Frontier EGA/PY-3030D Bedienungsanleitung

Ver.1.36

MULTI-SHOT PYROLYZER

MODEL EGA/PY-3030D

OPERATION MANUAL

www.frontier-lab.com

A-2 Ver.1.36

BEFORE USING THIS PYROLYZER

1. Thank you for purchasing Frontier Laboratories’ Multi-Shot pyrolyzer. Read through this operation

manual carefully before attempting any operation, particularly if you are a first-time user. This manual

is designed to assist you with your daily operations.

2. This manual contains categorized descriptions of the installation, operation, maintenance,

trouble-shooting, etc of the Multi-Shot pyrolyzer. We recommend that you read this manual along with

the operation manual of the gas chromatograph you are using.

3. Consumable parts are described in Appendix-1 and 2. Parts can be purchased from your local sales

representative office.

Physical appearance and specifications are subject to modifications without notice.

PRODUCT WARRANTY

Frontier Laboratories Ltd. warrants this product against defects or failures in accordance with the warranty

terms and conditions stipulated in a separate sheet. The product warranty can also be downloaded from

our website.

ABOUT PRODUCT SUPPORT PERIOD

We will stock consumable and maintenance parts and will accept inspection and repair orders seven

years from the date of product sales termination. However, in the event where electronic parts supplied

from parts manufacturers are discontinued; thus our stock level becomes too low, we may not be able to

provide support even within seven years from the date of product sales termination,.

A-3 Ver.1.36

FOR YOUR SAFETY

Warning symbol and signal words

The following warnings and precautions labels are affixed to this product and this manual. When these

precautions are displayed, it indicates that misoperation may cause severe injury to your body and the

products

In this manual, the safety instructions are ranked as warning, caution, and caution hot.

To use this product safely and properly, be sure to read the safety precautions and warnings before

attempting to operate. If this product is used in a manner not instructed in this manual, the protective

functions of this product may not be activated. Frontier Laboratories Ltd. will not be responsible for

losses incurred due to the neglect of these precautions and warnings.

Other important handling information is placed in a frame like this.

It indicates that incorrect handling may cause severe personal

burn.

CAUTION

HOT

This hazard signs indicates that incorrect handling may cause

hazardous conditions, resulting in death or severe personal injury.

This sign indicates that incorrect handling may cause hazardous

conditions resulting in minor or moderate personal injury and

physical damage.

CAUTION

WARNING

A-4 Ver.1.36

Operation of the pyrolyzer with the furnace temperature over 800°C for a long period time will

shorten the useful lifetime of the furnace heater. Operation of the pyrolyzer over 800°C should be 20

minutes or less. Also, when the pyrolyzer is at standby, keep the furnace temperature below 200°C.

This will extend the useful time of the furnace heater.

IMPORTANT NOTE WHEN OPERATING PYROLYZER OVER 800°C

There is a risk of severe burn. Always ensure that the protective

housing cover is placed properly on the pyrolyzer. When removing

the cover from the pyrolyzer, make sure that the furnace

temperature is 100°C or below.

CAUTION

HOT

Risk of electrical shock. Do not remove the temperature controller

housing cover, unless you are a service engineer certified by

Frontier Laboratories Ltd..

WARNING

If dust is deposited on the power code plug or the cable

connectors, clean them thoroughly. Be sure to unplug the power

code. Do not use water or organic solvent. Use a dry cloth or

brush. There is a risk of fire, if dusty connectors are used.

WARNING

This product uses compressed air or nitrogen for cooling the

pyrolyzer furnace. Ensure that you have a good ventilation if

nitrogen gas is used. There is a risk of suffocation, if it is used in a

confined area with poor ventilation.

WARNING

When flammable solvents such as benzene, toluene, or acetone

are used for your sample, work in a well-ventilated area such as in

a hood and area where no open flame is used nearby to avoid

catching fire.

CAUTION

The interface needle of the pyrolyzer has a very sharp point. When

replacing the interface needle, be sure to wear protective gears

such as gloves, safety goggles, etc.

CAUTION

The pyrolyzer uses a quartz pyrolysis tube. If this tube is broken,

broken pieces have very sharp edges. When replacing the tube, be

sure to wear protective gears such as gloves, safety goggles, etc.

CAUTION

A-5 Ver.1.36

CONTENTS IN THE PACKAGE

A-6 Ver.1.36

A-7 Ver.1.36

TABLE OF CONTENTS

BEFORE USING THIS PYROLYZER·················································································A-2

PRODUCT WARRANTY ·································································································A-2

ABOUT PRODUCT SUPPORT PERIOD ············································································A-2

FOR YOUR SAFETY······································································································A-3

CONTENTS IN THE PACKAGE ·······················································································A-5

TABLE OF CONTENTS··································································································A-7

CHAPTER 1 ABOUT MULTI-SHOT PYROLYZER······························································1-1

1.1 BACKGROUND OF DEVELOPMENT····················································································1-1

1.2 FEATURES OF EGA/PY-3030D···························································································1-3

1.3 PERIPHEREAL DEVICES···································································································1-4

1.4 SCHEMATIC OF MULTI-SHOT PYROLYZER FURNACE··························································1-5

CHAPTER 2 SPECIFICATIONS······················································································2-1

About cooling time of pyrolyzer furnace ·························································································2-3

CHAPTER 3 INSTALLATION·························································································3-1

3.1 PREPARING INSTALLATION······························································································3-1

3.1.1 Before installation······································································································3-1

3.1.2 Pumping down MS (for saving installation time) ·······························································3-2

3.2 REPIPING CARRIER GAS LINE···························································································3-2

3.3 SETTING UP GC INJECTION PORT·····················································································3-3

3.3.1 Replacing septum nut of GC injection port ······································································3-3

3.3.2 Replacing septum······································································································3-3

3.3.3 About injection port liner······························································································3-3

3.4 SETTING UP PYROLYZER FURNACE··················································································3-3

3.4.1 Installing quartz pyrolysis tube to pyrolyzer ·····································································3-3

3.4.2 Attaching interface union and needle·············································································3-3

3.4.3 Mounting pyrolyzer on GC···························································································3-3

3.5 CONNECTING TEMPERATURE CONTROLLER·····································································3-4

3.5.1 Connecting power cable to outlet··················································································3-4

3.5.2 Connecting to control PC ····························································································3-4

3.5.3 Hooking up remote signal cable····················································································3-4

3.6 CONNECTING COOLING GAS LINE ····················································································3-4

3.6.1 About cooling gas······································································································3-4

3.6.2 Connecting temperature controller and pyrolyzer······························································3-4

3.7 CONNECTING FURNACE PURGE GAS TUBE·······································································3-5

3.7.1 When He or N2 is used as a carrier gas ·········································································3-5

3.8 INSTALLING PERIPHERAL DEVICES···················································································3-6

A-8 Ver.1.36

3.8.1 Connecting Auto-Shot sampler (AS-1020E) ····································································3-6

3.8.2 Connecting other peripheral devices··············································································3-6

3.9 INSTALLING CONTROL SOFTWARE···················································································3-7

3.9.1 Installing USB serial communication device driver····························································3-7

3.9.2 Installing control software····························································································3-8

3.9.3 Setting COM port·······································································································3-8

3.10 FRONT, BACK, SIDE, AND TOP VIEWS·············································································3-10

3.10.1 Pyrolyzer ·················································································································3-10

3.10.2 Temperature Controller·······························································································3-11

CHAPTER 4 USING CONTROL SOFTWARE····································································4-1

4.1 START UP AND SCREEN LAYOUT······················································································4-1

4.1.1 Starting program ·······································································································4-1

4.1.2 Screen layout ···········································································································4-2

4.2BEFORE STARTING AN ANALYSIS·····················································································4-4

4.2.1 System configuration··································································································4-4

4.2.2 Set-up interface temperature························································································4-6

4.3SET-UP ANALYTICAL MODES AND OPERATION·································································4-7

4.3.1 Set-up for Single-Shot analysis and operation procedure···················································4-7

4.3.2 Set-up for Double-Shot analysis and operation procedure··················································4-9

4.3.3 Set-up for Direct EGAt analysis and operation procedure···················································4-12

4.3.4 Set-up for Heart-Cut EGA analysis and operation procedure ··············································4-14

4.4OTHER FUNCTIONS ·······································································································4-17

4.4.1 Saving/loading analysis set-ups····················································································4-17

4.4.2 Temperature calibration of pyrolyzer furnace and other set-ups···········································4-17

4.4.3 Printing set-ups·········································································································4-20

4.4.4 Set-up the Py Conditioning Table··················································································4-20

CHAPTER 5 FOUR ANALYSIS METHODS AND SAMPLE PREPARATION····························5-1

5.1 SINGLE-SHOT ANALYSIS··································································································5-1

5.2 EVOLVED GAS ANALYSIS (EGA)························································································5-3

5.3 DOUBLE-SHOT ANALYSIS·································································································5-5

5.4 HEART-CUT ANALYSIS·····································································································5-7

5.5 SAMPLE PREPARATIONS ·································································································5-9

5.6 SELECTION OF SAMPLE CUPS AND STICKS·······································································5-11

CHAPTER 6 MAINTENANCE·························································································6-1

6.1 ROUTINE MAINTENANCE··································································································6-1

6.1.1 Cleaning sample cups (Eco-cup)······················································································6-1

6.1.2 Replacing and cleaning quartz pyrolysis tube······································································6-3

6.1.3 Interface needle············································································································6-7

6.1.4 GC injection port···········································································································6-8

A-9 Ver.1.36

6.2 REGULAR MAINTENANCE·································································································6-9

6.2.1 Pyrolyzer furnace········································································································6-9

6.2.2 GC injection port·········································································································6-10

6.2.3 Temperature Controller································································································6-10

6.2.4 When not in use for a long period of time·········································································6-10

6.2.5 List of recommended replacement parts ··········································································6-11

6.2.6 Periodic maintenance and inspection··············································································6-11

CHAPTER 7 TROUBLESHOOTING ················································································7-1

7.1 PYROLYZER FURNACE ····································································································7-1

7.2 TEMPERATURE CONTROLLER··························································································7-3

7.3 TYPICAL TROUBLESHOOTING PROCEDURE ······································································7-4

7.4 LIST OF ERROR CODES FROM COTROL SOFTWARE···························································7-6

CHAPTER 8 GUARANTEE OF BASIC PERFORMANCE (REPRODUCIBILITY) ······················8-1

CONSUMABLE PARTS LIST ··············································································· Appendix-1

PYROLYZER MAJOR CONSUMABLE PARTS ························································ Appendix-3

LIST OF OPTIONAL PRODUCTS·········································································· Appendix-4

1-1 Ver.1.36

CHAPTER 1 ABOUT MULTI-SHOT PYROLYER

1.1 BACKGROUND OF DEVELOPMENT

Pyrolysis gas chromatography (Py-GC) can be used to characterize most materials including

insoluble materials and complex materials at trace levels often without any pretreatment of the

samples. Unique information about the sample, which is unobtainable by other analytical techniques,

makes Py-GC techniques essential in virtually every type of laboratory. Historically, data obtained

using Py-GC has suffered from poor reproducibility and poor recoveries of reactive compounds.

Frontier Laboratories has overcome these shortcomings by designing a system based on a technique

developed by Emeritus Professor Shin Tsuge of Nagoya University. Professor Tsuge’s technique

utilizes a small cup. Sample is placed in the cup which then free-falls into a micro furnace. The

sample temperature goes from ambient to the pyrolysis (i.e., furnace) temperature in several tens of

milliseconds. This system features precise temperature control and minimal condensation of

pyrolyzates in the system. In 1992, Frontier Laboratories commercialized the Double-Shot pyrolyzer.

The Double-Shot pyrolyzer added a completely new dimension to polymer analysis. For the first time

the volatile compounds and pyrolyzates originating from a polymer could be analyzed separately.

The Double-Shot pyrolyzer features a temperature programmable furnace which can be used to

perform Evolved Gas Analysis (EGA). With this technique, volatiles and pyrolyzate gasses from a

polymeric sample evolve continuously as the sample is heated. A plot of sample temperature vs.

detector response is termed as an EGA thermogram. EGA is similar to thermal gravimetric analysis

(TGA). EGA is currently used in many research laboratories for the detailed determination of the

thermal and chemical behavior of polymers, and also in production facilities as a quality control

method.

Frontier Laboratories also offers a number of Ultra ALLOY®metal capillary columns. They provide

contamination resistance about four times greater and thermal stability 50ºC higher than columns

made using fused silica tubing. They are ideally suited for the analysis of pyrolyzates ranging from C1

to over C100.

Our research and development team has devoted years of basic research to improve the quality of

the Double-Shot pyrolyzer and has developed and commercialized a variety of peripheral devices.

These have greatly expanded the application areas of the Double-Shot pyrolyzer.

Over the past 20 years, a variety of high performance polymeric materials have appeared in the

market which has generated a demand for a quantitative technique to characterize these materials.

In particular, the thermal decomposition behaviors of the materials at high temperatures are of

considerable interest. The sheer number of new formulations and additive packages has increased

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