Perkinelmer TGA 4000 User Manual

THERMAL ANALYSIS

TGA 4000
Installation and Hardware
Guide

Release History

Part Number Release Publication Date

09931396 C January 2018

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.

Or contact: http://www.perkinelmer.com/contactus/

Notices

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

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 © 2018 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

Notes, Cautions and Warnings ..................................................................... 8

Symbols Used on the Instruments .....................................................................11

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

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

Europe ......................................................................................................14

South Korea ..............................................................................................14

United States (FCC) ...................................................................................14

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

Pollution Degree 2 .....................................................................................15

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

Prepare the Laboratory ............................................................................ 17

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

Electrical Requirements ..............................................................................18

Environmental Requirements ......................................................................18

Purge Gas and Pneumatic Supply ...............................................................19

Space Requirements ..................................................................................19

Install Multiple Analyzers ........................................................................ 21

Install Multiple Analyzers ..................................................................................22

Install a TGA 4000 ................................................................................... 25

Safety Precautio ns for the TGA 40 00 .................................................................26

Important Specifi cations ............................................................................28

Decontamination and Cleaning ..........................................................................29

Decontamination .......................................................................................29

Cleaning the Instr ument ............................................................................29

General Laboratory Safety ..........................................................................29

TGA 4000 Warning Label s .................................................................................30

Warning Labels on the Up per Ring Around the Furnace................................30

Warning Labels on the Back of the TGA 4000 ..............................................32

Install a TGA 4000 ...........................................................................................34

Unpack the TGA 4000 .......................................................................................35

Parts Included ...........................................................................................36

Set Up the TGA 4000 System Components.........................................................38

Select the Correct Voltage ..........................................................................38

Connect the Purge Gas Supply to the TGA 4000 ..........................................40

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

Connect the Cooling Device to the TGA 4000 ..............................................41

Level the TGA 4000 ...................................................................................45

Connect the TGA 4000 System Com ponents ......................................................46

Configure the TGA 4000 ...................................................................................48

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

Calibrate the TGA 4000 ....................................................................................50

Furnace Calibration ....................................................................................50

Temperature Calibration ............................................................................51

Weight Calibration .....................................................................................53

TGA 4000 Hardware ................................................................................. 55

TGA 4000 Thermogravimetric Analyzer ..............................................................56

Features of the T GA 4000 .................................................................................57

Heating .....................................................................................................58

Sample Handling ............................................................................................. 59

Sample Preparation ................................................................................... 59

Sample Pans ............................................................................................. 59

Sample Atmosphere .................................................................................. 59

Loading the Sample into the TGA 4000 ....................................................... 60

Calibration ....................................................................................................... 61

Maintenance .................................................................................................... 62

Cleaning the Furnace and Sample Holder.................................................... 62

Cleaning the Cover .................................................................................... 62

Changing the Sample Thermocouple .......................................................... 63

TGA 4000 Part Numbers................................................................................... 65

Miscellaneous Part Numbers ...................................................................... 66

AS 8000 Autosampler............................................................................... 67

AS 8000 Autosampler ....................................................................................... 68

Safety Precautions for the AS 8000 ................................................................... 70

How the AS 8000 Autosampler Works ............................................................... 71

Autosampler Work Cycle ............................................................................ 71

Reduced Time Cycle .................................................................................. 73

AS 8000 Autosampler Gripper Alignment ........................................................... 74

AS 8000 Sample Handling ................................................................................ 75

Sample Preparation ................................................................................... 75

Sample Pans ............................................................................................. 75

Sample Loading ........................................................................................ 75

Running a Play List with the AS 8000 ................................................................ 78

Troubleshooting .............................................................................................. 82

Error Messages from the TGA 4000 ............................................................ 85

AS 8000 Autosampler Maintenance ................................................................... 86

Cleaning and Decontamination ................................................................... 86

Replace the Sample Thermocouple in a TGA 4000, Pyris 6 TGA or STA 6000

with AS 8000 Autosampler ............................................................................... 87

Introduction

6 . TGA 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 softw are 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 . TGA 4000 Installation and Hardware Guide

Symbols Used in Online Help

The Pyris help files contain information and warnings that must be followed by the user to
ensure safe operation and to maintain the instrument(s) in a safe condition.

Possible hazards that could harm the user or result in damage to the instrument are clearly
stated at appropriate places throughout Help.

All eight-digit numbers are PerkinElmer part 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 so me

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 . TGA 4000 Installation and Har d ware 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 . TGA 4000 Installation and Har d ware 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
d'aide. Seul un représentant du service PerkinElmer devrait être
autorisé à servir l'instrument.

AVERTISSEMENT

Safety and Regulatory Information . 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 . TGA 4000 Installation and Har d ware 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 instrument 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 equi pment 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 Communications 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 co ntain 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 . TGA 4000 Installation and Har d ware Guide

WEEE Instructions for PerkinElmer Products

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 recovery programs vary by regulatory authority at
your location. Contact your local responsible body (for example, your laboratory manager) or
authorized representative for information regarding 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.

Prepare th e Lab orat ory

18 . TGA 4000 Installation and Har d ware Guide

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.

Prepare the Laboratory . 19

• 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 safely 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 1 A 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.

20 . TGA 4000 Installation and Har d ware Guide

Install Multiple Analyzers

22 . TGA 4000 Installation and Har d ware 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 Mul tiport RS-232 Card (P/N 0940-2018). Installation of
the universal serial bus MUST be done before insta lling any analyzer.

A Pyris Series USB Multiport is an RS-232 m odule 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 0940-2020) and EdgePort/8 (P/N 0940-2019). 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 available (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 . 23

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.

24 . TGA 4000 Installation and Har d ware Guide

Install a TGA 4000

26 . TGA 4000 Installation and Har d ware 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'instruments lisent
et comprennent les précautions suivantes. Il est conseillé
de publier une copie de ces précautions sur ou près de
l'instrument lui-même.

Safety Precautions for the TGA 4000

WARNING

AVERTISSEMENT

The following precautions must be observed when using the TGA 4000:

• Never switch off the computer until it has completed its normal shutdown procedure.

• Never press the Reset button on the computer if the Pyris software appears to

malfunction. Press the CTRL–ALT–DEL keys simultaneously and select Task Manager.
From the Task Manager, close the Pyris software.

• Never remove the outer instrument cover of the TGA 4000 without shutting the
instrument down and disconnecting its power cord from the power source.

• Before connecting the TGA 4000 to the power outlet, check the voltage setting and
fuse.

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

• Do not disconnect cables or tubes from the TGA 4000 while the instrument is on.

• Never open the furnace when it is at a high temperature.

• Always observe the proper startup and shutdown procedures with the TGA 4000 and all

related instruments.

• 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.

• Use proper lifting posture when lifting the analyzer. The TGA 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 equipment or with
material contained in it.

Install a TGA 4000 . 27

To re move the furnace lid, always use tweezers; the furnace
might be hot .

Pour retirer le couvercle du four, utilisez toujours une pince
à épiler; le four pourrait être chaud.

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 TGA 4000. Operate the TGA 4000 in a fume
hood.

Assurez-vous toujours qu'il existe une ventilation adéquate
lorsque vous utilisez le TGA 4000. F a i te s fonct io nner le TGA
4000 dans u ne ho tt e a sp i ra nt e .

Ne pas exposer le support de l'échantillon aux contra intes mécaniques.
Si aucun refroidissement externe n'est appliqué, ne pas utiliser le TGA

WARNING

AVERTISSEMENT

WARNING

AVERTISSEMENT

WARNING

AVERTISSEMENT

CAUTION

ATTENTION

Do not expose the sample holder to mechanical stress. If no external
cooling is applied, do not ope rate the TGA 4000 above 50 °C.

4000 au-dessus de 50 ° C.

28 . TGA 4000 Installation and Har d ware Guide

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 TGA 4000 . 29

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.).

30 . TGA 4000 Installation and Har d ware Guide

HOT SURFACE

SURFACE CHAUDE

TGA 4000 Warning La bels

Warning Labels on the Upper Ring Around the Furnace

WARNING

AVERTISSEMENT

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

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

Install a TGA 4000 . 31

Toxic Gases – Fume Ventilation System

Gaz toxiques - Système de ventilation des fumées

WARNING

AVERTISSEMENT

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 instrument.

32 . TGA 4000 Installation and Har d ware Guide

Always keep airflow unobstructed

Toujours garder le flux d'air dégagé
Pour maintenir une ventilation adéquate, ne bloquez pas l'arrière de

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 TGA 4000

WARNING

AVERTISSEMENT

WARNING

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

l'instrument.

.

.

AVERTISSEMENT

Install a TGA 4000 . 33

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

.

34 . TGA 4000 Installation and Har d ware Guide

Install a TGA 4000

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

• Prepare the Laboratory (refer to page 18)

• Unpack the TGA 4000

• Set Up the TGA 4000 System Components

• Connect the TGA 4000 System Components

• Configure the TGA 4000

• Calibrate the TGA 4000

Install a TGA 4000 . 35

Unpack the TGA 4000

The TGA 4000 System consists of the following components:

• TGA 4000 Thermogravimetric Analyzer

• Spares and Accessory Kit

• Personal Computer

• Printer (Optional)

• Pyris

• Chiller (Optional)

The TGA 4000 comes set u p to operate at voltages of 200–240 V . However, it can easily be
set up to run at voltages of 100–120 V. Follow the instructions on page 38 to set your
TGA 4000 to the proper voltage for your laboratory.

The TGA 4000 comes wrapped in plastic and is surrounded by foam on all sides of the
analyzer. 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.

Examine the box for any damage. Check the contents of the Accessories kit against the
packing list. If any part is damaged or missing, contact the carrier and PerkinElmer
immediately.

36 . TGA 4000 Installation and Har d ware Guide

Parts Included

The Spares and Accessories Kit contains the f ollowing parts:

Description Part Number Quantity

Level indicator N5202088 1

Gas restrictor 01541498 1

Tweezers - flat forceps 09908400 1
Hose clamps 09920044 2

Fuse 6.3 A 09991662 2

Fuse 3.15 A 09991629 1

Magnet L9003459 1
Sample pan kit N5200040 1

Sample holder (3 pieces, 1 installed) N5203020 2

Calibration standards kit 02190071 1

Alsiflex paper (5 pieces) N5376819 1
Tubing adaptor, female 1/4 to 1/8 09903906 2

Calibration weight N5200042 1

Ceramic furnace ri ng N5376800 1

Install a TGA 4000 . 37

Also included with the TGA 4000 are:

Description Part Number Quantity
Tygon tubing for coolant 02506519 3 m

Teflon tubing for purge gas 02506483 6 m

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

USB cable — 1

Male RJ45 to DB9 modem cable 09410042 1

Power cable — 1

The procedure for unpacking the TGA 4000 is complete.
If you have purchas ed the AS 8000 Autosampler, this is installed at the factory.

— 2

38 . TGA 4000 Installation and Har d ware Guide

Ensure that the mains power lead is disconnected fro m 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 TGA 4000 System Components

Place the TGA 4000 on your laboratory 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 the system comp onents listed below before switching
on the TGA 4000:

• Select the correct voltage

• Install the gases

• Install the cooling device

• Level the TGA 4000.

Select the Correct Voltage

The TGA 4000 ac c epts the following voltages: 100–120 V and 200–240 V (50/60 Hz).
It is configured and shipped with 220 V selected . Selection of the correct voltage for your lab

can be done at the AC inlet plug at the r ear of the TGA 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 text in an upright position and the arrow
pointing at the small line represents the volt age that has been selected.

To change the voltage:

.

WARNING

AVERTISSEMENT

.

Install a TGA 4000 . 39

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, we are showing you where the fuses go. The fuse that is

installed is for 220V.

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.

40 . TGA 4000 Installation and Har d ware Guide

5. Reinsert the fuse holder.

Connect the Purge Gas Supply to the TGA 4000

The TGA 4000 has two sample purge gas inlets a nd a system purge gas inlet at the back of
the analyzer. The system purge gas must be a dry inert gas; preferred gases are nitrogen
and air (the latter only when measurements are performed in oxidative atmospheres). The
dry inert gas flows through the balance chamber to maintain a constant environment, to
prevent absorption or desorption of vapors, and to protect the balance against gaseous
products that evolve from the samples. The system purge gas must be present in the
balance chamber at all times. The system purge gas flow rate is controlled by a needle valve
inside the analyzer, and is preset to 40 ml/min. The system has an equilibration time of more
than 1 hour so you should leave this flow on permanently if the analyzer is used frequently.

NOTE: The TGA 4000 analyzer has a mass flow co ntroller 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 0154-1498) or a Float Displacement Flow Meter (P/N 0290-1624) 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. The sample purge (reaction) gas enters the furnace directly below the sample and
flows via the furnace wall to the sample. The reaction gas purges the sample holder/furnace
area. Since the furnace and sample holder are ceramic, any noncorrosive gas can 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 flow rate should not exceed the flow rate of the system purge gas.

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 and System Purge Gas Lines to the TGA 4000.

Install a TGA 4000 . 41

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

Perform the following procedure to connect your sample purge gas and system purge gas
lines to the TGA 4000 analyzer regardle ss of the other components in the purge gas line.
Assuming all the other components of the purge gas line are installed, you will now connect
1/8-in. Teflon tubing to the TGA 4000 using a female connector.

The TGA 4000 System Purge Gas for Balance (1 p c) and Sample Pur ge 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 Sample 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 TGA 4000 (Your instrument may
show a slight variation):

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

instrument.

Connect the Cooling Device to the TGA 4000

The TGA 4000 has an integrated cooling system. The cooli ng inlet and outlet are located at
the rear of the analyzer and are marked Cooling Liquid In and Cooling Liquid Out. The
TGA 4000 is not used in subambient conditions; its temperature range is 15 °C–995 °C.
Therefore, the only cooling devices available for the TGA 4000 are the Polyscience Chiller
(P/N N537-0220/N537-0221, 120 V and 220 V, respectively) and circulating tap water. The
coolant or tap water flows through the cooling jacket that is wrapped around the furnace. It
is important that no condensation forms on the cooling jacket.

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

42 . TGA 4000 Installation and Har d ware Guide

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

roidisseur. 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

20 ° C à 100 ° C, 5 0%

.

vous que les évents d'air de refroidissement à l'avant et à

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

.

Connecting to the Chiller

When using the chiller, connect the cooling supply to the TGA 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. Distilled water is recommended

–20 °C to 100 °C, 50% ethylene glycol in water is recommended.
Un fluide approprié doit être utilisé ave c le ref

être efficace jusqu'à -

entre 15 ° C et 90 ° C. Po ur une utilisation de ­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.

Assurez­minimum 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 tighten with a suitable wrench.

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

4. Push a hose (compatible with the d esired coolant) o nto 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 connecti on 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.

Install a TGA 4000 . 43

4000 n'acceptera PAS la 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

liquide doit être exempt 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 Sele ct/Set control on the front panel until the Pump/AutoTune m enu 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

CAUTION

ATTENTION

Setting the Coolant Temperature

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

The heat exchanger of the TGA 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 TGA

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

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.

44 . TGA 4000 Installation and Har d ware Guide

4000 n'acceptera PAS la pression. Par
conséquent, la régulation du débit devrait être effectuée avant que l'eau
entre dans le TGA 4000.

90

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

d'air influenceront

négativement la qualité du signal de mesure.

The degree fraction figure s 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 TGA 4000.

2. Connect one hose to the Cooling Liquid In tube. Place a hos e clamp around the hose
and tube to secure the hose in place.

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

4. Connect the other hose to the Cooling Li quid Out tube. Place a hose clamp around the
hose and tube to secure the hose in place.

5. Connect the other end of the hose to a suitable drain.

The temperature of the cooling liquid should not change more then 0.4 °C/hour in the case
of tap water.

CAUTION

ATTENTION

CAUTION

ATTENTION

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

L'échangeur de chaleur du TGA

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 will negatively
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 bulles

Install a TGA 4000 . 45

Level the TGA 4000

1. Lift the analyzer up at the front and turn each foot until it is screwed all the way into
the bottom of the analyzer.

NOTE: The analyzer is heavy. When lifting it along the front edge, be sure your hand is

firmly underneath it and can support the analyzer while you adjust the feet.

2. Position the analyzer in the exact spot on the bench where you will be using it.

3. Check whether the analyzer rocks on the bench, or if one foot is not touching the
bench. If so, lift the analyzer and slightly turn the foot clockwise to extend it. Lower the
analyzer to check that it does not rock. Once all of the feet are touching the bench,
make sure that the analyzer is steady.

4. Place the level provided in the Spares kit on the furnace plate on the top of the
analyzer.

5. Look at the level to see if the bubble is centered. If not, readjust the feet as in step 3
until the bubble is centered in the level.

The TGA 4000 is level when the bubble is centered inside the ring.

6. Once the analyzer appears to be level, again make sure all of the feet are in contact
with the bench and that the analyzer does not rock.

This procedure is complete.

46 . TGA 4000 Installation and Har d ware Guide

Connect the TGA 4000 System Components

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

Follow the steps below to co nnect the TGA 4000 t o the computer .

CAUTION

ATTENTION

The image below shows the connections on the TGA 4000 (Your instrument may show a
slight variation):

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

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

1. Connect one end of the USB cable to the back of the TGA 4000.

2. Connect the other end of the USB cable to 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, power on the system in the following order:
– Computer
– TGA 4000
– Printer

Install a TGA 4000 . 47

6. Turn on the sample purge gas, if you are going to use it (recommended flow rate =

30 ml/min), the system purge gas (recommended flow rate = 40 ml/min), and the
water for the cooling system or any other accessories for the cooling device you are
using.

7. Carefully grasp the sample holder with tweezers at the upper, shaped part.

8. Insert the alumina rod of the sample holder down through the center hole in the bottom

of the furnace. Move it downward until you feel a slight resistance. Move the sample
holder another 10 mm until you feel it stop.

DO NOT EXERT EXCESSIVE FORCE.

48 . TGA 4000 Installation and Har d ware Guide

Configure the TGA 4000

The Pyris Software must be configured for the TGA 4000. This must be done before the
TGA 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 t he screen.

2. Select the Add Analyzer 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 connect ed to port 1 of an EdgePort
USB. Click the Add button.

The TGA 4000's Configuration dialog box is displayed.

4. The system detects the type of analyzer that is attached and displays the default name

and other info rmation for a TGA 4000 in this dialog box. Select the accessories that are
attached to the analyzer (for example, Autosampler).

Install a TGA 4000 . 49

5. Click OK to accept the selections.

6. Click OK to exit the Configuration dialog box or select Add Ana l y z e r t o 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 by the Pyris
software.

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

Starting t h e Pyri s M ana ger

1. Select Pyris Manager from the Pyris Software group. The Pyris Manager is displayed on

the screen.

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

3. Now that the system is switched on, the TGA 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 butto n
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 installation of the TGA 4000 is complete. The analyzer is ready to be calibrated.

on the control panel and click on the button.

50 . TGA 4000 Installation and Har d ware Guide

Calibrate the TGA 4000

The TGA 4000 T hermogravimetric Analyzer has been calibrated at the factory. However, it
must be calibrated again before obtaining data from your samples. 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 TGA 4000 is shipped with the reference materials alumel, nickel, and iron for the
temperature calibration and a 100 mg stainless steel sphere for the weight calibration in the
Accessories kit.

The Calibration page in Pyris is accessed from the View menu of the Method Editor.
The three calibration routines should be performed in the order:

• Furnace

• Temperature

• Weight

Furnace Calibration

NOTE: The Furnace calibration must be performed before the Temperature calibration.

1. Make sure the sample holder is empty.

2. To verify thermocouple operation, program the temperature to 100 °C. Enter 100 in the

Go To Temp entry field of the control panel and click the Go To Temp button

on the control panel.

3. Check that the current sample temperature displayed in the status panel is at or below

the intended minimum calibration temperature. The easiest way to accomplish this is to

click the Go To Load button

4. While in Instrument Viewer or Method Editor, select Calibrate from the View menu.

5. Select the Furnace tab in the Calibration window.

6. In the Minimum field, enter a minimum temperature at which the calibration will begin.

This should be below your normal operating region.

NOTE: When selecting minimum and maximum temperatures for the furnace calibration,

select the limits so that they encompass the temperature range in which you plan to
operate. Maximum temperature minus minimum temperature must be greater than
100 °C or the furnace calibration will not be performed.

on the control panel.

7. In the Maximum field, enter a maximum temperature at which the calibration will end.

This should be above your normal operating region.

Install a TGA 4000 . 51

8. Click the Begin Calibration button.

A message stating that the system defaults will be used for all temperature calibrations
if you perform a furnace calibration is displayed. If you wish to continue, click OK. The
Furnace calibration begins immediately. The Furnace Calibration dialog box is displayed
showing the approximate time remaining in the calibration.

You can stop the calibration, which takes about an hour, by clicking the Stop
Calibration button.

9. When the calibration routine is finished, click the Save and Apply button in the

Calibration window to send the new calibration values to the analyzer and save the
calibration file.

10. Select the Temperature Calibration tab or the Close button to close the Calibration
window and begin using the new calibration values.

Temperature Calibration

NOTE: You must perform a Furnace calibration before a Temperature calibration.

To calibrate the temperature of the TGA 4000, perform the following steps:

1. While in Instrument Viewer or Method Editor, select Calibrate from the View menu.
The Calibration window is displayed.

2. Restore the default temperature calibration by selecting Temperature from the Restore
menu (this step is optional).

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.
Select OK to save the default file.

4. Click Close to close the Calibration window.

The TGA 4000 is calibrated by performing two runs each using two or three of the magnetic
standards provided: alumel, nickel, and iron. These are supplied with the instrument. The
runs should use the same conditions under which you would run your samples. This
temperature calibration uses the Curie transition of the materials, that is, the point at which
the magnetic properties disappear.

The first run of each reference material should use the lower scanning rate (for example,
5 °C/min) and the second run the higher scanning rate (for example, 50 °C/min). You must
run at least two reference mater ials but you can use all three if desired. Therefore, you will
do from four to six runs in order to perform a tem perature calibration.

After you have completed the steps above, go on to the following steps to complete the
temperature calibration:

5. From the Method Editor, select Open Method from the File menu and double-click
Alumel.t6m, Nickel.t6m, or Iron.t6m, depending on the sample you are going to run.

6. Place an empty sample pan on the sample holder that is already in place in the furnace.

7. Place the furnace lid back on the analyzer.

52 . TGA 4000 Installation and Har d ware Guide

8. Click the Zero Weight button on the control panel.
The weight of the empty sample pan is displayed in the Zero field on the Sample Info

page.

9. Remove the furnace lid. Without removing the pan, place a 1–2 mm length
(approximately 20 mg) of reference material in the sample pan.

10. Place the furnace l id on the analyzer, position the plastic spacer and the magnet over
the center of the lid, and click the Sample Weight button on the control panel.

The weight appears in the Weight field in the Sample Info page.

11. Complete the other information on the Sample Info page.

12. To run Curie points, you must run the reference material under the same experimental
conditions that you will run your samples. Check the purge gas type, coolants used, a nd
the scanning rate.

The first run of a reference material is performed at a scanning rate of 5 °C/min.

13. Start the run by clicking the Start Method button in the control panel.

14. When the run is finished, remove the sample pan and repeat steps 5 through 13 for the
same reference material but at a scanning rate of 50 °C/min.

15. After the second run for one reference material, repeat steps 5 through 14 for the other
reference material(s) you choose to use.

16. For each data file collected, open the Data Analysis window, select the data file, and
calculate the Offset value by performing an Onset calculation at the end of the Curie
point transition. Note the Onset result.

17. When all runs are complete and Onset calculations have been performed, select the
Calibrate command in the View menu.

The Calibration window appears.

18. Select the Temperature Calibration tab. Enter the Operator name. Enter the names of
the reference materials used, the expected Onset values (provided in the
documentation accompanying the reference materials), and the measured Onset results
at the two scanning rates for each reference material.

19. Enter the scanning rates used in the Rate 1 and Rate 2 fields and click the appropriate
option to indicate which references to use for the calibration: 1 and 2 or 1, 2, and 3.

20. 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.

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

Install a TGA 4000 . 53

Weight Calibration

To perform a weight calibration of the TGA 4000:

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

2. Select the Weight tab in the Calibration window.

3. Enter the weight of the reference material in the Ref. Weight box.
A 100 mg calibration weight is supplied with the instrument.

4. Click Begin Calibration.

5. To prepare for a zero weight reading, place a clean sample pan in the sample holder
and then replace the furnace cover.

6. Click OK in the dialog box.

7. When the zero weight reading is stable in the Read Zero field, click OK in the dialog
box.

8. Place the reference weight into the crucible. You can either first remove the crucible
from the furnace and place the weight in it or place the weight with the crucible in
place. Replace the furnace cove r. Click OK in the dialog box.

9. When the weight reading is stable in the Read Value field, click OK in the dialog box.
The calibration is complete.

10. Click Save and Apply to send the new calibration value to the analyzer and save the
calibration file.

The TGA 4000 calibrati on is comple te .
This completes the installation of the TGA 4000.

TGA 4000 Hardware

56 . TGA 4000 Installation and Har d ware Guide

TGA 4000 Thermogravimetric Analyzer

The TGA 4000 Thermogravimetric Analyzer features reliability, robustness, low cost of
operation, and ease of use, all of which make it an outstanding analyzer for quality control
laboratories.

The TGA 4000 is controlled by Pyris software, installed on the computer to which the
analyzer is connected. The TGA 4000 measures the weight of a substance as a function o f its
temperature or the time. Weight changes can be measured accurately, generating
information on various processes in a sample such as dehydration, degradation, oxid ation,
etc. Also, since measurements can be performed in a well-defined atmosphere, the behavior
of a sample in atmospheres other than air can be studied easily. The TGA 4000 can be used
for component analysis (weight %), evaluation of stabilizers, loss on drying, proximate
analysis, lubricating oil analysis, and oxidatio n studie s. The information it provides is
essential to industries such as plastics and polyme rs; automotive; semiconductors and
electronics; adhesives; paints and coating s; fuels; ceramics, clays, and soil; food;
pharmaceuticals; and medical devices and equipment.

For more information on the TGA 4000, see the following topics:

• Features of the TGA 4000

• Safety Precautions

• Sample Handling

• Calibration

• Maintenance

• TGA 4000 Part Numbers

• Autosampler

TGA 4000 Hardware . 57

Features of the TGA 4000

The TGA 400 has a high-performance balance and furnace for maximum accuracy and
precision. The top-loading balance allows easy sample loading and unloading. The balance is
protected from sample debris by a balance p urge gases, and thick stainless steel wall act as
a heat sink to thermally isolate the balance from the furnace. The TGA 4000 has a top­loading microbalance. The sample pan is placed onto the sample holder which connect s to
the microbalance via a very thin rod.

The furnace has a large isothermal zone, which keeps your samples at the same temperature
as the furnace throughout a temperature program. This increa ses reproducibility of
temperature measurements. The compact ceramic furnace is inert and corrosion resistance,
enabling the use of a wide range of reactive gases. The built-in mass flow controller monitors
and controls the purge gas flowrates and pressures, and can switch automatically between
sample gases using Pyris software.

The rapid cooling r ate of the furnace is achieved by mounting the furnace in a liquid-cooled
jacket. To reduce the heating power at high temperatures, the cooling jacket is nickel plated.
You can use various types of cooling liquids in the integrated cooling system. During
operation, the cooling liquid must flow through the heat exchanger at a constant flow rate
and the cooling liquid should be at a temperature such that there is no condensation inside
the analyzer. The recommended cooling device is the Chiller (P/N N537-0220/N537-0221,
120 V and 220 V, respectively).

Forced air cooling is also possible. A small air p ump is mounted inside the instrument and

activated by clicking the Cooling Air button
cooling reduces cycle times, improving productivity.

Pyris supports the AS 8000 autosampler accessory. The autosampler allows testin g of up to
45 samples. The unique two-piece carousel allows removal of one section while the other is
in operation. Combined with the Pyris Player software, the runs are entirely automated. You
can create play lists that contain multiple methods for analyzing one sample; multiple
samples to be analyzed by one method, and many ways to perform postrun data analysis.

on the control panel. Forced air and liquid

58 . TGA 4000 Installation and Har d ware Guide

Heating

The basic temperature range of the TGA 4000 is from ambient to 995 °C. Since the system is
liquid-cooled, it is possible, in principle, to begin a run at subambient temperatures.
However, condensation of water vapor on the cooling tubes around the furnace could occur
and should be avoided. Reducing condensation is the user’s responsibility.

The maximum heating rate at high temperatures is limited by the supply voltage, as shown
in the following table:

Supply Voltage / V Maximum heating rate at

900 °C / °C min

180 or 90 42 0
200 or 100 134 26

220 or 110 200 118

230 or 115 200 138

-1

Maximum heating rate at
995 °C / °C min-1

240 or 120 200 143
250 or 125 200 145

The heating rate can be set in 0.1 °C/min increments. In general, lower heating rates lead to
better separation of transitions. For most experiments, a heating rate of 20 °C/min is
optimal. The free heating rate of the TGA 4000 furnace has been limited to 200 °C/min.

TGA 4000 Hardware . 59

Sample Handling

The TGA 4000 meas ures the change in weight of a sample as a function of temperature or
time. The materials and techniques used to obtain data with a TGA 4000 are d iscussed
below.

Sample Preparation

The thermogravimetric analyzer analyzes solid samples in powder, crystal, or granular form.
Although quantitative accuracy will remain the same r egardless of sample shape, the
qualitative appearance of a run may be affected by the sample configuration. The best
sample form for optimum performance is powder or fine granules. Solid materials can be
sliced into small pieces with a razor or knife.

Sample Pans

The preferred sample pan is the self-centering, thin-walled, ceramic sample pan provided
with the instrument. The sample centers itself in the pan and the pan centers itself on the
sample holder. Three sample pans are provided in the Spares kit.

Other sample pans can also be used. The only requirement that the pans must meet is that
they do not react or melt within the temperature range of interest and that the sample does
not form alloys with the material of the sample pan.

Sample Atmosphere

It is important that the TGA 4000 is able to operate in various gas atmospheres. The change
from one atmosphere to another should be rapid. The TGA 4000 has one purge gas inlet for
the system purge gas inlet and two sample purge gas inlets at the back of the analyzer. The
system purge gas should be a dry inert gas that flows t hrough the microbalance chamber.
This keeps the environment of the balance constant, prevents absorption or desorption of
vapors, and protects the balance against gaseous products evolving from the samples. The
system purge gas has a flow rate of 40 ml/min. Since the equilibration time of the analyzer is
significant, it is recommended that the balance protective gas be present at all times.

You can control the atmosphere in which the sample is run by using a sample reactive or
purge gas to displace or introduce reactive gases into the sample furnace. Recommended
purge gases are air, nitrogen, argon, oxygen, and helium. When changing from one purge
gas to another, always check the temperature calibration. A flow rate of 20–40 ml/min is
recommended.

The reaction gas enters the furnace/sample area directly, just below the sample, and flows
via the furnace wall to the sample. Thus, dead volume can be low resulting in a small gas
change time constant. The time constant depends on the flow rate.

NOTE: The flow rate for the system purge gas should be equal to or greater than that for

the sample purge gas.

60 . TGA 4000 Installation and Har d ware Guide

The gas atmosphere should be pure (99.9% minimum), especially if you use nitrogen. There
should be no trace of oxygen as this could lead to unwanted reactions. The gas must be
dry.

The degradation byproducts from the sample leave the instrument directly via a small hole in
the furnace cover. These byproducts could be harmful , s o use adequate suction such a fume
hood. There is some condensation of less volat ile products on the cold spots of the analyzer:
the lower side of the cover and the upper inner side of the cooling jacket. These spots can
be cleaned easily with a suitable solvent. Conde nsa tion may also occur on the top inner side
of the cooling jacket. To prevent this, use the porous ceramic furnace cover to absorb the
less volatile byproducts. When necessary, this ring should be changed.

Loading the Sample into the TGA 4000

Use the following procedure to load samples or remove samples:

1. Using tweezers, remove the stainless steel cover off of the top of the analyzer. Place it
on the stainless steel ring surrounding the opening to the furnace.

2. Place the sample inside the sample pan.

3. With tweezers, carefully place the sample pan with sample onto the sample holder and
make sure that the pan is centered.

4. Replace the lid.

TGA 4000 Hardware . 61

Calibration

The furnace, temperature, and weight are calibrated by the service engineer upon
installation. The TGA 4000’s cal ibration should remain unchanged for quite some time,
provided that there are no changes in the instrument’s operating conditions. Even when the
system is shut off, the calibration values are stored so that the next time the instrument is
turned on, it will still be calibrated. Some of the conditions that could change either the
temperature or the weight calibration of the TGA 4000 and require reca libration are as
follows:

• If the operating temperature range of your experiments changes, recalibration may be
necessary. Check the temperature calibration in the range of interest to determine if the
current calibration is still valid.

• If the purge gas type or purge gas flow rate changes, the calibration should be checked
for highest accuracy.

• If a new furnace is installed, the temperature calibration should be checked.

• If a new sample holder is installed, the system should be recalibrated.

• If a new sample thermocouple is installed or if the existing thermocouple has been

disturbed, you should perform a temperature calibration.

• If the analyzer is moved or re-leveled, you should perform a weight calibration.

62 . TGA 4000 Installation and Har d ware Guide

Ne pas enlever le couvercle du four lorsqu'il chauffe à des températures

Maintenance

The TGA 4000 Thermogravimetric Analyzer needs little routine maintenance other tha n
giving it the proper treatment of a sensitive electromechanical device. Avoid contamination of
the furnace by always using a balance protective gas a nd a purge gas. If the f urnace should
become contaminated, clean it as soon as possible.

Maintenance includes the following procedures:

• Cleaning the Furnace and Sample Holder

• Cleaning the Cover

• Changing the Sample Thermocouple

Cleaning the Furnace and Sample Holder

When the furnace and sample holder have become contaminated with reaction products, the
best method of cleaning them is to heat the furnace up to 995 °C in an air or oxygen
atmosphere for approximately 10 minutes. This should remove all products that can be
oxidized.

CAUTION

ATTENTION

CAUTION

ATTENTION

If the sample holder becomes contaminated, remove it from the furnace and clean it gently
with a small brush.

When a sample has dropped into the furnace, remove the sample holder first, if present, and
then remove the sample material, preferably with a vacuum. Take care that material does
not fall into the hole for the sensor.

Do not touch the sample thermocouple (in the TGA 4000)..
Ne pas toucher l'échantillon de thermocouple (dans le TGA 4000).

Do not remove the furnace lid when he ating at high temperatures.

élevées.

Cleaning the Cover

The reaction byproducts from the samples run inside the STA 6000, TGA 4000 and Pyris 6
TGA furnace and condense on cold spots of the instrument: the bottom side of the cover and
the top inner part of the cooling jacket. The bottom side of the cover can be cleaned easily
with a tissue and some solvent. This should be done on a regular basis. The top inner side of
the cooling jacket can be cleaned in a similar manner. To keep the top of the cooling jacket
clean, a ring of porous ceramic material is provided and should be positioned as seen in the
figure displayed by clicking here. The ring should be replaced when necessary.

TGA 4000 Hardware . 63

Changing the Sample Thermocouple

The sample thermocouple has a limited lifetime because of the range of temperatures and
the high maximum temperature it withstands. Therefore, the TGA 4000 and Pyris 6 TGA are
designed so that a user can change the sample thermocouple.

To remove the sample thermocouple, perform the following procedure:

1. Switch off the analyzer and the remove the power cord.

2. Remove the furnace lid.

3. Remove the porous ceramic ring.

4. Remove the sample holder.

5. Remove the three screws of the top stainless steel furnace plate and then remove the
plate.

6. Lift the tape off the top of the furnace to free the thermocouple.

7. Unplug the yellow thermocouple plug.

64 . TGA 4000 Installation and Har d ware Guide

8. While holding the plug, gently lift the thermocouple up and out of the furnace. Be
careful not to bend the thermocouple. Note how the thermocouple is positioned in the
furnace wall.

To install a new sample thermocouple, perform the following steps:

1. While holding the new thermocouple by its yellow plug, gently lower it into the furnace.
Make sure that the lower vertical ceramic bead goes into the slit in the furnace wall.
The two wires at the end of the thermocouple should be inside the furnace, near the
center hole, but n ot over it. The horizontal bead at the to p of the thermocouple should
lie inside the groove at the top of the cooling jacket.

2. Connect the thermocouple plug with the connector at the side of the jacket.

3. Replace the tape covering the thermocouple at the top of the cooling jacket.

4. Replace the stainless steel furnace plate and replace the three screws.

5. Position the sample holder in the furnace.

6. Reposition the porous ceramic ring.

7. Place the furnace lid back on top of the analyzer.

8. Reconnect the pow er cord and switch on the analyzer.

Perform a temperature calibration.

TGA 4000 Hardware . 65

TGA 4000 Part Numbers

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

www.perkinelmer.com/supplies

selection of high-quality thermal analysis 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 N520-0110).

Part No. Description Quantity

01541498 H restrictor 1

02190071
includes:

09988015
N5190869
09988018
09909608

09908400 Tweezers – flat forceps 1

L9003459 Magnet (with plastic spacer) 1

N5200040 Ceramic sample pans 1
N5203020 Sample holder (3) 2

www.perkinelmer.com

Calibration standards Kit

Alumel calibration standard
Nickel calibration standard
Iron calibration standard
Calibration specification card

.

1

1
1
1
1

(+1 installed)

09903906 Female connector 1/8 in. to 1/4 i n. 2

09920044 Hose clamps 2
N5200042 Calibration weight 1

N5376800 Ceramic furnace ri ng 1

09991629 Fuse 3.15 A slow blow 1

09991662 Fuse 6.3 A slow blow 2
N5376819 Alsiflex strips 5

66 . TGA 4000 Installation and Har d ware Guide

Also included with the TGA 4000 are:

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

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

• 5/16-in. pipe for Swagelok Cooling Liquid In and Out connectors

• USB cable for communicating to the computer

• Power cable

Miscellaneous Part Numbers

Part Number Description

N5370210 TGA 4000

N5370211 TGA 4000 with Autosampler

N5202070 Mini drybox
09991662 Fuse for 100–120 VAC, 6.3 A T, 250 VAC, 5 x 20 mm

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

AS 8000 Autosampler

68 . TGA 4000 Installation and Har d ware Guide

Maximum load

0.5A

Maximum supply voltage

24V DC

Fuses

Fused by parent instrument (0.9A)

Pollution degree

2

Overvoltage category

II

Protection class

IP20

AS 8000 Autosampler

The AS 8000 autosampler accessory brings automation capability to the DSC 4000, DSC
6000, STA 6000 and TGA 4000 when use d in conjunction with the Pyris software Player
feature.

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

operate the AS 8000 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 8000 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 8000 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 autos ampler 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.

AS 8000 Autosampler . 69

• 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 pla te. 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.

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 a nalyses together to be run in any order. See the Software
help for details.

The following topics discuss the AS 8000 autosampler in more detail:

• Safety Precautions

• How the Autosampler Works

• Autosampler Gripper Alignment

• Sample Handling

• Running a Play List

• Troubleshooting

• Maintenance

• Replace a Sample Thermocouple in a TGA

70 . TGA 4000 Installation and Har d ware Guide

To remove the furnace lid(s) of the parent instrument,
always use tweezers. The 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

est bien

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

Safety Precautions for the AS 8000

The safety precautions to be followed when using the AS 8000 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 8000
is properly attached to the base plate on the parent instrument.

Avant d'allumer l'instrument parent, assurez-vous que l' AS 8000

AS 8000 Autosampler . 71

How the AS 8000 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 to recognize it.
See the software Help for details.

The AS 8000 autosampler is computer controlled and fully automated. Information between
the host computer with Pyris software and the AS 8000 is sent via the parent instrument's
connection to the computer via the RS-232 port. Light switch sensors by the furnace acc ess
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 sam ple 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.

72 . TGA 4000 Installation and Har d ware 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 f urnace.

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 8000 Autosampler . 73

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.
The procedure below is 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 implies 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 procedure above.

74 . TGA 4000 Installation and Har d ware Guide

AS 8000 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 perfor m a
gripper alignment procedure.

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

clicking the Autosampler Control button
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 not necessary to have sample
pans in positions 12 and 33. If you wish to use the pr evious calibration's values as a
start for this calibration, click the radio button. (The calibration values are stored in the
firmware on the AS 8000 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 instrument.

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 8000 Autosampler . 75

AS 8000 Sample Handling

Sample Preparation

See the sample preparation instructions for the parent instrument.

Sample Pans

The types of sample 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 p ans are 10, 25, 30, and 50 µL.

Sample Loading

Before loading the sample int o the crucibles 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.

76 . TGA 4000 Installation and Har d ware 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 8000 Autosampler . 77

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.

78 . TGA 4000 Installation and Har d ware Guide

Running a Pl ay Lis t wi th the AS 8000

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 have 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 previous 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. Turn on the chiller and adjust according to its
instructions.

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

5. Turn on the power to the system components.

6. Prepare your samples.

7. 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 8000 Autosampler . 79

– Click OK and the Tare/Weigh System dialog box appears. The AS 8000 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 tar ing is complete, click the Done
button. The Sample List will be filled in.

80 . TGA 4000 Installation and Har d ware 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 fi nd 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 clicking 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 8000 Autosampler . 81

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

9. Start playback of the play list by clicking the Start at Top button o r 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 8000 autosampler. The AS 8000
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.

82 . TGA 4000 Installation and Har d ware Guide

Troubleshooting

When the AS 8000 autosampler malfunctions, in most case s 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 8000 malfunctions.

To continue normal operation with the parent instrument, power off the instrument and
power 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 8000
assembly

Replace
controller PCB

Check gear
wheels

Remove external
object

Recalibrate the
AS 8000

Check gear
wheels

Remove external
object

Replace DSC
inner lid

ERR_DUE_TO_PARENT Parent instrument has

entered fatal error state
that results in the AS
8000 also entering error
state

ERR_GRP_WIRE_BROKEN Gripper wire is broken or

no AS 8000 mechanics
connected

Error occurred
in parent
instrument

Gripper wire is
broken

AS 8000
connector not
connected

AS 8000 cable
not OK

Check parent
instrument

Replace gripper
assembly

Connect AS 8000
connector

Check AS 8000
cable

AS 8000 Autosampler . 83

Error message ID Error Possible

Cause

ERR_GRP_NO_SAMPLE Gripper contains no

sample when entering
furnace. Light switch in
state

CST_FURN_PUT_SAMPLE
during an automatic

calibration

ERR_GRP_NOT_EMPTY Gripper still holds sample

while moving OUT of
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

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

Sample sticks to
gripper fingers

Light switch is
blocked

Light switch in
not OK

AS 8000 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 8000
mechanics

Check/replace AS
8000 connection
board

ERR_MICRO_SWITCH Microswitch is activated

when gripper is NOT in
reset state

Microswitch is
not OK

Microswitch
wiring not OK

AS 8000 cable
not OK

Replace gripper
assembly

Check
microswitch
wiring

Check/replace AS
8000 connection
board

84 . TGA 4000 Installation and Har d ware 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

ERR_NOT_AT_SENS Sensor position not

reached during
autocalibrating the
sensor position

Failure picking
sample out of
furnace

Incorrect
horizontal
baseplate
adjustment

Incorrect
horizontal
calibration

AS 8000 run
was interrupted
after putting a
sample in
furnace and
restarting

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 8000

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 8000 Autosampler . 85

Error Mes sag es f rom th e TGA 4000

Error message ID Error Possible Cause Corrective

Action

ERR_DUE_TO_AUTOSAMPLER AS 8000 entered

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

ERR_AUTOSAMPLER_RESPONS Timeout on

command.
Response from
command
transmitted to AS
8000

ERR_AUTOSAMPLER_I2C_WD No link between

TGA and AS 8000
via I2C

Refer to AS 8000
error message

I2C connection
cable defective

I2C connection
cable defective

Refer to AS 8000
troubleshooting
(above)

Replace I2C cable

Replace I2C cable

86 . TGA 4000 Installation and Har d ware 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 8000 Autosample r Maint enance

The exterior surfaces of the AS 8000 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 8000 Autosampler . 87

Replace the Sample Thermocouple in a TGA 4000, Pyris 6 TGA or STA 6000 with AS 8000 Autosampler

1. Switch off the instrument.

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 the furnace. The positioning is
performed by the service engineer upon installation.

4. Place your fingers in the indents in the sides of the base plate and lift the autosampler
up and away from the instrument.

5. Remove the furnace lid and the lid holder.

6. Remove the base plate thermocouple cover.

7. Remove the alumina furnace cover disk.

8. Remove the alsiflex strip.

9. Remove the sample holder.

88 . TGA 4000 Installation and Har d ware Guide

10. Remove the thermocouple by disconnecting the thermocouple connector and gently
pulling the thermocouple out of the furnace.

11. Install the new thermocouple and replace the sample holder, alumina furnace cover
disk, and the alsiflex strip.

12. Replace the lid holder and furnace lid.

13. Replace the base plate thermocouple cover.

14. Place the autosampler on top of the base plate, aligning the screw holes.

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

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

After installing a new sample thermocouple, you will have to perform the gripper alignment
procedure.