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UltiMate FLM-3100B

Dionex UltiMate FLM-3100, UltiMate FLM-3300, UltiMate FLM-3200, UltiMate FLM-3100B, UltiMate FLM-3300B Operating Instructions Manual

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UltiMate 3000 Series
Flow Managers and
Thermostatted Column Compartments
Operating Instructions
Revision: 1.1 Date: September 2007
© 2007 Dionex
Operating Instructions
Declaration of Conformity
Product: Flow Manager and Column Compartment Types: FLM-3100, FLM-3200, FLM-3300 FLM-3100B, FLM-3200B, FLM-3300B
Dionex Softron GmbH herewith declares conformity of the above products with the respective requirements of the following regulations:
• Low-Voltage Equipment Directive 73/23/EEC changed by 93/68/EEC
• EMC Directive 2004/108/EG
The electrical safety of the products was evaluated based on the following standard:
• EN 61010-1: 2002 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: 2004 Electrical equipment for measurement, control and laboratory use EMC Requirements
This declaration is issued for the manufacturer
Dionex Softron GmbH Dornierstrasse 4 D-82110 Germering
by the President, Dr. Peter Jochum.
August 1, 2007 _________________________ Dr. Peter Jochum
Operating Instructions Page I
Page II Operating Instructions
Table of Contents
1 Introduction................................................................................................................... 1
1.1 How to Use This Manual.......................................................................................1
1.2 Safety Information .................................................................................................1
1.2.1 Symbols on the Instrument and in the Manual .................................................. 2
1.2.2 General Safety Precautions................................................................................ 3
1.2.3 Consignes Générales de Sécurité....................................................................... 5
1.3 Intended Use .......................................................................................................... 8
1.4 Federal Communications Commission (FCC) Note.............................................. 8
2 Overview ........................................................................................................................9
2.1 Product Overview .................................................................................................. 9
2.2 Theory of Operation (UltiFlow) ..........................................................................11
2.3 Supported Configurations.................................................................................... 12
2.3.1 General............................................................................................................. 12
2.3.2 Biocompatible Flow Managers........................................................................ 13
2.4 General Flow Manager Design............................................................................ 17
2.5 Column Switching Valve..................................................................................... 18
2.6 Flow Splitter ........................................................................................................ 19
2.7 Front Panel Display and Controls........................................................................ 20
2.8 Rear Panel Connectors......................................................................................... 21
2.9 Leak Sensors........................................................................................................22
2.10 System Wellness..................................................................................................23
3 Installation................................................................................................................... 25
3.1 Facility Requirements.......................................................................................... 25
3.2 Unpacking............................................................................................................ 25
3.3 Positioning the Flow Manager in the UltiMate 3000 System.............................. 26
3.4 Connecting the Flow Manager............................................................................. 27
3.4.1 USB.................................................................................................................. 27
3.4.2 Power Connection............................................................................................ 27
3.4.3 Digital I/O........................................................................................................ 28
3.5 Opening the Front Panel Door............................................................................. 28
3.6 Preparing the Flow Manager ............................................................................... 29
3.6.1 Installing a Separation Column .......................................................................31
3.6.2 Connecting the Capillaries to the Column Switching Valve...........................35
3.6.3 Installing a Trap Column.................................................................................36
3.6.4 Connecting the Flow Splitter...........................................................................37
3.7 Manual Injection Port .......................................................................................... 39
Operating Instructions Page i
4 User Interface ..............................................................................................................41
4.1 Power-Up.............................................................................................................41
4.2 Status Screen........................................................................................................ 41
4.3 Soft Key Menus ................................................................................................... 42
4.4 Menu Structure and Layout ................................................................................. 43
4.4.1 Main Menu....................................................................................................... 45
4.4.2 Control Menu................................................................................................... 46
4.4.3 Information Menu............................................................................................ 47
4.4.4 Configuration Menu......................................................................................... 48
5 Software Control by Chromeleon ............................................................................. 49
5.1 General................................................................................................................. 49
5.2 Installing the Flow Manager in Chromeleon.......................................................49
5.3 Assigning the Flow Splitter ................................................................................. 56
5.4 Operating the Flow Manager with Chromeleon .................................................. 57
5.5 Column Identification System (Column ID) .......................................................58
5.6 Splitter Identification System (Splitter ID).......................................................... 59
5.7 Diagnostics........................................................................................................... 60
6 Troubleshooting ..........................................................................................................61
6.1 Overview.............................................................................................................. 61
6.2 Error Messages .................................................................................................... 62
6.3 Chromeleon Diagnostics Messages ..................................................................... 66
7 Routine Maintenance.................................................................................................. 69
7.1 General Notes ...................................................................................................... 69
7.2 Maintenance Intervals.......................................................................................... 71
7.3 Flow Control Valve .............................................................................................72
7.4 Replacing the Fuses ............................................................................................. 73
7.5 Drying the Fluid Leak Sensor.............................................................................. 74
7.6 Exchanging the Splitter Cartridge) ...................................................................... 76
7.7 Column Switching Valve..................................................................................... 79
7.8 Shutting Down the Flow Manager....................................................................... 81
8 Technical Information................................................................................................ 83
9 Accessories, Consumables and Spare Parts ............................................................. 85
9.1 Standard Accessories (included in the shipment)................................................ 85
9.2 Consumables, Spare Parts, and Optional Accessories......................................... 86
10 Technical Appendix - Pin Assignment...................................................................... 91
11 Index............................................................................................................................. 93
Page ii Operating Instructions
UltiMate 3000 Series: Flow Managers and Column Thermostats
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 user. However, in order to obtain a full understanding the flow manager and thermostatted column compartment, Dionex recommends that you review the manual thoroughly before beginning operation of the module.
Almost all descriptions in the manual apply to all flow managers of the UltiMate 3000 system and cover both the standard (stainless steel) and biocompatible models. Therefore, the terms "the flow manager" and/or "the FLM" are used throughout the manual. If some detail applies to only one model or version, the model (or version) is identified by name.
Note: The device configuration may vary (e.g., one or two column switching valves);
therefore, not all descriptions necessarily apply to your particular instrument.
The descriptions in this manual refer to firmware version 2.30 and Chromeleon
version 6.80 Service Pack 2.
The information contained in this manual is subject to change without notice and should not be construed as a commitment by Dionex. Dionex 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 Dionex be liable for incidental or consequential damages in connection with or arising from the use of this document.
CHROMELEON® is a registered trademark of Dionex. UltiMate™ is a trademark of Dionex. All other trade or company names mentioned are subject to the copyright and the property and trademark rights of the respective companies.
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 Dionex.
1.2 Safety Information
The CE Mark label and cTUVus Mark safety label on the instrument indicate that the instrument is in compliance with the related standards (→ pages I and II).
Operating Instructions Page 1
1.2.1 Symbols on the Instrument and in the Manual
The table below 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 au ce manuel pour éviter un risque de blessure à l'opérateur et/ou de protéger l'instrument contre des dommages.
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, refer to the WEEE Information section in the manual binder. Étiquette de WEEE (Waste Electrical and Electronic Equipment) —Pour plus d'information, référez-vous à la section WEEE Information dans ce fichier.
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 2 Operating Instructions
UltiMate 3000 Series: Flow Managers and Column Thermostats
1.2.2 General Safety Precautions
When working with analytical instrumentation, you should know the potential hazards of using chemical solvents.
Tips: Before initial operation of the flow manager, make sure that you are familiar
with the contents of this manual.
Observe any warning labels on the device and refer to the related sections in
these operating instructions.
For the general safety precautions in French, refer to Consignes Générales
de Sécurité (→ page 5).
Please observe the following general safety precautions when operating the instrument or carrying out any maintenance work:
• Install the HPLC system in a well-ventilated laboratory. If the mobile phase includes volatile or flammable solvents, do not allow them to enter the workspace.
• For minimum interference effects, all components of the analytical system should be connected to the same mains output (same phase).
• The flow manager is primed with a mixture of isopropanol and water (20:80). During initial operation of the flow manager, make sure that the used solvents used are miscible. Otherwise, follow the appropriate intermediate steps.
• To prevent damage to the flow manager when lifting or moving, always lift the unit by the bottom sides or sides. Lifting the flow manager by the bottom front or by the front panel door may damage the door.
• The front panel tilts downward. Do not place any heavy objects on the open front panel door. This may damage the door.
• Do not touch any metal parts inside the column chamber while the temperature set point is > 50 °C (122 °F). Wait for the chamber to cool down, for example, before changing a column or before performing any maintenance procedures.
• When operating the HPLC system, always set a lower pressure limit for the system pump. This prevents damage resulting from leakage or from running the pump dry.
• When connecting the capillaries, make sure that the connectors are free from contaminants. Even minute particles may cause damage to the flow splitter, flow control valve, and column.
Operating Instructions Page 3
• Use only standard HPLC solvents (HPLC-grade: 0.2 µm filtered) and buffers that are compatible with components in the flow path of the flow manager. Note the special properties of the solvents such as viscosity, boiling point, UV absorption (UV/VIS detector), and refractive index (refractive index detector). Buffer concentration: typically up to 1 mol/L (0.1 mol/L if chloride ions are present).
• After operation, rinse out buffers and solutions that form peroxides from your HPLC system.
• Before switching from buffer to organic solution, rinse the analytical system thoroughly with deionized or HPLG-grade water.
• When switching to another solvent, ensure that the new solvent is miscible with the one contained in the pump. Otherwise, the analytical system can be damaged; for example, by flocculation.
• Avoid open flames and sparks, in particular if the mobile phase includes volatile or flammable solvents.
• If a leak occurs, turn off the flow manager immediately, stop the pump flow, and remedy the situation.
• When the front, side or rear panels are removed, dangerous electrical connections will be exposed. Disconnect the flow manager from all power sources before removing the panels. Remove panels only when instructed to do so in these instructions.
• Always replace blown fuses with the original spare fuses from Dionex (→ Replacing the Fuses, page 73).
• Replace faulty power cords and communication cables.
• Many organic solvents and buffers are toxic. Know the toxicological properties of all
mobile phases that you are using.
• If the toxicological properties of a sample are unknown to you, treat it as if it contains a potentially harmful substance.
• Wear goggles when handling mobile phases or operating the instrument. An eye wash facility and a sink should be close to the unit. If any mobile phase splashes on the eyes or skin, wash the affected areas with sufficient water and seek medical attention.
• Dispose of all waste mobile phase in an environmentally safe manner that is consistent with all local regulations. Do not allow flammable and/or toxic solvents to accumulate. Follow a regulated, approved waste disposal program. Never dispose of flammable and/or toxic solvents through the municipal sewage system
Page 4 Operating Instructions
UltiMate 3000 Series: Flow Managers and Column Thermostats
• In an UltiMate 3000 system, some tubing is made of PEEK. While this polymer has superb chemical resistance to most organic solvents, it tends to swell when it is 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 (swelling or attack by acid is not a problem with brief flushing procedures).
• Do not use PEEK tubing that is stressed, bent, or kinked.
• Wear goggles when handling fused silica tubing (e.g., during, installation and cutting).
• Before interrupting operation for several days or more, observe the precautions in Shutting Down the Flow Manager (→ page 81).
• Use original Dionex spare parts only. Substituting non-Dionex parts or using non-Dionex
accessories may impair the performance of the instrument.
• Do not use the module in ways other than those described in this manual.
1.2.3 Consignes Générales de Sécurité
Veuillez noter: Avant de commencer à utiliser l'instrument, assurez-vous que vous
vous êtes familiarisés avec le contenu de ce manuel.
Observez les étiquettes d'avertissement sur l'appareil et référez-vous
aux sections correspondantes dans ce mode d'emploi.
Veuillez observer les consignes générales de sécurité suivantes lorsque vous utilisez l'instrument ou que vous procédez à des opérations de maintenance:
• Installez le système HPLC dans un laboratoire bien ventilé. Si la phase mobile contient des solvants volatils ou inflammables, empêchez qu'ils ne pénètrent dans l'espace de travail.
• Afin d'éviter au maximum les interférences, tous les éléments du système analytique doivent être raccordés à la même ligne secteur (même phase).
• L'instrument est stocké sous isopropanol et eau. Au cours démarrage de l'instrument, assurez-vous que les solvants utilisés soient miscibles. Sinon, suivez les étapes intermédiaires appropriées.
• 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.
Operating Instructions Page 5
• Ne touchez à aucune partie en métal à l'intérieur du compartiment de colonne tant que le point de réglage de température est > 50 °C (122 °F). Attendez que le four refroidisse, par exemple, avant de changer une colonne ou avant de procéder à tous travaux de maintenance.
• 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 connectez les capillaires, assurez-vous que les raccords sont exempts de tout contaminant. Même d'infimes particules peuvent causer des dommages au système (ex. diviseur de débit, vanne de régulation de débit et colonne).
• Utilisez uniquement des solvants HPLC (qualité HPLC : filtrés à 0.2 µm) et des sels compatibles avec les composants des circuits hydrauliques de l’instrument. Vérifiez les propriétés spécifiques des solvants telles que la viscosité, le point d'ébullition, l'absorption UV (détecteur UV/VIS) et l’indice de réfraction (réfractomètre). Concentration en sels: généralement inférieure à 1 mol/L (0.1 mol/L si présence d’ions chlorure).
• 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.
• 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!
• Evitez les flammes nues et les sources d’étincelles à proximité, en particulier si la phase mobile contient des solvants volatils ou inflammables.
• Si une fuite se produit, arrêtez immédiatement l’instrument, stoppez le débit de la pompe et remédiez au problème.
• Quand les capots de protection de l’appareil sont démontés, vous êtes exposés à des connexions électriques sous haute tension. 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.
• Remplacez toujours les fusibles grillés par des fusibles de rechange d'origine Dionex (→ Replacing the Fuses, page 73).
• Remplacez les cordons d'alimentation électrique et les câbles de communication défectueux.
• De nombreux solvants organiques et solutions salines sont toxiques. Informez-vous des propriétés toxicologiques de toutes les phases mobiles que vous utilisez.
• Les propriétés toxicologiques de nombreux échantillons peuvent être mal connues. Au moindre doute concernant un échantillon, traitez-le comme s'il contenait une substance potentiellement dangereuse.
Page 6 Operating Instructions
UltiMate 3000 Series: Flow Managers and Column Thermostats
• Portez des lunettes de protection lorsque vous manipulez des phases mobiles ou que vous utilisez l'instrument. Une installation permettant de se laver les yeux ainsi qu'un lavabo doivent se trouver à proximité du système. Si une phase mobile, quelle qu'elle soit, entre en contact avec vos yeux ou votre peau, rincez abondamment la zone affectée à l’eau, puis consultez un médecin.
• Débarrassez-vous de tous les déchets de phase mobile de manière écologique, conformément à la règlementation en vigueur au niveau local. Empêchez impérativement l'accumulation de solvants inflammables et/ou toxiques. Suivez un programme d'élimination des déchets règlementé et approuvé. Ne jetez jamais de solvants inflammables et/ou toxiques dans le système municipal d'évacuation des eaux usées.
• Dans un système UltiMate 3000, certains tubes 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 (ces acides peuvent cependant être utilisés dans le cadre de procédures de nettoyage, à condition que l’exposition soit brève).
• N'utilisez pas de tubes PEEK écrasés, pliés ou abîmés.
• Portez des lunettes de protection lorsque vous manipulez des capillaires en silice fondue
(par example pendant l'installation ou découper).
• Avant d'interrompre le fonctionnement pendant plusieurs jours ou plus, observez les précautions figurant en Shutting Down the Flow Manager (→ page 81).
• Utilisez des pièces de rechange d'origine Dionex. Effectuer des remplacements par des pièces ne provenant pas de Dionex ou utiliser des accessoires ne provenant pas de Dionex peut affecter les performances de l'instrument.
• N'utilisez pas l'instrument de manière autre que celles décrites dans ce manuel.
Operating Instructions Page 7
1.3 Intended Use
The flow manager is designed to perform equally well as a dependable system for routine analyses or as a sophisticated research instrument for use in nano, capillary, and micro HPLC (high performance liquid chromatography) applications, especially as part of the UltiMate 3000 system. However, it can also be used with other HPLC systems if adequate control inputs and outputs are available. A PC with USB port is required.
The flow manager is 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 Analyst® (Applied Biosystems/MDS Sciex), Compass™/ HyStar™ (Bruker Daltonics), or Xcalibur™ (Thermo Scientific). To do so, installation of the DCMS Chromatography Mass Spectrometry Link) software is required in addition to the installion of the data system.
Please note that the flow manager may only be operated with the accessories originally supplied with the instrument (→ page 85) and within its technical specifications (→ page 83).
Link
(Dionex
Use only standard solvents and water of at least HPLC grade (0.2 µm filtered), or better LC­MS grade and buffers that are compatible with components in the flow path of the flow manager. If water from water purification systems that are not properly maintained is used, polymeric contamination may seriously damage the column and may rapidly block solvent filters. Note the special properties of the solvents such as viscosity, boiling point, UV absorption (UV/VIS detector), and refractive index (refractive index detector).
Buffer concentration: typically up to 1 mol/L (0.1 mol/L if chloride ions are present).
If there is a question regarding appropriate usage, contact Dionex before proceeding.
Dionex is not liable for any damage, material or otherwise, resulting from inappropriate or improper use of the instrument.
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 8 Operating Instructions
UltiMate 3000 Series: Flow Managers and Column Thermostats
2 Overview
2.1 Product Overview
The flow manager is a reliable module of the UltiMate 3000 system and performs equally well as a dependable system for routine analyses or as a sophisticated research instrument for nano, capillary, and micro HPLC applications. The design has been optimized for minimum dead volume and maximum efficiency.
• The flow splitter (→ Fig. 1, page 11) delivers the low flow rates required for nano, capillary, and micro HPLC applications. The flow manager is fitted with a flow splitter identification system that allows you to store splitter-specific information on a chip card and read it out whenever you want.
• An electronic splitter identification module (→ Splitter Identification System (Splitter ID), page 59) automatically adapts the system settings to the used splitter cartridge. The module also allows you to store splitter-specific information (split ratio, flow control settings) on a chip card and read it out whenever you want. In addition, the parameters required for flow splitting are set automatically.
• UltiFlow™ technology with active control of the splitter flow keeps the set flow rates constant, independent of outside influences. Thus, the flow rate is not influenced by the solvent composition, solvent gradients, different viscosities, or analyses at different temperatures. In the same way, effects from column ageing and partial clogging will be compensated.
• Thermoelectric elements heat or actively cool the column chamber and all internal components to the desired temperature. Heat exchangers allow fast temperature changes and ensure independence from the ambient temperature, even if the temperature set point is below the ambient temperature.
• The flow manager allows compartment cooling by max. 15K from the ambient temperature. The lower temperature limit is +5 °C (+41 °F).
• The columns can be warmed up to max. +85 °C (+185 °F). An increase in temperature from 20 °C to 50 °C (68 °F to 122 °F) is realized in less than 25 minutes. This corresponds to an average performance of 2-4 K per minute.
• Temperature control allows keeping the column temperature constant. If the ambient temperature changes during the analysis, the increased heating or cooling ensures that the column temperature remains constant. The maximum deviation is ± 0.1 °C.
• Several columns of different length (maximum length: 30 cm) can be installed in the column chamber. An electronic column identification module allows GLP-compliant documentation of the column type and all important column parameters (→ Column Identification System (Column ID), page 58).
Operating Instructions Page 9
• Depending on the configuration, the flow manager is equipped with one or two column switching valves (→ Supported Configurations, page 12), e.g., for applications that require different columns at frequent intervals at similar temperatures.
• The flow manager is fully controlled by the Chromeleon Chromatography Management System, providing a high degree of system integration.
• All surfaces in the column chamber are made of materials that provide maximum
resistance to the most commonly used HPLC solvents.
• The flow managers of the UltiMate 3000 system are available as biocompatible versions,
also. For information about the characteristics of the biocompatible devices, refer to section 2.3.2 (→ page 13).
Page 10 Operating Instructions
UltiMate 3000 Series: Flow Managers and Column Thermostats
r
Valve
2.2 Theory of Operation (UltiFlow)
The fundamental requirement on a flow manager for liquid chromatography is the ability to create constant low flow rates for nano, capillary, and micro HPLC applications, as well as to equalize the temperature. The flow managers of the UltiMate 3000 system are fitted with a flow splitter with integrated flow control that ensures constant flow rates, ranging from micro liter to nano liter flows. The flow rate is influenced neither by varying column backpressures nor by the temperature or solvent viscosity.
The flow splitter is equipped with two fluidic resistors that split the flow from the pump in the reciprocal ratio of the resistance. To ensure identical pressure drop at both resistors, the outputs of the flow splitter are connected via a cross arm with integrated flow meter. A controller adjusts the unbalance flow to a very low offset value near zero to flush the cross arm with fresh solvent permanently. To ensure this, the waste path includes an adjustable valve that adjusts in dependence of the column pressure (→ Fig. 1).
This innovative method creates constant low flow rates based on the split ratio and the pump flow. Different lowest flow rates are created by different pump flow rates, but they are always split according to the split ratio. This is independent of the solvent composition and the column pressure.
Column
Control
Detecto
Waste
Pump
Flow splitter
Flow meter
1:100
Fig. 1: Operation principle of flow splitting with control
For temperature equalization, temperature stability is more important than the absolute precision of the setting. The flow manager contains advanced electronic circuits that can maintain the selected temperature with a precision of ±0.1 °C.
The thermo-optimized design reduces the time required to equilibrate the temperature between the column and the solvent. The Peltier elements of the flow manager heat up and cool down the columns. The heat exchanger inside the column chamber also helps to bring the air and all components in the chamber to the desired temperature, including the flow splitter and column switching valve(s).
Operating Instructions Page 11
These procedures ensure that
• The temperature of the stationary phase remains constant over the total column length.
• The column and the solvent have the same temperature during the analysis.
In this way, analytical separation is performed at the nominal temperature, thus, minimizing fronting and tailing as well as retention time variations.
2.3 Supported Configurations
2.3.1 General
For an overview of the currently available models, refer to the list below. If you have any questions, do not hesitate to contact your Dionex sales representative or distributor.
Application Description Part No.
FLM-3100 with two 10-port micro switching valves 5720.0010
Nano HPLC
Capillary and/or Monolithic HPLC
Micro HPLC
FLM-3100B, same as FLM-3100, but biocompatible version 5721.0010
FLM-3200 with 10-port micro and 6-port nano switching valves (1 each) 5720.0020
FLM-3200B, same as FLM-3200, but biocompatible version 5721.0020
FLM-3300 with one 10-port micro switching valve 5720.0030
FLM-3300B, same as FLM-3300, but biocompatible version 5721.0030
Tip: These flow managers are fitted with a splitter cartridge
for a split ratio of 1:1000.
FLM-3100 with two 10-port micro switching valves 5720.0015
FLM-3100B, same as FLM-3100, but biocompatible version 5721.0015
FLM-3200 with 10-port micro and 6-port nano switching valves (1 each) 5720.0025
FLM-3200B, same as FLM-3200, but biocompatible version 5721.0025
FLM-3300 with one 10-port micro switching valve 5720.0035
FLM-3300B, same as FLM-3300, but biocompatible version 5721.0035
Tip: These flow managers are fitted with a splitter cartridge
for a split ratio of 1:100.
FLM-3100 with two 10-port micro switching valves 5720.0018
FLM-3100B, same as FLM-3100, but biocompatible version 5721.0018
FLM-3200 with 10-port micro and 6-port nano switching valves (1 each) 5720.0028
FLM-3200B, same as FLM-3200, but biocompatible version 5721.0028
FLM-3300 with one 10-port micro switching valve 5720.0038
FLM-3300B, same as FLM-3300, but biocompatible version 5721.0038
Tip: These flow managers are fitted with a splitter cartridge
for a split ratio of 1:6.
Page 12 Operating Instructions
UltiMate 3000 Series: Flow Managers and Column Thermostats
Tip: All flow managers are equipped with a flow splitter. When the flow
manager is operated with Chromeleon, systems for column and/or splitter identification are supported (→ sections 5.5, page 58 and 5.6, page 59).
For information about how to replace a cartridge, refer to section 7.6 (→ page 76).
For information about the switching valve, refer to section 2.5 (→ page 18).
If you have any questions, do not hesitate to contact your Dionex sales representative or distributor.
2.3.2 Biocompatible Flow Managers
The FLM-3100B, FLM-3200B, and FLM-3300B flow managers extend UltiMate 3000 flow manager series by biocompatible device versions. Except for the flow splitter parts that are exposed to solvent and the switching valve(s) with the connected components, the biocompatible flow managers are identical to the standard devices (stainless steel). Therefore, almost all descriptions of the standard devices apply to the biocompatible versions, also. If some detail applies to only one version, the version will be identified. The differences are as follows:
Switching valve
The biocompatible flow managers are fitted with PAEK switching valves. As PAEK valves have deeper connection ports (→ Fig. 2), preassembled fitting connections (see below) must be used. This is essential for a zero dead volume connection.
Fitting not
preassembled correctly
Switching valve
Fitting
preassembled correctly
Fig. 2: Capillary connection on the switching valve
Important: Do not use a stainless steel nut and/or ferrule to connect the
components to the PAEK valve. To avoid damage to the valve, use only the supplied capillaries and fittings, as well as original Dionex spare parts.
Important: N’utilisez jamais de vis et/ou ferrules métalliques pour les connexions
sur une vanne biocompatible en PAEK. Afin d’éviter tout dommage à la vanne, utilisez seulement les capillaires et raccords fournis, ainsi que des pièces d’origine Dionex.
Operating Instructions Page 13
Follow the steps below to connect the components to the biocompatible switching valve. The description refers to the connection of a nano column, but applies to the other components, as well.
1. To establish a zero dead volume fitting connection between the column and the
switching valve, a finger-tight nut, ferrule, and sleeve are required. Slide the finger­tight nut and the ferrule onto the sleeve as shown in Fig. 3.
Column
Sleeve Finger-tight nut Ferrule
Fig. 3: Fitting connection
2. Insert the sleeve with the nut and the finger-tight nut in a port on the preassembly tool
(part no. 6000.0065) and tighten the nut by two or three manual turns. (The preassembly tool is included in the application kits for the biocompatible UltiMate 3000 system.)
Fig. 4: Preassembly tool
Important: To avoid damage to the biocompatible switching valve, neither
preassemble the fitting connection on the switching valve nor use any tool to tighten the finger-tight nut.
Important: Afin d’éviter tout dommage à la vanne d’injection biocompatible,
ne l’utilisez jamais pour le pré-sertissage des raccords, et n’utilisez aucun outil pour visser les raccords à serrage manuel.
3. Push the sleeve all the way into the port. It is essential for a zero dead volume
connection that the assembly seats firmly.
Fig. 5: Preassembling the fitting connection
Page 14 Operating Instructions
UltiMate 3000 Series: Flow Managers and Column Thermostats
4. Tighten the nut in the port until it is finger tight.
5. Carefully turn the nut an additional 1/4 turn (90°) past the point at which the ferrule
starts to grab the sleeve.
Tip: Dionex cannot provide a torque specification because the force
required to tighten the nut can vary due to the friction between nut and the thread, as well as the composition and wall thickness of the component to be connected.
6. Remove the preassembled fitting from the tool and inspect the fitting. When you
gently pull the ferrule, you should not be able to move the ferrule on the sleeve. If the ferrule sleeve moves laterally (→ Fig. 6), re-insert the fitting all the way into the preassembly tool and tighten it an additional 1/8 turn past finger-tight.
Fig. 6: Inspecting the fitting
7. Remove and re-inspect the fitting. Repeat the previous step if necessary.
8. Insert the column (or the fused silica capillary) all the way through the sleeve until it
extends the sleeve (→ Fig. 7).
Fig. 7: Inserting the column
Operating Instructions Page 15
9. Pull the column back (→ Fig. 8) and install the preassembled fitting with the column
to the appropriate port on the switching valve. Make certain that the column does not extend the sleeve when installing it into the port
Fig. 8: Pulling the column back
10. Tighten the nut finger-tight. To avoid the formation of dead volumes, make certain
that the column inlet enters all the way to the bottom of the valve port (e.g. push the column into the valve).
11. Tighten the nut additional 1/4 turn past finger-tight.
12. Start flow delivery and check for leakage. In case of any leakage, stop flow delivery
and remove the fitting. Repeat steps 8 till 11.
Tip: If you cannot use finger-tight fittings due to limited space, you may use the
long hex style nuts, instead (→ Fig. 9; part no. 6721.0017; the nuts are included in the application kits for the biocompatible UltiMate 3000 system, also). Follow the above steps and then connect the hex nut to the appropriate port on the switching valve. Tighten the nut with a ¼" wrench.
Fig. 9: Long hex style nut
Page 16 Operating Instructions
UltiMate 3000 Series: Flow Managers and Column Thermostats
2.4 General Flow Manager Design
7
7
5 5 6
5 5 6
1 2 3 4
1 2 3 4
Fig. 10: Open FLM-3100 (here: with two 2-position/10-port switching valves)
No. Description
1 Switching valve (2-position/10-port micro switching valve)
(in Chromeleon: ValveLeft or MsvPosition, depending on the device type)
2
Column bracket with column clip (→ section 3.6.1, page 31)
3
Flow splitter (→ section 7.6, page 76)
4 Switching valve (if installed: 2-position/10-port micro valve or 2-position/6-port nano valve)
(in Chromeleon: ValveRight)
5
Slots for the column ID chip cards (→ section 5.5, page 58)
6
Slot for the flow splitter chip card (→ section 5.6, page 59)
7
Locking mechanism for the front panel door (→ section 3.5, page 28)
Important: Use only the capillaries shipped with the flow manager and original
spare capillaries from Dionex. Install the capillaries and fittings only at the positions for which they are intended.
Reuse used fittings and ferrules only for the same capillary connection.
This is to avoid increased dead volume.
To connect the capillaries to the switching valve, install only the
ferrules and fitting screws provided in the accessories kit.
Operating Instructions Page 17
Important: Utilisez uniquement les capillaires fournis avec l'instrument et les
capillaires de rechange d'origine Dionex. Installez les capillaires et les raccords uniquement dans les positions pour lesquelles ils sont prévus.
La réutilisation des raccords et ferrules n’est possible que pour la
connexion capillaire d’origine, afin d’éviter l’apparition de volumes morts.
Pour brancher les capillaires à une vanne d'injection, installez
uniquement les ferrules et les raccords livrés avec la vanne et respectez les instructions d'installation du fabricant.
2.5 Column Switching Valve
Depending on the instrument configuration, the flow manager is equipped with one or two switching valves (2-position/10-port micro and/or 2-position/6-port nano valves), e.g., for applications that require different columns at frequent intervals at similar temperatures.
The switching valve automatically selects the column to be used. The valve is installed in the column chamber and is brought to the temperature equilibrium as well. The valve positions are programmed and controlled in Chromeleon. (For details, refer to the Chromeleon online Help.)
For information about how to connect the capillaries to the valve, refer to Connecting the Capillaries to the Column Switching Valve (→ page 35).
For more information about the valve, refer to the technical appendix (→ page 91).
Page 18 Operating Instructions
UltiMate 3000 Series: Flow Managers and Column Thermostats
2.6 Flow Splitter
The flow manager is equipped with a flow splitter (→ Fig. 11) that delivers the low flow rates required for nano, capillary, and micro HPLC applications. Splitter cartridges with different split ratios are available for the different applications.
For information about the cartridge types and installation details, refer to section 7.6 (→ page 76).
1
2
3
4
2
6
5
1
Fig. 11: Flow Splitter
No. Description
1 Splitter cartridge outlets
2 Flow sensor connectors
3 Flow control valve connector
4 Capillary connector, depending on your application. (The nano (capillary or micro) flow set in
Chromeleon is output here.) For the application shown in Fig. 24 (→ page 35), connect the capillary to the flow manager's right switching valve (port 4).
5 Splitter cartridge
6 Pump connector
Operating Instructions Page 19
2.7 Front Panel Display and Controls
3
1
2
Fig. 12: Front panel
No. Front Panel Element Description
1 Display Shows information about the flow manager, e.g.:
- General information upon power-up (→ section 4.1, page 41)
- Status screen (→ section 4.2, page 41)
- Various functions and menus that can be accessed via soft keys (→ section 4.3, page 42)
- Error messages (→ section 6, page 61)
2 Standby button Switches the flow manager to Standby mode (the LED is lighted).
To cancel Standby mode and resume operation, press the Standby button again (the LED is not lighted). Note: To allow the flow manager to change the mode, press the Standby button for at least 1 second.
3
LEDs
Power The LED is blue when the flow manager is on.
Connected The LED is green when the flow manager is controlled by Chromeleon.
Status The LED is green when the flow manager has reached the target temperature
and no error has been detected. The LED is orange when the flow manager has not yet reached the target temperature or when the door is open. The LED is red when an error has been detected, e.g., a leak.
Page 20 Operating Instructions
UltiMate 3000 Series: Flow Managers and Column Thermostats
2.8 Rear Panel Connectors
1
3
2
4
7
Fig. 13: Rear panel connectors
No. Description
1 Power switch
2
Fuse holder (→ section 7.3, page 72)
6 5
3 Main power receptacle
4 Type label
5
6 USB (Universal Serial Bus Interface) port for connection to the server PC
7 Waste port for directing any liquid from the waste path of the flow splitter to an appropriate waste
Digital I/O for communication with external devices (→ section 3.4.3, page 28)
(→ section 3.4.1, page 27)
container, page 30)
Operating Instructions Page 21
2.9 Leak Sensors
The flow manager contains two leak sensors to detect any humidity or gases that may accumulate in the column chamber. When a certain humidity or gas concentration is reached in the chamber (while the door is closed), the corresponding sensor is activated. Eliminate the cause for the leakage, wearing the appropriate protective clothing, and ventilate the inside before closing the door.
In addition, the flow manager contains a fluid leak sensor to detect liquid leaks from the flow control valve in the enclosure. The fluid leak sensor is installed in the rear of the enclosure (in a tray on the right). When liquid is detected in tray, e.g., due to clogging of the waste outlet (→ Fig. 18, page 30), the sensor is activated. Eliminate the cause for the leakage and dry the sensor as described in section 7.5 (→ page 74).
On the Control > Leak control display menu (→ page 46), set the sensitivity for the sensors and determine whether an acoustic beep shall alert you in case of an alarm. (You can open the Leak control display menu also via the Leak soft key (→ page 42).)
If one of the sensors detects a leak, the Status LED on the instrument's front panel is red and the related error message appears on the front panel display.
Tips: The Status LED remains red as long as the sensor is exposed to humidity,
gas, or moisture. The Clear soft key on the navigation bar (→ page 45) allows you to remove the error message from the front panel display.
If a beep alerts you, you can turn off the beep for the current alarm from the Control > Leak control display menu by setting All leak alarms to silent. If the humidity or gas sensor was activated, you can turn off the alarm also by opening the front panel door. Beeping stops in any case when the cause for the leakage has been eliminated. A new beep sounds when one of the sensors is activated again.
If the flow manager is operated by Chromeleon, you can also determine the
leak sensor mode in Chromeleon. If a sensor is activated, the related error message appears on the front panel display and the error is logged in the Chromeleon audit trail.
Inspect the flow manager for leaks every day. Tighten or replace leaking
capillary connections if necessary.
Page 22 Operating Instructions
UltiMate 3000 Series: Flow Managers and Column Thermostats
2.10 System Wellness
The flow manager supports several system wellness and reliability features that can help you detect small problems before they turn into big ones:
• Leak detector (→ page 21)
• Door status monitoring
• Column ID features for a GLP-compliant documentation of the column status (→ Column Identification System (Column ID), page 58)
• Flow splitter ID for the documentation of the splitter type and characteristics
(→ Splitter Identification System (Splitter ID), page 59)
Tip: If the flow manager is operated by Chromeleon, the system wellness features
are also available in Chromeleon (→ Diagnostics, page 60).
If an error is found, the Status LED on the front panel is red and an error message appears on the front panel display (→ Troubleshooting, page 61). If the flow manager is operated by Chromeleon, the error is also logged in the Chromeleon Audit Trail.
Operating Instructions Page 23
Page 24 Operating Instructions
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