Organic Elemental Analysis

Flash 2000
Elemental Analyzer
Operating Manual

P/N 31712052, Revision B September 2009 HOME

© 2008 Thermo Fisher Scientific Inc. All rights reserved.

Published by Thermo Fisher Scientific, 19 Mercers Row, Cambridge, CB5 8Bz, United Kingdom
Tel: +44 (0) 1223 347400; Fax: +44 (0) 1223 347403

Trademarks

Flash 2000 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 September 2008

Second Edition, released September 2009

For Research Use Only. Not for use in diagnostic procedures.

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Contents
Declaration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ix

Preface . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . xi
Compliance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . xiii
Safety Alerts and Special Notices . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . xiii
Safety Symbols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . xiii
Types of Alerts and Signal Words. . . . . . . . . . . . . . . . . . . . . . . . . . . . xiv
Special Notices . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . xiv
Instrument Markings and Symbols . . . . . . . . . . . . . . . . . . . . . . . . . . . . xiv
Using the Flash 2000 Document Set . . . . . . . . . . . . . . . . . . . . . . . . . . . xvi

Chapter 1 Preliminary Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13

Classification of the Instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
Environmental Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
Technical Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
Safety Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
Use of Gases. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
Purity of Gases . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
Nominal Pressure of Gases . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
Safety Cut Off Device . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
Instrument Cleaning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
Instrument Configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
Standard Outfit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17

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

The Units Constituting the Instrument . . . . . . . . . . . . . . . . . . . . . . . . . 21
Analytical Section. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
Furnaces. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
Thermal Conductivity Detector (TCD) . . . . . . . . . . . . . . . . . . . . . . . 22
Chromatographic Columns . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
Adsorption Filters. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
Reactors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
Autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
Control Section . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
Pneumatic Compartment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
Electronic Compartment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23

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Automation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .23
Pneumatic Circuit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .23

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

Front Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .26
Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .26
Top Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .27
Furnaces Compartment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .28
Fixing Plates for the Reactors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .29
Fittings for Gas Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .29
Detector Compartment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .30
Description of the Detection System . . . . . . . . . . . . . . . . . . . . . . . . . . . .32
Electrical Compartment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .33
Low Voltage Section . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .33
Main Voltage Section . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .34
Connections Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .35
Interface Section. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .36
Power Supply Section. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .36
Gas Supply Section . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .36
Transformers Compartment. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .37
Devices for the Furnaces Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . .37
Devices Supplying the Furnaces . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .38
Synoptic Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .38
Autosamplers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .40
MAS 200R Autosampler for Solid Samples . . . . . . . . . . . . . . . . . . . . .40
NoBlank Sampling Device . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .40
AI 3000/AS 3000 II Autosampler for Liquid Samples . . . . . . . . . . . . .40
CM2 Manual Sampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .40
Manual Injection Device for Liquids . . . . . . . . . . . . . . . . . . . . . . . . . . . .40

Chapter 4 Pneumatic Circuits . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41

Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .41
Pressure Regulators . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .42
EFC-t Module . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .43
Pneumatic Circuit for CHNS-O and CHN-O Configurations . . . . . . . .44
Pneumatic Circuit for CHN and CHNS Configurations . . . . . . . . . . . . .45
Pneumatic Circuit for O, S and NCS Configurations . . . . . . . . . . . . . . .46
Pneumatic Circuit for NC, NC-Soils, NC-Filters and NC-Sediments
Configurations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .47
Pneumatic Circuit for N, N Lubricant, N/Protein and N-Brew
Configurations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .48
Pneumatic Circuit for NC-IRMS Configuration . . . . . . . . . . . . . . . . . . .49
Pneumatic Circuit for Flash HT Configurations . . . . . . . . . . . . . . . . . . .50
OH Configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .50
NC Configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .51

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Chapter 5 Preparation of Reactors and Adsorption Filters . . . . . . . . . . . . . . . . . . . . . 55

Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .55
Reactors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .55
Adsorption Filters. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .55
Gas Chromatographic Columns. . . . . . . . . . . . . . . . . . . . . . . . . . . . . .56
Filling Materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .56
Introduction to the Preparation of Reactors and Filters . . . . . . . . . . . . . .57
CHN Configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .58
CHN-O Configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .59
CHNS Configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .61
CHNS-O Configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .62
S (Sulfur) Configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .64
O (Oxygen) Configuration. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .65
N (Nitrogen) Configuration. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .66
N Lubricant Configurations. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .67
NC Configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .68
NCS Configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .69
NC-Soils, NC-Sediments, NC-Filters Configurations . . . . . . . . . . . . .70
N/Protein and N-Brew Configurations . . . . . . . . . . . . . . . . . . . . . . . .71
NC Configuration with the Flash IRMS . . . . . . . . . . . . . . . . . . . . . . .72
NC Configuration with the Flash HT . . . . . . . . . . . . . . . . . . . . . . . . .73
Preparing the Reactors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .74
Preparing the Adsorption Filters. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .79

Chapter 6 Connecting Reactors and Adsorption Filters . . . . . . . . . . . . . . . . . . . . . . . . 83

Installing the Reactors into the Furnaces . . . . . . . . . . . . . . . . . . . . . . . . .83
Preliminary Operations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .84
Installing the Adsorption Filters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .90
Preliminary Operations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .91
Removing the Reactors. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .93
Removing the Adsorption Filters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .95

Chapter 7 Preparing the Sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97

Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .97
Homogenizing the Sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .97
Soils, Sediments and Minerals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .98
Carbons . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .98
Metals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .98
Plastics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .99
Vegetal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .99
Liquids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .99
Sample Weighing Technique . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .99
Solid Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .100
Liquid Samples. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .100

Chapter 8 Analytical Methods. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 109

Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .110

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Analytical Method for CHN Configuration . . . . . . . . . . . . . . . . . . . . . .111

Pneumatic Diagram Description . . . . . . . . . . . . . . . . . . . . . . . . . . . .111
Sequence of the Method Stages . . . . . . . . . . . . . . . . . . . . . . . . . . . . .112
Analytical Method for CHN-O Configuration . . . . . . . . . . . . . . . . . . .113
Pneumatic Diagram Description . . . . . . . . . . . . . . . . . . . . . . . . . . . .113
Sequence of the Method Stages . . . . . . . . . . . . . . . . . . . . . . . . . . . . .114
Analytical Method for CHNS Configuration . . . . . . . . . . . . . . . . . . . . .115
Pneumatic Diagram Description . . . . . . . . . . . . . . . . . . . . . . . . . . . .115
Sequence of the Method Stages . . . . . . . . . . . . . . . . . . . . . . . . . . . . .116
Analytical Method for CHNS-O Configuration . . . . . . . . . . . . . . . . . .117
Pneumatic Diagram Description . . . . . . . . . . . . . . . . . . . . . . . . . . . .117
Sequence of the Method Stages . . . . . . . . . . . . . . . . . . . . . . . . . . . . .118
Analytical Method for S (Sulfur) Configuration . . . . . . . . . . . . . . . . . . .119
Pneumatic Diagram Description . . . . . . . . . . . . . . . . . . . . . . . . . . . .119
Sequence of the Method Stages . . . . . . . . . . . . . . . . . . . . . . . . . . . . .120
Analytical Method for O (Oxygen) Configuration . . . . . . . . . . . . . . . . .121
Pneumatic Diagram Description . . . . . . . . . . . . . . . . . . . . . . . . . . . .121
Sequence of the Method Stages . . . . . . . . . . . . . . . . . . . . . . . . . . . . .122
Analytical Method for N (Nitrogen) Configuration . . . . . . . . . . . . . . . .123
Pneumatic Diagram Description . . . . . . . . . . . . . . . . . . . . . . . . . . . .123
Sequence of the Method Stages . . . . . . . . . . . . . . . . . . . . . . . . . . . . .124
Analytical Method for NC Configuration . . . . . . . . . . . . . . . . . . . . . . .125
Pneumatic Diagram Description . . . . . . . . . . . . . . . . . . . . . . . . . . . .125
Sequence of the Method Stages . . . . . . . . . . . . . . . . . . . . . . . . . . . . .126
Analytical Method for NCS Configuration . . . . . . . . . . . . . . . . . . . . . .127
Pneumatic Diagram Description . . . . . . . . . . . . . . . . . . . . . . . . . . . .127
Sequence of the Method Stages . . . . . . . . . . . . . . . . . . . . . . . . . . . . .128
Analytical Method for NC-Soils, NC-Sediments and NC-Filters
Configurations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .129
Pneumatic Diagram Description . . . . . . . . . . . . . . . . . . . . . . . . . . . .129
Sequence of the Method Stages . . . . . . . . . . . . . . . . . . . . . . . . . . . . .130
Analytical Method for N Lubricant, N/Protein and N-Brew
Configurations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .131
Pneumatic Diagram Description . . . . . . . . . . . . . . . . . . . . . . . . . . . .131
Sequence of the Method Stages . . . . . . . . . . . . . . . . . . . . . . . . . . . . .132
Analytical Method for NC-IRMS Configuration . . . . . . . . . . . . . . . . . .133
Pneumatic Diagram Description . . . . . . . . . . . . . . . . . . . . . . . . . . . .133
Sequence of the Method Stages . . . . . . . . . . . . . . . . . . . . . . . . . . . . .134
Analytical Method for NC-HT Configuration . . . . . . . . . . . . . . . . . . . .135
Pneumatic Diagram Description . . . . . . . . . . . . . . . . . . . . . . . . . . . .135
Sequence of the Method Stages . . . . . . . . . . . . . . . . . . . . . . . . . . . . .136

Chapter 9 Instrument Start-up . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 139

Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .139
Powering on the System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .139
Installation of Eager Xperience. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .140
Eager Xperience Main Menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .141
Analytical Configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .144
Leak Test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .146

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Detector Signal Level . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .148

Chapter 10 Guide to Run Analyses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 151

Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .151
Directory for Analyses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .152
Current Maintenance Program. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .152
Instrument Calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .154
Sample Table . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .156
Determination of the Blank Value . . . . . . . . . . . . . . . . . . . . . . . . . . . . .159
Evaluation of the Blank Value . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .162
Sequence of Analyses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .163
Quality Control and Check of Analytical Results . . . . . . . . . . . . . . . . . .168
Post-Analysis Operations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .172
Putting the Instrument in Standby Mode. . . . . . . . . . . . . . . . . . . . . .172
Shutting Off Furnaces, Detector and Cutting Off Gas Flows . . . . . . .173
Wake-up and Auto-Start Functions . . . . . . . . . . . . . . . . . . . . . . . . . .174
Auto-Start Function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .175
Analytical Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .176

Chapter 11 Applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 179

Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .179
Sample Oxidation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .179
Choosing the Weighing Range. . . . . . . . . . . . . . . . . . . . . . . . . . . . . .181
Automatic Oxygen Dosage. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .182

Chapter 12 Use of Eager Simplified User Interface. . . . . . . . . . . . . . . . . . . . . . . . . . . . 185

Simplified User Interface . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .185

Chapter 13 Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 191

Instrument Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .191
Current Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .192
Periodic Maintenance. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .192
Replacing Reactors and Adsorption Filters . . . . . . . . . . . . . . . . . . . .192
Replacement of the Filling Materials . . . . . . . . . . . . . . . . . . . . . . . . .192
Replacement of the Gas Chromatographic Column . . . . . . . . . . . . . .196
Replacement of the O-Rings of the Reactors Coupling Unions . . . . .198
Installing and Servicing the MAS 200R Autosampler. . . . . . . . . . . . . . .200
Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .200
Installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .200
Switching Box . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .201
The Sample Tray . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .201
Current Maintenance of the MAS 200 R Autosampler. . . . . . . . . . . .203
Installing and Servicing the CM2 Manual Sampler . . . . . . . . . . . . . . . .206
Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .206
Installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .206
Current Maintenance of the CM2 Sampler . . . . . . . . . . . . . . . . . . . .207

Chapter 14 Troubleshooting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 209

Safety Cut Off . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .209

Thermo Scientific Flash 2000 Elemental Analyzer - Operating Manual vii

Contents

EFC-t Module . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .211

Appendix A Customer Communication . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 213

How to Contact Us . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .213
Reader Survey . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .214

Abbreviations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 215

Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 217

viii Flash 2000 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

19 Mercers Row
Cambridge
CB5 8BZ
United Kingdom

Thermo Scientific Flash 2000 Elemental Analyzer - Operating Manual ix

3

x Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific

 P

Preface
This Operating Manual contains descriptions of the features and components of the Flash
2000 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 2000 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 instruments and its
major features.

Chapter 3, “Instrument Description,” , gives you a detailed description of the instrument

components.

Chapter 4, “Pneumatic Circuits,” , describes the pneumatic circuit of each instrument

configuration in the pre-run condition.

Thermo Scientific Flash 2000 Elemental Analyzer - Operating Manual xi

Preface

Part 2, “Preparation,” , provides description of the reactors and adsorption filters required to
run analyses with instructions for their preparation, and also description of gas
chromatographic columns. Moreover it contains instructions to install and remove the system
reactors and filters, to perform sample preparation and weighing, and also how to start up the
instrument before running analyses.

Chapter 5, “Preparation of Reactors and Adsorption Filters,” , provides instructions for the
preparation of the reactors and the adsorption filters, and it also reports the types of analytical
columns currently used.

Chapter 6, “Connecting Reactors and Adsorption Filters,” , contains the instructions to install
reactors and adsorption filters into the elemental analyzer, and it also provides information on
how to remove them.

Chapter 7, “Preparing the Sample,” , describes some techniques for the sample preparation,
also it provides basic instructions to homogenize and weigh the sample.

Chapter 8, “Analytical Methods,” , describes the analytical methods used for all configurations
of the Flash 2000 elemental analyzer.

Part 3, “Analysis,” , contains information and operating sequences to perform the analysis
preparation, execution and interpretation.

Chapter 9, “Instrument Start-up,” , contains information and operating procedures to prepare

the instrument for running analyses.

Chapter 10, “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.

Chapter 11, “Applications,” , contains guidelines referring to the applications of the Flash
2000 elemental analyzer.

Chapter 12, “Use of Eager Simplified User Interface,” , provides information about the use of
the “easy” version of the Eager 300 software.

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 13, “Maintenance,” , 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 200 R Autosampler and the CM2 Manual Sampler.

Chapter 14, “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.

xii Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific

 Preface

The Index contains an alphabetical list of key terms and topics in this guide, including cross
references and the corresponding page numbers.

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 2000 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.

Thermo Scientific Flash 2000 Elemental Analyzer - Operating Manual xiii

Preface

This symbol indicates that chemical damage or physical injury will, could, or
may occur.

This symbol indicates the presence of radioactive material.

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 2000. See the asterisk.

Symbol Description

Direct Current

*
Alternating Current

xiv Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific

 Preface

Symbol Description

Both direct and alternating current

3 Three-phase alternating current

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

Thermo Scientific Flash 2000 Elemental Analyzer - Operating Manual xv

Preface

Symbol Description
* 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.

Using the Flash 2000 Document Set

The Flash 2000 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 2000 Document Set (PN 317 120 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 317 120 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 317 120 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 2000.

Other available manuals are:

• Eager Xperience Software 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.
• Flash HT Elemental Analyzer User Guide (PN 317 082 71)
This guide is an additional section of the Flash 2000 Operating Manual containing the
instruction to operate on the Flash HT Elemental Analyzer.

xvi Flash 2000 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 30% and 85%.
• 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 2000 Elemental Analyzer - Operating Manual 13

1 Preliminary Information
Technical Features

Technical Features
The following table summarizes the major technical features of the Flash 2000 elemental
analyzer.
Table 1. Technical features of the instrument
Features Description
Instrument configurations Fourteen
Detector Thermal conductivity detector (TCD)
External interface RS 232 serial line
Instrument control Eager Xperience for Windows™
Power supply 230 Vac; 50/60 Hz; 1400 VA
Dimensions (cm) Height 50 (54 with fittings); Width 59, Depth 58
Mass (kg) 65

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 2000. 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 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.

Purity of Gases
The Flash 2000 uses Helium and Oxygen with 99.995% minimum purity.

14 Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific

 1 Preliminary Information
Safety Cut Off Device

Nominal Pressure of Gases

The nominal pressure of the gases to supply the Flash 2000, as indicated on the instrument rear
panel, are:
• Maximum 250 kPa (2.5 bar) for He
• Maximum 250-300 kPa (2.5-3 bar) for O2 according to the analytical configuration

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 14, “Troubleshooting,”

Instrument Cleaning
 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 2000 elemental analyzer is available in fourteen different versions. Analytical
techniques, pneumatic circuits and standard outfits are different for each version.

Table 2. Flash 2000 Series: Instrument versions

Configuration Description
CHN Analyzer For the determination of the amount (%) of carbon, hydrogen
and nitrogen, contained in organic and inorganic chemical
products and in substances of different nature and origin, be they
solid, liquid or gaseous samples.

Thermo Scientific Flash 2000 Elemental Analyzer - Operating Manual 15

1 Preliminary Information
Instrument Configuration

Table 2. Flash 2000 Series: Instrument versions, continued

Configuration Description
CHN-O Analyzer For the determination of the amount (%) of carbon, hydrogen,
nitrogen and determination of oxygen, contained in organic and
inorganic chemicals and in substances of different nature and
origin, be they solid, liquid or gaseous samples.

The determination of carbon, hydrogen and nitrogen is performed in

a single sample analysis, whereas oxygen determination is performed
separately.
CHNS Analyzer For the simultaneous determination of the amount (%) of carbon,
hydrogen, nitrogen and sulfur, contained in organic and inorganic
chemical products and in substances of different nature and
origin, be they solid, liquid or gaseous samples.
CHNS-O Analyzer For the determination of the amount (%) of carbon, hydrogen,
nitrogen, sulfur and determination of oxygen, contained in
organic and inorganic chemical products and in substances of
different nature and origin, be they solid, liquid or gaseous
samples.

The determination of carbon, hydrogen, nitrogen and sulfur is

performed in a single sample analysis, whereas oxygen determination
is performed separately.
S Analyzer For the determination of the amount (%) of sulfur contained in
organic and inorganic chemical products and in substances of
different nature and origin, be they solid, liquid or gaseous
samples.
O Analyzer For the determination of the amount (%) of oxygen contained in
organic and inorganic chemical products and in substances of
different nature and origin, be they solid, liquid or gaseous
samples.
N Analyzer For the determination of the total amount of nitrogen present in
organic and inorganic chemical products and in substances of
different nature and origin, be they solid, liquid or gaseous
samples.
N Lubricant Analyzer For the determination of the total amount of nitrogen present in
lubricants, lubricant additives, fuel additives, petrochemical
products.

16 Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific

 1 Preliminary Information
Standard Outfit

Table 2. Flash 2000 Series: Instrument versions, continued

Configuration Description
NC Analyzer For the determination of the amount (%) of nitrogen and carbon
contained in materials of different kinds:

• Synthetic materials: polymers, rubbers, tyres, etc.

• Explosives: nitrocellulose, TNT, gun powder, etc.
• Special materials: carbon fibers, glass fibers, conductive
polymers, graphite, etc.
• Metallurgy: metal powders, steels, etc.
• Environmental analyses: muds, discards, organic wastes, etc.
NCS Analyzer For the simultaneous determination of the amount (%) of
nitrogen, carbon and sulfur contained in organic and inorganic
chemical products and in substances of different nature and
origin, be they solid, liquid or gaseous samples.
NC-Soils Analyzer For the determination of the nitrogen and carbon content in soil
samples.
NC-Sediments Analyzer For the determination of the nitrogen and carbon content in
sediments.
NC-Filters Analyzer For the determination of the nitrogen and carbon content in
particulate samples filtered on Whatman filters.
N/Protein Analyzer For the determination of the nitrogen and protein amount in
products of biological origin; it can also be used in determining
nitrogen content in samples of different nature, generally
agricultural products and foodstuff.
N-Brew Analyzer For the determination of nitrogen content in samples of different
nature, belonging to the brewing industry, such as malt, barley,
wort and beers.
NC-IRMS Analyzer 1 Flash 2000 analyzer able to be coupled to an Isotopic Ratio Mass
Spectrometer (IRMS).for the determination of Nitrogen and
Carbon.
Flash 2000 HT analyzer Flash 2000 analyzer with the left furnace at high temperature
1 (1450 °C) for the determination of Oxygen and Hydrogen by
pyrolysis and with the right furnace at 1000 °C for the
determination of Nitrogen and Carbon (or Sulfur).
1.For detains about these configurations refer to the Flash 2000 HT User

Standard Outfit
Flash 2000 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.

Thermo Scientific Flash 2000 Elemental Analyzer - Operating Manual 17

1 Preliminary Information
Standard Outfit

18 Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific

 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
• Pneumatic Circuit

The Units Constituting the Instrument

The instrument, in its different configurations, consists in a single structure subdivided into
two sections:
• Analytical Section
• Control Section

Analytical Section
It comprises the following major components:

Furnaces
Each furnace consists of a 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.
• Furnace Cooling
The cooling time varies according to the operating temperature setting.

The Flash 2000 analyzer can be equipped with one or two furnaces according to the
instrument configuration.

Thermo Scientific Flash 2000 Elemental Analyzer - Operating Manual 21

2 Structure of the Instrument
Control Section

• LEFT Furnace
Present in all configurations.
• RIGHT Furnace
Present only when required by the instrument configuration.

Thermal Conductivity Detector (TCD)

It is located in a thermostatic chamber at controlled programmable temperature. This
chamber also accommodates the analytical column.

Chromatographic Columns
The chromatographic column performs the chromatographic separation of the reaction
products generated during the combustion or pyrolysis process.

The column can be kept at room temperature, or it can be placed in the thermostatic chamber
of the TCD detector according to the instrument configuration.

The CHNS-O and CHN-O instrument versions use two analytical columns placed inside the
thermostatic chamber.

Adsorption Filters
They can be made of glass or Plexiglas according to the analytical configuration. Refer to
Chapter 5, “Preparation of Reactors and Adsorption Filters,” .

Reactors
These are tubes made of quartz or special alloy filled with different materials according to the
analytical configuration. Refer to Chapter 5, “Preparation of Reactors and Adsorption Filters,”
.

Autosampler
It performs the automatic injection into the reactor of samples.

Control Section
The control section consists of two major components:

Pneumatic Compartment
It consists of two pressure reducers, two pressure gauges and of 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 Circuits,” .

22 Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific

 2 Structure of the Instrument
Automation

Electronic Compartment
It comprises the electronic boards for the instrument power supply and control.

Automation
The instrument is fully controlled by the computer through Eager Xperience 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 is a synoptic panel where you can monitor the
instrument statuses.

Eager Xperience is 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
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

Pneumatic Circuit
Each configuration of the Flash 2000 elemental analyzer has its own dedicated pneumatic
circuit. For details, please refer to Chapter 4, “Pneumatic Circuits,” .

Thermo Scientific Flash 2000 Elemental Analyzer - Operating Manual 23

2 Structure of the Instrument
Pneumatic Circuit

24 Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific

 3

Instrument Description
This chapter gives you a detailed description of the instrument components.

Contents
• Front Panel
• Rear Panel
• Top Panel
• Furnaces Compartment
• Fixing Plates for the Reactors
• Fittings for Gas Connections
• Detector Compartment
• Description of the Detection System
• Electrical Compartment
• Connections Panel
• Transformers Compartment
• Synoptic Panel
• Autosamplers
• Manual Injection Device for Liquids

Thermo Scientific Flash 2000 Elemental Analyzer - Operating Manual 25

3 Instrument Description
Front Panel

Front Panel
It comprises:
• Furnaces compartment
Also refer to paragraph “Furnaces Compartment” on page 28.
• Synoptic panel
Also refer to paragraph “Synoptic Panel” on page 38.
• Compartment for the TCD detector thermostatic chamber and for the gas
chromatographic column.
Refer to paragraph “Detector Compartment” on page 30.

Figure 1. Instrument front panel

Synoptic panel

Access to the thermostatic

chamber

Access to the furnaces

Rear Panel
It comprises:
• Panel for connections including:
− interface section
− gas inlet section
− electrical section
Also refer to paragraph “Connections Panel” on page 35.
• Cooling fan
• Transformers compartment
Also refer to paragraph “Transformers Compartment” on page 37.

26 Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific

 3 Instrument Description
Top Panel

Figure 2. Instrument rear panel

Cooling fan

Connection panel

Transformer compartment panel

Top Panel
It comprises:
• Fittings for mounting and securing the furnaces reactors
• Fittings for gas connection.

Also refer to paragraph “Fixing Plates for the Reactors” on page 29

Figure 3. Instrument top panel

Autosampler

Fittings for reactors

Gas connections

Thermo Scientific Flash 2000 Elemental Analyzer - Operating Manual 27

3 Instrument Description
Furnaces Compartment

Furnaces Compartment
The furnaces compartment can be reached from the instrument front and removing (lifting)
the cover. The furnaces are accessible by removing the protecting plate.

Figure 4. Furnace compartment with protecting plate

Plate protecting
the furnace
compartment

WARNING Do not open the furnaces compartment during operation because very high
temperatures are reached.

The protecting plate can be removed only when the furnaces temperature shown is near
the room temperature.

Figure 5. Furnaces compartment

Left furnace Right furnace

28 Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific

 3 Instrument Description
Fixing Plates for the Reactors

The furnaces can reach the following maximum temperatures:

• LEFT Furnace: 1100 °C (1500 °C for HT)
• RIGHT Furnace: 1100 °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.

Fixing Plates for the Reactors

These plates, on top of the furnaces compartment, accommodate the following components:
• Connections and fittings for the reactors.
• Automatic or manual sampler.

Figure 6. Fixing Plates for the Reactors

Fixing plate

Fittings for Gas Connections

They are located on the middle bottom part of the instrument rear panel. Gas inlet ports are
directly connected to the pressure regulators.

Figure 7. Gas connection ports

Gas inlet port

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3 Instrument Description
Detector Compartment

Table 4. Gas Inlet Ports and Pressure Setting

Port Description Pressure value to be set
He Inlet port for Helium 250 kPa (2.5 bar)
O2 Inlet port for Oxygen 250-300 kPa (2.5-3 bar) according to
the instrument configuration

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

Detector Compartment
It is located on the right front part of the instrument and can be reached by opening the door.
Figure 8 shows the inside of the detector compartment.

Figure 8. View of the detector compartment

Gauges

Adsorption filters
Protecting plate

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 3 Instrument Description
Detector Compartment

The detector compartment houses the pressure regulators, the gauges and the thermal
conductivity detector (TCD), located behind the protecting plate and the gas
chromatographic column. Refer to “Access to the Detector” on page 31. The adsorption filters
are housed in this compartment.

Note One or two adsorption filters may be required, according to the instrument
configuration.

 Access to the Detector

1. Open the right side door to have access to the thermostatic chamber,
2. To reach the detector, remove the adsorption filters from the fastening clips.
3. Undo the four fixing screws on the protecting plate.

Figure 9. Access to the detector

Fixing screws

adsorption filters Protecting plate

Fixing screws

Figure 10 shows the detector compartment, the heating block surrounding the detector, and
the gas chromatographic column.

Note One or two analytical columns may be required, according to the instrument
configuration.

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3 Instrument Description
Description of the Detection System

Figure 10. TCD detector compartment

Heating block

TCD detector

Chromatographic
column

Description of the Detection System

It 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.
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 5 V constant voltage and are electrically protected if
their temperature exceeds 220 °C (Safety Cut Off )

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 3 Instrument Description
Electrical Compartment

Electrical Compartment
It is located on the right part of the instrument, and it is accessible by removing the right side
cover. Behind the electrical compartment, there is the Connections Panel (for more details,
refer to the relevant paragraph, page 35).

CAUTION Before opening the electrical compartment, cut off power supply to the
instrument and disconnect the power cord.

The electrical compartment, shown in Figure 11, comprises:

• Low voltage section
• Mains voltage section
• EFC electronic flow controller for gas regulation

Figure 11. Electrical compartment internal view

Low Voltage Section

It contains the electronic boards to operate and control the instrument. These boards (in
double EUROCARD format, except the EV Control Box and FP1112 boards) are interlocked
through a mother board.

Function of the Electronic Boards

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

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3 Instrument Description
Electrical Compartment

Table 6. Description of the Function of the Electronic Boards

Board Function
MB 1112 Mother board. It provides interlocking between low voltage boards
and with the rest of the instrument.

This board can be connected to a NiCd 3,6 V; 280 mA/h

rechargeable battery located nearby.

The rechargeable battery replacement must be performed by specialized

technical personnel
CPU 1112 This board has full control of the instrument operation.
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.
EV Control Box Receives voltage supply from the TRF 1112 board. It operates the gas
controlling solenoid valves contained in the EFC flow controller.

The board is provided with a T0,16A 127/III (5 x 20 mm) protection

fuse.
HWD 1112 Provides power supply to the HWD detector filaments.

Allows the detector oven thermoregulation and also amplifies and

converts the detector signal to send it to the PC.
TCR 1112 Operates and controls the furnaces thermoregulation.
PWR 1112 Receives voltage supplies from the TRF 1112 transformers board.

It generates voltage supply for the electronic control circuits.

FP 1112 Synoptic panel

Main Voltage Section

It contains the mains power circuits and the Safety Cut Off device.

The following Table 7 reports the function of each component present in the mains voltage
section.

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 3 Instrument Description
Connections Panel

Description
Table 7. Description of the components of the Main voltage section
Component Description
TRF 1112 Transformers Receives the mains power and supplies it to the following devices:
Board
• Cooling fan
• Furnaces transformers
• Heater of the detector thermostatic chamber

Six fuses are provided on the board. See Table 8.

AC 1112 Furnaces Supplies 48 Vac power to the furnaces. It contains the SSR relays
Power Supply for the furnaces control.

Also refer to paragraph “Devices for the Furnaces Control” on

page 37.

Two fuses are provided on the board. See Table 8.

Breaker Instrument ON/OFF main switch.

Table 8. Fuses of the High voltage section

Board Fuse Type Protection
TRF 1112 F1 F1A; IEC 127/I (5 x 20 mm) Power supply to LEFT and
RIGHT furnaces transformers
F2 F0.315A; IEC 127/I (5 x 20 mm) Fan
F3 F1.6A; IEC 127/I (5 x 20 mm) Main power (Breaker)
F4 F1A; IEC 127/I (5 x 20 mm) LEFT and RIGHT furnaces
transformers
F5 F0.315A; IEC 127/I (5 x 20 mm) Fan
F6 F1,6A; IEC 127/I (5 x 20 mm) Mains power (Breaker)
AC 1112 F1 FF12 A; IEC 269 (1.3 x 38 mm) LEFT Furnace power circuit
F2 FF12 A; IEC 269(1.3 x 38 mm) RIGHT Furnace power circuit

Connections Panel
The panel, shown in Figure 12, is subdivided into three sections:
• interface
• power supply
• gas inlets

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3 Instrument Description
Connections Panel

Figure 12. View of the Connections Panel

Interface Section

Power supply Gas inlets

Interface Section
It comprises:
• 9-pin connector marked RS 232 to dialog with the computer via serial line.
• 25-pin connector marked AUX CONNECTOR for the autosampler for liquids if
required.
• 2-pin connector marked Autosampler for the MAS 200R autosampler for solids.

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 connector.

Gas Supply Section

It comprises the gas inlet ports. Refer to paragraph “Fittings for Gas Connections” on page 29.

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 3 Instrument Description
Transformers Compartment

Transformers Compartment
Located in the right bottom part of the instrument, it is accessible from the rear panel by
removing the relevant cover.

It contains the electrical devices to power the furnaces and control their temperature.

CAUTION Before opening the compartment, switch the instrument off and disconnect
the power cord.

Figure 13 shows the devices contained in this compartment.

Figure 13. Transformer compartment internal view

Devices for the Furnaces Control

The following Table 9 describes the function of each device:

Table 9. Description of the Devices Controlling the Furnaces

Device Function
LTA-1 LEFT They read the values of the thermocouple present in the relevant furnace
LTA-1 RIGHT and send the signals to the TCR 1112 board.

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3 Instrument Description
Synoptic Panel

Table 9. Description of the Devices Controlling the Furnaces, continued

Device Function
SSR LEFT Solid state relays contained in the AC 1112 board.
SSR RIGHT Each SSR is 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.

Devices Supplying the Furnaces

The following Table 10 reports the function of each device:

Table 10. Description of the Devices Supplying the Furnaces

Device Function
T1 Transformer Supplies 48V voltage to the right furnace resistor. It is provided with a
safety thermal protection, which cuts off power in case of overheating
and then displays an error message.
T2 Transformer Supplies 48V voltage to the left furnace resistor. It is provided with a
safety thermal protection, which cuts off power in case of overheating
and then displays an error message.

Synoptic Panel
This panel shows the instrument operating conditions, and it is located on the right side of the
instrument front panel.
Each synoptic is provided with a LED, which lights up when the relevant function is active.

Figure 14. Synoptic panel

The following Table 11 illustrates the meaning of each synoptic:

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 3 Instrument Description
Synoptic Panel

Table 11. Description of the synoptic

Synoptic LED Meaning
Power On When lit, the instrument is powered.

Ready When lit, the instrument is ready to run analyses.

Run When lit, an analysis is in progress.

Stand By When lit, the instrument is in stand-by condition.

During this condition, gas flows are decreased to
10 ml/min, and the furnaces temperature is
reduced to 50% of the set value.

Wake Up When lit, the instrument has been programmed

for a timed automatic startup (Ready Condition).

Furnace On Two LEDs are provided, one for each furnace.

When one is lit, the relevant furnace is powered.

Oven On When lit, the detector oven is powered.

TCD When lit, the detector filaments are powered.

Safety Cut Off It lights up when an alarm condition occurs.

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3 Instrument Description
Autosamplers

Autosamplers
The Flash 2000elemental analyzer can be configured with the following autosamplers:

MAS 200R Autosampler for Solid Samples

It is mounted directly on the connecting fitting of the concerned reaction tube.
It consists of:
• Anodized aluminium block provided on the left with fittings for carrier gas and purge gas
lines connection.
• 32-position sample-holding tray.
Up to 4 optional trays are available to accommodate 125 samples.

Note When the analyzer is equipped with two MAS 200R autosamplers, it is possible to
switch from a channel to the other by using a dedicated Switching Box. See “To Install the
MAS 200R Autosampler on the Flash 2000” on page 200.

NoBlank Sampling Device

This device, interposed between MAS 200R autosampler and Flash 2000 instrument, reduces
the Nitrogen blank value due to the sampler movement.
The device is particularly suggested for Flash 2000 configuration coupled to IRMS
instrument.

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) or 105-position (AS 3000) sample tray

CM2 Manual Sampler

It is mounted directly on the connecting fitting of the concerned reaction tube. It consists of:
• Base block provided with a hole for the manual introduction of samples.

Manual Injection Device for Liquids

It allows the direct injection of a liquid sample into the reactor using a syringe.

40 Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific

 4

Pneumatic Circuits
This chapter describes the pneumatic circuit of each instrument configuration in the pre-run
condition.

Contents
• Introduction
• Pressure Regulators
• EFC-t Module
• Pneumatic Circuit for CHNS-O and CHN-O Configurations
• Pneumatic Circuit for CHN and CHNS Configurations
• Pneumatic Circuit for O, S and NCS Configurations
• Pneumatic Circuit for NC, NC-Soils, NC-Filters and NC-Sediments
Configurations
• Pneumatic Circuit for N, N Lubricant, N/Protein and N-Brew
Configurations
• Pneumatic Circuit for NC-IRMS Configuration
• Pneumatic Circuit for Flash HT Configurations

Introduction
Each of the instrument configurations of the Flash 2000 Elemental Analyzer works with a
different analytical technique, and therefore has a different pneumatic circuit.
All pneumatic circuits have the following common components:
• The EFC Electronic Flow Controller for gases.
• Inlet gases pressure regulators and relevant gauges.
• The TCD Thermal Conductivity Detector.

According to each analytical configuration, the pneumatic circuit can comprise:

• One or two reactors.
• One or two gas chromatographic columns.

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4 Pneumatic Circuits
Pressure Regulators

• One or two adsorption filters or none.

The filling of reactors and absorbent filters, and the type of analytical columns vary according
to the instrument configuration. For more details refer to Chapter 7, “Preparing the Sample,”
IMPORTANT All the pneumatic circuits described in this chapter are represented in the
PreRun condition.

Pressure Regulators
Pressure regulators, located in the detector compartment and schematically shown in
Figure 15, allow the manual adjustment of the Helium and Oxygen inlet pressure.

Figure 15. Pressure Regulators

O2 He

PI2 PI1

PRV2 PRV1

O2 He

Pressure regulators are common to all analyzers. They consist of the following components.
See Figure 12:

Table 12. Pressure regulators

Component Description and function
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

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 4 Pneumatic Circuits
EFC-t Module

EFC-t Module
The EFC-t module, schematically shown in Figure 16 is common to all analyzers. It consists
of the following components. See Table 13.

Figure 16. Thermoregulated EFC-t module

EVP2 1
S2 F

(5)
2
S2 S1
F
F
(6)
EV1 2 1 4 He

(7) F
3 1
6,5 cc/min. 6 7 5 O2 2
300 kPa
EV3 1 EV4 1
3 1
EV4 EV3 EVP2 EV2 EVP1
2 2
EV2 2 EV1
(4)
S1

EVP1 1
(1)

2
(2)
O2 He

Table 13. Parts of the EFC-t module

Component Description
He Inlet port for Helium.
O2 Inlet port for Oxygen.
EV1 Two-way solenoid valve to control Oxygen inlet.
EV2 Three-way solenoid valve to control Helium inlet and to allow switching
between Helium and Oxygen.
EV3 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.
EV4 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 200R 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 EVP1 electronic controller
(proportional valve).
S2 Electronic flow sensor for Helium as reference gas. It cooperates with the
EVP2 electronic controller (proportional valve).
EVP1 Electronic flow controller for Helium as carrier gas and Oxygen to control
the flowrates of gases according to the flow values set.
EVP2 Electronic flow controller for Helium as reference gas to control the
flowrate according to the required flow value.

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4 Pneumatic Circuits
Pneumatic Circuit for CHNS-O and CHN-O Configurations

Pneumatic Circuit for CHNS-O and CHN-O Configurations

The pneumatic diagram shown in Figure 17 is common to CHNS-O and CHN-O
configurations.

Figure 17. Pneumatic Circuit for CHNS-O and CHN-O Configurations

S2

EVP2 1

F He PRV1
2 He
PI1
(5)

F
IN OUT (6)
F O2 PRV2 O2
EV1 2 PI2
CC2 TCD
IN OUT (7) F
3 1
6,5 cc/min.
CC1 300 kPa
EV3 1 EV4 1
3 1

2 2
EV2 2
4 VENT (4)
S1
1 SAMPLER
AS 2 EVP1 1
(1)
F1

2
3 CARRIER (2)
EFC - T

R2 R1

It comprises the following components:

Table 14. Components of the Pneumatic Circuits for CHNS-O and CHN-O
Component Description
EV1-EV2 They constitute the EFC module. Refer to paragraph “EFC-t Module” on
EV3-EV4 page 43.
EVP1-EVP2
S1-S2
AS Autosampler
R1 Quartz reactor for CHNS determination
R2 Quartz reactor for Oxygen determination
F1 Adsorption filter
CC1 Gas chromatographic column for CHNS determination
CC2 Gas chromatographic column for Oxygen determination
TCD TCD thermal conductivity detector

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 4 Pneumatic Circuits
Pneumatic Circuit for CHN and CHNS Configurations

Pneumatic Circuit for CHN and CHNS Configurations

The pneumatic diagram shown in Figure 18 is common to CHN and CHNS configurations.

Figure 18. Pneumatic Circuit for CHNS and CHN Configurations

S2

EVP2 1

F He PRV1
2 He
PI1
(5)

F F O2 PRV2
IN OUT (6) O2
EV1 2 PI2
TCD
IN OUT (7) F
3 1
6,5 cc/min.
CC 300 kPa
EV3 1 EV4 1
3 1

2 2
EV2 2
4
VENT (4)
S1
1 SAMPLER
AS 2 EVP1 1
(1)

2
F1 CARRIER (2)
EFC - T

R1

It comprises the following components:

Table 15. Components of the Pneumatic Circuits for CHNS and CHN
Component Description
EV1-EV2 They constitute the EFC module. Refer to paragraph “EFC-t Module” on
EV3-EV4 page 43.
EVP1-EVP2
S1-S2
AS Autosampler
R1 Reactor
F1 Adsorption filter
CC1 Gas chromatographic column
TCD TCD thermal conductivity detector

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4 Pneumatic Circuits
Pneumatic Circuit for O, S and NCS Configurations

Pneumatic Circuit for O, S and NCS Configurations

The pneumatic diagram shown in Figure 19 is common to O, S and NCS configurations.
Pneumatic Circuit for O, S and NCS Configurations.

Figure 19. Pneumatic Circuit for O, S and NCS Configurations

S2

EVP2 1

F He PRV1
2 He
PI1
(5)

F F O2 PRV2
IN OUT (6) O2
EV1 2 PI2
TCD
IN OUT (7) F
3 1
6,5 cc/min.
CC 300 kPa
EV3 1 EV4 1
3 1

2 2
EV2 2
4
VENT (4)
S1
1 SAMPLER
AS 2 EVP1 1
(1)

2
F1 CARRIER (2)
EFC - T

R1

It comprises the following components:

Table 16. Components of the Pneumatic Circuit for O, S and NCS

Component Description
EV1-EV2 They constitute the EFC module. Refer to paragraph “EFC-t Module” on
EV3-EV4 page 43.
EVP1-EVP2
S1-S2
AS Autosampler
R1 Reactor
F1 Adsorption filter
CC1 Gas chromatographic column
TCD TCD thermal conductivity detector

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 4 Pneumatic Circuits
Pneumatic Circuit for NC, NC-Soils, NC-Filters and NC-Sediments Configurations

Pneumatic Circuit for NC, NC-Soils, NC-Filters and NC-Sediments

Configurations
The pneumatic diagram shown in Figure 20 is common to NC, NC-Soil, NC-Filters and
NC-Sediments configurations.

Figure 20. Pneumatic Circuit for NC, NC-Soils, NC-Filters and NC-Sediments Configurations

S2

EVP2 1

F He PRV1
2 He
PI1
(5)

F F O2 PRV2
IN OUT (6) O2
EV1 2 PI2
TCD
IN OUT (7) F
3 1
6,5 cc/min.
CC 300 kPa
EV3 1 EV4 1
3 1

F2
2 2
EV2 2
VENT (4)
4 CP S1
1 SAMPLER
AS 2 EVP1 1
(1)

2
F1 EFC - T
CARRIER (2)

R2 R1

It comprises the following components:

Table 17. Components of the Pneumatic Circuit for NC, NC-Soils, NC-Filters, NC-Sediments
Component Description
EV1-EV2 They constitute the EFC module. Refer to paragraph “EFC-t Module” on
EV3-EV4 page 43.
EVP1-EVP2
S1-S2
AS Autosampler
R1 Oxidation reactor
R2 Reduction reactor
F1 Adsorption filter for carbon dioxide
F2 Adsorption filter for water
CC1 Gas chromatographic column
TCD TCD thermal conductivity detector

Thermo Scientific Flash 2000 Elemental Analyzer - Operating Manual 47

4 Pneumatic Circuits
Pneumatic Circuit for N, N Lubricant, N/Protein and N-Brew Configurations

Pneumatic Circuit for N, N Lubricant, N/Protein and N-Brew

Configurations
The pneumatic diagram shown in Figure 21 is common to N, N Lubricant N/Protein and
N-Brew configurations.

Figure 21. Pneumatic Circuit for N, N Lubricant N/Protein and N-Brew Configurations

S2

EVP2 1

F He PRV1
2 He
PI1
(5)

F F O2 PRV2
IN OUT (6) O2
EV1 2 PI2
TCD
IN OUT (7) F
3 1
6,5 cc/min.
CC 300 kPa
EV3 1 EV4 1
3 1

F2
2 2
EV2 2
4 VENT (4) CP S1
1 SAMPLER
AS 2 EVP1 1
(1)

2
F1 CARRIER (2) EFC - T

R2 R1

It comprises the following components:

Table 18. Components of the Pneumatic Circuit for N, N Lubricant, N/Protein and N-Brew
Component Description
EV1-EV2 They constitute the EFC module. Refer to paragraph “EFC-t Module” on
EV3-EV4 page 43.
EVP1-EVP2
S1-S2
AS Autosampler
R1 Oxidation reactor
R2 Reduction reactor
F1 Adsorption filter for carbon dioxide
F2 Adsorption filter for water
CC Gas chromatographic column
TCD TCD thermal conductivity detector
CP Pressure stabilizing cylinder

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 4 Pneumatic Circuits
Pneumatic Circuit for NC-IRMS Configuration

CAUTION The pressure stabilizing cylinder CP is not present in the N Configuration.

It avoids the introduction of air from the point 4 during the extended combustion of
samples with very high weigh.

Pneumatic Circuit for NC-IRMS Configuration

The pneumatic diagram shown in Figure 22 is common to N and C configurations with the
IRMS detector.

Figure 22. Pneumatic Circuit for NC-IRMS Configuration

S2

EVP2 1

F He PRV1
2 He
PI1
(5)

(OSR) F
IN OUT (6)
F O2 PRV2 O2
EV1 2 PI2
CC TCD
IN OUT (7) F
3 1
6,5 cc/min.
(OCR) 300 kPa
EV3 1 EV4 1
3 1

2 2
EV2 2

AS S1
F2 VENT (4)
4
EVP1 1
1 SAMPLER (1)
2
2
3 CARRIER (2)
EFC - T

R2 R1

It comprises the following components:

Table 19. Components of the Pneumatic Circuit for NC-IRMS Determinations

Component Description
EV1-EV2 They constitute the EFC module. Refer to paragraph <Pantone>EFC-t
EV3-EV4 Module page 43.
EVP1-EVP2
S1-S2
AS Autosampler
R2 Oxidation reactor
F2 Adsorption filter for water
CC Gas chromatographic column
TCD TCD thermal conductivity detector
(OSR-OCR) Oven without TCD detector - Oven with TCD detector

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4 Pneumatic Circuits
Pneumatic Circuit for Flash HT Configurations

Pneumatic Circuit for Flash HT Configurations

The left furnace at high temperature (1450 °C) is used for the determination of Oxygen and
Hydrogen by pyrolysis while the right furnace, at 1000 °C, is used for the determination of
Nitrogen and Carbon (or Sulfur).

OH Configuration
The pneumatic diagram is shown in Figure 23. The OH configuration use the left furnace at
high temperature.

Figure 23. Pneumatic Circuit Flash HT for OH Configuration

Hydrogen and Oxygen Configurations

R1 To ConFlow III
AS AS

2 3

Right Furnace 0 ..1100 ˚C

Left Furnace 0 ..1450 ˚C

Out 1

Out 4
Column
TCD

He Input Column

O2 Input H2O TRAP

Reference
2 5
Carrier

6 1

7 4
EFC-T

It comprises the following components:

Table 20. Components of the Pneumatic Circuit for O and H Determinations

Component Description
EFC-t Electronic Flow Controller Termoregulated module
AS Autosampler
Left Furnace Left furnace at high temperature (1450 °C)
Right Furnace Right furnace (1100 °C)
H2O Trap Filter for water
TCD Thermal Conductivity Detector

Note For detains about this configuration refer to the Flash HT User Guide
(PN 317 082 71).

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 4 Pneumatic Circuits
Pneumatic Circuit for Flash HT Configurations

NC Configuration
The pneumatic diagram is shown in Figure 24. The NC configuration uses the right furnace.

Figure 24. Pneumatic Circuit Flash HT for NC Configuration.

Nitrogen and Carbon Configuration

To ConFlow III
AS AS
2 3

Right Furnace 0 ..1100 ˚ C

Left Furnace 0 ..1450 ˚ C

Out 1

Out 4
Column
TCD

Column
He Input

O 2 Input H2O TRAP

Reference
2 5
Carrier

6 1

7 4
EFC-T

It comprises the following components:

Table 21. Components of the Pneumatic Circuit for NC Determinations

Component Description
EFC-t Electronic Flow Controller Thermoregulated module
AS Autosampler
Left Furnace Left furnace at high temperature (1450 °C)
Right Furnace Right furnace (1100 °C)
H2O Trap Filter for water
TCD Thermal Conductivity Detector

Note For detains about this configuration refer to the Flash 2000 HT User Guide
(PN 317 082 71).

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4 Pneumatic Circuits
Pneumatic Circuit for Flash HT Configurations

52 Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific

 Part 1

Preparation
 5

Preparation of Reactors and Adsorption Filters

This chapter provides instructions for the preparation of the reactors and the adsorption
filters, and it also reports the types of analytical columns currently used.

Contents
• Introduction
• Filling Materials
• Introduction to the Preparation of Reactors and Filters
• Preparing the Reactors
• Preparing the Adsorption Filters

Introduction
Each instrument configuration requires its own dedicated reactors, adsorption filters and
analytical columns. Except for a few “ready for use” reactors, the reactors and the adsorption
filters must be prepared by the user.

Reactors
The reactors can be quartz tubes or special steel tubes.
• The quartz and special steel tubes have a conical bottom end.
• The special steel reactors have their top end provided with two through-holes.

The filling materials used vary according to the analytical determination required.
Refer to paragraph “Filling Materials” on page 56.

Note The special steel reactors, used for combustion, require the presence of a crucible.
For more details, refer to the operating sequence on page 78.

Adsorption Filters
They can be glass or Plexiglas filters.

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5 Preparation of Reactors and Adsorption Filters
Filling Materials

The filling materials used vary according to the analytical determination required.
Refer to paragraph “Filling Materials” on page 56.

Gas Chromatographic Columns

The columns are made of steel, except in N, N/Protein and N-Brew configurations, which
require PTFE columns.

Note Gas chromatographic columns are “ready for use”, and therefore they do not require
any preparation.

The following Table 22 reports the characteristics of reactors, filters and gas chromatographic
columns required for each analytical determination.

Table 22. Characteristic of reactors, filters and gas chromatographic columns

Characteristics Analytical Determination

NC-Sediments
Length (cm)

N Lubricant

IRMS (NC)

HT (O/H)
NC-Filters
OD (mm)

N/Protein

HT (NC)
NC-Soils
ID (mm)

S (TCD)
Material

S (FPD)

N-Brew
CHNS
CHN
NCS

NC
O
N

Quarts 45 18 14             
Reactors

Special Steel 45 25 23      

Glass 11 10 8       
Filters

Plexiglas 23 30 22      

Steel 100 6 5  

200 6 5    

300 6 5  
Columns

PTFE 15 6 4 

50 8 6  

80 6 4 

100 8 6  

200 6 5   

Filling Materials
The following table reports the materials used to fill reactors, adsorption filters and gas
chromatographic columns.

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Table 23. Material required for filling reactors, filters and chromatographic columns
Characteristics Analytical Determination
Filling Material

NC-Sediments
N Lubricant

IRMS (NC)

HT (O/H)
NC-Filters
N/Protein

HT (NC)
NC-Soils
S (TCD)
S (FPD)

N-Brew
CHNS
CHN
NCS

NC
O
N
Quartz Wool                

Electrolytic Copper    

Copper Oxide      

Reduced Copper            
Reactors

Chromium Oxide   

Silvered Cobaltous/Cobaltic Oxide     

Quartz Chips 

Metallized Carbon 

Oxidation Catalyst      

Quartz Wool            

Soda Lime     
Filters

Molecular Sieves 3 Angstrom    

Magnesium Procreate (Andorran)         

Silica Gel    

Multi-separation Column (PTFE) 

Multi-separation Column (S.Steel)    

Oxygen Separation Column 

Columns

Nitrogen Separation Column (50 cm)  

Nitrogen Separation Column (100 cm)  

CHNS/NCS Packed Column  

Sulphur Separation Column  

IRMS Separation Column   

Introduction to the Preparation of Reactors and Filters

The preparation of reactors and adsorption filters must be done according to the specifications
and quantities reported in the table referring to each instrument configuration. If required,
also refer to Chapter 4, “Pneumatic Circuits,” .

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5 Preparation of Reactors and Adsorption Filters
Introduction to the Preparation of Reactors and Filters

CHN Configuration
The following Table 24 reports the characteristics of the components required for CHN
determination, and the type and size of the filling materials to be used for a proper
preparation of the reactor.

Table 24. Components required for CHN determination

Reference Component Characteristic Filling material
R Reactor Material: Quartz 1. Quartz Wool
2. Copper Reduced
3. Chromium Oxide
4. Silvered Copulates/Copulated
Oxide
CC Gas chromatographic Material: Steel ---
column Length: 2 meters
Diameter: 6 x 5 mm

Size of the Filling Material

IMPORTANT If the sample to be analyzed presents particular characteristics (high presence of

inorganic material) we suggest to insert the quartz crucible into the oxidation/reduction reactor. In
this case it is necessary to eliminate the Quartz Wool between Chromium Oxide and high quality
Copper reduced and between the high quality Copper reduced and Copulates-Cobalt Oxide.

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CHN-O Configuration
The following Table 25 reports the characteristics of the components required for CHN-O
determination, the type and size of the filling materials to be used for a proper preparation of
reactors and adsorption filter.

Table 25. Components required for CHN-O determination

Reference Component Characteristic Determination Filling material
R1 Reactor Material: Quartz CHN 1. Quartz Wool
2. Copper Reduced
3. Chromium Oxide
4. Silvered Cobaltous/Colbaltic
Oxide
CC1 Gas chromatographic Material: Steel CHN ---
column Length: 2 meter
Diameter: 6 x 5 mm
R2 Reactor Material: Quartz Oxygen 1. Quartz Wool
5. Quartz Turnings
6. Nickel Plated Carbon
F Adsorption filter Material: Quartz Oxygen 1. Quartz Wool
7. Soda Lime
8. Magnesium Perchlorate
(Anhydrone)
CC2 Gas chromatographic Material: Steel Oxygen ---
column Length: 1 meter
Diameter: 6 x 5 mm

Size of the Filling Material

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5 Preparation of Reactors and Adsorption Filters
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CHN Determination

IMPORTANT If the sample to be analyzed presents particular characteristics (high presence

of inorganic material) we suggest to insert the quartz crucible into the oxidation/reduction
reactor. In this case it is necessary to eliminate the Quartz Wool between Chromium Oxide
and high quality Copper reduced and between the high quality Copper reduced and
Cobaltous-Cobaltic Oxide.

Oxygen Determination

IMPORTANT If the sample to be analyzed presents particular characteristics (high

presence of inorganic material) we suggest to insert the quartz crucible into the reactor of
pyrolysis. In this case it is necessary to reduce from 30 mm to 20 mm the Quartz Wool in
the lower section of the reactor

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 5 Preparation of Reactors and Adsorption Filters
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CHNS Configuration
The following Table 26 reports the characteristics of the components required for CHNS
determination, and the type and size of the filling materials to be used for a proper
preparation of the reactor.

Table 26. Components required for CHNS determination

Reference Component Characteristic Filling material
R Reactor Material: Quartz 1. Quartz Wool
2. Electrolytic Copper
3. Copper Oxide
C Crucible Material: Quartz ---
CC Gas chromatographic Material: Steel ---
column Length: 2 meters
Diameter: 6 x 5 mm

Size of the Filling Material

IMPORTANT If the sample to be analyzed presents particular characteristics (high

presence of inorganic material) we suggest to insert the quartz crucible into the
oxidation/reduction reactor. In this case it is necessary to reduce the Quartz Wool between
Copper Oxide and Electrolytic Copper up to obtain a thin layer and to reduce the Copper
Oxide proportionally as shown in the previous figure.

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CHNS-O Configuration
The following Table 27 reports the characteristics of the components required for CHNS-O
determination, and the type and size of the filling materials to be used for a proper
preparation of reactors and adsorption filter.

Table 27. Components required for CHNS-O determination

Reference Component Characteristic Determination Filling material
R1 Reactor Material: Quartz CHNS 1. Quartz Wool
2. Copper Oxide
3. Electrolytic Copper
C Crucible Material: Quartz --- ---
CC1 Gas chromato-graphic Material: Steel CHNS ---
column Length: 2 meters
Diameter: 6 x 5 mm

R2 Reactor Material: Quartz Oxygen 1. Quartz Wool

4. Nickel Plated Carbon
5. Quartz Turning
F Adsorption filter Material: Glass Oxygen 1. Quartz Wool
6. Soda Lime
7. Magnesium Perchlorate
(Anhydrone)
CC2 Gas chromatographic Material: Steel Oxygen ---
column Length: 1 meter
Diameter: 6 x 5 mm

Size of the Filling Material

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 5 Preparation of Reactors and Adsorption Filters
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CHNS Determination

IMPORTANT If the sample to be analyzed presents particular characteristics (high

presence of inorganic material) we suggest to insert the quartz crucible into the
oxidation/reduction reactor. In this case it is necessary to reduce the Quartz Wool between
Copper Oxide and Electrolytic Copper up to obtain a thin layer and to reduce the Copper
Oxide proportionally as shown in the previous figure.

Oxygen Determination

IMPORTANT If the sample to be analyzed presents particular characteristics (high

presence of inorganic material) we suggest to insert the quartz crucible into the reactor of
pyrolysis. In this case it is necessary to reduce from 30 mm to 20 mm the Quartz Wool in
the lower section of the reactor.

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5 Preparation of Reactors and Adsorption Filters
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S (Sulfur) Configuration
The following Table 28 reports the characteristics of the components required for S
determination, and the type and size of filling materials to be used for a proper preparation of
reactor and adsorption filter.

Table 28. Components required for S (Sulfur) determination

Reference Component Characteristic Filling materials
R Reactor Material: Quartz 1. Quartz Wool
2. Copper Oxide
3. Electrolytic Copper
C Crucible Material: Quartz
F Adsorption filter Material: Glass 1. Quartz Wool
4. Magnesium Perchlorate (Anhydrone)
CC Gas chromatographic Material: Steel ---
column Length: 1 meter
Diameter: 6 x 5 mm

Size of the Filling Material

IMPORTANT If the sample to be analyzed presents particular characteristics (high

presence of inorganic material) we suggest to insert the quartz crucible into the
oxidation/reduction reactor. In this case it is necessary to reduce the Quartz Wool between
Copper Oxide and Electrolytic Copper up to obtain a thin layer and to reduce the Copper
Oxide proportionally as shown in the previous figure.

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O (Oxygen) Configuration
The following Table 29 reports the characteristics of the components required for O
determination, and the type and size of the filling materials to be used for a proper
preparation of reactor and adsorption filter.

Table 29. Components required for O (Oxygen) determination

Reference Component Characteristic Filling materials
R Reactor Material: Quartz 1. Quartz Wool
2. Metallized Carbon
3. Quartz Turnings
F Adsorption filter Material: Glass 1. Quartz Wool
4. Soda Lime
5. Magnesium Perchlorate (Anhydrone)
CC Gas chromatographic Material: Steel ---
column Length: 1 meter
Diameter: 6 x 5 mm

Size of the Filling Material

IMPORTANT If the sample to be analyzed presents particular characteristics (high

presence of inorganic material) we suggest to insert the quartz crucible into the reactor of
pyrolysis. In this case it is necessary to reduce from 30 mm to 20 mm the Quartz Wool in
the lower section of the reactor.

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5 Preparation of Reactors and Adsorption Filters
Introduction to the Preparation of Reactors and Filters

N (Nitrogen) Configuration
The following Table 30 reports the characteristics of the components required for N
determination, and the type and size of the filling materials to be used for a proper
preparation of reactors and adsorption filters.

Table 30. Components required for N (Nitrogen) determination

Reference Component Characteristic Filling materials
R1 Reactor Material: Quartz 1. Quartz Wool
2. Copper Oxide
3. Silvered Cobaltous/Cobaltic Oxide
R2 Reactor Material: Quartz 1 Quartz Wool
4. Copper Reduced
F1 Adsorption filter Material: Plexiglas 1. Quartz Wool
5. Soda Lime
F2 Adsorption filter Material: Plexiglas 1. Quartz Wool
6. Molecular Sieves
7. Silica Gel
CC Gas chromatographic Material: PTFE ---
column Length: 50 cm
Diameter: 8 x 6 mm

Size of the Filling Material

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 5 Preparation of Reactors and Adsorption Filters
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N Lubricant Configurations
The following Table 31 reports the characteristics of the components required for N
Lubricant determination, and the type and size of the filling materials to be used for a proper
preparation of reactors and adsorption filters.

Table 31. Components required for N Lubricant determination

Reference Component Characteristic Filling materials
R1 Reactor (See note below) Material: Special Steel 1. Quartz Wool
2. Oxidation Catalyst
R2 Reactor Material: Special Steel 1. Quartz Wool
3. Copper Reduced
F1 Adsorption filter Material: Plexiglas 1. Quartz Wool
4. Soda Lime
F2 Adsorption filter Material: Plexiglas 1. Quartz Wool
5. Molecular Sieves
6. Silica Gel
CC Gas chromatographic Material: PTFE ---
column Length: 100 cm
Diameter: 8 x 6 mm
CR Crucible Material: HPAR --

Size of the Filling Material

Note The R1 combustion reactor requires the use of a crucible CR.

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5 Preparation of Reactors and Adsorption Filters
Introduction to the Preparation of Reactors and Filters

NC Configuration
The following Table 32 reports the characteristics of the components required for NC
determination, and the type and size of the filling materials to be used for a proper
preparation of reactors and adsorption filter.

Table 32. Components required for NC determination

Reference Component Characteristic Filling materials
R1 Reactor Material: Quartz 1. Quartz Wool
2. Copper Oxide
3. Silvered Cobaltous/Cobaltic Oxide
R2 Reactor Material: Quartz 1. Quartz Wool
4. Copper Reduced
F Adsorption filter Material: Glass 1. Quartz wool
5. Magnesium perchlorate (Anhydrone)
CC Gas chromatographic Material: Steel ---
column Length: 2 meters
Diameter: 6 x 5 mm

Size of the Filling Material

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 5 Preparation of Reactors and Adsorption Filters
Introduction to the Preparation of Reactors and Filters

NCS Configuration
The following Table 33 reports the characteristics of the components required for NCS
determination, and the type and size of the filling materials to be used for a proper
preparation of reactor and adsorption filter.

Table 33. Components required for NCS determination

Reference Component Characteristic Filling materials
R Reactor Material: Quartz 1. Quartz Wool
2. 3. Copper Oxide
Electrolytic Copper
C Crucible Material: Quartz ---
F Adsorption filter Material: Glass 1. Quartz wool
4, Magnesium Perchlorate (Anhydrone)
CC Gas chromatographic Material: Steel ---
column Length: 2 meters
Diameter: 6 x 5 mm

Size of the Filling Material

IMPORTANT If the sample to be analyzed presents particular characteristics (high

presence of inorganic material) we suggest to insert the quartz crucible into the
oxidation/reduction reactor. In this case it is necessary to reduce the Quartz Wool between
Copper Oxide and Electrolytic Copper up to obtain a thin layer and to reduce the Copper
Oxide proportionally as shown in the previous figure.

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5 Preparation of Reactors and Adsorption Filters
Introduction to the Preparation of Reactors and Filters

NC-Soils, NC-Sediments, NC-Filters Configurations

The following Table 34 reports the characteristics of the components required for NC-Soils,
NC-Sediments and NC-Filters determinations, and the type and size of the filling materials
to be used for a proper preparation of reactors and adsorption filter.

Table 34. Components required for NC-Soils, NC-Sediments and NC-Filters Determinations
Reference Component Characteristic Filling materials
R1 Reactor (See note below) Material: Special Steel 1. Quartz Wool
2. Oxidation Catalyst
R2 Reactor Material: Quartz 1. Quartz Wool
3. Copper Reduced
F Adsorption filter Material: Glass 1. Quartz Wool
4. Magnesium Perchlorate (Anhydrone)
CC Gas chromatographic Material: Steel ---
column Length: 2 meters
Diameter: 6 x 5 mm
CR Crucible Material: HPAR ---

Size of the Filling Material

Note The R1 combustion reactor requires the use of a crucible CR.

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Introduction to the Preparation of Reactors and Filters

N/Protein and N-Brew Configurations

The following Table 35 reports the characteristics of the components required for N/Protein
and N-Brew determinations, and the type and size of the filling materials to be used for a
proper preparation of reactors and adsorption filters.

Table 35. Components required for N/Protein and N-Brew Determinations

Reference Component Characteristic Filling materials
R1 Reactor (See note below) Material: Special Steel 1. Quartz Wool
2. Oxidation Catalyst
R2 Reactor Material: Special Steel 1. Quartz Wool
3. Copper Reduced
F1 Adsorption filter Material: Plexiglas 1. Quartz Wool
4. Soda Lime
F2 Adsorption filter Material: Plexiglas 1. Quartz Wool
5. Molecular Sieves
6. Silica Gel
CC Gas chromatographic Material: PTFE N/Protein
column Length: 50 cm
Diameter: 8 x 6 mm
Material: PTFE N-Brew
Length: 100 cm
Diameter: 8 x 6 mm

Size of the Filling Material

Note The R1 combustion reactor requires the use of a crucible CR.

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5 Preparation of Reactors and Adsorption Filters
Introduction to the Preparation of Reactors and Filters

NC Configuration with the Flash IRMS

The following Table 36 reports the characteristics of the components required for NC
determinations with the Flash IRMS, and the type and size of the filling materials to be used
for a proper preparation of reactors and adsorption filter.

Table 36. Components required for NC Determination with the Flash IRMS
Reference Component Characteristic Filling materials
R1 Reactor Material: Quartz 1. Quartz Wool
2. Chromium Oxide
3. Silvered Cobaltous-Cobaltic Oxide
R2 Reactor Material: Quartz 1. Quartz Wool
4. Copper Reduced
F Absorption Filter Material: Plexiglas ---
CC Gas chromatographic Material: Stainless Steel ---
Column Length: 3 meters
Diameter: 6 x 5 mm

Size of the Filling Material

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 5 Preparation of Reactors and Adsorption Filters
Introduction to the Preparation of Reactors and Filters

NC Configuration with the Flash HT

The following Table 37 report the characteristics of the components required for NC
determinations with the Flash HT, and the type and size of the filling materials to be used for
a proper preparation of reactor and adsorption filter.

Table 37. Components required for NC Determination with the Flash IRMS
Reference Component Characteristic Filling materials
R2 Reactor Material: Quartz 1. Quartz Wool
2. Chromium Oxide
3. Silvered Cobaltous-Cobaltic Oxide
F2 Absorption Filter Material: Plexiglas 1. Quartz Wool
4. Magnesium Perchlorate (Anhydrone)
CC2 Gas chromatographic Material: Stainless Steel ---
Column Length: 3 meters
Diameter: 6 x 5 mm

Size of the Filling Material

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5 Preparation of Reactors and Adsorption Filters
Preparing the Reactors

Preparing the Reactors

According to the instrument configurations, 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 of the concerned
instrument configuration, as described in paragraph “Introduction to the Preparation of
Reactors and Filters” on page 57.

Please remember that:

• all reactors have a conical bottom end.
• special steel reactors have the upper end provided with two through-holes.

WARNING 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.

The filling of reactors requires the use of quartz wool. Before handling
quartz wool, we recommend to wear gloves and face protection.

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 procedure should be carried out on a wide and clean workbench.

 To Fill the Quartz Reactor

The following procedure provides instructions for filling a quartz reactor.

Material Required
Quartz reactor
Compression rod
Filling material

Use the following procedure to fill the quartz reactor:

1. Starting from the reactor bottom (conical end), introduce a sufficient amount of quartz
wool to form the required layer, as shown in Figure 25.

Note In the CHNS, NCS and S Configuration, Electrolytic Copper is used. The copper
wires (about 14 cm long) must be inserted in the reactor through the conical part and
pulled inside avoiding their braiding.

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 5 Preparation of Reactors and Adsorption Filters
Preparing the Reactors

Figure 25. Introduction of quartz wool into the reactor conical end

Quartz wool

Conical part

2. Plug with your finger the mouth of the reactor conical end. Gently press the quartz wool
using the rod provided, as shown in Figure 26.

Figure 26. .Compression of quartz wool into the quartz reactor

Figure 27. Filling of the quartz reactor

3. Turn the reactor conical end downward and rest it delicately onto the workbench.

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5 Preparation of Reactors and Adsorption Filters
Preparing the Reactors

4. Pour sequentially the required filling materials into the reactor, as shown in Figure 27,
ensuring that each layer has the indicated size. At each step gently press the quartz wool
using the rod provided.
5. The last step of the sequence consists in introducing a sufficient quantity of quartz wool
to form the last required layer, as shown in Figure 28.

Figure 28. Introduction of quartz wool as last layer of the sequence

Quartz wool

6. Delicately press the quartz wool using the rod provided.

 To Fill the Special Steel Reactor

The following operating procedure provides instructions for filling a steel reactor.

Material required
Special steel reactor
Compression rod
Filling materials

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

Use the following procedure to fill the steel reactor:

1. Introduce into the bottom end of the reactor a sufficient amount of quartz wool to form
the required layer, as shown in Figure 29.

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 5 Preparation of Reactors and Adsorption Filters
Preparing the Reactors

Figure 29. Introduction of quartz wool into the bottom end of the reactor

Reactor bottom end Quartz wool

2. Plug with your finger the mouth of the reactor bottom end. Gently press the quartz wool
using the rod provided, as shown in Figure 30.

Figure 30. Compression of quartz wool into the special steel reactor

3. Turn the bottom end of the reactor downward and delicately rest it onto the workbench.

Figure 31. Filling of the special steel reactor and compression of materials

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5 Preparation of Reactors and Adsorption Filters
Preparing the Reactors

4. Pour sequentially the required filling materials into the reactor, ensuring that each layer
has the indicated size.
Note When the oxidation catalyst is used (refer to Table 23 on page 57), it must be
introduced into the reactor homogeneously.

At each step gently press the quartz wool using the rod provided.
5. The last step of the sequence consists in introducing a sufficient quantity of quartz wool
to form the last required layer, as shown in Figure 32.

Figure 32. Introduction of quartz wool as last layer of the sequence

6. Gently press the quartz wool using the rod provided.

 To Prepare the Crucible

The following operating procedure provides instructions for the preparation of the crucible
you will use with the special steel reactors required for combustion.

Material required
Quartz wool
Compression rod

Use the following procedure to prepare the crucible:

1. Hold the crucible as shown in Figure 33. Introduce into the bottom end of the crucible a
sufficient quantity of quartz wool to form a 2 cm layer.

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 5 Preparation of Reactors and Adsorption Filters
Preparing the Adsorption Filters

Figure 33. Introduction of quartz wool into the crucible

Quartz wool

Crucible

2. Gently press the quartz wool using the rod provided, as shown in Figure 34.

Figure 34. Compression of quartz wool into the crucible

Preparing the Adsorption Filters

According to the instrument configurations, the filling materials are introduced into the
empty filter to form a series of layers of defined dimensions.

For a proper preparation of the layers, refer to the filling diagram of the concerned instrument
configuration, as described in paragraph “Introduction to the Preparation of Reactors and
Filters” on page 57.

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5 Preparation of Reactors and Adsorption Filters
Preparing the Adsorption Filters

According to the analytical configuration required, the following adsorption filters can be
used:
• large filter (Plexiglas)
• small filter (Glass)

WARNING 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.

The filling of reactors requires the use of quartz wool. Before handling
quartz wool, we recommend to wear gloves and face protection.

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 procedure should be carried out on a wide and clean workbench.

 To Fill the Adsorption Filter

The following procedure provides instructions for filling an adsorption filter.

Material required
Glass or Plexiglas filter according to the instrument configuration
Compression rod
Filling materials

Introduce into either of the tube ends a sufficient amount of quartz wool to form the required
layer as shown in Figure 35.

Figure 35. Introduction of quartz wool into the tube

Threaded end Quartz wool

3. While plugging the tube mouth with your hand, press gently the quartz wool using the
rod provided.

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 5 Preparation of Reactors and Adsorption Filters
Preparing the Adsorption Filters

4. Screw the nut complete with its seal onto the threaded mouth, as shown in Figure 36.

Figure 36. Nuts and seals for adsorption filters

Seal Seal

Nut Nut

5. Pour sequentially the required filling materials into the adsorption filter, ensuring that
each layer has the indicated size. At each step gently press the quartz wool using the rod
provided.

CAUTION Soda Lime must be wetted before using. Pour 0.5 ml of water on the Soda
Lime surface on the side that will be connected to the reduction reactor

6. Do the last layer using a sufficient quantity of quartz wool to form the required layer.
7. Complete the procedure by screwing on the second nut complete with its seal, as shown
in Figure 37.

Figure 37. Preparation of the adsorption filters

Packing material
Nut

Nut Seal

Nut Nut

Packing material Seal

Figure 38 shows the result of the filling operation of an adsorption filter.

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5 Preparation of Reactors and Adsorption Filters
Preparing the Adsorption Filters

Figure 38. Result of the filling of a large adsorption filter and of a small one

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 6

Connecting Reactors and Adsorption Filters

This chapter contains the instructions to install reactors and adsorption filters into the
elemental analyzer, and it also provides information on how to remove them.

Contents
• Installing the Reactors into the Furnaces
• Installing the Adsorption Filters
• Removing the Reactors
• Removing the Adsorption Filters

Installing the Reactors into the Furnaces

The following Table 38summarizes the type of reactor to be used and the furnace where it
must be installed according to your instrument configuration.

Refer to paragraph “Introduction to the Preparation of Reactors and Filters” on page 57.

Note The reactors of special steel used for combustion require the use of a crucible.

Table 38. Reactors and furnaces

Determination Left furnace Right furnace
CHN Quartz reactor ---
CHN-O Quartz reactor Quartz reactor
CHNS Quartz reactor ---
CHNS-O Quartz reactor Quartz reactor
S (Sulphur) Quartz reactor ---
O (Oxygen) Quartz reactor ---
N (Nitrogen) Quartz reactor Quartz reactor
N Lubricant Special steel reactor + SS crucible Special steel reactor
NC Quartz reactor Quartz reactor
NCS Special steel reactor ---

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6 Connecting Reactors and Adsorption Filters
Installing the Reactors into the Furnaces

Table 38. Reactors and furnaces, continued

Determination Left furnace Right furnace
NC-Soils Special steel reactor + SS crucible Quartz reactor
NC-Sediments Special steel reactor + SS crucible Quartz reactor
NC-Filters Special steel reactor + SS crucible Quartz reactor
N/Protein Special steel reactor + SS crucible Special steel reactor
N-Brew Special steel reactor + SS crucible Special steel reactor
IRMS (NC) Quartz reactor ---
HT (NC) Quartz Reactor
HT (O/H) Special reactor ---

Preliminary Operations
Before installing the reactors do the following:
1. Check that the furnaces are at room temperature.
2. Open the furnaces compartment by lifting the cover and removing the protecting plate.
Refer to paragraph “Furnaces Compartment” on page 28.
3. Remove the autosampler, if installed, by manually undoing the fixing nut, as shown in
Figure 39.

Figure 39. Removing the autosampler

Autosampler Nut

 To Install the Quartz Reactors into the Furnaces

The following procedure contains the instructions to install the quartz reactors.
.
Note The figures in this operating sequence show the installation of a reactor into the left
furnace.

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 6 Connecting Reactors and Adsorption Filters
Installing the Reactors into the Furnaces

WARNING The reactors must be installed with the furnaces at room temperature.

Material required
O-ring

CAUTION Do not use mechanical tools to screw or unscrew the fixing nut.

1. Remove the fixing nut.

2. Delicately introduce the reactor into the furnace ensuring that the tube conical end is
turned downward, as shown in Figure 40.

Figure 40. Introduction of the quartz reactor into the furnace

Reactor

Conical end

3. Guide the reactor inside the furnace. The reactor conical end must fit into the coupling
union located on the base of the furnaces compartment, as shown in Figure 41.

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6 Connecting Reactors and Adsorption Filters
Installing the Reactors into the Furnaces

Figure 41. Driving the reactor into the furnace

Furnace

Reactor
Coupling union
Base

4. Gently press the edge of the reactor until introduction is complete, as shown in Figure 42.

Figure 42. Complete the introduction of the reactor

5. Slip on the O-ring with its conical section turned upwards as shown in Figure 43.

Figure 43. O-ring

O-ring

6. Manually screw the autosampler fixing nut.

Note If required by your instrument configuration, install the reactor into the right
furnace following the same instructions reported in this operating sequence.

The autosampler installed on the right channel is used only for CHNS-O and CHN-O
configurations

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 6 Connecting Reactors and Adsorption Filters
Installing the Reactors into the Furnaces

7. To complete the operation manually screw the fixing nut or the autosampler nut if
installed.
8. Put on again the protecting plate and the cover of the furnaces compartment.

 To Install the Special Steel Reactors into the Furnaces

The following procedure contains the instructions to install the special steel reactors into the
left and right furnaces.
.
Note The figures in this operating sequence show the installation of a reactor into the left
furnace.

WARNING The reactors must be installed with the furnaces at room temperature.

Material required
Tool for steel tubes
O-ring

1. Remove the fixing nut.

CAUTION Do not use mechanical tools to screw or unscrew the fixing nut.

Figure 44. Introducing the special steel reactor into the furnace

Tool for steel tube

Reactor

2. Introduce the tool, provided in the standard outfit, into the holes located on the top end
of the 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 45.

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6 Connecting Reactors and Adsorption Filters
Installing the Reactors into the Furnaces

Figure 45. Driving the reactor into the furnace

Furnace

Reactor
Coupling union
Base

4. Turn the reactor clockwise and push until completely in place, as shown in Figure 46.

Figure 46. The reactor in place

5. Slip on the O-ring as shown in Figure 47.

Figure 47. O-ring

6. By using the tool for special steel reactors, introduce the crucible into the combustion
reactor, which is in the left furnace. See Figure 48.

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 6 Connecting Reactors and Adsorption Filters
Installing the Reactors into the Furnaces

Figure 48. Introduction of the crucible into the combustion reactor

Crucible

Crucible

Combustion reactor
Tool (housed in the
left furnace)

7. Manually screw the autosampler nut. See Figure 49.

CAUTION Do not use mechanical tools to screw or unscrew the fixing nut.

Figure 49. Mounting the autosampler on the left furnace

8. Install the reduction reactor into the right furnace: in case of steel tubes following the
instructions of previous operating sequence. In case of quartz tubes refer to the operating
sequence “To Install the Quartz Reactors into the Furnaces” on page 84.
9. At the end of the operation, manually screw the fixing nut or the autosampler nut if
installed. See Figure 50.

Note The autosampler installed on the right channel is used only for CHNS-O and
CHN-O configurations.

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6 Connecting Reactors and Adsorption Filters
Installing the Adsorption Filters

Figure 50. Mounting the fixing nut on the right furnace

10. Put on again the protecting plate and the cover of the furnaces compartment.

Installing the Adsorption Filters

The following Table 39 summarizes the type of adsorption filter required and the channel to
which it should be connected according to instrument configuration.
Refer to paragraph “Introduction to the Preparation of Reactors and Filters” on page 57.

Table 39. Adsorption filters

Determination Left furnace Right furnace
CHN --- ---
CHN-O --- Glass filter
CHNS --- ---
CHNS-O --- Glass filter
S (Sulphur) Glass filter ---
O (Oxygen) Glass filter ---
N (Nitrogen) --- Two Plexiglas filters in series
N Lubricant --- Two Plexiglas filters in series
NC --- Glass filter
NCS Glass filter ---
NC-Soils --- Glass filter
NC-Sediments --- Glass filter
NC-Filters --- Glass filter
N/Protein --- Two Plexiglas filters in series
N-Brew --- Two Plexiglas filters in series
IRMS (NC) Plexiglas filter ---
HT (NC) --- Plexiglas filter
HT (O/H) Plexiglas filter ---

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 6 Connecting Reactors and Adsorption Filters
Installing the Adsorption Filters

Preliminary Operations
The following preliminary operations are required to install the adsorption filters.
1. Have access to the detector compartment by opening the right side door of the
instrument. Refer to paragraph “Detector Compartment” on page 30. Figure 51shows the
detector compartment.

Figure 51. Detector compartment

 To Connect and Install the Adsorption Filters

The following operating procedure contains the instructions to install the adsorption filters.
Figure 52 shows the result of the installation of two adsorption filters connected in series.

Figure 52. Adsorbtion filters installed in the detector compartment

Single filter Two filters in series

According to your instrument configuration, do the installation and connection of the

adsorption filters following the instructions of next paragraphs Single Filter or Two Filters in
series.

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6 Connecting Reactors and Adsorption Filters
Installing the Adsorption Filters

Single Filter
To connect the filter do the following:
1. Connect the filter inlet to the connection coming from the reactor.
2. Connect the filter outlet to the connection coming from the gas chromatographic
column.
3. Secure the filter by means of the appropriate clips.

Two Filters in series

To connect two filters in series do the following:
1. Connect the filters to one another, as shown in Figure 53, and then to the circuit as per
relevant diagram. Refer to “Introduction to the Preparation of Reactors and Filters” on
page 57.

Figure 53. Connection of two filters in series

2. Introduce the filter into the securing clips, as shown in Figure on page 93.

Figure 54. Installation of the filters into the detector compartment

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 6 Connecting Reactors and Adsorption Filters
Removing the Reactors

Removing the Reactors

Before starting this operation:
• Check that the furnaces are at room temperature.
• Open the furnaces compartment by lifting the cover and removing the protecting plate.
Refer to paragraph “Furnaces Compartment” on page 28.
• Undo the nuts securing the reactors. If the autosampler is installed, manually unscrew the
fixing nut to remove it as shown in Figure 39 page 84.

 To Remove the Quartz Reactors from the Furnaces

The following operating procedure contains the instructions to remove the quartz reactors
from the left and right furnaces.
.

Note The figures in this operating sequence show the installation of a reactor into the left
furnace.

WARNING The reactors must be installed with the furnaces at room temperature.

1. Remove the O-ring from the top of the reactor as shown in the left image of Figure 55.
2. Using both hands turn the tube counterclockwise and simultaneously pull it upward as
shown in the right image of Figure 55.

Figure 55. O-ring and removal of the reactor from the furnace

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6 Connecting Reactors and Adsorption Filters
Removing the Reactors

 To Remove Special Steel Reactors from the Furnaces

The following operating procedure contains the instructions to remove the special steel
reactors from the left and right furnaces.

WARNING The reactors must be installed with the furnaces at room temperature.

Material required
Tool for special steel reactor
Tool for crucible

1. Remove the O-ring from the top of the reactor as shown in Figure 56.

Figure 56. Removal of the steel reactor o-ring

2. Remove the crucible from the combustion reactor (left furnace) using the appropriate tool
as shown in Figure 57.

Figure 57. Removal of the crucible

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 6 Connecting Reactors and Adsorption Filters
Removing the Adsorption Filters

3. By using the proper tool, remove the reactor turning it counterclockwise and
simultaneously pulling it upwards, as shown in Figure 58.

Figure 58. Removal of the reactor

Removing the Adsorption Filters

Before starting this operation:
1. Open the right side door of the instrument to have access to the detector compartment.
Refer to paragraph “Detector Compartment” on page 30.

 To Remove the Adsorption Filter

The following operating procedure contains the instructions to remove the adsorption filter
from the system.
1. Remove the filter from the securing clips.
2. Disconnect the filter inlet and then its outlet from the relevant connections.

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 7

Preparing the Sample

This chapter describes some techniques for the sample preparation, also it provides basic
instructions to homogenize and weigh the sample.

Contents
• Introduction
• Homogenizing the Sample
• Sample Weighing Technique

Introduction

WARNING 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 (e.g. under a fumes hood), strictly obeying
the company safety regulations.

Homogenizing the Sample

Before the analysis the sample must be properly homogenized. This paragraph gives you basic
information on how to prepare the most currently analyzed materials.

Table 40 on page 98 gives you indications to weigh the sample according to your instrument
configuration.

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7 Preparing the Sample
Homogenizing the Sample

Table 40. Information on sample weighing

Sample Information
Soils In soils, sulfur is often present as ion sulfate, and therefore it is
necessary to add 5-10 mg of vanadium pentoxide (V2O5) every
10-20 mg of soil to ensure complete conversion of inorganic sulfur
into sulfur dioxide.
Minerals The sulfur content in minerals can vary from a few percent units
(e.g. bauxite) to definitely higher values (e.g. pyrite).
If the mineral to be analyzed is unknown, a pre-analysis is
recommended. Once the sulfur content is defined, the required
Sulfur

analyses with proper sample amounts can be performed:

Example: For minerals rich in sulfur, samples of 2-5 mg are

prepared. For minerals with sulfur traces, samples of 10-20 mg are
prepared.
Plants Plants are rich in Nitrogen, Carbon and Hydrogen, but relatively
poor in Sulfur. Therefore, after the first analysis, check that the peak
of sulfur dioxide is correctly integrated.

Soils The Nitrogen content in such samples is generally very low (0.1%).
Nitrogen

Sediments Set a very high sensitivity of integration and use Oxygen of

maximum purity grade.

Soils, Sediments and Minerals

Before the analysis, samples of such nature and origin require homogenizing, which can be
performed by means of proper mills allowing the simultaneous preparation of several samples.
A first coarse homogenizing on sample amounts of a few hundreds of grams is followed by
finer homogenizing on a few dozens of grams, until optimum granularity (100-200 μm) is
reached. The resulting sample is dried in an oven.

Carbons
The technique to homogenize carbons is the same as that used for the preparation of soils,
sediments and minerals, but the sample drying requires specific operations:
The samples are dried in an oven for one hour at 105°C, left in the air for the same time to let
them acquire again their natural moisture and then stored in airtight containers. Finally they
are put into driers.

Metals
The sample preparation technique is a function of the metal hardness.
Special machines can be used as drills, mills or lathes.
In case of particularly hard materials, use a diamond file.

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 7 Preparing the Sample
Sample Weighing Technique

You should obtain metal chips as small and light as possible. The homogenizing degree
depends on the particle size.

The quantity of sample for the analysis is a function of the alloy composition.
• For cast irons, prepare samples of 10-20 mg.
• For steels and other metal alloys, weigh 40-50 mg.

Plastics
Polymers are generally available as pellets, or only rarely as powders.
If you don’t want or cannot homogenize the sample, you can cut the pellets into small pieces
and analyze 2-3 mg.

The same process is used for synthetic and natural rubbers.

Vegetal
To prepare samples of vegetal products, two types of mills are normally used:
• Blade mills to homogenize cereals, leaves, forage and wood. In these mills, devices with 1
mm mesh sieves are used for N/Protein determination.
• Ball mills to homogenize samples of fruit and vegetables after lyophilization. These mills
use devices for finer granulometry.

The sample amount to be analyzed depends on the type of determination and on the
homogenizing degree.

Liquids
Liquid samples are prepared according to a procedure that depends on the sample volatility.
Liquid samples with limited volatility are weighed in traditional tin containers.
However, to avoid sample losses, we suggest to use two containers for each sample.
If the sample is characterized by high viscosity, it should be properly mixed before being
drawn for injection.

Samples injectable by micro syringes can be introduced manually using the optional manual
injection device, or automatically using the autosampler for liquids.

Sample Weighing Technique

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
• Tools to seal the container containing the sample.

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7 Preparing the Sample
Sample Weighing Technique

Samples of different nature require specific weighing techniques.

Note The technique of two containers is suggested to prevent sample losses due to
defective sealing of the container and consequently prevent the autosampler
contamination.

The weighing procedure requires a series of operations according to the sample nature.

Solid Samples
Solid samples are introduced directly into the tin container using a spatula.

According to the sample quantity to be analyzed, refer to the following operating procedures:
• “Weighing Technique for Large Quantities of Solid Samples” on page 101.
• “Weighing Technique for Small Quantities of Solid Samples” on page 104.

Liquid Samples
The weighing procedure changes according to the sample type.

Samples Characterized by Limited Volatility

• If the sample density is 1 or close to 1
Introduce the sample directly into the tin container for liquids using a syringe of 10 or
100 μl capacity according to the instrument configuration.
• 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.

Refer to the following operating procedures:

• “Weighing Technique for Liquid Samples” on page 105.
• “Weighing Technique for Liquid Samples Deposited on Adsorbent Material” on
page 107.

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 slide along the container walls as
shown in Figure 59 on page 101.

Note Only for N Determination, according to the sample viscosity, it may be necessary to
adsorb the sample on a Chromosorb WAW® (only for N, N-Brew and N/Protein
Configurations) layer previously introduced into the tin container.

Refer to the following operating procedure:

• “Weighing Technique for Viscous Samples” on page 108.

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 7 Preparing the Sample
Sample Weighing Technique

Samples Available in Liquid Phase

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

 Weighing Technique for Large Quantities of Solid Samples

The following procedure contains the instructions to weigh large quantities of solid samples.

Materials required
Balance
Tin disks
Spring tweezers
Sealing device and cylindrical tool
Spatula
Brush

Figure 59. Accessories required to weigh solid samples

Sealing device

Lever

Tin disks Brush

Spring rweezers Cylindrical tool

1. By using the tweezers, take a tin disk and rest it on the cavity of the sealing device, as
shown in Figure 60.
2. By sing the cylindrical tool, press the tin disk and make it enter the cavity of the sealing
device, as shown in Figure 60.

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7 Preparing the Sample
Sample Weighing Technique

Figure 60. Preparation of the tin container (1)

Tin disk Tweezers Tin disk Cylindrical tool

Sealing device

3. Press the top of the sealing device downwards to have the container come out of the
cavity.
4. Take out the container using the spring tweezers, as shown in Figure 61.
5. Put the prepared container on a clean surface.

Figure 61. Preparation of the tin container (2)

6. Using a spatula, introduce some sample into the tin container until sufficiently filled, then
delicately press the sample using the cylindrical tool, as shown in Figure 62.

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 7 Preparing the Sample
Sample Weighing Technique

Figure 62. Introduction and compression of the sample

7. IClose the container using the lever located on the top surface of the sealing device.
8. Press the top of the sealing device downwards to have the container come out of the
cavity.
9. Remove the container using the spring tweezers, as shown in Figure 63.

Figure 63. Removal of the closed container and cleaning of the contact surface

10. Weigh the container obtained and take note of the value.

We suggest the following weighing procedure to prevent sample losses due to defective sealing.
a. Using the tweezers, take a tin disk and rest it on the cavity of the sealing device, as
shown in Figure 60.
b. Using the cylindrical tool, press the tin disk and make it enter the cavity of the sealing
device, as shown in Figure 60.
c. Press the top of the sealing device downwards to have the container come out of the
cavity.

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7 Preparing the Sample
Sample Weighing Technique

d. Take out the container using the spring tweezers, as shown in Figure 61.
e. Put the prepared container on a clean surface.
f. Prepare a second container placing another tin disk on the cavity of the sealing device.
g. Using the cylindrical tool, gently press the disk to obtain a half-open container.
h. Place both containers on the balance pan and do the tare.
i. Take the first container and put it into the cavity of the sealing device.
j. Using a spatula, introduce some sample into the tin container until sufficiently filled,
then delicately press the sample using the cylindrical tool, as shown in Figure 62.
k. Close the container using the lever located on the top surface of the sealing device.
l. Press the top of the sealing device downwards to have the container come out of the
cavity.
m. Remove the container using the spring tweezers, as shown in Figure 63, and rest it on
a clean surface.
n. Clean the contact surfaces using the brush.
o. Put the half-open container on the cavity of the sealing device and place thereon the
container containing the sample,
p. Using the cylindrical tool, introduce the containers into the sealing device and then
repeat steps k, l, m and n of this procedure.
q. Weigh the container obtained and take note of the value.

 Weighing Technique for Small Quantities of Solid Samples

We suggest the following weighing procedure to prevent sample losses due to defective sealing.

The following procedure contains the instructions to weigh small quantities of solid samples.

Materials required
Electronic micro balance
Tin containers for small weighings
Two spring tweezers
Spatula

1. Take two containers for small weighings, put them onto the balance pan and do the tare.
2. Remove one of the containers from the balance pan and put it onto a clean surface. Using
a spatula, introduce into the container the sample quantity required for the analysis.
3. Weigh the container with sample and read the value. If the weight is correct for the
analysis to be run, remove the two containers from the balance pan and rest them on a
clean surface.
4. Close the container containing the sample using two spring tweezers, as shown in
Figure 64, to obtain a pellet.

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 7 Preparing the Sample
Sample Weighing Technique

Figure 64. Preparation of the container for small sample quantities

5. Introduce the pellet into the second container and close the latter in the same way.
6. Put the container obtained onto the balance pan, weigh it and take note of the value.

 Weighing Technique for Liquid Samples

The following operating procedure contains the instructions to properly weigh liquid samples.

Materials required
Electronic micro balance
Tin container for liquid samples
Spring tweezers
Sealing device (optional)
Spatula
10 or 100 μl syringe according to the instrument configuration

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7 Preparing the Sample
Sample Weighing Technique

Figure 65. Accessories to weigh liquid samples

4 2
5

3 6
1

1. Container for liquid 2. Spring tweezers

3. Sealing device 4. Lever
5. Sample-holding slide 6. Syringe

1. Take a tin container for liquid samples and put it onto the micro balance pan. Do the tare.
2. Place the tin container into the appropriate position in the slide of the sealing device, then
inject the sample using a syringe, as shown in Figure 66.

Figure 66. Housing for the container and sample injection

3. Put the slide with the container into the sealing device and tighten the container using the
appropriate lever, as shown in Figure 67.

Figure 67. Closing and removing the container

4. Remove the slide from the sealing device and then the container with the sample from the
slide, as shown in Figure 67.
5. Put the container onto the micro balance pan, weigh it and take note of the weight value.

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 7 Preparing the Sample
Sample Weighing Technique

 Weighing Technique for Liquid Samples Deposited on Adsorbent Material

The following operating procedure contains the instructions to properly weigh liquid samples
previously deposited on adsorbent material.

Materials required
Balance
Tin containers for liquid samples
Two spring tweezers
Spatula
100 μl syringe
Chromosorb WAW® (Only for N, N/Protein and N-Brew Determinations)

Note Chromosorb WAW ® is an extremely porous inert inorganic material, made of

silicates and completely free from Nitrogen. When Chromosorb is free from
contamination, its contribution to the blank value is negligible.

1. Introduce one or two spatula tips of Chromosorb WAW® into the tin container.
2. Put the container with the adsorbent material and an empty container onto the balance
pan and do the tare.
3. Remove the containers from the balance pan and rest them onto a clean surface.
4. Using the syringe, introduce the liquid sample depositing it on the layer of adsorbent
material contained in the container, as shown in Figure 68.

CAUTION Do not wet the container walls during sample introduction.

Figure 68. Weighing of a liquid sample deposited on adsorbent material

1 2 3 4

1. Empty container 2. Layer of adsorbent material

3. Introduction of the sample 4. Closed container

5. Close the container using two spring tweezers or the sealing device.
6. Introduce the container with the sample into the second container and close the latter in
the same way.
7. Weigh the container and take note of the weight value.

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7 Preparing the Sample
Sample Weighing Technique

 Weighing Technique for Viscous Samples

The following operating procedure contains the instructions to properly weigh viscous
samples.

According to its viscosity, a sample can be weighed as described in either of the following
operating sequences:
• “Weighing Technique for Liquid Samples” on page 105.
• “Weighing Technique for Liquid Samples Deposited on Adsorbent Material” on
page 107.

CAUTION When a liquid sample is too viscous to be drawn by means of a syringe, use the
spatula provided in the instrument standard outfit, as shown in Figure 69.

Figure 69. Introduction of a viscous sample into the container

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 8

Analytical Methods
This chapter describes the analytical methods used for all configurations of the Flash 2000
elemental analyzer.

Contents
• Introduction
• Analytical Method for CHN Configuration
• Analytical Method for CHN-O Configuration
• Analytical Method for CHNS Configuration
• Analytical Method for CHNS-O Configuration
• Analytical Method for S (Sulfur) Configuration
• Analytical Method for O (Oxygen) Configuration
• Analytical Method for N (Nitrogen) Configuration
• Analytical Method for NC Configuration
• Analytical Method for NCS Configuration
• Analytical Method for NC-Soils, NC-Sediments and NC-Filters Configurations
• Analytical Method for N Lubricant, N/Protein and N-Brew Configurations
• Analytical Method for NC-IRMS Configuration
• Analytical Method for NC-HT Configuration

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8 Analytical Methods
Introduction

Introduction
Each configuration of the Flash 2000 elemental analyzer has its own dedicated analytical
method.

The description of the analytical method is illustrated by diagrams referring to the concerned
instrument configuration.

When necessary, also refer to Chapters 1, 4 and 5 for more information concerning the
components of the instrument and their functions. The analytical method used in each
instrument configuration includes different subsequent steps leading to determine the percent
composition of the components of interest through the transformation of the solid or liquid
sample into gas.

Note To develop and perform the analytical cycle, refer to the relevant chapter contained
in Section III.

For correct sample analyses all pneumatic lines must be leak-free. Therefore, a preliminary
leak check is recommended before starting analytical cycles.

IMPORTANT All the pneumatic diagram visualized in the chapter are in the Pre-analysis
stage.

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 8 Analytical Methods
Analytical Method for CHN Configuration

Analytical Method for CHN Configuration

An autosampler AS is connected to a quartz reactor R1 housed in an furnace at a temperature
of 900 °C. This reactor is connected to the analytical column CC, which on its turn is
connected to a channel of the thermal conductivity detector TCD.

Figure 70. Instrument parts diagram and pneumatic diagram for CHN determination

S2

EVP2 1

F He PRV1
2 He
PI1
(5)

F F O2 PRV2
IN OUT (6) O2
EV1 2 PI2
TCD
IN OUT (7) F
3 1
6,5 cc/min.
CC 300 kPa
EV3 1 EV4 1
3 1

2 2
EV2 2
4
VENT (4)
S1
1 SAMPLER
AS 2 EVP1 1
(1)

2
F1 CARRIER (2)
EFC - T

R1

Pneumatic Diagram Description

Helium He flows to the flow sensor S1, through the solenoid valve EV2, and directly to the
flow sensor S2. Both flow sensors are connected to relevant proportional valves EVP1 and
EVP2.
The proportional valve EVP1, connected to the autosampler AS, controls the Helium flow
through the whole pneumatic circuit as far as the solenoid valve EV3. This valve, normally
open, exhausts Helium to the atmosphere through Vent 4.

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8 Analytical Methods
Analytical Method for CHN Configuration

The proportional valve EVP2, connected to the detector reference channel RF, controls the
Helium flow as far as the solenoid valve EV4. This valve, normally open, allows Helium to
reach point 1 of the autosampler and purge the zone where the sample is housed.
The Oxygen line O2 is connected to the solenoid valve EV1.
This valve controls the Oxygen inlet.

Sequence of the Method Stages

During pre-analysis the solenoid valve EV1 shuts off the Oxygen flow, whereas the solenoid
valve EV2 allows Helium to flow in the circuit. When Start Analysis is pressed, the valve EV1
opens, whereas the valve EV2 switches to allow Oxygen to flow in as far as the combustion
reactor R1 for a preset time.
After a few seconds, the sample, weighed in a tin container and stored in the autosampler, is
dropped into the combustion reactor. Tin, coming in contact with the 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, valves EV1 and EV2 return to their
original position restoring Helium flow.
The combustion products are conveyed across the reactor R1, where oxidation is completed.
Nitrogen oxides possibly formed are reduced to elemental nitrogen and Oxygen excess is
retained.

Note Sulfur and halogenated compounds (Chlorine, Bromine, etc.), possibly present in
the sample, do not affect the analysis, since the silvered cobaltous/cobaltic oxide catalyst
holds back both SO2 and halogens.

Then the gas mixture (N2, CO2 and H2O) flows into the chromatographic column CC1,
where separation takes place.
The eluted gases are conveyed to the thermal conductivity detector TCD that generates
electrical signals, which properly processed by the Eager Xperience software provide Nitrogen,
Carbon and Hydrogen percentages.

112 Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific

 8 Analytical Methods
Analytical Method for CHN-O Configuration

Analytical Method for CHN-O Configuration

CHN Determination: An autosampler AS is connected to a quartz reactor R1 placed in an
furnace at a temperature of 900 °C. This reactor is connected to the analytical column CC1,
on its turn connected to a channel of the thermal conductivity detector TCD.

Oxygen Determination: A second autosampler AS is connected to a reactor R2 placed in an

furnace at a temperature of 1060 °C. An adsorption filter F is connected to the reactor outlet.
The F outlet is connected to the analytical column CC2, on its turn connected to the other
channel of the thermal conductivity detector TCD.

Figure 71. Instrument parts diagram and pneumatic diagram for CHN-O determination

S2

EVP2 1

F He PRV1
2 He
PI1
(5)

F
IN OUT (6)
F O2 PRV2 O2
EV1 2 PI2
CC2 TCD
IN OUT (7) F
3 1
6,5 cc/min.
CC1 300 kPa
EV3 1 EV4 1
3 1

2 2
EV2 2
4 VENT (4)
S1
1 SAMPLER
AS 2 EVP1 1
(1)
F1

2
3 CARRIER (2)
EFC - T

R2 R1

Pneumatic Diagram Description

Helium He flows to the flow sensor S1, through the solenoid valve EV2, and directly to the
flow sensor S2. Both flow sensors are connected to relevant proportional valves EVP1 and
EVP2.

The proportional valve EVP1, connected to the autosampler AS, controls the Helium flow
through the whole pneumatic circuit as far as the solenoid valve EV3.

Thermo Scientific Flash 2000 Elemental Analyzer - Operating Manual 113

8 Analytical Methods
Analytical Method for CHN-O Configuration

This valve, normally open, exhausts Helium to the atmosphere through Vent 4.
The proportional valve EVP2 controls Helium flowing to the circuit comprising R2, F and
CC2 as far as the solenoid valve EV4. This valve, normally open, allows Helium to reach point
1 of the autosampler and purge the area where the sample is housed.

Note When two autosamplers are installed on the elemental analyzer, the point 1 (purge)
must be connected to the autosampler that you intend to use for the analysis.

When a single autosampler is installed, to pass from the CHN configuration to the O
Configuration, or vice-versa, change the position of the autosampler from R1 to R2 or
voice-overs. The Oxygen line O2 is connected to the solenoid valve EV1.This valve controls
the Oxygen inlet.

Sequence of the Method Stages

CHN Determination
During pre-analysis, the solenoid valve EV1 shuts off the Oxygen flow, whereas the solenoid
valve EV2 allows Helium to flow in the circuit. When Start Analysis is pressed, the valve EV1
opens, whereas the valve EV2 switches to allow Oxygen to flow in as far as the combustion
reactor R1 for a preset time.
After a few seconds the sample, weighed in a tin container and stored in the autosampler, is
dropped into the combustion reactor.
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, valves EV1 and EV2 return
to their original position restoring Helium flow.
The combustion products are conveyed across the reactor R1, where oxidation is completed.
Nitrogen oxides possibly formed are reduced to elemental nitrogen, and Oxygen excess is
retained.

Note Sulfur and halogenated compounds (Chlorine, Bromine, etc.), possibly present in
the sample, do not affect the analysis, since the silvered cobaltous/cobaltic oxide catalyst
holds back both SO2 and halogens.

Then the gas mixture (N2, CO2 and H2O) flows into the chromatographic column CC1,
where separation takes place. The eluted gases are conveyed to the thermal conductivity
detector TCD that generates electrical signals, which properly processed by the Eager 300
software provide Nitrogen, Carbon and Hydrogen percentages.

Oxygen Determination
No switching of valves. When Start Analysis is pressed, the sample, weighed in a silver
container and stored in the autosampler, is dropped into the reactor R2 where it undergoes
instant pyrolysis. During pyrolysis, N2, CO and H2 form. The pyrolysis products cross the
adsorption filter F where halogenated compounds (Chlorine, Bromine, etc.) are retained.
The gas mixture flows into the chromatographic column CC2, where carbon monoxide is
separated from other gases.
Then the eluted gases are conveyed to the thermal conductivity detector TCD that generates an
electrical signal, which properly processed by the Eager Xperience software provides Oxygen
percentage.

114 Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific

 8 Analytical Methods
Analytical Method for CHNS Configuration

Analytical Method for CHNS Configuration

An autosampler AS is connected to a quartz reactor R1 placed in an furnace at a temperature
of 900 °C. This reactor is connected to the analytical column CC, on its turn connected to a
channel of the thermal conductivity detector TCD.

Figure 72. Instrument parts diagram and pneumatic diagram for CHNS determination

S2

EVP2 1

F He PRV1
2 He
PI1
(5)

F F O2 PRV2
IN OUT (6) O2
EV1 2 PI2
TCD
IN OUT (7) F
3 1
6,5 cc/min.
CC 300 kPa
EV3 1 EV4 1
3 1

2 2
EV2 2
4
VENT (4)
S1
1 SAMPLER
AS 2 EVP1 1
(1)

2
F1 CARRIER (2)
EFC - T

R1

Pneumatic Diagram Description

Helium He flows to the flow sensor S1, through the solenoid valve EV2, and directly to the
flow sensor S2. Both flow sensors are connected to relevant proportional valves EVP1 and
EVP2.
The proportional valve EVP1, connected to the autosampler AS, controls the helium flow
through the whole pneumatic circuit as far as the solenoid valve EV3. This valve, normally
open, exhausts Helium to the atmosphere through Vent 4.
The proportional valve EVP2, connected to the detector reference channel TCD, controls the

Thermo Scientific Flash 2000 Elemental Analyzer - Operating Manual 115

8 Analytical Methods
Analytical Method for CHNS Configuration

Helium flow as far as the solenoid valve EV4. This valve, normally open, allows Helium to
reach point 1 of the autosampler and purge the zone where the sample is housed.
The Oxygen line O2 is connected to the solenoid valve EV1.
This valve controls the Oxygen inlet.

Sequence of the Method Stages

During pre-analysis, the solenoid valve EV1 shuts off the Oxygen flow, whereas the solenoid
valve EV2 allows Helium to flow in the circuit.
When Start Analysis is pressed, the valve EV1 opens, whereas the valve EV2 switches to allow
Oxygen to flow in as far as the combustion reactor R1 for a preset time.
After a few seconds the sample, weighed in a tin container and placed in the autosampler, is
dropped into the combustion reactor. 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 valves EV1 and EV2 return to their
original position restoring the Helium flow. The combustion products are conveyed across the
reactor R1 where oxidation is completed. Nitrogen oxides and sulfur trioxide, possibly
formed, are reduced to elemental nitrogen and sulfur dioxide, and the Oxygen excess is
retained.
Then the gas mixture (N2, CO2, H2O e SO2) flows into the chromatographic column CC1
where separation takes place. The eluted gases are sent to the thermal conductivity detector
TCD that generates electrical signals, which, properly processed by the Eager Xperience
software, provide the percentages of Nitrogen, Carbon, Hydrogen and Sulfur contained in the
sample.

116 Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific

 8 Analytical Methods
Analytical Method for CHNS-O Configuration

Analytical Method for CHNS-O Configuration

CHNS Determination: An autosampler AS is connected to a quartz reactor R1 placed in an
furnace at the temperature of 900 °C. This reactor is connected to the analytical column CC1,
on its turn connected to a channel of the thermal conductivity detector TCD.

Oxygen Determination: A second autosampler AS is connected to a reactor R2 placed in an

furnace at the temperature of 1060 °C. To the reactor outlet an adsorption filter F is
connected. The F outlet is connected to the analytical column CC2, on its turn connected to
the other channel of the thermal conductivity detector TCD.

Figure 73. Instrument parts diagram and pneumatic diagram for CHNS-O determination

S2

EVP2 1

F He PRV1
2 He
PI1
(5)

F
IN OUT (6)
F O2 PRV2 O2
EV1 2 PI2
CC2 TCD
IN OUT (7) F
3 1
6,5 cc/min.
CC1 300 kPa
EV3 1 EV4 1
3 1

2 2
EV2 2
4 VENT (4)
S1
1 SAMPLER
AS 2 EVP1 1
(1)
F1

2
3 CARRIER (2)
EFC - T

R2 R1

Pneumatic Diagram Description

Helium He flows to the flow sensor S1, through the solenoid valve EV2, and directly to the
flow sensor S2. Both flow sensors are connected to relevant proportional valves EVP1 and
EVP2.
The proportional valve EVP1, connected to the autosampler AS, controls the Helium flow

Thermo Scientific Flash 2000 Elemental Analyzer - Operating Manual 117

8 Analytical Methods
Analytical Method for CHNS-O Configuration

through the pneumatic circuit as far as the solenoid valve EV3. This valve, normally open,
exhausts Helium to the atmosphere through Vent 4.
The proportional valve EVP2 controls the Helium flow in the circuit comprising R2, F and
CC2 as far as the solenoid valve EV4. This valve, normally open, allows Helium to reach point
1 of the autosampler and purge the area where the sample is housed.

Note When two autosamplers are installed on the elemental analyzer, the point 1 (purge)
must be connected to the autosampler that you intend to use for the analysis.

When a single autosampler is installed, to pass from the CHNS configuration to the O
Configuration, or vice-versa, change the position of the autosampler from R1 to R2 or
vice-versa. The Oxygen line O2 is connected to the solenoid valve EV1. This valve controls the
Oxygen inlet.

Sequence of the Method Stages

CHNS Determination
During pre-analysis the solenoid valve EV1 shuts off the Oxygen flow, whereas the solenoid
valve EV2 allows Helium to flow in the circuit. When Start Analysis is pressed, the valve EV1
opens, whereas the valve EV2 switches to allow Oxygen to flow in as far as the combustion
reactor R1 for a preset time.
After a few seconds the sample, weighed in a tin container and stored in the autosampler. is
dropped into the combustion reactor.
Tin, coming in contact with an extremely oxidizing environment, triggers a strong exothermic
reaction. Temperature reaches approximately 1800 °C instantly causing the sample
combustion. At the end of the time set for Oxygen introduction, the valves EV1 and EV2
return to their original position restoring the Helium flow.
The combustion products are conveyed across the reactor R1 where oxidation is completed.
Nitrogen oxides and sulfur trioxide possibly formed are reduced to elemental nitrogen and
sulfur dioxide, and Oxygen excess is retained.
Then the gas mixture (N2, CO2, H2O e SO2) flows into the gas chromatographic column
CC1 where separation occurs.
The eluted gases are conveyed to the thermal conductivity detector TCD that generates
electrical signals, which, properly processed by the Eager 300 software, provide the Nitrogen,
Carbon, Hydrogen and Sulfur percentages contained in the sample.

Oxygen Determination
No switching of valves. When Start Analysis is pressed, the sample, weighed in a silver
container and stored in the autosampler, is dropped into the reactor R2 where it undergoes
instant pyrolysis.
During pyrolysis, N2, CO and H2 form. The pyrolysis products cross the adsorption filter F
where halogenated compounds (Chlorine, Bromine, etc.) are retained.
The gas mixture flows into the chromatographic columns CC2 where carbon monoxide is
separated from the other gases.
Then the eluted gases are conveyed to the thermal conductivity detector TCD that generates an
electrical signal, which, properly processed by the Eager Xperience software, provides the
Oxygen percentage.

118 Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific

 8 Analytical Methods
Analytical Method for S (Sulfur) Configuration

Analytical Method for S (Sulfur) Configuration

An autosampler AS is connected to a reactor R1 placed in an furnace at the temperature of
900°C. To the reactor outlet an adsorption filter F1 is connected. The F1 outlet is connected
to the analytical column CC, on its turn connected to the thermal conductivity detector TCD.

Figure 74. Instrument parts diagram and pneumatic diagram for S (Sulfur) determination

S2

EVP2 1

F He PRV1
2 He
PI1
(5)

F F O2 PRV2
IN OUT (6) O2
EV1 2 PI2
TCD
IN OUT (7) F
3 1
6,5 cc/min.
CC 300 kPa
EV3 1 EV4 1
3 1

2 2
EV2 2
4
VENT (4)
S1
1 SAMPLER
AS 2 EVP1 1
(1)

2
F1 CARRIER (2)
EFC - T

R1

Pneumatic Diagram Description

Helium He flows to the flow sensor S1, through the solenoid valve EV2, and directly to the
flow sensor S2. Both flow sensors are connected to the relevant proportional valves EVP1 and
EVP2.
The proportional valve EVP1, connected to the autosampler AS, controls the Helium flow in
the whole pneumatic circuit as far as the solenoid valve EV3. This valve, normally open,
exhausts Helium to the atmosphere through Vent 4.
The proportional valve EVP2, connected to the detector reference channel TCD, controls the
Helium flow as far as the solenoid valve EV4. This valve, normally open, allows Helium to
reach point 1 of the autosampler and purge the zone where the sample is housed.

Thermo Scientific Flash 2000 Elemental Analyzer - Operating Manual 119

8 Analytical Methods
Analytical Method for S (Sulfur) Configuration

The Oxygen line O2 is connected to the solenoid valve EV1.

This valve controls the Oxygen inlet.

Sequence of the Method Stages

During pre-analysis the solenoid valve EV1 shuts off Oxygen flow, whereas the solenoid valve
EV2 allows Helium to flow in the circuit.

When Start Analysis is pressed, the valve EV1 opens, whereas the valve EV2 switches to allow
Oxygen to flow in as far as the combustion reactor R1 for a preset time.
After a few seconds, the sample, weighed in a tin container and stored in the autosampler, is
dropped into the combustion reactor.

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 valves EV1 and EV2 return to their
original position restoring the Helium flow. The combustion products are conveyed across the
reactor R1 where oxidation is completed. Nitrogen oxides and sulfur trioxide possibly formed
are reduced to elemental nitrogen and sulfur dioxide, and the Oxygen excess is retained.
Then the gas mixture (N2, CO2, H2O and SO2) flows through the adsorption filter F1,
which retains water, then into the chromatographic column CC1 where separation takes place.
The eluted gases are conveyed to the thermal conductivity detector TCD that generates an
electrical signal, which, properly processed by the Eager Xperience software, provides the
Sulfur percentage.

120 Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific

 8 Analytical Methods
Analytical Method for O (Oxygen) Configuration

Analytical Method for O (Oxygen) Configuration

An autosampler AS is connected to a reactor R1 placed in an furnace at the temperature of
1060 °C. To the reactor outlet an adsorption filter F1 is connected. The filter F1 outlet is
connected to the analytical column CC, on its turn connected to the thermal conductivity
detector TCD.

Figure 75. Instrument parts diagram and pneumatic diagram for O (Oxygen) determination

S2

EVP2 1

F He PRV1
2 He
PI1
(5)

F F O2 PRV2
IN OUT (6) O2
EV1 2 PI2
TCD
IN OUT (7) F
3 1
6,5 cc/min.
CC 300 kPa
EV3 1 EV4 1
3 1

2 2
EV2 2
4
VENT (4)
S1
1 SAMPLER
AS 2 EVP1 1
(1)

2
F1 CARRIER (2)
EFC - T

R1

Pneumatic Diagram Description

Helium He flows to the flow sensor S1, through the solenoid valve EV2, and directly to the
flow sensor S2. Both flow sensors are connected to the relevant proportional valves EVP1 and
EVP2.
The proportional valve EVP1, connected to the autosampler AS, controls the Helium flow in
the whole pneumatic circuit as far as the solenoid valve EV3. This valve, normally open,
exhausts Helium to the atmosphere through Vent 4. The proportional valve EVP2, connected
to the detector reference channel TCD, controls the Helium flow as far as the solenoid valve
EV4.

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8 Analytical Methods
Analytical Method for O (Oxygen) Configuration

This valve, normally open, allows Helium to reach point 1 of the autosampler and purge the
zone where the sample is housed.
The Oxygen line O2 is connected to the solenoid valve EV1. This valve controls the Oxygen
inlet.

Sequence of the Method Stages

No switching of valves. When Start Analysis is pressed, the sample, weighed in a tin container
and stored in the autosampler, is dropped into the reactor R1 where it undergoes instant
pyrolysis.
During pyrolysis, N2, CO and H2 form. The pyrolysis products cross the adsorption filter F
where halogenated compounds (Chlorine, Bromine, etc.) are retained.
The gas mixture flows into the chromatographic column CC where carbon monoxide is
separated from the other gases.
Then the eluted gases are conveyed to the thermal conductivity detector TCD that generates an
electrical signal, which, properly processed by the Eager Xperience software, provides the
Oxygen percentage.

122 Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific

 8 Analytical Methods
Analytical Method for N (Nitrogen) Configuration

Analytical Method for N (Nitrogen) Configuration

An autosampler AS is connected to a quartz reactor R1 placed in an furnace at the
temperature of 900 °C. This reactor, on its turn, is connected in series to a second reactor R2
placed in an furnace at the temperature of 680 °C. To the reactor R2 outlet two filters F1 e F2
are connected in series. The filter F2 outlet is connected to the analytical column CC, on its
turn connected to the thermal conductivity detector TCD.

Figure 76. Instrument parts diagram and pneumatic diagram for N (Nitrogen) determination

S2

EVP2 1

F He PRV1
2 He
PI1
(5)

F F O2 PRV2
IN OUT (6) O2
EV1 2 PI2
TCD
IN OUT (7) F
3 1
6,5 cc/min.
CC 300 kPa
EV3 1 EV4 1
3 1

F2
2 2
EV2 2
VENT (4)
4 CP S1
1 SAMPLER
AS 2 EVP1 1
(1)

2
F1 EFC - T
CARRIER (2)

R2 R1

Pneumatic Diagram Description

Helium He flows to the flow sensor S1, through the solenoid valve EV2, and directly to the
flow sensor S2. Both flow sensors are connected to the relevant proportional valves EVP1 and
EVP2. The proportional valve EVP1, connected to the autosampler AS, controls the Helium
flow in the whole pneumatic circuit as far as the solenoid valve EV3. This valve, normally
open, exhausts Helium to the atmosphere through Vent 4.

Thermo Scientific Flash 2000 Elemental Analyzer - Operating Manual 123

8 Analytical Methods
Analytical Method for N (Nitrogen) Configuration

The proportional valve EVP2, connected to the detector reference channel TCD, controls the
helium flow as far as the solenoid valve EV4.
This valve, normally open, allows Helium to reach point 1 of the autosampler and purge the
zone where the sample is housed. The Oxygen line O2 is connected to the solenoid valve EV1.
This valve controls the Oxygen inlet.

Sequence of the Method Stages

During pre-analysis the solenoid valve EV1 shuts off Oxygen, whereas the solenoid valve EV2
allows Helium to flow in the circuit.

When Start Analysis is pressed, the valve EV1 opens, whereas the valve EV2 switches to allow
Oxygen to flow in as far as the combustion reactor R1 for a preset time. After a few seconds,
the sample, weighed in a tin container and stored in the autosampler, is dropped into the
combustion reactor. 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 valves EV1 and EV2 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 the oxidation of components 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.
Then the gas mixture passes across the two adsorption filters F1 e F2 connected in series. The
first filter holds back carbon and sulfur dioxides, whereas the second filter retains water.
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 the
Eager Xperience software, provides the Nitrogen percentage.

124 Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific

 8 Analytical Methods
Analytical Method for NC Configuration

Analytical Method for NC Configuration

An autosampler AS is connected to a quartz reactor R1 placed in an furnace at the
temperature of 900 °C. This reactor, on its turn, is connected in series to a second reactor R2
placed in an furnace at the temperature of 680 °C. To the R2 outlet an adsorption filter F1 is
connected. The filter F1 outlet is connected to the analytical column CC, on its turn
connected to the thermal conductivity detector TCD.

Figure 77. Instrument parts diagram and pneumatic diagram for NC determination

S2

EVP2 1

F He PRV1
2 He
PI1
(5)

F F O2 PRV2
IN OUT (6) O2
EV1 2 PI2
TCD
IN OUT (7) F
3 1
6,5 cc/min.
CC 300 kPa
EV3 1 EV4 1
3 1

F2
2 2
EV2 2
VENT (4)
4 CP S1
1 SAMPLER
AS 2 EVP1 1
(1)

2
F1 EFC - T
CARRIER (2)

R2 R1

Pneumatic Diagram Description

Helium He flows to the flow sensor S1, through the solenoid valve EV2, and directly to the
flow sensor S2. Both flow sensors are connected to relevant proportional valves EVP1 and
EVP2. The proportional valve EVP1, connected to the autosampler AS, controls the Helium
flow in the whole pneumatic circuit as far as the solenoid valve EV3. This valve, normally
open, exhausts Helium to the atmosphere through Vent 4.

Thermo Scientific Flash 2000 Elemental Analyzer - Operating Manual 125

8 Analytical Methods
Analytical Method for NC Configuration

The proportional valve EVP2, connected to the detector reference channel TCD, controls the
Helium flow as far as the solenoid valve EV4.
This valve, normally open, allows Helium to reach point 1 of the autosampler and purge the
zone where the sample is housed. The Oxygen line O2 is connected to the solenoid valve EV1.
This valve controls the Oxygen inlet.

Sequence of the Method Stages

During pre-analysis the solenoid valve EV1 shuts off Oxygen, whereas the solenoid valve EV2
allows Helium to flow in the circuit. When Start Analysis is pressed, the valve EV1 opens,
whereas the valve EV2 switches to allow Oxygen to flow in as far as the combustion reactor R1
for a preset time.
After a few seconds, the sample. weighed in a tin container and stored in the autosampler, is
dropped into the combustion reactor.
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 valves EV1 and EV2 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 the oxidation of components 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.

Note Sulfur and halogenated compounds (Chlorine, Bromine, etc.), possibly present in
the sample, do not affect analysis, since the silver-plated cobalt oxide catalyst holds back
both SO2 and halogens.

The gas mixture then crosses the adsorption filter F1 that retains water. Nitrogen and carbon
are eluted in the chromatographic column CC and then conveyed to the thermal conductivity
detector TCD that generates electrical signals, which, properly processed by the Eager
Xperience software, provide the Nitrogen and Carbon percentages.

126 Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific

 8 Analytical Methods
Analytical Method for NCS Configuration

Analytical Method for NCS Configuration

An autosampler AS is connected to a reactor R1 placed in an furnace at the temperature of
900 °C. To the reactor outlet an adsorption filter F1 is connected. The filter F1 outlet is
connected to the analytical column CC, on its turn connected to the thermal conductivity
detector TCD.

Figure 78. Instrument parts diagram and pneumatic diagram for NCS determination

S2

EVP2 1

F He PRV1
2 He
PI1
(5)

F F O2 PRV2
IN OUT (6) O2
EV1 2 PI2
TCD
IN OUT (7) F
3 1
6,5 cc/min.
CC 300 kPa
EV3 1 EV4 1
3 1

2 2
EV2 2
4
VENT (4)
S1
1 SAMPLER
AS 2 EVP1 1
(1)

2
F1 CARRIER (2)
EFC - T

R1

Pneumatic Diagram Description

Helium He flows to the flow sensor S1, through the solenoid valve EV2, and directly to the
flow sensor S2. Both flow sensors are connected to relevant proportional valves EVP1 and
EVP2.
The proportional valve EVP1, connected to the autosampler AS, controls the Helium flow in
the whole pneumatic circuit as far as the solenoid valve EV3. This valve, normally open,
exhausts Helium to the atmosphere through Vent 4.
The proportional valve EVP2, connected to the detector reference channel TCD, controls the
Helium flow as far as the solenoid valve EV4. This valve, normally open, allows Helium to
reach point 1 of the autosampler and purge the zone where the sample is housed.

Thermo Scientific Flash 2000 Elemental Analyzer - Operating Manual 127

8 Analytical Methods
Analytical Method for NCS Configuration

The Oxygen line O2 is connected to the solenoid valve EV1. This valve controls the Oxygen
inlet.

Sequence of the Method Stages

During pre-analysis the solenoid valve EV1 shuts off Oxygen, whereas the solenoid valve EV2
allows Helium to flow in the circuit. When Start Analysis is pressed, the valve EV1 opens,
whereas the valve EV2 switches to allow Oxygen to flow in as far as the combustion reactor R1
for a preset time.
After a few seconds, the sample. weighed in a tin container and stored in the autosampler, is
dropped into the combustion reactor.
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 valves EV1 and EV2 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.
Nitrogen oxides and sulfur trioxide possibly formed are converted into elemental nitrogen and
sulfur dioxide, and the Oxygen excess is retained.
Then the gas mixture (N2, CO2, H2O and SO2) crosses the adsorption filter F1 that retains
water, and flows to the chromatographic column CC1 where separation occurs.
The eluted gases are conveyed to the thermal conductivity detector TCD that generates
electrical signals, which, properly processed by the Eager Xperience software, provide
Nitrogen, Carbon and Sulfur percentages.

128 Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific

 8 Analytical Methods
Analytical Method for NC-Soils, NC-Sediments and NC-Filters Configurations

Analytical Method for NC-Soils, NC-Sediments and NC-Filters

Configurations
An autosampler AS is connected to a steel reactor R1 placed in an furnace at the temperature
of 900 °C. This reactor on its turn is connected to a second reactor R2 placed in an furnace at
the temperature of 680 °C. To the R2 outlet an adsorption filter F1 is connected. The filter
F1 outlet is connected to the analytical column CC, on its turn connected to the thermal
conductivity detector TCD.

Figure 79. Instrument parts diagram and pneumatic diagram for NC-Soils, Sediments and Filters determination

S2

EVP2 1

F He PRV1
2 He
PI1
(5)

F F O2 PRV2
IN OUT (6) O2
EV1 2 PI2
TCD
IN OUT (7) F
3 1
6,5 cc/min.
CC 300 kPa
EV3 1 EV4 1
3 1

F2
2 2
EV2 2
4 VENT (4) CP S1
1 SAMPLER
AS 2 EVP1 1
(1)

2
F1 CARRIER (2) EFC - T

R2 R1

Pneumatic Diagram Description

Helium He flows to the flow sensor S1, through the solenoid valve EV2, and directly to the
flow sensor S2. Both flow sensors are connected to relevant proportional valves EVP1 and
EVP2. The proportional valve EVP1, connected to the autosampler AS, controls the Helium
flow in the whole pneumatic circuit as far as the solenoid valve EV3. This valve, normally
open, exhausts Helium to the atmosphere through Vent 4.

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8 Analytical Methods
Analytical Method for NC-Soils, NC-Sediments and NC-Filters Configurations

The proportional valve EVP2, connected to the detector reference channel TCD, controls the
helium flow as far as the solenoid valve EV4. This valve, normally open, allows Helium to
reach point 1 of the autosampler and purge the zone where the sample is housed. The Oxygen
line O2 is connected to the solenoid valve EV1. This valve controls the Oxygen inlet.

Sequence of the Method Stages

During pre-analysis the solenoid valve EV1 shuts off Oxygen, whereas the solenoid valve EV2
allows Helium to flow in the circuit. When Start Analysis is pressed, the valve EV1 opens,
whereas the valve EV2 switches to allow Oxygen to flow in as far as the combustion reactor R1
for a preset time.
After a few seconds, the sample, weighed in a tin container and stored in the autosampler, is
dropped into the combustion reactor.
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 valves EV1 and EV2 return to their
original position restoring the Helium flow.
The gas mixture (N2, CO2, H2O e 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. Then the gas mixture crosses the adsorption filter F1 which retains water.
Nitrogen and Carbon are then eluted in the chromatographic column CC and conveyed to
the thermal conductivity detector TCD that generates electrical signals, which, properly
processed by the Eager Xperience software, provide the Nitrogen and carbon percentages
contained in the sample.

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 8 Analytical Methods
Analytical Method for N Lubricant, N/Protein and N-Brew Configurations

Analytical Method for N Lubricant, N/Protein and N-Brew

Configurations
An autosampler AS is connected to a steel reactor R1 placed in an furnace at the temperature
of 950 °C. This reactor on its turn is connected to a second reactor R2 placed in an furnace at
the temperature of 840 °C. To the R2 outlet two filters F1 and F2 are connected in series.
The filter F2 outlet is connected to the analytical column CC, on its turn connected to the
thermal conductivity detector TCD.

Figure 80. Instrument parts diagram and pneumatic diagram for N-Lubricant, N/Protein and N-Brew determination

S2

EVP2 1

F He PRV1
2 He
PI1
(5)

F F O2 PRV2
IN OUT (6) O2
EV1 2 PI2
TCD
IN OUT (7) F
3 1
6,5 cc/min.
CC 300 kPa
EV3 1 EV4 1
3 1

F2
2 2
EV2 2
4 VENT (4) CP S1
1 SAMPLER
AS 2 EVP1 1
(1)

2
F1 CARRIER (2) EFC - T

R2 R1

Pneumatic Diagram Description

Helium He flows to the flow sensor S1, through the solenoid valve EV2, and directly to the
flow sensor S2. Both flow sensors are connected to relevant proportional valves EVP1 and
EVP2.

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8 Analytical Methods
Analytical Method for N Lubricant, N/Protein and N-Brew Configurations

The proportional valve EVP1, connected to the autosampler AS, controls the Helium flow in
the whole pneumatic circuit as far as the solenoid valve EV3. This valve, normally open,
exhausts Helium to the atmosphere through Vent 4. The proportional valve EVP2, connected
to the detector reference channel RF, controls the Helium flow as far as the solenoid valve EV4.
This valve, normally open, allows Helium to reach the point 1 of the autosampler and purge
the zone where the sample is housed. The Oxygen line O2 is connected to the solenoid valve
EV1. This valve controls the Oxygen inlet.

Sequence of the Method Stages

During pre-analysis the solenoid valve EV1 shuts off Oxygen, whereas the solenoid valve EV2
allows Helium to flow in the circuit. When Start Analysis is pressed, the valve EV1 opens,
whereas the valve EV2 switches to allow Oxygen to flow in as far as the combustion reactor R1
for a preset time.
After a few seconds, the sample, weighed in a tin container and stored in the autosampler, is
dropped into the combustion reactor.
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 valves EV1 and EV2 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.
Then the gases pass through the two adsorption filters F1 and F2 connected in series. The
first filter retains carbon and sulfur dioxides, whereas the second filter holds back water.
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 the
Eager Xperience software, provides the nitrogen-protein percentage.

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 8 Analytical Methods
Analytical Method for NC-IRMS Configuration

Analytical Method for NC-IRMS Configuration

An autosampler AS is connected to a quartz reactor R1 placed in an furnace at the
temperature of 900 °C. This reactor, on its turn, is connected in series to a second reactor R2
placed in an furnace at the temperature of 680 °C. To the R2 outlet an adsorption filter F1 is
connected. The filter F1 outlet is connected to the analytical column CC, on its turn
connected to the thermal conductivity detector TCD, the continuous flow interface CFI and
to the isotopic ratio mass spectrometer IRMS.

Figure 81. Instrument parts diagram and pneumatic diagram for NC-IRMS determination

S2

EVP2 1

F He PRV1
2 He
PI1
(5)

(OSR) F
IN OUT (6)
F O2 PRV2 O2
EV1 2 PI2
CC TCD
IN OUT (7) F
3 1
6,5 cc/min.
(OCR) 300 kPa
EV3 1 EV4 1
3 1

2 2
EV2 2

AS S1
F2 VENT (4)
4
EVP1 1
1 SAMPLER (1)
2
2
3 CARRIER (2)
EFC - T

R2 R1

Pneumatic Diagram Description

Helium He flows to the flow sensor S1, through the solenoid valve EV2, and directly to the
flow sensor S2. Both flow sensors are connected to relevant proportional valves EVP1 and
EVP2. The proportional valve EVP1, connected to the autosampler AS, controls the Helium
flow in the whole pneumatic circuit as far as the solenoid valve EV3. This valve, normally
open, exhausts Helium to the atmosphere through Vent 4.

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8 Analytical Methods
Analytical Method for NC-IRMS Configuration

The proportional valve EVP2, connected to the detector reference channel TCD, controls the
Helium flow as far as the solenoid valve EV4.
This valve, normally open, allows Helium to reach point 1 of the autosampler and purge the
zone where the sample is housed. The Oxygen line O2 is connected to the solenoid valve EV1.
This valve controls the Oxygen inlet.

Sequence of the Method Stages

During pre-analysis the solenoid valve EV1 shuts off Oxygen, whereas the solenoid valve EV2
allows Helium to flow in the circuit. When Start Analysis is pressed, the valve EV1 opens,
whereas the valve EV2 switches to allow Oxygen to flow in as far as the combustion reactor R1
for a preset time.
After a few seconds, the sample. weighed in a tin container and stored in the autosampler, is
dropped into the combustion reactor.
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 valves EV1 and EV2 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 the oxidation of components 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.

Note Sulfur and halogenated compounds (Chlorine, Bromine, etc.), possibly present in
the sample, do not affect analysis, since the silver-plated cobalt oxide catalyst holds back
both SO2 and halogens.

The gas mixture then crosses the adsorption filter F2 that retains water. Nitrogen and carbon
are eluted in the chromatographic column CC and then conveyed to the thermal conductivity
detector TCD (it generates electrical signals which, properly processed by the Eager Xperience
software, provide the Nitrogen and Carbon percentages) to the CFI device.and to the IRMS
detector.

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 8 Analytical Methods
Analytical Method for NC-HT Configuration

Analytical Method for NC-HT Configuration

IMPORTANT Only the NC configuration is considered

An autosampler AS is connected to a quartz reactor R2 placed in the right furnace at the

temperature of 950 °C. To the R2 outlet an adsorption filter F2 is connected. The filter F2
outlet is connected to the analytical column CC2, on its turn connected to the thermal
conductivity detector TCD, the continuous flow interface CFI and to the isotopic ratio mass
spectrometer IRMS.

Figure 82. Instrument parts diagram and pneumatic diagram for NC-HT determination

EVP2 1
S2 F Nitrogen and Carbon Configuration
2
To ConFlow III
(5) AS AS
F 2 3
F
(6)
EV1 2
Right Furnace 0 ..1100 ˚ C
Left Furnace 0 ..1450 ˚ C

(7) F
3 1
6,5 cc/min.
300 kPa
EV3 1 EV4 1
Out 1

Out 4
3 1
Column

2 2
2
TCD
(4) EV2
S1
Column

EVP1 1
(1)
He Input
2
(2) O 2 Input H2O TRAP
O2 He
Reference
2 5
PI2 PI1
Carrier
A
6 1

7 4
B PRV2 PRV1 EFC-T

O2 He

Pneumatic Diagram Description

Helium He flows to the flow sensor S1, through the solenoid valve EV2, and directly to the
flow sensor S2. Both flow sensors are connected to relevant proportional valves EVP1 and
EVP2. The proportional valve EVP1, connected to the autosampler AS, controls the Helium
flow in the whole pneumatic circuit as far as the solenoid valve EV3. This valve, normally
open, exhausts Helium to the atmosphere through Vent 4.

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8 Analytical Methods
Analytical Method for NC-HT Configuration

The proportional valve EVP2, connected to the detector reference channel TCD, controls the
Helium flow as far as the solenoid valve EV4. This valve, normally open, allows Helium to
reach point 1 of the autosampler and purge the zone where the sample is housed. The Oxygen
line O2 is connected to the solenoid valve EV1. This valve controls the Oxygen inlet.

Sequence of the Method Stages

During pre-analysis the solenoid valve EV1 shuts off Oxygen, whereas the solenoid valve EV2
allows Helium to flow in the circuit. When Start Analysis is pressed, the valve EV1 opens,
whereas the valve EV2 switches to allow Oxygen to flow in as far as the combustion reactor R2
for a preset time.
After a few seconds, the sample. weighed in a tin container and stored in the autosampler, is
dropped into the combustion reactor. 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 valves EV1 and EV2 return to their
original position restoring the Helium flow. The gas mixture generated by combustion is
conveyed across the reactor R2 where the oxidation of components is completed.

Note Sulfur and halogenated compounds (Chlorine, Bromine, etc.), possibly present in
the sample, do not affect analysis, since the silver-plated cobalt oxide catalyst holds back
both SO2 and halogens.

The gas mixture then crosses the adsorption filter F2 that retains water. Nitrogen and carbon
are eluted in the chromatographic column CC2 and then conveyed to the thermal
conductivity detector TCD (it generates electrical signals which, properly processed by the
Eager Xperience software, provide the Nitrogen and Carbon percentages) to the CFI
device.and to the IRMS detector.

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 Part 1

Analysis
 9

Instrument Start-up

Contents
• Introduction
• Powering on the System
• Installation of Eager Xperience
• Eager Xperience Main Menu
• Analytical Configuration
• Leak Test
• Detector Signal Level

Introduction
To analyze any type of sample the instrument must be in the correct operating conditions.

Proceed according to the following operating sequences:

• Powering on
• Installation of Eager Xperience software into the PC
• Analytical configuration
• Leak checking
• Adjustment of the detector signal level

CAUTION Before starting the operating sequences, make sure that instrument, reactors,
adsorption filters, autosampler (or manual injection device for liquids) and any
complementary units are properly installed as described in previous chapters.

Powering on the System

Switch on the instrument lifting the breaker located at the back of the instrument (position I).
At the powering on, the indicating LED Power On on the synoptic panel light up. Switch on
the computer and any complementary units by means of relevant switches.

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9 Instrument Start-up
Installation of Eager Xperience

Installation of Eager Xperience

 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 83 is displayed.

Figure 83. 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 84 is displayed.
Figure 84. 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

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 9 Instrument Start-up
Eager Xperience Main Menu

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 FlashEA.
7. Follow the prompted indications. At the end of the installation, the Main Menu is
displayed.

Eager Xperience Main Menu

The Main Menu of Eager Xperience, shown in Figure 85, is the starting point to enter all
menus and relevant functions. Menus and icons of Main Menu are described in the following
Table 41 and Table 42 respectively.

Figure 85. Eager Xperience Main Menu

Table 41. 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

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9 Instrument Start-up
Eager Xperience Main Menu

Table 41. Main Menu: description of the menus, continued

Menu Description Submenus and Options
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
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 42. Main Menu: description of the icons

Icon Function Description
Load method Use this icon to load a previously saved analytical
method.

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 9 Instrument Start-up
Eager Xperience Main Menu

Table 42. Main Menu: description of the icons, continued

Icon Function Description
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.
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.

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9 Instrument Start-up
Analytical Configuration

Analytical Configuration
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.

 To Configure the Analyzer

1. In Main Menu of Figure 85 on page 141, choose File > Instrument Configuration. The
following window is displayed.

Figure 86. 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 the configuration of your
instrument.

CAUTION NCS, CHN, CHNS, Sulfur and Oxygen configurations use the LEFT furnace
only. Do not set any temperature for the RIGHT furnace.

Note The option Undefined can be used in case the desired operating conditions
are different from those defined for the instrument configuration.

c. If the instrument is coupled with an IRMS detector, check the function Simple
Instrument control for IRMS. At the reboot of Eager Xperience, the simplified
Main Menu for IRMS is visualized as shown in Figure 87.

Figure 87. Main menu for IRMS

d. Click Elemental analyzer setup to enter the dialog window of Figure 88 where the
configuration parameters have to be set.

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 9 Instrument Start-up
Analytical Configuration

Figure 88. Configuration dialog window

e. In the section Elemental Analyzer Connection select the computer serial port
(COM1, COM2 etc.) to which the instrument is connected.
f. In the section Type verify that the instrument in use is Flash 2000.
g. In the section Instrument Settings choose the following settings:
i. Line Frequency = 50 Hz
ii. TCD Settings Source = Internal
iii. TCD Settings Polarity = Positive

Note For the Oxygen determination in CHN-O and CHNS-O configurations,

select the negative polarity. If the same configurations two autosamplers are used,
refer to the relevant Analytical Method described in Chapter 8.

h. 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 88, then click Ok to return to Main
Menu.
2. In the main menu, select File and then the option Load System Defined Method. The
file name of the loaded method is displayed in the grid Filename of method in use of
Main Menu.
3. In Main Menu select Edit and then the option Edit Elemental Analyzer Parameters or

just click the icon . The following window appears where the analyzer operating
parameters are displayed.

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9 Instrument Start-up
Leak Test

Figure 89. Example of analyzer parameters

a. Click Send to transfer the operating parameters to the instrument.

b. From now on the analyzer is working. The furnaces begin to heat, Helium flows in
the circuit and the LEDs Furnace, Oven and TCD lights up on the synoptic panel.

After about 50 minutes the instrument furnaces reach the temperature settings and
the LED Ready on the synoptic panel lights up.

The instrument is now ready to run analyses. However, before starting an analytical
cycle, a leak test must be carried out to check that reactors, filters, if any, and gas
chromatographic columns have been properly installed.

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.

 To Check the Leaks

1. In Main Menu select View and then the option View Elemental Analyzer Status or just

click the icon . The following window appears.

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 9 Instrument Start-up
Leak Test

Figure 90. Status of the analyzer

2. Select the option Special Functions. The following window will appear.

Figure 91. Special function window

3. In the section Command click the button Leak Test. The box of Figure 92 is displayed
with the leak test parameters.

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9 Instrument Start-up
Detector Signal Level

Figure 92. Leal test parameters box

a. Click Start to begin the operation. A window will appear where you will be requested
to perform the Autozero. After 300-360 seconds (Leak test time), Carrier Flow and
Reference Flow must be within 0 and 3 mL/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 and
filters locking nuts. Rarely, leaks may be due to the autosampler.

b. Leaks in the system are generally due to incorrect closure of the reactors and filters
locking nuts. Rarely, leaks may be due to the autosampler.
c. To terminate the leak test and restore the flow operating values, click Stop and Done.

Detector Signal Level

To adjust the level of the TCD detector signal, follow the instructions reported in the
following operating sequence.

 To Adjust the Detector Signal Level

1. In Main Menu select View > View Elemental Analyzer Status or justclick the icon .
The window of Figure 90 on page 147 will be displayed.
2. Select the option Detector. The following window will appear.

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 9 Instrument Start-up
Detector Signal Level

Figure 93. Detector parameters status

3. In the section TCD, click the button Auto-Adjust Level at 1000 μV. At the end of the
operation, the value 1000 is set representing the analysis starting point.

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9 Instrument Start-up
Detector Signal Level

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 10

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
• Determination of the Blank Value
• 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 of analyses
• Program the current maintenance (recommended operation)
• Choose the calibration
• Set a sample table
• Determine the blank value
• Run the sequence of analyses
IMPORTANT Before starting operating sequences, make sure that the instrument
start-up operations have been performed as described in Chapter 9, “Instrument
Start-up,”

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10 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
• and all that is necessary to run the analysis.

Current Maintenance Program

Each reactor, each filter and relevant fillings need to be replaced according to the analytical
configuration used. For each configuration, an average life of its components has been
established. The View Maintenance option will indicate when the different components have
to be replaced. To start the maintenance program, do what described in the following
operating sequence.

 To Start-up the Current Maintenance Program

1. In the main menu select View > View Maintenance. According to your analytical
configuration, a window like the following one is displayed.

Figure 94. Maintenance program schedule

The example of Figure 94 shows the analytical circuit components for which the
maintenance routine is required.

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 10 Guide to Run Analyses
Current Maintenance Program

Component Description
Left Represents the oxidation reactor
In Figure 94 Left 1 represents the crucible or ashes, whereas Left 2
represents the oxidation reactor.
Right Represents the reduction o pyrolysis reactor.
Ads Filter 1 Represents the first adsorbent filter.
Ads Filter 2 Represents the second adsorbent filter.

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. 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, in the menu Edit select Set Maintenance > Default. A window like the
one below will appear. The values shown cannot be changed.

Figure 95. Maintenance: Example of default condition

Condition Description
Life time indicates the preset maximum number of analyses each individual
component can perform.
Number of runs to 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 until indicates the number of analyses to be performed before next
next maintenance maintenance
Number of runs since indicates the number of analyses performed after last maintenance
last maintenance

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10 Guide to Run Analyses
Instrument Calibration

3. If you want to use a different maintenance program from the default one, in the menu
Edit, select the option Set Maintenance > Manual. A window like the following will be
displayed.

Figure 96. Maintenance: Manual program

In the window of Figure 96, you can change any value by clicking on the different boxes and
entering the desired new value.

Instrument Calibration
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:

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 10 Guide to Run Analyses
Instrument Calibration

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 s

To select the calibration method or view the calibration curves of a memorized method, do
what described in the following operating sequence.

 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 97. Method editor

b. Select the option Calculation Parameter.

i. In the section Calibration Method, select the calibration method required.
ii. If desired, in the section Heat value, select in the box Calculation the type of
sample between the options None, Liquids and Solids.
Click on the icon shown on the box right side to display the calculation scheme
related to the selected option.
iii. In the case of N/Protein and N-Brew configurations, 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.
a. At the end of analyses of the standard samples, it is possible to visualize the calibration
curve operating as follows:
b. In Main Menu choose View > View Calibration curve. A window similar to one
below will be displayed.

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Sample Table

Figure 98. Example of Calibration curves

c. Select Calib. Method. According to the calculation method, the calibration points
with peak area and concentration will be displayed.

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.

Figure 99. Example of Sample table

 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.

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Sample Table

Figure 100. 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.
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 only if the instrument configuration is N/Protein or N-Brew.
For all other configurations set 0 (zero).
iii. Select the Category to which the sample belongs only if the instrument
configuration is N/Protein or N-Brew. For all other configurations this parameter
is not edited. To enter the sample category, press the arrow. The following
window is displayed.

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Sample Table

Figure 101. Window to select the sample category

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 sampler 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.

The following Figure 102 and show an example of edited sample table referred to the
N/Protein instrument configuration.

Figure 102. N/Protein: Window of sample table editing

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Determination of the Blank Value

Figure 103. N/Protein: Example of sample table

Determination of the Blank Value

For the determination of the blank value, do what described in the following operating
sequence.

 To Determine the Blank Value

1. Put in the autosampler an airtightly closed container. When N/Protein is used, it is

suggested to introduce about 50-80 mg of sugar into the container to avoid that a high
quantity of oxygen freely flows on the reduction reactor.
2. In Main Menu select Edit > Sample table or just click the icon . The sample table
appears. See Figure 99 on page 156.
a. 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 104. Window for the sample type selection

b. In the window of Figure 104 select Blank, then click OK to confirm and go back to
the sample table.
c. Click OK to confirm and go back to Main Menu.
3. In Main Menu, select the menu Run > Start Single Sample Data Acquisition.
4. Once the analysis run time has elapsed, compare the chromatogram obtained with that of
the final test provided with the instrument.

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Determination of the Blank Value

To compare the chromatogram obtained with that of the final test and to check the blank
value, there are two procedures according to whether a printer is available or not.
• In the first case refer to the operating sequence “To Check the Blank Value with a Printer
Available” on page 160.
• In the second case refer to the operating sequence “To Check the Blank Value with No
Printer Available” on page 162.

 To Check the Blank Value with a Printer Available

Operate as follows:
1. In Main Menu select Edit > Method or just click the icon . The Method editor
window is displayed.

Figure 105. Example of Method editor windows

2. Select Report Parameters. The window of Figure 106 will appear.

Figure 106. Report parameter window

a. In the section Report format, select in the box Report type the option Standard,
then tick the option Append to summarize.

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Determination of the Blank Value

b. In the section Report on, select in the box Report destination the option Printer.
3. In the window of Figure 105 select the tag Report Stripchart. The following dialog
window is displayed.

Figure 107. Report stripchart window

a. In the section Stripchart annotation uncheck the function Autoscaling.

b. If required, in the section Stripchart options modify the values as desired.
4. Click OK to confirm the settings.
5. In the main menu select Recalculation > Recalculation. The following dialog window is
displayed.

Figure 108. Recalculation window

a. In the section Integration options tick the function Identify peaks.

b. In the section Chromatogram source tick the function Sample sequence.

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Determination of the Blank Value

c. In the section Recalculate sample(s) from Sample Sequence set First Sample 1 and
Last Sample 1.
6. Click OK. The report of values will be printed.

 To Check the Blank Value with No Printer Available

To check the blank value with no printer available, do the following:

1. In Main Menu select the menu Recalculation > Recalculation. The dialog window of
Figure 109 is displayed.

Figure 109. Recalculation window

a. In the section Integration options tick the function Review report text.
b. In the section Integration options tick the function Identify peaks.
c. In the section Chromatogram source tick the function Sample sequence.
d. In the section Recalculate sample(s) from Sample Sequence set First Sample 1 and
Last Sample 1.
2. Click OK. The report of values is displayed.

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.

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Sequence of Analyses

Table 43. Blanl value diagnostic guide

Blank Cause and remedy
Nitrogen If the nitrogen value is definitely higher than that indicated, repeat the blank
according to the above described procedures.
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.
Carbon High values are due to contamination. Always work on perfectly clean
surfaces and always keep the containers in a closed container.
Hydrogen The hydrogen blank comes from catalysts and more generally from the
circuit. The value tends to decrease in time.
Sulfur Generally absent or negligible
Oxygen Generally negligible. High values are due to the container contamination.

IMPORTANT All blank values are memorized and subtracted to the sample values. As a
consequence, definitely high values may affect analytical precision.

Sequence of Analyses

IMPORTANT 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, do what described in the following operating sequence.

 To Perform the Analytical Sequence

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 164
• “Mode 2: Automatic Entry of the Weights from the Balance to the PC” on page 165

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Sequence of Analyses

Mode 1: Manual Entry of the Weights

1. Weigh 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 99 on page 156 is displayed.
a. Enter the sample name, type and weight. In case of N/Protein and
N-Brew analyzers, also specify the sample category. See Figure 99 on page 156.
3. The analytical sequence, after the blank analysis, includes an analysis named Bypass: a
standard substance is analyzed to condition the instrument and at the same time to show
the progress of the analysis to the operator, by means of the chromatogram obtained, then
three standards and three unknown samples of other composition than the standard
substance are analyzed.
a. In the sample table grid, click on the column Type. Click the arrow shown to display
the window for the sample type selection.
b. According to the sample type, select Bypass, Standard, Unknown or Blank as shown
in Figure 110.

Figure 110. Selection of the sample type

Note Selecting Standard, the following window appears. Set here the desired standard.

Figure 111. Selection of the standard

4. 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 112.

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Sequence of Analyses

Figure 112. Edit standard table

5. At the end of the sample table editing, select the number following the last edited sample.
6. Select the menu Edit sample > Insert line or just click the icon .
7. In the main menu, select the menu Run > Start sequence of sample.
8. Click Start Now.
9. 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 Results and Final Test Results” on page 167.

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 113. 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 113 is displayed again.

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Sequence of Analyses

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 114. Weight from balance

6. Put the container on the balance plate. Perform the tare pressing Tare. Introduce the
sample then wait for stabilization.
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.

a. At the end of the sample table editing, to automatically stop the sample sequence,
select the number following the last edited sample.
Select the menu Edit sample >Insert line or just click the icon .
8. In Main Menu, select the menu Run > Start sequence of sample.

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
Results and Final Test Results” on page 167.

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Sequence of Analyses

 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 115. 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, “Preparing the Sample,”

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 165.

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10 Guide to Run Analyses
Quality Control and Check of Analytical Results

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.

Quality Control and Check of Analytical Results

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.

 Method to Compare Results

After having analyzed the standard samples and checked the instrument precision. do the
following:
1. In Main Menu, select the menu Recalculation > Summarize results or just click the

icon . The Summarize result table will be displayed. See Figure 115 on page 167.
2. Select the menu Edit and then the option Select reference compounds. A table like the
following will be displyed.

Figure 116. Example of the reference compounds selection table

a. In the textbox Name, enter the sample name.

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Quality Control and Check of Analytical Results

b. In the text boxes Nitrogen, Carbon, Hydrogen, Sulphur, Oxygen, enter the
supposed theoretical percentages of the different elements to be analyzed.
3. 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

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:
4. Go to the table of Figure 116 doing what described in steps 1 and 2.
Select the sample to be compared, then click OK. The Summarize Results table will be
displayed.
5. In Summarize Results, select the sample to be compared as shown in the example of
Figure 117.

Figure 117. 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 118, you will read the name of the
analyzed sample followed by one or more LEDs according to the number of analyzed
elements.
Figure 118. Summarize Results Table: Comparison of samples (2)

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Quality Control and Check of Analytical Results

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.

 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 119. 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.

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Quality Control and Check of Analytical Results

Figure 120. Summarize graphic (2)

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 121.

Figure 121. Summarize graphic (3)

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Post-Analysis Operations

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.

 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 122 is displayed.

Figure 122. Analyzer parameters

2. In the section Other, select the function Set instrument to St-By by ticking the proper
box.
3. Click Send to send the command to the instrument and click OK.

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Post-Analysis Operations

 Automatic Setting of the St-By Function

1. In Main Menu, click the icon . The window of Figure 123 is displayed.

Figure 123. 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.

 To Shut Off Temperature, Detector and Gas

1. In Main Menu, just click the icon . The window of Figure 124 is displayed.

Figure 124. Sequence start window (2)

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Post-Analysis Operations

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 125 on is displayed.

Figure 125. 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.

 To Set Weak-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 Auto-ready menu. The window of Figure 126 is displayed.

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Post-Analysis Operations

Figure 126. Status of the analyzer

a. In the section Control, 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:

 To Set Auto-Start Functions

1. In Main Menu, click the icon . The following window is displayed.

Figure 127. Start sequence

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10 Guide to Run Analyses
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 2000 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 44. 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.
Carbon peak tailing or split. Too much ashes inside the Check ashes and remove
reactor. them.
The sample analyzed was too Weigh a lower amounts of
large. sample.
Hydrogen peak is a split The tube connecting reactor Cut off the clogged tube
peak. and column is clogged. portion.
Bad separation between High Nitrogen blank value. Check the Nitrogen blank
Nitrogen and Carbon peaks. value. Eventually repeat the
analysis.
Copper exhausted. Replace the reactor.

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Analytical Troubleshooting

Table 44. Analytical troubleshooting guide, continued

Problem Diagnosis Remedy
Peak between Nitrogen and Oxygen line contaminated. Exclude autosampler and
Carbon peaks. check the Oxygen blank.
Inadequate Oxygen purity. Use Oxygen with adequate
purity.
Exclude autosampler and
check the Oxygen blank.
High Carbon blank. Tin containers Check the tin container box,
contaminated. tweezers, work bench are
clean.
Memory effect due to bad Remove ashes and analyze
combustion of previously lower amounts of sample.
run analyses.
Decreasing Nitrogen blank Oxygen line contaminated. Wait 10-20 minutes for
values. complete purging of the
Oxygen line.
Repeat blank analysis.
Increasing Nitrogen blank Copper exhausted Replace the reactor.
values.
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

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 11

Applications
This chapter contains guidelines referring to the applications of the Flash 2000 elemental
analyzer.

Contents
• Introduction
• Sample Oxidation
• Automatic Oxygen Dosage

Introduction
Elemental analysis has many fields of application. Among the most important are:
• Pharmaceuticals, with synthesis products.
• Petrochemical Industry, with oil and its derivatives,
• Industrial chemistry, with polymers.
• Environment, with the analyses of soils, sediments, waters.
• Food, with protein analysis, etc.

The Flash 2000 analyzer, thanks to the Eager Xperience software, can analyze different types
of samples. You only have to follow the indications concerning the sample weighing to obtain
precise and reproducible results, not only with standard substances, but also with all other
substances you will analyze later.

However, sometimes samples to be analyzed may not be homogeneous and others may be of
difficult combustion. In any case, as a general rule, weigh a quantity of substance adequate to
the sample nature and to the type of determination.

Sample Oxidation
To obtain precise and reproducible results the sample must be completely oxidized.

This is simple enough when the sample weighing range is narrow, but when the weight is
doubled or tripled, oxygen requirements must strictly follow the weight increase.

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11 Applications
Sample Oxidation

This is obtained by changing the rate and time of oxygen introduction. On this matter please
refer to the instructions given in the operating sequence To Change the Oxygen Quantity.

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, graphite requires more Oxygen than a soil or an organic substance, though at
equal weight. If we always use for all samples the maximum Oxygen quantity, we will obtain
excellent results, but copper will only last for few analyses.

To establish the Oxygen quantity required to combustion, do what described in the operating
sequence “To Establish the Required Oxygen Quantity” on page 181.

For N/Protein and N-Brew analyzers we recommend to always use the OxyTune® function
(Automatic Oxygen Dosing System). Refer to paragraph “Automatic Oxygen Dosage” on
page 182.

 To Change the Oxygen Quantity

1. In Main Menu select Edit > Edit Elemental Analyzer Parameters or just press the icon

. The following window is displayed with the analyzer operating parameters.

Figure 128. Example of analyzer parameters

2. Select Flow/Timing tag. The following tag is displayed.

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Sample Oxidation

Figure 129. FlowTTiming tag

a. To change the time of oxygen introduction, enter the desired value in the appropriate
box Oxygen Injection End in the section System timing.
b. To change the oxygen flow rate, enter the flow value in the appropriate box Oxygen
in the section Gas flow.

 To Establish the Required Oxygen Quantity

Do the following:
1. Analyze the sample setting the Oxygen flow to its maximum value (300 mlLmin).
2. At the end of the analysis, run a blank. If the area value found is equal or very close to the
traditional blank value (±50%), it means that the sample is completely burnt without
leaving any memory effects.
3. To know how much Oxygen was given in excess, repeat the sample run reducing the
Oxygen flow until the blank value is definitely higher than the traditional one. So you will
establish the Oxygen quantity required for the combustion of that kind of sample with
that particular weight.

Note The same result can be obtained by presetting a value of oxygen flow and varying
the time of oxygen injection Oxy Inj End.

IMPORTANT The calibration and analysis of samples must be performed under the same
conditions of Oxy Flow and Oxy Inj End.

This procedure is useful when you have to analyze a number of samples of the same nature. In
the analytical sequence, you will try to keep the same weighing range for all samples.

Choosing the Weighing Range

This choice is a function of the sample kind, but also of the type of determination.

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Automatic Oxygen Dosage

• Simultaneous Analysis of 3 or 4 elements (CHN, CHNS, NCS)

The weighing range is generally between 1 and 3 mg for organic substances, and up to
maximum 20 mg for inorganic samples (e.g. soils, sediments, rocks).
• Nitrogen-Carbon Analysis
The weighing range is generally between 1 and 3 mg for organic substances, and up to
maximum 100 mg for soils and sediments.
• Single Runs of Sulfur and Oxygen
The weighing range is generally between 1 and 3 mg for organic substances, and up to
maximum 20 mg for inorganic samples.
• Nitrogen analyses in samples of any nature except food samples
We recommend a weighing range between 1 and 20 mg independently of the sample
nature.
• Nitrogen analyses in geological materials (soils, sediments, etc.)
We recommend a weighing range between 100 mg and 1g according to the sample nature.
Refer to “Method for Oxygen Dosage (OxyTune®)” on page 182 on.
• Nitrogen analyses in food and agricultural samples
We recommend a weighing range between 100 and 500 mg according to the sample
nature. Refer to “Method for Oxygen Dosage (OxyTune®)” on page 182.

Automatic Oxygen Dosage

In nitrogen-protein analyses you may often need to analyze samples of very different
composition both as percentage and nature.

There are samples that for them nature require a minimum Oxygen quantity versus other
samples that require greater Oxygen amounts. To avoid that the user be obliged every time to
modify the weighing range or adjust the Oxygen quantity, the software provides a table
comprising various categories where samples of different nature are memorized or can be
memorized. Refer to paragraph “Sample Table” on page 156.

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:

Method for Oxygen Dosage (OxyTune®)

1. A fixed Oxygen flow of 300 mL/min was set.
2. The blank value (container + 50-80 mg of sugar) was checked by repeatedly injecting
Oxygen (using Oxygen of 99.995% purity grade) for 30 seconds in a resulting theoretical
quantity of 150 mL.
3. Standardization was performed using Aspartic Acid with weight ranging from 50 to 100
mg and injecting fixed Oxygen amounts for 30 seconds in a resulting theoretical quantity
of 150 mL.
4. Samples having different nature were analyzed as follows:

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 11 Applications
Automatic Oxygen Dosage

a. 200 mg of sample weighed and Oxygen was injected for 60 seconds in a resulting
theoretical quantity of 300 mL.
b. At the end of the analysis, after taking note of the value, the blank was run again.
c. The same procedure (sample analysis and subsequent blank analysis) was followed
reducing the injection time at every sequence run. Checking the increased blank
value, the combustion critical point was established.
d. After having established the combustion critical point, the ideal
Oxygen/sample weight factor (obtained dividing the Oxygen quantity injected by the
sample weight) was found and stored in an appropriate category.
e. The sample analysis was repeated starting by reducing the weight to
100 mg, and then progressively increasing the sample weight until reaching the
maximum quantity accepted by the container.
Being ideal factor multiplying value memorized, the Oxygen amount for each single
analysis was automatically calculated simply selecting the category the sample belongs
to.

Based on these results, the following table was created:

Table of Sample Category

This table, shown in Figure 130 is displayed following the instructions of the operating
sequence “To Fill Sample Table” on page 156.

Figure 130. Table of sample category

The table contains:

• Four categories of samples - A, B, C, D. where the ideal factor values (Oxygen/sample
weight-sample nature) of the samples have been prefixed.

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11 Applications
Automatic Oxygen Dosage

• The nature of samples.

• Four free categories - E, F, G, H - where sample names not considered (extraneous) in
categories - A, B, C, D - can be memorized.
When a free category is selected, the ideal factor value, calculated by using the Oxygen
Dosage method OxyTune®, must be entered in the appropriate box.
Before memorizing the sample name in the new category and the ideal factor value, the
procedure previously described must be repeated.

Note The correct selection of the group to which the sample belongs helps you keep the
analyzer perfectly efficient.

CAUTION Non compliance with allocation criteria may adversely affect analytical results.

The sample category - Blank, Bypass and Standard - is the same and is marked by the symbol
@.
When @ is selected, a set time is entered and consequently an equal Oxygen quantity
independently of the sample quality and nature.
This time has been preset at 30 seconds, but it can be changed according to particular
analytical requirements.

CAUTION In analyses of Nitrogen traces, e.g. in starches analysis where Nitrogen content
is below 0.1%, it is advisable to evaluate the blank value injecting the same Oxygen
quantity as that used for the sample.

The @ category can also be used for Unknown samples, when sample quantities below 100
mg are weighed. Independently of the nature of the weighed samples, enter:
• 10 seconds of Oxygen for samples between 0 and 20 mg.
• 20 seconds of Oxygen for samples between 20 and 50 mg.
• 30 seconds of Oxygen for samples between 50 and 100 mg.

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 12

Use of Eager Simplified User Interface

This chapter provides information about the use of the simplified user interface of Eager
Xperience.

Contents
• Simplified User Interface

The possibility of using a simplified version of Eager Xperience is mainly addressed to users
who do not posses a specific expertise in the instrumental field. This option however also
concerns those who, having to run every day analyses of samples of the same nature, do not
need any special functions of Eager Xperience. For this purpose the software is provided with a
“password” system, which makes the application of its functions more or less extended.
Normally the password is dedicated to the laboratory head, which allows the use of the entire
software, besides one or more passwords dedicated to the operator or operators of the
instrument. In this way the laboratory head has the possibility to prevent the operator from
using the appropriate software functions he deems and to act in any moment in case of need.
To use the simplified version of Eager Xperience, do what described in the following operating
sequence.

ATTENTION The use of the simplified user interface is NOT available with Eager
Xperience USB and A/D versions.

Simplified User Interface

 To use the Simplified User Interface

1. In Main Menu, select File > System administration. Reply by clicking Ok to the message
displayed. The window of Figure 131 is visualized, where passwords must be entered.

Figure 131. User password window (1)

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12 Use of Eager Simplified User Interface
Simplified User Interface

• The first password, dedicated to the laboratory head (System Manager), becomes active by
clicking Add Password and entering the name in the text-box. Press Ok to confirm. See
the top section of Figure 132.
• The second password, dedicated to the operator (Limited rights), becomes active using the
same procedure. See the bottom section of Figure 132.

Figure 132. User password window (2)

2. To exclude the functions that have not to be available to the operator, click Edit Path.
The window of Figure 133 is displayed.

Figure 133. User path window

3. Select the option Enable Simplified user interface by ticking the appropriate box.
4. Select the functions that have to be available by ticking the relevant boxes.
5. Click Update. In the page displayed, it is requested to generate a directory for this
application.

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 12 Use of Eager Simplified User Interface
Simplified User Interface

6. Click OK. In the window of Figure 132 click Update again. A message concerning the
password is displayed.

 to Start The Simplified User Interface

1. When the operator (Limited Rights) opens the software, a window like that shown in
Figure 134 will be displayed.

Note The number of icons in the window corresponds to the previously selected
functions.

Figure 134. Sample table of the simplified user interface (1)

2. In the window of Figure 135 select the Submit new sample to analyze icon to edit the
sample table. A window like the one below is displayed.

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12 Use of Eager Simplified User Interface
Simplified User Interface

Figure 135. Window of submit sample to run

3. Enter the Sample name and the chr filename, followed by a number. Then the file names
and the sample names will continue to be progressively numbered.
4. Select the type of the sample to be analyzed: Sample type.
5. In the section Instrument select, in Data Method, one of the methods previously saved
in the folder Simplified UI Method:.
6. Enter the sample Weight and, in case of N/Protein and N-Brew configurations, the
multiplying factor Protein f: and the sample Category. Click Add.
7. Edit the table for all samples to be analyzed. At the end of editing, the sample table will
appear filled with all information previously entered, as shown in the example of
Figure 136. The boxes of the Status column show a Q (Queue).

Figure 136. Sample table of the simplified user interface (2)

8. To send the start to the instrument select the icon and reply Yes to the question Are
you sure to run queued samples?. At the end of the analytical sequence the instrument
automatically stops.
9. To view the results, choose View > View only result of sheet.

Note If at the end of each analysis you want to read directly the result, in the menu
View enable the function Last sample calculated results. If for any reason you need to
stop the analytical cycle, click the icon named Put sample on queue (no run).

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 Part 1

Maintenance and
Troubleshooting
 13

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 200R Autosampler and the CM2 Manual Sampler.

Contents
• Instrument Maintenance
• Installing and Servicing the MAS 200R Autosampler
• Installing and Servicing the CM2 Manual Sampler

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

Note 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.

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13 Maintenance
Instrument Maintenance

Current Maintenance
• Replacement of reactors and adsorption filters and their filling materials.
For instrument configurations using special steel reactors for combustion it may be
necessary also to clean the crucible done with same material.

Periodic Maintenance
• Replacement of the gas chromatographic column. The column lifetime in Flash 2000
instrument is evaluated in years.
• Replacement of the seals of the reactors coupling unions placed on the furnace
compartment base.

Note 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 173.

Replacing Reactors and Adsorption Filters

The replacement of reactors and adsorption filters is performed after a preset number of
analyses according to the setting entered in paragraph “Current Maintenance Program” on
page 152.

Replace and install reactors and filters according to the operating sequences described in
Chapter 6, “Connecting Reactors and Adsorption Filters,”
• “To Remove the Quartz Reactors from the Furnaces” on page 93
• “To Remove Special Steel Reactors from the Furnaces” on page 94
• “To Remove the Adsorption Filter” on page 95
• “To Install the Quartz Reactors into the Furnaces” on page 84
• “To Install the Special Steel Reactors into the Furnaces” on page 87

Replacement of the Filling Materials

The replacement of reactors and adsorption filters requires the replacement of their filling
materials. This operation comprises two steps:
• Removing the exhausted filling material from the reactor.
• 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.

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Instrument Maintenance

 To Replace the Filling Material in Quartz Reactors

Material required
Tool for cleaning quartz reactors P/N 276 06010 (included in the Standard Outfit of all
Flash Configurations)
Filling materials

CAUTION Before starting the operation, check that the furnaces are at room temperature.

Remove the quartz reactor from the furnace following the instructions given in the operating
sequence “To Remove the Quartz Reactors from the Furnaces” on page 93, then do the
following:
1. Introduce the cleaning tool into the reactor as shown in Figure 137.

Figure 137. Removing the Filling Material from a Quartz Reactor

2. Rotate the tool exerting a slight pressure to scrape off the filling material.
3. Collect the removed filling material as shown in Figure 138.
4. Repeat steps 1 and 2 until complete elimination of the exhausted filling materials.

Figure 138. Collection of the Material Removed from a Quartz Reactor

5. 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 Chapter 5, “Preparation of Reactors
and Adsorption Filters,” according to the analyzer configuration.

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13 Maintenance
Instrument Maintenance

 To Replace the Filling Material in Special Steel Reactors

Material required
Tool for cleaning special steel reactors P/N 276 06025 (included in the Standard Outfit of
N/Protein, N-Brew and NC-Soils, NC-Sediments and NC-Filters Configurations)
Filling materials

CAUTION Before starting the operation, check that the furnaces are at room temperature.

Remove the special steel reactor from the furnace following the instructions given in the
operating sequence “To Remove Special Steel Reactors from the Furnaces” on page 94, then
do the following:
1. Introduce the cleaning tool into the reactor as shown in Figure 139.

Figure 139. Removal of the Filling Material from a Special Steel Reactor

2. Rotate the tool exerting a slight pressure to scrape off the filling material and collect the
removed filling material as shown in Figure 140.
3. Repeat steps 1 and 2 until complete elimination of the exhausted filling materials.

Figure 140. Collection of the Filling Material Removed from a Special Steel Reactor

4. 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 and Filters” on page 57 and “Preparing the Reactors” on page 74, according to
the analyzer configuration.

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 13 Maintenance
Instrument Maintenance

 To Clean the Crucible

Materials Required
Tool for cleaning quartz reactors P/N 276 06010
Quartz wool

Remove the crucible following the instructions given in the operating sequence “To Prepare
the Crucible” on page 78, then do the following:

CAUTION Perform the operation with the furnaces at room temperature.

1. Introduce the cleaning tool into the crucible as shown in Figure 141.

Figure 141. Removal of Quartz Wool and Ashes from the Crucible

2. Rotate the cleaning tool exerting a slight pressure in a way to scrape off the filling material
and collect the material removed.
3. At the end of the operation, introduce new quartz wool into the crucible as described on
page 78.

 To Replace the Filling Material in Adsorption Filters

Material Required
Filling materials

Remove the adsorption filter from the detector compartment according to the instructions
given in the operating sequence “To Remove the Adsorption Filter” on page 95, then do the
following:
1. Unscrew the filter nut and remove the filling material.
Note ome adsorption filters contain materials that can be regenerated, such as for instance
molecular sieves. Therefore it is recommended to properly collect the material removed
from the filter.

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13 Maintenance
Instrument Maintenance

2. Restore the sequence of the layers of filling materials introducing the new ones into the
filter. To do this, refer to paragraphs “Introduction to the Preparation of Reactors and
Filters” on page 57 and “Preparing the Adsorption Filters” on page 79, according to the
analyzer configuration.

Replacement of the Gas Chromatographic Column

The instrument rarely requires the gas chromatographic column replacement, however, in
case, operate according to the instructions given in the following operating sequence.

 To Replace the Gas Chromatographic Column

Material Required
Open end wrenches for the column fittings

The gas chromatographic column can be installed outside or housed in the detector
compartment.
1. Open the instrument right door. Also refer to paragraph “Detector Compartment” on
page 30.

Figure 142. View of the Detector Compartment

2. Remove adsorption filters from their securing clips.

Note According to the instrument configuration, there can be one or two adsorption
filters in the detector compartment.

3. Undo the 4 fixing screws securing the protection panel.

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 13 Maintenance
Instrument Maintenance

Figure 143. Access to the detector

Fixing screws

Clips securing the

adsorption filters Protecting plate

Fixing screws

Figure 144 shows the detector compartment, the heating block where the detector is housed,
and the gas chromatographic column.

Note According to the instrument configuration there can be one or two analytical
columns.

Figure 144. Compartment housing the chromatographic column

Heating block

TCD detector

Chromatographic
column

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13 Maintenance
Instrument Maintenance

4. Unscrew the fittings from the column ends and remove the column from the
compartment.
5. Introduce the new column and connect its ends to the fittings.
6. Re-mount the protection panel and the adsorption filters.

Replacement of the O-Rings of the Reactors Coupling Unions

To perform this operation, operate as described in the following operating sequence.

 To Replace the O-Rings of the Reactors Coupling Unions

Materials Required
Allen wrench
Screwdriver
Spare seals

CAUTION Before starting the operation, check that the furnaces are at room temperature.

1. Open the furnaces compartment by lifting the cover and removing the protection wall.
Also refer to paragraph “Furnaces Compartment” on page 28.
2. Remove the reactors from the furnaces according to the instructions given in the
operating sequence “To Remove the Quartz Reactors from the Furnaces” on page 93
or “To Remove Special Steel Reactors from the Furnaces” on page 94.
3. Loosen the allen screws securing the reactors coupling unions to the base as shown in
Figure 145.

Figure 145. Removal of the Reactors Coupling Unions

Reactor
coupling
union

Allens crews

4. Remove the reactors coupling unions from the base and rest them on a clean surface, as
shown in Figure 146.

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 13 Maintenance
Instrument Maintenance

Figure 146. View of the reactors coupling unions

Screw-
driver

Reactor
coupling
O-ring union

5. Using the small screwdriver, remove the O-ring from each union, as shown in Figure 147.

Figure 147. 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 148.

Figure 148. Introduction of the O-ring from the coupling union

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13 Maintenance
Installing and Servicing the MAS 200R Autosampler

Installing and Servicing the MAS 200R Autosampler

Introduction
The MAS 200R autosampler for solids consists of an anodized aluminium block having on its
left side the inlets for carrier and purge gas lines. Its modular structure allows to run up to 125
unattended analyses.

The base unit is provided with one 32-position sample tray, but it can accommodate three
other 32-position trays to reach a capacity of 125 samples. Each sample tray is installed in a
specific position defined by the numbering, and therefore they are not interchangeable.

Installation
The autosampler is directly installed on the connecting nut of the concerned reactor.

 To Install the MAS 200R Autosampler on the Flash 2000

The following operating sequence provides instructions to install the autosampler on the Flash
2000.

Note The installation sequence is common to all instrument configurations.

Material Required
8 mm wrench

Proceed as follows:
1. 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.
2. Manually screw the autosampler nut on the concerned channel.

Note The MAS 200 R Standard Outfit includes two reactor connectors: 18 mm OD
for Quartz reactor and 25 mm OD for HPAR. Screw the suitable connectors to the
autosampler inserting the right relative o-ring. Also the o-ring are included in the
Standard Outfit.

Figure 149. Installation of the MAS 200R on the Flash 2000

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 13 Maintenance
Installing and Servicing the MAS 200R Autosampler

3. Connect the signal cable of the MAS 200R autosampler to the 2-pin connector, marked
Autosampler, on the real panel of the analyzer.

Switching Box
When the analyzer is equipped with two MAS 200R autosamplers, it is possible to switch
from a channel to the other by using a dedicated Switching Box as schematically shown in the
following figure:

Figure 150. Scheme of the switching box

A B
SWITCHING
BOX
A B

Autosampler

1
2

3
4

MAS200 R MAS200 R
"A" "B"

The Sample Tray

The sample tray, shown in Figure 151, can contain up to 32 samples numbered 0 to 31.
It is provided with a reference pin to be introduced into the seat marked 0 (zero).
The correct alignment of the pin is critical for the installation of the sample tray on the MAS
200 R autosampler.

Figure 151. Sample tray

Seat “zero”
Alignment pin

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13 Maintenance
Installing and Servicing the MAS 200R Autosampler

 To Install the Sample Tray

The following operating sequence provides instructions for the correct installation of the
sample tray.
1. Manually rotate the toothed wheel clockwise until the guide located on its rim is perfectly
aligned with the metal pin of the autosampler body, as shown in Figure 152.

Figure 152. Alignment of the Toothed Wheel

Guide to the
toothed wheel

Metal pin

2. Check that the tray reference pin is in correspondence with the seat marked “zero”, as
shown in Figure 151..
3. Place the sample tray, with the reference pin in correspondence with the “zero” seat, onto
the toothed wheel, paying attention to have the base match with the guides, as shown in
Figure 153.
4. Rotate the sample tray clockwise to select the sample position 1.

Figure 153. Installation of the Sample Tray

5. Place the protection cover over the sample tray, as shown in Figure 154, with the surface
marked “Side up” turned towards you.

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 13 Maintenance
Installing and Servicing the MAS 200R Autosampler

Figure 154. Protection cover

CAUTION Before starting samples analyses, make sure that the protection cover is
positioned over the sample tray. A complete deaeration of the area where samples are
housed is only possible if the cover is in place.
Pay attention to no invert the cover; the surface marked “Side-up” must be turned
towards you.

Current Maintenance of the MAS 200 R Autosampler

The MAS 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 shaft housed
in the autosampler.

To do this, operate as described in the following operating sequence.

 To Clean the Shaft of the MAS 200R Autosampler

This operating sequence provides instructions for the MAS autosampler maintenance.
Materials Required
Cross screwdriver
Cloth
Silicon grease (For use at pressures down to 10-6 mm Hg)

1. In Main Menu, select the menu Edit > Edit Elemental Analyzer parameters or just click

the icon . The Analyzer Parameter window will be displayed.

2. Select the Flow/Timing option. Set Carrier Off in the Gas Flow box.
3. Click Send and wait 2-3 minutes to discharge the gas out the circuit.
4. Remove the autosampler cover undoing the two fixing screws, as shown in Figure 155.

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13 Maintenance
Installing and Servicing the MAS 200R Autosampler

Figure 155. Removal of the MAS 200R autosampler cover

Cross
screwdriver

Fixing screws

Cover

5. From Main Menu select the menu View > View Elemental Analyzer status or directly

click the icon .

6. In the Status window select the Special function tag , then click Step sampler tray
position. The autosampler mechanism pushes the shaft forward and then ejects it.
7. Take out the shaft from the autosampler, as shown in Figure 156.

Figure 156. Removal of the shaft

8. Eliminate possible traces of dirt from the shaft seals using a dry clean cloth.
9. Place and smear a slight layer of silicon grease on the o-ring. Do not use solvents.

Figure 157 shows the shaft of the MAS autosampler.

Figure 157. Shaft of the autosampler

O-ring Rack

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 13 Maintenance
Installing and Servicing the MAS 200R Autosampler

10. Re-introduce the shaft into the autosampler until in place keeping its rack turned
downward, as shown in Figure 158.

Figure 158. Reinstalling the shaft (1)

11. Slightly pushing the shaft with one finger of your hand, as shown in Figure 159, click
Step Sampler tray position again.
The autosampler mechanism first tries to eject the shaft, then, on the motor reversal, the
mechanism will hook the shaft and draw it inside the autosampler (2).

Figure 159. Reinstalling the shaft (2)

12. Re-install the autosampler cover using the two fixing screws.
13. Return to Analyzer Parameter window. Restore the operating conditions setting the
carrier gas flow to the initial value.

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13 Maintenance
Installing and Servicing the CM2 Manual Sampler

Installing and Servicing the CM2 Manual Sampler

Introduction
The CM2 manual sampler, shown in Figure 160, consists of a base block provided with a
sampling chamber and a lever for the injection of samples into the reactor.

The sample is placed inside the sampling chamber, which must then be closed by turning the
appropriate nut. On the Start command, after the time delay set in the method, push the lever
towards the sampler and the sample will fall into the reactor. The lever is the brought to its
starting position.

Figure 160. CM2 manual sampler

Installation
The sampler is directly installed on the connecting nut of the concerned reactor.

 To Install the CM2 Manual Sampler

The following operating sequence provides instructions to install the autosampler on the Flash
2000.

Note The installation sequence is common to all instrument configurations.

Material Required
8 mm wrench

1. Connect the tubes coming from the gases connections, located on the analyzer, to the
relevant connections on the sampler.
a. Connect the tube for Helium as carrier gas (connection 2) to the connection located
on the left side of the sampler.
b. Connect the tube for Helium as reference gas (connection 1) to the connection
located on the lower part of the sampler.
2. Manually screw the autosampler nut on the concerned channel.

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 13 Maintenance
Installing and Servicing the CM2 Manual Sampler

Current Maintenance of the CM2 Sampler

The CM2 sampler does not usually require maintenance. However, when the instrument is
extensively used, it is a good practice to replace the three seals inside it. To do this, operate as
described in the following operating sequence.

 To Replace the CM2 Sampler Seals

The following operating sequence provides instructions to maintaining the CM2 manual
sampler.

CAUTION The dismounting and re-assembling of the sampler MUST be performed with
great care and under very clean operating conditions, because the presence of even the
smaller solid particle in the sampling mechanism may jeopardize the performance of the
sampler producing high blank values.

Material Required
Spanner
Seals (O-ring)
Screwdriver

Figure 161. Parts of the CM2 manual sampler

Proceed as follows referring to Figure 161.

1. Remove the CM2 manual sampler from the analyzer.
2. Insert a spanner into the hole A and unscrew the handle14.

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13 Maintenance
Installing and Servicing the CM2 Manual Sampler

3. Unscrew the locking nut 3.

4. Remove the shaft 2 completely together with parts 12, 4, 15, 7, 13, 6 and 8.
5. Take off the pin 12 from the shaft 2 and remove the ring 4.
6. Remove clip 15 from both ends
7. Take off 6, 7 and 8.
8. Replace the three o-rings 13.
9. Reassemble all parts in the reversed order.
10. When introducing the shaft 2, check that its plane is down and make sure that the hole of
the body 1 and the hole of 2 are aligned.
11. The manual sampler should slide smoothly and easily into the body. Otherwise check
again the alignment between the shaft 2 and the pin 12.
12. Screw the locking nut 3.
13. Insert a spanner into the hole A and screw the handle 14.

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 14

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.

 To Display the Error Message

Proceed as follows:
1. In the Main menu select View > View Elemental Analyzer Status or just press the icon

.
2. In the displayed dialog window, select the option Special Functions. The dialog window
of Figure 162 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 45 to find out the error status and have mode information.

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14 Troubleshooting
Safety Cut Off

Figure 162. Special function window

1. Error Message Reading Box

The following Table 45 reports the error messages and the explanation of the relevant
correlated problem.

Table 45. Error messages

Message Description
Voltage supplied to electric circuit is too low. Not
significant error.
safety cut off When voltage returns within limits, the instrument
Voltage out limit
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

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.

210 Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific

 14 Troubleshooting
EFC-t Module

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 46 to find the component responsible of the EFCt module malfunctioning
and to solve the relevant problem.

Table 46. 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.

Thermo Scientific Flash 2000 Elemental Analyzer - Operating Manual 211

14 Troubleshooting
EFC-t Module

212 Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific

 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:

Thermo Fisher Scientific

19 Mercers Row, Cambridge, CB5 8BZ

United Kingdom

Tel: +44(0)1223 347400 Fax: +44(0)1223 347403

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.

Thermo Scientific Flash 2000 Elemental Analyzer - Operating Manual 213

A Customer Communication
Reader Survey

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Manual: Operating Manual
Part No.: 317 082 41

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214 Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific

 G

Abbreviations
This section lists and defines terms used in this guide. It
also includes acronyms, metric prefixes, symbols and
abbreviations.
A B C D E F G H I J K L M N O P Q R S T U V W X Y Z

A ampere ft foot

ac alternating current g gram

ADC analog-to-digital converter GND electrical ground

b bit h height

B byte (8 b) h hour

baud rate data transmission speed in events per second H hydrogen

C Carbon harmonic distortion A high-frequency disturbance

that appears as distortion of the fundamental sine
°C Celsius wave
cm centimeter He Helium
CPU central processing unit (of a computer) HPAR High Performance Alloy Reactor
CSE Customer Service Engineer HV high voltage
<Ctrl> control key of the keyboard Hz hertz (cycles per second)
d depth IEC International Electrotechnical Commission
DAC digital-to-analog converter in. inch
dc direct current I/O input/output
DS data system k kilo (103 or 1024)
EMC electromagnetic compatibility K Kelvin
ESD electrostatic discharge kg kilogram
ºF Fahrenheit kPa kilopascal
FSE Field Service Engineer l length

Thermo Scientific Flash 2000 Elemental Analyzer - Operating Manual 215

Glossary:

l liter surge A sudden change in average RMS voltage level,

with typical duration between 50 μs and 2 s.
LAN Local Area Network
S sulphur
lb pound
TCD Thermal Conductivity Detector
LED light-emitting diode
transient A brief voltage surge of up to several
m meter (or milli [10-3]) thousand volts, with a duration of less than 50 μs.
M mega (106) V volt
μ micro (10-6) V ac volts, alternating current
min minute V dc volts, direct current
mL o ml milliliter VGA Video Graphics Array
mm millimeter w width
m/z mass-to-charge ratio W Watt
N nitrogen
When a unit of measure has a quotient (e.g. Celsius degrees
n nano (10-9) per minute or grams per liter) this can be written as
negative exponent instead of the denominator:
O oxygen For example:
°C min-1 instead of °C/min
Ω ohm g L-1 instead of g/L

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.

216 Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific

 I

Index

A Autosamplers 40
AI 3000/AS 3000 II for Liquid Samples 40
Adsorption Filter
CM2 Manual Sampler 40
Filling 80
MAS 200 for Solids 40
Adsorption Filters 55
Auto-Start Function 174, 175
AI 3000/AS 3000 II Autosampler 40
Analyses
Sequence B
Execution 163 Balance Parameters Settin 166
Analytical Method Blank Value
CHN Configuration 111 Checking with No Printer Available 162
CHN-O Configuration 113 Checking with Printer Available 160
CHNS Configuration 115 Determination 159
CHNS-O Configuration 117
N (Nitrogen) Configuration 123
N Lubricant 131
C
N-Brew 131 Calculation Parameter 155
N-Brew Configuration 131 Calibration Curves 155
NC Configuration 125 View 155
NC-Filters Configuration 129 calibration methods 154
NC-HT 135 Classification 13
NC-IRMS 133 CM2 Manual Sampler
NCS Configuration 127 Current Maintenance 207
NC-Sediments Configuration 129 Installation 206
NC-Soil 129 Replacing the Seals 207
N-Protein Configuration 131 Servicing 206
O (Oxygen) Configuration 121 Connecting the Adsorption Filters 91
S (Sulfur) Configuration 119 Connections Panel 35
Analytical Methods Control Section 22
Introduction 110 Electronic Compartment 23
Analytical Results Pneumatic Compartment 22
Comparison 167 Current Maintenance 192
Analytical Section 21, 21 Current Maintenance Program 152
Adsorption Filters 22
Cutting Off
Autosampler 22
Gas Flows 173
Chromatographic Columns 22
Furnaces 21
Reactors 22 D
Thermal Conductivity Detector (TCD) 22 Detection System
Analytical Troubleshooting 176 Description 32
Applications Detector Compartment 30
Automatic Oxygen Dosage 182 Access to the Detector 31
Introduction 179 Detector Signal Level 148
Sample Oxidation 179 Adjustment 148
How to Change the Oxygen Quantity 180 Directory for Analyses 152
Automation 23

Thermo Scientific Flash 2000 Elemental Analyzer - Operating Manual 217

Index: E

E NC-Filters Analyzer 17
NCS Analyzer 17
Eager Xperience
NC-Sediments Analyzer 17
Installation Menu 140
NC-Soil Analyzer 17
Eager Xperience Software 140
N-Protein Analyzer 17
Edit Standard Table 165 O Analyzer 16
EFC Module 43 S Analyzer 16
Electrical Compartment 33 Instrument Maintenance 191
Low Voltage Section 33 Instrument Start Up
Rechargeable battery 34 Introduction 139
Mains Voltage Section 34
Elemental analyzer setup 144
Environmental Conditions 13 L
Leak Test 146
Checking 146
F
Filling Materials 56
Fixing Plates for the Reactors 29
M
Found Values 169 Maintenance 191
Front Panel 26, 26 Cleaning the Crucible 195
Replacing the Filling Material in Adsorption Filters 195
Furnaces Compartment 28
Replacing the Filling Material in Quartz Reactor 193
Replacing the Filling Material in Special Steel Reactors 194
G Manual Injection Device for Liquids 40
Gas Chromatographic Column MAS Autosampler
Replacement 196 Cleaning the Cylinder 203
Replacing 196 Cleaning the Shaft 203
Gas Chromatographic Columns 56 Current Maintenance 203
Installation 200
Installing the Sample Tray 202
I Servicing 200
Installing the Adsorption Filters 90, 91 The Sample Tray 201
Preliminary Operations 91 Maximum relative humidity 13
Installing the CM2 Manual Sampler 206 Method for Oxygen Dosage (Oxy Tune) 182
Installing the MAS Autosampler on the Elemental Analyzer Modulo EFC 211
200
Installing the Reactors into the Furnaces 83
Preliminary Operations 84 N
Quartz Reactor 84 N Lubricant Analyzer 16
Spaecial Steel Reactor 87 NoBlank Sampling Device 40
Instrument Notes 99
Classification 13
Cleaning 15
Configuration 15
O
Safety 15 O-Rings of the Reactors Coupling Unions
Sleeping Mode 172 Replacing 198
Instrument Calibration 154
Instrument Configuration 144 P
N Lubricant Analyzer 16 Periodic Maintenance 192
NC-IRMS HT 17 Pneumatic Circuit 23
OH-IRMS HT 17 CHN Configurations 45
CHN-O Analyzer 16 CHN-O Configurations 44
CHNS Analyzer 16 CHNS Configuration 45
CHNS-O Analyzer 16 CHNS-O Configurations 44, 44
N Analyzer 16 N 48
N-Brew Analyzer 17 N Configuration 48, 49
NC Analyzer 17

218 Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific

 Index: Q

N Lubricant 48 Q
N/Protein 48
Quartz Reactor
N-Brew 48
Filling 74
NC Configuration 47
NC-Filters Sediments Configuration 47
NC-IRMS HT Configuration 51 R
NCS Configuration 46 Reactors 55
NC-Sediments Configuration 47 Rear Panel 26
NC-Soil Configuration 47 Recalculation 167
O Configuration 46
Removing Reactors from the Furnaces
OH-IRMS HT Configuration 49
Quartz Reactor 93
S Configuration 46
Special Steel Reactor 94
Pneumatic Circuits
Removing the Adsorption Filters 95
EFC Module 43
Removing the Reactors 93
Pollution degree 13
Replacement of the Filling Materials 192
Powering on the System 139
Replacement of the O-Rings of the Reactors Coupling Unions
Preparation of Reactor and Filters
198
N Lubricant Configurations 67
Replacing Adsorption Filters 192
Preparation of Reactors
Introduction 57 Replacing Reactors 192
Results
Preparation of Reactors and Adsorpion Filters
Graphic Display 170
N-Brew 71
Interpretation 167
NC with the Flash HT 73
NC with the Flash IRMS 72 RS 232 36
CHN Configuration 58
CHN-O Configuration 59 S
CHNS Configuration 61
Safety Cut Off 34, 209
CHNS-O Configuration 62
Safety Cut Off Device 15
N (Nitrogen) Configuration 66
Safety Information 14
NC Configuration 68
Nominal Pressure of Gases 15
NC-Filters Configuration 70
Purity of Gases 14
NCS Configuration 69
Use of Gases 14
NC-Sediments Configurations 70
NC-Soil Configurations 70 Sample table
N-Protein Configuration 71 Fill 156
O (Oxygen) Configuration 65 Sample Weighing Technique 99
S (Sulfur) Configuration 64 Samples
Preparation of Reactors and Filters N-Brew Configuration 71 Comparison 169, 169
Preparing the Adsorption Filters 79 Shutting Off 173
Preparing the Crucible 78 Detector 173
Preparing the Reactors 74 Furnaces 173
Special Steel Reactor
Preparing the Sample
Filling 76
Homogenizing
Carbons 98 Standard Outfit 17
Preparing the Samples Standard Warranty xiii
Homogenizing 97 Summarize results 167, 170
Liquids 99 Synoptic Panel 38
Metals 98
Minerals 98 T
Plastics 99
Technical Features 14
Sediments 98
Soils 98 Temperature 13
Vegetals 99 Theoretical Values 169
Introduction 97 Top Panel 27
Transformers Compartment 37
Devices for the Furnaces Control 37

Thermo Scientific Flash 2000 Elemental Analyzer - Operating Manual 219

Index: U

Devices Supplying the Furnaces 38

Transients 13
Troubleshooting 209

U
Units Constituting the Instrument 21
Use of Eager Simplified User Interface 185

V
Voltage variations 13

W
Wake-up Function 174, 174
Weighing Technique 99
Large Quantities of Solid Samples 101
Liquid Samples 100, 105
Deposited on Adsorbent Material 107
Small Quantities of Solid Samples 104
Solid Samples 100
Viscous Samples 108

220 Flash 2000 Elemental Analyzer - Operating Manual Thermo Scientific