PerkinElmer DSC 4000 Installation And Hardware Manual

THERMAL ANALYSIS

DSC 4000
Installation and Hardware
Guide

Release History

Part Number Release Publication Date

09931392 A September 2017

Any comments about the documentation for this product should be addressed to:

User Assistance
PerkinElmer, Inc.
710 Bridgeport Avenue
Shelton, Connecticut 06484-4794
U.S.A.

Notices

The information contained in this help file is subject to change without notice .

Except as specifically set forth in its terms and conditions of sale, PerkinElmer makes no
warranty of any kind with regard to this help file, including, but not limited to, the implied
warranties of merchantability and fitness for a particular purpose.

PerkinElmer shall not be liable for errors contained herein for incidental consequential damages in
connection with furnishing, performance or use of this material.

Copyright Information

This help file contains proprietary information that is protected by copyright.
All rights are reserved. No part of this file may be reproduced in any form whatsoever or translated into

any language without the prior, written permission of Perk inElme r, Inc.
Copyright © 2017 PerkinElmer, Inc.

Trademarks

Registered names, trademarks, etc. used in this help file, even when not specifically marked as such,
are protected by law.

PerkinElmer is a registered trademark of PerkinElmer, Inc.
Pyris is a trademark of PerkinElmer, Inc.

Microsoft and Windows are registered trademarks of Microsoft Corporation in the United States and
other countries.

Contents

Introduction ............................................................................................... 5

Pyris Installation ............................................................................................... 6

Safety and Regulatory Information ........................................................... 7

Symbols Used in Online Help ............................................................................. 8

Symbols Used on the Instruments ...................................................................... 8

Electrical Warnings ...........................................................................................12

Electromagnetic Compatibility (EMC) .................................................................14

Electrical Safety ...............................................................................................15

WEEE Instructio ns for PerkinElmer Products ......................................................16

Prepare the Laboratory ............................................................................ 18

Prepare the Laboratory .....................................................................................19

Electrical Requirements ..............................................................................19

Environmental Requirements ......................................................................19

Purge Gas and Pneumatic Supply ...............................................................20

Space Requirements ..................................................................................20

Install Multiple Analyzers ........................................................................ 23

Install Multiple Analyzers ..................................................................................24

Install a DSC 4000 ................................................................................... 27

Safety Preca utio ns for t he DSC 40 00 .................................................................28

DSC 4000 Warning Labe ls .................................................................................32

Warning Labels on the Upper Ring Around the Furnace................................32

Warning Labels on the Back of the DSC 4000 ..............................................34

Install a DSC 4000 ...........................................................................................36

Unpacking the DSC 4000 ..................................................................................37

Set Up the DSC 4000 System Components .........................................................39

Select the Correct Voltage for the DSC 4000 ...............................................39

Connect the Purge Gas Supply to the DSC 4000 ..........................................41

Connect the Purge Gas and System Purge Gas Lines to the DSC 4000 ..........41

Connect the Cooling Device to the DSC 4000...............................................42

Connect the DSC 4000 System Components ......................................................47

Configure the DSC 4000 ...................................................................................48

Starting the Pyri s Manager .........................................................................49

Calibrate the DSC 4000.....................................................................................50

DSC 4000 Hardware ................................................................................. 53

DSC 4000 ........................................................................................................54

Furnace and Sensor Design ........................................................................54

Cooling .....................................................................................................55

Calibration of the DSC 4000 ..............................................................................56

Temperature Calibration ............................................................................56

Perform Indium and Zinc Runs ...................................................................57

Perform a Peak Area with Onset Calculation ................................................57

Performing a Temperature Calibration.........................................................58

Heat Flow Calibration .................................................................................58

Operating Variables and Sample Handling ..........................................................60

Temperature Range ...................................................................................60

Scanning Rate ...........................................................................................60

Subambient Operation of the DSC 4000 .............................................................61

DSC 4000 Maintenance .....................................................................................62

DSC 4000 Part N umbers ...................................................................................63

Miscellaneous Part Numbers .......................................................................64

AS 6000 Autosampler............................................................................... 65

AS 6000 Autosam pler ....................................................................................... 66

Safety Precautions for the AS 6000 ................................................................... 68

How the AS 6000 Autosampler Works ............................................................... 69

Autosampler Work Cycle ............................................................................ 69

Reduced Time Cycle .................................................................................. 71

AS 6000 Autosampler Gripper Alignment ........................................................... 72

AS 6000 Sample Hand ling ................................................................................ 73

Sample Preparation ................................................................................... 73

Sample Pans ............................................................................................. 73

Sample Loading ........................................................................................ 73

Running a Play List with the AS 6000 ................................................................ 76

Troubleshooting .............................................................................................. 80

Error Messages from the DSC 4000 ............................................................ 83

AS 6000 Autosampler Maintenance ................................................................... 84

Cleaning and Decontamination ................................................................... 84

Install a Reference Pan in a DSC 4000, DSC 6000, Pyris 6 DS C or Jade DSC

with AS 6000 Autosampler ............................................................................... 85

Introduction

6 . DSC 4000 Installation and Hardware Guide

Pyris Installation

NOTE: If you are going to install multiple analyzers, or just want to install a universal serial

bus, see

This user’s guide gives information on the installation of your PerkinElmer Thermal Analysis
System, and details about the operation and maintenance of the hardware. This information
can also be found in the Pyris Installation and Har d ware Help provided with your Pyris
software.

Information on the operation of the Pyris software can be found in the software Help.
In general, the installation procedure consists of the following steps:

• Prepare the laboratory

• Unpack the thermal analysis system

• Set up the required system components (for example, purge gases, cooling supply, and

analyzer-specific items)

Install Multiple Analyzers

before you begin to install an analyzer.

• Connect the system components

• Configure the analyzer

• Calibrate the analyzer

Safety and Reg ul at ory

Information

8 . DSC 4000 Installation and Hardware Guide

Symbols Used in Thi s Manual

Bold text refers to text that is displayed on the screen.
UPPERCASE text, for exampl e ENTER or ALT, refers to keys on the computer keyboard. '+' is

used to show that you have to press two keys at the same time, for example, ALT+F.
All eight-digit numbers are PerkinElmer par t numbers unless stated otherwise.

Notes, Cautions and Warnings

Three terms, in the following standard formats, are also used to highlight special
circumstances and warnings.

NOTE: A note indicates additional, significant information that is provided with some

procedures.

CAUTION

einen Geräteschaden zu vermeiden.

undgå en beskadigelse af apparatet.

este tipo de circunstancias.

figurent dans un encadré semblable à celui-ci.

riquadro come questo.

opgevolgd, om beschadiging van het instrument te voorkomen.

Safety and Regulatory Informati on . 9

We use the term CAUTION to inform you about situations that could
result in serious damage to the instrument or other equipment. Details
about these circumstances are in a box like this one.

Caution (Achtung)

Bedeutet, daß die genannte Anleitung genau befolgt werden muß, um

Caution (Bemærk)

Dette betyder, at den nævnte vejledning skal overholdes nøje for at

Caution (Advertencia)

Utilizamos el término CAUTION (ADVERTENCIA) para advertir sobre
situaciones que pueden provocar averías graves en este equipo o en
otros. En los recuadros como éste se proporciona información sobre

Caution (Attention)

Nous utilisons le terme CAUTION (ATTENTION) pour signaler les
situations susceptibles de provoquer de graves détériorations de

l'instrument ou d'autre matériel. Les détails sur ces circonstances

Caution (Attenzione)

Con il termine CAUTION (ATTENZIONE) vengono segnalate
situazioni che potrebbero arrecare gravi danni allo strumento o ad
altra apparecchiatura. Troverete informazioni su tali circostanze in un

Caution (Opgelet)

Betekent dat de genoemde handleiding nauwkeurig moet worden

Caution (Atenção)

Significa que a instrução referida tem de ser respeitada para evitar a
danificação do aparelho.

10 . DSC 4000 Installation and Hardware Guide

Verletzung des Benutzers kommen kann.

overholdes.

este tipo de circunstancias.

dans un encadré semblable à celui-ci.

informazioni su tali circostanze in un riquadro come questo.

genomen, dit kan leiden tot verwondingen van de gebruiker.

We use the term WARNING to inform you about situations that could
result in personal injury to yourself or other persons. Details about
these circumstances are in a box like this one.

WARNING

Warning (Warnung)

Bedeutet, daß es bei Nichtbeachten der genannten Anweisung zu einer

Warning (Advarsel)
Betyder, at brugeren kan blive kvæstet, hvis anvisningen ikke

Warning (Peligro)

Utilizamos el término WARNING (PELIGRO) para informarle sobre
situaciones que pueden provocar daños personales a usted o a otras
personas. En los recuadros como éste se proporciona información sobre

Warning (Danger)

Nous utilisons la formule WARNING (DANGER) pour avertir des
situations pouvant occasionner des dommages corporels à l'utilisateur
ou à d'autres personnes. Les détails sur ces circonstances sont données

Warning (Pericolo)

Con il termine WARNING (PERICOLO) vengono segnalate situazioni
che potrebbero provocare incidenti alle persone. Troverete

Warning (Waarschuwing)

Betekent dat, wanneer de genoemde aanwijzing niet in acht wordt

Warning (Aviso)

Significa que a não observância da instrução referida poderá causar um

ferimento ao usuário.

Safety and Regulatory Informati on . 11

Caution

off

Symbols Used on t he Ins trume nts

Caution, hot surface.
Attention surface chaude.

Caution, risk of electric shock.
Attention, risque d'électrocution.

Documentation must be consulted to determine
the nature of the potential hazard and any actions which have to be
taken.

Attention
La documentation doit être consultée pour déterminer
La nature du risque potentiel et des actions qui doit être pris.

Caution – Cold surface
Attention, Surface froide

The following additional graphic symbols used on the instrument:

Indicates alternating current

Indicates the primary protective gr ounding terminal

Indicates the

Indicates the on position of the main power switch

position of the main power switch

12 . DSC 4000 Installation and Hardware Guide

connected to true electrical ground. Any interruption of the protective

terre de prote ction peut nuire à la protection fournie par l'instrument.

Electrical Warnings

Connect the instrument to an AC line p ower outlet that has a
protective ground connection. To ensure satisfactory and safe

WARNING

operation of the instrument, it is essential that the protective ground
conductor (the green/yellow lead) of the line power cord is

AVERTISSEMENT

WARNING

ground conductor, inside or outside the instrument, or disconnection
of the protective ground terminal may impair the protection provided
by the instrument.

Connectez l'instrument à une prise de courant de ligne AC qui a une
connexion de terre de protection. Pour assurer un fonctionnement
satisfaisant et sécurisé de l'instrument, il est essentiel que le
conducteur de terre de protection (le fil vert / jaune) du cordon
d'alimentation de la ligne soit connecté à une vraie terre électrique.
Toute interruption du conducteur de terre de protection, à l'intérieur
ou à l'extérieur de l'instrument, ou la déconnexion de la borne de

Do not operate the instrument with any covers or parts removed.

Ne pas utiliser l'instrument avec des couvertures ou des pièces
retirees.

AVERTISSEMENT

Do not attempt to make adjustments, replacements, or repairs to
this instrument except as described in this help file. Only a

WARNING

PerkinElmer service representative should be permitted to service
the instrument.

N'essayez pas de faire des ajustements, des remplacements ou des
réparations à cet instrument, sauf comme décrit dans ce fichier

AVERTISSEMENT

d'aide. Seul un représentant du service PerkinElmer devrait être
autorisé à servir l'instrument.

Safety and Regulatory Informati on . 13

N'utilisez que des fusibles avec la note de courant requise et du type

Use only fuses with the required current rating and of the specified
type for replacement.

WARNING

AVERTISSEMENT

spécifié pour le remplacement.

14 . DSC 4000 Installation and Hardware Guide

Electromagnetic Compatibility (EMC)

Europe

All information concerning EMC standards is in the Declaration of Conformity, and these
standards may change as the European Union adds new requirements.

PerkinElmer instruments have been designed and manufactured, having regard to the state
of the art, to ensure that:

• the electromagnetic disturbance generated does not exceed the level above which
radio and telecommunications equipment or other equipment cannot operate as
intended;

• it has a level of immunity to the electromagnetic disturbance to be expected in its
intended use which allows it to operate without unacceptable degradation of its
intended use.

South Korea

This device complies with MSIP (Ministry 0f Science, ICT, and Future Planning) EMC
Registration requirements. This instrument is reg istered as a Class B instrume nt for
residential and/or buiness use.

B급 기기 (가정용 방송통신기자재)
이 기기는 가정용(B급) 전자파적합기기로서 주
로 가정에서 사용하는 것을 목적으로 하며, 모든
지역에서 사용할 수 있습니다.

United States (FCC)

This equipment has been tested and found to comply with the limits for a Class B digital
device, pursuant to part 15 of the FCC Rules. These limits are designed to provide rea sona b le
protection against harmful interference when the equipment is operated in a commercial
environment. This equipment generates, uses, and can radiate radio frequency energy and, if
not installed and us ed in accordance with the instructi on manual, may cause harmful
interference to radio communications. Operation of this equipment in a residential
environment may cause harmful interference in which the user will be required to correct the
interference at their own expense.

NOTE: Changes or modifications not expressly approved by PerkinElmer could cause the

instrument to violate FCC (U.S. Federal Communicat ions Commission) emission
regulations, and because of this violation could void the user’s authority to operate
this equipment.

Safety and Regulatory Informati on . 15

Electrical Safety

This analyzer conforms to IEC publication 61010-1 (“Safety requirements for electrical
equipment for measurement, control and laboratory use”) as it applies to IEC Class 1
(earthed) appliances, and therefore meets the requirements of the Low Voltage Directive
2006/95/EC.

Pollution Degree 2

This product will operate safely in environments that contain nonconductive foreign matter
up to Pollution Degree 2 in EN/IEC 61010-1.

Normally only non-conductive POLLUTION occurs. Occasionally, however, a temporary
conductivity caused by condensation must be expected.

16 . DSC 4000 Installation and Hardware Guide

WEEE Instructions for PerkinElmer Pro ducts

or

A label with a crossed-out wheeled bin symbol and a rectangular bar indicates that the
product is covered by the Waste Electrical and Electronic Equipment (WEEE) Directive and is
not to be disposed of as unsorted municipal waste. Any products marked with this symbol
must be collected separately, according to the regulatory guidelines in your area.

The objectives of this program are to preserve, protect and improve the quality of the
environment, protect human health, and utilize natural resources prudently. Requirements
for waste collection, reuse, recycling, and re c overy programs vary by regulatory authority at
your location. Contact your loca l r esponsible body (for example, your laboratory manager) or
authorized representative for informat ion reg arding applicable disposal regulations. Contact
PerkinElmer at the web site listed below for information specific to PerkinElmer products.

Web address:

www.perkinelmer.com/WEEE

For Customer Care telephone numbers select “Contact us” on the web page.
Products from other manufacturers may also form a part of your PerkinElmer system. These

other producers are directly responsible for the collection and processing of their own waste
products under the terms of the WEEE Directive. Please contact these producers directly
before discarding any of their products.

Consult the PerkinElmer web site (above) for producer names and web addresses.

Safety and Regulatory Informati on . 17

Prepare th e Lab orat ory

Prepare the Laboratory . 19

Prepare the Laboratory

The following sections describe requirements for your Thermal Analysis System. Make sure
your laboratory meets all of the requirements before you try to install the system. You should
step through the topics in the order presented below.

Before starting installation, please read the Safety and Regulatory Information.

• Electrical Requirements

• Environmental Requirements

• Purge Gas and Pneumatic Supply Requirements

• Space Requirements

Electrical Requirements

Power Source

An independent power source should be provided for the system, including the computer.
The power source should not be associa ted with heavy-duty equipment such as large motors,
or with possible sources of high-frequency interference such as photocopying systems,
discharge lamps, or radio transmitters. The power supply should be fused at a maximum of
20 A (120 V systems) or 16 A (200–240 V systems).

Line Voltage

PerkinElmer analyzers and their associated inst ruments are designed to operate within a line
voltage range of 10% of the nameplate voltage or other such voltage selected at installation
to suit the particular country or region. (The range for 240 V systems is +6%, –10%.) The
supply must be smooth, clean, earthed and free of transient voltages over 40 V.

The frequency range is ±1% for 50 Hz and 60 Hz systems.

Instrument Maximum Power Requirements

Refer to the Safety Precautions for the instrument.

Environmental Requirements

You must provide the following laboratory conditions for your Thermal Analysis System:

• A clean area, free from vibration and strong magnetic fields.

• An adequate and stable power source for all system components.

• The area must have a relative humidity of 20–75% (without condensation).

• For optimum performance, the temperature of the area should be between 10 °C and

35 °C (50 °F and 95 °F).

• The instrument will operate safely between 5 °C and 40 °C.

• Place the system components in an area that is not in direct sunlight or direct contact

with heating and co oling ducts or units.

20 . DSC 4000 Installation and Hardware Guide

• The instruments are for indoor use only.

• The storage temperature is between 20 °C and 60 °C.

• The altitude limitation for the operation of this instrument is 2000 m.

• The altitude for storage of this instrument is 0–12000 m.

• The installation overvoltage ca tegory for all instruments is Category II.

• The pollution degree is 2 for all instruments. (This product will operate safel y in

environments that contain nonconductive foreign matter up to Pollution Degree 2 in
EN/IEC 61010-1.)

• The instrument must be positioned so that the appliance coupler can be removed to
completely disconnect the power from the instrument.

NOTE: If the equipment is used in a manner not specified by PerkinElmer, the protection

provided by the equipment may be impaired.

Purge Gas and Pneumatic Supply

The recommended purge gas for all Thermal Analyzers at ambient temperatures is argon or
nitrogen with a minimum purity of 99.9%. Other gases, such as air or oxygen, may also be
used. Air or oxygen is recommended for the purge gas when performing oxidation studies
(DSC analyses).

The purge gas for any instrument must be dry. Use a size 1A cylinder equipped with a
pressure regulator that has a shutoff valve at the outlet. The shutoff valve should have
1/4-in. NPT male threads on the outlet side for connection to the analyzer’s purge gas line.

Space Requirements

Refer to the Safety Precautions for the instrument.
Once all of the above requirements are met, you can install your analyzer.

Prepare the Laboratory . 21

Install Multiple Analyzers

24 . DSC 4000 Installation and Hardware Guide

Install Multiple Analyzers

The only way to attach multiple instruments to your computer is via a universal serial bus.
PerkinElmer no longer supports the Multiport RS-232 Card (P/N 09402018). Installation of
the universal serial bus MUST be done before insta lling any analyzer.

A Pyris Series USB Multiport is an RS-232 module that uses the USB port on the PC and
features plug-and-play intelligent connectivity. The USBs supported by PerkinElmer are the
EdgePort/4 (P/N 09402020) and EdgePort/8 (P/N 09402019). They eliminate the need to
install cards into dedicated computer slots and reconfigure the system. Computers with
standard USB allow peripherals to be automatically configured as soon as they are physically
attached without the need to reboot or run setup.

NOTE: Some PerkinElmer analyzers now have USB ports in addition to, or sometimes in

place of, RS-232 ports. If you are working with these analyzers, you will need to use
a USB hub device instead of the Edgeport to con nect multiple analyzers to a single
computer. A suitable 7-port USB hub is availa ble (P/N HH10151008). Contact your
PerkinElmer Service Representative for further information.

To install an EdgePort:

1. Attach one end of the USB cable to one of the USB connectors at the back of the
computer.

Install Multiple Analyzers . 25

2. Attach the other end of the connector cable to the USB port on the EdgePort.

EdgePort/4

EdgePort/8

DO NOT connect any instruments to the EdgePort at this time.

If your computer is connected to the Internet, it will now download the software drivers
for the EdgePort. Once this process is completed, you can install the individual analyzers
by connecting them to the RS-232 ports on the EdgePort and configuring them in the
Pyris software.

26 . DSC 4000 Installation and Hardware Guide

Install a DSC 4000

28 . DSC 4000 Installation and Hardware Guide

Be sure that all instrument operators read and understand
the following precautions. It is advisable to post a copy of
these precautions on or near the instrument itself.

Assurez-vous que tous les opérateurs d' instr uments lisent
et comprennent les précautions suivantes. Il est conseillé
de publier une copie de ces précautions sur ou près de
l'instrument lui-même.

Never touch the outer and inner furnace lid s. The
temper at ur e o f the furnac e c a n re a c h a s h ig h as 445 ° C. Use
tweezers to remove the lids.

Ne touchez jamais les couvercles extérieurs et intérieurs du
four. La température du four peut atteindre 445 ° C. Utiliser
une pince à épiler pour enlever les couvercles.

Safety Precautions for the DSC 4000

WARNING

AVERTISSEMENT

The following precautions must be observed before and when using the DSC 4000
Differential Scanning Calorimeter:

• Before connecting the DSC 4000 to the main outlet, check the main voltage setting and
fuse.

• The DSC 4000 requires a good earth ground that is common to the earth ground of the
computer.

• Check that the power cord supplied is appropriate for your country and is undamaged
before connecting it to the main voltage supply.

• Use proper lifting posture when lifting the analyzer. The DSC 4000 with autosampler
weighs 19 kg. Lift the autosampler from underneath. Never attempt to lift the analyzer
by the autosampler (if installed) or by any cables a ttached.

• When cleaning the instrument, consul t PerkinElmer if there is any doubt about the
compatibility of decontamination or cleaning agents with parts of the equi pment or with
material contained in it.

WARNING

AVERTISSEMENT

Install a DSC 4000 . 29

Do not touch the inside of the fur nace; it might be hot and
internal pollution can cause loss of performance.

Ne pas toucher l'intérieur du four; il pourrait être chaud et
la pollution interne peut entraîner une perte de
performance.

Always ensure that there is adequate ventilation when
operating the DSC 4000. O pe r a te t he D SC 4000 in a f ume
hood.

Assurez-vous toujours qu'il existe une ventilation adéquate
lorsque vous utilisez le DSC 4000. Faites fonctionner le DSC
4000 dans u ne ho tt e a sp i ra nt e .

ques. Si

aucun refroidissement externe n'est a ppliqué, n'utilisez pas le DSC 4000

dessus de 50 ° C. Le DSC 4000 s'éteint automatiquement lorsque la

température intérieure monte au-dessus de 70 ° C.

WARNING

AVERTISSEMENT

WARNING

AVERTISSEMENT

CAUTION

ATTENTION

Do NOT expose the sensor surfaces to mechanical stress. If no external
cooling is applied, do not operate the DSC 4000 above 50 °C. The DSC
4000 will automatically shut off when the inner temperature rises above
70 °C.

NE PAS exposer les surfaces du capteur aux contraintes mécani
au-

CAUTION

ATTENTION

Do not exert excessive forces on the sensor disks.
Ne pas exercer de forces excessives sur les disques du capteur.

30 . DSC 4000 Installation and Hardware Guide

de la manipul ation du couver cle
du four extérieur, de sorte que sa doublure en céramique n'est pas
endommagée..

CAUTION

ATTENTION

• Avoid contamination of the furnace, use high-purity purge gases to purge any reaction
products out of the furnace, and heat the furnace to temperatures above 430 °C ONLY
when absolutely necessary.

• Check that the cooling liquid supply is circulating before starting a run.

• Ensure the purge gases are set to the recommended flow rates. A rate that is too high

will disturb the inner furnace lid.

• Do not operate the instrument in a cold room. The ambient temperature and the
temperature of the instrument should be between 10 °C and 30 °C.

• Never open the furnace when it is at an elevated temperature.

Care must be taken when handling the outer furnace lid so its ceramic
lining is not damaged.

Des précautions doivent être prises lors

Important Specifications

Maximum power consumption 430 VA
Supply voltage 100–120 V or 220–240 V
Supply voltage frequency 50–60 Hz
Fuses 6.3 AT or 3.15 AT
Safe temperature range 10–40 °C
Dimensions L x H x D 38 x 17 x 41 cm (H 29 cm with autosampler)
Weight 17 kg (19 kg with autosampler)

Install a DSC 4000 . 31

Decontamination and Cleaning

Decontamination

Before using any cleaning or decontamination methods except those specified by
PerkinElmer, users should check with PerkinElmer that the proposed method will not damage
the equipment.

Customers wishing to return instrumentation and/or associated materials to
PerkinElmer for repair, maintenance, warranty or trade-in purposes are advised
that all returned goods must be certified as clean and free from contamination.

The customer's responsible body is required to follow the “Equipment Decontamination
Procedure” and complete the “Certificate of Decontamination”. These documents are
available on the PerkinElmer public website:

http://www.perkinelmer.com/Content/technicalinfo/dts_instrumentdeconprocedure.pdf
If you do not have access to the internet contact Customer Care:

Customer Care USA:

(8:30 a.m. – 7 p.m. EST)

1-800-762-4000 (inside the USA)
([phone] (outside the USA)

Customer Care Canada: 800-561-4646
Customer Care EU: 0800 40 858 (Brussels)

0800 90 66 42 (Monza)

If you are located outside of these regions, please call your local PerkinElmer sales office for
more information.

Cleaning the Instr ument

Exterior surfaces may be cleaned with a soft cloth, dampened with a mild detergent and
water solution. Do not use abrasive cleaners or solvents.

General Laboratory Safety

Your laboratory should have all equipment ordina r ily required for the safety of individuals
working with chemicals (fire extinguishers, first-aid equipment, safety shower and eye-wash
fountain, spill cleanup equipment, etc.).

32 . DSC 4000 Installation and Hardware Guide

HOT SURFACE
The furnace at the center of the ring may be hot.

SURFACE CHAUDE
Le four au centre de l 'anneau peut être chaud.

DSC 4000 Warning Labels

Warning Labels on the Upper Ring Around the
Furnace

WARNING

AVERTISSEMENT

NOTE: If you have an autosampler installed, this labe l is positioned on the autosampler.

Toxic Gases – Fume Ventilation System

.

Gaz toxiques - Système de ventilation des fumées

.

WARNING

Install a DSC 4000 . 33

Without adequate ventilation, potentially toxic vapors can build up
in the laboratory. Your laboratory must have a reliable fume
ventilation system before you use this instr ument

AVERTISSEMENT

Sans ventilation adéquate, des vapeurs potentiellement toxiques
peuvent s'accumuler en laboratoire. Votre laboratoire doit disposer
d'un système de ventilation fiable avant d'utiliser cet instrument

34 . DSC 4000 Installation and Hardware Guide

Always keep airflow unobstructed

Toujours garder le flux d'air dégagé

For protection against fire hazard replace only with the
same type and rating of fuse

Pour la protection contre les risques d'incendie, remplacer
uniquement par le même type et le même type de fusible

Warning Labels on the Back of the DSC 4000

WARNING

AVERTISSEMENT

WARNING

AVERTISSEMENT

To maintain adequate ventilation do not block the back of the
instrument.

Pour maintenir une ventilation adéquate, ne bloquez pas l'arrière de
l'instrument.

.

.

Install a DSC 4000 . 35

Grounding circuit continuity is vital for the safe operation of
equipment. Never operate equipment with the grounding
connector disconnected. Disconnect supply cord before
operating

La continuité du circuit de mise à la terre est essentielle
pour la sécurité de fonctionnement de l'équipement.
N'utilisez jamais d'équipement avec le conne cteur de mise à
la terre déconnecté. Débranchez le cordon d'alimentation
avant d'utiliser.

WARNING

AVERTISSEMENT

.

36 . DSC 4000 Installation and Hardware Guide

Install a DSC 4000

The installation pr ocedure for the DSC 4000 consists of the following steps:

• Prepare the Laboratory (refer to page 19)

• Unpack the DSC 4000

• Set Up the DSC 4000 System Components

• Connect the DSC 4000 System Components

• Configure the DSC 4000

• Calibrate the DSC 4000

Install a DSC 4000 . 37

Unpacking the DSC 4000

The DSC 4000 System consists of the following components:

• DSC 4000

• Personal Computer

• Pyris Software

• Printer (optional)

• Intracooler 6P (optional)

• Portable Cooling Device (optional)

• Chiller (optional)

• Autosampler (optional)

The autosampler is an optional accessory that is used to automate the running of multiple
samples. It is factory installed. The sample tray holds up to 45 samples. Runs can be
sequenced and postrun data analyzed by using a play list which is created using the Pyris
Player software.

The DSC 4000 comes wrapped in plastic and is surrounded by foam on all sides of the
analyzer. The DSC 4000 weighs 17 kg (37 lb), or 19 kg (42 lb) with the autosamp ler
installed. To unpack the analyzer, follow the steps below:

1. Remove the foam inserts from the box.

2. Remove the analyzer from the box.

3. Remove the foam from all sides, turning the analyzer on end as necessary.

4. Remove the tape and plastic from around the analyzer.

5. Remove the tape from the outer furnace lid and remove the lid. Place it to the side.

6. Remove the packing material from inside the furnace area.

7. Remove the tape from the connectors on the rear of the instrument.

When unpacking each box of your shipment, check all the parts included against the shipping
list. If any part is damaged or missing, contact the delivery service and PerkinElmer
immediately.

The DSC 4000 is shipped with a Spares Kit. If you have purchased the AS 6000 Autosampler,
this is installed at the factory.

38 . DSC 4000 Installation and Hardware Guide

Also included with the DSC 4000 are :

Description Part Number Quantity
Tygon tubing for coolant 0250-6519 3 m

Teflon tubing for purge gas 0250-6483 6 m

5/16-in. pipe for Swagelok Cooling Liquid In

— 2

and Out connectors
RS-232 cable — 1

Male RJ45 to DB9 modem cable 0941-0042 1

Power cable — 1

Place the analyzer carefully on the prepared bench. Unpack the remaining of the DSC 4000
and place them nearby. You will need these parts for the installation of the analyzer.

Install a DSC 4000 . 39

Ensure that the mains power lead is disconnected from the
instrument before pro ce e d i ng

Assurez-vous que le cordon d'alimentation secte ur es t
débranché de l' instr ument avant de continuer

Set Up the DSC 4000 System Components

Place the DSC 4000 on your labora tory bench. Do not plug in the power cord until instructed.
The computer and printer should already be on the bench and installed according to each
item’s instructions.

Be sure to set up all of the system components listed below before switching on the
DSC 4000:

• Select the correct voltage

• Install the purge gases

• Install the cooling device

Select the Correct Voltage for the DSC 4000

The DSC 4000 accepts the following voltages: 100–120 V and 200–240 V (50/60 Hz).
It is configured and shipped to operate at 200–240 V. Selection of the correct voltage for

your lab can be done at the AC inlet plug at the rear of the DSC 4000.
First check whether the voltage sele ction corresponds to the voltage in your laboratory. This

can be seen easily: the voltage range with the t ext in an upright position and the arrow
pointing at the small line represents the volt age that has been selected.

To select the correct voltage for the DSC 4000 in your laboratory:

.

WARNING

AVERTISSEMENT

.

40 . DSC 4000 Installation and Hardware Guide

1. Remove the fuse holder with a screw driver by gently prying it out of the compartment.

2. Once the holder is out far enough to hold onto, slide the fuse holder out of the slot.

3. Remove the fuse (3.15 A) from the 220 V position. This can be done using the point of
a pencil to gently lift the fuse out of the holde r .

NOTE: It may be necessary to move the fuse slightly towards the back of the fuse pack

before prying it out of the holder.

NOTE: In the figure above, the fuse that is installed is for 220 V.

4. Insert the fuse (6.3 A) for 110 V (it goes into the right side when 110–120 V is in the
upright (legible) position).

NOTE: Ensure that the head of the fuse makes contact at both ends of the fuse holder.

5. Reinsert the fuse holder.

Install a DSC 4000 . 41

Connect the Purge Gas Supply to the DSC 4000

The DSC 4000 has a system purge gas inlet and two sample purge gas inlets at the back of
the analyzer. The system purge gas purges the outer portion of the sample holder/heat
exchanger assembly with dry gas. This facility must ALWAYS be used when working with the
analyzer. The dry gas, preferably dry nitrogen, prevents condensation of water vapor on the
measuring cell. The system purge gas flow rate is controlled by a needle valve inside the
analyzer, and is preset to 40 ml/min.

NOTE: The DSC 4000 analyzer has a mass flow controller built into the analyzer. However, if

you have an autosampler and are using the dry box purge, this does not have a mass
flow controller. Therefore, it is necessary to use either an H restrictor
(P/N 01541498) or a Float Displacement Flow Meter (P/N 02901624) to obtain the
proper flow rates. The gas must be dry. A flow rate of between 20 and 40 ml/min
is recommended.

The sample purge gas inlets (A and B) are used to purge the furnace, and are part of the
internal gas selector (which has two inlets and one outlet). Argon or nitrogen of 99.9%
minimum purity is recommended for purging the sample area. Other gases such as a ir or
oxygen may also be used. The flow rate of the sample purge gas is controlled using the
software.

NOTE: The gas must be dry. A flow rate of between 20 and 40 ml/min is recommended.

The procedure for connecting the purge gas supply includes the following steps:

• Connect the purge gas line to the system gas supply.

• Install a filter dryer (optional).

• Connect the purge gas lines to the DSC 4000.

Connect the Purge Gas and System Purge Gas Lines to
the DSC 4000

Perform the following procedure to connect your sample purge gas and system purge gas
lines to the DSC 4000 analyzer regardless of the other components in the purge gas line.

42 . DSC 4000 Installation and Hardware Guide

Assuming that all the other components of the purge gas line are installed, you will now
connect 1/8-in. Teflon tubing to the DSC 4000 using a female connector.

The DSC 4000 sys tem purge gas (1 pc) and sample purge gas (2 pcs) connectors are
mounted to the back of the analyzer.

1. Place the 1/8-in. Teflon tubing from your dry purge gas line onto the inlet labelled
system purge gas ALWAYS REQUIRED.

2. Place the 1/8-in. Teflon tubing from your system purge gas line onto the inlet sample
purge A.

If a second sample purge line is desired, connect it to sample purge B (1/8-in. Teflon
tubing).

Connecting purge and system gas lines to the DSC 4000:

NOTE: The dry box purge inlet is only used when an autosampler is installed on the

instrument.

Connect the Cooling Device to the DSC 4000

The DSC 4000 has an integrated cooling system tha t accepts various types of cold gases and
liquids. In standard configuration, the cooling system operates from ambient to 445 °C.
Normal tap water can be used for the coolant. The recommended cooling system for the
range of –20 °C to 445 °C is the Polyscience Chiller (N537-0220/N5370221, 120 V and 22 0 V,
respectively).

The Intracooler 2S for DSC 4000 is the cooling device for the r ange of –65 °C to 445 °C.
The Portable Cool ing Device (PCD) can be used to quickly cool the DSC 4000 to ambient

temperature, or to cool below room temperature for occasional subambient measurements.
The PCD (P/N N5202068) can be filled with ice, ice water, liquid nitrogen or any other
cooling mixtures.

NOTE: When operating the analyzer with a cooling device you MUST use a purge gas.

Install a DSC 4000 . 43

for operation at temperatures between 15 °C and 90 °C. For operation at

Un fluide approprié doit être utilisé ave c le refroidi sseu r. Le fluide devrait

20 ° C. Tout inférieur à celui qui affecterait le

pouvoir de transport de la pompe du refroidisseur. L'eau distillée est
recommandée pour un fonctionnement à des températures comprises

0%

.

à l'avant et à

l'arrière du refroidisseur ne sont pas bloqués. Maintenir un espace

.

Connecting to the Chiller

When using the chi ller, connect the c ooling supply to the DSC 4000 as follows:

CAUTION

ATTENTION

CAUTION

ATTENTION

An appropriate fluid must be used with the chiller. The fluid should be
effective down to –20 °C. Any lower than that would impair the
conveyance power of the chiller's pump. Distille d wa ter is recommended

–20 °C to 100 °C, 50% ethylene glycol in water is recommended.

être efficace jusqu'à -

entre 15 ° C et 90 ° C. P our une utilisation de -20 ° C à 100 ° C, 5
d'éthylène glycol dans l'eau sont recommandés

Ensure that the cooling air vents at the front and rear of the cooler are
not blocked. Maintain a minimum space of 15–20 cm.

Assurez-vous que les évents d'air de refroidissement
minimum de 15-20 cm

1. Make sure that the chiller is switched off but that its power cord is plugged into a power
supply.

2. Screw one of the barbed hose couplings shipped with the chiller into the OUTLET
connection on the chiller unit, and t ighten with a suitable wrench.

3. Couplings suitable for several different hose sizes are provided with the chiller.

4. Push a hose (compatible with the desired coolant) onto the OUTLET coupling and
secure with a hose clamp.

5. Slide the other end of the hose over the metal tube labeled COOLING LIQUID IN on the
thermal analyzer. Place a hose clamp around the hose and metal tube to secure the
hose in place.

6. Screw a barbed hose coupling into the INLET connection on the chiller unit, and tighten
with a suitable wrench.

7. Push a hose onto the INLET coupling and secure with a hose clamp.

8. Connect the other end of the hose to the COOLING LIQUID OUT connector on the
analyzer. Place a hose clamp around the hose and the metal tube to secure the hose in
place.

Setting Up The Chiller

1. Fill the reservoir with coolant.
Ensure that the cooling coils are completely covered. The maximum coolant level is

25 mm below the top of the reservoir.

44 . DSC 4000 Installation and Hardware Guide

pression.
Utilisez le débit le plus bas qui procure un refroidissement suf fisant pour
votre expérience afin de minimiser la pression dans le système.

Il est essentiel de maintenir un débit constant de liquide de

bulles d'air. Des
changements dans le débit de liquide ou la présence de bulles d'air
réduiront la qualité du signal de mesure.

2. Switch the chiller on at the mains supply and at the switch on the rear of the control
unit (NOT using the Power switch on t he front of the control unit).

3. When switching on the chiller for the first tim e, select the display language by rotating
the Select/Set control on the front panel, and then pressing to select the desired option.

The chiller controller will continue with its start-up sequence and then display “Standby”
when ready.

4. Set the safety set temperature on the controller using a flat screwdriver to rotate the
control to the maximum temperature to which the bath should be heated.

5. Press the Power switch on the front panel.
The pump will begin operating.

6. Top up the coolant reservoir to compensate for the fluid in the external circuit.

7. Rotate the Select/Set control on the front panel until the Pump/AutoTune menu is
displayed.

8. Press the Select/Set control until the pump speed bar is highlighted.

9. Rotate the Select/Set control to adjust the pump speed, and press the control to accept
the new setting.

CAUTION

ATTENTION

The heat exchanger of the DSC 4000 will NOT accept pressure. Use the
lowest flow rate that provides sufficient cooling for your experiment to
minimize the pressure in the system.

L'échangeur de chaleur du DSC 4000 n'acceptera PAS la

CAUTION

ATTENTION

It is essential to maintain a very constant flow rate of coolant. The liquid
should be free of air bubbles. Changes in the liquid flow rate or the
presence of air bubbles will reduce the quality of the measurement
signal.

refroidissement. Le liquide doit être exempt de

Setting the Coolant Temperature

When using a circulator, the temperature must be controlled to within 0.2 °C (set point
± 0.1 °C).

1. Press and release the Select/Set control on the front panel.
The set point temperature value is highlighted.

2. Turn the control to set the temperature to the nearest whole degree Celsius.

3. Press the control again.

Install a DSC 4000 . 45

L'échangeur de chaleur du DSC 4000 n'acceptera PAS la pression. Par

l'eau

entre dans le DSC 4000.

90

min). Le liquide doit être exempt de bulles d'air. Les changements

bulles d'air influenceront

négativement la qualité du signal de mesure.

The degree fraction figures are highlighted.

4. Turn the control to select the desired fraction of a degree.

5. Press the control to accept the value.

Connecting to Tap Water

When using tap water:

1. Make sure the tap water is conveniently located near the DSC 4000.

2. Connect a hose to the Cooling Liquid In connector. Secure with a clamp.

3. Connect the other end of this hose to the tap.

4. Connect the other hose to the Cooling Li quid Out connector. Secure with a clamp.

5. Connect the other end of the hose to a suitable drain.
The tap water must be continuously circulated through the heat exchanger with a low

flow rate of 5–15 l/h during the operation of the analyzer. The temperature of the
cooling liquid ma y not change more tha n 0.4 °C/hour in the case of tap water.

CAUTION

ATTENTION

CAUTION

ATTENTION

The heat exchanger of the DSC 4000 will NOT accept pressure.
Therefore, flow regulation should be done before the water enters the
DSC 4000.

conséquent, la régulation du débit devrait être effectuée avant que

It is essential to maintain a very constant flow rate of approximately 5
l/h (80–90 ml/min). The liquid should be free of air bubbles. Changes in
the liquid flow rate or the presence of air bubbles w ill negat ively
influence the quality of the measurement signal.

Il est essentiel de maintenir un débit très constant d'environ 5 l/h (80­ml/
dans le débit de liquide ou la présence de

46 . DSC 4000 Installation and Hardware Guide

Frosting is possible on the rear of the D SC 4000. To prevent this problem

Le givrage est possible à l'arrière du DSC 4000. Pour éviter ce problème,
le tube d'échappement doit être correctement installé sur l'analyseur.

Connecting to the Intracooler for the DSC 4000:

CAUTION

ATTENTION

the exhaust tube must be properly installed on the analyzer.

Exhaust tube installation:

• For the KTS Kinetics Cooler use the entire piece as it does fit over the hose.

• For the PolyScience Intracooler use a piece that slips over the two chiller pipes,

approximate ly 3.5 cm long.

Precautions for Intracooler s:

• Do not lift or move the unit by pulling the flexible line.

• Do not make any sharp bends in the flexible line.

• Do not block or restrict air f l ow to the vents on the unit.

• Do not operate the unit in temperatures above 32 °C.

• Do not operate at a line volt age outside of 110 V +/-10% or 220 V +/-10% when

operating at 50/60 Hz.

Install a DSC 4000 . 47

Connect the DSC 4000 System Components

The computer and optional printer should already be connected together and the Pyris
software already installed. To complete the connection of the system components, the
DSC 4000 has to be connected to the computer.

CAUTION

ATTENTION

The image below shows the connections on the DSC 4000:

Make sure that the computer is off before plugging in the DSC 4000.
Assurez-vous que l'ordinateur est éteint avant de brancher le DSC 4000.

Make sure all comp onents are turned off and unplugged before you begin.

1. Connect one end of the RS-232 cable to the back of th e DSC 4000.

2. Connect the other end of the RS-232 cable to COM1 on the back of the computer.

3. Connect the printer and printer cable to the computer.

4. Connect the analyzer, printer and computer power cor ds to AC outlets.

5. Once the system connections are made, switch on the system in the following order:

– Computer
– DSC 4000
– Printer

6. Turn on the purge ga s and dry gas, the w ater for the DSC 4000 cooling system or any
other accessories for the cooling device you are using.

48 . DSC 4000 Installation and Hardware Guide

Configure the DSC 4000

The Pyris software must be configured for the DSC 4000. This must be done before the
DSC 4000 Application can be recognized.

1. Select Pyris Config from the Pyris group under PerkinElmer Applications in the
Programs menu accessed from the Start button or select Configure Analyzer from the
Pyris Manager Start button menu. The Pyris Configuration dialog box appears on the
screen.

2. Click the Add Analyz e r button. The Add Analyzer dialog box appears.

3. From the list of available ports, select the port to which you connected the analyzer.
Remember that COM5 appears when an analyzer is connected to port 1 of an EdgePort
USB. Click the Add button. The DSC 4000's Configurat ion dia log box is displayed.

4. The system detects the type of analyzer that is attached and displays the default name
and other information for a DSC 4000 in this dialog b ox. Select the accessories that are
attached to the analyzer.

5. Click OK to accept the selections.

Install a DSC 4000 . 49

6. Click OK to exit the Configuration dialog box or select Add Ana l y z e r to add another
analyzer to the configuration. Remember that the analyzer must be connected to the
communications po rt and switched on; otherwise, it will not be recognized b y the Pyris
software.

Once the Pyris software has been configured for the DSC 400 0, the DSC 4000 Application can
be started from Pyris Manager.

Starting the Pyris Manager

1. Select Pyris Manager from the Pyris Software group in Programs on the Start menu.
The Pyris Manager is displayed on the screen.

2. Select DSC 4000 from the Pyris Manager . The DSC 4000 control panel is displayed.

3. Now that the system is switched on, the DSC 4000 should be conditioned before using
for the first time (and when it has been switched off for long periods of time).

This is to remove any water vapor that has been adsorbed to the furnace wall during
transport and/or storage. To do this, enter 150 °C in the temperature field beneath the

Go To Temp button
Alternatively, you can set up a method to heat to 150 °C at a heating rate of 5 °C/min.
When the analyzer has cooled to ambient temperature, it is ready for normal use.

The configuration for the DSC 4000 is complete. The analyzer is ready to be calibrated.

on the control panel and click on the button.

50 . DSC 4000 Installation and Hardware Guide

Calibrate the DSC 4000

Upon installation, the DSC 4000 must be calibrated for temperature and heat flow before
routine operation. Calibration is accomplished by running high-purity standards or reference
materials with known temperature and energy transitions . The data obtained after running
these materials (that is, temperature transitions and
calibration routine to automatically calibrate the analyzer. Once the analyzer is calibrated, it
will remain calibrated, even when the system is switched off, unless there are major changes
to the analyzer’s operating conditions.

The DSC 4000 is shippe d with a Spares Kit that contains reference materials. Additional
reference materials can be ordered through www.perkinelmer.com/supplies. Indium and zinc
are generally used for routine calibration.

1. Cut and weigh a small piece of each reference material (indium and zinc), each between
5 and 10 mg. Record the weights.

The DSC 4000 Spares Kit includes precrimp ed, preweighed samples of indium and zinc
(P/N N5190762). If you use these samples, be sure to use the small sample.

2. Encapsulate the reference material in a standard sample pan.
To achieve the best temperature repeatability, samples should be flattened and placed

in the center of t he sample pan, then encapsulated.

H values) are used in the Pyris

3. Using tweezers, place the encapsulated sample into the sample area of the sample
holder (left side); place an empty sample pan and lid into the reference side of the
sample holder (right side).

4. Using tweezers, cover the furnace with the inner and the outer furnace covers.

5. To open the IndCal method from the Method Editor, select File, Open Method, and
then choose Indcal.d6m from the Program Files\PerkinElmer\Pyris\Methods directory.

You can also use the calibration method file for zinc called Zinccal.d6m.

6. In the Sample Info page, fill in the sample information. Enter the weight of the indium
sample and the file name under which the data will be saved.

7. Click the Start Method button on the DSC 4000 control panel.
The run starts; when completed, the file will be saved with the file name entered in the

method.

8. After the run is complete, perform a Peak Area calculation, include the Onset
temperature and note the Onset result.

9. Repeat steps 1–8 for each reference material you are using to calibrate the DSC 4000.
Up to ten reference materials can be used to calibrate the temperature program of the

analyzer.

10. From the Method Editor, select Calibrate from the View menu.

11. Select the Temperature tab.

Install a DSC 4000 . 51

12. Enter the name of the reference material used, the Expected Onset value, the
Measured Onset value just measured for each reference material, and click the check
box in the Use column.

13. Select the Heat Flow tab.

14. Enter the name of the reference material used (we recommend indium for this
calibration), the Expected

H value, the Measured H result just measured, and the

Weight of the reference material used.

15. Click the Save and Apply button. In the Save As dialog box, select the default.d6c
calibration file and click OK. Answer Yes to overwrite the existing file to save the new
calibration values.

16. Click Close to exit Calibration and send the new calibrati on values to the DSC 4000.

The DSC 4000 calibration is complete.
This completes the installation of the DSC 4000.

DSC 4000 Hardwar e

54 . DSC 4000 Installation and Hardware Guide

DSC 4000

The DSC 4000 Differential Scanning Calorimeter is a single-furnace, heat-flux DSC. Heat flow
is determined by measuring a temperature difference over a very accurately known thermal
resistance. This analyzer is used to character ize materials, design products, predict product
performance, optimize processing conditions, and improve quality. The DSC 4000 system
permits the direct calorimetric measurement, characterization, and analysis of thermal
properties of materials. Under the control of the Pyris software on your PC, the DSC 4000 is
programmed from an initial to a final temperature through transitions in the sample material
such as melting, glass transitions, solid-state transitions, or crystallization. Usually the
DSC 4000 is programmed to scan a temperature range at a linear rate for the study of these
endothermic and exothermic reactions. Endotherms and exotherms can be shown as an
upward or downward deviation from the baseline.

The DSC 4000 ha s an integrated cooling system which accepts vario us types of cold liquids.
This allows operation from –100 °C to 445 °C. The DSC 4000 can b e used with a ra nge of
commercial circulating coolers, and for occasional subambient operation can be used w ith the
Portable Cooling Device.

The DSC 4000 is also upgradeable to the DSC 6000.

Furnace and Sensor Design

A low-mass, alumina-coated aluminum furnace forms the heart of the DSC 4000. The furnace
is designed for ruggedness and resistance to chemical corrosion. Because of its low mass,
the furnace can heat and cool rapidly. A pl atinum resistance sensing device measures and
controls the furnace temperature.

The atmosphere surrounding the sample is controlled very efficiently since the gas enters
above the sample crucible. This is extremely important when performing oxidative stability
experiments. The purge gas is also preheated resulting in minimal disturbance of the signal.

The sample is placed on a precisely machined sensor disk constructed of 90% nickel/10%
chromium. This rugged and durable disk provides high thermal conductivity and a very low
time constant for superior instrument response. Highly sensitive thermocouples measure the
temperature at both the sample and reference positions. The DSC 4000 accommodates a
wide range of PerkinElmer sample pans. Over two dozen different pan types are available.

DSC 4000 Hardware . 55

Do not attempt to service the DSC 4000. Servi ce must be
performed by a PerkinElmer Instruments Service
Representative

N'essayez pas de réparer le DSC 4000. Le service doit être
effectué par un représentant du service PerkinElmer
Instruments

Cooling

The DSC 4000 incorporates a built-in cooling chamber that lies below and is attached to the
furnace assembly. The chamber uses a simple in/out design which allows for the use of any
noncorrosive circulating liquid or cooling gas. Cooling liquids include water and ethylene
glycol.

For cooling with liquids, many commercial circulating coolers are available that can be
interfaced to the DSC 4000. The Polyscience Chiller (P/N N5370220/N5370221, 120 V and
220 V, respectively) is the recommended cooling device for the range –20 °C to 445 °C. The
Intracooler (P/N N5374098/N5374099) is recommended for the range –65 °C to 445 °C. The
Intracooler accessory allows rapid cooling between sample runs, allowing fast sample
turnaround. The Portable Cooling Device (P CD) can also be used to quickly cool the
DSC 4000 to ambient temperature, or to cool below room temperature for occasional
subambient measurements. The PCD (P/N N5202068) can be filled with ice, ice water, liquid
nitrogen or any other cooling mixtures.

WARNING

AVERTISSEMENT

Other topics related to the DSC 4000 are:

• Safety Precautions

• Calibration

• Operating Variables and Sample Handling

• Subambient Operation

• Maintenance

• Part Numbers

.

.

• Autosampler

56 . DSC 4000 Installation and Hardware Guide

Calibration of the DSC 4000

The DSC 4000 has been calibrated at the factory for both temperature and heat flow. Under
normal conditions, the analyzer does not need temperature recalibration. As a result of the
use of high-precision Pt100 sensors, the tempe rature accuracy does not vary over the
temperature range and remains constant for long periods of time.

We recommend that the temperature calibration and heat flow calibration be checked using
the precrimped samples of indium and zinc before obtaining data. We also recommend that
you perform calibrations in the following order:

• Temperature Calibration

• Heat Flow Calibration

Temperature Calibration

The DSC 4000 has been calibrated at the factory for temperature. Under normal conditions
the DSC 4000 does not need temperature calibration. As a result of the use of high-precision
sensors, the temperature accuracy does not vary over the temperature range and remains
constant for long periods of time.

NOTE: It is recommended that a baseline correction be performed before temperature

calibration.

At least two measured onset temperatures are necessary to calibrate the DSC 4000. The
calibration materials selected must have at least a 50 °C temperature difference in their
theoretical Onset temperatures. Indium and zinc are the recommended calibration materials.
However, other reference materials can be used to calibrate the analyzer but they must be
pure, for example, distilled water.

To calibrate the temperature of the DSC 4000:

1. While using the Instrument Viewer or the Method Editor in the Pyris software, select
Calibrate from the View menu.

The Calibration window is displayed.

2. Restore the default temperature calibration by selecting Temperature from the Restore
menu. If you are going to perform a heat flow calibration, restore all default calibration
values by selecting the All command.

3. Click the Save and Apply button in the Calibrat ion window to send the default values
to the analyzer and save the current calibra tion file. The Save As dialog box appears.
Click OK to save the default file.

4. Select Close to close the Calibration window and begin using the new calibration
values.

After you have performed these steps, go on to the following topics to complete the
temperature calibration of the DSC 4000:

• Perform Indium and Zinc Runs

• Perform a Peak Area with Onset Calculation

• Perform a Temperature Calibration

DSC 4000 Hardware . 57

Perform Indium and Zinc Runs

In performing an indium and zinc run, you can use the precrimped, preweighed samples of
indium and zinc or you can prepare your own samples for calibration. To perform the run,
follow the steps below:

1. Place the sample pan containing indium or zinc in the sample area of the sample holder
and place the reference sample pan in the reference area of the sample holder.

2. Using tweezers, cover the furnace with the inner and the outer furnace covers.

3. If not already displayed, select the Method Editor icon

4. From the File menu, select Open Method.
The Open Method dialog box displays the methods available in the default methods

directory.

5. Select the IndCal.d6m method if using indium or ZincCal.d6m if using zinc.

6. In the Sample Info page, fill in the samp le information. Enter the weight of the indium
or zinc sample and the file name under which the data file is to be saved.

7. Click the Start button
The run starts. When finished, the data file will be saved with the file name that you

entered in the method.

After performing the indium and zinc runs, you must pe rform a peak area with onset
calculation.

in the control panel to start the run.

from the toolbar.

Perform a Peak Area with Onset Calculation

For the indium and zinc runs that you performed, a Pea k Area with Onset calculation is
performed. The data file you just collected should be displayed in the Data Analysis window.
Perform an onset calculation on the data as follows:

1. Select Onset from the Calc menu.
The Onset Calculation dialog box appears.

2. Enter the Left Lim it and the Right Limit. You can also click on the two red X’s that
appear on the curve and drag them to the desired left and right limits. The Left Limit
and the Right Limit fields will be filled in on the dialog box.

3. Click the Calculate button.

4. Record the Onset value for temperature calibration and
If you performing a heat flow calibration, you will need the

5. Repeat steps 1–4 for the zinc calibration run.

Once you obtain the Onset values, you can perform a temperature calibration.

H for heat flow calibration.

H values.

58 . DSC 4000 Installation and Hardware Guide

Performing a Temperature Calibration

The measured Onset values for indium and zinc are used to calibrate the temperature of the
DSC 4000, DSC 6000, Pyris 6 DSC and the Jade DSC. To perfor m the temperature calibration,
perform the following steps:

1. With either the Instrument Viewer or the Method Editor as the active window, select
Calibrate from the View menu.

The Calibrate dialog box is displayed.

2. Select the Temperature tab.

3. Enter the name of the reference material that you used.

4. Enter the expected onset temperature for the reference material in the Exp. Onset field
(for example, 156.60 for indi um).

5. In the Meas. Onset field, enter the onset temperature that you obtained when you
performed the peak area with onset calculation.

6. Enter the Method used for the calibration.

7. Select the check b ox in the Use column for each reference material used in the
calibration.

8. Click the Save and Apply button in the Calibration window to send the new calibration
values to the analyzer and save the current calibration file.

9. Go to the Heat Flow calibration procedure or click Close to cl ose the Calibration window
and begin using the new calibration values.

Heat Flow Calibration

It is recommended that indium be used when performing a heat flow calibration. However,
the heat flow calibration can be performed using any one of the following materials:

Calibration Substance Heat of Fusion (J/g)

Cyclopentane 8.60

Gallium 79.87

Indium 28.45

Lead 23.01

Tin 60.46

Zinc 108.37

DSC 4000 Hardware . 59

1. While using the Instrument Viewer or the Method Editor, select Calibrate from the View
menu.

2. Restore the default Heat Flow calibration by selecting Heat Flow from the Restore
menu.

If you performed a Temperature calibrat ion just prior to starting a Heat Flow calibration
and selected All from the Restore menu, then you do not need to restore the default
Heat Flow calibration here.

3. Click Save and Apply.

4. Click Close in the Calibration window.

5. In Data Analysis, use the same data file obtained when you performed the indium run,
or perform a run using another reference material.

6. Perform a Peak Area with Onset calculation and note the

H result, or use the H
result recorded for the reference material when you performed this step for
temperature calibration.

The measured

H value for indium is used to calibrate the heat flow of the DSC 4000. If you
just performed the temperature calibration on a data file, the data file should still be
displayed.

To perform the heat flow ca l i bration, perform the following steps:

1. With either the Instrument Viewer or the Method Editor as the active window, select
Calibrate from the View menu.

The Calibrate dialog box is displayed.

2. Select the Heat Flow tab.

3. Enter the name of the reference material you used.

4. Enter the expected

5. Enter the measured

H for the reference material used (for example, 28.45 for indium).

H result.

6. Enter the Weight of the reference material used.

7. Enter the calibration method used.

8. Click the Save and Apply button in the Calibrat ion window to send the new calibration
value to the analyzer and save the current calibration file.

9. Click Close to close the Calibration window and begin using the new calibration values.

60 . DSC 4000 Installation and Hardware Guide

Operating Variables and Sample Handling

The DSC 4000, DSC 6000, Pyris 6 DSC and the Jade DSC measure differential temperature
and report the heat flow to the sample as it is heated, cooled, or held isothermally. The
following topics discuss the materials and techniques used to obtain data with a DSC 4000,
DSC 6000, Pyris 6 DSC or a Jade DSC.

Temperature Range

The temperature range for your analysis depends on the sample and the type of experiment
you are performing. The Pyris 6 DSC can be used to analyze samples from a temperature of
–120 °C to 200 °C when used with cold nitrogen gas or from ambient to 445 °C. The
DSC 4000 can be used to analyze samples from –65 °C to 445 °C with the Intracooler with
the PCD. The DSC 6000 and Jade DSC can be used to analyze samples from a temperature
of –170 °C to 300 °C when used with liquid nitrogen or from –65 °C to 445 °C with the
Intracooler (P/N N5374098/N5374099).

Scanning Rate

The DSC 4000, DSC 6000, Pyris 6 DSC and the Jade DSC allow heating rates of 0.1 to
100 °C/min in steps of 0.1 °C/min. Proper selection of heating rate will increase efficiency of
your analysis at the desired sensitivity. Genera lly, slower heating rates improve the peak
resolution while faster heating rates improve the a p parent sensitivity. Heating rates greater
than 40 °C/min are generally used for rapidly heating or cooling the analyzer to the
beginning temperature of the next segment or to selected isothermal temperatures in the
temperature program. Typical experimental heating rates range from 5 to 20 °C/min. Slower
rates can be used for liquid crystals and purity analyses. Refer to the Help for other topics on
operating variables and sample handling:

• Sample Preparation

• Sample Pans

• Sample Encapsulat ion

• Sample Atmosphere

• Loading the Sample into the DSC

DSC 4000 Hardware . 61

Subambient Operation of the DSC 4000

The DSC 4000 can be operated in the subambient mode. The Intracooler (N537-4098 /
N5374099) is recommended for the range –65 °C to 445 °C. The Portable Cooling Device
(PCD) can be used to quickly cool the DSC 4000 to ambient temperature, or to cool below
room temperature for occasional subambient measurements. The PCD (P/N N5202068) can
be filled with ice, ice water, liquid nitrogen or any other cooling mixtures.

Subambient operation of the DSC 4000 is covered in the following topics in the Help:

• Precautions for Subambi ent Ope ra tio n

• Operating the DSC 4000 in the Subambient Temperature Range

• Portable Cooling Device (PCD)

62 . DSC 4000 Installation and Hardware Guide

DSC 4000 Maintenance

The DSC 4000 needs little routine maintenance other than proper treatment as a sensitive
electromechanical device.

Since the sensor dis k is the hottest component in the furnace area, it will usually remain
clean and free of condensates. However, samples may ooze out of sample pans or be
accidentally spilled onto the sensor disk. Such materials should be removed at low
temperatures whenever possible by using tweezers or moistened cotton swabs.

Solvents should not be placed directly on the sensor. Moisten a cotton swab or a tissue with
solvent; then clean the sensor or upper portion of the furnace wall with the swab.

Any residual sample that has carbonized may remain on the sensor disk after it has been
cleaned with a solvent. To remove the residue, gently scrub the sensor with a fiberglass or
nylon brush. Be careful not to exert excessive force when scrubbing the sensor since it can
be damaged. The sensor must be as clean and flat as possible for proper operation.

To avoid contaminating the furnace, use a purge gas at proper flow rates. If the furnace
becomes contaminated, clean it as soon as possible.

Cleaning and Decontamination

Before using any cleaning or decontamination methods except those specified by
PerkinElmer, you should check with PerkinElmer that the proposed method will not damage
the equipment.

DSC 4000 Hardware . 63

DSC 4000 Part Numbers

Supplies, accessories, and replacement parts can be ordered directly from PerkinElmer.

www.perkinelmer.com/supplies

selection of high-quality thermal a nalysis supplies.
To place an order, request a free catalog, or ask for information:

• If you are located within the U.S., call toll free at 1-800-762-4000, 8 :30 a.m. – 7 p.m.
EST. Your order will be shipped promp tly, usually within 24 hours.

• If you are located outside the U.S., call your local PerkinElmer sales office.

, PerkinElmer's web-based catalog service, offers a full

or go on-line to
Below is a list of the part numbers that are in the Spares kit (P/N N5200031).

Part No. Description Quantity

03190033 Indium calibrating reference material 1

03190036 Zinc calibrating reference material 1

09908400 Tweezers 1

01541498 H restrictor 1

N5190762 Kit – crimped indium/zinc calibrating reference

N5390123 Aluminum pans and covers (100) 1

Also included with the DSC 4000 are

• Tygon tubing (P/N 02506519) for connection of liquid coolant

www.perkinelmer.com

materials

.

1

• Hose clamps (P/N 09920044)

• Teflon tubing (P/N 02508059) for purge gas connection

• RS-232 cable for communicating to the computer

• Power cable

64 . DSC 4000 Installation and Hardware Guide

Miscellaneous Part Numbers

Part Number Description

N5370212 DSC 4000

N5370213 DSC 4000 with Autosampler

N5202068 Portable Cooling Device

N5202070 Mini drybox

09991662 Fuse for 100–120 VAC, 6.3 AT, 250 VAC, 5 x 20 mm

09991629 Fuse for 220–240 VAC, 3.15 AT, 250 VAC, 5 x 20 mm

AS 6000 Autosampler

66 . DSC 4000 Installation and Hardware Guide

AS 6000 Autosampler

The AS 6000 auto sampler accessory brings automation capability to the DSC 4000,
DSC 6000, STA 6000 and TGA 4000 when used in conjunction with the Pyris software Player
feature. It offers faster sampling rates than the AS 6 Autosampler.

NOTE: If you have an STA 6000, then you will need firmware for Pyris version 9.1 o r later to

operate the AS 6000 autosampler. Select Programs > Pyris Software > Pyris User

manuals > Pyris Installation manuals > Upgrading Pyris Software
Installation.pdf for more information.

• The autosampler is powered by the power supply of the parent instrument.

• The part of the autosampler that manipulates t he sample pan is called the gripper. It

comprises three fingers, 120° apart from each other. They extend out of the end of the
gripper housing.

• There are only two ranges of motion for the gripper: the gripper arm moves up and
down and rotates. This allows the gripper to access each sample pan in the trays,
transfer a pan from the tray, through the furnace access hole in the base plate, to the
furnace, and then r eturn it to its posi tion on the tray. Movement in these two directions
also allows the gripper a sufficient range of motions to access the furnace lid(s) and
move it onto and off of the furnace access hole.

• For the DSC 4000 and DSC 6000, you can use the existing robotic sample pans sealed
with the Universal crimper press. All other standard sample pans (sealed and vented)
can also be used. For the TGA 4000 and the STA 6000 the standard crucible (ceramic
pan) is used.

• The AS 6000 communicates with the computer via the parent instrument's connection
to the computer via the RS-232 port.

• The parent instrument communicates with the AS 6000 via an I2C bus.

• The autosampler operates over the full temperature ranges of the TGA 4000, STA 6000,

DSC 4000 and DSC 6000.

• When power is supplied the three-finger gripper mechanism, the metal shrinks and the
fingers open; when power is not supplied, the metal expands and the fingers close.

• The autosampler operates with a feedback system from the instrument. When a sample
pan is located properly on the sensor the a utosampler senses this and rises up out of
the furnace.

• The light switch sensors by the furnace hole detect the presence of a sample pan or
furnace lid being placed in the furnace hole. If the autosampler is supposed to be
removing a lid, for example, and the gripper fails t o pick up the lid, it is detected by the
sensors and error message is displayed.

• The autosampler is fully automated and controlled by the software. The two-piece
sample tray holds up to 45 samples for efficient unattended operation.

• One tray holds 22 samples and the other 23 samples. This difference means that you
cannot mistakenly place one tray in the wrong position. The trays have recesses on the
bottom which catch positioning pins in the base plate. The positioning pins for one tray
are located in different places than those for the other tray, which also prevents one
tray from being inserted into the wrong location.

AS 6000 Autosampler . 67

The trays can be removed independently so that you can load one with fresh samples
while the autosampler runs samples in the other. You could also add samples to the
tray “in use” to replace samples that are completed by pausing the play list.

The Pyris Player feature allows for creation of sequences or play lists to operate the
autosampler and instrument. During an autosampler sequence, you can perform multiple
experiments, curve optimization, calculations, a nd printing. With Pyris Player, you can create
Sample Groups that group similar analyses together to be run in any order. See the software
Help for details.

The following topics discuss the AS 6000 autosampler in more detail:

• Safety Precautions

• How the Autosampler Works

• Autosampler Gripper Alignment

• Sample Handling

• Running a Play List

• Troubleshooting

• Maintenance

• Install a Reference Pan into a DSC

68 . DSC 4000 Installation and Hardware Guide

To remove the furnace lid(s) of the parent instrument,
always use tweezers. T he furnace lid(s) might be hot

Pour retirer le (s) couvercle (s) du four de l'instrument
parent, utilisez toujours une pince à épiler. Le (s) couvercle
(s) du four pourrait être ch aud

vous que l'AS 600 0 est bien

attaché à la plaque de base de l'instrument parent.

Safety Precautions for the AS 6000

The safety precautions to be followed when using the AS 6000 autosampler are the same as
those for the parent instrument: STA 6000, DSC 4000, DSC 6000, or the TGA 4000. In
addition, the following two precaut ions should be kept in mind:

.

WARNING

AVERTISSEMENT

CAUTION

ATTENTION

.

Before switching on the parent instrument, make sure that the AS 6000
is properly attached to the base plate on the parent instrument.

Avant d'allumer l'instrument parent, assurez-

AS 6000 Autosampler . 69

How the AS 6000 Autosampler Works

The autosampler has to be configured into the DSC 4000, the DSC 6000, the STA 6000 or
the TGA 4000 via the Pyris Configurat ion dialog box in or der for the software t o recognize it.
See the software Help for details.

The AS 6000 autosampler is computer controlled and fully automated. Information between
the host computer with Pyris software and the AS 6000 is sent via the pare nt instrument's
connection to the computer via the RS-232 port. Light switch sensors by the furnace access
hole detect the presence or absence of a furnace lid or sample pan. An error message is
generated and displayed in the software and on the LCD of the parent instrument if the
sensors detect the presence of an object when there should not be one and vice versa.

NOTE: The instrument cannot detect if a sample pan is present in the furnace from a

previous power on period. If you turn off the instrument with a sample pan in the
furnace, you must remove the pan before loading another sample during the
following power on session.

In general, you place samples in sample pans and load the pans in the sample trays. The
sample trays are then placed on the base plate on the parent instrument. At the beginning of
a run, the gripper arm is up all the way and is over the home position. The fingers are
closed. The furnace lid (for the TGA 4000) or lids (for the DSC 4000 or DSC 6000) are on the
lid holders in the furnace access hole. The gripper device is instructed via a command in the
Pyris software to begin a session.

Autosampler Work Cycle

When you begin a sample run by starting a play list, the autosampler performs a typical work
cycle. If you use the Sample Group instead of a regular play list, many steps are
automatically added to the play list by the software. These additional steps are seen when
you select View History. For example, if you wish to run two or more samples, you have to
include a Return Sample line after the Start Method line for each sample before a Load
Sample. When usi ng Sample Group, the s oftware adds that Return Sample line automatically
when the play list is played back.

NOTE: Play lists created in previous versions of software are compatible with new versions

of Pyris software. However, new play lists may not be compatible with older versions
of Pyris, or with older instruments.

A typical work cycle for the autosampler on a DSC 4000 or a DSC 6000 and used with a play
list is as follows:

NOTE: Before the start of a play list, the gripper should be over the home position and there

should be no sample pan in the furnace. The lower furnace lid and the upper lid
should be in place.

1. Start the play list. Your play list may have an explicit Load Sample command, or, if
using a Sample Group, the entry Sample List implie s Load Sample. Upon reaching this
line in the list, the gripper swings around to remove the upper lid and place it on the
ring.

2. The gripper then removes the lower lid and places it on the ring.

3. The gripper retrieves the sample pan and places it in the furnace.

4. The lower lid is placed within the furnace.

70 . DSC 4000 Installation and Hardware Guide

5. The upper lid is placed on the furnace.

6. The gripper retur ns to the home position.

7. The method runs.

8. At the end of the run, the system removes the upper lid and places it on the ring.

9. The system removes the lower lid and places it on the ring.

10. The sample pan is removed from the furnace and returned to its place in the tray.

11. The system places the lower lid back into the furnace.

12. The upper lid is placed back on the lid holder.

13. The gripper goes to the home position.

14. The data analysis list for the sample is performed.

15. If there is another sample in the list, the work cycle, starting with step 1, begins again.
To remove the last sample from the furnace do a “Prepare Sample -Return Sample # #”
as the last Play list step, where # # is the last sample loaded.

A typical work cycle for the autosampler on a TGA 400 0 or an STA 6000 and used with a play
list is as follows:

NOTE: Before the start of a play list, the gripper should be over the home position and there

should be no sample pan in the furnace. The furnace lid should be in place on the lid
holder over the furnace.

1. Start the play list. Your play list may have an explicit Load Sample command, or, if
using a Sample Group, the entry Sample List implie s Load Sample. Upon reaching this
line in the list, the gripper swings around to remove the furnace lid and place it on the
ring.

2. The gripper retrieves the specified sample pan and places it in the furnace.

3. The furnace lid is placed on the lid holder.

4. The gripper retur ns to the home position.

5. The method runs.

6. At the end of the run, and after the end condition temperature is achieved, the system
removes the furnace lid and places it on the ring.

7. The sample pan is removed from the furnace and returned to its place in the tray.

8. The furnace lid is placed back on the lid holder.

9. The gripper goes to the ho me position.

10. The data analysis list for the sample is performed.

11. If there is another sample in the list, the work cycle, starting with step 1, begins again.

AS 6000 Autosampler . 71

Reduced Time Cycle

A reduced time cycle is available for the STA 6000, DSC 4000 and DSC 6000.
This feature is accomplished by using either a Sample Group or by doing successive Load

Sample commands wi thout an explicit R eturn Sample.
If you do this, the step(s) where the furnace lid(s) is (are) replaced is eliminated and the

next sample is immediately loaded.
Below the procedure for the work cycle for DSC 4000/DSC 6000 for multiple samples using

the reduced cycle time.

1. Start the play list. Your play list may have an explicit Load Sample command, or, if
using a Sample Group, the entry Sample List implie s Load Sample. Upon reaching this
line in the list, the gripper swings around to remove the upper lid and place it on the
ring.

2. The gripper then removes the lower lid and places it on the ring.

3. The gripper retrieves the sample pan and places it in the furnace.

4. The lower lid is placed within the furnace.

5. The upper lid is placed on the furnace.

6. The gripper retur ns to the home position.

7. The method runs.

8. The data analysis list for the sample is performed.

9. The system removes the upper lid and places it on the ring.

10. The system removes the lower lid and places it on the ring.

11. The sample pan is removed from the furnace and returned to its place in the tray.

12. The gripper retrieves the next sample pan and places it in the furnace.

13. The system places the lower lid back into the furnace.

14. The upper lid is placed back on the lid holder.

15. The gripper goes to the home position.

The procedure for the STA 6000/TGA 4000 is similar to the pr ocedure above.

72 . DSC 4000 Installation and Hardware Guide

AS 6000 Autosampler Gripper Alignment

The autosampler is aligned at the factory. However, if you install a reference pan into your
DSC instrument or change the sample thermocouple of your TGA instrument, change the
sensor, or if the gripper does not grasp the sample pans correctly, you should perform a
gripper alignment procedure.

1. Access the procedure from the Autosampler Control dialog box which is displayed by

clicking on the Autosampler Control button
instrument. Click Align to open the Autosampler Alignment Wizard.

NOTE: When running an autosampler alignment, make sure that the temperature is 22 °C

(ambient temperature). If the temperature is too high the grippers will not align.

2. The first wizard informs you that the upper furnace lid should be in place on top of the
furnace access hole for either parent instrument. The lower furnace lid for the DSC
4000 or 6000 should be in its place on the ring. It is no t necessary to have sample pans
in positions 12 and 33. If you wish to use the previous calibration's values as a start for
this calibration, click on the radio button. (The calibration val ues are stored in the
firmware on the AS 6000 controller board.) Otherwise, the default values will be used to
start. Click Next to continue.

3. The gripper moves from the home position to location 12. The buttons in the next
wizard are used to move the gripper with respect to the dimple of location 12 so that
the fingers are even around the dimple. You also have to adjust the height of the
fingers above the tray surface. There should be only 0.1 mm between the tray and the
finger. Use the buttons on the wizard to move the gripper up and down and left and
right. When satisfied with the positioning, click Next. The gripper swings around to
position 33.

4. Do the same thing for position 33 as you did for 12. Click Next.

on the control panel of your

5. The last wizard screen is displayed. Click Finish to exit from the Autosampler Alignment
Wizard and return to the Autosampler Control dialog box.

NOTE: After you complete the alignment procedure check your purge gas. If the purge gas

was turned off during the alignment procedure turn the purge gas back on.

AS 6000 Autosampler . 73

AS 6000 Sample Handling

Sample Preparation

See the sample preparation instructions for the parent instrument.

Sample Pans

The types of samp le pans that you can use for the DSC 4000 and DSC 6000 with
autosampler are all sizes of the standard robotics sample pans that are available. The sample
pans must be sealed using the Universal Crimper press which comes with the system. The
capacities for the sample pans are 10, 25, 30, and 50 µL.

Sample Loading

Before loading the sam ple into the cruci bles for the TGA 4000 or STA 4000, you will have to
tare the crucibles, that is, have the system weigh them so the weight of the crucible is not
included in the data. Load the empty crucibles into the sample trays. You can do this with
the trays off of the autosampler or while they are still in place. After filling the locations with
crucibles, carefully place th e trays back onto t he autosampl er, making sure that the two
“buttons” on the bottom side of each tray engage the holes in the autosampler. If you keep
the trays on the autosampler, load the sample into the crucible while it is off the tray and
then use tweezers to place the crucible onto the tray.

You can tare all of the crucibles in the tray using the Pyris Player Tare All feature. To do this
your play list must contain a Sample Group. If you are creating a new play list, select Sample
Group as the first entry. If you are using an existing play list, it should have a Sample Group
in it in order to use t he tare feature.

In a new play list, with Sample Group highlighted, click the Tare All button to display the
Advanced Tare Options dialog box. If you choose This Group Only; Populate from Tray,
the Sample List is filled with a line for each posit ion in the trays that contains a crucible and
the tare weight of the crucible is included. You can also add sample lines yourself and then
select This Group Only; Sample List Items Only from the dialog box. Only the crucibles in
the positions that you selected for your Sample List will be tared.

74 . DSC 4000 Installation and Hardware Guide

When you click the OK button in the Advanced Tare Options dialog box, the Tare/Weigh
System screen appears:

The Sample List will now display the tare weights of the crucibles:

AS 6000 Autosampler . 75

Once the empty crucibles are tared, remove each crucible and load the prepared sample into
each one. Return the crucible to the correct position in the tray. Now the system can weigh
all the samples before running the play list, or you can have each sample weighed at the
beginning of its run. With Sample List highlighted, click the Weigh List button. The
Tare/Weigh System dialog box appears. The system automatically starts the program to
weigh each sample in the list. After the last sample, if there was a missing sample
encountered, a message is displayed:

The following samples could not be weighed. It i s possible that the crucibles are
empty.

A list of samples follows. Click the dialog box's Close button to clear the box.
Click the Done button in the Tare /Weigh System window. The Sample List will now display

the weights of each sample.
For efficient use of the autosampler and to increase sample throughput, you can use remove

one tray after the samples have been run and replace the crucibles with empty ones while
the samples in the other tray are being run.

76 . DSC 4000 Installation and Hardware Guide

Running a Pl ay Lis t wi th the AS 60 00

Pyris Player is the backbone of Pyris Software for Windows automation. It was created with
autosamplers in mind. In addition to the standard p lay list items — Load Sample, Run
Method, Return Sa mple — there is also a Sample Group. The Sam p le Group simplifies
grouping like samples together (as you would ha ve in a sample tray of the autosampler).
These like samples use the same test method and data analysis as part of the Sample Group.
A Sample Group consists of a Sample List and a Data Analysis List. A specific method is
selected for the samples in the Sample List. The Data Analysis List allows you to access all
necessary functions for data recall, curve manipulation, optimization, and calculations for
automatic data analysis.

Before starting a run, perform the steps below:

NOTE: Pyris play lists created using previo us version of Pyris software are usually compatible

in later versions of Pyris. And play lists crea ted for one instrument may be compatible
with other instruments of the same type. However, play lists created in later versions
of software may not be compatible with earlier versions of software.

1. Review the safety and warning notes for the analyzer.

2. Verify that the p urge gas (if you are using it) and cooling device tubes are properly
connected at the rear of the instrument.

3. Turn on the gas and adjust the pressure.

4. Turn on the chiller and adjust according to its instructions.

5. Verify that the electrical and cable connections between the computer and the
instrument and other components of the system are properly connected.

6. Turn on the power t o the system components.

7. Prepare your samples.

8. Start Pyris software and click the parent instrument's button in the Pyris Manager. Click
the Pyris Player button on the toolbar:

new one.
There are many ways to use the play list with the autosampler. A quick way to create a

play list for an STA 6000 or a TGA 4000 using the Sample Group feature is given below:

– Load empty sample pans into the locations y ou want to use in the sample tray.

Create a new play list that contains only a Sample Group. Click the Tare All
button. In the Advanced Tare Options dialog box, select This Group Only;
Populate from Tray.

. Either open an existing play list or create a

AS 6000 Autosampler . 77

– Click OK and the Tare/Weigh System dialog box appears. The AS 6000 begins

the procedure of taring the sample pans present on the sample trays. As it finds
and tares each pan, it populates the Sample List and includes the tare weight for
the sample pan in the Sample line. When taring is complete, click the Done
button. The Sample List will be filled in.

78 . DSC 4000 Installation and Hardware Guide

– Remove the sample trays from the autosampler, or leave them in place, to load

the crucibles. If you removed the trays, carefully return them to the autosampler
and make sure that the two knobs on the bottom of each tray engage the holes
in the autosampler plate.

– Now you can have the system weigh each sample in the list. You can also choose

to have each sample weighed right before the run starts. To weigh all the
samples before starting the play list, highlight the Sample List line. A message
informing you that a method has not been selected is displayed. You can select
the method after the samples have been weighed. Click Weigh List. The
Tare/Weigh System screen appears and the system begins to weigh the samples
listed in the Sample List. When finished, the weights are displayed, along with
the tare weights, in each Sample line.

– Next you need to add some items to the Dat a Analysis List. If you have not

entered a method for the Sample List , ho wever, you cannot fill in the Data
Analysis List. To enter a method, highlight the Sample List line. Type in the name
of the method in the Method Name field or click the Browse button and find and
select the method you want to use. Edit the method's program and initial state
parameters by clicking the Edit Method button. When finished editing, close the
Method Editor by clickin g the window's Close button in the upper-right-hand
corner.

– Click the Data Analysis List line and then Add a step. Select Display Curve. The

default selection in the Edit Step area is Use Current Run. After adding the
display of a curve, addition items are listed in the Player Step Options box when
you add another step.

AS 6000 Autosampler . 79

9. Save the play list by selecting Save Player from the File menu.

10. Start playback of the play list by clicking the Start at Top button or the Start at Current
Item button on the Player toolbar. These are the first two b uttons on the toolbar:

NOTE: If you select the Start at Current Item button, the focused item must be a main-level

item, that is, Prepare Sample, Data Analysis, or Sample Group. However, if you are in
a Sample Group, you can start a play list from a Sample line in the Sample List.

NOTE: If you select Go To Load, Go To Temp, or Hold at Temp from the control panel while

a play list is running, the current sample run will end and the playback of the play list
ends.

This is just one example of using a play list with the AS 6000 autosample r. The AS 6000
autosampler on a DSC 4000 or DSC 6000 does not have the Tare /Weigh feature, s o the
creation of a Samp le Group is not automated. You will have to weigh the samples before
placing them in the s ample pans and crimping the pans. You have to enter the weights into
the Sample Details area of the Edit Step: Sample section of the dialog box.

80 . DSC 4000 Installation and Hardware Guide

Troubleshooting

When the AS 6000 autosampler malfunctions, in most cases it will generate an error
message which is sent to the computer and is displayed in the Pyris software. The
troubleshooting list below should be used if the AS 6000 malfunctions.

To continue normal operation with the parent instrument, switch off the instrument and
switch it back on after 10 seconds. Depending on the error, normal operation may or may
not be possible. If normal operation can not be resumed, the problem has to be resolved by
a service engineer.

Error message ID Error Possible

Cause

ERR_NO_12VOLT No +12 V power supply

available (stepper motor
power supply)

ERR_HOR_STEP_BLOCKED Horizontal stepper motor

blocked

ERR_VER_STEP_BLOCKED Vertical stepper motor

blocked

Overload
condition in
switched power
supplies

12 V power
supply not OK

Blocked gear
wheels

Blocked by
external object

Incorrect
calibration

Blocked gear
wheels

Blocked by
external object

Inner lid of DSC
misplaced

Corrective
Action

Check stepper
motor wires

Replace AS 6000
assembly

Replace
controller PCB

Check gear
wheels

Remove external
object

Recalibrate the
AS 6000

Check gear
wheels

Remove external
object

Replace DSC
inner lid

ERR_DUE_TO_PARENT Parent instrument has

ERR_GRP_WIRE_BROKEN Gripper wire is broken or

entered fatal error state
that results in the
AS 6000 also entering
error state

no AS 6000 mechanics
connected

Error occurred
in parent
instrument

Gripper wire is
broken

AS 6000
connector not
connected

AS 6000 cable
not OK

Check parent
instrument

Replace gripper
assembly

Connect AS 600 0
connector

Check AS 6000
cable

AS 6000 Autosampler . 81

Error message ID Error Possible

Cause

ERR_GRP_NO_SAMPLE Gripper contains no

sample when entering
furnace. Light switch in
state

There was no
sample pan at
the reserved
position on the
sample tray

CST_FURN_PUT_SAMPLE
during an automatic

calibration

ERR_GRP_NOT_EMPTY Gripper still holds sample

while moving OUT of

Sample sticks to
gripper fingers

furnace during state
CST_FURN_PUT_SAMPLE
or in state
CST_PERFORM_TEST

ERR_LIGHT_SWITCH Light switches are not

functioning or ar e
blocked when the
gripper is in raised
position

Light switch is
blocked

Light switch in
not OK

AS 6000 cable
is not OK

Corrective
Action

Place a sample
on position 0 of
the sample tray

Clean gripper tips
Use clean sample

pans

Remove object
that blocks light
switch

Replace AS 6000
mechanics

Check/replace
AS 6000
connection board

ERR_MICRO_SWITCH Microswitch is activated

when gripper is NOT in
reset state

Microswitch is
not OK

Microswitch
wiring not OK

AS 6000 cable
not OK

Replace gripper
assembly

Check
microswitch
wiring

Check/replace
AS 6000
connection board

82 . DSC 4000 Installation and Hardware Guide

Error message ID Error Possible

Cause

ERR_FURN_NOT_EMPTY Furnace still contains a

sample while trying to
load a new one. This
error can be generated
only after loading at
least one sample after
power on, as the
instrument cannot detect
if a sample is present in
the furnace from a
previous power on
period

Failure picking
sample out of
furnace

Incorrect
horizontal
baseplate
adjustment

Incorrect
horizontal
calibration

AS 6000 run
was interrupted
after putting a
sample in
furnace and
restarting

ERR_NOT_AT_SENS Sensor position not

reached during
autocalibrating the
sensor position

Vertical stepper
missed steps
because it was
blocked while
running at slow
speed. (During
slow gripper
speed, the
stepper blocked
detection is
disabled.)

Corrective
Action

Check if gripper
fingers are bent.
Replace gripper
assembly

Adjust baseplate

Recalibrate the
AS 6000

Reset parent
instrument and
setup link again

Check the DSC
lower lid position

ERR_NO_ZERO_DETECT Zero position is not

detected

No detection of
the gripper
fingers because
of direct
sunlight at the
light switches

Gripper
assembly
displaced

Do not place
instrument in
direct sunlight

Align gripper
assembly

AS 6000 Autosampler . 83

Error Messages from the DSC 4000

Error message ID Error Possible Cause Corrective

Action

ERR_DUE_TO_AUTOSAMPLER AS 6000 entered

fatal error state.
This caused DSC
to enter fatal
error state

ERR_AUTOSAMPLER_RESPONS Timeout on

command.
Response from
command
transmitted to
AS 6000

ERR_AUTOSAMPLER_I2C_WD No link between

DSC and AS 6000
via I2C

Refer to AS 6000
error message

I2C connection
cable defective

I2C connection
cable defective

Refer to AS 6000
troubleshooting
(above)

Replace I2C cable

Replace I2C cable

84 . DSC 4000 Installation and Hardware Guide

There are no user-serviceable parts inside the autosampler.
Refer all servicing to a qualified PerkinElmer Instruments
service engineer.

Il n'y a pas de pièces réparables par l'utilisateur à l'intérieur
de l'échantillonneur automatique. Renvoyez tous les
services à un ingénieur de service qualifié PerkinElmer
Instruments.

AS 6000 Autosample r Maint enance

The exterior surfaces of the AS 6000 may be cleaned with a soft cloth, dampened with a mild
detergent and water solution.

The bushings of the gripper fingers should also be kept clean. Use a cotton swab dampened
with a mild detergent and water solution to carefully wipe them clean. Use the same method
to clean the two sample trays.

Cleaning and Decontamination

Before using any cleaning or decontamination methods except those specified by
PerkinElmer, you should check with PerkinElmer that the proposed method will not damage
the equipment.

WARNING

AVERTISSEMENT

AS 6000 Autosampler . 85

Install a Refere nce P an in a DSC 4000,
DSC 6000, Pyris 6 DSC or Jade DSC with
AS 6000 Autosampler

When running samples with the DSC 4000, DSC 6000, Pyris 6 DSC or the Jade DSC it is
recommended that a reference capsule be used in the furnace. The best reference material is
an empty sample pan and lid of the same type in which the sample material is encapsulated.
Because the autosampler and its base plate cover access to the reference pan area, they
have to be removed first. The procedure to do this and place a reference pan inside is as
follows:

1. Make sure that the power is off.

2. Remove both sample trays.

3. Remove the four screws that attach the autosampler to the base plate.

NOTE: Never remove the screws from the plate that is directly attached to the analyzer's

cover. This plate is positioned with respect to t he furnace. The positioning is
performed by the service engineer upon installation.

4. Place the tips of your fingers in the indents in the sides of the base plate and lift the
autosampler to disengage the D connector and the two standoffs on the base plate.

5. Remove the upper furnace lid and the base plate lid holder.

6. Remove the lower furnace lid and the lower furnace lid holder.

This exposes the reference pan position. The sam p le pan position is the one closer to
the side of the instrument. The reference pan position is closer to the center of the
instrument.

86 . DSC 4000 Installation and Hardware Guide

7. Place a reference pan on the reference position.

8. Replace the lower furnace lid holder.

9. Replace the base plate lid holder.

10. Use the furnace lid holder alignment tool to position the lower furnace lid holder
properly with respect to the upper lid holder.

Make sure that the tool is all the way down.

11. Look down throug h the tool and make sure that the furnace is centered in the tool.

12. Carefully remove the alignment tool without disturbing the lower furnace li d holder.

13. Place the autosampler on top of the base plate, aligning the two holes near the D
connector that engage the two standoffs on the base plate. Gently push the
autosampler down to snap in place.

14. Attach the autosampler to the base plate with the four screws.

15. Place the sample trays on the auto sampler with tray 1–22 toward the front and tray 23–
45 on the rear.

After placing a reference pan within the instrument and replacing the autosampler, you
should run through the gripper alignment procedure to make sure that the grip p er aligns
with the sample pans at locations 12 and 33.