Thermo Scientific Dionex UltiMate 3000 Series Operating Instructions Manual
  1. Manuals
  2. Brands
  3. Thermo Scientific Manuals
  4. Security Sensors
  5. Dionex UltiMate 3000 Series
  6. Operating instructions manual

Thermo Scientific Dionex UltiMate 3000 Series Operating Instructions Manual

Fluorescence detectors
Hide thumbs Also See for Dionex UltiMate 3000 Series:
Table of Contents

Advertisement

Quick Links

Download this manual See also: 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

Advertisement

Table of Contents
loading
Need help?

Need help?

Do you have a question about the Dionex UltiMate 3000 Series and is the answer not in the manual?

Questions and answers

Subscribe to Our Youtube Channel

Related Manuals for Thermo Scientific Dionex UltiMate 3000 Series

Summary of Contents for Thermo Scientific Dionex UltiMate 3000 Series

  • Page 1 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...
  • Page 2 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Operating Instructions...
  • Page 3 ( O r i g i n a l D e c l a r a t i o n o f C o n f o r m i t y) Product: Thermo Scientific Dionex UltiMate 3000 - Detector Types:...
  • Page 4 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Page II Operating Instructions...

  • Page 5: Table Of Contents

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Table of Contents 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...
  • Page 6 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 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 ..................
  • Page 7 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 Troubleshooting ......................
  • Page 8 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Page iv Operating Instructions...

  • Page 9: Introduction

    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.
  • Page 10 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.

  • Page 11: Safety

    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...
  • Page 12 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.

  • Page 13: Safety Precautions

    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.
  • Page 14 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).
  • Page 15 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.

  • Page 16: Consignes De Sécurité

    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...
  • Page 17 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...
  • Page 18 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. ♦...
  • Page 19 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! •...

  • Page 20: Intended Use

    • 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.
  • Page 21 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.

  • Page 22: Federal Communications Commission (Fcc) Note

    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.

  • Page 23: Overview

    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. •...

  • Page 24: Operating Principle

    UltiMate 3000 Series: 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°...
  • Page 25 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.
  • Page 26 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Component Description Xenon lamp Light source for the UV to near-infrared wavelength range Lamp optics Receives the light beam emitted from the xenon lamp and focuses it so that the beam passes through the excitation monochromator. Excitation Lets only light with the selected excitation wavelength pass.

  • Page 27: Configurations

    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.

  • Page 28: Interior Components

    UltiMate 3000 Series: 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.

  • Page 29: Front Panel Elements

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 2.5 Front Panel Elements Fig. 5: Front panel view Front Panel Function Element Display 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 30: Rear Panel

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 2.6 Rear Panel Fig. 6: Rear panel Description 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 31: Usb Port

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 2.6.3 USB Port The Chromeleon Chromatography Management System uses a USB connection to control the detector. Data is transferred digitally via the appropriate USB cable (→ page 32). The PC must be equipped with a USB port. To ensure trouble-free operation, use only the cables shipped with the detector.

  • Page 32: Flow Cells

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 2.8 Flow Cells The detector is shipped without a flow cell. The following flow cells are available for the detector: Volume Flow cell Flow cell type Flow cell volume Heat exchanger Part no. material and/or inlet capillary Analytical,...

  • Page 33: Lamp

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 2.9 Lamp The light source is a xenon flash lamp with a power of 15W. The flash frequency of the lamp varies, depending on the selected lamp mode. The lamp is turned on when data acquisition starts, and automatically turned off after data acquisition was stopped to extend its lifetime.

  • Page 34: Detector Control

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 2.11 Detector Control The detector can be controlled by the Chromeleon Chromatography Management System. To operate the detector with Chromeleon, an appropriate Chromeleon version and the corresponding license are required. Tip: All software details in this manual refer to Chromeleon 6.80, unless stated otherwise.

  • Page 35: System Wellness, Predictive Performance, And Diagnostics

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 2.12 System Wellness, Predictive Performance, and Diagnostics System Wellness monitors the health of the detector. Therefore, the detector supports several performance and reliability features that can help you detect small problems before they turn into big ones: •...
  • Page 36 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Page 28 Operating Instructions...

  • Page 37: Installation

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 3 Installation 3.1 Facility Requirements The installation site must meet the following requirements: • The main power switch and the main power receptacle are on the rear panel. Make sure that ♦ Free and unrestricted access to the main power switch is ensured at all times. ♦...

  • Page 38: Unpacking

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 3.2 Unpacking All electrical and mechanical components of the detector are carefully tested before the instrument is shipped from the factory. After unpacking the detector, inspect the module for any signs of mechanical damage, which might have occurred during transit. Tips: Immediately report any shipping damage to both, the incoming carrier and Thermo Fisher Scientific.

  • Page 39: Positioning The Detector In The Ultimate 3000 System

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 3.3 Positioning the Detector in the UltiMate 3000 System If the detector is part of an UltiMate 3000 system, for example, for analytical HPLC applications, you should stack the individual modules. However, the arrangement of the system modules depends on the application.

  • Page 40: Connecting The Detector

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 3.4 Connecting the Detector 3.4.1 General Information Verify that Chromeleon is installed on the computer and that the license code is entered before you connect the detector to the USB port on the Chromeleon computer and turn on the detector power.
  • Page 41 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Solvent rack Pump Autosampler Column compartment Fluorescence detector Fig. 8: Example for the rear panel connections on an UltiMate 3000 system Operating Instructions Page 33...

  • Page 42: Connecting The Power Cord

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 3.4.3 Connecting the Power Cord Use the power cord shipped with the device to connect the detector to the main power source. No manual adjustment is required to adapt the line voltage to local voltage requirements.
  • Page 43 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 4. Slide the left guide bar of the DAC board onto the green edge next to the USB port. USB port Guide bar Fig. 10: Installing the DAC board 5. Push the board partially into the enclosure. Apply slight pressure between the two analog outputs to push the board further into the enclosure until it locks into position.
  • Page 44 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 3.4.4.3 Configuring the Analog Outputs Make the required settings for the analog outputs in Chromeleon. 1. On the Detector page in the Properties dialog of the detector, verify that the DAC Board check box is selected (→ page 42). When the check box is cleared, the analog outputs will not be available in Chromeleon.

  • Page 45: Setting Up The Detector In Chromeleon

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 3.5 Setting Up the Detector in Chromeleon This section provides brief instructions for setting up the detector in Chromeleon. For details, see the Chromeleon Help. Tip: When the detector is connected to the Chromeleon computer, verify that the Chromeleon software is installed before turning on the detector power for the first time.
  • Page 46 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 7. Windows Vista, Windows 7, and Windows Server 2008 will automatically detect the new detector and perform the USB installation. If Windows fails to detect the detector and launches a wizard instead, this indicates that you connected the detector to the computer and turned on the power for the first time before you installed Chromeleon.

  • Page 47: Installing The Detector

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 3.5.2 Installing the Detector After the USB software for the detector has been installed (→ page 37), install and configure the detector in Chromeleon: 1. Start the Chromeleon Server Monitor (→ page 37) and the Chromeleon server if they are not yet running.

  • Page 48: Configuring The Detector

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 3.5.3 Configuring the Detector 3.5.3.1 Initial Installation During the installation, Chromeleon connects to the detector and transfers the settings from the instrument firmware to Chromeleon, setting the options on the wizard pages accordingly.
  • Page 49 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS ♦ Click Write to save the data currently delivered by the detector as a demo file. Enter the file name in the Virtual Mode File Name field or select a name from the list. Tip: When recording virtual mode files in Chromeleon 6.80, the size of the file is limited to 35MB.
  • Page 50 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Detector Page The Detector page shows the detector configuration. Fig. 12: Detector page FLD Type • Select the detector type. Make sure that the selected option corresponds to the actually installed detector type. Device Name •...
  • Page 51 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Signals Page The page lists all signal channels that the detector can record. A name is defined for each channel. To allow raw data collection for a channel, select the Enabled check box next to the channel name.

  • Page 52: Setting Up The Detector In Dcmslink

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 3.6 Setting Up the Detector in DCMSLink To set up the detector in DCMSLink, refer to DCMSLink Installation Guide, which is provided on the DCMSLink DVD in the Additional Documents\DCMSLink User Documents folder. 1.

  • Page 53: Preparation For Operation (Startup)

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 4 Preparation for Operation (Startup) 4.1 Overview After you have unpacked, positioned and connected the detector as described in sections 3.1 through 3.5 (→ page 29 and following), prepare the detector for operation. Follow the sequence of steps below: 1.

  • Page 54: General Precautions For Connecting Capillaries

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 4.2 General Precautions for Connecting Capillaries When connecting capillaries, observe the following general precautions: • Observe the precautionary statements for capillaries and capillary connections in section 1.2.2 (→ page 5). • UltiMate 3000 systems with stainless steel fluidics are shipped with Viper capillary kits. The kits include a Viper capillary for connecting the detector to the separation column when the system includes only one detector.

  • Page 55: Connecting The Drain System

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS ♦ Conventional fitting connections (non-Viper) Do not over-tighten these fitting connections. If you observe leakage on the connection, tighten a little further. If leakage still exists, first consider cleaning the connection port with a cleaning swab (part no.

  • Page 56: Installing The Flow Cell

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 4.4 Installing the Flow Cell Observe the following when installing a flow cell: • Always hold flow cells by the flow cell body with the type label. Do not touch the optical block of the flow cell (→...
  • Page 57 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS • The backpressure on the flow cell must not exceed 20 bar (analytical flow cell) or 40 bar (micro flow cell). Do not connect any capillaries or instruments to the flow cell out line as this might generate a higher backpressure.
  • Page 58 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 2. Insert the flow cell straight into the cell opening. Fig. 17: Inserting the flow cell 3. Tighten the flow cell screws hand-tight. Flow cell screws Fig. 18: Tighten the flow cell screws 4.

  • Page 59: Equilibrating The System

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 4.5 Equilibrating the System Before using the detector for sample analysis, equilibrate the UltiMate 3000 system: 1. Pump the starting solvent through the entire system until the system is free of any other liquid composition.

  • Page 60: General Guidelines For Detector Operation

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 4.6 General Guidelines for Detector Operation The following sections offer general guidelines for detector operation. For information about how to optimize the detector performance, see section 5.7 (→ page 77). 4.6.1 Mobile Phases Mobile phase quality significantly affects detection limits and instrument performance.

  • Page 61: Mobile Phase Delivery System

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 4.6.2 Mobile Phase Delivery System The pumping system should deliver continuous flow while ensuring intermixing of the mobile phase (if gradient elution is used). Fluctuations in pump backpressure can cause baseline noise. If the noise is synchronized with the pump stroke, check your HPLC pump. The plastics present in some solvent delivery systems from third-party manufacturers are not fully compatible with the solvents commonly used in chromatography.
  • Page 62 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS • The flow cells are sensitive to dirt and dust. Therefore: ♦ Always keep unused flow cells in their original dust-free packaging. ♦ Always hold flow cells by the flow cell body with the type label. Do not touch the optical block of the flow cell (→...

  • Page 63: Operation And Maintenance

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 5 Operation and Maintenance The detector can be controlled by the Chromeleon Chromatography Management System. For details, see section 5.4 (→ page 64) and the following. 5.1 Power-Up To start the detector for the first time, turn on the main power switch on the rear panel of the detector.
  • Page 64 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS View the progress of data acquisition on the detector display After data acquisition was started via Chromeleon (AcqOn), you can monitor the progress of data acquisition on the display. The display shows a scaled fluorescence value (in counts) at the selected wavelength.

  • Page 65: Menus On The Detector Display

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 5.3 Menus on the Detector Display Via the menus that are available on the front panel display, you can make several settings or access information directly from the detector. For information about the menus, see section 5.3.1 (→ page 58). Showing the menu key Four white spots can be found on the front panel below the display.

  • Page 66: Detector Menus

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 5.3.1 Detector Menus Fig. 24 shows an overview of the detector menus. For information about the general menu layout and structure, see page 59. For information about the individual commands and parameters, see sections 5.3.3 through 5.3.5 (→ page 61 and following pages). Main 2.

  • Page 67: General Menu Layout And Structure

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 5.3.2 General Menu Layout and Structure In general, the menu layout is as follows: > Main (1..3) 1. Control 2. Diagnostics 3. Service ∨ ∧ Select Back Fig. 25: Menu layout (here Main menu) Description Reports the menu name and the number of items on the menu list.
  • Page 68 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS To … Select ... Toggle between two operating states (for example, between Silent and Audible in the Toggle Leak sensor mode). Confirm the selection and perform the action. For example, if you change the brightness of the display, you have to select OK to confirm the change.

  • Page 69: Main Menu

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 5.3.3 Main Menu The Main menu provides top-level access to the menu structure. To open the Main menu, show the function keys and select Menu (→ page 57). > Main (1..3) 1. Configuration 2.

  • Page 70: Configuration Menu

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 5.3.4 Configuration Menu The Configuration menu provides information about the detector configuration and allows you to make the required settings or change the settings. > Configuration (1..3) 1. Reset to factory defaults 2.

  • Page 71: Diagnostics Menu

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 5.3.5 Diagnostics Menu The Diagnostics menu provides information for diagnostics purposes (read-only). > Diagnostics (1..4) 1. System 2. Sensors 3. Flow Cell 4. Temperatures ∨ ∧ Select Back Fig. 28: Diagnostics menu You can see the following information (all information is read-only): To …...

  • Page 72: Operation With Chromeleon

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 5.4 Operation with Chromeleon Before you begin, verify that 1. The Chromeleon software is installed on the computer and the license code is entered. 2. The detector is connected to the Chromeleon computer via a USB connection. Tip: Verify that Chromeleon is installed on the computer and that the license code is entered before you connect the detector to the USB port on the Chromeleon computer and turn on the detector power.

  • Page 73: Direct Control

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS When the detector is correctly connected to Chromeleon The Connected LED on the front panel is green. • • Front panel input related to the measurement is disabled. • Functions for estimating the lifetime of consumables and monitoring and recording service and (re)qualification information are provided (→...
  • Page 74 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 5. Change the display filter level if necessary. Right-click in the commands list and select the filter level on the menu. Fig. 29: Commands dialog box 6. Verify that the detector is connected to Chromeleon. If it is not, select Connect to connect the detector.

  • Page 75: Automated Control

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 3. Verify that the detector is connected to Chromeleon (the LED next to the Connect button is green). If it is not, click Connect. Fig. 30: Detector control panel (here FLD-3400RS) The control panel provides access to the operating parameters and commands required for routine operation of the detector.
  • Page 76 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS To create a program with the Program Wizard 1. Open the Program Wizard. On the File menu, select New, and then select Program File. 2. The wizard guides you through program creation. On each wizard page, make the desired settings or accept the default values.
  • Page 77 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS When you record multiple channels (FLD-3400RS only), the baseline noise increases at higher data collection rates. The maximum data collection rate and response time depend on a number of parameters and are always automatically calculated on the basis of the selected parameters.
  • Page 78 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS To create a program manually 1. Open an existing program. Select and double-click the program you want to open. —or— On the File menu, select Open. In the dialog box, select Program on the Object of Type list and select the program.

  • Page 79: Smartstartup And Smartshutdown

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS To start a program Program for sample analysis 1. Create a sample list (sequence). A sequence must include the program and a method for evaluating the sample data (for example, for peak identification, area determination, and amount determination).

  • Page 80: Operational Settings

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 5.5 Operational Settings 5.5.1 Detecting Liquid Leaks in the Detector Leak detection is enabled as a standard when the detector is shipped. When leak detection is active and the leak sensor reports a leak •...

  • Page 81: Operational Modes Of The Detector

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 5.6 Operational Modes of the Detector 5.6.1 Single-Channel Mode A fluorescence detector is usually operated in single-channel mode, that is, a single excitation/emission wavelength pair is measured. As this mode provides the highest possible data rates and best signal-to-noise ratio, always use the single-channel mode for very small peaks.

  • Page 82: Zero Order Mode

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 5.6.3 Zero Order Mode In Zero Order Mode, the grating of the emission monochromator is set to the position of zero order. In this position, the monochromator lets the entire spectrum pass, rather than only a certain wavelength.
  • Page 83 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Emission Scan The wavelength on the excitation monochromator is kept constant, while the emission monochromator scans a wavelength range. The result is an emission spectrum of the sample. Synchro Scan A user-defined excitation wavelength range is scanned, while the emission wavelength is scanned synchronously with a fixed distance.

  • Page 84: Scans (Only Chromeleon 7.1 Or Later)

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Complete the following steps to record an emission spectrum: 1. Open the Commands dialog box for the detector. Under ScanStartEmWavelength, enter the first wavelength of the range to be scanned, and the last wavelength under ScanEndEmWavelength.

  • Page 85: Optimizing Detector Performance

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 5.7 Optimizing Detector Performance The performance of the detector can be optimized by careful selection of key operating parameters. The table summarizes these parameters, indicates the performance characteristics affected, and offers guidelines for selecting the parameters. Operating Parameter Performance characteristics affected Selection...

  • Page 86: Determining The Optimum Excitation And Emission Wavelength

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 5.7.1 Determining the Optimum Excitation and Emission Wavelength The most important parameters that need to be optimized are the excitation and emission wavelength. Note the following key criteria for determining the wavelength for an analysis: •...
  • Page 87 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Method using 2 samples of different concentrations with a diode array detector and the fluorescence detector If your UltiMate 3000 system includes a diode array detector (DAD-3000 or DAD-3000RS), you can use the UV spectrum determined with the diode array detector to find the optimum excitation wavelengths and retention times.
  • Page 88 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Wavelength switching in Chromeleon Thermo Fisher Scientific recommends using the single-channel mode to record data by switching the wavelengths in-between the detected peaks of the various sample components, rather than to simultaneously measure all interesting wavelengths in multi-channel mode. Use the Program Wizard to set the start wavelengths for one channel (→...

  • Page 89: Sensitivity (Detector Sensitivity)

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 5.7.2 Sensitivity (Detector Sensitivity) The sensitivity is used to optimize the signal-to-noise ratio in a chromatogram. Depending on the intensity of the fluorescence, it may be necessary to adjust the sensitivity several times during an analysis.
  • Page 90 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Fig. 35: Effects of the Sensitivity setting Determining the optimum Sensitivity Determine the optimum sensitivity in a separate sample run after you have determined the optimum wavelengths (→ page 78). Use a sample (standard) with the maximum expected concentration of the analytes and select a sensitivity at which a saturation is not expected (for example;...
  • Page 91 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Therefore, use the MaxPMTSaturation parameter to optimize the Sensitivity (→ Fig. 35 right). This parameter continuously stores the maximum PMT saturation in percent of the saturation value. A program example can be found in the Chromeleon Help. 1.
  • Page 92 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Run a sample and read out the MaxPMTSaturation values in Chromeleon and evaluate the results: Value What you should do... Increase the Sensitivity. The following is a rough guideline: < 30% < 30 %: by one stage <...

  • Page 93: Filter Wheel Setting (Fld-3400Rs Only)

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 5.7.3 Filter Wheel Setting (FLD-3400RS only) To prevent this stray light from reaching the PMT, additional optical edge filters are installed in the light path between the flow cell and the emission monochromator. This reduces direct scattering of light from the light source.

  • Page 94: Response Time And Data Collection Rate

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS • You can manually select the filter wavelength. Available filters are 280 nm, 370 nm, 435 nm or 530 nm. The selected emission wavelength must not be more than 15 nm below the filter wavelength. In special situations (for example, if the emission wavelength is near the cut-off wavelength of a filter), setting the filter manually may provide better results than the Auto setting.

  • Page 95: Multi-Channel Performance

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Data collection rate • Data can be generated with a maximum collection rate of 100 Hz or 200 Hz (FLD-3400RS under Chromeleon 7.1 or later). The LongLife lamp mode supports a maximum data collection rate of 20 Hz. •...

  • Page 96: Flow Cell Temperature

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 5.7.6 Flow Cell Temperature The temperature of a sample influences its fluorescence. Thus, a problem with fluorescence detection is that the results can strongly be influenced by fluctuations in ambient temperature. The FLD allows you to heat the flow cell and thus keep temperatures inside the flow cell at a constant level.

  • Page 97: Baseline Behavior

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS You can select the Lamp Mode directly in the Program Wizard (→ page 68) if you have selected a single wavelength channel. Tip: You can change the lamp mode during a measurement, for example, from LongLife mode (between the peaks) to Standard or HighPower mode (for the interesting peaks).

  • Page 98: Monitoring System Functions

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 5.8 Monitoring System Functions This section provides a short overview of some special functions for qualification, documentation and monitoring the system that Chromeleon supports for the detector. Some functions are available also on the control panel for the detector. For additional information about a function, see the Chromeleon Help.
  • Page 99 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS To perform wavelength verification You can perform wavelength verification via Chromeleon. Wavelength verification can take a few minutes. During this time, data acquisition is not possible. 1. Open the Commands dialog box for the detector. 2.

  • Page 100: Recording The Flow Cell Temperature

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 5.8.2 Recording the Flow Cell Temperature The FLD_FlowCell channel for recording the flow cell temperature is available in the Commands dialog box for the detector and on the FLD Options page in the Program Wizard (→...

  • Page 101: Shutting Down The Detector

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 5.9 Shutting Down the Detector Observe the following precautions before interrupting the operation or before shipping the detector: • Even during periods of detector inactivity, a flow cell or the cover shipped with the detector must be installed.
  • Page 102 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS To create a standby or shutdown program Select one of the following alternatives: • Select and perform the operating commands and parameters from the Commands dialog box. • Create and run a corresponding program to automate the process (→ page 67). •...

  • Page 103: Routine And Preventive Maintenance Intervals

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 5.10 Routine and Preventive Maintenance Intervals The detector is made of high-quality components and materials to minimize maintenance requirements. All surfaces are well resistant to weak acids, alkali, and organic solvents. Nevertheless, immediately wipe up all liquids spilled onto the detector surface by using lint-free cloth or paper.
  • Page 104 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Page 96 Operating Instructions...

  • Page 105: Troubleshooting

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 6 Troubleshooting 6.1 Overview The following features help you to identify and eliminate the source for problems that may occur during the operation of the detector or UltiMate 3000 system. Status Screens The status indicators on the front panel provide a quick visual check of the operational status of the detector.

  • Page 106: Messages On The Detector Display

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 6.2 Messages on the Detector Display Each time a fault or error occurs during the operation of the detector, the Status LED on the front panel door changes to red (or orange) and a message appears on the detector display.
  • Page 107 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Message Remedial Action Flow cell temperature Verify that the flow cell is properly installed. Open and close the front sensor not found. panel door. Turn the detector off and on again by pressing the power switch on the rear of the detector.
  • Page 108 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Message Remedial Action PMT sensitivity restored The Sensitivity was restored to the initial value (= x) after automatic for <CHANNEL> - new adjustment. sensitivity is x. Scan command with equal Enter a different start and end time for the wavelength scan range. start and end position.
  • Page 109 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS When the detector is operated with Chromeleon and if communication between Chromeleon and the detector cannot be established, related messages may appear in the Chromeleon Audit Trail. Message Remedial Action The USB connection between the detector and the Chromeleon server FLD-3100@USB-1610103 - may be interrupted.

  • Page 110: Operating Problems

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 6.3 Operating Problems The following table provides information about common operating problems that might occur with an UltiMate 3000 system and lists probable causes, as well as remedial actions. For more information, also see the manuals for the other modules of the UltiMate 3000 system.
  • Page 111 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Problem Probable Cause Remedial Action Analysis run takes a The flow cell is still being Check the set flow cell temperature. At long time to start or preheated. high flow rates, the flow cell may not does not start at all.
  • Page 112 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Problem Probable Cause Remedial Action Peak broadening, The capillaries are clogged, or Replace the capillaries. Use different peak tailing, capillary connections bad. capillaries, for example, Viper increased dead time capillaries. (Cont'd) The sample loop is clogged. Replace the needle (→...
  • Page 113 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Problem Probable Cause Remedial Action Negative peaks Sample solvent and mobile Dissolve the sample in the mobile phase. phase differ in composition. The fluorescence of the solute Select a different wavelength pair. Use a is lower than the fluorescence mobile phase with less background of mobile phase.
  • Page 114 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Problem Probable Cause Remedial Action Poor peak area Carry-over occurs in the Flush the needle using an appropriate precision system. solvent (→ Autosampler Manual). (Cont'd) The capillary connections are Check and tighten the capillary not installed properly or they connections.

  • Page 115: Service

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 7 Service 7.1 General Notes and Safety Precautions The following sections describe all procedures for the detector that the user may perform. All other maintenance and service procedures must be performed only by Thermo Fisher Scientific service personnel.

  • Page 116: Lamp

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 7.2 Lamp The lamp must be replaced only by Thermo Fisher Scientific Service for Dionex HPLC Products. Never try to exchange the lamp or open the enclosure yourself. You can monitor the lamp age. This function can help to decide when a lamp is due to be replaced.

  • Page 117: Flow Cell

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 7.3 Flow Cell 7.3.1 Flushing the Flow Cell Flush the flow cell when you suspect that eluent or sample components may have deposited on the cell walls. Complete the following steps: 1. Flush the flow cell with HPLC-grade water. 2.

  • Page 118: Replacing The Flow Cell

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 7.3.2 Replacing the Flow Cell Observe the following when removing or installing a flow cell: Warning: 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.
  • Page 119 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 7.3.2.1 Removing the Flow Cell 1. Stop the pump flow. 2. Open the front panel door and disconnect the capillaries from the cell inlet and outlet connection ports, if applicable. Close the flow cell inlet and outlet with the dummy plugs that were installed when the flow cell was shipped.
  • Page 120 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 7.3.2.2 Installing the Flow Cell 1. Insert the flow cell straight into the cell opening. Fig. 39: Inserting the flow cell 2. Tighten the flow cell screws (→ Fig. 38) hand-tight. 3. Remove the dummy plugs on the flow cell in and out connection ports. Reconnect the flow cell inlet to the separation column and reconnect the waste capillary to the flow cell outlet.

  • Page 121: Drying The Leak Sensor

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 7.4 Drying the Leak Sensor The leak sensor is installed inside the detector and reports a leak when liquid collects in the drip tray under the fluid connections. Eliminate the cause for the leakage and dry the leak sensor.

  • Page 122: Replacing The Main Power Fuses

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 7.5 Replacing the Main Power Fuses Warning: Turn off the main power switch. Disconnect the power cord from its source. Avertissement: Avant de remplacer les fusibles, arrêtez le détecteur. Assurez-vous de bien débrancher le cordon d'alimentation de la source secteur. 1.

  • Page 123: Updating The Detector Firmware

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 7.6 Updating the Detector Firmware The detector is shipped with the most recent firmware version. The detector firmware is also included in Chromeleon. To check which firmware version is installed in the detector and which version is included in Chromeleon: •...
  • Page 124 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 3. Right-click the detector in the timebase and select Properties on the menu. 4. On the General page (→ page 40), the firmware version provided by Chromeleon for the detector is displayed in the Firmware field. If more than one firmware version is available for the detector in Chromeleon, select the version from the Firmware list.

  • Page 125: Technical Information

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 8 Technical Information Specification FLD-3100 FLD-3400RS Optical Design: Two monochromators with concave holographic gratings and hyperbolic mirrors for highest efficiency in light transmission Light source: Xenon flash lamp (15W); Three different flash frequencies (HighPower, Standard, LongLife) can be selected.
  • Page 126 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Specification FLD-3100 FLD-3400RS Flow cells: Analytical standard flow cell: Cell volume: 8 µL; pressure limit: 20 bar Wetted parts: carbon reinforced PTFE, fused silica, stainless steel Micro flow cell: Cell volume: 2 µL; pressure limit: 40 bar Wetted parts: carbon reinforced PTFE, fused silica, stainless steel Identification of flow cell type and serial number by mean of an built-in ID chip.

  • Page 127: Accessories, Consumables, And Spare Parts

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 9 Accessories, Consumables, and Spare Parts Accessories, spare parts, and consumables for the detector are always maintained at the latest technical standard. Therefore, part numbers are subject to alteration. However, updated parts will always be compatible with the parts they replace. 9.1 Standard Accessories The following standard accessories are shipped with the detector.

  • Page 128: Optional Accessories

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 9.2 Optional Accessories Description Part no. Remarks Analytical flow cell 6078.4230 For installation details, see page 48. For details about the flow cell, see page 117. Micro flow cell 6078.4330 For installation details, see page 48. For details about the flow cell, see page 117.

  • Page 129: Consumables And Spare Parts

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 9.3 Consumables and Spare Parts The part number always refers to the packing unit. Unless otherwise stated, the packing unit is 1 unit. For more information, contact the Thermo Fisher Scientific sales organization for Dionex HPLC Products.
  • Page 130 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Page 122 Operating Instructions...

  • Page 131: Appendix: Common Mobile Phases

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 10 Appendix: Common Mobile Phases The mobile phase composition affects its UV cutoff, that is, the minimum effective wave- length for the measurement. In general, mobile phases are solvents, such as, water, acetonitrile, methanol, or other substances.
  • Page 132 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Page 124 Operating Instructions...

  • Page 133: Index

    UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS 11 Index SmartShutdown ..........71 SmartStartup ..........71 USB Driver ........... 37 2D Scans ............74 Wavelength Calibration ........ 91 2nd PMT ............42 Wavelength Verification ....... 91 Chromeleon Dialog Detector ............42 3D Scans ............
  • Page 134 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Emission Monochromator ......... 17 Infrared Detector ..........19 Emission Scan ............ 75 Installation Emission Wavelength ........78 Connections ..........32 Equilibration ............51 In Chromeleon ..........37 Equilibration (SmartStartup Wizard) ....51 In DCMSLink ..........
  • Page 135 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Response Time ..........86 RMA Number ..........107 Ok ..............60 Operating Hours (Lamp) ........108 Operating Instructions.......... 1 Safety ..............3 Operating Principle ..........16 Safety Precautions ..........5 Operating Problems ......... 102 Scans Operation ............
  • Page 136 UltiMate 3000 Series: Fluorescence Detectors FLD-3100 and FLD-3400RS Unit Description Wavelength Calibration ........90 Flow Cells ............. 24 Wavelength Verification ........90 Overview ............15 Fails ............105 Unpacking ............30 Steps to Perform ........... 91 USB ..............32 Wellness ............27 USB Configuration File ........

This manual is also suitable for:

Fld-3100Fld-3400rs

Table of Contents