Thermo Scientific Dionex UltiMate 3000 Series, FLD-3100, FLD-3400RS Operating Instructions Manual
Thermo Scientific Dionex
UltiMate 3000 Series
Fluorescence Detectors
FLD-3100 and FLD-3400RS
Operating Instructions
(Original Operating Instructions)
Revision: 1.3
Date: September 2013
© 2013 Thermo Fisher Scientific Inc.
Doc. No. 4820.7850
UltiMate 3000 Series:
Fluorescence Detectors FLD-3100 and FLD-3400RS
Operating Instructions
UltiMate 3000 Series:
Fluorescence Detectors FLD-3100 and FLD-3400RS
Declaration of Conformity
(Original Declaration of Conformity)
Product: Thermo Scientific Dionex UltiMate 3000 - Detector
Types: FLD-3100 and FLD-3400RS
Dionex Softron GmbH herewith declares conformity of the above products with
the respective requirements of the following regulations:
• Low-Voltage Directive 2006/95/EC
• EMC Directive 2004/108/EC
The electrical safety of the products was evaluated based on the following
standard:
• DIN EN 61010-1:2010
Safety requirements for electrical equipment for measurement, control
and laboratory use, Part 1: General Requirements
The Electromagnetic Compatibility (EMC) of the products was evaluated based
on the following standard:
• DIN EN 61326:2006
Electrical equipment for measurement, control and laboratory use
EMC Requirements
This declaration is issued for the manufacturer
Dionex Softron GmbH
Part of Thermo Fisher Scientific Inc.
Dornierstraße 4
D-82110 Germering
by the Managing Director, Rüdiger Obst, and
the Vice President HPLC, Fraser McLeod.
September 2, 2013
Operating Instructions Page I
UltiMate 3000 Series:
Fluorescence Detectors FLD-3100 and FLD-3400RS
Page II Operating Instructions
UltiMate 3000 Series:
Fluorescence Detectors FLD-3100 and FLD-3400RS
Table of Contents
1 Introduction ................................................................................................................... 1
1.1 How to Use This Manual ........................................................................................... 1
1.2 Safety ......................................................................................................................... 3
1.2.1 Symbols on the Instrument and in the Manual ................................................. 3
1.2.2 Safety Precautions ............................................................................................ 5
1.2.3 Consignes de Sécurité ....................................................................................... 8
1.3 Intended Use ............................................................................................................ 12
1.4 Federal Communications Commission (FCC) Note ................................................ 14
2 Overview ...................................................................................................................... 15
2.1 Unit Description ....................................................................................................... 15
2.2 Operating Principle .................................................................................................. 16
2.3 Configurations ......................................................................................................... 19
2.4 Interior Components ................................................................................................ 20
2.5 Front Panel Elements ............................................................................................... 21
2.6 Rear Panel ................................................................................................................ 22
2.6.1 Power Switch .................................................................................................. 22
2.6.2 Fuse Cartridge ................................................................................................ 22
2.6.3 USB Port ......................................................................................................... 23
2.6.4 Analog Outputs (Optional) ............................................................................. 23
2.7 Fluid Connections .................................................................................................... 23
2.8 Flow Cells ................................................................................................................ 24
2.9 Lamp ........................................................................................................................ 25
2.10 Leak Sensor .......................................................................................................... 25
2.11 Detector Control .................................................................................................. 26
2.12 System Wellness, Predictive Performance, and Diagnostics ............................... 27
3 Installation ................................................................................................................... 29
3.1 Facility Requirements .............................................................................................. 29
3.2 Unpacking ................................................................................................................ 30
3.3 Positioning the Detector in the UltiMate 3000 System ........................................... 31
3.4 Connecting the Detector .......................................................................................... 32
3.4.1 General Information ....................................................................................... 32
3.4.2 Connecting the USB Cable ............................................................................. 32
3.4.3 Connecting the Power Cord ............................................................................ 34
3.4.4 Connecting the Analog Outputs (Optional) .................................................... 34
3.5 Setting Up the Detector in Chromeleon ................................................................... 37
3.5.1 Loading the USB Driver for the Detector ...................................................... 37
3.5.2 Installing the Detector .................................................................................... 39
3.5.3 Configuring the Detector ................................................................................ 40
3.6 Setting Up the Detector in DCMSLink .................................................................... 44
Operating Instructions Page i
UltiMate 3000 Series:
Fluorescence Detectors FLD-3100 and FLD-3400RS
4 Preparation for Operation (Startup) ........................................................................ 45
4.1 Overview .................................................................................................................. 45
4.2 General Precautions for Connecting Capillaries ...................................................... 46
4.3 Connecting the Drain System .................................................................................. 47
4.4 Installing the Flow Cell ............................................................................................ 48
4.5 Equilibrating the System .......................................................................................... 51
4.6 General Guidelines for Detector Operation ............................................................. 52
4.6.1 Mobile Phases ................................................................................................. 52
4.6.2 Mobile Phase Delivery System ....................................................................... 53
4.6.3 Flow Cells ....................................................................................................... 53
5 Operation and Maintenance ...................................................................................... 55
5.1 Power-Up ................................................................................................................. 55
5.2 Detector Display ...................................................................................................... 55
5.3 Menus on the Detector Display ................................................................................ 57
5.3.1 Detector Menus ............................................................................................... 58
5.3.2 General Menu Layout and Structure ............................................................... 59
5.3.3 Main Menu ...................................................................................................... 61
5.3.4 Configuration Menu ........................................................................................ 62
5.3.5 Diagnostics Menu ........................................................................................... 63
5.3.6 Service Menu .................................................................................................. 63
5.4 Operation with Chromeleon ..................................................................................... 64
5.4.1 Connecting to Chromeleon ............................................................................. 64
5.4.2 Direct Control ................................................................................................. 65
5.4.3 Automated Control ......................................................................................... 67
5.4.4 SmartStartup and SmartShutdown .................................................................. 71
5.5 Operational Settings ................................................................................................. 72
5.5.1 Detecting Liquid Leaks in the Detector .......................................................... 72
5.5.2 Adjusting the screen brightness or contrast .................................................... 72
5.6 Operational Modes of the Detector .......................................................................... 73
5.6.1 Single-Channel Mode ..................................................................................... 73
5.6.2 Multi-Channel Mode (FLD-3400RS Only) .................................................... 73
5.6.3 Zero Order Mode ............................................................................................ 74
5.6.4 2D Scans ......................................................................................................... 74
5.6.5 3D Scans (only Chromeleon 7.1 or later) ....................................................... 76
5.7 Optimizing Detector Performance ........................................................................... 77
5.7.1 Determining the Optimum Excitation and Emission Wavelength.................. 78
5.7.2 Sensitivity (Detector Sensitivity) .................................................................... 81
5.7.3 Filter Wheel Setting (FLD-3400RS only) ...................................................... 85
5.7.4 Response Time and Data Collection Rate ...................................................... 86
5.7.5 Multi-Channel Performance ........................................................................... 87
5.7.6 Flow Cell Temperature ................................................................................... 88
5.7.7 Lamp Mode ..................................................................................................... 88
5.7.8 Baseline Behavior ........................................................................................... 89
5.8 Monitoring System Functions .................................................................................. 90
5.8.1 Wavelength Calibration and Verification ....................................................... 90
Page ii Operating Instructions
UltiMate 3000 Series:
Fluorescence Detectors FLD-3100 and FLD-3400RS
5.8.2 Recording the Flow Cell Temperature ........................................................... 92
5.8.3 Predictive Performance................................................................................... 92
5.8.4 Operational Qualification and Performance Qualification ............................. 92
5.9 Shutting Down the Detector .................................................................................... 93
5.10 Routine and Preventive Maintenance Intervals ................................................... 95
6 Troubleshooting .......................................................................................................... 97
6.1 Overview .................................................................................................................. 97
6.2 Messages on the Detector Display ........................................................................... 98
6.3 Operating Problems ............................................................................................... 102
7 Service ........................................................................................................................ 107
7.1 General Notes and Safety Precautions ................................................................... 107
7.2 Lamp ...................................................................................................................... 108
7.3 Flow Cell ................................................................................................................ 109
7.3.1 Flushing the Flow Cell ................................................................................. 109
7.3.2 Replacing the Flow Cell ............................................................................... 110
7.4 Drying the Leak Sensor ......................................................................................... 113
7.5 Replacing the Main Power Fuses........................................................................... 114
7.6 Updating the Detector Firmware ........................................................................... 115
8 Technical Information .............................................................................................. 117
9 Accessories, Consumables, and Spare Parts .......................................................... 119
9.1 Standard Accessories ............................................................................................. 119
9.2 Optional Accessories ............................................................................................. 120
9.3 Consumables and Spare Parts ................................................................................ 121
10 Appendix: Common Mobile Phases ........................................................................ 123
11 Index ........................................................................................................................... 125
Operating Instructions Page iii
UltiMate 3000 Series:
Fluorescence Detectors FLD-3100 and FLD-3400RS
Page iv Operating Instructions
UltiMate 3000 Series:
Fluorescence Detectors FLD-3100 and FLD-3400RS
1 Introduction
1.1 How to Use This Manual
The layout of this manual is designed to provide quick reference to the sections of interest
to the reader. However, in order to obtain a full understanding of your Thermo Scientific™
Dionex™ detector, Thermo Fisher Scientific recommends that you review the manual
thoroughly before beginning operation.
All descriptions in the manual apply to the following variants of the fluorescence detector in
the UltiMate™ 3000 series:
• FLD-3100
• FLD-3400RS
The following conventions apply to the descriptions throughout this manual:
• The term "the detector" or "the device" is used throughout the manual. If some detail
applies to only one version, the detector is identified by name.
• If not otherwise stated, the descriptions for the Viper™ capillary connections apply also
to the nanoViper™ and possible other Viper capillary connections.
• The device configuration may vary. Therefore, not all descriptions necessarily apply to
your particular module.
• The representation of a component in this manual may be slightly different from the real
component. However, this does not influence the descriptions.
• The descriptions in this manual refer to firmware version 1.41 and Chromeleon™ 6.80
Service Release 13. If you want to operate the detector from Chromeleon 7, note the
information on page 26.
This manual is provided "as is". Every effort has been made to supply complete and
accurate information and all technical specifications have been developed with the utmost
care. The information contained in this manual should not be construed as a commitment
by Thermo Fisher Scientific. Thermo Fisher Scientific assumes no responsibility for any
errors that may appear in this document. This document is believed to be complete and
accurate at the time of publication. In no event shall Thermo Fisher Scientific be liable for
incidental or consequential damages in connection with or arising from the use of this
document.
The information contained in this document is subject to change without notice.
Operating Instructions Page 1
UltiMate 3000 Series:
Fluorescence Detectors FLD-3100 and FLD-3400RS
All rights reserved, including those for photomechanical reproduction and storage on
electronic media. No part of this publication may be copied or distributed, transmitted,
transcribed, stored in a retrieval system, or transmitted into any human or computer language,
in any form or by any means, electronic, mechanical, magnetic, manual, or otherwise, or
disclosed to third parties without the express written permission of Thermo Fisher Scientific
Inc.
Trademarks
Analyst is a registered trademark of AB Sciex.
Compass and Hystar are trademarks of Bruker Daltonics.
Empower is a registered trademark of Waters Corp.
PEEK is a trademark of Victrex PLC.
LiChrosolv is a registered trademark of Merck KGAA.
Windows and Windows Vista are registered trademarks of Microsoft Corp.
All other trademarks are property of Thermo Fisher Scientific Inc. and its subsidiaries.
Page 2 Operating Instructions
UltiMate 3000 Series:
Fluorescence Detectors FLD-3100 and FLD-3400RS
1.2 Safety
The CE Mark label and cTUVus Mark safety label on the instrument indicate that the
detector is compliant with the related standards.
1.2.1 Symbols on the Instrument and in the Manual
The table shows the symbols used on the instrument:
Symbol Description
Alternating current—Courant alternatif
Power supply is on (-)—L'instrument est mis sous tension (-) and Power
supply is off (O)—L'instrument est mis hors tension (O)
Surface becomes hot during operation—La surface devient chaude lors du
fonctionnement.
Refer to the Operating Instructions to prevent risk of harm to the operator and
to protect the instrument against damage.
Référez-vous à ce manuel pour éviter tout risque de blessure à l'opérateur et/ou
protéger l'instrument contre tout dommage
Label according to the "Measures for Administration of the Pollution Control of
Electronic Information Products" (China RoHS) guideline
Étiquette "Measures for Administration of the Pollution Control of Electronic
Information Products" (China RoHS)
WEEE (Waste Electrical and Electronic Equipment) label—For more
information, see the WEEE Information section in the "Installation and
Qualification Documents for Chromatography Instruments" binder. Étiquette
WEEE (Waste Electrical and Electronic Equipment)—Pour plus d'informations,
référez-vous au chapitre WEEE Information dans le classeur "Installation and
Qualification Documents for Chromatography Instruments"
Operating Instructions Page 3
UltiMate 3000 Series:
Fluorescence Detectors FLD-3100 and FLD-3400RS
At various points throughout the manual, messages of particular importance are indicated
by certain symbols:
Tip: Indicates general information, as well as information intended to
optimize the performance of the instrument.
Important: Indicates that failure to take note of the accompanying information
could cause wrong results or may result in damage to the instrument.
Important: Indique que ne pas tenir compte de l'information jointe peut conduire
à de faux résultat ou endommager l'instrument.
Warning: Indicates that failure to take note of the accompanying information
may result in personal injury.
Avertissement: Indique que ne pas tenir compte de l'information jointe peut entraîner
des blessures corporelles.
Page 4 Operating Instructions
UltiMate 3000 Series:
Fluorescence Detectors FLD-3100 and FLD-3400RS
1.2.2 Safety Precautions
When working with analytical instrumentation, you must know the potential hazards of
using chemical solvents.
Tip: Before initial operation of the detector, make yourself familiar with
the contents of this manual.
For the safety precautions in French, see page 8.
Warning: All users of the device must observe the following safety precautions
and all additional safety precautions in this manual to avoid the
possibility of personal injury or damage to the device when
operating the device or carrying out any maintenance or service
procedures.
Observe any warning labels on the device and see the related
sections in these Operating Instructions.
• Protective equipment
When performing any work on or near the HPLC system, wear personal protective
equipment (protective clothing, safety gloves, safety glasses) as required by the hazard of
the mobile phase and sample. For information about the proper handling of a particular
substance and for advice on specific hazards, refer to the material safety data sheet for the
substance you are using. Observe the guidelines of Good Laboratory Practice (GLP).
An eyewash facility and a sink should be close to the device. If any substance splashes on
the eyes or skin, wash the affected area and seek medical attention.
• Hazardous substances
Many organic solvents, mobile phases, and samples are harmful to health. Be sure that
you know the toxic and infectious properties of all substances that you are using. You
may not know the toxic or infectious properties of many substances that you are using. If
you have any doubt about a substance, treat it as if it contains a potentially harmful
substance. For advice on the proper handling of a particular substance, refer to the Safety
Data Sheet (SDS) of the manufacturer. Observe the guidelines of Good Laboratory
Practice (GLP).
Dispose of waste substance in an environmentally safe manner that is consistent with all
local regulations. Do not allow flammable, toxic, and/or infectious substances to
accumulate. Follow a regulated, approved waste disposal program. Never dispose of
flammable, toxic, and/or infectious substances through the municipal sewage system.
• Hazardous gases
Install the HPLC system in a well-ventilated laboratory. If the mobile phase or sample
includes volatile or flammable solvents, do not allow them to enter the workspace. If the
mobile phase or sample includes volatile or flammable solvents, avoid open flames and
sparks.
Operating Instructions Page 5
UltiMate 3000 Series:
Fluorescence Detectors FLD-3100 and FLD-3400RS
• Electrostatic discharge
Discharge of electrostatic energy may lead to sparking and can constitute a fire hazard.
Keep in mind that liquid flowing through capillaries can generate static electricity. This
effect is particularly pronounced in insulating capillaries and with non-conductive
solvents (for example, pure acetonitrile).
Take appropriate measures to prevent the generation of static electricity near the HPLC
system. For example, make sure that the air humidity level in the laboratory is
sufficiently high and provide proper ventilation, wear anti-static clothing or shoes,
prevent accumulation of air bubbles in waste lines, and use grounded waste containers.
Use only non-conductive capillaries to direct solvents into the waste container. With
electrically conductive capillaries, make sure that they are properly grounded.
• Self-ignition of solvents
Do not use solvents for which the self-ignition temperature is below 150 °C. In case of
leakage, these solvents may self-ignite on a hot surface.
• Capillaries, capillary connections, open connections
♦ Capillaries, especially non-metallic capillaries may burst, slip out of their fittings or
may not be screwed in. This may result in substances spraying out of the open
connections.
♦ In an UltiMate 3000 system, some components are made of PEEK™. This polymer
has superb chemical resistance to most organic solvents. However, it tends to swell
when in contact with trichlormethane (CHCl3), dimethyl sulfoxide (DMSO), or
tetrahydrofuran (THF). In addition, it is attacked by concentrated acids, such as,
sulfuric acid and nitric acid or a mixture of hexane, ethyl acetate, and methanol. In
both cases, capillaries may start leaking or they can burst. Swelling or attack by
concentrated acids is not a problem with brief flushing procedures.
♦ Do not use tubing that is stressed, bent, kinked, or damaged.
♦ Capillary connections can be contaminated by harmful substances or harmful
substances can escape from open connections.
♦ Always wear safety glasses when handling fused silica tubing, for example, during
installation or when cutting capillaries to the length.
• Hot surfaces
♦ During operation, the lamps and the surrounding parts become extremely hot and
remain so for some time after the detector is turned off. To avoid possible injury,
allow sufficient time for the lamp to cool down after turning off the detector. Only
then start with the maintenance and repair work.
♦ Flow cells can become extremely hot during operation. To avoid possible injury,
allow sufficient time for the flow cell to cool down before replacing the cell.
• Disconnect the detector from all power sources before removing the panels. When the
panels are removed, dangerous electrical connections will be exposed. The enclosure
must be opened only by Thermo Fisher Scientific service personnel.
Page 6 Operating Instructions
UltiMate 3000 Series:
Fluorescence Detectors FLD-3100 and FLD-3400RS
• Always replace blown fuses with original spare part fuses authorized by Thermo Fisher
Scientific.
• Replace faulty communication cables.
• Replace faulty power cords. Never use a power cord other than the power cords provided
for the device.
• Use only the original spare parts and accessories authorized for the device by Thermo
Fisher Scientific.
• When lifting or moving the detector, always lift the unit by the bottom sides or sides. Do
not lift the detector by the front panel door. This may damage the door.
• Do not place any heavy objects on the open front panel door. This may damage the door.
• After operation, rinse out buffers and solutions that form peroxides.
• Before switching from buffer to organic solution, rinse the analytical system thoroughly
with deionized or HPLC grade water.
• When switching to another solvent, ensure that the new solvent is miscible with the one
contained in the HPLC system. If the solvents are not miscible, the system can be
damaged, for example, by flocculation.
• If a leak occurs, turn off the instrument and remedy the situation immediately.
• Use only standard solvents (HPLC grade or fluorescence grade for highest sensitivity)
and buffers that are compatible with all parts that may be exposed to solvents.
• Before interrupting operation for several days or more or when preparing the detector for
transport, observe the precautions for shutting down the detector (→ page 93).
• Do not use the detector in ways other than those described in these Operating
Instructions.
• Keep the operating instructions near the device to be available for quick reference.
Operating Instructions Page 7
UltiMate 3000 Series:
Fluorescence Detectors FLD-3100 and FLD-3400RS
1.2.3 Consignes de Sécurité
Si vous utilisez d'instrumentation analytique, vous devez connaître les risques d'utilisation
de produit chimiques.
Veuillez noter: Avant de commencer à utiliser l'instrument, assurez-vous que vous
vous êtes familiarisés avec le contenu de ce manuel.
Avertissement: Toutes les personnes utilisant l’instrument doivent observer les
consignes de sécurité suivantes et dans les autres chapitres de ce
manuel pour éviter une mise en danger de sa personne ou de
dommage à l’instrument pendant l’utilisation et des opérations de
maintenance ou service de l’instrument.
Observez les étiquettes d'avertissement sur l'instrument et référezvous aux sections correspondantes dans ce mode d'emploi.
• Equipment de protection
Pour tous les travaux sur le système HPLC ou à proximité, portez l'équipement de
protection personnel (vêtements de protection, gant de sécurité, lunettes de protection)
qui correspond aux risque découlant de la phase mobile et/ou de l'échantillon. Pour les
informations sur la manipulation correcte des composés et des recommandations pour les
situations de risque spécifiques, veuillez consulter la fiche de données de sécurité des
substances que vous utilisez. Veuillez respecter des directives des Bonnes Pratiques de
Laboratoire (BPL).
Une installation permettant de se laver les yeux ainsi qu'un lavabo doivent se trouver à
proximité du système. Si une substance, quelle qu'elle soit, entre en contact avec vos
yeux ou votre peau, rincez abondamment la zone affectée à l’eau, puis.
• Substances dangereuses
De nombreux solvants organiques, phases mobiles et échantillons sont nuisibles à la
santé. Informez-vous de propriétés toxicologiques et infectieuses de toutes les substances
que vous utilisez. Les propriétés toxicologiques et infectieuses de nombreuses substances
peuvent être mal connues. Au moindre doute concernant une substance, traitez-la comme
s'il contenait une substance potentiellement dangereuse. Pour des instructions comment
utiliser correctement des composés particuliers, veuillez consulter à la fiche de données
des sécurités du fabricant respectif. Veuillez respecter des directives des Bonnes
Pratiques de Laboratoire (BPL).
Débarrassez-vous de tous les déchets de substances de manière écologique,
conformément à la règlementation en vigueur au niveau local. Empêchez impérativement
l'accumulation de solvants inflammables, toxiques et/ou infectieux. Suivez un
programme d'élimination des déchets règlementé et approuvé. Ne jetez jamais de
solvants inflammables, toxiques et/ou infectieux dans le système municipal d'évacuation
des eaux usées.
Page 8 Operating Instructions
UltiMate 3000 Series:
Fluorescence Detectors FLD-3100 and FLD-3400RS
• Gaz dangereux
Installez le système HPLC dans un laboratoire bien ventilé. Si la phase mobile ou
l’échantillon contient des solvants volatils ou inflammables, vous devez assurer qu'ils ne
pénètrent dans l'espace de travail. Si la phase mobile ou l’échantillon contient des
solvants volatils ou inflammables, évitez les flammes nues et les sources d’étincelles à
proximité.
• Décharge électrostatique
Décharge électrostatique peut provoquer la formation d'étincelles et peut présenter un
risque d’incendie. Veuillez noter que des solvants fluides dans les capillaires peuvent se
charger automatiquement. Cet effet se peut produire particulièrement forte dans les
capillaires isolants et avec des solvants non-conducteurs (par exemple, l'acetonitrile pur).
Prenez des mesures appropriées pour éviter les charges électrostatiques à proximité du
système HPLC. Par exemple, s'assurez qu'il y a une humidité de l'air suffisante et une
ventilation adéquate dans la laboratoire, portez des vêtements ou équipement de
protection antistatique, évitez l'accumulation de bulles d'air dans les lignes de déchets et
utilisez des réservoirs à déchets mis à la terre.
Utilisez uniquement des capillaires non-conducteurs pour diriger solvants au réservoir de
déchets. Capillaires électriquement conducteur devrait être mis à la terre.
• Inflammation spontanée des solvants
N’utilisez aucun solvants avec une température d‘auto-inflammabilité inférieure à
150° C. Si une fuite se produit, ces solvants peuvent s’auto-enflammer au contact d’une
surface chaude.
• Capillaires, connecteur capillaires, connexions ouvertes
♦ Des capillaires, en particulier les capillaires non-métalliques, pourraient fendre ou
glisser des connecteurs ou ne peuvent pas être vissés. Ceci peut en résulter aussi que
des substances pourraient jaillir des connexions ouvertes.
♦ Dans un système UltiMate 3000, certaines composantes sont en PEEK. Bien que ce
polymère présente une excellente résistance chimique à la plupart des solvants
organiques, il a tendance à gonfler lorsqu'il est en contact prolongé avec du
chloroforme (CHCl3), du diméthyle sulfoxyde (DMSO) ou du tétrahydrofurane
(THF). De plus, il est attaqué par des acides concentrés tels que l'acide sulfurique et
l'acide nitrique ou d'un composé du hexane, éthyle acétate et méthanol. Ceci peut
causer des capillaires de fuite ou risquer des capillaires d’éclater. Ces acides peuvent
cependant être utilisés dans le cadre de procédures de nettoyage, à condition que
l’exposition soit brève.
♦ N'utilisez pas de capillaires écrasés, pliés, abimés ou endommagés.
♦ Les connecteurs capillaires pour pourrait être contaminé par des substances
dangereuses ou des substances dangereuses pourrait sortir des connexions ouvertes.
Operating Instructions Page 9
UltiMate 3000 Series:
Fluorescence Detectors FLD-3100 and FLD-3400RS
♦ Dans un système UltiMate 3000 Bio RS, certains capillaires du système Viper sont
faits d'alliage de nickel-cobalt MP35N. Contact avec la peau peut provoquer une
réaction chez les personnes qui sont sensibles au nickel/cobalt.
♦ Portez des lunettes de protection lorsque vous manipulez des capillaires en silice
fondue (pendant l'installation, découpe, etc.).
• Surface chaude
♦ Lampes et les parties environnantes deviennent très chaudes pendant le
fonctionnement. Pour éviter toute blessure, vous attendez après mise hors tension
jusqu'à ce que les lampes soient refroidies. Commencer seulement alors les travaux
d'entretien.
♦ Les cellules de mesure peuvent devenir très chaudes pendant le fonctionnement. Pour
éviter toute blessure, vous attendez jusqu'à ce que la cellule est refroidi avant de
remplacer le capteur.
• Quand les capots de protection de l’appareil sont démontés, vous êtes exposés à des
connexions électriques sous haute tension deviennent accessibles. Débranchez
l'instrument de toute source d'alimentation électrique avant de retirer les capots. Ne
démontez les capots de protection que si cela est explicitement demandé au cours de ces
instructions. Les capots de protection devraient être démontés uniquement par le
personnel de service de Thermo Fisher Scientific.
• Remplacez toujours les fusibles grillés par des fusibles de rechange autorisés par Thermo
Fisher Scientific (→ page 114).
• Remplacez les câbles de communication défectueux.
• Remplacez les cordons d'alimentation électrique défectueux. Utilisez uniquement les
cordons d’alimentation électrique spécifique à l’instrument.
• Utilisez seulement des pièces de rechange originales et des accessoires autorisés par
Thermo Fisher Scientific.
• Réglez toujours une limite de pression minimum pour le système HPLC. Ceci prévient
les dommages résultant de fuites ou du fonctionnement à sec de la pompe.
• Lorsque vous soulevez ou l’instrument, tenez-le toujours par le dessous ou par les côtés
de l'unité. Soulever l’instrument par la partie avant inférieure ou par le panneau avant
peut endommager la porte.
• Ne placez aucun objet lourd sur la porte ouverte du panneau avant. Ceci pourrait
endommager la porte.
• Après utilisation, purgez le système des tampons et des susceptibles de former des
peroxydes.
• Lorsque vous passez d’une solution saline à un solvant organique, effectuez un rinçage
intermédiaire du système HPLC à l'eau dé-ionisée ou qualité HPLC.
Page 10 Operating Instructions
UltiMate 3000 Series:
Fluorescence Detectors FLD-3100 and FLD-3400RS
• Lorsque vous passez à un autre solvant, assurez-vous que le nouveau solvant soit
miscible avec celui qui se trouve dans le système HPLC. Dans le cas contraire, le
système HPLC peut être endommagé; par exemple, par des floculations!
• Si une fuite se produit, arrêtez immédiatement l’instrument, stoppez le débit de la pompe
et remédiez au problème.
• Utilisez uniquement des solvants de qualité HPLC ou qualité fluorescence (pour
maximiser la sensibilité) et des solutions salines compatibles avec les matériaux exposés
phase mobiles.
• Avant d'interrompre le fonctionnement pendant plusieurs jours ou plus, observez les
précautions figurant en page 114).
• De nombreux solvants organiques et solutions salines sont toxiques. Informez-vous des
propriétés toxicologiques de toutes les phases mobiles que vous utilisez.
• N'utilisez pas l'instrument de manière autre que celles décrites dans ce manuel.
• Conservez ce manuel á proximité de l’instrument pour pouvoir le consulter facilement.
Operating Instructions Page 11
UltiMate 3000 Series:
Fluorescence Detectors FLD-3100 and FLD-3400RS
1.3 Intended Use
For Research Use Only. Not for use in diagnostic procedures. The device is designed to be
operated only be qualified and authorized personnel. All users must know the hazards
presented by the device and the used substances.
The detector is designed for laboratory research use in high-performance liquid
chromatography (HPLC) or ultra-high performance liquid chromatography (UHPLC)
applications. It is part of the UltiMate 3000 system, but can be used also with other HPLC
systems if adequate control inputs and outputs are available.
The detector can be controlled by the Chromeleon Chromatography Management System.
Being part of the UltiMate 3000 system, the detector can also be operated with other data
systems, such as
• Xcalibur™, Compass™/HyStar™, or Analyst®. Installation of the DCMS
Link
(Thermo
Scientific Dionex Chromatography Mass Spectrometry Link) software is required in
addition to the installation of the data system.
• Empower™. Installation of the Thermo Scientific Dionex Instrument Integration
Software is required in addition to the installation of the data system.
For more information, contact the Thermo Fisher Scientific sales organization for Dionex
HPLC Products.
Keep the following in mind:
• Note that the detector may be operated only with accessories and spare parts
recommended by Thermo Fisher Scientific (→ page 119) and within its technical
specifications (→ page 117).
• Note the special properties of the solvents, such as the viscosity, boiling point, and UV
absorption (UV/VIS detector). Also observe the information about the solvent
compatibility of the other UltiMate 3000 system modules. For more information, refer to
the Operating Instructions for the modules.
• Buffer concentration: Typically up to 1 mol/L (< 0.1 mol/L chloride ions).
• Also observe the information about the solvent compatibility and buffer concentrations of
the other UltiMate 3000 system modules. For more information, refer to the Operating
Instructions for the modules.
Page 12 Operating Instructions
UltiMate 3000 Series:
Fluorescence Detectors FLD-3100 and FLD-3400RS
If there is any question regarding appropriate usage, contact Thermo Fisher Scientific before
proceeding.
Warning: If the device is used in a manner not specified by Thermo Fisher
Scientific, the protection provided by the device could be impaired.
Thermo Fisher Scientific assumes no responsibility and will not be
liable for operator injury and/or instrument damage. Whenever it is
likely that the protection is impaired, the instrument must be
disconnected from all power sources and be secured against any
intended operation.
Avertissement: Si l'instrument est utilisé de façon non spécifiée par Thermo Fisher
Scientific, la protection prévue par l'instrument pourrait être altérée.
Thermo Fisher Scientific n'assume aucune responsabilité et ne sera
pas responsable des blessures de l'operateur et/ou des dommages de
l'instrument. Si la protection de l'instrument n'est pas garanti à tout
moment, débranchez l'instrument de toutes les sources d'alimentation
électrique et assurez-vous que l'instrument n'est pas utilisé
involontairement.
Operating Instructions Page 13
UltiMate 3000 Series:
Fluorescence Detectors FLD-3100 and FLD-3400RS
1.4 Federal Communications Commission (FCC) Note
This equipment has been tested and found to comply with the limits for a Class A digital
device, pursuant to part 15 of the U.S. FCC Rules. These limits are designed to provide
reasonable protection against harmful interference when the equipment is operated in a
commercial environment. This equipment generates, uses, and can radiate radio frequency
energy and, if not installed and used in accordance with the instruction manual, may cause
harmful interference to radio communications. Operation of this equipment in a residential
area is likely to cause harmful interference, in which case the user will be required to
correct the interference at his expense.
Page 14 Operating Instructions
UltiMate 3000 Series:
Fluorescence Detectors FLD-3100 and FLD-3400RS
2 Overview
2.1 Unit Description
The detector is a high-quality instrument designed for HPLC analysis as part of the
UltiMate 3000 system.
• A xenon flash lamp is used to exite a wavelength range of 200 to 880 nm.
• With the unique Dual-PMT option, the wavelength range can be extended to the near
infrared spectral region (up to 900 nm) without any loss in sensitivity in the UV/VIS
spectral region.
• Data collection rates in single channel mode of up to 100 Hz (FLD-3100) or up to 200 Hz
(FLD-3400RS under Chromeleon 7) allow rapid separations in UHPLC. The wavelength
switching time is < 250 ms.
• The detector is optimized for high sensitivity (signal-to-noise ratio higher than 550 for
the Raman spectrum of water), over the entire lifetime of the lamp. It is thus possible to
detect even smallest peaks.
• The flow cells are equipped with an active temperature control to ensure improved
reproducibility when ambient temperatures fluctuate.
• To suppress the higher-order radiation typical of grating spectrometers and scattering of
light, the detector is equipped with an optical filter. Users can select the wavelength range
that is suppressed by the filter for FLD-3400RS detectors.
• The FLD-3400RS can measure up to four channels (2D data) with independent
parameters (wavelengths, sensitivity, filter wheel) simultaneously.
• The detector can be controlled by the Chromeleon Chromatography Management
System. This provides a high degree of system integration, as well as maximum analysis
efficiency due to comprehensive data analysis and evaluation features in Chromeleon.
• Various safety and monitoring features are provided for optimum system performance
and reliability (→ page 27).
• All parts that may be exposed to solvents are made of materials that provide optimum
resistance to the most commonly used solvents and buffer solutions in HPLC.
Operating Instructions Page 15
UltiMate 3000 Series:
Absorption of light
Emission of
Fluorescence Detectors FLD-3100 and FLD-3400RS
2.2 Operating Principle
Fluorescence detectors are optical detectors. In a fluorescence detector, the sample is
exposed to light at a defined wavelength (excitation). The thus excited sample substance
emits light at a higher wavelength (emission). The photomultiplier is positioned at an angle
of 90° to the light source and detects the light that was emitted from the fluorescing
substances. In contrast to UV/Vis detectors, a fluorescence detector measures a very weak
light signal rather than the difference between light intensities (absorbance).
Fig. 1: Simplified presentation of absorption in a molecule
light of a longer
wavelength
Fig. 2: Simplified presentation of the light emission in a molecule (fluorescence)
Fluorescence is used, for example, in highlighters or in whitening agents (optical
brighteners). Fluorescent paint used in highlighters reacts to the blue and near, non-visible
ultraviolet range of the daylight and gives off light at a longer wavelength (typically bluegreen, yellow and red).
As shown in Fig. 3 (→ page 17), the light beam from the xenon lamp (no. 1) is focused by the
lamp optics (no. 2) through the entrance of the excitation monochromator (no. 3). The
excitation monochromator transmits only light of the user-selected wavelength to the sample
inside the flow cell (no. 4). Most of the light penetrates the sample. A reference detector
(no. 5) behind the flow cell measures the intensity of this light. The excitation light stimulates
the sample to emit fluorescence light.
Page 16 Operating Instructions
UltiMate 3000 Series:
Fluorescence Detectors FLD-3100 and FLD-3400RS
When the light exits the flow cell, it is focused by the emission optics (no. 6) through the
emission monochromator (no. 8).
A cut-off filter, which lets only light above a certain wavelength pass, is located before the
emission monochromator. In the FLD-3100, the filter has a fixed cut-off wavelength
(280 nm). In the FLD-3400RS, a filter wheel (no. 7) is installed. With the help of a motor the
wheel can be moved to 5 different positions with different cut-off wavelengths. The selectable
filter helps to achieve an even better sensitivity and increase flexibility during method
development.
The emission monochromator transmits only the light with the user-selected emission
wavelength to a photomultiplier tube (PMT) (no. 9), where the light is measured. A second
optional red-sensitive photomultiplier tube (no. 10) measures light in the near infrared region
(up to 900 nm).
Fig. 3: Optics setup (schematic)
Operating Instructions Page 17
UltiMate 3000 Series:
Fluorescence Detectors FLD-3100 and FLD-3400RS
No. Component Description
1 Xenon lamp Light source for the UV to near-infrared wavelength range
2 Lamp optics Receives the light beam emitted from the xenon lamp and focuses it so
that the beam passes through the excitation monochromator.
3 Excitation
monochromator
4 Flow cell The eluent with the analyte travels through the flow cell. The excitation
5 Reference detector Measures the excitation light intensity though the flow cell.
6 Emission optics Receives the light beam emitted from the flow cell and focuses it so that
7 Filter wheel Carries the optical filter, which is used to cut off light up to a certain
8 Emission
monochromator
9 PMT Photomultiplier tube (PMT) - Converts the emitted light to a
10 Second PMT (Optional) A second red-sensitive photomultiplier tube measures light in
Lets only light with the selected excitation wavelength pass.
light passes through the flow cell to the reference detector, the
fluorescence light exits the flow cell at an angle of 90° to the excitation
light.
the beam passes through the emission monochromator.
wavelength. The FLD-3400RS provides five filter positions with
different cut-off wavelengths.
Lets only light with the selected emission wavelength pass.
measureable current signal.
the near infrared region (up to 900 nm).
Page 18 Operating Instructions
UltiMate 3000 Series:
Fluorescence Detectors FLD-3100 and FLD-3400RS
2.3 Configurations
The detector is available in the following configurations:
Detector Description Part no.
FLD-3400RS detector for measurements up to 200 Hz*. Up to four
5078.0020
wavelengths can be recorded simultaneously.
FLD-3400RS detector with Dual-PMT 5078.0025
FLD-3100 detector for measurements up to 100 Hz. However, only
5078.0010
one wavelength can be recorded.
FLD-3100 detector with Dual-PMT 5078.0015
*Only with Chromeleon 7.1 or later
Dual-PMT
The variants of the FLD with Dual PMT are equipped with a second PMT for the near
infrared region (up to 900 nm) (→ no. 10, Fig. 3, page 17). Depending on the PMT setting,
the instrument selects the suitable PMT for each measurement, or you can manually select
which PMT should be used. For emission scans, you can scan with both PMTs
simultaneously.
Detectors with a single PMT can later be upgraded with a second PMT by the Thermo
Fisher Scientific Service for Dionex HPLC Products.
Operating Instructions Page 19
UltiMate 3000 Series:
1
1
2
3
Fluorescence Detectors FLD-3100 and FLD-3400RS
2.4 Interior Components
The front panel door tilts downward to provide easy access to the inside front panel, for
example, for maintenance and repair work.
Important: The open front panel door is not designed to carry weight. Therefore,
you should not place any objects on the open front panel door.
Important: Ne placez aucun objet lourd sur la porte ouverte du panneau avant.
Ceci pourrait endommager la porte.
Fig. 4: Interior view from the front
No. Description
1
Slots in the enclosure to route the flow cell capillaries to the outside (→ page 23)
Two more slots with capillary guides are provided in the enclosure bottom.
2
Leak sensor (→ page 25)
3 Flow cell
No flow cell is installed when the detector is shipped. Before initial operation, install a flow cell.
Page 20 Operating Instructions
1
2
3
2.5 Front Panel Elements
UltiMate 3000 Series:
Fluorescence Detectors FLD-3100 and FLD-3400RS
Fig. 5: Front panel view
No. Front Panel
Element
1 Display
2 Standby button Switches the detector to Standby mode (the LED is lighted). To cancel
3
LEDs
Power The LED is blue when the detector is on.
Connected The LED is green when the detector is controlled by Chromeleon.
Status The LED is red when an error has been detected, e.g. when the lamp has
Function
Shows information about the detector:
- General information upon power up (→ page 55)
- Status screen, depending on the operating mode (→ page 55)
- Various menus, accessible via the menu key (→ page 57)
- Messages (→ page 97)
Standby mode and resume operation, press the Standby button again (the
LED is not lighted).
Note: To allow the detector to change the mode, press the Standby button
for at least one second.
failed. In addition, the corresponding message appears on the front panel
display (→ page 97).
The LED is orange, for example, when the detector is booting.
Otherwise, the LED is green.
Operating Instructions Page 21
UltiMate 3000 Series:
6
Fluorescence Detectors FLD-3100 and FLD-3400RS
2.6 Rear Panel
1 2 5
3 4
Fig. 6: Rear panel
No. Description
1
2
3
4
5
6
Power switch (→ page 22)
Fuse cartridge (→ page 22)
Main power receptacle (→ page 34)
Type label
USB 2.0 (Universal Serial Bus) port for connection to the Chromeleon computer (→ page 23)
Analog outputs (optional, → page 34)
2.6.1 Power Switch
The power switch on the rear panel is the main power switch for the detector. Turn on the
power switch before initial operation of the detector and leave it on. For routine operation,
leave the main power switch on. For routine on/off control, use the standby button on the
front of the detector (→ page 21). Press and hold the button for about one second to allow
the detector to change the mode. Turn off the main power switch when instructed to do so,
for example, before performing a service procedure or when interrupting operation for
longer periods (one week or more). Observe the precautions on page 93.
2.6.2 Fuse Cartridge
The fuse cartridge contains two slow-blow fuses, rated at 2 A (5 x 20 mm). For
information about how to change the fuses, see page 114.
Page 22 Operating Instructions
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