- 144
E-Mail: [email protected]
Internet: http://www.netzsch-thermal-analysis.com
Service and Mainte- Service and maintenance have to be executed by NETZSCH Customer
nance Service personnel.
It is our pleasure to offer service contracts for our customers.
In case there is no existing service contract for your device, we invite

you to send us back the form enclosed with the appliance documenta-
tion.

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

and is safe to operate.
Authorized Operation Any operation of the instrument other than as authorized requires con-
sultation-with-NETZSCH.
Any use exceeding the (expanded) authorized operation is considered

unauthorized. The manufacturer will not be liable for any damage re-
sulting from such use.
Manufacturer's Re- Authorized operation of the instrument includes compliance with man-
quirements ufacturer's requirements regarding installation, commissioning, opera-
tion and maintenance.
Qualified Personnel Installation, use and maintenance of the instrument must be carried out
by authorized personnel only. These personnel must be introduced to
possible origin of danger.
Responsibility Responsibility for commissioning, operation and maintenance must be

clearly defined and compliance has to be ensured. The resulting respon-
sibilities can be clearly resolved under the aspect of safety.
Unauthorized Access The operator has to make sure that only trained personnel work on the
instrument.
Improper operations Any type of operation which interferes with the safety of the user and
the operability of the instrument should be avoided.
Unauthorized Changes Unauthorized modifications and changes which affect the safety of the
to the System instrument are not permitted.
Maintenance Obliga- The operator of the system is committed to provide immaculate oper-
tion ating conditions at every time.
Proper Set-up of the The operator has to ensure clear arrangement and cleanliness of work
Work Stations stations at the instrument by means of appropriate instruction and in-
spections.

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Shut-down For all maintenance work, the instrument must be switched off and un-
plugged.
Electrical Energy The unit may only be opened by qualified personnel. Moreover it is ab-
Danger solutely essential to previously turn it off and disconnect it from power
supply! Any work on electrical supply, electrical lines or electrical com-
ponents has to be carried out by qualified personnel only (electrical pro-
fessionals).
Removal of Protective Removing protective devices of the Instrument is solely permitted

Devices when switched off and unplugged. Furthermore, protective devices are
imperative to be replaced before restarting the instrument.
Checks following After maintenance or repair work, a check is necessary to ensure that all
Maintenance or Repair protective devices are in place and operate properly. Only then should
Work
the instrument be restarted.
Industry-specific Acci- The operator must observe the relevant regulations and protective
dent Prevention Regu- measures when handling required gases. In any case, the industry-spe-
lations
cific and local accident prevention regulations are also valid for the in-
strument.
Disposal of Production Production materials are to be disposed of according to local regula-

Materials tions.
Preventive Mainte- Products sent in for preventive maintenance or repair should, to the ex-
nance or Repair tent possible, be free of harmful substances (e.g. radioactive, toxic, caus-
tic 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. Per-
mission of NETZSCH-Gerätebau GmbH is required for repairs.
Operating Instruction Using the Operation Manual, the operator should prepare an operating
instruction which specifies the actions and tasks required for safe-oper-
ation.
The operating instruction should be placed in a suitable location at the

work place and has to be performed by the employees.

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Lighting at the Work- The lighting level on the working environment should be determined in
place such a way that safe work and an identification of risks at an early stage
are possible at all times. The minimum provided lighting level amounts
300 lx in the laboratory and 500 lx on the working environment.
Gases When handling with gases, take into account the relevant regulations
and protective measures. Consider possible reactions with materials.
Warning signs should be posted in appropriate places and be in accord-

ance with national and regional regulations.
Sealing material The Chemical resistance of used sealing material is hardly to be obliga-
tory estimated due to the multitude of inserted purge -and reaction
gases, concentrations, temperatures and contaminations.
Please make sure they meet the requirements, since we cannot assume
any guarantee.

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Safety Symbols
Below described symbols could be used to simplify orientation in this manual.
NOTE:
This sets particularly important information apart from the rest of
NOTE: the text.
ATTENTION!
These instructions must be followed exactly to avoid injury to the
ATTENTION! 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 next to this symbol are required for the installation
or modification of your instrument.
DANGER!
Hot surface! Danger of burn!
DANGER!
Cold surface! Danger of frostbite!
DANGER!
Danger of hand injury!
DANGER!
Danger of laser radiation!
DANGER!
Danger of optical radiation!
DANGER!
Danger of electric shock!
DANGER!
Toxic hazard!
Refer to instruction manual / booklet
Wear safety footwear
Wear protective gloves
Opaque eye protection must be worn

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Wear face shield
Wear a mask
CAUTION!
The instrument may only be opened when it is turned off and dis-
connected from the power supply!

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Information for the usage of Purge Gases
Fundamentally, using filler or purge gas requires consideration of the following safety-related in-
formation to avoid environmental hazards or damage to the instrument:
To reach operating temperatures of more than 1000°C it is inevitably necessary to use ceramic com-
ponents in the reaction zone (sample / furnace room). These components are exposed to continuous
changes in temperature. This might trigger crack formation and further lead to leakages, especially
in the hot area. The mentioned defects are hardly to be calculated in advance due to special prop-
erties of ceramic components. As a result they can’t be avoided through preventive maintenance
(replacement).
Dry, inert gases are recommended for purging. Prior to the introduction 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 to pass the expelled purge gas into a suitable exhaust hood. De-
pending on the measuring conditions (sample material, atmosphere, temperature range), deriva-
tive products can also be formed due to thermal reactions when using inert gases. These products
(e.g. HCN, CO, SO2, dioxin), 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 measurement.
Should that be the case, safety precautions are absolutely essential!
Humid gas mixtures may only be used if condensations inside furnace and measuring system can
be avoided. If a humid gas mixture is cooling down, the water begins to condensate at a certain
temperature. This temperature is called the dew point. The temperature must not fall below this
limit. NETZSCH offers special furnace types.
Should the measurement necessitate the usage of special gases in the sample chamber, a safety
check of the hazard potential of the gas or gas mixture is imperative. Therefore, 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)?
 Can be ensured that no toxic compounds will evolve from the gases or gas mixtures when
using the chosen application temperatures? In this connection, possible reactions between
the purge gas and the reaction gas should also be investigated.
 Is it exclusionary that the gases might corrode neither the leads nor the seals used in ei-
ther the system or the surrounding equipment (valves, manometer or flow meter)? Other-
wise leakages are to be expected.
 What side effects do the gases or gas mixtures have on the system's accessories? These ef-
fects might not result in leakages but could considerably increase wear and tear and fur-
ther end up in a total failure of the system.

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The following standards need to be observed and followed unconditionally:
Explosive gas mixtures may not on any term be utilized!

Gases or gas mixtures escaping from the measuring part
ATTENTION! unconditionally need to be deduced through am extractor
hood.
The measuring part has to be purged sufficiently with in-
ert gas after measurement.
Since restrictions for some components of the devices are valid in an oxygen free environment, we
direly recommend consultation with the manufacturer. (E.g. certain heating elements cannot be
operated up to their specified maximum temperature in inert environment since they are in need
of oxide-formation for preserving the protective layer).
Information concerning the possibility of using various gases can be found in appropriate technical
literature or can be requested from the manufacturer or retailer of gases.
Subsequent we offer a selection of purge gases including their limiting properties.
The list makes no claim to be 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 possi-
ble in the high temperature range
Air  oxidizing
 no technical safety limitations, but sample reactions are possi-
ble; application is possible above room temperature (maximum
application temperature is determined by furnace material,
sample carrier 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 tempera-
ture (maximum application temperature is determined by fur-
nace material, sample carrier type, crucible material)
 liquefaction could occur in the low temperature range (LN2)

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Carbon dioxide (CO2)  non-toxic

 german occupational exposure limit value: 5000 ml/m³ (ppm)
 non-flammable
 application is possible above room temperature
Hydrogen (H2)  flammable

 the instrument is not destined and suitable for usage in hydro-
gen atmosphere;
exposable mixtures might be forming inside the system during
the respective experiments
Ammonia (NH3)  toxic

 flammable
 danger of explosion when getting in contact with oxygen.
 for safety reasons it is forbidden to use an instrument in ammo-
nia atmosphere, that has been installed in the normal way (cor-
rosion of seals is possible)
Carbon monoxide (CO)  toxic

 flammable
 corrosive
 for safety reasons it is forbidden to use an instrument that has
been installed in the normal way CO - atmosphere
Hydrogen sulphide (H2S)  toxic

 flammable, corrosive
been installed in the normal way H2S- atmosphere

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Other reducing gases or gas mixtures
The instrument is unsuitable for usage in atmosphere of

gas mixtures or reducing gases; performing such experi-
ments might provoke explosive mixtures inside the sys-
ATTENTION!
tem
Chlorine (Cl2)  very toxic

 german occupational exposure limit value: 0,5 ml/m³ (ppm)
 non-flammable, corrosive, caustic
been installed in the normal way in Cl2 - atmosphere
Hydrogen chloride (HCl)  toxic

 non-flammable, corrosive, caustic
been installed in the normal way in HCl- atmosphere
Sulphur dioxide (SO2)  toxic

 non-flammable, corrosive
been installed in the normal way in SO2 - atmosphere
Fluorine (F2)  very toxic

 encourages burning, corrosive, caustic
been installed in the normal way in F2 - atmosphere
Hydrogen fluoride (HF)  very toxic

 very caustic, corrosive
been installed in the normal way in HF- atmosphere
Gaseous hydrocarbon  can form explosive gas mixtures when getting in touch with air;
for safety reasons it is forbidden to use an instrument that has
been installed in the normal way in such atmosphere
The AGW rates indicated are based on TRGS 900, and published
in the GESTIS-database! (http://gestis.itrust.de)
State: August 2015
Relevant national regulations are to be strictly adhered to!

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Safety Regulations for Handling Nitrogen/ Liquid Nitrogen LN2
Characteristics  Colorless, inert, harmful and incombustible liquid. Due to its

odorlessness there´s a lack of noticeable signs for its suffocating
impact.
 Leaking liquid is cryogenic (-196°C) and vaporizes rapidly.
 Liquid leads to frostbites and causes severe skin burn and eye
damage.
 Gas is lighter than air.
Safety Instructions  Handling a higher quantity of Nitrogen requires the availability

of a self-contained breathing apparatus in or in front of the
workspace.
 Fix an information sign!
 Treat containers, equipment and vessels carefully. Before refill-
ing, make sure they are well dried off. Eliminate the risk of fall-
ing over. Do not operate vessels abruptly or jerkily. Perform leak
tests at appropriate intervals.
 Icing of containers or equipment is to be removed by using
warm air or hot water only. Do not apply direct flame or incan-
descent materials for defrosting.
 For transportation do solely employ low pressure containers iso-
lated by glass wool or slag. For small quantities use metal-cased
Dewar vessels!
 Filling or decanting, make sure to prevent spillage. Only use well
dried containers!
 Pay attention to solely fill containers up to the upper limit (5 cm
below the rim) to avoid excessive pressure.
 Discharge overfilled containers.
 In case of nutrient nitrogen ensure fresh air supply. Possibly pro-
vide for suction and if necessary use a heavy breathing appa-
ratus.
 When expanding, there can occur rapid formation of cold fog
that might spread widely.
 If leakage of a high quantity of Liquid Nitrogen occurs in a
closed room (e.g. as a result of pipe break or vessel breach)
leave the area immediately, provide sufficient fresh air supply
and take immediate steps to eliminate the leak. Possibly make
use of a self-contained breathing apparatus since there might
be a lack of essential oxygen.
 Keep in mind that eating, drinking or storing aliments is prohib-
ited in the working area.
 Protective clothing, safety glasses and possibly even protective
screens and safety gloves need to be worn!

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 Entering a container or tank that is suspected to contain Nitro-

gen urgently requires the employment of a self-contained
breathing apparatus!
 Breathing apparatuses containing filter inserts are, in any case,
inadmissible.
 Rotational Instruction of employees and inscription in the re-
ceipt book are necessary. Mind the employment ban according
to regional regulations.
Information concern-  Neither gaseous nor Liquid Nitrogen are flammable and do not
ing case of fire or dam- by themselves constitute a fire or explosion risk.
age
 Firefighting claims to be coordinated in consideration of the vi-
cinity.
 Form a great security zone being located on the leeward side.
 Apply self-contained breathing apparatus.
Information concern-  Notwithstanding the fact that Nitrogen is physiologically inef-

ing health protection fective, an accumulation of about more than 81% impedes vital
respiration, eventually causing suffocation.
 Nitrogen doesn’t announce itself by any irritant or warning ef-
fect.
 Liquid Nitrogen causes frost damages. These are skin damages
similar to burn injuries.
First aid  Inform doctor or emergency hospital as quickly as possible.

 Body party affected by the cold liquid need to be defrosted by
water. Remove clothing carefully.
 Do not rub affected skin parts. Cover them with sterile dressing.
 Immediately provide fresh air in case of unconsciousness. If nec-
essary perform artificial respiration. Keep airways free.
 In case of unconsciousness place patient stably in side position,
also for transportation.
Additional Information  Mind safety regulations according to regional standards.

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Never touch objects, which have been in contact with Liq-

uid Nitrogen with your bare hands.
Always wear special safety glasses and gloves when han-
dling Liquid Nitrogen.
Please pay attention to all information for handling LN2

described in the operating manuals.
Safety Regulations for LN2 Dewar Vessels
The dewar vessel complies with the current valid Directive for Pressure Equipment and meets re-
quirements up to a pressure of 1.5 bar.
 The Dewar vessel is designed for use with Liquid Nitrogen only.
 For pressurization of the Dewar vessel use gaseous nitrogen exclusively (GN)!
 Not at any terms should the Dewar vessel be opened until the pressure has completely dissi-
pated! Monitor the pressure reduction.
 The Dewar vessel has to be kept vertical always.
 Escaping Liquid Nitrogen might cause serious injuries!
 A closed room storing Liquid Nitrogen vessels constantly contains evaporated nitrogen.1 l Liq-
uid Nitrogen releases about 700l nitrogen gas. Notwithstanding the fact that Nitrogen behaves
inertly and has no toxic impact, it displaces the atmospheric oxygen. Should the rate of atmos-
pheric oxygen drop below the minimum of 19%, danger of physical harm occurs.
 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.
 When removing the supply system from the Dewar vessel it can be extremely cold. Danger of
frostbite! In any case wait until the supply system has heated up to room temperature.
 In order to avoid damages to the Dewar head / withdrawal head it is forbidden to use hot air
instruments for deicing the components!
 Should it be impossible to let the cooling device completely dry down outside the storage vessel,
a non-negligibly amount of water will accumulate inside. It is important to remove the water
regularly by completely emptying the storage vessel, removing the ice/ water and letting the
vessel dry down entirely.
 Only in-house transport is allowed when vessel is upright, unpressurized.
 Never seal the Dewar vessel hermetically. Use only the stopper provided, the Dewar head or
withdrawal head.
 The Dewar vessel requires being transported emptily, in its original packaging and in compli-
ance with the current national and international regulations. Never stack vessels on top of
each other.

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The Dewar vessel containing Dewar head / withdrawal head is characterized by several precau-
tions to prevent possible dangers handling with LN2.
 Withdrawal head with integrated safety equipment:

Possible excess pressure is degrading through a safety valve (opening pressure: 1.5 bar).
 LN2-cooler CC 200 F3, control head operating by means of compressed gas (N2) en-
dowed with software driven magnetic valve:
 Dewar head CC300 head with heating device enabling controllable generation of pres-
sure (working pressure) in the storage vessel:
An additional safety valve (opening pressure 1.2 bar) allowing to degrade possible ex-
cessive pressure in the storage vessel, caused by a defect in isolation or heating.
Should there be any suspicion that the integrity of the

equipment has been compromised (for example as a re-
ATTENTION! sult of damage sustained during transit or during use), it
needs to 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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Handling of Fused Silica Parts and Al2O3-Parts
Fused Silica
Handling
Fused silica parts may only be touched by cotton or powder free latex gloves. Alternatively a fuzz
free tissue can also be used. Otherwise body perspiration or dirt particles could bake into the ma-
terial permanently when touching fused silica parts with the hands. Moreover the properties of the
material might change.
Cleaning
In case of soiled fused silica parts these parts have to be cleaned instantly or latest before heating
up. For cleaning purposes we recommend the use pure alcohol (e.g. ethanol).
Al2O3
Handling
Alumina parts also may only be touched by cotton or powder free latex gloves. Alternatively a fuzz
free tissue can be used. Touching these parts directly with the skin can cause that perspiration or
pollutants stick to the surface and will be visible there permanently.
Cleaning
If nevertheless pollutants are on the alumina they have to be cleaned before any further processing.
The cleaning can be done with pure alcohol, e. g. ethanol or acetone, ethyl alcohol, petroleum
ether. If necessary heat it up to 1600°C in air atmosphere and make an immediate controlled cooling
down to at least < 1000°C.
For further cleaning purposes contact qualified NETZSCH

service staff!
NOTE: Please take care to all safety regulations and laboratory in-
structions for the handling of chemicals!
Before using any cleaning or decontamination methods ex-
cept those specified by the manufacturer, these methods
should be checked in coordination with the manufacturer
to avoid any damage of equipment!

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DSC 3500
Chapter II -
Installation
36098 / Version 2.1 / January 2019 Chapter II / Page 17

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DSC 3500 Installation
Waste disposal
In the European Economic Area (EEA) the disposal of waste equipment is

regulated in the "Directive of the European Parliament and of the Council
on Waste Electrical and Electronic Equipment (WEEE)". The current offi-
cial journal on this matter is available on the European Parliament's
homepage.
The symbol for the separate collection of electrical and electronic equip-
ment is a crossed-out trash can.
Disposal with household waste (unsorted waste) or similar collections of
municipal waste is not permitted! Contact an authorized waste disposal
contractor in your country.
Installation
In most cases, your measuring system will be set up and put into
commission by one of our customer service engineers.
If you would like to set up your instrument yourself, please

read through the following sections carefully.

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Packaging
• If possible, keep the original packaging in which your instrument was delivered.
Should repairs become necessary or should you wish to add additional equipment
to your instrumentation, you can reuse the packaging to ensure damage-free re-
turn transport. Our environment will thank you as well.
• After unpacking, please check all delivered components for possible transport
damage, using the supplied delivery note as a checklist for the individual items.
• Should an item be missing, please contact us immediately.
NOTE!
Important notes for sending goods:

 NETZSCH cannot accept any liability whatsoever for damage caused by
improper packaging. To avoid damage during transport, always ship
components in their original packaging and suitable secondary packag-
ing!
 If the original packaging or the secondary packaging is damaged or no
longer available, packages can be purchased from NETZSCH to ensure a
safe transport of your goods.

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Placement Requirements
 When considering the best placement for your instrument, select:
• Rooms with low traffic and little vibration

• Rooms that are as dust-free as possible
• Rooms with the most constant temperature conditions possible (room tempera-
ture)
• Sturdy lab tables, concrete bases or stable wall brackets. (When using weighting
tables with air or rubber damping, please ensure that the damping behavior is ap-
propriate for the instrument.)
 Avoid:
• Direct sunlight to the instrument

• Drafts from windows, doors and air conditioning
• Placement in rooms with cast plaster or wooden flooring
• Installation in the direct vicinity of transfer stations or systems with strong mag-
netic stay fields
• Setting up thermoanalytical instruments near doors or walls bordering a hallway
or an elevator
measuring system A stable, shock-absorbent table with a working surface of ap-

prox. 2 m x 1 m is required for the measuring device (measuring
cell, computer, printer).
LN2 cooling system The LN2 cooling system requires 1 m x 1 m space. The cooling
(optional) system should be placed beside the table.
Installation Schematics
Refer to the separate booklet „Installation Notes“ for technical specifications

(such as dimensions, weights and connections) and example arrangements of the in-
strument with available devices.

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Connecting the System Components
Connecting the Computer System
Figure 1: Connecting the computer system
For connecting the computer system see also the technical documentation of the
comptuter manufacurer.

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Important notes for Software installation
Your DSC 3500 instrument communicates with the PC using the USB interface of the PC. This re-
quires the installation of suitable drivers delivered together with the Proteus Software.
→ Before initially connecting the DSC 3500 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 3500 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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Connecting the Linear Small Compressor
Figure 2: Connecting the linear small compressor

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Connecting the On-Off Valve Kit for Compressed Air Cooling
Input pressure max. 2 bar absolute (1 bar overpressure)
Figure 3: Connecting the on-off valve kit for compressed air cooling

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Connecting the Cooling device for Pressurized Air
For minimum temperature of 0°C or below (dependent on air pressure). Includes cold air genera-
tor 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)
Figure 4: Connecting the cooling device for pressurized air

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Connecting the Intracooler 40
Figure 5: Connecting the Intracooler 40
The installation of the Intracooler 40 should only be carried out by NETZSCH service
staff!
See separate manual Intracooler 40!

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Connecting the Intracooler 70 (230 V / 50 Hz)
Figure 6: Connecting the Intracooler 70 (230 V / 50 Hz)
staff!

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Connecting the Intracooler 70 (115 V / 60 Hz)
Figure 7: Connecting the Intracooler 70 (115 V / 60 Hz)
The mains connection of the IC 70 (115 V / 60 Hz) must be the same as the
addi-tional AC input (6)!
staff!

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Connecting the LN2 Cooler CC 200 F3
Figure 8: Connecting the LN2 cooler CC 200 F3 with magnetic valve
Please pay attention to all safety regulations for handling liquid nitrogen
(see chapter I)!

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Connecting the LN2 Cooler CC 300
Figure 9: Connecting the LN2 cooler CC 300
See separate manual CC 300!

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Connecting the Gas Supply
Depending on the equipment of the DSC 3500 instrument, the gas supply can be connected to the
following components:
 gas switches with sintering inserts

 mass flow controllers (MFCs)
 gas flow control device (optional)
Connecting the gas switches with sintering inserts
Figure 10: Connecting the gas supply (gas switches with sintering inserts)
 Connect the gas hoses as shown in Figure 10.
Adjusting the gas flow: see chapter IV

See also recommendations for the use of reactive purge gases (chapter I)!

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Connecting the Mass Flow Controllers (MFCs)
Figure 11: Connecting the gas supply (MFCs)
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. There-
fore, 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 ex-
ceeded, 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 I)!
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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Connecting the Gas Flow Control Device (optional) to the gas switches
If the gas flow control device is added a later date, check that the sintering inserts
are removed.
Removing the Sintering Inserts
 Remove the screwing (3x) and sealing

ring (3x).
 The screwings are marked:

40
(40 ml/min = gas flow adjusted by sinter-
ing insert)
60
(60 ml/min = gas flow
adjusted by sintering insert)
If you reinstall the nuts:

Use for "purge 1" and "purge 2" the nuts
marked with 40.
Use for "protective" the nut marked with
60.
Do not forget the seal.

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 Install in the screwing (3x) without sinter-

ing inserts.
Do not forget the seals (3x).
 Connect the gas flow control device as shown above.
 Max. input pressure 0.5 bar (only for gas flow control device).
 See also recommendations for the use of reactive purge gases!

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DSC 3500
Chapter III –
Specific Information
of the Instrument
36098 / Version 2.1 / January 2019 Chapter III / Page 35

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DSC 3500 Specific Information of the Instrument
Appropriate use
The DSC 3500 instrument is used for the determination of melting and glass transition tempera-
tures, grade of crystallization, heat capacity, phase transitions, decomposition points and for the
kinetic consideration of chemical processes.
Reasonable foreseeable misuse

Decomposition of PVC:
PVC samples should only be heated in inert gas atmospheres (N2) to a maximum of 220°C. Other-
wise, HCl can evolve and cause serious damage to the sensor. Use of flammable and/or explosive
gases or gas mixtures. Measurements of flammable and/or explosive materials or samples, which
will release flammable and/or explosive substances during measurement. Opening the furnace
cover at high or very low temperatures.
Safety information for operating the instrument
Safety Note!
 Wear safety boots during transport, commissioning and

maintenance.
NOTE!
 Two persons are required for transport.

 Ensure adequate stability of the instrument and the
substructure (such as table, etc.). Providing a suitable
substructure is the operator‘s responsibility. For the
weight and dimensions of the instrument, as well as for
additional accessories, please refer to the installation
notes.
 All cables and hoses must be installed in accordance
with accident prevention regulations and occupational
health and safety regulations and, where necessary,
covered with cable bridges. It is the operator‘s responsi-
bility to ensure that all such installations are imple-
mented conform to specifications.
 When setting up and positioning the instrument, keep
in mind how to best maintain access to the areas and
parts relevant to functionality. Final determination of
the best possible positioning and optimum access
height is the operator’s responsibility. Refer to EN ISO
14738:2008 for more information regarding ergonomic
recommendations for workstations.
36098 / Version 2.1 / January 2019 Chapter III/ Page 36

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WARNING!
 Use caution when opening the hot furnace. Danger of

burning at the furnace cover, furnace and crucible. Use
tweezers to remove the crucible.
 Use caution in area of cooling outlet! Hot gases can es-
cape here. There is a risk of burns.
 Use caution in area of cooling outlet! Cold gases can es-
cape here. There is a risk of freeze.
Only for instruments equipped with ASC:
 Pay attention during automatic operation of the ASC!
Never reach the hazardous area of moving parts of the
ASC (for example: gripper, arm, magazine cover)!
 Use caution in area of gripper and gripper pins! Gripper
pins are very thin because of constructional reasons. The
gripper pins can penetrate the skin when limbs are
trapped!
 Keep clearance of fingers and any other body part to
the area underneath the gripper pins and piercing pin.
Risk of stab injury because of jerky movement of pierc-
ing pin during operation.
Only for instruments with UV-Extension:
 Pay attention during operation with the UV-Extension!
Only switch on the light source when the light guides
are mounted on the light source as well as on the light
guide attachment.

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DANGER!
 The instrument may only be opened by qualified per-

sonnel. The device must be switched off and discon-
nected from the mains! Work on the electrical supply,
electrical cables and electrical assemblies may only be
carried out by trained personnel (electrical specialists).
 Only inert gases, air and some reaction gases (non toxic,
non combustible) may be used as purge gases.
 Explosive gas mixtures may not be utilized under any
circumstances!
 The sample composition along with the purge gas ap-
plied might result in the emission of harmful outgas-
sing. It is the operator’s responsibility to assess this and
ensure that any exhaust gases are discharged via the
gas outlet.
 Any gases or gas mixtures emerging from the measur-
ing part must, without exception, be properly diverted
by means of an extractor hood.
 The instrument must be purged sufficiently with an in-
ert gas after a measurement.

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Measuring Unit
height
depth
width
Figure 12: Measuring unit DSC 3500
Height: 380 mm
Width: 320 mm
Depth: 520 mm

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Operating Principle
gas outlet
outer lid
inner lids
reference
sample
heat flux sensor
heating
furnace block
cooling inlet purge gas
protective gas
cooling block
cooling outlet insulation
Figure 13: DSC 3500 cross-section of the measuring cell
Differential Scanning Calorimetry (DSC)

Technique in which the difference in heat flow to a sample and to a reference is monitored as a
function of temperature or time, while the sample is subjected to a controlled temperature pro-
gram. (DIN 51007, ASTM E 474).
Furnace  block
 miniature jacketed heater
 furnace temperature is measured by a thermocouple which is integrated
into the furnace wall
Sample cham-  closed with two additional lids

ber  the measuring cell is sealed with the instrument lid
Cooling  nitrogen cooling (liquid)

 air cooling (compressor), compressed air (electrovalve)
Sensor  DSC sensor system type E with high sensitivity
Purge gas  two separate purge gas inlets (sample chamber),

connected via a tee piece
 protective gas (furnace jacket)

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Open the Measuring Cell
cell lids
Figure 14: Open the measuring cell
Open the measuring cell by removing the cell lids.

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Front Panel of the Measuring Unit
Figure 15: Front panel with control LED
Function
blue POWER LED on: instrument is switched on
upper blue LED on: measurement is running

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Rear of the Measuring Unit
Figure 16: Rear of the measuring unit
No. label function

1 USB computer interface connection (USB)
2 LN2 cooling plug connection: liquid nitrogen cooling (6.351.35-00.0.00)
3 115V/T4A; 230V/T2A mains fuses
4 AC input 50/60 Hz power connection 230 (115) V
5 AC line on/off power switch: instrument "on/off"
6 AC input 50/60 Hz power connection 230 (115) V for cooling equipment
7 air cooling plug connection: air cooling (compressor or electrovalve)
8 protective screw connection: protective gas (jacket)
9 purge 2 screw connection: purge gas 2 (sample chamber)
10 purge 1 screw connection: purge gas 1 (sample chamber)
11 cooling out outlet for air and nitrogen cooling
12 cooling in inlet for air and nitrogen cooling
13 CC 300 plug connection: liquid nitrogen cooling CC 300
(0CC30060B10.000-00 or 15.000-00)

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14 optional optional connection

15 cover plate connection for Intracooler
Figure 17: Left side of the measuring unit

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Cooling Devices
Linear small compressor

Linear small compressor for cooling purposes
 Temperature range: 700°C to 40°C

 Quickest possible cooling time from 600°C to 40°C: 20 min
 Linear cooling at 20K/min to 160°C and at 10K/min to 100°C
Technical Specifications:
Voltage, alternating current: 230 V, 50/60 Hz or 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 in air at 20°C):
Allowable temperature of the medium: +5°C to 40°C
Allowable temperature of the environment: +5°C to 40°C
hose, inside diameter 6 mm
Gas connection:
outside diameter 8 mm
Flow medium: air
Weight: 6.6 kg
See separate operating manual!

The installation is described in Chapter II!

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Cooling Device for Compressed Air Cooling
Requirements on-site at customer’s location for compressed air:

 pressure: max. 2 bar absolute (1 bar overpressure)
 oil-free
 pure
 filtered
or
r
ode
3
No. Description
1 control cable
2 magnetic valve
3 compressed air connection (inlet or outlet, depending on device type)
4 compressed air connection (inlet or outlet, depending on device type)
The installation is described in Chapter II

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Cooling Device for Pressurized Air (Vortex)
The cooling device for pressurized air (Vortex) includes a cold air generator and a software-con-
trolled magnetic valve. Temperatures of ≤ 0°C can be reached (depending on the air pressure).
Requirements on-site at the customer’s location for compressed air:

 flow rate of approx. 200 l/min
 min. pressure: 6 bar
 max. pressure: 10 bar
 oil-free
 dry (pressure dew point of < 5°C)
 filtered (25 µm or better)
- Level of noise: up to 70 dB (A)

- Tube between cooling inlet (instrument) and cold air outlet (Vortex
NOTE: tube) should be insulated.
No. Description
1 control cable
2 magnetic valve
3 gas connection (compressed air inlet)
4 gas connection (cold air outlet)
5 outlet (hot air)
The installation is described in Chapter II

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LN2 Cooling System CC 200 F3

LN2 cooling system, operated with compressed gas (N2), software-controlled magnetic valve for
switching the LN2 supply on and off, with LN2 storage vessel.
4
5
2
6 1
10
9
7
Storage vessel (CS 60 S) Dewar head (CC 200 F3)

~ 300 mm / ~ 120 mm
Height: 950 mm Width / Depth:
210 mm
 Storage vessel: 450 mm Height (outside vessel): 4 kg
Width: 555 mm Weight of Dewar head:
Volume: 60 l
Weight empty / 46 / 98 kg
full:
No. Description
1 gas inlet (gas supply, forced N2 , 0.5 bar)
2 shut-off valve (from gas supply)
3 pressure relief valve (open at overpressure 0.5 bar)
4 manometer
5 magnetic valve
6 gas outlet (to instrument)
7 gas outlet (pressure relief)
8 shut-off valve (pressure relief)
9 clamping ring and centering ring
vessel 60 l
10
Please carefully heed all safety regulations for handling liquid nitrogen (LN2) or
gaseous nitrogen (GN2)!
The installlation is described at Chapter II.

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LN2 Cooling System CC 300
The LN2 cooling system CC300 for liquid and low-temperature gaseous nitrogen is used as an ad-
ditional cooling supplement for NETZSCH thermoanalytical instruments.
Dewar head with Dewar head with Storage vessel

supply system supply system and refill-
(without refilling de- ing device (optional)
vice)
Dewar head CS 60 S
Height (outside vessel): 250 mm Height: 950 mm
Weight of Dewar head: 14 kg  Storage vessel: 450 mm
Weight of refilling device: 2 kg Width: 555 mm
Voltage: 115/230V / 50/60Hz Volume: 60 l
Power consumption (max): 550 VA Weight empty / full: 46 / 98 kg
See seperate operating manual!

The installation is described in Chapter II.
Before using liquid nitrogen (LN2) or nitrogen (N2) it is of crucial im-

portance to familiarize oneself with the corresponding safety instruc-
tions. Those can be read through in Chapter I !

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Intracooler 40
Cooling system supplement (compressor cooling) for installation into DSC 214 / DSC 200 F3 / DSC
3500
Temperature range for above mentioned instrument: -40 ... +600°C
Intracooler IC40
Height: 430 mm (w/o hose)

Width: 200 mm
Depth: 360 mm
Weight 24 kg

The installation bis described in Chapter II.

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Intracooler 70
Cooling system supplement (compressor cooling) for installation into DSC 214 / DSC 200 F3 / DSC
3500
Temperature range for above mentioned instrument: -70 ... +600°C
Intracooler IC70
Height: 600 mm (w/o hose)

Width: 380 mm
Depth: 550 mm
Weight 50 kg


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Aluminum Cooling Body

Aluminum cooling body for non-controlled cooling, put on cell manually, max. working tempera-
ture 300°C.

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Gas Flow Control Device
Gas flow control for 3 gas pipes with 3 regulating valves and 3 flow meters.
Gas flow control for 3 gas pipes

Free-standing, including connectors with frits instead of the
device related standard frits, connecting and hose material.
measuring range for purge gases: 2x 6 ... 70 ml/min
measuring range for protective gas: 1x 5 ... 190 ml/min
Maximum input pressure 0.5 bar!
See also recommendations for the use of reactive purge gases in

Chapter I.

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Sealing Press
Sealing press for cold welding or pressure-tight sealing of crucibles. The toolkits must be selected
according to the desired sample container.
Unit
A
A Lever
B Press housing
C C Toolkit fastener
D Base plate
Sealing press no. 6.240.10-80.0.00 is used for sealing different types of crucibles. Each type of cru-
cible requires a different toolkit (see available toolkits). To seal a crucible, position it on the lower
part of the toolkit fastener along with its corresponding lid. Then lower the lever with a single
continuous motion to close or cold weld the crucible. The necessary force is defined by a spring in
the press housing.

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Available Toolkits:
6.240.10-81.0.00
Type of crucible: Toolkit for pressure-tight cold
welding of Al crucibles, Ø 6 mm:
Series 6.239.2-64.5xx
6.240.10-82.0.00
welding of Al crucibles, Ø 6 mm:
Series 6.240.10-65.1xx
6.240.10-83.0.00
Type of crucible: Toolkit for pressure-tight seal-
ing of the medium-pressure cru-
cibles:
6.240.1-68.1.00
6.240.10-85.0.00
welding of Concavus pans:
Series DSC21400A66.xxx
NGB814672
DSC21400A80.030-00
Type of crucible: Toolkit for inserting the slide-in
lids (NGB815051) into the Con-
cavus pan (NGB814672). Espe-
cially for polymer foil samples.
6.240.10-84.0.00
Type of crucible: Stamping tool kit for aluminum
crucibles for SFI-measurements
(Solid Fat Index):
NGB810405 (SFI-measurements)

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DSC 3500
Chapter IV –
Operate the Instrument
36098 / Version 2.1 / January 2019 Chapter IV / Page 56

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DSC 3500 Operate the Instrument
Operating the Instrument

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Short instructions – How to Start a Measurement
Explained below is how to:

 create a baseline
 set up a measurement,
 and measure a sample
Detailed information on the individual steps can be found in the hardware and
software manuals.
1. Make sure that all system components are correctly connected and that the cell is clean.
2. Switch on the com- 60 min

puter system and
measuring unit ap-
prox. 60 min. before
starting the meas-
urement. Start
3. Depending on your
measurement condi-
tions, have available
the required sup-
plies:
liquid nitrogen,
purge gases, etc.

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4. Remove the lids cell lids

from the measuring
cell. Use the twee-
zers for lid for re-
moving the cell lids.
5. Insert two empty

crucibles*.
For application tem-

peratures above
350°C, the crucible
lids should be perfo-
rated.
*for baseline (correc-

tion) measurements
reference position: sample position:

empty crucible empty crucible

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6. Replace the lids. cell lids

Use the tweezers for
lid for inserting the
cell lids.
7. Set the required Option 1: Option 2:

amount of purge (sintering inserts) (gas flow control device)
gas.
If no gas flow device is avail- If your DSC 3500 is equipped with a

able, the actual gas flow gas flow control device the gas flow
value is determined by the can be adjusted via the adjusting
overpressure which is set at knobs on the front.
the gas pressure reducer at
the gas bottle. For each gas
flow channel, i.e. purge 1,
purge 2 and protective a cal-
ibration table is given for
each instrument where it is
shown which nitrogen over-
pressure has to be set in or-
der to achieve a desired ni-
trogen gas flow.

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8. Start the DSC 3500

measurement pro-
gram.
9. Proceed as shown to
create a baseline:  File Menu
New
Measurement Definition
Setup
- check the instrument setup
Header
- select measurement type: Correction
- select temperature calibration file/
sensitivity calibration file
- define all sample settings (e.g. Identity, Name)
- define gases (purge and protective)
Temperature Program
- define all steps of the temperature program
Last Items
- define Filename
click Measure -
the program switches to the adjustment window

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10. Set the temperature

threshold values in
the adjustment dia-
log window.
Switch on the ini-
tial conditions if nec-
essary.
11. Start the measure-

ment.
12. Prepare the sample

and, if necessary,


perforate the cruci- HARDWARE
ble lid. Chapter IV
page Fehler!
Textmarke nicht
definiert.
13. Weigh the sample.

HARDWARE

Chapter IV
page 68
14. Seal the crucible

with the lid. HARDWARE


separate manual

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15. When the cell has cell lids

cooled, remove the
lids. Use the twee-
zers for lid for re-
moving the cell lids.
16. Remove the empty

crucible (right) and
place the sample
crucible on the right-
hand sample sup-
port.
reference position: sample position:

empty crucible sample crucible

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17. Replace the lids. cell lids

Use the tweezers for
lid for inserting the
cell lids.
18.Proceed as shown to
File Menu
combine the sample
measurement with
the correction meas-
urement: 
Open
use file from correction measurement!
sample mass = x mg!
Measurement Definition
Fast Definition
- select measurement type: Correction+Sample
- enter the sample mass in mg!
- define sample settings

e.g. to accept the settings from the
correction measurement (e.g. Identity, Name) set the checkmark for
Get these properties from just opened measurement
- define Filename
click Measure -
the program switches to the adjustment window

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19.Open the NETZSCH

Proteus Analysis pro-
gram.
After the measure-
ment is finished, you
can begin with the
evaluation.

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Preparing the Measurement
In thermoanalytical investigations, the test parameters have a significant influence on the re-
sults.
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 atmosphere
 temperature program
What do you need Assemble the required materials before starting the measurement:
for the measure-  purge gases (sample chamber and furnace jacket) liquid nitrogen
ment? (cooling), forced air (cooling)
 sealing press for cold sealing of Al crucibles
 sealing tool for pressure-tight crucibles
 tweezers (pointed for crucibles, offset for lids)
Calibration Observe below listed important notes:

 The instrument must be calibrated at least once per year.
 Measurements within limit ranges causes shorter calibration cy-
cles.
 It is Operators responsibility to define different calibration cy-
cles/ verification cycles according to valid industry specific stand-
ards.
 Calibration is required if other equipment (e.g. LN2 cooling de-
vice) has been added or removed from the instrument.
 Calibration is required after maintenance or repair (for example
exchange of sensor, thermocouples or electronic components).
 The calibration must be verified (using Indium) at least once per
month.
Please refer to separate Document “Temperature- and Sensitivity Cali-

bration for DSC214/ DSC204F1/ DSC3500” for further information re-
garding calibration of DSC Instruments.

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Calibration Kit A calibration kit is supplied with the DSC 3500.

NETZSCH calibrate your instrument prior to the delivery.
Preparing the When preparing the sample, the effects to be interpreted and the
sample 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 Compact solids, e.g. rubber or thermoplastic, are cut into thin 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 applica-

tion of the sample material increases the danger of
contaminating the heat-flux sensor!
PVC
PVC samples should only be heated in inert gas atmos-
pheres (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 bot-
tom, the lid should be placed on the crucible, with the convex side
down and sealed.
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.

Sirius
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 ma-
terials.) 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 (op-
tional).
The measuring cell must be recalibrated when pressure-tight crucibles
are used.
Evaporation reac- When investigating evaporation reactions, e.g. evaporation of water

tions 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 de- For measurements in defined atmospheres, a needle should be used to

fined atmospheres pierce one to five holes in the lid of the crucible.
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.
Select the sample

crucible Available Crucibles and notes can be found in the sepa-
rate document “Accessories for Differential Scanning Cal-
orimeters and Thermobalances“.
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.

Sirius
 After crimping, the bottom of the crucible must be plane

and free of scratches. If the bottom of the crucible is une-
ven, the heat transfer between the heat-flux sensor and
the sample is impaired!
Seal the crucible Certain types of crucibles can be cold-sealed with a special sealing
press.
The operation of the sealing press is described in a separate

manual!
Insert the Sample

crucibles
The lids could still be hot. Danger of burns! If possible, lay

the lid on the metal plate of the measuring cell.
cell lid
 Remove the cell lid and the interior lid.

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Use the tweezers for lid for removing the separate cell lids.
 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.
ok wrong
Reference crucible
The heat-flux resistance is primarily determined by the cruci-

ble 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 spe-

cific heat, this asymmetry can be compensated by using an
inert reference material.
The properties of the reference material (thermal conductiv-

ity, specific heat, etc.) should be similar to those of the sam-
ple.

Sirius
 Pick up the reference crucible from the top with the twee-
zers and place in the center of the left-hand support of the
heat-flux sensor.
Place the cell lids cell lid
 Replace the interior lid and the cell lid.

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Prior to inserting the lid wait until the furnace has cooled
down to at least 100°C. If the lids are installed at higher tem-
peratures 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.
Generate Purge Gas Atmosphere
Measurements can be run in static or dynamic atmospheres

inside the sample chamber.
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.
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. 40 ml/min
purge 2 approx. 40 ml/min
protective approx. 60 ml/min
If one of the purge gas inlets is not used it has to be closed

with a blind plug.

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Adjusting the gas Option 1: Option 2:

flow (sintering inserts) (gas flow control device)
If no gas flow device is available,

If your DSC 3500 is equipped with
the actual gas flow value is deter-
a gas flow control device the gas
mined by the overpressure which
flow can be adjusted via the ad-
is set at the gas pressure reducer at
justing knobs on the front.
the gas bottle. For each gas flow
channel, i.e. purge 1, purge 2 and
Option 3:
protective a calibration table is
(MFCs)
given for each instrument where it
is shown which nitrogen overpres- The gas flow for purge 1, purge 2
sure has to be set in order to and protective is controlled by the
achieve a desired nitrogen gas means of MFCs and can be ad-
flow. justed via the software (see Help
System Software).
Hints for special For special gas types the overpressure to be set can be calculated ac-
gases by using sin- cording the formula:
tering inserts overpressure to be set for special gas flow = overpressure to be set for
nitrogen* calibration factor
where the calibration factor in good approximation is given by:
calibratio nfactor  geometryfa ctor   specia lg as /  nitrogen
Calibration factors for special gases:
Oxygen 1.01
Argon 1.23
Helium 0.97
The accuracy of the gas flow setting by adjusting the overpressure at
the gas pressure reducer is strongly dependant on the quality of the gas
pressure reducer. Approximately ± 5 ml/min can be achieved.

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Purge gas switching

(O.I.T. extension)
If your instrument is equipped with MFC´s or gas switches with optional

gas flow control device, the gas flow can be programmed switched
on/off via the software (two for purge gas inlet to the sample and one
for protective gas for the measuring cell).
Set the start temperature for the measurement
 The start temperature for the measurement is entered via the soft-
ware.
 It is frequently the case that the temperature in the sample cham-
ber 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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Cooling with the 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.
Handling Be sure that the linear small compressor is connected to the meas-
uring 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 rea-
sons.

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Cooling with Liquid Nitrogen
General information Cooling with liquid nitrogen is required, if:

 cooling processes are being investigated, i.e. if the start tem-
perature is higher than the end temperature.
 measurements that are to be started below 0°C are normally
carried out at a heating rate  5 K/min.
To prevent icing of the measuring cell:
 Feed a dry protective gas, e.g. N2 (60…100 ml/min) into the

furnace jacket (use gas inlet "protective").
 Purge the sample chamber (N2, 40…50 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 (reduces 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 liq-
uid nitrogen (see chapter I).
How to operate the CC300 cooling system

(0CC30060B10.000-00 or 15.000-00)?
See separate operating manual CC 300!

Sirius
Cooling with the LN2 Cooler CC 200 F3 (magnetic valve controlled)
A B
from gas supply
DSC 214
E D
Be sure that the LN2 cooler is connected to the measuring unit (see:
Handling
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 depend-
ing on the software presettings.
Be sure that shut-off valve (A) is closed when dewar is empty.
Close your gas supply.

Removing the LN2 cooler
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.

Sirius
On-Off Valve Kit for Compressed Air Cooling
Be sure that the on-off valve kit for compressed air cooling is con-
Handling
nected to the measuring unit (see: chapter II – Installation).
presettings.
sons.
If liquid nitrogen cooling (6.351.23/24/25/35) is installed the high-

est allowed air pressure is 1 bar overpressure.
If liquid nitrogen cooling (6.351.23/24/25/35) is not installed the
highest allowed air pressure is 2 bar overpressure.
Cooling Device for Pressurized Air

Be sure that cooling device for pressurized air is connected to
Handling the measuring unit (see: chapter II – Installation).
presettings.
sons.
It is not possible to use the cooling device for pressurized
air with simultaneous connected liquid nitrogen cooling!

Sirius
Intracooler 40
Temperature range: -40°C up to 600°C
See separate manual of the Intracooler 40!
Intracooler 70
Temperature range: -70°C up to 600°C
See separate manual of the Intracooler 70!
Maintenance
 Make absolutely sure before every measurement that the

measuring cell is clean.
 Clean the measuring cell with an organic solvent (acetone, al-
cohol), using a lint-free cloth or paper towel.
 Carefully remove heavy soil from the surface with a glass fi-
ber brush or a fine diamond sponge.
Extreme caution should be exercised when using a diamond spo
remove soil.
Do not apply too much force!

 After cleaning remove all particles (vacuuming).
 Afterwards, the cell must be cleaned with acetone and baked

out.

Sirius
 If not absolutely required to achieve the goal of the investiga-

tion, the measurement should not be run to the maximum
temperature of the cell.
 Do not operate the instrument at the maximum temperature
for measurements of longer duration.
To achieve an optimal lifetime of the measuring cell it is rec-
ommended to prevent isothermal segments above 500°C and
heating rates < 10 K/min (exception: baking out the measur-
ing cell for cleaning purposes, see below).
 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 cham-
ber.
 Bake out the sample chamber if it is necessary due to contami-
nations.
Procedure:
 Heat the cell to 600°C (operation with Intracooler: 570°C) and
hold the temperature constant for maximum 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.

Sirius
DSC 3500 Sirius with Automatic Sample Changer (ASC)
The Instrument can be equipped with an automatic sample changer (ASC) optionally. When turn-
ing on the instrument the ASC is automatically switched on. The instrument executes a reference
run automatically at the first motion request. As soon as the gripper has reached its rest position,
the ASC is ready for operation.

Sirius
Measuring Part
5
3
6
2
1 control display (on/off)
2 measuring cell
3 gripper
function key
4 (open/close, emergency stop)
5 cell cover
6 crucible magazine

Sirius
Magazine
The magazine can be loaded with up to 20 crucibles. It can be removed from the instrument by
means of the handhold.
Haltegriff/handhold
Magazin/magazine

Sirius
Control Panel ASC
Funktionstaste/
function key
Function key
Triple assignment of the function key:

 Manual mode (ASC manger off)
open and close the measuring cell and emergency reset during movement
of the ASC
 ASC mode
emergency reset during movement of the ASC

Sirius
Prior to restarting:
 Check crucibles and their correct positioning.
ATTENTION!
If the sample still remains in the gripper after an error (e.g. sample sticks on the gripper) or after
switching on the measuring part, the gripper is moved to the rear position. To open the gripper,
push the function key and remove the sample. After the sample was removed, the measuring cell
is completely opened and operation can be continued.

Sirius
DSC 3500 Sirius with UV-Extension
See separate manual for light source.
The installation of the UV-Extension should only be carried out by NETZSCH service
staff!
Measuring part with UV-extension
Park position (ASC optional) Operating position (ASC optional)

Sirius
Components
No. Funktion
Cover sheet
Guide pin
Clamping screw for optical fibers
Light guide socket
Clamping screw for UV-extension
Clamping screw for light guide socket
Light guide

Sirius
The light guide has to be clamped on the back of the stand and into the light guide socket. The light
guide should protrude down about 1mm from the light guide socket. By loosening the screw 6, the light
guide socket can be aligned centrally to the furnace. By the screws 5, the complete UV extension is
fixed. Connect the DSC to the light source via the trigger cable.
To mount the UV-extension, the ASC must be moved to the "open" position. If the ASC obstruct the
mounting of the UV-extension, the ASC can be turned by hand carefully.
Max. furnace temperature when using the UV-extension is 200 ° C. To avoid mis-
use, a maximum temperature limit of 200 ° C should be set.
The UV-extension and the automatic sample changer may not be used at the
same time. When the ASC is in operation, the UV-extension have to be in the
park position.

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Transport
ATTENTION!
In order to lifting up and transport the measuring part two people are required.
Touch the measuring part on the bottom plate as shown in the figure to lift it upwards.
Cleaning
For cleaning purposes contact qualified NETZSCH service staff!
ATTENTION!
 Please take care to all safety regulations and laboratory instructions for the
handling of chemicals!
 Before using any cleaning or decontamination methods except those specified
by the manufacturer, responsible bodies should check with the manufacturer
that the proposed method will not damage the equipment!

Sirius
DSC 3500
Chapter V -
Appendix
36098 / Version 2.1 / January 2019 Chapter V / Page 90

Sirius
DSC 3500 Appendix
Sealing Tool
General Information
Sealing press for high-pressure sample crucibles 6.239.2-92.3.00, -92.31.00, -92.6.00, -92.8.00, -
92.9.00, -93.3.00, -93.31.00, -93.4.00, and -93.41.00 consisting of base plate, two-part press and ad-
justable torque wrench, with operating instructions.
Complete sub-assembly
(6.239.2-92.4.00)
Sealing press for high-pressure sample crucibles
No. Description
1 support fixture for high-pressure crucibles (GB396775)
2 dynamometric key for high-pressure crucibles (GB396776)

Sirius
DSC 3500 Appendix
Intended Use
The support fixture of the sealing press set is used to correctly position the high-pressure crucible
with sample, which is then closed firmly and tightly with a defined moment of force by means of
a torque wrench.

Sirius
DSC 3500 Appendix
Mounting the Support Fixture for High-Pressure Crucibles
 Mount the support fix-

ture to your table’s work
plate using the butterfly
screws.

Sirius
DSC 3500 Appendix
Adjusting the Torque Wrench
 By pulling the locking

sleeve 1 downward, you
will be able to adjust the
desired moment of force
with the handle 2 .
NOTE!
Please also refer to the man-
ufacturer’s operating man-
ual, which is included in the
scope of delivery!
NOTE!
We recommend a moment of
force of 3.7 Nm for correct
sealing of the crucible!
x = area for reading the value for the
desired moment of force
 Make sure that the lock-

ing sleeve is returned to
its upward position after
adjusting the moment of
force. If necessary, slide it
into this position manu-
ally.

Sirius
DSC 3500 Appendix
Using the Sealing Press Set with a High-Pressure Crucible
NOTE!
The Au sealing discs which are included in the high-pressure

crucible set serve as bursting discs (a safety device).
Before using, please note the following information:
 The Au sealing discs are intended for single usage
only.
 Care must be taken that the protective function of
the Au sealing disc as a bursting disc is not affected
by contamination from the sample itself or by out-
gassing of any substance from the sample. It is the
operator’s responsibility to ensure this.
 Unscrew the guide.

Sirius
DSC 3500 Appendix
 Insert the high-pressure

crucible into the hexagon
support.
 Next, insert the sample.
 Then insert the gold seal-
ing disc centered on top
of the high-pressure cru-
cible.
 Finally, screw on the
high-pressure lid securely
by hand.
NOTE!
For inserting the sample and
positioning the gold sealing
disc, the use of a pair of
tweezers is recommended!
For clean handling,

the use of appropriate gloves
is recommended.
 Screw the guide securely

back onto the foundation
by hand.

Sirius
DSC 3500 Appendix
 Adjust the torque

wrench. See the “Adjust-
ing the Torque Wrench”
section.
ATTENTION!
Please be sure to apply the
prescribed moment of force
here!
 Now insert the torque

wrench into the drill hole
of the guide and move it
downward carefully.
 While carefully rotating
the torque wrench, seek
out the locking notches
on the high-pressure lid.
ATTENTION!
Use extreme caution so that
you do not damage the
grooves on the lid or the
notches on the key!
NOTE!
For this step, use the torque
wrench provided!

Sirius
DSC 3500 Appendix
 Next, insert the square

key into the torque
wrench.
 Hold the handle with

one hand and rotate the
square key at the top
with the other until the
torque wrench clicks and
the desired moment of
force has been reached.
 Afterward, remove the

torque wrench.
 Unscrew the guide.
 Remove the tightly closed
high-pressure crucible
containing your sample.
You can now use it for
your measurement.
NOTE!
Heed the maximum allowa-
ble pressure and temperature
for each crucible!

Sirius
DSC 3500 Appendix
Spare Parts List
Sealing press for high-pressure sample crucibles

6.239.2-92.3.00, -92.31.00, -92.6.00, -92.8.00,
-92.9.00, -93.3.00, -93.31.00, -93.4.00 and
-93.41.00 consisting of base plate, two-part
press and adjustable torque wrench, with oper-
ating instructions 6.239.2-92.4.00
Component Parts of 6.239.2-92.4.00:
No. Description Quantity Order No.:

1 Torque wrench for sealing tool 6.239.2-92.4.00 1 GB396776
2 Guide 1 400 01 02 *
3 Lid support for sealing tool 6.239.2-92.4 1 NGB802623
4 Plate with hexagon insertion for sealing tool 6.239.2-92.4 1 NGB803373
5 Countersunk screw M4x16 2 400 01 05 *
6 Foundation 1 400 01 06 *
7 Base 1 400 01 08 *
8 Setscrew No.6 2 400 01 11 *
11 O-ring Ø 47x4 1 400 01 12 *
12 O-ring seal made of Viton (FKM), Ø 8 x 1.5 mm 2 NGB800590
13 Bit 1 NGB802622
*= only on request

Sirius
DSC 3500 Appendix
Technical Specifications
Refer to the document “Installation Notes”, which is included within the scope of delivery, for a selection
of technical specifications.
Heating System
Temperature range: -170 °C … 600 °C
Heating rates: 0.001 … 100 K/min (dependent on final temperature)

Cooling rates: 10 K/min down to -150 °C
Cooling System
(cooling times for nonlinear, non-controlled cooling)
liquid nitrogen: -170 °C … 600 °C

Cooling time 600 °C to -100 °C: typically 15 min
linear small compressor: RT … 600 °C
Cooling time 400 °C to 40 °C: typically 35 min
compressed air cooling: RT … 600 °C
Cooling time 400 °C to 40 °C: typically 20 min
(depending on air flow)
aluminum cooling body: For nonlinear cooling after measurement at temperatures

below 300 °C
Cooling time 300 °C to 100 °C: > 20 min
(depending on cooler temperature at beginning of cooling period)
Intracooler 40: -40 °C … 600 °C

Minimum cooling time from room temperature to -40 °C is
around 30 minutes*
(*Values are determined for an ambient temperature of 20 °C)
Intracooler 70: -70 °C … 600 °C

Minimum cooling time from room temperature to -70 °C is
around 30 minutes*
(*Values are determined for an ambient temperature of 20 °C)
Measuring System
DSC measuring range: -40 °C: +/- 600 mW

160 °C: +/- 650 mW
400 °C: +/- 850 mW
Technical resolution: 0.2 µW/digit
RMS noise: 1 µW
Peak-to-Peak noise: 5 µW
Enthalpy precision: 0.05 % (for indium)
Enthalpy accuracy: < 1 % for metals, < 2 % for most materials
Atmosphere
Gas atmosphere inert, oxidizing, static and dynamic operation

Sirius
DSC 3500 Appendix
Dimensions in mm (w x d x h) / Weight (net) in Kg
Measuring unit: 320 x 520 x 380 / 28
Power Supply
230 V / 115 V, 50 Hz / 60 Hz,

< 600 W (without cooling accessory)
Operational Conditions
Indoor use (laboratory)

Ambient temperature 20 °C +/- 5 °C
Relative air humidity 60 % +/- 20 %
Atmospheric pressure 1013 hPa +/- 30 hPa
Wall distance min. 30 cm
Technical specifications are subject to change

Sirius
DSC 3500 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.

TA for Polymers and Additives DSC-TG-DMA
Selb, Würzburg 1993
Kaisersberger E.; Knappe S.; Möhler H.; Rahner S.

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
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

Sirius
DSC 3500 Appendix
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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Operating Manual

DSC 3500 Sirius®

36098 / Version 2.1 / January 2019

36098 / Version 2.1 / January 2019 Contents / Page I

OPERATING PRINCIPLE ............................................................................................................ 40

36098 / Version 2.1 / January 2019 Contents / Page II

HINTS FOR SPECIAL GASES BY USING SINTERING INSERTS .......................................................................... 73

36098 / Version 2.1 / January 2019 Contents / Page III

36098 / Version 2.1 / January 2019 Chapter I / Page 1

Duplication Any duplication or transmission of this document, both electronic and

Proposals We welcome any comments, suggestions or new ideas con-

It is our pleasure to offer service contracts for our customers.

In case there is no existing service contract for your device, we invite

36098 / Version 2.1 / January 2019 Chapter I / Page 2

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

Any use exceeding the (expanded) authorized operation is considered

Responsibility Responsibility for commissioning, operation and maintenance must be

36098 / Version 2.1 / January 2019 Chapter I / Page 3

Removal of Protective Removing protective devices of the Instrument is solely permitted

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

The operating instruction should be placed in a suitable location at the

36098 / Version 2.1 / January 2019 Chapter I / Page 4

Warning signs should be posted in appropriate places and be in accord-

36098 / Version 2.1 / January 2019 Chapter I / Page 5

This symbol refers to more detailed information which can be

Refer to instruction manual / booklet

Wear safety footwear

Wear protective gloves

Opaque eye protection must be worn

36098 / Version 2.1 / January 2019 Chapter I / Page 6

Wear face shield

36098 / Version 2.1 / January 2019 Chapter I / Page 7

Information for the usage of Purge Gases

36098 / Version 2.1 / January 2019 Chapter I / Page 8

The following standards need to be observed and followed unconditionally:

Explosive gas mixtures may not on any term be utilized!

Subsequent we offer a selection of purge gases including their limiting properties.

The list makes no claim to be complete.

Helium (He)  chemically inert (inert gas)

Argon (Ar)  chemically inert (inert gas)

Nitrogen N2  largely inert

36098 / Version 2.1 / January 2019 Chapter I / Page 9

Carbon dioxide (CO2)  non-toxic

Hydrogen (H2)  flammable

Ammonia (NH3)  toxic

Carbon monoxide (CO)  toxic

Hydrogen sulphide (H2S)  toxic

36098 / Version 2.1 / January 2019 Chapter I / Page 10

Other reducing gases or gas mixtures

The instrument is unsuitable for usage in atmosphere of

Chlorine (Cl2)  very toxic

Hydrogen chloride (HCl)  toxic

Sulphur dioxide (SO2)  toxic

Fluorine (F2)  very toxic

Hydrogen fluoride (HF)  very toxic

36098 / Version 2.1 / January 2019 Chapter I / Page 11

Safety Regulations for Handling Nitrogen/ Liquid Nitrogen LN2

Characteristics  Colorless, inert, harmful and incombustible liquid. Due to its

Safety Instructions  Handling a higher quantity of Nitrogen requires the availability