Flash 4000 OPM

Organic Elemental Analysis
FLASH 4000
Elemental Analyzer
Operating Manual
P/N 317 110 52, Revision A October 2008 HOME
For Research Use Only

Not for use in Diagnostic
Procedures
© 2008 Thermo Fisher Scientific Inc. All rights reserved.
Published by Thermo Fisher Scientific, Voltaweg 22 2627 BC Delft, the Netherlands

Tel: +31(0)15 257 13 14 Fax: +31(0)15 257 22 97
Trademarks
Flash 4000 and Eager Xperience are trademarks of Thermo Fisher Scientific Inc.,and its subsidiaries. Other
brand and product names may be trademarks or registered trademarks of their respective companies.
Thermo Fisher Scientific Inc. provides this document to its customers with a product purchase to use in the
product operation. This document is copyright protected and any reproduction of the whole or any part of this
document is strictly prohibited, except with the written authorization of Thermo Fisher Scientific Inc.
The contents of this document are subject to change without notice. All technical information in this
document is for reference purposes only. System configurations and specifications in this document supersede
all previous information received by the purchaser.
Thermo Fisher Scientific Inc. makes no representations that this document is complete, accurate or error-
free and assumes no responsibility and will not be liable for any errors, omissions, damage or loss that might
result from any use of this document, even if the information in the document is followed properly.
This document is not part of any sales contract between Thermo Fisher Scientific Inc. and a purchaser. This
document shall in no way govern or modify any Terms and Conditions of Sale, which Terms and Conditions of
Sale shall govern all conflicting information between the two documents.
Release history:
First Edition, released October 2008
For Research Use Only. Not regulated for medical or veterinary diagnostic use by U.S. Federal Drug
Administration or other competent authorities.
C
Contents
Declaration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . vii
Preface . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .ix
Compliance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .xi
Safety Alerts and Special Notices . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .xi
Safety Symbols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .xi
Types of Alerts and Signal Words . . . . . . . . . . . . . . . . . . . . . . . . . . . . xii
Special Notices . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . xii
Instrument Markings and Symbols. . . . . . . . . . . . . . . . . . . . . . . . . . . . . xii
Using the Flash 4000 Document Set . . . . . . . . . . . . . . . . . . . . . . . . . . . xiv
Chapter 1 Preliminary Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15

Classification of the Instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
Environmental Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
Technical Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
Safety Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
Use of Gases . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
Purity of Gases . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
Nominal Pressure of Gases . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
Safety Cut Off Device . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
Instrument Cleaning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
Instrument Configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
Standard Outfit. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
Part 1 Description
Chapter 2 Structure of the Instrument. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21

The Units Constituting the Instrument . . . . . . . . . . . . . . . . . . . . . . . . . 21
Analytical Section . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
Autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
Reactors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
Furnaces . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
Water Condensate Drainage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
Regenerative Carbon Dioxide Filters . . . . . . . . . . . . . . . . . . . . . . . . . . 22
Chromatographic Column . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
Thermal Conductivity Detector (TCD) . . . . . . . . . . . . . . . . . . . . . . . 22
Thermo Scientific Flash 4000 Elemental Analyzer - Operating Manual iii

Contents
Control Section . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .22

Pneumatic Compartment. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .22
Electronic Compartments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .22
Automation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .22
Instrument Data System. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .23
Chapter 3 Instrument Description. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25

Front View. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .25
Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .26
Top View . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .27
Furnaces Compartment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .28
Fittings for Gas Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .28
Right Front Compartment. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .30
Regenerative Filters Compartment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .31
Filters Cooling Fans . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .31
Right Side Compartments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .32
Low Temperature Analytical Section . . . . . . . . . . . . . . . . . . . . . . . . . .32
Low Voltage Electrical Section . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .33
Description of the Detection System . . . . . . . . . . . . . . . . . . . . . . . . . . . .34
Water Condensate Drainage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .35
Electrical Compartment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .35
Low Voltage Section . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .36
Main Voltage Section . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .37
Connections Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .39
Status Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .41
Autosamplers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .41
MAS 4000 Autosampler for Solid Samples. . . . . . . . . . . . . . . . . . . . . .42
AI 3000/AS 3000 II Autosampler for Liquid Samples . . . . . . . . . . . . .42
Chapter 4 Pneumatic Circuit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45

Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .45
Pressure Regulators and Gauges . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .47
EFC-t Module . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .48
Water Condensate Drainage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .50
Solenoid Valves Manifold . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .51
Part 2 Preparation
Chapter 5 Analyzer Installation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55

Preliminary Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .55
Who Performs the Installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .55
Standard Outfit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .55
Electrical Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .55
Laboratory Temperature . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .56
Lift and Place the Flash 4000 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .56
Pneumatic Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .56
Electrical Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .56
MAS 4000 Autosampler. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .56
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Contents
Sample Tray. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .57

Sampling Phases. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .60
LAN Set-up . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .63
Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .63
LAN Area. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .63
Set-up . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .64
Chapter 6 Reactor Preparation and Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73

Introduction to the Preparation of Reactors . . . . . . . . . . . . . . . . . . . . . . .73
Preparing Reactors and Crucible . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .75
Reactors Installation and Replacement/Remotion . . . . . . . . . . . . . . . . . .80
Installation of the Reactors into the Furnaces . . . . . . . . . . . . . . . . . . . .80
Remotion of the Reactors from the Furnaces . . . . . . . . . . . . . . . . . . . .85
Chapter 7 Sample Preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89

Sample Weighing Technique . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .89
Solid Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .89
Liquid Samples. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .89
Weighing Technique for Solid Samples . . . . . . . . . . . . . . . . . . . . . . . . . .90
Chapter 8 Analytical Methods. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 95

Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .95
Analytical Method for N/Protein Configuration . . . . . . . . . . . . . . . . . . .95
Method Description. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .95
Diagram . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .96
Sequence of the Method Stages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .97
Part 3 Analysis
Chapter 9 Instrument Set-up . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 101

Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .101
Powering on the System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .102
Installation of Eager Xperience. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .102
Eager Xperience Main Menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .103
Analytical Configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .106
Edit Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .108
Method Title . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .108
Detection Parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .108
Integration Parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .109
Calculation Parameters. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .110
Report Parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .111
Report Stripchart . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .112
Operator ID/Info . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .112
The Elemental Analyzer Parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . .113
Analyzer Status. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .114
Detector Signal Level . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .116
Leak Test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .116
Thermo Scientific Flash 4000 Elemental Analyzer - Operating Manual v

Contents
Chapter 10 Instrument Start-up . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 119

Start-up . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .119
Chapter 11 Guide to Run Analyses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 123

Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .123
Directory for Analyses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .124
Current Maintenance Program. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .124
Instrument Calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .126
Sample Table . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .128
Sequence of Analyses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .134
Quality Control and Check of Analytical Results . . . . . . . . . . . . . . . . . .138
Post-Analysis Operations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .142
Putting the Instrument in Standby Mode. . . . . . . . . . . . . . . . . . . . . .142
Shutting Off Furnaces, Detector and Cutting Off Gas Flows . . . . . . .143
Wake-up and Auto-Start Functions . . . . . . . . . . . . . . . . . . . . . . . . . .144
Auto-Start Function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .145
Analytical Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .146
Part 4 Maintenance and Troubleshooting
Chapter 12 Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 149

Instrument Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .149
Current Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .150
Reactors Replacement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .150
Replacement of the Filling Materials . . . . . . . . . . . . . . . . . . . . . . . . .150
Replacement of the O-ring of the Reactors Coupling Unions. . . . . . .151
Replacement of the Gas Chromatographic Column . . . . . . . . . . . . . . . .153
Servicing the MAS 4000 Autosampler . . . . . . . . . . . . . . . . . . . . . . . . . .155
Current Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .155
Chapter 13 Troubleshooting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 157

Safety Cut Off . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .157
EFC-t Module . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .159
Appendix A Customer Communication . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 161

How to Contact Us . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .161
Reader Survey . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .162
Abbreviations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 163
Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 165
vi Flash 4000 Elemental Analyzer - Operating Manual Thermo Scientific

Declaration
Manufacturer: Thermo Fisher Scientific
Thermo Fisher Scientific is the manufacturer of the instrument described in this manual
and, as such, is responsible for the instrument safety, reliability and performance only if:
• installation
• re-calibration
• changes and repairs
have been carried out by authorized personnel and if:

• the local installation complies with local law regulations
• the instrument is used according to the instructions provided and if its operation is only
entrusted to qualified trained personnel
Thermo Fisher Scientific is not liable for any damages derived from the non-compliance
with the aforementioned recommendations.
Thermo Fisher Scientific
Elemental Analysis
Voltaweg 22
2627 BC Delft
The Netherlands
Thermo Scientific Flash 4000 Elemental Analyzer - Operating Manual vii

2
viii Flash 4000 Elemental Analyzer - Operating Manual Thermo Scientific

P
Preface
This Operating Manual contains descriptions of the features and components of the Flash
4000 elemental analyzer, inside, you will find all of the information necessary for routine
operation of your elemental analyzer, including operating sequences, sample injection
techniques, diagrams and descriptions of the major components.
The Flash 4000 Elemental Analyzer
This manual is organized as follows:

• Chapter 1, “Preliminary Information,” provides information on the classification of the
equipment, its safety and configurations. Basic technical features are also described.
• Part 1, “Description,” describes the structure of the instrument and the pneumatic
circuits.
− Chapter 2, “Structure of the Instrument,” describes the structure of the instrument
and its major features.
− Chapter 3, “Instrument Description,” gives you a detailed description of the
instrument components.
− Chapter 4, “Pneumatic Circuit,” describes the pneumatic circuit of the instrument in
the pre-run condition.
Thermo Scientific Flash 4000 Elemental Analyzer - Operating Manual ix

Preface
• Part 2, “Preparation,” provides description of the reactors and adsorption filters. Moreover,
it contains instructions to install and remove the system reactors, to perform sample
preparation and weighing, and also how to start up the instrument before running
analyses.
− Chapter 5, “Analyzer Installation,” provides instructions to install your Flash 4000
elemental analyzer.
− Chapter 6, “Reactor Preparation and Connections,” provides instructions for the
preparation and the installation of the reactors into the elemental analyzer and how to
remove them.
− Chapter 7, “Sample Preparation,” describes the technique for the sample preparation,
also it provides basic instructions to weigh the sample.
− Chapter 8, “Analytical Methods,” describes the analytical methods used for all
configurations of the Flash 4000 elemental analyzer.
• Part 3, “Analysis,” contains information and operating sequences to perform the analysis
preparation, execution and interpretation.
− Chapter 9, “Instrument Set-up,” contains information and operating procedures to set
the instrument for running analyses.
− Chapter 10, “Instrument Start-up,” sequences to prepare the instrument for running
analyses.
− Chapter 11, “Guide to Run Analyses,” contains information and operating sequences
to run sample analyses, and it also describes the comparison methods for a correct
evaluation of results. Practical advise for daily operation is also provided.
• Part 4, “Maintenance and Troubleshooting,” contains information and operating sequences
to perform the necessary maintenance of the instrument and also information concerning
troubleshooting in case of malfunctioning.
− Chapter 12, “Maintenance,” provides information on the current and periodic
maintenance of the instrument, and it also contains the operating sequences for the
maintenance of the MAS 4000 autosampler.
− Chapter 13, “Troubleshooting,” provides the information necessary to give you some
hints on instrument problems and how to solve them.
Appendix A, “Customer Communication.” contains information for direct contact with

Thermo Fisher Scientific offices worldwide. This appendix also contains a one-page Reader
Survey.
The Abbreviations contains definitions of terms used in this guide. It also includes
abbreviations, acronyms, metric prefixes, and symbols.
The Index contains an alphabetical list of key terms and topics in this guide, including cross
references and the corresponding page numbers.
x Flash 4000 Elemental Analyzer - Operating Manual Thermo Scientific

Preface
Compliance
We thoroughly test and evaluate our products to ensure full regulatory compliance with
applicable domestic and international regulations. Your system (hardware and software) is CE
Compliant and meets Electromagnetic Compatibility (EMC) and safety standards.
CAUTION Instrument Damage. Flash 4000 systems operate safely and reliably under
carefully controlled environmental conditions. If the equipment is used in a manner not
specified by the manufacturer, the protections provided by the equipment may be impaired.
If you maintain a system outside the specifications listed in this guide, failures of many
types may occur. The repair of such failures may be excluded from the documents regarding
your standard warranty and service contract coverage.
Safety Alerts and Special Notices

In this paragraph, safety alerts and other special notices appear in boxes.
Safety alerts are a combination of safety symbols and signal words designed to alert you to protect
yourself and/or your instrument. Please read about the types of safety alerts, signal words, and
the safety symbols that are presented in this guide and presented on the instrument.
Safety Symbols
Safety and special notices that may be found on your instrument and in this manual include
the following:
The General Warning symbol/sign is a triangle with an exclamation mark that is

used next to the signal word. In the vocabulary of ANSI Z535 signage this
symbol indicates a possible personal injury hazard exists. The ISO 3864-2
standard refers to this as the general warning sign. This symbol alerts you to an
action or sequence that, if improperly performed could results in damage to the
instrument or possible personal injury. This symbol is followed by signal words
such as Danger, Warning, or Caution indicating the risk.
This symbol indicates that an electrical shock hazard will, could, or may occur.
This symbol indicates a hot surface. Make sure the instrument is at room
temperature before touching, or else you will, could, or may incur burn injuries.
This symbol indicates a risk of fire or flammability, or that fire/flammability

damage will, could, or may occur.
This symbol indicates that a biohazard will, could, or may occur.
This symbol indicates that chemical damage or physical injury will, could, or
may occur.
This symbol indicates the presence of radioactive material.
Thermo Scientific Flash 4000 Elemental Analyzer - Operating Manual xi

Preface
This symbol indicates that eye damage will, could, or may occur. Eye protection
must be worn.
This symbol indicates the user must wear gloves when performing the
sequence.
Types of Alerts and Signal Words

Safety alerts that may or may not be associated with the use of this instrument. These
instructions are defined as follows:
DANGER safety alerts an imminent hazard exists that WILL result in death or serious
personal injury.
WARNING safety alerts you to an action or sequence that, if improperly performed, could
result in damage to the instrument or possible physical harm to the user. This symbol may
be followed by icons indicating special precautions that should be taken to avoid injury.
CAUTION safety alerts you to an action or sequence that, if performed improperly, could
damage the instrument.
Note alerts you to important information related to the test.
Special Notices
Tip Helpful information that can make a task easier.
Instrument Markings and Symbols

The following table explains the symbols used on Thermo Fisher Scientific instruments. Only a
few of them are used on the Flash 4000. See the asterisk.
Symbol Description
Direct Current
*
Alternating Current
Both direct and alternating current
3 Three-phase alternating current
xii Flash 4000 Elemental Analyzer - Operating Manual Thermo Scientific

Preface
Symbol Description
Earth (ground) terminal
Protective conductor terminal
Frame or chassis terminal
Equipotentiality
*
On (Supply)
*
Off (Supply)
Equipment protected throughout by DOUBLE INSULATION or

REINFORCED INSULATION (Equivalent to Class II of IEC 536)
* Instruction manual symbol affixed to product. Indicates that the user must
refer to the manual for specific Warning or Caution information to avoid
personal injury or damage to the product.
Caution, risk of electric shock
*
Caution, hot surface
*
Caution, biohazard
In-position of a bistable push control
Out-position of a bistable push control
* + -
Jack socket
* Symbol in compliance to the Directive 2002/96/EC on Waste Electrical and

Electronic Equipment (WEEE) placed on the european market after
August, 13, 2005.
Thermo Scientific Flash 4000 Elemental Analyzer - Operating Manual xiii

Preface
Using the Flash 4000 Document Set

The Flash 4000 Document Set (CD-Rom PN 317 095 10) includes all manuals in electronic
format, and serves as your library for information about the hardware and software of your
elemental analyzer.
The Flash 4000 Document Set (PN 317 110 50) as paper copy is also available. Furthermore,
Thermo Fisher Scientific part numbers (PN) for the paper copy manuals are provided for each
book title.
• Site Preparation and Installation Requirements (PN 317 110 51)
This manual describes how to set up a workspace for the instrument and accessories and
how to connect the main unit to the gas supplies and peripheral devices.
• Operating Manual (PN 317 110 52)
This manual provides the descriptions of the hardware and software and detailed
instructions for their use.
• Consumables and Spare Parts Catalog (PN 317 082 50)
This catalog contains a list of consumables and spare parts for the Flash 4000 elemental
analyzer.
Other available manuals are:

• Eager Xperience Software Operating Manual (PN 317 110 55)
This manual contains instruction to operate with Eager Xperience to the fully control of
the Flash elemental analyzers.
• AI 3000/AS 3000 II Autosampler for Flash Operating Manual (PN 317 094 45)
This manual contains description of the features and components of the AI 3000/AS 3000
II Autosampler for Flash elemental analyzers.
xiv Flash 4000 Elemental Analyzer - Operating Manual Thermo Scientific

1
Preliminary Information
This chapter provides information on the classification of the equipment, its safety and
configurations. Basic technical features are also described.
Contents
• Classification of the Instrument
• Technical Features
• Safety Information
• Safety Cut Off Device
• Instrument Cleaning
• Instrument Configuration
• Standard Outfit
Classification of the Instrument

Environmental Conditions
• Internal use.
• Altitude up to 2000 meters.
• Temperature from 15 to 35 °C.
• Maximum relative humidity between 5% and 95%.
• Voltage variations not exceeding ± 10 % of the nominal value.
• Transients according to installation categories II.
• Degree of pollution according to IEC 664 (3.7.3) 2.
Thermo Scientific Flash 4000 Elemental Analyzer - Operating Manual 15

1 Preliminary Information
Technical Features
Technical Features
The following table summarizes the major technical features of the Flash 4000 elemental
analyzer.
Table 1. Technical features of the instrument
Features Description
Instrument configurations One
Detector Thermal conductivity detector (TCD)
External interface RS 232 serial line, Local Area Network (LAN)
Instrument control Eager Xperience for Windows™
Power supply 230 Vac; 50/60 Hz; 2300 VA
Dimensions (cm) Height 47 (60 with fittings); Width 67, Depth 62
Mass (kg) 80
Safety Information
WARNING The instrument must be used according to the specifications of this guide.
Improper use can adversely affect the instrument protection. If the equipment is connected
to optional instruments, such as computer, balance, etc., the degree of insulation of
peripheral devices should be equivalent or higher (double or reinforced) than that of the
Flash 4000. The analyzer operation requires the use of chemical substances having different
hazard specifications. Before using chemicals, please read the hazard indications and
information reported in the Safety Sheet supplied by the manufacturer referring to the
relevant CAS (Chemical Abstract Service) number.
Use of Gases
The following gases are used with the instrument:
• Helium (He) as carrier, reference and purge gas.
• Oxygen (O2) as gas for sample oxidation.
WARNING Before using gases, carefully read the hazard indications and information
reported in the Safety Sheet supplied by the manufacturer referring to the CAS (Chemical
Abstract Service) number. It is the user’s responsibility to see that all local safety regulations
for the use of gases are obeyed.
IMPORTANT In absence of Helium the Flash 4000 goes in Safety Cut Off. See “Safety Cut
Off Device” on page 17.
Purity of Gases
The Flash 4000 uses Helium and Oxygen with 99.995% minimum purity.
16 Flash 4000 Elemental Analyzer - Operating Manual Thermo Scientific

Safety Cut Off Device
Nominal Pressure of Gases

The nominal pressure of the gases to supply the Flash 4000, as indicated on the instrument rear
panel, are:
• Maximum 600 kPa (6 bar) for He
• Maximum 600 kPa (6 bar) for O2
Safety Cut Off Device

When an alarm condition is detected, this device cuts off the power to the heating resistors of
the oxidation, reduction furnaces and to the traps.
For more details please refer to Chapter 13, “Troubleshooting,”
Instrument Cleaning
Y Instruments Cleaning
WARNING Cleaning must be performed with the instrument off, the furnaces at room
temperature and the power cord disconnected.
1. Externally clean the instrument with a soap and water solution, or with a household
non-abrasive product, carefully avoid seeping of the products used inside the instrument.
2. If you just suspect that a substance used for cleaning or a product submitted to analysis has
infiltrated inside the instrument, immediately shut down the instrument and call an
authorized customer support engineer for proper actions.The service engineer must be
fully informed on the nature of the concerned substance.
WARNING It is your responsibility to avoid that dangerous liquids and/or materials

seeping inside the elemental analyzer during operation and maintenance.
Instrument Configuration
The Flash 4000 elemental analyzer is available in the following version:
Table 2. Instrument configuration
Configuration Description
N/Protein Analyzer For the determination of the Nitrogen and protein amount
in food and animal feed products. It can also be used in
determining Nitrogen content in samples of different nature,
such as agricultural products, marine science, geological,
human/animal samples, material characterization.

Standard Outfit
Standard Outfit
Flash 4000 elemental analyzer is provided with its own standard outfit.
Use the standard outfit checklist accompanying the instrument to verify that all items have
been received.

Part 1
Description
2
Structure of the Instrument

This chapter describes the structure of the instrument and its major features.
Contents
• The Units Constituting the Instrument
• Analytical Section
• Control Section
• Automation
The Units Constituting the Instrument

The instrument consists in a single structure subdivided into two sections:
• Analytical Section
• Control Section
Analytical Section
It comprises the following major components:
Autosampler
It performs the automatic injection of the samples into the combustion reactor.
Reactors
These are tubes made of special alloy filled with different materials. Refer to Chapter 6,
“Reactor Preparation and Connections,” on page 73.
Furnaces
The Flash 4000 analyzer is equipped with two furnaces: LEFT and RIGHT. Each furnace
consists of a quartz candle surrounded by an electrical resistor. The candle is plunged in a
refractory material housed in a metal compartment.
• Furnace Temperature
The temperature is monitored by a thermocouple appropriately located in the furnace.

2 Structure of the Instrument
Control Section
• Furnace Cooling
The cooling time varies according to the operating temperature setting.
Water Condensate Drainage

It is used to condense and separate water in the combustion gases stream.
Regenerative Carbon Dioxide Filters

There are two regenerative filters used to eliminate the Carbon Dioxide in the combustion
gases.
Chromatographic Column
It performs the chromatographic separation of the reaction products generated during the
combustion process.
Thermal Conductivity Detector (TCD)

It is located in a thermostatic chamber at controlled programmable temperature.
Control Section
The control section consists of two major compartments:
Pneumatic Compartment
It consists of two pressure regulators, three pressure gauges and several lines fitted with an
thermoregulator electronic flow controller (EFCt), which ensures the switching between
helium and oxygen, and controls the flow values.
For more details, please refer to Chapter 4, “Pneumatic Circuit,” on page 45.
Electronic Compartments
They comprise the electronic boards for the instrument power supply and control.
Automation
The instrument is fully controlled by the computer through a dedicated software which is also
used for data acquisition, data handling and interpretation of the acquired results. Therefore
the instrument is not provided with independent keyboard and display. On the instrument
front there three status LEDs where you can monitor the instrument statuses.

Automation
Instrument Data System

The instrument is only and fully controlled by Eager Xperience dedicated software, designed
to be compatible with commercially available computers and Windows™ 2000/XP/Vista
operating system.
Table 3. Hardware minimum requirements

Components Description
Computer Any PC can be used, including laptop computer
Operating System: Windows™ 2000/XP/Vista
Pentium Processor minimum 256 MHz
Hard drive with at least 1 GB free
One free COM port for instrument contr
LAN device alternatively to COM port
One free COM port for balance, if required
One free COM port for AI 3000/AS 3000 II autosampler, if required
CD driver
Monitor Color 1024 x 768 or better
Printer Any printer accepted by the operating system

Automation

3
Instrument Description
This chapter gives you a detailed description of the instrument components.
Contents
• Front View
• Rear Panel
• Top View
• Furnaces Compartment
• Fittings for Gas Connections
• Right Front Compartment
• Regenerative Filters Compartment
• Right Side Compartments
• Description of the Detection System
• Water Condensate Drainage
• Electrical Compartment
• Connections Panel
• Status Panel
• Autosamplers
Front View
The front part of the instrument, shown in Figure 1, comprises:
• Furnaces compartment
Also refer to “Furnaces Compartment” on page 28.
• Status panel
Also refer to “Status Panel” on page 41.
• Right Front compartment
It includes:
− Pressure regulators and pressure gauges
− Water condense collector

3 Instrument Description
Rear Panel
Also refer to paragraph “Right Front Compartment” on page 30.
Figure 1. Instrument front view
Rear Panel
The rear part of the instrument, shown in Figure 2, comprises:
• Panel for connections including:
− interface section
− gas inlets section
Also refer to “Connections Panel” on page 39.
• Cooling fan
• Main voltage electronic section
Also refer to “Electrical Compartment” on page 35.
• Cooling fan of regenerative filters See “Regenerative Filters Compartment” on page 31.
• Transformer compartment
Also refer to “Electrical Compartment” on page 35.
• Breaker and Mains socket

Top View
Figure 2. Rear view
Gas inlet
section
Cooling fan
Interface
section
Breaker
Mains
socket
Top View
The top part of the instrument, shown in Figure 3, comprises:
• Top cover
• MAS 4000 autosampler
• Fittings for mounting and securing the reactors into the furnaces
• Fittings for gas connections
Figure 3. Instrument top view
MAS 4000 Gas fittings
Reactors fittings Top cover

Furnaces Compartment
Furnaces Compartment
The furnaces compartment, shown in Figure 4, is accessible from the instrument front
removing the front cover.
To remove the front cover it is necessary to open the lower door unscrewing the proper fixing
screw.
CAUTION Do not open the furnaces compartment during operation because very high
temperatures are reached.
The front cover can be removed only when the furnaces temperature shown is near the
room temperature.
Figure 4. Furnace compartment
Left furnace Right furnace
The furnaces can reach the following maximum temperatures:

• LEFT Furnace: 1020 °C
• RIGHT Furnace: 1020 °C
The furnace temperature is monitored by a thermocouple located inside the furnace.
The furnaces are cooled when required by the operator.
The cooling time depends on the operating temperature.
Fittings for Gas Connections

They are located on the top part of the instrument rear panel as shown in Figure 5. Gas inlet
ports are directly connected to the pressure regulators.

Fittings for Gas Connections
Figure 5. Gas connections
Oxygen inlet port Helium inlet port
Gas inlet pressure must be set as indicated in Table 4.
Table 4. Gas Inlet Ports and Pressure Setting

Port Description Pressure value to be set
He Inlet port for Helium 2-6 bar (200-600 kPa)
O2 Inlet port for Oxygen 5-6 bar (500-600 kPa)
Gas pressures must be set and controlled through the pressure regulators and the gauges of the
instrument.
Table 5 provides indications on the most currently used units of pressure.
Table 5. Pressure units conversion

To convert into multiply by
kPa bar 0.01
psi 0.145
bar kPa 100
psi 14.51
psi kPa 6.89476
bar 0.0689476

Right Front Compartment
Right Front Compartment

This compartment, shown in Figure 6, houses the pressure regulators, the gauges and the water
collecting bottle.
Figure 6. View of the right front compartment
Pressure Gauges
Pressure Regulators
Water collecting
bottle
• Pressure gauge (0-300 kPa) marked Combustion Reactor visualizes the pressure of Helium
in the pneumatic circuit. This pressure is not adjustable.
• Pressure gauge (0-300 kPa) marked He visualized the pressure of Helium.
Set this pressure to 120-150 kPa by turning the adjusting screw of the relevant pressure
regulator.
This allows to obtain a gas flow of 300 mL/min ± 50 mL/min (250÷350 mL/min) for the
filters regeneration.
• Pressure gauge (0-500 kPa) marked O2 visualized the pressure of Oxygen.
Set this pressure to 450-460 kPa by turning the adjusting screw of the relevant pressure
regulator. This allows to obtain a gas flow suitable for the combustion.

Regenerative Filters Compartment
Regenerative Filters Compartment

This compartment, shown in Figure 7, is accessible opening the front right door. These
elements trap carbon dioxide and not condensed water from the carrier gas.
Figure 7. Regenerative filters compartments
Filters
The filters do not require any periodical maintenance.
WARNING Do not remove the filter from its housing. The filter must be removed, only
when required, by authorized technical personnel.
Filters Cooling Fans

They are located on the rear of the instrument. Refer to “Rear Panel” on page 26.
Hot air exits through these funs. For this reason, there should be at least 30 cm (12 in.) free
space behind the instrument.
WARNING Do not expose gas tanks or bottles, chemicals, regulators, electrical cords, or
other temperature-sensitive items to exhaust vents.

Right Side Compartments

They are located on the right part of the instrument, as shown in Figure 8, and they are
accessible by removing the right side cover.
Figure 8. Right side compartments
Low temperature Low voltage

analytical section electrical section
These compartments comprise two sections:

1. Low temperature analytical section
2. Low voltage electrical section
Low Temperature Analytical Section

This compartment comprises the following devices as shown in Figure 9:
• Filters valves manifold
• Detector box containing the TCD chamber
Also refer to “Description of the Detection System” on page 34
• Chromatographic column
• Water condensate drainage
Also refer to “Water Condensate Drainage” on page 35
• Filter cooling fans carter
• Check valve

Figure 9. Low temperature analytical section
Filters valve
manifold
Filter cooling fan
Check valve
Chromatographic
column
TCD Detector box
Water condensate
drainage box
Low Voltage Electrical Section

It comprises the low voltage electronic boards. Refer to “Electrical Compartment” on page 35.

Description of the Detection System
Description of the Detection System

Detection system, as shown in Figure 10, consists of a thermal conductivity detector (TCD)
sensitive to any substance with thermal conductivity other than that of the carrier gas used.
The detector essentially consists of a stainless steel block provided with two pairs of filaments
(generally of tungsten/rhenium) having the same electrical resistance. The detector is housed in
a thermally insulated metal block (detector oven) and maintained at constant temperature.
Figure 10. Detection system
TCD detector box Internal view
The two pairs of filaments are electrically connected according to a Wheatstone bridge circuit
powered at constant voltage.
The first pair of filaments is fed with pure carrier gas (reference channel), whereas the second
pair is fed with the gas flowing from the reactor (analytical channel).
When the bridge is powered, the filaments heat at a temperature (resistance) that is a function
of the thermal conductivity of the gas feeding the filaments. The reference channel is exposed
only to pure carrier gas, whereas the analytical channel is exposed to the reactor effluents
(carrier gas + sample).
When pure carrier gas flows through both the reference and the analytical channels, a constant
temperature gradient is established between the elements and the detector walls, and the
Wheatstone bridge is balanced, namely there is no output signal.
As a component is eluted, a change in heat transfer occurs, with consequent variation of the
filaments temperature. Since electrical resistance is a function of temperature, the bridge
unbalances and the detector generates a signal proportional to the difference in thermal
conductivity between the eluted component and the carrier gas. The output signal is then sent
to the data acquisition board.
Note The filaments are powered at 5V constant voltage and are electrically protected if
their temperature exceeds 220 °C (Safety Cut Off ).

3Instrument Description

This device, shown in Figure 11, consists of an insulated chamber cooled by a Peltier element
and allows to condensate and separate water from the gas stream. The control of the Peltier
element is performed by the CLR-EAX board.
Figure 11. Water condensate drainage device
CLR-EAX board
LED
Water condensate
drainage box
The correct functionality of the device is indicated by a LED.
Every analysis, the condense is drained in the collecting bottle located into the right front
compartment of the instrument.
Electrical Compartment
CAUTION Before opening the electrical compartments, cut off power supply to the
instrument and disconnect the power cord.
The electrical compartment comprises:

• Low voltage section
Refer to “Low Voltage Section” on page 36.
• Mains voltage section
Refer to “Main Voltage Section” on page 37.
• EFCt electronic flow controller for gas regulation
Refer to “EFC-t Module” on page 48.

Low Voltage Section

It is located on the right part of the instrument, as shown in Figure 12, and it is accessible by
removing the right side cover. This section includes:
• The electronic boards to operate and control the instrument. Three of these board are
interlocked through a mother board.
• The electronic flow control thermostatic (EFC-t) module contained into the own metal
box.
Figure 12. Low voltage section and EFC-t box
Low Voltage Section
EFC-t Box
Function of the Low Voltage Electronic Boards

The following table reports the function of each electronic board present in the low voltage
section:
Table 6. Description of the function of the low voltage electronic boards

Board Description
MBR-EAX The Mother board provides interlocking between low voltage boards
(HWD, CPU and TST when present) and with the rest of the
instrument.
CPU-EAX This board has full control of the instrument operations.
It controls the communication between operator and machine through
Eager Xperience. Actuates the Safety Cut Off device, which puts the
instrument in safe conditions, when an alarm condition occurs. This
board can be connected to a Li 3 V; 220 mA/h chargeable battery
located nearby.

Table 6. Description of the function of the low voltage electronic boards, continued
Board Description
CPU-EAX CAUTION The rechargeable battery replacement must be performed
(continued) by authorized Thermo Fisher Scientific field service engineers.
HWD-EAX It allows the detector oven thermoregulation and also amplifies and
converts the detector signal to send it to the PC.
TST-EAX This board provides test points for technical diagnostic.
On the motherboard is present the slot for this board which is not
included with the instrument.
CAUTION This board must be used only by authorized Thermo
Fisher Scientific field service engineers.
EXT-EAX It provides the circuits for the communication between the elemental
analyzer and the external world through RS 232 serial line or Local
Area Network (LAN)
FRT-EAX Status panel.
This board is located on the instrument front.
CLR-EAX Peltier element control.
This board is located in the low temperature analytical section.
A fuse is provided on the board. See Table 7.

EFC-t Box
EFC-EAX It provides the electronic flow control of the gases through the six
solenoid valves contained in the EFC-t box.
EFCPS It receives the mains power (230 Vac) and provides the voltages to
supply the EFC-EAX board and the controlling four of the six solenoid
valves contained in the EFC-t box.
A fuse is provided on the board. See Table 7.
Table 7. Low Voltage Section: Protecting fuses

Board Fuse Type Protection
CLR-EAX F1 T2.5A; type MST Peltier
EFCPS F1 T350mA; IEC 127/III (5 x 20 mm) EFCPS board
Main Voltage Section

It is located in the rear part of the instrument, as shown in Figure 13, and it is accessible from
the rear panel by removing the relevant cover.
This compartment contains the mains power circuits with the Safety Cut Off device and the
electrical devices to power the furnaces, the filters and control their temperature.

Figure 13. Mains voltage section
Mains Voltage Section
The breaker and the Mains

socket are not visualized
Power Supply Section

It comprises:
• Breaker marked MAINS to switch the instrument On/Off.
Position I = instrument On; Position O = instrument Off
• 230 V; 50/60 Hz mains socket.
Function of the Mains Voltage Components

The following table reports the function of each component present in the main voltage
compartment:
Table 8. Description of the function of the mains section components

Component Function
Transformer It receives the mains power (230 Vac) from the PWR-EAX board and
supplies 48 Vac to the ACS-EAX board.
PWR-EAX This board performs the following operations:
• It receives the mains voltage through the ON/OFF main switch
(breaker)
• It furnishes the mains voltage to the main transformer
• It generates voltage to supply electronic boards, cooling fans and
filter valves
Six fuses are provided on the board. See Table 9.

Connections Panel
Table 8. Description of the function of the mains section components, continued

Component Function
ACS-EAX It receives 48 Vac power from the main transformer to supply properly
the furnaces and the filters.
Specific circuits read the values of the thermocouple present in the

relevant furnace.
Solid state relays (SSR) are coupled with a proper safety sensor, which
detects any malfunction. The SSRs control the power supply to the
relevant furnace and cut off power to the heating resistor when the
thermocouple detects temperature values exceeding the setpoint.
Five fuses are provided on the board. See Table 9.
Table 9. Protecting fuses

Board Fuse Type Protection
PWR-EAX F1 F1A; IEC 127/I (5 x 20 mm) Oven HWD
F2 F1A; IEC 127/I (5 x 20 mm)
F3 T315mA; IEC 127/III (5 x 20 mm) EFC-t Module and
F4 T315mA; IEC 127/III (5 x 20 mm) ACS-EAX card
F5 T800mA; IEC 127/III (5 x 20 mm) Rear fan and furnaces

fans
F6 T800mA; IEC 127/III (5 x 20 mm)
ACS-EAX F1 T16A; IEC 60068-1 (6.3 x 32 mm) Bottom filter power
circuit
F2 20A; series CH10 type go Right Furnace power
(10.3 x 38 mm) circuit
F3 20A; series CH10 type gC Left Furnace power
(10.3 x 38 mm) circuit
F4 T16A; IEC 60068-1 (6.3 x 32 mm) Top Filter power
circuit
F7 T3.15A; IEC 127/III (5 x 20 mm) Peltier
Connections Panel
The panel, shown in Figure 14, is subdivided into four sections:
• Gas inlets
• Interface
• Communication

Connections Panel
Figure 14. View of the connections panel
Gas Inlets Section Interface Section
4 Selection Switch
LAN Section Communication

Section
Gas Supply Section

It comprises the gas inlet ports. Refer to paragraph “Fittings for Gas Connections” on page 28.
Interface Section
It comprises:
• 15-pin connector marked MAS for the MAS 4000 autosampler for solid samples.
Communication Section
It comprises:
• 9-pin connector marked RS 232 to dialog with the computer via serial line.
• LAN communication port. See LAN Section.
• Selection switch
Note By using the selection switch located between the RS 232 and LAN connectors it is
possible to choose the desired type of communication.
LAN Section
The LAN (Local Area Network) section is easily recognizable by the presence on the analyzer
rear panel of a RJ45 connector, 2 LEDs for LAN activity and a reset button.
The Flash 4000 LAN is shipped with a default IP address, which may not match the LAN
needs of the sites where the analyzer must be installed.

Status Panel
To change the default values, contact your LAN administrator and ask for the IP address to be
assigned, the netmask, and eventually the port. The IP address and communication port may
be reset to default value by pushing the reset button, accessible from the rear panel of the
analyzer, for at least 5 seconds.
CAUTION The reset button is accessible introducing a little screwdriver into the relevant
passing hole.
To set the IP address and the LAN communication port, follow the instructions reported in
paragraph “LAN Set-up” on page 63.
Status Panel
Status panel, shown in Figure 15, is the user interface of the GC. It consists of a series of three
Status LEDs showing the instrument’s status.
Figure 15. Status panel
The LEDs (Light Emitting Diodes) indicate the operating status of Flash 4000 elemental
analyzer. Each status LED indicates the current operating mode and special settings activated
by the operator. Table 10 lists and explains each status LED.
Table 10. Status LED diodes descriptions

LED Description
Power /Safety This LED lights green when the instrument is turned ON.
When safety cut-off conditions occurs, the LED becomes red.
Ready/Standby This LED lights green when the instrument is Ready.
It turns to yellow when Standby mode is activated.
Maintenance This LED lights yellow when the maintenance is required.
Autosamplers
The Flash 4000 elemental analyzer can be configured with the following autosamplers.

Autosamplers
MAS 4000 Autosampler for Solid Samples

It is mounted directly on the connecting fitting of the concerned reaction tube. It consists of:
• Anodized aluminium block (sampler body) provided on the left with fittings for carrier gas
and purge gas lines connection.
• 31-position sample-holding tray.
Up to four sample tray are available to accommodate 124 samples.
• A motor for the piston.
• A motor for the tray.
• Two Hall sensors to detect the piston positions.
• MAS-EAX board, directly controlled by CPU, provides the drivers for both the piston and
tray motors.
• A viewer on the sampler body to observe the combustion
Figure 16. MAS 4000 Autosampler
Tray
Motors MAS-EAX
board
Viewer
Sampler body
AI 3000/AS 3000 II Autosampler for Liquid Samples

It is mounted on the analyzer by means of the appropriate support. It consists of:
• Sampling unit
• 8-position (AI 3000 II) or 105-position (AS 3000 II) sample tray.
Injection volume up to 125 μL with a 250 μL syringe capacity.

Autosamplers
Figure 17. AI 3000/AS 3000 II autosampler

Autosamplers

4
Pneumatic Circuit
This chapter describes the pneumatic circuit of the configuration in the pre-run condition.
Contents
• Introduction
• Pressure Regulators and Gauges
• EFC-t Module
• Water Condensate Drainage
• Solenoid Valves Manifold
Introduction
The pneumatic circuit, schematically shown in Figure 18 and Figure 19 has the following
common components:
• Inlet gases pressure regulators and relevant gauges
• EFC-t Electronic Flow Controller for gases
• Two reactors
• Valves manifold
• Water condensate drainage (Water drain)
• Regenerative carbon dioxide filters
• One gas chromatographic column
• TCD Thermal Conductivity Detector

4 Pneumatic Circuit
Introduction
Figure 18. Pneumatic circuit block diagram
He Pressure F2
Valves
Regulators EFCt
Manifold
O2 and Gauges
F1
Vent AS
EV5
Water
Carrier Drain CC
Filters Purge R1 R2
Reference
Water Drain
CC = Chromatographic Column
F1 = Adsorption filter
F2 = Adsorption filter TCD
R1 = Oxidation Reactor
R2 = Reduction Reactor
Figure 19. Pneumatic circuit schematic diagram
EFC-t Module Front Panel - FP

S2 PI1
F
He PRV1
SVP2 T He
1
(5) 2
PI2
F PRV2
F O2
IN O
OUT SV1 2
(6) 2
6,5 ml/min @ 300 kPa - O

TCD 2 3 1 PI3
F
IN OUT (7)
Carrier Red 2
SV3 1 SV4 1 SV2 3
1
CC
Combustion furnace
2 2 2
Green Reduction furnace
CV S1 1
Vent
4
(4) 1
2
SVP1
(1) (2)
R1 R2
Reference
Autosampler AS
Solenoid valves block - SVB

(7) (2)
F F
600 sccm @ 30 psi - AIR Water Drain WD
1
SV8 3 1 3 SV9 SV5
1
2
2 Vent
2
Bottom - BF White (6) F F (4) Top - TF
White
B
Blue (5) F F (3) Blue
2 2
3 1 1 3
SV7 SV6
(8) (1)
The components of the pneumatic circuit is listed inTable 11.

4 Pneumatic Circuit
Pressure Regulators and Gauges
Table 11. Components of the pneumatic circuit

Component Description
PRV1-PRV2 Pressure regulators and gauges. See “Pressure Regulators and
PI1-PI2-PI3 Gauges” on page 47.
SV1-SV2-SV3-SV4 They are the solenoid valves (SV), the electronic flow controllers
SVP1-SVP2-S1-S2 (SVP) and the electronic flow sensors (S) of the EFC-t module.
See “EFC-t Module” on page 48.
AS Autosampler
R1 Oxidation reactor
R2 Reduction reactor
WD-SV5-B Water condensate drainage device. Refer to “Water Condensate
Drainage” on page 50.
SV6-SV7-SV8-SV9 Solenoid valves for the control of the two generative filters.
Bottom-BF Bottom regenerative CO2 filter
Top-TF Top regenerative CO2 filter
CC Gas chromatographic column
TCD TCD thermal conductivity detector
CV Check valve
Pressure Regulators and Gauges

Pressure regulators, located in the detector compartment and schematically shown in Figure 20,
allow to visualized and regulate the pressure of the Helium and Oxygen lines.
Figure 20. Pressure regulator
Front Panel - FP
PI1
PRV1
He
To EFC-t Module Gas Supply

PI2
PRV2
O
2
PI3
Carrier
To Autosampler
Carrier
From EFC-t Module
Reference
Pressure regulators consist of the components listed in theTable 12.

4 Pneumatic Circuit
EFC-t Module
Table 12. Parts of pressure regulators and gauges

Components Description and Functions
He Inlet port for Helium
O2 Inlet port for Oxygen
PRV1 Helium pressure regulator
PI1 Helium pressure gauge
PRV2 Oxygen pressure regulator
PI2 Oxygen pressure gauge
PI3 Carrier pressure gauge
EFC-t Module
The electronic flow control thermostatic (EFC-t) module, schematically shown in Figure 21,
contains some solenoid valves that are placed in the manifold maintained at the constant
temperature of 42 °C. Every variation of temperature does not influence the flows of the gas.
See Table 13.
Figure 21. Thermo-regulated EFC-t module schematic diagram
EFC-t Module
S2
F
SVP2 1 He
(5) From
2
To TCD Pressure Regulators
F
F O
(6) 2
SV1
2
6,5 ml/min @ 300 kPa - O

From TCD 2
3 1
(7) F
SV3 SV4 1 SV2 1

1 3
2 2 2
S1
To TCD
(4) 1
2
Reference SVP1 To Autosampler
(1)
(2)
To Autosampler
Table 13. Parts of the EFC-t module

Component Description and Function
He Inlet port for Helium.
O2 Inlet port for Oxygen.
SV1 Three-way solenoid valve.
• To control Oxygen inlet.

4 Pneumatic Circuit
EFC-t Module
Table 13. Parts of the EFC-t module, continued

SV2 Three-way solenoid valve.
• To control Helium inlet.
• To allow switching between Helium and Oxygen.
SV3 Two-way solenoid valve normally open.
• To control the inlet of Helium flowing back from the TCD detector
analytical channel.
The gas is exhausted to the outside through the Vent port.

The valve is closed during the leak test.
SV4 Two-way solenoid valve normally open.
• To control the inlet of Helium flowing back from the TCD detector
reference channel.
The gas is used to eliminate air from the MAS 4000 autosampler.
The valve is closed during the leak test.
S1 Electronic flow sensor for Helium as carrier gas and Oxygen during the
sampling stage. It cooperates with the SVP1 electronic controller
(proportional valve).
S2 Electronic flow sensor for Helium as reference gas.
It cooperates with the SVP2 electronic controller (proportional valve).

SVP1 Electronic flow controller for Helium as carrier gas and Oxygen.
• To control the flowrates of gases according to the flow values set.
SVP2 Electronic flow controller for Helium as reference gas.
• To control the flowrate according to the required flow value.

4 Pneumatic Circuit

The water condensate drainage, schematically shown in Figure 22, consists of the following
components. See Table 14.
Figure 22. Water condensate drainage schematic diagram
Carrier
From Reactor R2
Water Drain WD
1
SV5
2
Vent
Carrier Helium
To Solenoid from regenerative
Valves Block CO2filter
Table 14. Parts of the water drain

WD Water condensate drainage device
SV5 Two-way solenoid valve to eliminate the condense into the collector.
B Water collector

4 Pneumatic Circuit
Solenoid Valves Manifold

The solenoid valves manifold, schematically shown in Figure 23, consists of the following
components. See Table 15.
Figure 23. Solenoid valves manifold schematic diagram
He To Chromatography
Column
(7) (2)
F F
600 ml/min @ 30 psi - AIR
SV8 3 1 1 3 SV9
2 2
Bottom - BF (6) F F (4) Top - TF
(5) F F (3)
2 2
3 1 1 3
SV7 SV6
(8) (1)
To Water From Water

Collector Condensate Drainage
Table 15. Parts of the solenoid valves manifold

Component Description and Functions
SV6-SV9 Three-way solenoid valves to control the carrier and He gas from/to
the TOP regenerative CO2 filter
SV7-SV8 Three-way solenoid valves to control the carrier and He gas from/to
the BOTTOM regenerative CO2 filter
Top TF TOP regenerative CO2 filter
Bottom BF BOTTOM regenerative CO2 filter

4 Pneumatic Circuit

Part 2
Preparation
5
Analyzer Installation
This chapter provides instruction to install your Flash 4000 elemental analyzer.
Contents
• Preliminary Information
• MAS 4000 Autosampler
• Sample Tray
• LAN Set-up
Preliminary Information
This chapter contains the preliminary information for the installation and connection of the
Flash 4000 elemental analyzer and for the electrical requirements.
Who Performs the Installation

Flash 4000 elemental analyzer should be installed by authorized Thermo Fisher Scientific
field service engineers, who will check its correct operation. For more details, please contact
your Thermo Fisher Scientific local representatives. Should the instrument not be installed
by Thermo Fisher Scientific personnel, please strictly adhere to the following instructions.
Standard Outfit
Use the standard outfit checklist accompanying the instrument to verify that all items have
been received.
Electrical Requirements
The instrument must be electrically supplied as indicated in “Technical Features” on
page 16.

5 Analyzer Installation
MAS 4000 Autosampler
CAUTION The power line and the connections among the instruments must maintain
good electrical grounding. Poor grounding represents a danger for the operator and may
seriously affect the instrument performance.
Do not connect the Flash 4000 elemental analyzer to lines feeding devices of a heavy duty
nature, such as motors, UV lamps, refrigerators and other devices that can generate
disturbances.
If other instruments, such as computer, balance, printer, etc., have to be connected to the
same electrical line as the Flash 4000, ensure that such electrical line is capable of
withstanding such electrical consumptions by calculating the total absorption.
Laboratory Temperature
The instrument is generally best located in an environment where atmospheric conditions can
be controlled and extreme temperatures avoided.
The precision of the instrument can be regarded as a function of the precision of the
laboratory temperature control. Therefore do not place the instrument near heating or air
conditioning vents which may cause differential heating and drafts.
In laboratories with windows, venetian blinds should be installed to protect the instrument
from direct sunlight.
Lift and Place the Flash 4000

To move the elemental analyzer from the floor to the working place will require at least two
people. They will position themselves at the sides of the instrument, putting their hands
underneath it.
Pneumatic Connections
Verify that the pneumatic connections have been properly carried out as described in Chapter
3 of the Site Preparation and Installation Requirements manual.
Electrical Connections
Verify that the electrical connections have been properly carried out as described in Chapter 3
of the Site Preparation and Installation Requirements manual.
If LAN connection has been carried out, perform the set-up following the instruction
reported in paragraph “LAN Set-up” on page 63.
MAS 4000 Autosampler

MAS 4000 autosampler for solid samples, provided with the analyzer, consists of an anodized
aluminium block having on its right side the inlets for carrier and purge gas lines. Its modular
structure allows to run up to 124 unattended analyses.

Sample Tray
The base unit is provided with one 31-position sample tray. Up to three optional 31-position
sample trays can be added to reach a capacity of 124 samples.
Each sample tray is installed in a specific position defined by the numbering, and therefore
they are not interchangeable.
Figure 24. MAS 4000 autosampler
4 Sample tray
5 lens
Optical
Sampler3 body 1 Purge/reference gas inlet
2 Carrier gas inlet
6 Sampler fixing nut
Reactor fittings
Y To install MAS 4000 autosampler
WARNING Before starting, make sure that the analyzer is powered OFF.
1. The autosampler must be directly installed on the connecting nut of the combustion
reactor.
2. Place the autosampler on the top cover of the analyzer in correspondence of the
combustion reactor.
3. Manually screw the autosampler nut on the combustion channel.
4. Fix the autosampler.
5. Connect the tubes coming from the gases connections 1 and 2 located on the analyzer, to
the relevant connections 1 and 2 of the autosampler.
6. Connect the signal cable of the MAS 4000 autosampler to the 15-pin connector, marked
MAS, on the real panel of the analyzer.
WARNING To avoid damaging the MAS 4000 autosampler, NEVER connect/disconnect
the signal cable when the analyzer is powered ON.
Sample Tray
The sample tray, shown in Figure 25, can contain up to 31 samples. Up to four sample trays,
numbered 1to 4, can be added. The sample numbering is detailed in Table 16. Each sample
tray is provided with a locating mark to be aligned to the seat marked 0 (zero).

Sample Tray
Any sample has to place in the locating mark position. The correct alignment of the
locating mark is important for the installation of the sample tray on the MAS 4000
autosampler.
Under the tray, in correspondence of the locating mark, there are present:
• the sampling hole through which the sample will pass during the sampling sequence.
• the guide pin
Figure 25. Sample tray top and bottom view
A B
2
3
1
2
1
A. Sample tray top view B. Sample tray bottom view

1. Locating mark 1. Locating mark
2. Seat marked 0 (zero) 2. Sampling hole
3. Guide pin
Table 16. Sample tray numbering

Sample Tray Locating Mark Numbering
#1 Seat marked 0 (zero) from 1 to 31
#2 Seat marked 0 from 32 to 62
Y To install the sample tray
1. Before starting, verify that the guide slot, located on the tray holder hub, is perfectly
aligned with the sampler body. If not, click on the red switch, located on the left hand side
of the sampler body. The tray holder hub turns until the guide slot reaches the correct
position.
Figure 26 shows the wrong and the correct position of the guide slot on the tray holder
hub.

Sample Tray
Figure 26. Tray holder hub
WRONG CORRECT 1
A
1
3
2 2
1
2
4
5
1. Tray holder hub 2. Guide slot
3. Sampler body 4. Red switch
5. Collar
2. Take the sample tray and manually move the locating mark until it is aligned to the seat
marked 0 (zero).
3. Place the sample tray on the tray holder hub paying attention to properly insert the guide
pin, located under the tray in correspondence of the locating mark, into the guide slot.
Verify that also the sampling hole is perfectly positioned on the white collar on the
sampler body. If not, adjust manually.
4. Place the samples to be analyzed, previously prepared, in the sample tray seats starting
from the seat #1. Up to 31 samples can be allocate.
5. If additional sample trays are required, install them in the correct order one over the other,
paying attention that the relevant locating marks are in correspondence with the relevant
seats marked 0 (zero), and accommodating the samples properly. See Table 16.
IMPORTANT Before installing an additional sample tray, make sure that the samples to be
analyze have been placed in all the seats of the previous tray installed.
6. Place the protection cover over the sample tray.
Figure 27 shows the result of the trays installation with the relevant locating mark aligned to
the respective seat marked 0 (zero).
Figure 27. Four trays alignment
Sample tray #4
Sample tray #3
Locating mark Sample tray #2
Sample tray #1

Sample Tray
Sampling Phases
Sampling cycle happens in three phases as schematically shown in Figure 28 on page 61.
• Loading
The sample that is going to be analyzed drops in the sampler body.
• Purging
The sample is purged by a flow of purge Helium (reference gas).
• Sampling
The sample drops into the combustion reactor.
Sampling Cycle Description

1. When the start signal is send from the Flash 4000 to MAS 4000, the tray moves the seat
containing the sample #1 on the sampling hole. The sample drops into the sample
chamber provided in the piston inside the sampler body.
2. The piston moves until the sample chamber reaches the purging position where a flow of
Helium washes the sample for a prefixed time.
3. After the purge time, the piston moves until the sample chamber is aligned with the
reactor. The sample drops into the reactor where the flash combustion happens after few
seconds.
Tip The flash combustion can be observed looking through the viewer on the sampler
body.
Before sampling Flash combustion
4. When a new start signal is send, the sampling cycle is repeated for the sample #2 and so
on for all the samples put in the sample tray.
5. If additional trays are present, after the sampling of the sample #31, at the next start
command, the locating mark (seat 0) of the first tray hooks the locating mark (seat 0) of
the second tray.
This allows the correct sampling of the samples put into the seats provided in the second
tray.
The same mechanism is repeated also for the third and the fourth tray if installed. See
Figure 29 on page 62.

Sample Tray
Figure 28. Sampling cycle
2
LOADING
3
4
8
1 5
6
7
PURGING
OUT
Purge
He IN
SAMPLING
1. Sample body 2. Trays

3. Sample seat 4. Sample
5. Sample chamber 6. Piston
7. Reactor 8. Viewer

Sample Tray
Figure 29. Sampling mechanism

LAN Set-up
LAN Set-up
This paragraph contains a few notes on how to set-up and start using the LAN port of the
Flash 4000 elemental analyzer.
Introduction
The Flash 4000 featuring LAN (Local Area Network) capabilities is easily recognizable by the
presence on the rear panel of a RJ45 connector, 2 LEDs for LAN activity, a reset button and a
switch to select the communication via RS232 or LAN.
Figure 30. Lan device
5
3
6
4 1
1. RJ45 connector 2. LED marked 100 Mdps

3. LED marked 10 Mdps 4. Reset button
5. RS 232 port 6. Selecting switch
LAN Area
IP Address and LAN Communication Port

The Flash 4000 is shipped with a default IP address, that may not match the needs of the
LAN of the site where the analyzer must be installed.
To change the default values, contact your LAN administrator and ask for the IP address to be
assigned, the netmask, and eventually the port.
• The IP address is a 3 digits x 4 fields number given by the network administrator e.g.
192.168.127.10
• The netmask is a 3 digits x 4 fields number given by the network administrator e.g.
255.255.255.0
• The port is a 4 digits number given by the network administrator e.g. 4001 (4001 is
usually the CPU/LAN default)
The default IP address of the Flash 4000 is 192.168.127.254.
Reset Button
To reset the IP address and communication port to default value, push the reset button,
located on the rear panel of the Flash 4000 for at least 5 seconds.

LAN Set-up
Network Cables
Two network cables are included in the standard outfit of the Flash 4000:
• a reversed RED patch for computer to Flash 4000 direct connection. This is used for the
initial set-up operation and in the case you do not want connecting the instrument in
remote mode.
• a standard GREY patch for Flash 4000 to local area network connection.
The principle of connection between Flash 4000 and PC is schematically shown in the
following figure.
Set-up
To set the desired IP and set up the LAN communication port of the Flash 4000 then to
configure the data system, please follow the instruction reported in To Set- up the Flash 4000
operating sequence.
Y To Set- up the Flash 4000
Material Required
PC (desktop or portable)
Network connecting RED cable
Network connecting GREY cable
To properly set the desired IP address and set up the LAN communication port of the Flash
4000, perform the following steps:
1. Verify that the instrument and the PC are switched off.
2. By using the LAN reversed RED patch included in the standard outfit, connect a PC
(desktop or portable) directly to the RJ45 connector marked LAN located on the rear
panel of the Flash 4000.

LAN Set-up
3. Switch on the instrument as well as the PC.

4. Make sure your PC communicates with the CPU/LAN IP. To do this, from the Start
menu, run the “Command Prompt” and type “Ping 192.168.127.254”. The Flash 4000
should answer as reported in the following figure.
• If the default IP address 192.168.127.254 is reachable, please jump to “To operate

when the IP address is reachable” on page 66.
• If your PC is not able to communicate with the default IP address, it is necessary to
set your computer to a different IP address, following the instruction reported in the
operating sequence To operate when IP address is not reachable.
Y To operate when IP address is not reachable
1. Select the Local Area Network connection properties of your computer (please refer to
specific operating system instructions to access this configuration).
2. Select the Internet Protocol TCP/IP and then click on Properties.

3. Make sure the IP address of the computer you are using is set for same default network of
the Flash 4000.

LAN Set-up
4. Select an IP in the range 192.168.127.1 to 192.168.127. 253 and set the subnet as shown
in the next figure.
5. At this point confirm by clicking OK, and restart from point 3 to make sure the Flash
4000 default IP is now reachable.
Note Should you still have problems, please check the cable connection, and go through
the reset procedure of the Flash 4000. The CPU/LAN is hence reset to the default IP
address. Refer to “Reset Button” on page 63.
6. Proceed following the instructions reported in the operating sequence To operate when
the IP address is reachable.
Y To operate when the IP address is reachable
When the IP is reachable it means that the PC is communicating with the Flash 4000 LAN. It
is now possible to set the LAN communication port.
1. Start a command prompt and type telnet 192.168.127.254
2. The telnet program connects to the IP 192.168.127.254 and shows the following page:
3. Confirm the default selection (1) by pressing Enter. The following page will be visualized.

LAN Set-up
With arrows, Enter and Esc keys you’ll navigate the program.
4. Select server Config to enter the new IP address and netmask.
With arrows and Enter keys you’ll point to the different parameters to be set.
In this page you’ll need to enter the new assigned IP needed for the LAN environment
where the Flash 4000 is installed. Also the netmask is entered in the same menu section.
In this example the IP set is 192.168.0.101.
Press ESC when done with the settings of this menu, to return to upper level menu.
Press the right arrow key to select OP_mode, and then press ENTER.
5. By moving the selection with the up/down arrow keys, make sure that Raw connection
(TCP Server) is selected and then confirm with Enter key.
Press ESC when done, to return to upper level menu.
6. Use the arrow key to select Serial Port.

LAN Set-up
Make sure the Serial port is selected as follows:

Parameters Set to:
Baud Rate 9600
Parity None
Data Bit8
Stop bit 1
Flow Control RTS/CTS
UART FIFO Enabled
Press ESC when done, to return to upper level menu.

7. When back to main menu, please select Exit.
CAUTION Please confirm to make the changes effective, and remember that from
now on, the Flash 4000 LAN will respond to the newly assigned IP Address.
8. Disconnect the Flash 4000 from direct RED patch, and connect it to its final destination
LAN environment by using the grey patch.
At this point check the communication opening again the Internet Protocol (TCP/IP)
Properties page and select Obtain an IP address automatically.
9. As a final check, start from the computer that should be used for controlling the newly
installed Flash 4000 and run Command Prompt.
Then type ping xxx.xxx.xxx.xxx, where the xxx.xxx.xxx.xxx is the new IP you just
configured.
The Flash 4000 should answer as follows:

LAN Set-up
The Flash 4000 is now ready for LAN control through the Thermo Fisher Scientific data
systems. Now it is necessary to configure the data system to access the Flash 4000 through
the configured IP address.
The data systems that support the Flash 4000 control is Eager Xperience.
Data System Configuration
It is advisable to use the self adhesive labels you find in the standard outfit of the Flash
4000 to annotate the IP address and the TCP Port that have been set in the elemental
analyzer. Stick the label in a place that can be easily referenced when it will be necessary to
configure the data system.
10. Install, and start the Data System as described in the specific manual, and go to
Instrument configuration. The Flash 4000 configuration page features the possibility to
control the instrument through the COM ports or to specify a direct TCP/IP address.
11. Just enter the IP address of the Flash 4000 and complete the configuration in the usual
way.
When the Advanced button is pressed, it is possible to set the communication port used
by the TCP/IP protocol and the timeout.
The parameters set by default are those necessary for standard operations; however your
LAN may be provided with Firewall services that may prevent the Port 4001 to be used.
For this reason you have here the possibility to set an alternative port number. However,
the number of the port entered in this box must correspond to the port assigned to Flash
4000 setup described on step 5.
After selecting Raw connection (TCP server), it will be possible to enter the Select for
more setting menu and to enter a different TCP port rather than the default 4001.

LAN Set-up
Moreover the Flash 4000 Instrument configuration advanced settings feature a box for
timeout. This timeout is set by default to 500 ms, and it’s appropriate for most of the
LAN environments. However should the LAN be extremely slow, this time can be
increased to allow slower access to the autosampler.
Note If the connection is performed through hubs over a 10 Mbit/s network, it is
suggested that no more than five Flash 4000 are connected on the same network
trunk. In the case of switched network, this warning can be ignored.
Alternative Configuration
An alternative to the direct setup of the Flash 4000, it is also possible to use a management
program designed for sites where multiple Flash 4000 elemental analyzers with LAN option
are available.
In this case a specific program must be installed and used to monitor, setup, or update each of
the instruments connected.
The program to be installed is named DSSETUP.EXE, and it is in the CD of the data system,
as well as included in the CD of this manual.
Run the installation setup program DSSETUP.EXE:
Deselect the check box COM Port Mapping Tools, since it is not required in the management
of Flash 4000 elemental analyzers.
Please just follow the detailed route proposed step-by-step by the installation program, and
when finished, you can run the program. The first time after the installation the program
starts automatically.
12. From main menu select the Locate Server and the program will automatically search for
all Flash 4000 elemental analyzers connected to the network.
By double-clicking on any of the found Flash 4000, you can setup the program directly

LAN Set-up
Any change can be entered individually for a certain parameter, and when OK is pressed,
the parameter is updated to the instrument on edit.

LAN Set-up

6
Reactor Preparation and Connections

This chapter provides instructions for the preparation of the reactors and them installation
into the elemental analyzer and how to remove them.
Contents
• Introduction to the Preparation of Reactors
• Preparing Reactors and Crucible
• Reactors Installation and Replacement/Remotion
Proceed according to the following operating sequences:
Introduction to the Preparation of Reactors

.
Note The reactors are special steel tubes. The reactors used for combustion require the
crucible.
The following Table 17 and Table 18 report the characteristics of the components required
for N/Protein determination and the type and size of the filling materials to be used for a
proper preparation of reactors.
Table 17. Components required for N/Protein determination

Reference Component Characteristic Filling material
R1 Reactor Material: Special Steel Platinum supported Alumina
Copper Oxide
Quartz Wool
R2 Reactor Material: Special Steel Quartz Wool
Reduced Copper
CR Crucible Material: Special Steel Ultra temperature ceramic
disk
CC Gas chromatographic Material: SS
column Length: 80 cm
Diameter: 10 x 9 mm

6 Reactor Preparation and Connections
Introduction to the Preparation of Reactors
Size of the Filling Material
R1 R2
2 40 mm
CR
260 mm
CR R1 R2
4 360 mm
10 mm 1
15 mm 2
145 mm 3
40 mm
20 mm 2 2
CC
1. Ultra temperature ceramic disks- 2. Quartz wool

3. Platinum supported on alumina and copper oxide 4. Reduced copper
R1. Combustion reactor R2. Reduction reactor
CR. Crucible CC. Chromatographic column

Preparing Reactors and Crucible

The filling materials are introduced into the reactor in a way to form a series of layers of
defined dimensions. For a proper preparation of the filling layers, refer to the filling diagram
as described in paragraph “Introduction to the Preparation of Reactors” on page 73.
Please remember that:

• all reactors have a conical bottom end.
• special steel reactors have the upper end provided with two through-holes.
CAUTION Before using the filling materials required for this operation, please read the
hazard warnings and information reported in the Safety Data Sheets provided, referring to
the relevant CAS (Chemical Abstract Service) number.
Always use original Thermo Fisher Scientific materials and products. The use of materials
not meeting the technical specifications of our products does not ensure a good operation
of the instrument and may even damage it.
The filling of reactors and crucible requires the use of quartz wool and ceramic
disks respectively. Before handling these materials, we recommend to wear
gloves and face protection.

• “To Fill the Special Steel Reactors” on page 75
• “To Prepare the Crucible” on page 78
The filling procedures should be carried out on a wide and clean workbench.
Y To Fill the Special Steel Reactors
The following operating sequence provides instructions for filling the combustion and
reduction reactors.
Material Required
Special steel reactors
Compression rod
Filling material
Lubricant (silicon grease)
Use the following operating sequence to fill the steel reactors:

Note To measure the different layers, we recommend the use of the compression rod
marking each time the measure on the reactor.

To Fill the Combustion Reactor

1. Introduce a sufficient amount of quartz wool into the bottom end of the reactor to form
the required layer as shown in Figure 31.
Figure 31. Introduction of quartz wool into the bottom end of the combustion reactor
Reactor
Quartz wool
2. Mix a proper amount of platinum supported on alumina (PtAl2O3) and copper oxide
(CuO) as shown in Figure 32.
Figure 32. Filling materials mixture
Filling material mixture
3. By using a spatula, introduce a proper amount of the prepared platinum supported on

alumina and copper oxide mixture into the top of the reactor to form the required layer as
shown in Figure 33.
Figure 33. Filling of the combustion reactor with the mixed filling material (1)
4. Introduce a sufficient quantity of quartz wool to form the last required layer.

5. Gently push down the quartz wool by using the rod provided without overpressuring.
6. Place and smear a slight layer of silicon grease on the conical bottom end of the reactor.
To Fill the Reduction Reactor

1. Introduce a proper amount of quartz wool into the bottom end of the reactor to form the
required layer as shown in Figure 34.
Figure 34. Introduction of quartz wool into the bottom end of the reduction reactor
Reactor
Quartz wool
2. Introduce a proper amount of reduced copper into the upper end of the reactor as shown
in Figure 35.
Figure 35. Filling of the reduction reactor with the filling material
Reduced copper
3. Introduce a sufficient amount of quartz wool to form the last required layer.
4. Gently push down the quartz wool by using the rod provided without overpressuring.
5. Place and smear a slight layer of silicon grease on the conical bottom end of the reactor.

Y To Prepare the Crucible
The following operating sequence provides instructions for the preparation of the crucible you
will use with the special steel reactors required for combustion.
Figure 36. Crucible
2
1
3
1. Crucible body 2. Crucible bottom end

3. Ultra temperature ceramic disks
Material Required
Ultra temperature ceramic disks
Use the following sequence to prepare the crucible:

1. Unhook the bottom end of the crucible from the body as shown in Figure 37.
Figure 37. Crucible disassembling
2. Hold the crucible bottom end as shown in Figure 38. Introduce two ultra temperature
ceramics disks into the bottom end of the crucible.

Figure 38. Introduction of ultra temperature ceramics disks into the crucible
3. Hook the crucible bottom end to the crucible body as shown in Figure 39.
Figure 39. Crucible reassembling

Reactors Installation and Replacement/Remotion

This paragraph contains the instructions to install the reactors into the furnaces of the
elemental analyzer and it also provides information on how to remove them.
Installation of the Reactors into the Furnaces

Note The reactors of special steel used for combustion require the use of a crucible.
Table 18. Reactor and furnaces

Determination Reactor in Left Furnace Reactor in Right Furnace
N/Protein Special steel reactor Special steel reactor
(combustion) + special steel (reduction)
crucible
Before installing the reactors perform the following operations:

• Check that the furnaces are at room temperature.
• Open the lower door unscrewing the proper fixing screw.
• Remove the autosampler front cover.
CAUTION The reactors must be installed with the furnaces at room temperature.

• “To Install the Combustion Reactor” on page 80
• “To Install the Reduction Reactor” on page 83
Y To Install the Combustion Reactor
Material Required
Tool for steel tube
O-ring
Proceed as follows:
1. Remove the autosampler, if installed, from the connecting fitting of the reactor tube by
manually undoing the fixing nut, as shown in Figure 40.
Note It is not necessary removing completely the autosampler from the analyzer and
disconnecting the signal cable.

Figure 40. Autosampler remotion
MAS 4000 autosampler Autosampler fixing nut
2. On the conic part of the reactor smear a small quantity of o-ring lubricant.
3. Introduce the reactor into the furnace as shown in Figure 41.
Figure 41. Introducing the combustion reactor into the furnace
Combustion reactor
4. Guide the reactor into the furnace. The conical part should slide into the coupling union
located on the base of the furnaces compartment, as shown in Figure 42.
Figure 42. Driving the reactor into the furnace
Furnace
Reactor
Coupling union Base
5. Push the reactor up to reach the correct placement, as shown in Figure 43.

Figure 43. The reactor in place
6. Slip on the O-ring as shown in Figure 44.
Figure 44. O-ring
O-ring
7. Using the tool for special steel reactors, introduce the crucible into the combustion
reactor, which is in the left furnace. See Figure 45.
Figure 45. Introduction of the crucible into the combustion reactor
Crucible
removing
tool
Crucible
8. Manually screw the autosampler nut. See Figure 46.

Do not use mechanical tools to screw or unscrew the fixing nut.
Figure 46. Mounting the autosampler on the left furnace
At the end of the operation, proceed as follows:

9. Reinstall the autosampler.
10. Close the lower door and fix it with the screw.
11. Reinstall the autosampler front cover.
Y To Install the Reduction Reactor
Material Required
Tool for steel tube
O-ring
1. On the conic part of the reactor smear a small quantity of lubricant.

2. Introduce the tool, provided in the standard outfit, into the holes located on the top end
of the reactor. Introduce the reactor into the furnace as shown in Figure 47.
Figure 47. Introducing the reduction reactor into the furnace
Reduction
reactor

3. Guide the reactor into the furnace. The conical part should slide into the coupling union
located on the base of the furnaces compartment, as shown in Figure 48.
Figure 48. Driving the reactor into the furnace
Furnace
Reactor
Coupling Base
Union
4. Push the reactor up to reach the correct placement, as shown in Figure 49.
Figure 49. The reactor in place
Reactor
removing
tool
5. Slip on the O-ring as shown in Figure 50.
Figure 50. O-ring
O-ring
6. Manually screw the fixing nut as shown in Figure 51.

Figure 51. Mounting the fixing nut on the right furnace
At the end of the operation, proceed as follows:

• Close the lower door and fix it with the screw.
• Reinstall the autosampler front cover.
Remotion of the Reactors from the Furnaces

Before starting carry out the following operations:
7. Check that the furnaces are at room temperature.
8. Open the lower door unscrewing the proper fixing screw.
9. Remove the autosampler front cover.
CAUTION The reactors must be removed with the furnaces at room temperature.
Make sure that the gas flows are OFF.

• “To Remove the Combustion Reactor” on page 85
• “To Remove the Reduction Reactor” on page 87
Y To Remove the Combustion Reactor
The following operating sequence contains the instructions to remove the combustion reactor
from the furnace.
Material Required
Tool for special steel reactor
Tool for crucible

Proceed as follows:
1. Remove the autosampler, if installed, by manually undoing the fixing nut as shown in
Figure 40 on page 81.
2. Remove the O-ring from the top of the reactor as shown in Figure 52.
Figure 52. O-ring
O-ring
3. Remove the crucible from the combustion reactor (left furnace) using the appropriate tool
as shown in Table 53.
Figure 53. Crucible removal
Crucible removing tool
Crucible
4. Using the proper tool, remove the reactor turning it counterclockwise and simultaneously
pulling it upwards, as shown in Figure 54.
Figure 54. Removal of the reactor
Reactor
removing
tool
At the end of the operation proceed as follows:

5. Reinstall the autosampler.

6. Close the lower door and fix it with the screw.
7. Reinstall the autosampler front cover.
Y To Remove the Reduction Reactor
The following operating sequence contains the instructions to remove the reduction reactor
from the furnace.
Material Required
Tool for special steel reactor
Proceed as follows:
1. Remove the autosampler front cover.
2. Remove the fixing nut as shown in Figure 55.
Figure 55. Fixing nut removal
3. Remove the O-ring from the top of the reactor as shown in Figure 56.
Figure 56. O-ring
O-ring

4. Using the proper tool, remove the reactor turning it counterclockwise and simultaneously
pulling it upwards, as shown in Figure 57.
Figure 57. Removal of the reactor
At the end of the operation proceed as follows:

• Close the lower door and fix it with the screw.
• Reinstall the autosampler front cover.

7
Sample Preparation
This chapter describes the technique for the sample preparation and the basic instructions to
weigh the sample.
Contents
• Sample Weighing Technique
• Weighing Technique for Solid Samples
Sample Weighing Technique

CAUTION Be very careful in preparing samples, because the substances to be analyzed
may be dangerous.
Read the Safety Data Sheets referring to the different chemicals and handle them in the
appropriate environment (for example, under a fumes hood), strictly obeying the
company safety regulations.
To define the weighing range, you should know the nature (organic, inorganic,
metal-organic) and origin (pure chemical, natural product) of the substance to be analyzed.
For weighing samples, the following materials are required:

• Balance
• Capsulator
• Cylindrical tool
Solid Samples
Solid samples are introduced directly into the tin container by using a spatula. According to
the sample quantity to be analyzed, refer to “Weighing Technique for Solid Samples” on
page 90.
Liquid Samples
The sampling will be according to the sample nature.

7 Sample Preparation
Weighing Technique for Solid Samples
Samples Characterized by Limited Volatility

• If the sample density is 1 or close to 1 (water, beer, juice and wine are typical examples)
Introduce the sample by using a syringe of 100 μl capacity.
• If the sample density varies significantly, even in samples of the same nature (milk is a typical
example)
Only for N determination, let the sample be adsorbed on a Chromosorb WAW® layer
previously introduced into the container.
Samples Characterized by High Viscosity

They must be properly mixed before being drawn.
To introduce the sample, take some using a spatula and let it without touching the container
walls. Only for N Determination, according to the sample viscosity, it may be necessary to
adsorb the sample on a Chromosorb WAW® layer previously introduced into the tin container.
Samples Available in Liquid Phase

They can be injected directly into the reactor as follows:
• Manually, through the manual injection device by using a micro syringe.
• Automatically, by using the autosampler for liquid samples.

The following operating sequence contains the instructions to weigh large quantities of solid
samples.
Y To Weigh the Solid Samples
Material required
Tin disks
Capsulator
Cylindrical tool
Spatula
Tweezers
Balance
Figure 58 shows the accessories required to weigh solid samples.

Figure 58. Accessories required to weigh solid samples
Tweezers Capsulator
Tin disk
Spatula
Cylindrical
tool
1. By using tweezers, take a tin disk and rest it on the cavity of the capsulator.
2. By using the cylindrical tool, press the tin disk and make it enter the cavity of the
capsulator, as shown in Figure 59.
Figure 59. Preparation of the tin container
3. By using a spatula, introduce the sample into the tin container until it is sufficiently filled
as shown in Figure 60.
Figure 60. Introduction of the sample
4. Delicately close the tin container with your hand as shown in Figure 61.

Figure 61. Compression of the sample (1)
5. By using the cylindrical tool, press the tin container filled with the sample into the cavity
of the capsulator, as shown in Figure 62.
Figure 62. Compression of the sample (2)
6. Remove the container filled with the sample from the capsulator as shown in Figure 63.
Figure 63. Tin container filled with sample (1)
Note The tin container filled with the sample should have a spherical shape. See
Figure 64.

Figure 64. Tin container filled with sample (2)


8
Analytical Methods
This chapter describes the analytical methods used for the Flash 4000 elemental analyzer.
Contents
• Introduction
• Analytical Method for N/Protein Configuration
Introduction
The analytical method includes different subsequent steps to determine the percent
composition of Nitrogen through the transformation of the solid or liquid sample into gas.
CAUTION For correct sample analyses the pneumatic lines must be leak-free. Therefore, a
preliminary leak check is recommended before starting analytical cycles.
Analytical Method for N/Protein Configuration

Method Description
Refer to Figure 65 and Figure 66.
Figure 65. Schematic diagram
AS
R1 R2 WD F1 F2 CC
TCD

8 Analytical Methods
Diagram
An autosampler AS is connected to a special steel reactor R1 placed in an furnace at the
temperature of 950 °C.
This reactor is connected to a second reactor R2 placed in an furnace at the temperature of
840 °C. The R2 is connected to the condensate water drainage WD that is connected to two
adsorption filters F1 and F2. These are connected in parallel and working alternatively. The
outlet of the filter F2 is connected to the analytical column CC, on its turn connected to the
thermal conductivity detector TCD.
Figure 66 shows the system pneumatic circuit in the pre-analysis stage.
Figure 66. Pneumatic diagram
EFC-t Module Front Panel - FP
PI1
S2
F
He PRV1 He
SVP2 T
1
2
(5)
PI2
F
O 2 PRV2
F O 2
SV1
IN OUT (6) 2
TCD 6,5 ml/min @ 300 kPa - O

2 3 1
PI3
F
IN OUT (7)
CC
Carrier Red
2
SV3 1 SV4 SV2 3 1
1
AS
2 2 2 Green
CV 1
S1
Combustion furnace
Reduction furnace
Vent
4
(4) 1
SVP1
(1) (2)
R1 R2
Reference
(7) (2)
Water
F F drain
600 sccm @ 30 psi - AIR

WD
SV8 SV9 SV5

3 1 1 3
Vent
2 2
Bottom - BF (6) F F (4) Top - TF

White White
Blue Blue
B
(5) F F (3)
2 2
3 1 1 3
SV7 SV6
(8) (1)
Reference helium He flows to the flow sensor S1, through the solenoid valve SV2. Both flow
sensors are connected to the relevant proportional valves SVP1 and SVP2.
The flow of helium is split in two streams: carrier and reference.
The reference helium flows to the TCD through the flow sensor S2. Then, the reference
helium is used as purge gas by the sample into the autosampler.
The carrier helium is controlled by the flow sensor SV2. At the moment of the combustion,
the carrier helium is exchanged with the oxygen flow through the solenoid valve SV2.

Sequence of the Method Stages

During pre-analysis the solenoid valve SV1 shuts off Oxygen, whereas the solenoid valve SV2
allows Helium to flow in the circuit.
When Start Analysis is pressed, and the combustion is started, the solenoid valve SV1 opens,
whereas the solenoid valve SV2 switches to allow Oxygen to flow in as far as the combustion
reactor R1 for a preset time.
The sample, weighed in a tin container and stored in the autosampler, is dropped into the
combustion reactor after a few seconds. Tin, coming in contact with an extremely oxidizing
environment, triggers a strong exothermic reaction.
Temperature rises to approximately 1800 °C instantly causing the sample combustion.
At the end of the time set for Oxygen introduction, the solenoid valves SV1 and SV2 return to
their original position restoring the Helium flow. The gas mixture (N2, CO2, H2O and SO2)
generated by combustion is conveyed across the reactor R1 where oxidation is completed.
Then the mixture crosses the reactor R2 where Nitrogen oxides possibly formed are converted
into elemental Nitrogen, and the Oxygen excess is retained.
The gases pass in the water drain WD where water is condensed and separated from the
stream. Then the CO2 filters F1 and F2 adsorbs the Carbon Dioxide and the water fraction
which has passed the WD. Nitrogen is then eluted in the chromatographic column CC and
conveyed to the thermal conductivity detector TCD that generates an electrical signal, which,
properly processed by Eager Xperience, provides the Nitrogen-Protein percentage.


Part 3
Analysis
9
Instrument Set-up
This chapter contains information and operating sequences to set the instrument for
running analyses.
Contents
• Introduction
• Powering on the System
• Installation of Eager Xperience
• Eager Xperience Main Menu
• Analytical Configuration
• Edit Method
• The Elemental Analyzer Parameters
• Analyzer Status
• Detector Signal Level
• Leak Test
Introduction
To analyze any type of sample the instrument must be in the correct operating conditions.
• “To power the system on” on page 102
• “To Install Eager Xperience” on page 102
• “To Configure the Analyzer” on page 106
• “To Check Leaks” on page 117
• “To Adjust the Detector Signal Level” on page 116
CAUTION Before starting the operating sequences, make sure that instrument, reactors,
regenerative CO2 filters, autosampler (or manual injection device for liquids) and any
complementary units are properly installed.

9 Instrument Set-up
Powering on the System
Powering on the System

Y To power the system on
1. Switch on the instrument lifting the breaker, located at the back of the instrument, on the
position I. At the powering on, the indicating LED Power on the status panel lights up
green.
2. Switch on the computer and any complementary units by means of relevant switches.
Installation of Eager Xperience

Y To Install Eager Xperience
Material required
Eager Xperience package
The software Eager Xperience can be installed in a system provided with Windows™
2000/XP/Vista operating systems. The free space on the PC hard disk must be at least 30 MB.
Eager Xperience is installed by using the CD provided in the standard outfit and operating as
follows:
1. When the CD is introduced into the CD driver of the PC, the installation menu shown
in Figure 67 is displayed.
Figure 67. Eager Xperience installation menu
Note If the installation menu does not automatically appear, start the CD Autorun
program through the Windows™ Start-Run command.
2. Start installation by clicking the push-button Install Eager Xperience for Flash.
3. Follow the instructions prompted step by step.
4. At the end of installation, in the page Start-Program Eager Xperience, double-click the
Eager Xperience for Flash icon. The window of Figure 68 is displayed.

9 Instrument Set-up
Eager Xperience Main Menu
Figure 68. Selection of the instrument
5. Click the icon of the instrument selected.

The program is designed to work with four instruments. Each icon corresponds to one
instrument. The instrument name shown below the icon can be changed. To do this, click
on the existing name and overwrite the new one.
6. Eager Xperience proceed with the registration and the activation of some drivers needed for
the correct functioning of the software.
a. Click Ok to the answers prompted step by step.
b. At the end of the operation, reboot the computer. Start Eager Xperience again selecting
Start > Programs > Eager Xperience > Eager Xperience for Flash.
7. Follow the prompted indications. At the end of the installation, the Main Menu is
displayed.

The Main Menu of Eager Xperience, shown in Figure 69, is the starting point to enter all
menus and relevant functions. Menus and icons of Main Menu are described in the following
Table 19 and Table 20 respectively.
Figure 69. Eager Xperience Main Menu

9 Instrument Set-up
Table 19. Main Menu: description of the menus

Menu Description Submenus and Options
File This menu contains functions • Set language
concerning the instrument • Colour set
operation. • Instrument configuration
It is used during the analyzer • System administration
installation procedure. • Installation qualification
• Load method
• Load system defined method
• Save method
• Copy method from...
• Printer setup
• Print method
• Exit Eager Xperience
Run Use this menu to choose the type • Start sequence of samples
of start command to be sent to the • Stop running sequence
analyzer, and also to stop the • Start single sample data acquisition
analytical cycle or abort the • Stop data acquisition
current analysis. • Abort data acquisition
• Run macro
Edit This menu provides functions • Edit Method
related to the instrument setup • Component table
and analytical parameters. • Sample table
• Wizard method development
• Edit Elemental Analyzer parameters
View Use this menu to monitor the • View sample being acquired
analysis in real time, read the • Last sample calculated results
result of the last sample run, check • View Calibration curve
the calibration curve, compare • View Chromatograms
and overlay chromatograms, • Overlay Chromatograms
check the instrument status and • Operate on Chromatograms
maintenance. • Compare Chromatograms
• View Elemental Analyzer Status
• View Maintenance
Recalculation Use this menu to cancel the • Reset calibration factor
calibration curve and the results of • Recalculation
previous analyses. You can • Summarize results
recalculate previous results
individually or sequentially.
It also provides the summary of
results.
Tools Use this menu when the ashes • Ashes removal
removal and/or reactor • Reactor replacement
replacement is required as • Cleaning the MAS piston
maintenance

9 Instrument Set-up
Table 19. Main Menu: description of the menus, continued

Menu Description Submenus and Options
Help Use this menu to enter Eager • Help
Xperience help program. It is • About Eager Xperience
subdivided into different modules,
each one designed to cover specific
issues of the module currently in
use.
Table 20. Main Menu: description of the icons

Icon Function Description
Load method Use this icon to load a previously saved analytical
method.
Save method Use this icon to store new operating methods.
Wizard method Use this icon to develop new operating methods

development
Edit method This icon accesses to the integration and calculation

parameters, and to the parameters for printing
analytical reports.
Components Table This table contains the stored retention times, which
allow to identify N, C, H, S and O.
Sample Table This table contains all functions related to sample

records, and the function allowing communication
with the balance.
Summarize results This feature contains analytical results, print options
and chromatograms.
Recalculation This function allows to recalculate previous results.
View Maintenance This icon allows to program current maintenance by

recording the number of analyses run by each reactor
of the analytical circuit.
Edit Elemental Analyzer Use this icon to open the pages containing the
Parameters commands for the setting of temperatures, flows,
times, detector and the analyzer control functions.
View Elemental Analyzer This function comprises the pages displaying the
Status analyzer conditions.
It contains special functions to check the system
pneumatic tightness (Leak Test), to check the baseline
level, and to program automatically the “Autoready”
function.

9 Instrument Set-up
Analytical Configuration
Table 20. Main Menu: description of the icons, continued

Icon Function Description
Start sequence Use this icon to start a series of analyses having
different current and timed requirements. At the end
of the analytical cycle, the instrument can either be put
in Standby Mode or the furnace and detectors be
switched off, or the gas flows turned off.
Stop sequence Use this function to stop in any moment the sequence
of analyses only completing the current run.
The analytical conditions are set in our laboratories during the final test of the analyzer. To put
the analyzer in operating conditions, you only have to follow the instructions reported in the
next operating sequence.
Y To Configure the Analyzer
1. In Main Menu of Figure 69 on page 103, choose File > Instrument Configuration. The
following window is displayed.
Figure 70. Instrument name and configuration
a. In the section Instrument name, type the instrument serial number (6 digits; for
example 991234). See the label located on the instrument rear panel.
b. In the section Analytical instrument configuration select N/Protein option.
Note The option Undefined can be used in case the desired operating conditions
are different from those defined for the instrument configuration.
c. Click Elemental analyzer setup to enter the dialog window of Figure 71 where the
configuration parameters have to be set.

9 Instrument Set-up
Figure 71. Configuration dialog window
d. In the section Elemental Analyzer Connection select the computer serial port
(COM1, COM2 etc.) to which the instrument is connected.
If the LAN control of the Flash 4000 is required, select network address and enter the
I.P. address. Use Advanced button to set the LAN communication port used by the
TCP-IP protocol and timeout.
e. In the section Type verify that the instrument in use is Flash 4000.
f. In the section Instrument Settings choose the following settings:
i. Line Frequency = 50 Hz
ii. TCD Settings Source = Internal
iii. TCD Settings Polarity = Positive
g. In the section Sampler Setting select the type of autosampler installed on the
instrument.
i. In the case of autosampler for liquid sample, also specify the computer serial port,
to which the autosampler is connected, and the number of vials.
ii. Click Ok to go back to the window of Figure 71, then click Ok to return to Main
Menu.

9 Instrument Set-up
Edit Method
Edit Method
In Main Menu choose Edit > Edit Method or just click the icon . The Edit Method dialog
box is visualized.
Figure 72. Edit Method
Method editor tabs allow to modify the method parameters and to access the following
sections:
Method Title
Method Title tab
This tab allows to add a comment to the method. This comment will be displayed in Main
Menu and saved with the parameters of the analysis.
Detection Parameters
Detection parameters is the section of the analytical method that contains all the parameters
for the data acquisition.

9 Instrument Set-up
Edit Method
Detection Parameters tab
This tab provides the following functions:
Function Description
Time Base This box specifies if you want to work with a time base in seconds
or minutes.
Actual Sample This box indicates the sample being acquired.
Baseline Background It permits to compensate the acquired chromatogram with the
Compensation baseline background.
Integration Parameters
Integration parameters is the section of the analytical method that contains all the parameters
for the integration.
Integration Parameters tab
This tab provides the following functions.
This dialog box contains all the parameters used for the integration algorithm. The
integration algorithm is based on the following parameters.
Parameter Description
Peak Width It specifies the width of the peaks to be integrated.
Peak Threshold It is used by the integration algorithm to discriminate the peaks
from the baseline or the signal noise.

9 Instrument Set-up
Edit Method
Parameter Description
Minimum Area The peak having an area lower than the entered value are rejected.
Skim Ratio It determines whether overlapping peaks are integrated by using
tangential skim or perpendicular drop methods.
If the ratio between the areas of two or more consecutive peaks is

higher than the entered value, then a tangent correction is
performed.
Real Time Plot It contains the scale and the offset for the display of the
chromatogram being acquired in the module View sample being
acquired.
Test Integration Click this button to verify the entered parameters of a stored
chromatogram. You can modify the integration parameters until
the desired integration is achieved.
Time Event Click this button to set all the parameters that need to be change to
improve the integration or different peak shape.
Calculation Parameters
Calculation parameters is the section of the analytical method that contains all the parameters
for the calculation of the element percentage.
Calculation Parameters tab
This tab provides the lowwowing functions:
Calibration Method It allows to specify the calibration method by which the analyzed
sample will be processed. See Instrument Calibration.
Heat Value It allows to perform heat value calculations or to estabilish the
Calculation calorific content of solid or liquid samples in an automatic manner.
Protein It allows to perform the calculation of the protein content a sample
in a fully automatic manner.
CO2 Emission Factor This option allows to perform the CO2 emission factor either for
liquid or for solid samples in an automatic manner. The calculation
of the Carbon Dioxide emission factor is based on the percentage
composition of the elements and on the Gross Heating Value.

9 Instrument Set-up
Edit Method
Report Parameters
Report parameters is the section of the analytical method that contains all the parameters for
the report.
Report Parameters tab
This tab provides the following functions.
Report Type Choose among the following report types:
• Standard report
• Extended report
• Summary report
• Custom report
Include Signal to It permits to choose the peak of interest and the baseline portion
Noise Report on which the noise evaluation should be done.
Include Calibration Check this option to have the printout of the samples calibration
Report report for each of the calibration levels.
Append for
Summarize Click the icon and select the result to append for summarize,
normally Element %.
Standard Report On Choose among the following reports:
• None: It will not generate any report at all.
• Printer: It will send the report directly to the printer.
• ASCII: It will send the report to an ASCII disk file.
• DIF: It will send the report to a DIF file.
• Excel: It will send the report to a XLS file.
• HTML: It will send the report to HTML format.
Concentration Unit Normally %
Report Title It permits to enter a text to be printed as a title of the report
generated by the system.
Report Publisher It is the tool to create or modify the file report layout.

9 Instrument Set-up
Edit Method
Report Stripchart
Report stripchart permits to select and to set the stripchart options to be included in the
report printout.
Report Stripchart tab
This tab provides the following functions:
Stripchart Options This box contains the parameters used for the generation of the
stripchart report.
Stripchart Title This box permits to enter a text to be printed as a title of all
stripchart generated by the system.
Strichart Annotation Check the options of interest.
Operator ID/Info
Operator ID/ Infotab
In this tab the operator can store the informations for future reference.

9 Instrument Set-up
The Elemental Analyzer Parameters
The Elemental Analyzer Parameters

In the elemental analyzer parameters you can find the following.
Y To Edit Elemental Analyzer Parameters
1. In Main Menu, choose File > Instrument name and configuration and enable the
elemental parameter setting by ticking the relevant check box as shown in Figure 73.
Figure 73. Enable Elemental Analyzer Parameters Setting
2. In Main Menu, choose Edit > Edit Elemental Analyzer Parameters or just click the icon
. The following tabs are visualized where the analyzer operating parameters are
displayed. Refer to Table 21.
Table 21. Elemental analyzer parameters tabs

Tab Description
Temperature In this tab it is possible to set:
• the combustion reactor temperature in °C
• the reduction reactor temperature in °C
• the TCD cell temperature in °C
Flow/Timing In this tab it is possible to set:

• the carrier gas flow in mL/min
• the reference gas flow in mL/min
• the system timing in minutes

9 Instrument Set-up
Analyzer Status
Tab Description
Oxygen/CO2 Traps In this tab it is possible to set:
• the trap heating time in minutes
• the trap cooling time in minutes
Detector In this tab it is possible to:

• set time events to modify, during acquisition at a
preset time, the signal sensitivity (Gain)
• to force the autozero at the Gain change
Analyzer Status
This fuction allows to visualized the status of the elemental analyzer through five tabs. This
function is accessible from Main Menu choosing View> View Elemental Analyzer Status or
just clicking the icon .
The following dialog window is displayed.
Figure 74. View Elemental Analyzer Status dialog window
The Flash 4000 Status tabs are reported in Table 22:

9 Instrument Set-up
Analyzer Status
Table 22. Status tabs

Tab Description
General In this tab it is possible:
• to visualize the parameters set in the method such
as temperature and flows.
• to turn on and off the furnace temperature and the
flows.
• to visualize the status of the instrument such as
Ready, Run, Sampling, Oxygen injection, etc.
Detector In this tab it is possible:

• to visualize the status of the TCD filaments.
• Adjust the detector signal level.
For details refer to “Detector Signal Level” on
page 116.
Stand-by/Wake-up In this tab it is possible:

• to turn the instrument in the Standby condition
by clicking Deactive/Active.
• to power on the instrument programming the
dedicated timed function (Wake-up).
Trap Functions In this tab it is possible:

• to visualize the status of the traps as In use,
Regeneration, Heating, Cooling.
• to perform a regeneration of the traps by clicking
Start regeneration cycle Top or Bottom.

9 Instrument Set-up
Detector Signal Level
Table 22. Status tabs, continued

Tab Description
Special Functions In this tab it is possible:
• to perform a leak test.
For details refer to “Leak Test” on page 116.
• to disable the sampling and the oxygen injection.
Detector Signal Level

Y To Adjust the Detector Signal Level
1. In Main Menu choose View > View Elemental Analyzer Status or just click the icon .
The dialog window of Figure 75 is displayed. Select the tab Detector.
Figure 75. Detector parameters window
2. Click Auto Adjust Level at 1000 μV. At the end of the operation, the value 1000 is set
representing the analysis starting point.
Leak Test
The leak test must be performed any time a component of the pneumatic circuit is replaced.
Operate according to the instructions reported in the following operating sequence.

9 Instrument Set-up
Leak Test
Y To Check Leaks
1. In Main Menu choose View > View Elemental Analyzer Status or just click the icon .
The dialog window of Figure 76 is displayed. Select the tab Special Function.
Figure 76. Analyzer status
2. In the section Command click Leak Test. The dialog window with the leak test
parameters is displayed as shown in Figure 77.
Figure 77. Leak test parameters dialog window
a. Click Start to begin the operation. A window will appear where you will be requested
to perform the leak test with the CO2 trap regeneartion on the last use.
b. A second window will appear where you will be requested to perform the Autozero.
c. After some seconds (Leak test time), Carrier flow and Reference flow must be
within 0 and 5mL/min. Higher values indicate that the system is not leak-free.
Note Leaks in the system are generally due to incorrect closure of the reactors
locking nuts.
3. To terminate the leak test and restore the flow operating values, click Stop and Done.

9 Instrument Set-up
Leak Test

10
Instrument Start-up
This chapter contains information and operating sequences to prepare the instrument for
running analyses.
Contents
• Start-up
CAUTION Before starting the following operating sequences, make sure that instrument,
reactors, autosampler (or manual injection device for liquids) and any complementary
units are properly installed.
Start-up
Y To Start-up the instrument
1. In Main Menu choose Edit > Edit Elemental Analyzer Parameters or just click the
icon .
2. Select the Flow/Timing tab and set 300 mL/min for both carrier and reference flows as
shown in the following Figure 78.
Figure 78. Flow/Timing tab
Set 300
Set 300

10 Instrument Start-up
Start-up
3. Click Send to trasfer the operating parameters to the instrument. Click Ok to exit.
4. In Main Menu choose View> View Elemental Analyzer Status or just clicking the icon
.
5. Select the Special function tab and start the leak test by clicking Leak test as shown in
Figure 79. For detail refer to “Leak Test” on page 116.
Figure 79. Special Functions tab
Click this button

to start Leak Test
If there is not any leak, proceed as follows:

6. In Main Menu choose Edit > Edit Elemental Analyzer Parameters or just click the icon
.
7. Select the Temperature tab and set the combustion, reduction and TCD temperatures
according to the Test Report received as shown in the example of Figure 80.
Figure 80. Temperature tab
Set temperatures
8. Click Send to transfer the operating parameters to the instrument. Click Ok to exit.

Start-up
9. In Main Menu choose View> View Elemental Analyzer Status or just clicking the icon
.
10. Select the Detector tab and turn on the filaments of the TCD as shown in Figure 81.
Figure 81. Detector tab
Turn filaments On
11. Wait the Ready of the instrument and perform again the leak test. For details refer to
“Leak Test” on page 116.
12. Wait the stabilization of the TCD signal, then adjust the detector signal. For details refer
to “Detector Signal Level” on page 116.
13. It is possible to start the analysis.

Start-up

11
Guide to Run Analyses

This chapter contains information and operating sequences to run sample analyses, and it
also describes the comparison methods for a correct evaluation of results. Practical advise for
daily operation is also provided.
Contents
• Introduction
• Directory for Analyses
• Current Maintenance Program
• Instrument Calibration
• Sample Table
• Sequence of Analyses
• Quality Control and Check of Analytical Results
• Post-Analysis Operations
• Analytical Troubleshooting
Introduction
To program and analyze any type of sample, do the following:
• Create a directory for analyses
• Program the current maintenance (recommended operation)
• Choose the calibration
• Set a sample table
• Run the sequence of analyses
• Determine the blank value
CAUTION Before starting operating sequences, make sure that the instrument start-up
operations have been performed as described in Chapter 9.

11 Guide to Run Analyses
Directory for Analyses
Directory for Analyses

Before analyzing a sample, you should create a directory where you will store the operating
method comprising:
• Sample table
• Integration parameters
• Calculation parameters
• All that is necessary to run the analysis
Current Maintenance Program

The reactor and relevant fillings need to be replaced. The View Maintenance option will
indicate when the different components have to be replaced. To start the maintenance
program, do as described in the following operating sequence.
Y Start-up of the Current Maintenance Program
1. In Main Menu select View > View Maintenance; a window like the following one is
displayed.
Figure 82. Maintenance: Example of program schedule
Component Description
Left 1 It represents the crucible.
Left 2 It represents the oxidation reactor.
Right It represents the reduction reactor.
The example above shows the analytical circuit components for which the maintenance
routine is required.

Current Maintenance Program
a. In the diagram the active components are indicated with colored areas and show on
the left the numerical scale of their lifetime. The meaning of each colored area is
indicated in the upper section of the diagram.
b. The components not present in the concerned instrument configuration are indicated
by a dashed line.
2. To view in detail the default conditions of the components of the concerned instrument
configuration, choose Edit > Set Maintenance >Default. A window like the one shown
in Figure 83 is displayed. The values shown cannot be changed.
Figure 83. Maintenance: Example of default condition
Table 23. Maintenance default condition

Condition Description
Life time It indicates the preset maximum number of analyses each individual
component can perform.
Number of runs to It indicates that when any of the components will still have to run
warning message only 10 analyses to reach the number set in Lifetime, each program
page will display the message Check Maintenance. If the message is
ignored and analyses are continued, when the preset number of runs
is reached, the message Alarm will be displayed. This does not stop
the analytical cycle.
Number of runs It indicates the number of runs after them the maintenance will be
until next required.
maintenance
Number of runs It indicates the number of runs performed after the last maintenance.
since last
maintenance
3. To use a different maintenance program from the default one, choose Edit > Set
Maintenance > Manual. A window like the following will be displayed.
a. In the window of Figure 84, you can change any value by clicking on the different
boxes and entering the desired new value.

Instrument Calibration
Figure 84. Maintenance: Example of manual program
Eager Xperience offers three calibration methods:
• K-Factor
• Linear
• Non Linear
All tests are performed with the K-Factor method that is generally used by most users. This
method consists in obtaining a constant of calculation by means of the following formula:
K =%Th*(I-b)/w
where:
Th = Theoretical percentage of the standard

w = Weight in milligrams of the standard
I = Area integral of the standard
b = Blank area integral
For the calculation of an Unknown sample, Eager Xperience will use the reverse formula:
%Unknown = K*w/(I-b)
where:
K = K-factor
w = Weight in milligrams of the sample
I = Area integral of the sample
b = Blank area integral
The Linear method is generally used when samples very different from each other are
analyzed in the same analytical sequence. In this way the errors due to the detector response
linearity are minimized.

The Non-Linear method is used when the analyzer is connected to another detector having a
response of exponential type. To select the calibration method or view the calibration curves of
a memorized method, do as described in the following operating sequence.
Y To Calibrate Method and Curves
1. Select the calibration method

a. In Main Menu choose Edit > Method or just click the icon. The following
window will be displayed:
Figure 85. Method editor
b. Select the option Calculation Parameter.

i. In the section Calibration Method, select the calibration method required.
ii. In the section Protein, tick Protein Calculation. Click on the icon shown on the
box right side to display the relevant calculation scheme.
2. View the calibration curves. At the end of analyses of the standard samples, it is possible
to visualize the calibration curve operating as follows:
a. In Main Menu choose View > View Calibration curve. A window similar to one
below will be displayed.
Figure 86. Example of Calibration curves
b. Select Calib. Method. According to the calculation method, the calibration points
with peak area and concentration will be displayed.

Sample Table
Sample Table
The sample table of the analytical method contains all information concerning the series of
samples to be acquired and processed. To enter the sample table, do as described in the
following operating sequences.
In Main Menu select Edit > Sample table or just click the icon . Sample Table will be
displayed.
Figure 87. Example of Sample table
Y To Fill Sample Table
1. Select Edit sample >Fill Sample table or just click the icon . The following window
will be displayed, which offers all the functions necessary to fill, change or cancel Sample
Table.
Figure 88. Window to fill Sample Table
a. In the section Samples edit as follows:

i. Do not enter Sample Name now. Sample name, or sample monogram will be
entered from time to time as required.
ii. In the text box Filename, enter the filename to be used to save the sample.

Sample Table
iii. In the box Number samples, enter the number of samples, up to 200, to be
analyzed.
iv. Check that Unknown is ticked
2. Leave Sample name idx and Filename idx set as 1.
a. In the section Sampler, enter the parameters if the instrument is equipped with the
autosampler for liquids.
b. In the left bottom section, enter the following.
i. Leave Weight set as 1.
The weight is entered time by time. In case of direct injections of constant
volumes, the sample volume can be entered directly.
ii. Set Protein factor.
3. At the end of editing, click Replace. The sample table appears again. In the sample table
grid you will find all information entered.
Note In the case of liquid samples analyses with the autosampler for liquid, the
column Density will be displayed in the sample table grid in which insert the density
of the liquid sample that will automatically be turned into weight.
Figure 89 shows an example of edited sample table referred to the N/Protein instrument
configuration.
Figure 89. N/Protein: Example of Sample Table
Y To Enter the Weight
The sample weights may be manually entry or automatically transferred from the balance to
the PC. These two modes are explained below.
• “Mode 1: Manual Entry of the Weights” on page 130
• “Mode 2: Automatic Entry of the Weights from the Balance to the PC” on page 130

Sample Table
Mode 1: Manual Entry of the Weights

1. Weight the samples and put them sequentially into the autosampler tray.
2. In Main Menu select Edit > Sample Table or just click the icon . The Sample Table
of Figure 89 on page 129 is displayed.
a. Type sample name and weight.
Mode 2: Automatic Entry of the Weights from the Balance to the PC

1. Connect the RS 232 connecting cable between balance and PC.
2. Select Sample Table > Balance > Balance Setup. The following window is displayed:
Figure 90. Balance parameters setting
3. Select the computer serial port to which the balance is connected. Pay attention that the
serial port must be different respect the serial port selected for the analyzer.
4. Select Balance menu.
a. Choose the type of balance in use.
b. Press OK. The dialog window of Figure 90 is displayed again.
c. Press OK to return to Sample Table.
5. In Sample Table select Balance > Receive weight. After you have selected the sample
number desired (e.g. sample number 3), click on Weight. Pressing the down arrow the
following window is visualized:
Figure 91. Weight from balance
6. Put the container on the balance plate. Perform the tare pressing Tare. Introduce the
sample then wait for stabilization.

Sample Table
7. Clicking Weight, the value of the weight is automatically transferred. The sample table is
ready to acquire the value of the next weight.
Note If the balance Mettler Toledo AB54S is used, perform the tare by using the
command located on the balance control panel.
Y To Select the Sample Type
1. In the sample table grid, click on the column Type. Click the arrow shown to display the
window for the sample type selection.
2. According to the sample type, select Bypass, Standard, Unknown or Blank as shown in
Figure 92.
Figure 92. Selection of the sample type
Note Selecting Standard, the following window appears. Set here the desired standard.
Figure 93. Selection of the standard
3. Click OK to confirm and go back to the sample table.
Note New standards may be memorized by clicking Edit Standard Table. After the
number 5, add the standards of interest and the percentages of the relevant elements.
Refer to the following Figure 94.

Sample Table
Figure 94. Edit standard table
Y To Select the Category
To obtain precise and reproducible results the sample must be completely oxidized.
If the major objective of the analysis is to obtain the best precision of results, it is particularly
important that catalysts, and specially Copper, last as long as possible.
Therefore you have to establish how much Oxygen is required to burn a sample of that
particular nature as a function of its weight.
For example, chocolate requires more Oxygen than a soil or an organic substance, though at
equal weight.
We recommend to always use the OxyTune® function (Automatic Oxygen Dosing System).
Selecting, after the weight entry, the category to which the sample belongs, the system will
deliver the right Oxygen quantity required for a complete combustion. This condition is
obtained by a feature provided thanks to the method below. It is important to select the
correct sample category to avoid an incomplete combustion (not enough Oxygen) and the
premature exhaustion of the Copper.
Eight fixed categories can be choose in order to have a correct Oxygen dosage for different
sample matrices. There are:
• Glucose
• EDTA
• Pasta, flours, beans, gluten, cereals
• Starch
• Cocoa
• Ham
• Salame
• Cheese
The selection is performed by clicking the category of interest. For special samples do not
included in the previous categories it is possible to develop a specific category.

Sample Table
Y To Develop a Specific Category
Note This operating sequence gives you a general indication to set the correct category
according to the sample nature.
Flows
Flow 1 and Flow 2 are the flows of Oxygen. Both can assume the following values: 125, 250,
500, 750, 1000, 1250, 1500 mL/min.
• If the sample is rich in fat
In this case the combustion could happen with difficulty with the risk of cracked. To
avoid the cracked it is suggested to set a low flow of Oxygen (125 - 1000 mL/min).
• If the sample is rich in water
In this case the combustion happens more easily. It is suggested to set a low flow of
Oxygen and an high Oxygen Delay time.
Time Ratio
It is the ratio between Time 1 (Flow 1) and Time 2 (Flow 2).
Oxygen Caps
It is the quantity of Oxygen required to oxidize the tin caps. For the 63-mm tin caps it is 0.1
liters.
Oxygen Sample
It is the quantity of Oxygen required to oxidize one gram of sample.
Oxygen Delay
When this time is elapsed, the Oxygen is injected into the circuit.
Purge
It is the duration of the sample purge. It depends on the concentration of nitrogen in the
sample. If the percentage of nitrogen in the sample is lower than 0.5%, it is suggested to set
Trace Purge to 50 s.
Y To Set the Sample Humidity
1. In the Humidity column enter the percentage of humidity present in each sample when
known.

Sequence of Analyses
CAUTION Before shipment, every instrument is submitted to an analytical final test
procedure according to the concerned instrument configuration.
The results of this test are included in the documentation set accompanying the
equipment. When the instrument is used for the first time, before analyzing any unknown
sample, it is advisable to repeat the test maintaining the selection of standards and their
weighing range.
To correctly run the analysis, proceed as described in the following operating sequence.
Y To Perform the Analytical Sequence
How to Perform the Analytical Sequence the First Time

1. Prepare the samples in this order:
• Bypass
It consists of 1000 mg of glucose
• Blank
It consists of 1000 mg of glucose
• Standard
It consists of 500 mg of EDTA
• Unknown 1
500 mg of EDTA
• Unknown 2, 3, 4
1000 mg of Pasta reference material
2. Place the samples in the sample tray in the same order.
3. In the sample table grid, click on the column Type. Click on the arrow displayed and the
following window will appear for the sample type selection.
Figure 95. Sample type selection
4. Select Bypass, then click OK to confirm and go back to the Sample Table.

5. Repeat the step 3 for all the other samples selecting the proper type. Then click OK to
confirm.
6. At the end of Sample Table editing, to automatically stop the sample sequence, select the
number following the last edited sample.
Select Edit sample > Insert line or just click the icon .
7. In Main Menu, select Run > Start sequence of sample.
8. Click Start Now.
At the end of the analytical sequence, the results obtained must be compared with those of the
final test, doing what described in the operating sequence “Comparison Between Analytical Re-
sults and Final Test Results” on page 135.
How to Perform the Analytical Sequence

1. Prepare the samples to analyze. The first sample should be a Bypass consisting of 1000
mg of Pasta reference material. All the other samples will be Unknown.
2. Place the samples in the sample tray.
3. In the Sample Table grid, click on the column Type. Click on the arrow displayed to carry
out the sample type selection.
4. Repeat the step 3 for all the samples. Then click OK to confirm.
5. At the end of the Sample Table editing, to automatically stop the sample sequence, select
the number following the last edited sample.
Select Edit sample > Insert line or just click the icon .
6. In Main Menu, select Run > Start sequence of sample.
7. Click Start Now.
At the end of the analytical sequence, the results obtained must be compared with those of the
final test, doing what described in the operating sequence “Comparison Between Analytical Re-
sults and Final Test Results” on page 135.
Y Comparison Between Analytical Results and Final Test Results
To highlight results, do the following.

1. In Main Menu, select Recalculation > Summarize results or just click the icon . The
following table is displayed.

Figure 96. Example of Summarize Results
2. In the text box Group, enter number 1 for samples 5, 6 and 7.

a. If you want the data printout, select Print > Print single group.
b. If you want to read the statistical result, select one by one samples 6, 7 and 8, then
select View > Statistical calculation. The display will show a window with the
statistical data referring to the selected item.
Interpretation of Results
If the results obtained are satisfactory, go on with your samples sequence. If on the contrary
the results are not correct, try to identify the cause and find the remedy.
Tip It is suggested to see Chapter 7, “Sample Preparation,”
The cause of the error is generally due to incorrect sample weighing. Always observe the
indicated weighing ranges using, if possible, the direct connection between balance and
computer, selecting in the Sample Table the option Receive Weight from Balance in Balance
menu.
Note Should an electronic balance be connected to the instrument, remember to check

the parameters of the connection, selecting in the Sample table the menu Balance and
then the option Balance setup. Refer to “Mode 2: Automatic Entry of the Weights from
the Balance to the PC” on page 130.
3. If the weight of an unknown sample is wrong, the error immediately becomes clear from
its percentage result. On the contrary, if the error is due to the weight of one or more
standards, the three results of the unknown sample will all be wrong.
4. Another cause of error is the incorrect integration of the peak. If it happens, the correction
of the baseline is required proceeding as follows:

a. Open the chromatogram selecting the sample to adjust. In Main Menu choose View
> View Chromatogram > Peak.
b. To modify the baseline, choose the option Move peak start or Move peak end
accordingly.
c. Save the new chromatogram.
d. Recalculate the chromatogram following the instruction in sub-paragraph Sample
Recalculation.
Sample Recalculation
1. In Main Menu select Recalculation > Recalculation. The relevant dialog window is
displayed.
Figure 97. Recalculation (1)
a. In the section Integration options tick the function Identify peaks.

b. In the section Chromatogram source tick the function Sample sequence.
c. In the section Recalculate sample(s) from Sample Sequence set the First Sample
and the Last Sample to recalculate.
d. Click OK.
Evaluation of the Blank Value
The blank value is a function of the type of containers used and of Oxygen purity. Check that
the values found are within acceptable limits versus those reported in the final test certificate.
If the values found are higher, refer to the following Table 24.

Quality Control and Check of Analytical Results
Table 24. Blank values diagnostic guide

Blank Cause and Remedy
Nitrogen If Nitrogen value is definitely higher than that indicated, repeat the blank analysis.
If the area value decreases, it means that the connection tube between Oxygen cylinder
and instrument contains air. To solve this problem disconnect the joint for some time
and let Oxygen flow to the atmosphere.
Should the blank repetition not cause a significant decrease in the area value, it means
that Oxygen used has not a proper purity degree. Use Oxygen of required purity.
IMPORTANT All blank values are memorized and subtracted to the sample values. As a
consequence, definitely high values may affect analytical precision.

Quality control, particularly for food, often requires the daily analysis of the same materials,
specially in Nitrogen-Protein analyses.
Therefore it is important to define the maximum and minimum acceptable values. These
values can be stored and used as comparative parameters for next analyses.
A similar condition occurs if the user has many samples to run for which he knows the
supposed theoretical values. In this case too, we recommend to memorize the maximum and
minimum values to make the comparison between the theoretical and found values easier and
quicker. To use this comparison method, do what described in the following operating
sequence.
Y Method to Compare Results
After having analyzed the standard samples and checked the instrument precision, do the
following:
1. In Main Menu, select Recalculation > Summarize results or just click the icon . The
Summarize result table is displayed. See Figure 96 on page 136.
2. Select Edit > Select reference compounds. A table like the following will appear.
Figure 98. Sample of the reference compound selection
a. In the textbox Name, enter the sample name.

b. In the text box Nitrogen enter the supposed theoretical percentage of the element to
be analyzed.
c. Click OK. For each value a minimum-maximum percent deviation (box +%) versus
the entered value is automatically calculated. The calculation of this deviation is made
by an algorithm, which takes into account the entered percentage and the
instrumental error.
Note If the acceptable error range is wider than that automatically calculated, it
can be manually changed.
Y Comparison Between Found Values and Theoretical Values
At the end of the analytical cycle, to compare the values found with the theoretical ones, do
the following:
1. Go to the table of Figure 99 doing as described in points 1 and 2 of the previous operating
sequence. Select the sample to be compared then click OK. The Summarize Results table
is displayed.
2. Select the sample to be compared as shown in the example of Figure 99.
Figure 99. Summarize Results Table: Comparison of samples (1)
a. Select View > Compare to reference compound. On the left side over the
Summarize Results table, as shown in Figure 100, you will read the name of the
analyzed sample followed by one or more LEDs according to the number of analyzed
elements.
Figure 100. Summarize Results Table: Comparison of samples (2)

Green light = Indicates that the values found are close to the theoretical values and
within the preset error limits.
Red light = Indicates that the values found are far from the theoretical values.
Y Graphic Display of the Result
If a single element is analyzed, the result can be graphically displayed. This is particularly
useful when the sample is routinely analyzed and when it is more important to have the result
within the preset error limits rather than the absolute value found.
To display the graph of the result, do the following:

1. In the Summarize results table, select the group of samples to be displayed.
2. Click the Show summary graph of selected group icon . A window like the following
is displayed.
Figure 101. Summarize graphic (1)
a. Click Componds. In the Compound of reference selection window that appears,

select the sample corresponding to the analyzed one and click OK.
b. A window like the following appears, where a graph is plotted consisting of two
parallel green lines, a white middle line and red small squares.

Middle line = Theoretical value

Green lines = Minimum and maximum acceptable values
Red square = Sample analyzed
c. If the analyzed sample, represented in the graph by a red square, is within the two
green lines, it means that, independently of its absolute value, it has a value close to
the theoretical one and is within acceptable error limits.
The red square, when clicked, becomes white and the percent value is displayed, as
shown in Figure 103.

Post-Analysis Operations
To obtain precise accurate and constant in time results, and at the same time to reduce
operating costs, we recommend you follow some practical suggestions.
Putting the Instrument in Standby Mode

When the work session is over, the instrument should be put in Standby Mode. In this
condition, the temperatures of the Left and Right Furnaces are reduced by 50% versus
operating temperatures, and the Helium flows on both channels are brought to 20 mL/min.
When the instrument goes in Standby Mode, the deactivated adsorption filter is regenerated.
After the regeneration the carrier flows through both adsorption filters and the filter purge is
stopped.
The Standby function can be activated manually or automatically at the end of the analytical
sequence.
Y To Set the Standby Function Manually
Proceed as follows:
1. In Main Menu, select View > View Elemental Analyzer Status or just click the icon .
The page of Figure 104 is displayed.
Figure 104. Status of the analyzer
2. In the section Instrument status click Active button.

Y To Set the Standby Function Automatically
Proceed as follows:
1. In Main Menu, click the icon . The window of Figure 105 is displayed.
Figure 105. Sequence start window (1)
2. In the section Elemental analyzer conditions while start sequence is finished, enable
the Force to Stand-by function by ticking the appropriate check box.
The analyzer will automatically go to the Standby condition, when the last sample has
been analyzed.
Shutting Off Furnaces, Detector and Cutting Off Gas Flows

The shut off of furnaces and detector and the cut off of gas flows can be programmed as
described in the following operating sequence.
Y To Shut Off Temperature, Detector and Gas
1. In Main Menu, just click the icon . The window of Figure 106 is displayed.
Figure 106. Sequence start window (2)

2. In the section Elemental analyzer conditions while start sequence is finished, enable
the function Shut-Off temperature, detector and gas by ticking the appropriate check
box.
3. When the oxidation reactor requires cleaning, the furnace should be switched off and
then the Helium flow reduced using the Stand-by function.
a. In Main Menu, select Edit > Edit Elemental Analyzer parameters or just click the
icon . The window of Figure 107 on is displayed.
Figure 107. Edit elemental analyzer parameters
b. In the section Furnaces, tick the box Left Furnace to enable the Off condition.
c. In the section Other, enable the function Set instrument to Stand-by by ticking the
appropriate check box.
d. Click Send to send the command to the instrument, then click OK.
Wake-up and Auto-Start Functions

These are timed functions, which can be programmed to minimize dead times.
Y To Set Wake-up Function
To pass from Stand-by to Ready status, operate as follows:

1. In Main Menu, select View > View Elemental Analyzer status or just click the icon .
2. Select the Stand-by/Wake-up menu. The window of Figure 108 is displayed.

Figure 108. Status of the analyzer
a. In the section Set Wake-up, set the desired date and time of activation of the
Wake-up function.
b. Click Activate and then OK to confirm.
Auto-Start Function
If you desire Auto-Ready to be followed by Auto-Start, programming an analytical sequence,
do the following:
Y To Set Auto-Start Functions
1. In Main Menu, click the icon . The following window is displayed.
Figure 109. Start sequence

Analytical Troubleshooting
2. Enable the function Enable time programmed sequence start by ticking the appropriate
check box.
a. In the section Starting time click Now.
b. In the Start Date/Time text box enter the date and time of the function activation.
IMPORTANT The function activation should be programmed with a delay of at least
60 minutes versus the time programmed for the Auto-Ready Function to allow the
analyzer to reach a good thermal equilibrium.
Analytical Troubleshooting
If the instrument has been correctly installed, the gas characteristics are as required and
maintenance has been regularly carried out, Flash 4000 will provide correct results.
The lack of the above conditions will be indicated by anomalies in the chromatograms and the
relevant analytical reports. The following table reports the most common anomalies with the
relevant diagnosis and remedy.
Table 25. Analytical troubleshooting guide

Problem Diagnosis Remedy
High Nitrogen blank. Presence of leak. Check that Helium and
Oxygen lines are sealed and
in case eliminate possible
leak.
Oxygen line or cylinder Purge for any minutes.
contaminated. Replace the contaminated
cylinder.
Autosampler not purged. Check that the Helium flow
is correct.
High constant Nitrogen Oxygen cylinder Replace the Oxygen cylinder.
blank in several sequential contaminated.
analyses.
Presence of leak in the Identify leaks and remove
autosampler system. them.
Decreasing Nitrogen blank Oxygen line contaminated. Wait 10-20 minutes for
values. complete purging of the
Oxygen line.
Repeat blank analysis.
Retention times very delayed Presence of leaks in the Perform Leak Test.
respect the normal pneumatic circuit.
chromatogram.
Presence of obstructions in Reach and remove the
the pneumatic circuit. obstruction dissecting the
pneumatic circuit

Part 4
Maintenance and
Troubleshooting
12
Maintenance
This chapter provides information on the current and periodic maintenance of the
instrument, and it also contains the operating sequences for installation and maintenance of
the MAS 4000 autosampler.
Contents
• Instrument Maintenance
• Reactors Replacement
• Replacement of the Gas Chromatographic Column
• Servicing the MAS 4000 Autosampler
WARNING If, for technical reasons, it is necessary to work on parts of the machine that
may involve hazardous operations (moving parts, components under voltage, etc.).
Thermo Fisher Scientific authorized Technical Service has to be called.
This situation can be identified because the access to these moving parts is possible only
using a tool and because the concerned removable protective covers bear a warning symbol
that draws the operator’s attention to the specific warnings included in the documentation
accompanying the instrument. In case the work has to be carried out by the operator, the
latter must prove to be adequately trained to perform the specific maintenance operation.
WARNING When the instrument is switched off, consider that its does not cool down
immediately, but heat tends to concentration in the upper part of the furnaces area. The
openings provided for the chamber aeration will cause a slow cooling of same, which
however, in the vicinity of the areas marked with the symbol “hot surfaces”, might even
reach temperatures higher than ambient temperature. Therefore in the minutes
immediately following the instrument switching off, the operator must consider this risk
and pay adequate attention during any maintenance operations following the use of the
instrument.
Instrument Maintenance
The instrument will be generally serviced by Thermo Fisher Scientific authorized technical
personnel for all the warranty period or, after warranty, possibly according to a Programmed
Service Contract. For more information contact your local Thermo Fisher Scientific office.

12 Maintenance
Reactors Replacement
Current Maintenance
Replacement of crucible, reactors and their filling material.
The instrument configuration uses special steel reactors for combustion it may be necessary
also to clean the crucible done with same material.
• Periodic Maintenance
Replace the o-ring of the reactors coupling unions placed on the furnace compartment
base.
For some maintenance operations, furnaces and oven need to be at room temperature. Follow
the instructions given in paragraph “Shutting Off Furnaces, Detector and Cutting Off Gas
Flows” on page 143.
The replacement of reactors is performed when required by the maintenance program
schedule according to the setting entered in paragraph “Current Maintenance” on page 155.
Replace and install reactors according to the operating sequences described in Chapter 6
“Reactor Preparation and Connections” on page 73.
Replacement of the Filling Materials

The replacement of reactor requires the replacement of their filling materials. This operation
comprises two steps:
1. Removing the exhausted filling material from the reactor.
2. Restoring the sequence of the layers of filling materials using new reagents.
Perform these operations according to the instructions given in the following operating
sequences.
Y To Replace the Filling Material in Special Steel Reactors
Material Required
Tool for cleaning special steel reactors
Filling materials
WARNING Before starting the operation, check that the furnaces are at room
temperature and the gases are turned off.
1. Remove the special steel reactor from the furnace following the instructions given in the
operating sequence “To Remove the Combustion Reactor” on page 85, then do the
following operation.

12 Maintenance
2. Introduce the cleaning tool into the reactor.

3. Rotate the tool exerting a slight pressure to scrape off the filling material.
4. Collect the removed filling material as shown in Figure 12-2.
5. Repeat steps 1 and 2 until complete elimination of the exhausted filling materials.
6. At the end of the operation restore the layers of filling materials introducing into the
reactor the new ones. To do this, refer to paragraphs “Introduction to the Preparation of
Reactors” on page 73 and “Preparing Reactors and Crucible” on page 75.
Y Cleaning the Crucible
WARNING Before starting check that the gases are turned off.
Material Required
Tool for cleaning quartz reactors
Ultra temperature ceramic disks
1. Remove the crucible following the instructions given in the operating sequence “To
Prepare the Crucible” on page 78, then do the following operations:
WARNING The crucible can be removed paying proper attention even when the reactor
is hot. Rest the crucible on a surface resistant to heat and remove ashes only when the
crucible is cold.
2. Introduce the cleaning tool into the crucible.

3. Rotate the cleaning tool exerting a slight pressure in a way to scrape off the filling material
and collect the material removed.
4. At the end of the operation, introduce two new ultra temperature ceramic disks into the
crucible.
Replacement of the O-ring of the Reactors Coupling Unions

To perform this operation, operate as described in the following operating sequence.
Y To Replace of the O-ring of the Reactors Coupling Unions
Material Required
XX-inch wrench
Screwdriver or spatula
Spare seals

12 Maintenance
WARNING Before performing this operation, check that the furnaces are at room
temperature and the gases are turned off.
1. Open the furnaces compartment.

2. Remove the reactors from the furnaces according to the instruction given in the operating
sequence “To Remove the Combustion Reactor” on page 85.
3. Remove the reactors coupling unions from the base, as shown in Figure 110.
Figure 110. Coupling unions removal
4. Disconnect the coupling unions as shown in Figure 111, and rest them on a clean surface.
Figure 111. View of the reactors coupling unions
5. By using a small screwdriver or a spatula, remove the o-ring from each union, as shown in
Figure 112.

12 Maintenance
Replacement of the Gas Chromatographic Column
Figure 112. Removal of the o-ring from the coupling union
6. Put a new o-ring into each union making sure, by using an appropriate tool, it correctly
fits its seat, as shown in Figure 12-10.
Figure 113. Introduction of the o-ring into the coupling union
7. Reconnect the coupling union and remount it in its seat as shown in Figure 114.
Figure 114. Coupling union reinstallation

The instrument rarely requires the gas chromatographic column replacement, however, in
case, operate according to the instructions given in the following operating sequence.
Y To Replace the Gas Chromatographic Column
WARNING Before starting check that the gases are turned off.

12 Maintenance
Material Required
Open end wrenches for the column fittings
1. Access to the side compartment removing the right side panel. The chromatographic
column is located in the low temperature analytical section as shown in Figure 115.
Figure 115. Right side compartments
Chromatographic
column
Low temperature
analytical section
2. By using the wrenches for column fittings, disconnect the inlet and outlet tubings
unscrewing the relative retaining nut, then remove the column from the fixing clips as
shown in Figure 116.
Figure 116. Chromatographic column
Fixing Clips Inlet/Outlet End

Retaining Nuts
3. Fix the new column with the fixing clips, then reconnect the inlet and outlet tubings.
4. Finger-tighten the retaining nuts until them start to grip the column.
5. Use the wrenches to tighten the retaining nuts. Use no more pressure than is necessary to
obtain a good seal (1/4 to 1/2 turn).

12 Maintenance
Servicing the MAS 4000 Autosampler

Current Maintenance
The MAS 4000 autosampler does not normally require maintenance. However, when the
instrument is extensively used, it is a good practice to clean from time to time the piston
housed in the autosampler.
To do this, operate as described in the following operating sequence.
Y Cleaning the Piston of the MAS 4000 Autosampler
This operating sequence provides instructions for the MAS autosampler maintenance.
Material Required
Dry clean cloth
Before starting the reactor must be to room temperature.

1. In the main menu, select Tools > Cleaning the MAS piston. The system automatically
decrease the pressure inside the circuits.
2. Turn up the autosampler front cover.
3. After few minutes the message to remove the piston is displayed.
4. Take out the piston from the autosampler, as shown in Figure 117
5. Eliminate possible traces of dirty from the piston seals using a dry clean cloth.
Figure 117. Removal the piston
Autosampler top Piston

cover

12 Maintenance
Figure 118. Piston of the autosampler
Sample room
O-Rings
Rack
6. Re-introduce the piston into the autosampler until in place keeping its rack turned
downward, as shown in Figure 119.
Figure 119. Re-installing the piston (1)
7. Slightly pushing the piston with one finger, as shown in Figure 120, click Piston
movement again. The autosampler mechanism first tries to eject the piston, then, on the
motor reversal, the mechanism will hook the piston and draw it inside the autosampler.
8. Click Ok.
9. Turn down the autosampler front cover.
Figure 120. Re-installing the piston (2)
10. Return to Analyzer Parameter window. Restore the operating conditions.

13
Troubleshooting
This chapter provides information necessary to find out instrument troubles and to solve
them.
Contents
• Safety Cut Off
• EFC-t Module
Safety Cut Off

Instrument malfunctioning, due to a component failure or to abnormal operating
conditions, is identified by the red lighting of the Safety Cut Off LED indicator.
When lit, this LED indicates that the furnaces and detector oven power has been cut off for
safety reasons.
The Safety Cut Off status is followed by an error message about the possible cause of error.
Y To Display the Error Message
Proceed as follows:
1. In the Main menu select View > View Elemental Analyzer Status or just click the icon
.
2. In the displayed dialog window, select the option Special Functions. The dialog
window of Figure 121 is displayed.
3. Read the error message in the reading box located on the lower right side of the window,
below the buttons Help and OK.
4. Refer to Table 26 to find out the error status and have more information.

13 Troubleshooting
Safety Cut Off
Figure 121. Special function window
1
1. Error Message Reading Box
The following Table 26 reports the error messages and the explanation of the relevant
correlated problem.
Table 26. Error messages

Message Description
safety cut off Voltage supplied to electric circuit is too low. Not
Voltage out limit significant error.
When voltage returns within limits, the instrument
automatically goes back to operating conditions.
safety cut off Furnaces control SSR relay is overheated
SSR thermal protection
safety cut off Right furnace has exceeded the set temperature limit.
out of limit right Temperature has been set with furnace missing
safety cut off Left furnace has exceeded the set temperature limit.
out of limit left
safety cut off The detector oven temperature exceeds the 220 °C.
Oven limit Error may be due to a probe malfunction, etc.
safety cut off The Oxygen pressure supply is too low.

Oxygen pressure too low
safety cut off Error is due to a top trap malfunction.

Top trap fault
safety cut off Error is due to a bottom trap malfunction.

Bottom trap fault

13 Troubleshooting
EFC-t Module
CAUTION The error message is generally due to the specific cause indicated. Sometimes,
it may generated by different electric factors or caused by failures not depending on the
system. In this case contact the Technical Service.
EFC-t Module
The failures that may be generated on the EFCt Module are connected to the breakage or to
the malfunctioning of solenoid valves and flow sensors.
Refer to the Table 27 to find the component responsible of the EFCt module malfunctioning
and to solve the relevant problem.
Table 27. EFC-t module troubleshooting

Failure Defective Component Remedy
Oxygen does not flow to the EV1 Check voltage supply
point 2 of the autosampler Replace the solenoid valve
EV2 Check voltage supply
Replace the solenoid valve
The Helium flow measured on Flow sensor 1 or 2. Replace flow sensor
point 1 or 2 cannot be adjusted
EVP1 or EVP2 Check voltage supply
Replace the solenoid valve
The pneumatic circuit is EV3 and/or EV4 Check voltage supply
perfectly close but the flow value Replace the solenoid valve
don’t decrease up to zero
performing the Leak Test.

13 Troubleshooting
EFC-t Module

A
Customer Communication
Thermo Fisher Scientific provides comprehensive technical assistance worldwide and is
dedicated to the quality of our customer relationships and services.
How to Contact Us
This appendix contains contact information for Thermo Fisher Scientific office. To contact
your local Thermo Fisher Scientific office or affiliate, please refer to:
Voltaweg 22
2627 BC Delft, the Netherlands
Tel: +31 15 257 13 14
Fax: +31 15 257 22 97
This appendix also contains a one-page Reader Survey. Use this survey to give us feedback on
this manual and help us improve the quality of our documentation.

A Customer Communication
Reader Survey
Reader Survey
Product: Flash 4000 Elemental Analyzer
Manual: Operating Manual
Part No.: 317 110 55
Please help us improve the quality of our documentation by completing and returning this
survey. Circle one number for each of the statements below:
Strongly Agree Neutral Disagree Strongly

Agree Disagree
The manual is well organized. 1 2 3 4 5

The manual is clearly written. 1 2 3 4 5
The manual contains all the information I need. 1 2 3 4 5
The instructions are easy to follow. 1 2 3 4 5
The instructions are complete. 1 2 3 4 5
The technical information is easy to understand. 1 2 3 4 5
Examples of operation are clear and useful. 1 2 3 4 5
The figures are helpful. 1 2 3 4 5
I was able to install the system using this manual. 1 2 3 4 5
If you would like to make additional comments, please do. (Attach additional sheets if
necessary).
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
Fax or mail this form to:

Voltaweg 22
2627 BC Delft
The Netherlands
Tel: +31 15 257 13 14
Fax: +31 15 257 22 97

A
Abbreviations ft foot
g gram
GND electrical ground

This section lists and defines terms used in this guide. It
also includes acronyms, metric prefixes, symbols and h height
abbreviations.
h hour
A ampere
H hydrogen
ac alternating current
harmonic distortion A high-frequency disturbance
ADC analog-to-digital converter
that appears as distortion of the fundamental sine
b bit wave
B byte (8 b) He Helium
baud rate data transmission speed in events per second HPAR High Performance Alloy Reactor
C Carbon HV high voltage
°C Celsius Hz hertz (cycles per second)
cm centimeter IEC International Electrotechnical Commission
CPU central processing unit (of a computer) in. inch
CSE Customer Service Engineer I/O input/output
<Ctrl> control key of the keyboard k kilo (103 or 1024)
d depth K Kelvin
DAC digital-to-analog converter kg kilogram
dc direct current kPa kilopascal
DS data system l length
EMC electromagnetic compatibility l liter
ESD electrostatic discharge LAN Local Area Network
ºF Fahrenheit lb pound
FSE Field Service Engineer LED light-emitting diode

Glossary:
m meter (or milli [10-3]) V volt
M mega (106) V ac volts, alternating current
μ micro (10-6) V dc volts, direct current
min minute VGA Video Graphics Array
mL o ml milliliter w width
mm millimeter W Watt
m/z mass-to-charge ratio When a unit of measure has a quotient (e.g. Celsius degrees
per minute or grams per liter) this can be written as
N nitrogen
negative exponent instead of the denominator:
n nano (10-9) For example:
°C min-1 instead of °C/min
O oxygen g L-1 instead of g/L
Ω ohm
p pico (10-12)
Pa pascal
PCB printed circuit board
PN part number
psi pounds per square inch
RAM random access memory
<Return> <Return> key on the keyboard
RF radio frequency
ROM read-only memory
RS-232 industry standard for serial communication
s second
slow average A gradual long-term change in average

RMS voltage level, with typical duration greater than
2 s.
surge A sudden change in average RMS voltage level,

with typical duration between 50 μs and 2 s.
S sulphur
TCD Thermal Conductivity Detector
transient A brief voltage surge of up to several

thousand volts, with a duration of less than 50 μs.

I
Index Communication port 41

Compare Results Method 138
Connections panel 26
Conventions Used xi
Numerics Cooling fan 26
Crucible
32-position sample tray 57
Cleaning 151
Current maintenance 123
A Cutting Off
Adsorption Filters 22 Gas Flows 143
Altitude 15 Cylindrical tool 89
Analytical Configuration 106
Analytical Methods 95 D
Analytical Results
Detection System 34
Check of 138
Detector filaments 34
Comparison 135
Detector Signal
Analytical Sequence 134, 135
Level Adjustment 116
Analytical Troubleshooting 146
Autosampler 21
Autosamplers E
AI 3000/AS 3000 II 42 Eager Xperience
CM2 Manual Sampler 42 Installation Menu 102
MAS 4000 42 Eager Xperience Software 102
Auto-Start Function 144, 145 Installation 102
EFC-t Module 48
B Electrical Compartment 35
Electrical Connections 56
Balance 89
Electrical Requirements 55
Blank Value
Electronic Compartments 22
Evaluation 137
Electronic Flow Controller 45
blank value 123
Elemental Analyzer setup 106
Elemental Analyzer Status 117
C Environmental Conditions 15
Calculation Parameter 124, 127
Calibration 123, 126
F
Calibration Curves 127
View 127 Filling Material
Replacing 150
Calibration methods 126
Capsulator 89 Filter cooling fans carter 32
Filters 45
Category
Develop 133 Filters Compartment 31
Check valve 32 Filters Cooling Vents 31
Chromatographic Column 22 Filters valves manifold 32
Classification 15 Fittings 28

Index: G
FlashEA 4000 MAS 4000 Autosampler 155

Lift 56 Cleaning the Shaft 155
Found Values MAS 4000 autosampler 27
Comparison 139 Maximum relative humidity 15
front cover 28, 28 Modulo EFC 159
front right door 31
Furnaces 21 N
Furnaces Compartment 28
Network Cables 64
Furnaces compartment 25
G O
Oxygen Caps 133
Gas Chromatographic Column
Oxygen Samp 133
Replacing 153
Gas Connection
Fittings 28 P
Gas inlets 39 Pneumatic Circuit 45
Gas Supply 40 Components 47
Pneumatic Compartment 22
I Pneumatic Connections 56
Pollution degree 15
Installation 55, 55
Post-Analysis 142
Instrument
Classification 15 Power On 102
Cleaning 17 Power Supply 38, 39
Configuration 17 Pressure Gauges 47, 47
Safety 17 pressure gauges 25, 45
Sleeping Mode 142 Pressure Regulators 47, 47
Instrument Configuration 106 Pressure regulators 25
Instrument Data System 23
Integration parameters 124 Q
Interface 39, 40
Quality Control 138
IP Address 40, 63
Default 63
R
L Reactors 21
Filling Materials
Laboratory Temperature 56
Replacement 150
LAN Communication Port 63
reactors 45
LAN Option 39, 40 Reactors Coupling Unions 151
LAN Set-up 63
Recalculation 135
Leak Test 116
Reference Compound Selection Table 138
Liquid Samples 89 Results
Low Temperature Analytical Section 32 Graphic Display 140
Low Voltage Electrical Section 33 Interpretation 136
lower door 28 Right Front Compartment 25, 30
Right Side Compartments 32
M Run Analyses 123
Mains Voltage Components 38
Maintenance 124, 149 S
Current 150 Safety Cut Off 157, 157
Default Conditions 125
Safety Cut Off Device 17
Periodic 150
Safety Information 16
set 125
Nominal Pressure of Gases 17
Start-up 124

Index: T
Purity of Gases 16 Water Drain 32, 45, 50

Use of Gases 16 Weight
Sample Manual Entry 130
High Viscosity 90 Weights
Limited Volatility 90 Automatic Entry from the Balance 130
Liquid Phase 90
Sample Table 128, 130
Example 129
Sample table 124
Fill 128
sample table 123
Sample Tray
Installation 58
Sample Type 134
Sample Type Selection 134
Sample Weighing Technique 89
Samples
Comparison 139, 139
Sampling Delay 133
Sequence of Analyses 134
sequence of analyses 123
Sequence Start 146
service contract coverage xi
Shutting Off 143
Detector 143
Furnaces 143
Solenoid Valves Block 50
Solid Samples 89
Standard Outfit 18, 55
Standard Warranty xi
Start-up 101, 119
Status Panel 25, 41
Summarize results 135, 140
T
TCD chamber 32
Technical Features 16
Temperature 15
Theoretical Values
Comparison 139
Thermal Conductivity Detector (TCD) 22, 45
Time Ratio 133
Transients 15
Troubleshooting 157
V
Valves manifold 45
Voltage variations 15
W
Wake-up Function 144, 144
Water Condensate Drainage 50

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Organic Elemental Analysis

P/N 317 110 52, Revision A October 2008 HOME

For Research Use Only

Published by Thermo Fisher Scientific, Voltaweg 22 2627 BC Delft, the Netherlands

First Edition, released October 2008

Chapter 1 Preliminary Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15

Chapter 2 Structure of the Instrument. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21

Thermo Scientific Flash 4000 Elemental Analyzer - Operating Manual iii

Control Section . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .22

Chapter 3 Instrument Description. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25

Chapter 4 Pneumatic Circuit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45

Chapter 5 Analyzer Installation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55

iv Flash 4000 Elemental Analyzer - Operating Manual Thermo Scientific

Sample Tray. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .57

Chapter 6 Reactor Preparation and Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73

Chapter 7 Sample Preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89

Chapter 8 Analytical Methods. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 95

Chapter 9 Instrument Set-up . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 101

Thermo Scientific Flash 4000 Elemental Analyzer - Operating Manual v

Chapter 10 Instrument Start-up . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 119

Chapter 11 Guide to Run Analyses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 123

Part 4 Maintenance and Troubleshooting

Chapter 12 Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 149

Chapter 13 Troubleshooting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 157

Appendix A Customer Communication . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 161

vi Flash 4000 Elemental Analyzer - Operating Manual Thermo Scientific

have been carried out by authorized personnel and if:

Thermo Fisher Scientific

Thermo Scientific Flash 4000 Elemental Analyzer - Operating Manual vii

viii Flash 4000 Elemental Analyzer - Operating Manual Thermo Scientific

The Flash 4000 Elemental Analyzer

This manual is organized as follows:

Thermo Scientific Flash 4000 Elemental Analyzer - Operating Manual ix

Appendix A, “Customer Communication.” contains information for direct contact with

x Flash 4000 Elemental Analyzer - Operating Manual Thermo Scientific

Safety Alerts and Special Notices

The General Warning symbol/sign is a triangle with an exclamation mark that is

This symbol indicates a risk of fire or flammability, or that fire/flammability

This symbol indicates that a biohazard will, could, or may occur.

This symbol indicates the presence of radioactive material.

Thermo Scientific Flash 4000 Elemental Analyzer - Operating Manual xi

Types of Alerts and Signal Words

Note alerts you to important information related to the test.

Instrument Markings and Symbols

Both direct and alternating current

3 Three-phase alternating current

xii Flash 4000 Elemental Analyzer - Operating Manual Thermo Scientific

Earth (ground) terminal

Protective conductor terminal

Frame or chassis terminal

Equipment protected throughout by DOUBLE INSULATION or

Caution, risk of electric shock

In-position of a bistable push control

Out-position of a bistable push control

* Symbol in compliance to the Directive 2002/96/EC on Waste Electrical and

Thermo Scientific Flash 4000 Elemental Analyzer - Operating Manual xiii

Using the Flash 4000 Document Set

Other available manuals are:

xiv Flash 4000 Elemental Analyzer - Operating Manual Thermo Scientific

Classification of the Instrument

Thermo Scientific Flash 4000 Elemental Analyzer - Operating Manual 15

16 Flash 4000 Elemental Analyzer - Operating Manual Thermo Scientific

Nominal Pressure of Gases

Safety Cut Off Device