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Waters 2414 Operator's Manual

Refractive index detector
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Waters 2414
Refractive Index
Detector
Operator's Guide
71500241402/Revision C
Copyright © Waters Corporation 2015-2017
All rights reserved

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  • Page 1 Waters 2414 Refractive Index Detector Operator’s Guide 71500241402/Revision C Copyright © Waters Corporation 2015-2017 All rights reserved...
  • Page 2 May 31, 2017, 71500241402 Rev. C...

  • Page 3: Copyright Notice

    Corporation 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 Waters Corporation be liable for incidental or consequential damages in connection with, or arising from, its use.

  • Page 4: Contacting Waters

    Contacting Waters ® Contact Waters with enhancement requests or technical questions regarding the use, transportation, removal, or disposal of any Waters product. You can reach us via the Internet, telephone, or conventional mail. Waters contact information: Contacting medium Information Internet The Waters Web site includes contact information for Waters locations worldwide.

  • Page 5: Safety Hazard Symbol Notice

    Tubing connected to this drain directs the flow to an appropriate waste container. Equipment repair or disposal Direct questions regarding repair or disposal to Waters at the address and telephone number given on page iv.

  • Page 6: Fcc Radiation Emissions Notice

    Appendix A for a comprehensive list of warning and caution advisories. Operating this instrument When operating the Waters 2414 Reflective Index Detector, follow standard quality-control (QC) procedures and the guidelines presented in this section. May 31, 2017, 71500241402 Rev. C...

  • Page 7: Applicable Symbols

    For compliance with the Waste Electrical and Electronic Equipment Directive (WEEE) 2012/19/EU, contact Waters Corporation for the correct disposal and recycling instructions. May 31, 2017, 71500241402 Rev. C...

  • Page 8: Audience And Purpose

    Waters 2414 Reflective Index Detector. This guide sets forth procedures for unpacking, installing, using, maintaining, and troubleshooting the Waters 2414 Reflective Index Detector. It also includes appendices for safety warnings and specifications. Intended use of the Waters 2414 Refractive Index Detector The 2414 Refractive Index (RI) Detector is designed for high-performance liquid chromatography (HPLC) applications.

  • Page 9: Emc Considerations

    When analyzing samples from a complex matrix such as soil, tissue, serum/plasma, whole blood, and other sources, note that the matrix components can adversely affect LC/MS results, enhancing or suppressing ionization. To minimize these matrix effects, Waters recommends you adopt the following measures: •...

  • Page 10: Ec Authorized Representative

    EC authorized representative Waters Corporation Stamford Avenue Altrincham Road Wilmslow SK9 4AX UK Telephone: +44-161-946-2400 Fax: +44-161-946-2480 Contact: Quality manager May 31, 2017, 71500241402 Rev. C...

  • Page 11: Table Of Contents

    Safety advisories ....................vi Operating this instrument ..................vi Applicable symbols ................... vii Audience and purpose..................viii Intended use of the Waters 2414 Refractive Index Detector......viii Calibrating ....................... viii Quality-control ....................viii EMC considerations ....................ix ISM Classification: ISM Group 1 Class B ............ix EC authorized representative ..................
  • Page 12 Supported IEEE-488 and Ethernet configurations.......... 53 Ethernet signal cable connections ................ 54 Connecting to a Waters data control system via the Ethernet port ....54 IEEE-488 signal cable connections ............... 55 Connecting to a Waters data control system via the IEEE-488 bus interface....................
  • Page 13 Connecting to a Waters PowerLine system controller via the IEEE-488 bus interface......................57 Setting the IEEE-488 address................58 Making inject start signal cable connections ........... 58 Connecting to a manual injector ............... 60 Analog-out/event-in (I/O) connections ..............60 Connecting to a stand-alone Alliance Separations Module ......62 Connecting to the Waters 746 Data Module ............
  • Page 14 Navigating the user interface ................91 Operating in RIU mode ..................92 Using the display in RIU mode ................. 92 Navigating to and from the home screen in RIU mode ........95 Setting up a run in RIU mode................98 Programming timed events, threshold events, and methods ......
  • Page 15 Specific warnings ..................... 157 Notices ........................158 Bottles Prohibited symbol ................... 159 Required protection ..................... 159 Warnings that apply to all Waters instruments ..........160 Electrical and handling symbols ................. 165 Electrical symbols .................... 165 Handling symbols .................... 166 B Specifications .................... 167 2414 refractive index detector specifications .............
  • Page 16 May 31, 2017, 71500241402 Rev. C...

  • Page 17: Introduction

    Introduction Contents: Topic Page Use of refractive index detectors ............. 18 Operating principles ................ 18 Detector description ................. 27 May 31, 2017, 71500241402 Rev. C...

  • Page 18: Use Of Refractive Index Detectors

    1 Introduction Use of refractive index detectors The major advantage of refractive index detectors lies in the universal nature of their response. They are well-suited to analyze compounds that are without strong UV chromophores, fluorophores, or electrochemical or ionic activity. RI detectors are used to analyze carbohydrates and lipids and in polymer analyses by gel-permeation or size-exclusion chromatography.
  • Page 19 Wavelength The refractive index of a medium has a specific value that changes with the wavelength of the incident light beam. The 2414 refractive index detector uses monochromatic light at a fixed wavelength, so the effect of different wavelengths of light on RI is not discussed in this guide.
  • Page 20 1 Introduction Effect of density on RI: Weight percent sucrose in water Density (g/mL) Weight percent methanol in water Density (g/mL) May 31, 2017, 71500241402 Rev. C...
  • Page 21 Operating principles Measuring refraction The extent to which a beam of light is refracted when it enters a medium depends on these properties: • Angle at which the light enters the new medium (the angle of incidence) • Refractive indices of the old and new media The angle of a refracted light beam through the new medium is its angle of refraction.
  • Page 22 1 Introduction = Angle of refraction θ = RI of medium 1 = RI of medium 2 You can use Snell’s Law to calculate the RI of a sample solution from the angle of incidence, the RI of the solvent, and the angle of refraction. Using changes in RI for sample detection As the separated components of a sample pass through the refractometer flow cell:...

  • Page 23: Differential Refractometry

    Differential refractometry The 2414 refractive index detector can measure extremely small changes in refractive index to detect the presence of sample. The small difference in RI between a reference solution and a sample solution is referred to as Δ...
  • Page 24 1 Introduction External angle of deflection The amount of light falling upon the elements of the photodiode is determined by the external angle of deflection (φ), as shown in the figure, below. The φ determines the magnitude of the shift (Δ ) of the image cast on the photodiode by the light beam.
  • Page 25 The change in φ determines the shift (Δ ) of the light beam on the photodiode. Because the 2414 detector uses a dual-pass optics bench assembly, the light beam passes through the flow cell twice before reaching the photodiode, doubling the image shift.

  • Page 26: Common Ri Detection Problems

    The shift in the amount of the light beam striking each element of the dual-element photodiode results in a change in the output voltage from the 2414 detector. The integrator or chart recorder registers the changes in output voltage as peaks in your chromatogram.

  • Page 27: Detector Description

    The detector is designed for high-performance liquid chromatography applications. It can operate as a stand-alone unit with an integrator or chart recorder, or with a Waters system controller or Waters data system. Refer to Chapter “Specifications” for system specifications, and to Chapter “Preparing Solvents”...
  • Page 28 • Ethernet support – Allows the 2414 detector to operate as a component of an HPLC system controlled by a data control system, such as Empower 2, using Ethernet communications.

  • Page 29: Operation Modes

    Detector description Operation modes The 2414 detector operates as a single-channel detector, but can be configured to operate in one of two modes to acquire refractive index signal data: RIU mode and 410 emulation mode. Additionally, the detector can monitor temperature as an auxiliary channel.
  • Page 30 Auto-Zero on keypad/panel active 410 emulation mode When the 2414 detector is controlled by a data control system such as an Empower workstation, it automatically reconfigures to the 410 mode of operation enabling the detector’s backward compatibility features. In 410 mode, the detector monitors a single channel, in millivolts, and does not support stand-alone method programmability.

  • Page 31: Flow Path

    – Auto-Zero on keypad/panel active Flow path When the 2414 detector is acquiring data, its normal configuration for flow allows mobile phase to pass through the sample flow cell and then to waste or to the recycle valve. During analysis, the solvent sample takes the following path: Enters through the inlet tubing port.
  • Page 32 “purge out” port. A programmatically controlled solenoid valve determines the fluid path. When you purge the 2414 refractive index detector, solvent takes this path: Enters through inlet tubing port. Passes through the sample in tube of the countercurrent heat exchanger.
  • Page 33 Detector description Flows through the sample side of the flow cell. Flows out to the cross fitting, bypassing the countercurrent heat exchanger. Flows through the reference side of the flow cell. Exits through the pressure relief valve, to the purge outlet tubing port. Flow path during purge: Flow cell End Cap HE...

  • Page 34: Fluid Path Components

    The recycle valve ports and their corresponding outlet lines are labelled accordingly. A recycle external event input can be triggered to put the 2414 detector into recycle mode. The input puts the detector in recycle mode on each transition, according to how the event is configured.
  • Page 35 Detector description 2414 external plumbing and valves: Inlet line Solenoid purge valve Recycle valve Pressure relief valve TP01901 Countercurrent heat exchanger The low-dispersion, countercurrent heat exchanger minimizes temperature fluctuations in the sample stream. The device’s sample inlet and outlet lines are coaxial, which facilitates heat exchange between incoming and outgoing fluids.
  • Page 36 32 page 33 indicate the paths of solvent and sample in the 2414 refractive index detector during normal operation and during a purge, respectively. The following table provides the inner diameters of the sample and fluid lines. Fluid line diameters:...

  • Page 37: Optics

    Detector description during equilibration or at other times when the unit is not performing an analysis. Insulated sample inlet tubing To ensure good thermal isolation, use insulated tubing to connect the temperature-controlled column to the detector’s sample inlet. Optics The detector’s optics bench assembly consists of these components: •...

  • Page 38: Electronics

    The difference in the amount of light striking the elements of the photodiode (because of sample refraction) results in a deflection from the baseline on the chromatogram. Electronics The 2414 detector has both analog and digital components and includes a front-panel keyboard and these printed circuit (PC) boards and their interconnections: •...
  • Page 39 DC power supply – Provides voltage for the analog and digital circuitry. It is the DC power source for the detector. Filtering noise The 2414 detector uses a Hamming filter and RC filter to minimize noise: • Hamming filter – A digital finite impulse response filter, which creates the same amount of peak height attenuation as the RC filter, but enhances the filtering of high frequency noise.

  • Page 40: Temperature Control

    1 Introduction The default time constant of 1.0 second in Hamming mode is satisfactory for most applications. To calculate an appropriate time (filter) constant for special applications, use the formula: TC = 0.2 * PW where TC = Time constant (filter) setting PW = Peak width at half the height of the narrowest peak Polarity Detection peaks can be positive or negative.

  • Page 41: Startup Diagnostics Tests

    Startup diagnostics tests On startup, the 2414 detector runs a series of automated diagnostic tests. An error message appears if any of the tests fail. These startup diagnostic tests include: •...
  • Page 42 1 Introduction May 31, 2017, 71500241402 Rev. C...

  • Page 43: Installing The Detector

    Installing the Detector This chapter describes the procedures for selecting the site for installing the detector, unpacking and inspecting the instrument, installing fuses, and connecting plumbing components. For information on connecting the detector to other devices, see Chapter “Connecting Signal Cables”.

  • Page 44: Dimensions

    2 Installing the Detector Dimensions The following figure shows the dimensions of the 2414 refractive index detector. Dimensions of the 2414 detector: 50.3 cm (19.8 in) 21 cm (8.2 in) 28.4 cm (11.2 in) TP01497 To avoid electric shock, do not access the instrument inside Warning: the top cover.

  • Page 45: Site Selection Requirements

    Site selection and power requirements Site selection requirements Install the 2414 detector in an area that meets the requirements listed in the table below. Installation site requirements: Parameter Requirement Operating temperature 15 to 40 °C (59 to 104 °F); avoid direct...

  • Page 46: Unpacking And Inspection

    Report any damage or discrepancy when you inspect the contents of the carton immediately to the shipping agent. U.S. and Canadian customers must contact Waters Technical Service at 800 252-4752. Other customers, may phone their local Waters subsidiary or local Waters Technical Service representative.

  • Page 47: Connecting To The Electrical Power Supply

    Connecting to the electrical power supply Connecting to the electrical power supply To connect the 2414 refractive index detector to the AC power supply: Plug the receptacle end of the power cord into the AC power input receptacle on the rear panel of the detector (see the figure on page 46).

  • Page 48: Connecting A Column Or Second Detector

    2 Installing the Detector Tubing connections: Inlet line Solenoid purge valve Recycle valve Pressure relief valve TP01901 Connecting a column or second detector Use only the insulating sample inlet tubing assembly supplied in the startup kit to connect a column or second detector to the detector. This tubing assembly has been prepared with thermal insulation sleeving to moderate the effect of ambient air temperature variations.

  • Page 49: Connecting To Waste

    Connecting tubing and attachments To connect a column or other detector to the detector: Insert one end of the inlet tubing assembly into the inlet port of the index detector. ¼ Tighten the compression screw -turn past finger-tight. Repeat step 2, inserting the other end of the inlet tubing assembly into the outlet fitting of the column or another detector.

  • Page 50: Connecting The Valve Pack Drip Tray

    2 Installing the Detector Connect the tubing to the white plastic fitting located under the three valves on the front of the detector (see the figure on page 48). Insert the other end of the tubing into the waste container. Connecting the valve pack drip tray A factory-installed drip tray lies beneath the three valves of the valve pack.

  • Page 51: Connecting Signal Cables

    Connecting Signal Cables This chapter describes procedures for making signal connections between the detector and other HPLC system components. Contents: Topic Page Component connection overview ............. 52 Ethernet signal cable connections........... 54 IEEE-488 signal cable connections ..........55 Analog-out/event-in (I/O) connections..........60 Connecting to an external column heater........

  • Page 52: Component Connection Overview

    Empower 2, connected via the Ethernet network. The Ethernet port also supports the Tip: Waters PC-based Autoloader utility for installing firmware (see the Waters 2414 Refractive Index Detector release notes for details). IEEE-488 Any of the following systems: • Waters data control system, such as...

  • Page 53: Supported Ieee-488 And Ethernet Configurations

    The remainder of this chapter describes the types of available signal connections for the detector. Supported IEEE-488 and Ethernet configurations You can operate a 2414 detector controlled by a data control system in one of these configurations: • Where all system modules, including the detector, communicate with the data system via an IEEE-488 bus interface •...

  • Page 54: Ethernet Signal Cable Connections

    3 Connecting Signal Cables Ethernet signal cable connections You can use its Ethernet port to connect the detector to a Waters data control system, such as Empower 2 software, that supports Ethernet communications. HPLC system under Empower 2 software control via Ethernet:...

  • Page 55: Ieee-488 Signal Cable Connections

    Ethernet port for communications. Connecting to a Waters data control system via the IEEE-488 bus interface You can use the IEEE-488 bus to connect the detector to a Waters data system in any of the following configurations: •...
  • Page 56 2414 RI detector Module When connected to a Waters data system, the 2414 detector is automatically configured to operate in 410 (remote) mode. You use the data control software to create instrument methods and method sets to control the detector and other HPLC system components.

  • Page 57: Connecting To A Waters Powerline System Controller Via The Ieee-488 Bus Interface

    HPLC system components, including the 2414 detector. To connect the detector to a Waters PowerLine system controller, use the IEEE-488 interface cables as shown in the figure below. Each fluid-handling unit is configured with either of the following injectors: •...

  • Page 58: Setting The Ieee-488 Address

    To exit the configuration functions, press Home. Making inject start signal cable connections An IEEE-488 data system used with the 2414 detector requires that the data system or controller receive an inject start signal from the autosampler or manual injector to initiate data collection and time-based programs.
  • Page 59 If multiple devices in your system require an inject start signal, Requirement: connect trigger wires from the same (inject out) terminal on the injector to each device. 2414 RI detector inject start connections: Inject start input connection Inject start output source (on detector connector A)

  • Page 60: Connecting To A Manual Injector

    To connect the detector to instruments not using a digital communications interface (that is, neither Ethernet nor IEEE-488), you use the analog-out/event-in (I/O) connectors on the rear panel. This section describes signal connections between the 2414 detector’s analog-out/event-in connectors and the following components: •...
  • Page 61 Analog-out/event-in (I/O) connections The following figure and table describe the two I/O connectors (and their corresponding pin-outs) on the detector’s rear panel. Rear panel analog-out/event-in connectors: B (inputs and outputs) A (inputs and outputs) 1 + Auto Zero 1 + Inject Start 2 - Auto Zero 2 - Inject Start 3 GROUND...

  • Page 62: Connecting To A Stand-Alone Alliance Separations Module

    When you use the Alliance Separations Module as a stand-alone controller (that is, not on an Ethernet or IEEE-488 bus interface or under data system control), you can make the following signal connections using the 2414 detector’s analog-out/event-in connectors: •...
  • Page 63 Analog-out/event-in (I/O) connections Generating auto zero on injecting To generate the auto zero function on the 2414 detector at the start of an injection from the Alliance Separations Module, make the connections shown in the table and figure below. Detector connections to an Alliance Separations Module:...
  • Page 64 To generate the chart mark function on the detector at the start of an injection from the separations module, make the connections shown in the table and figure below. 2414 detector connections to a separations module: Separations module Detector (connector A)
  • Page 65 Generating chart mark and auto zero signals To generate both a chart mark and an auto zero signal from the separations module to the 2414 detector, make the connections shown in the table and figure below. Detector connections to a separations module:...

  • Page 66: Connecting To The Waters 746 Data Module

    Connecting to the Waters 746 Data Module To send an integrator, analog, output signal (–2V to +2V) from the detector to the Waters 746 Data Module, make the connections shown in the table and figure below. Analog output connections to a 746 data module:...

  • Page 67: Connecting To A Chart Recorder

    Analog-out/event-in (I/O) connections Connecting to a chart recorder To send an analog output signal from the 2414 detector to a chart recorder, make the connections shown in the table and figure below. Analog output connections to a chart recorder: Chart recorder...

  • Page 68: Connecting To A Data Control System Using Analog Signals

    3 Connecting Signal Cables Connecting to a data control system using analog signals To send an integrator analog output signal (–2 V to +2 V) from the 2414 detector to an Empower, Millennium , or MassLynx data control system (through a two-channel SAT/IN Module), make the connections shown in the table and figure, below.

  • Page 69: Connecting Injection Trigger Signals

    12 + Auxiliary Out 13 - Auxiliary Out Injector Connecting injection trigger signals The 2414 detector accepts the following injection trigger signals from a manual injector: • Auto-zero signal to automatically adjust the zero offset of the detector each time the injector makes an injection •...
  • Page 70 3 Connecting Signal Cables Each time the detector receives a signal from a manual injector, it performs the corresponding auto zero, inject start, or chart mark function. To send an auto zero or chart mark signal from a manual injector to the detector, make the connections shown in the tables and figures, below.
  • Page 71 Analog-out/event-in (I/O) connections Chart mark connections to a manual injector: Detector (connector A) Manual injector connector Pin 9, Chart Mark + (red) Two spade-lug terminal connectors (both cables can be functionally Pin 10, Chart Mark – (black) identical) or similar connectors. Chart mark connections to a manual injector: Manual Detector...

  • Page 72: Polarity Connections

    13 - Switch Polarity connections The Polarity and Polarity Enable contact closures on the rear panel of the 2414 detector determine the peak polarity of the output signal according to the following conditions (negative polarity results in negative, or inverted, peaks): •...

  • Page 73: Connecting To An External Column Heater

    Closed Unchanged Connecting to an external column heater The 2414 detector can control one optional, external, column heater through the EXT 1 port (external column heater port) on its rear panel. The port is a standard 9-pin DIN connector. External column heater port:...
  • Page 74 3 Connecting Signal Cables May 31, 2017, 71500241402 Rev. C...

  • Page 75: Preparing Solvents

    Preparing Solvents Proper solvent selection and preparation are critical in differential refractometry to prevent baseline changes such as drift, noise, or an erratic baseline. To avoid chemical hazards, always observe Good Warning: Laboratory Practices when handling solvents. Refer to the Material Safety Data Sheets shipped with solvents for handling information.

  • Page 76: Common Solvent Problems

    4 Preparing Solvents Common solvent problems The 2414 detector measures changes in the refractive index (RI) of the solution flowing through the sample side of the flow cell. However, factors other than the presence of dissolved sample molecules can affect a solution’s RI.

  • Page 77: Preparation Checklist

    Selecting a solvent Preparation checklist The following solvent preparation guidelines help to ensure stable baselines and good resolution: • Filter solvents with a 0.22-µm filter. • Degas the solvent. • Stir the solvent. • Protect solvents from drafts and shock. Water Use water only from a high-quality water purification system.
  • Page 78 4 Preparing Solvents intend to use for your analysis has an RI significantly different from the sample components. Refractive indices of common solvents: Solvent Solvent Fluoroalkanes 1.25 Tetrahydrofuran (THF) 1.408 Hexafluoroisopropanol 1.2752 Amyl alcohol 1.410 (HFIP) Methanol 1.329 Diisobutylene 1.411 Water 1.33 -Decane...

  • Page 79: Solvent Degassing

    Solvent degassing Refractive indices of common solvents: (Continued) Solvent Solvent Isooctane 1.404 Aniline 1.586 Cyclopentane 1.406 Carbon disulfide 1.626 Solvent degassing Using degassed solvents is the most important step in solvent preparation. Degassing provides: • Stable baselines and enhanced sensitivity •...

  • Page 80: Solvent Degassing Methods

    4 Preparing Solvents is endothermic, the solubility increases when you heat the solvent. For example, the solubility of He in H O decreases with an increase in temperature, but the solubility of He in benzene increases with an increase in temperature.

  • Page 81: Solvent Degassing Considerations

    To increase the length of membrane, you can connect two or more vacuum chambers in series. When you are using the Alliance separations module with the 2414 detector, set the in-line degasser to “on” degas mode.
  • Page 82 4 Preparing Solvents May 31, 2017, 71500241402 Rev. C...

  • Page 83: Operating The Detector

    Operating the Detector Contents: Topic Page Powering-on..................84 Operating in RIU mode ..............92 Operating in 410 (stand-alone) mode..........107 Operating in 410 (remote) mode............112 Configuring the detector..............113 Optimizing performance ..............117 Powering-off..................121 May 31, 2017, 71500241402 Rev. C...

  • Page 84: Powering-On

    Initial home screen (410 mode): The 2414 detector automatically switches to 410 mode, from RIU mode, Note: when connected to a Waters data control system via the IEEE-488 or Ethernet connector. When initialization is completed, you can change the default settings to suit your needs.

  • Page 85: Diagnostics Failure At Startup

    If one or more of the internal startup diagnostics checks fails, the detector beeps and displays an error message. Using Help The 2414 detector provides limited context-sensitive help. When you press “?” (Shift HOME) from a point in the program associated with an online Help screen, the Help screen appears.
  • Page 86 5 Operating the Detector ° • Navigation to specific screens (HOME, TEMP C, DIAGnostics, TRACE, CONFIGURE, and METHOD) • Primary function keys (Chart Mark, Auto Zero, Run/Stop, Reset Clock, Purge, Lock, Recycle, Polarity, System Information, Previous, Cancel +/–, and Clear Field) •...
  • Page 87 Powering-on For numerical entries from 1 to 9 on choice lists or menus, enter the number corresponding to the desired item, and then press Enter. For the number 10, select 0, and then press Enter. To go to the end of a choice list, select “•”. For entries numbered 11 or 12, scroll to the desired item on the choice list, and then press Enter.
  • Page 88 5 Operating the Detector Keypad description: (Continued) Description Unshifted Shifted s, t – On screens with entry fields (edit, check box, or choice list), the active field has a thickened border. Use the arrow keys to make a different field active. (s moves up or left; t moves down or right.) On screens with a scrollable list, these keys move the highlight up (toward the beginning of the list) or down (toward the end).
  • Page 89 Powering-on Keypad description: (Continued) Description Unshifted Shifted TRACE – Displays the RIU Scale – When the RIU trace Scale monitor trace. screen is visible, this TRACE function permits modification of the display range in the X (time) and Y (RIU) dimensions. Shift –...
  • Page 90 5 Operating the Detector Keypad description: (Continued) Description Unshifted Shifted 5 – See 0–9 above. Lock – When you are on the Lock home screen, enables or disables the keypad lock feature. Use the lock function to prevent inadvertent changes to detector settings.

  • Page 91: Navigating The User Interface

    Navigating the user interface When operating the 2414 detector use these steps to navigate through its screens and menus: Press the Enter key (or the s and t keys) to navigate among editable fields on a display.

  • Page 92: Operating In Riu Mode

    5 Operating the Detector • Press the corresponding number key to select an item immediately. • Use the s and t keys to scroll through the list, and then press Enter. The s and t keys do not increment or decrement numerical Note: field entries.
  • Page 93 Operating in RIU mode Refractive index, function, and message icons The HOME, TEMP °C, and CONFIGURE screens in the detector program display the icons or fields shown in the figure above. Mode, function, and message screen icons: Icon or field Icon/field name Function Home1(status),...
  • Page 94 5 Operating the Detector Mode, function, and message screen icons: (Continued) Icon or field Icon/field name Function Local (Method #) / Local/Method number – If Remote Control the detector is not controlled by a data system or other control device over the IEEE-488 bus, it displays a cursive “m”...

  • Page 95: Navigating To And From The Home Screen In Riu Mode

    Operating in RIU mode Navigating to and from the home screen in RIU mode Pressing HOME brings you to the home screen, from most screens. From the home screen, you can access several secondary functions. To move to the secondary function screens of the home screen, press Next. These are the secondary functions in RIU mode: •...
  • Page 96 5 Operating the Detector Secondary functions of the RIU mode home screen: Home 1 Home 2 Home 3 Home 4 Press Next From the home screen, you can access the following functions, either from the home screen or by pressing the Next key: •...
  • Page 97 Operating in RIU mode The RIU-FS range is 500 to 1 µRIU (default is 500). Changing the Refractive Index Units Full Scale Warning: (RIU-FS) setting affects the 2-V Detector output. The RIU Full Scale setting is a parameter used to generate an analog output voltage (detector output) with the appropriate scaling factor.

  • Page 98: Setting Up A Run In Riu Mode

    5 Operating the Detector 2000-mV range). This is useful for making minor adjustments, and for nulling any offset between the 2414 refractive index detector and a connected external data system. µRIU offset – Provides an offset for adjusting the detector output. The µRIU and the range is ±500.0 µRIU.

  • Page 99: Programming Timed Events, Threshold Events, And Methods

    Operating in RIU mode • Attenuation (RIU-FS) • Filter type • Time constant • Detector oven temperature • Column heater module temperature (if available or present) Depending on other functions you can choose to perform during a run, there are several other parameters you must program. The table on page 93 contains the function descriptions, fields, screen number, type of function, display units, allowable ranges, and the default settings for the home screen...
  • Page 100 If you enter a time that is not in sequence with the events entered previously, the timed event list is sorted automatically when you press Next. The 2414 detector allows programming of the timed events shown in the following table.
  • Page 101 Operating in RIU mode Method choice list screen: From the Method choice list, press 1, Timed events. An active field for entering the time of the event is displayed. Result: Enter the time for the event. When you begin entering the time, additional fields appear.
  • Page 102 5 Operating the Detector If the 2414 detector is configured with the Waters 717plus Autosampler or another external device, the inject start programmed from that device starts the method. If you are working in real time, under current conditions (method *), at...
  • Page 103 Operating in RIU mode threshold value required in mRIU, an additional field is displayed (Switch). Threshold events screen: The “threshold” selection in the table on page 100 allows you to Tip: modify this initial Threshold value as a timed event. Press Enter to advance to the next (Switch) field, or press the s or t key to move among the five fields on the threshold events screen.
  • Page 104 5 Operating the Detector Method choice list: Enter a number from 1 to 10 and press Enter. A brief message (“Storing * as method ”) appears. When the Result: display returns to the Method choice list, the method is stored. Retrieving a method To retrieve a previously stored method: Return to the Method choice list by pressing METHOD (Shift Temp ×C).
  • Page 105 Operating in RIU mode Resetting a method Resetting a stored method is a two-step process. First, you reset the current conditions to the defaults; then you save the defaults in one of the storage locations. To clear one or more methods: Before you clear the method, to prevent loss of the current conditions, Note: store them in one of the available storage slots.
  • Page 106 5 Operating the Detector • If you press Enter, the following conditions occur: – All timed events are deleted. – All threshold events are disabled. – All other operating parameters of the method (RIU-FS, Filter, Time Constant, etc.) are set to defaults. •...

  • Page 107: Operating In 410 (Stand-Alone) Mode

    Operating in 410 (stand-alone) mode Unlike RIU mode, you cannot program or use methods stored in the 2414 detector in 410 mode. The 410 (stand-alone) mode emulates the Waters 410/2410 by displaying the % Full Scale value used by the Waters 410 and 2410 Detectors and driving the Detector Out signal on the 2414 detector output.
  • Page 108 5 Operating the Detector Home screen 410 mode: % Full scale Polarity Shift Keypad lock / unlock Sensitivity Mode Detector Next screen temperature You can recall the home screen from any page by pressing the HOME key. At the first use of the detector, the home screen shows the factory-set defaults. After the first use, the home screen shows the settings displayed before the detector was last powered-off.

  • Page 109: Navigating To And From The Home Screen In 410 Mode

    Operating in 410 (stand-alone) mode Mode, function, and message screen icons: (Continued) Icon or field Icon/field name Function Keypad Unlock / Lock Open lock = Unrestricted keypad entry Closed lock = Parameter changes not allowed Sticky Diagnostics When the Home screen displays the wrench icon, a sticky diagnostic is active.
  • Page 110 5 Operating the Detector • Voltage offset • Enable/disable keypad entries Secondary functions of the 410 mode home screen: Home 1 Press Next Home 2 Press Next Home 3 Press Next Home 4 Press Next May 31, 2017, 71500241402 Rev. C...
  • Page 111 Sensitivity settings are 1, 2, 4, 8, 16, 32, 64, 128, 256, 512, and 1024 (default is 4). Sensitivity is a parameter used to generate the Waters 410-compatible Integrator Output signal. The user interface provides a means for setting Sensitivity as well as displaying it.

  • Page 112: Setting Up A Run In 410 Mode

    Operating in 410 (remote) mode The 2414 detector operates in 410 (remote) mode when it is under active control by a Waters data control system or system controller, such is the case when it is connected to any of these systems: •...

  • Page 113: Configuring The Detector

    With a data control system, you use the data control software to create instrument methods and method sets to control the 2414 detector and other HPLC system components. See the data control software documentation for more information on configuring the 2414 detector and operating in 410 (remote) mode.
  • Page 114 5 Operating the Detector Setting the IEEE address IEEE address – Enter the detector’s IEEE-488 bus address, from 2 through 29. If you press the CE key, the detector is removed from IEEE control. The default IEEE address is 14. Setting detector mode When connected to the data control software, the detector defaults to Note:...
  • Page 115 Configuring the detector Use the Enter key and the numeric keypad or the s and t keys to select the appropriate entry. • Auto zero – Configure the Auto Zero input to auto zero the refractive index output. You determine the response of the channel using the Enable Auto Zero function explained in the table on page 100 and shown...
  • Page 116 5 Operating the Detector • Rectangular wave (in seconds) – If the switch is programmed to initiate a rectangular wave as a timed or threshold event, then the period of the signal (the width of one pulse period in a rectangular wave or pulse train) is as specified in this field (range is 0.2 to 60 seconds).

  • Page 117: Optimizing Performance

    Optimizing performance Displaying system info The System Info key (Shift 4) displays information about the detector, including the serial number, the software version number, and the IEEE address, if applicable. Optimizing performance You can adjust the noise level, peak height, peak direction, and the temperatures of the internal oven and column heaters to optimize the performance of the detector.
  • Page 118 Temperature These screens control the internal detector oven and, if configured, Waters column heater module. These screens are the same for RIU and 410 modes. Temperature screen 1: May 31, 2017, 71500241402 Rev. C...
  • Page 119 The temperature of the column heater connected to the column heater module port on the rear panel can be set in the range ambient 5 to 150 °C. The 2414 detector, which has access to the column heater module temperature sensor, will then try to achieve and maintain the setpoint temperature, sending control signals to the external hardware.

  • Page 120: Operating The Trace And Scale Functions

    This is used to null any offsets between the 2414 detector and a connected chart recorder or data system. The offset is added after any polarity has been applied to the output (default is 0 mV).

  • Page 121: Powering-Off

    Removing buffered mobile phase To remove mobile phase from the fluid path of the 2414 detector: Replace the buffered mobile phase with 100% HPLC-quality water and flush the system for 10 minutes at 2 mL/min.
  • Page 122 5 Operating the Detector Replace the 100% water mobile phase with a solution of 90% methanol:10% water, and flush the system for 10 minutes at 2 mL/min. If your storage solvent is incompatible with your column, Notice: remove the column before flushing. Follow the recommended procedures for injector purging and priming for the pump in use with your HPLC.

  • Page 123: Maintenance Procedures

    Maintenance Procedures Contents: Topic Page Decontaminating the fluid path ............124 Replacing fuses................. 126 May 31, 2017, 71500241402 Rev. C...

  • Page 124: Decontaminating The Fluid Path

    6 Maintenance Procedures Detector maintenance involves cleaning the fluid path and replacing fuses. To avoid electrical shock, Warning: • do not open the detector’s cover. The detector’s components are not user-serviceable. • do not disconnect an electrical assembly while the detector is powered-on.
  • Page 125 Decontaminating the fluid path • A separate waste container for acid waste • If you use an acid as a cleaning solvent, a means of measuring the pH of the acid effluent If you use 6N nitric acid and operate the detector at high Notice: sensitivities, flush the system extensively with water to remove all traces of the acid.

  • Page 126: Replacing Fuses

    6 Maintenance Procedures 10. Take the detector out of purge mode and stop the pump or solvent delivery system. 11. Reattach the column and reequilibrate the detector. Replacing fuses Required item • Flat-blade screwdriver • Replacement fuse: F 3.15 A, 250 V Identifying a faulty fuse Suspect a faulty fuse if you encounter any of these problems: •...
  • Page 127 Replacing fuses Removing and replacing the fuse: Fuse receptacle Power input Fuse holder Remove and discard the old fuse. Make sure that the new fuse is properly rated for your requirement To avoid fire, replace the fuse only with another of the same Warning: type and rating.
  • Page 128 6 Maintenance Procedures May 31, 2017, 71500241402 Rev. C...

  • Page 129: Error Messages, Diagnostic Functions, And Troubleshooting

    Error Messages, Diagnostic Functions, and Troubleshooting Consult this chapter when diagnosing problems with your 2414 detector. Because the detector measures bulk properties of the system the source of an apparent detector problem can lie with the chromatography itself or the other instruments in your system.

  • Page 130: Error Messages

    7 Error Messages, Diagnostic Functions, and Troubleshooting Error messages The detector can display two types of error messages: • Messages requiring you to recycle power, and then contact Waters Technical Service if the error persists (see “Accessing the diagnostic functions” on page 134).

  • Page 131: Operational Error Messages

    Purge valve not present Recycle power to the Detected or detected detector, and examine the purge valve. If the error persists, contact Waters Technical Service. No source LED LED is defective Recycle power to the detected detector. If the error persists, contact Waters Technical Service.
  • Page 132 7 Error Messages, Diagnostic Functions, and Troubleshooting bubbles before you recycle power. If the error persists, contact Waters Technical Service. Error messages preventing operation: Error message Description Corrective action System cannot respond Fatal error Recycle power to the detector. If the error persists, contact Waters Technical Service.
  • Page 133 Verify external room point has not been temperature to come to temperature is not a reached temperature factor. If the error persists, contact Waters Technical Service. Column temperature Allow external column Verify external room set point has not been heater temperature to...

  • Page 134: Performing Diagnostic Functions

    Performing diagnostic functions The detector runs both user-selectable and service diagnostic tests. You access the user diagnostic tests by pressing the DIAG key. Only qualified Waters service personnel can access service diagnostics. To exit any diagnostic when completed, press DIAG to return to the diagnostics choice list or HOME to return to the Home screen.
  • Page 135 Performing diagnostic functions To access user-selectable diagnostic functions: Press the DIAG key on the detector’s front panel. The detector displays the Diagnostics choice list. Result: Diagnostics choice list: To access a specific diagnostic test, select the test you want to run, and press Enter, or press a number, from 1 to 6, that corresponds to the diagnostic number on the detector’s keypad.
  • Page 136 1. Autozero offset 2. Oven/column heater 3. Simulate Peak 4. Valve 5. Previous choices Service Diagnostics Diagnostics used by Waters service personnel May 31, 2017, 71500241402 Rev. C...

  • Page 137: Using The Optimize Led Diagnostic Function

    Performing diagnostic functions Using the Optimize LED diagnostic function To use the Optimize LED diagnostic function, press DIAG 2. This diagnostic function automatically sets the energy level of the internal LED. An error message appears if the energy level is too high or too low. This message commonly appears when the detector was purged recently or is about to begin a new analysis, or when a mobile phase composition change affects the flow cell.
  • Page 138 7 Error Messages, Diagnostic Functions, and Troubleshooting Monitoring contact closures and setting switches To monitor the contact closures and control switch output: On the Input & output choice list, press 2, Switch & events, to monitor the eight contact closure inputs and control the single switch output. The Input &...

  • Page 139: Display And Keypad Diagnostic Tests

    When the keypad is operating properly, each key location is Result: filled in and then cleared with another press of the key. If any key does not respond when pressed, contact your Waters service representative. Press Enter twice to exit the keypad diagnostic. Requirement:...

  • Page 140: Using The Other Diagnostic Functions

    7 Error Messages, Diagnostic Functions, and Troubleshooting Using the Other diagnostic functions The Other diagnostics menu provides four additional diagnostic functions: • Auto zero offsets – Use this diagnostic function to display the auto zero offset. • Oven/Column Heater – Use this diagnostic function to display the internal oven and, if any, the column heater status.
  • Page 141 Performing diagnostic functions To specify the exact peaks: Enter a peak height, in µRIU, from 1 to 999. In 410 mode, the peak height is converted from RIU to the Note: corresponding value, depending on the sensitivity setting. Enter a peak width in seconds. The width must be greater than 0 or less than or equal to Requirement: the period of peak repetition.

  • Page 142: Troubleshooting

    2414 detector. Most detector problems are relatively easy to correct. If you are unable to correct a problem or a failed condition, contact Waters Technical Service. When you contact Waters To expedite your request for service, have the following information available when you call Waters Technical Service: •...

  • Page 143: Hardware Troubleshooting

    IEEE address set incorrectly Bad IEEE-488 cable Check the IEEE-488 cable. Replace the IEEE-488 cable. Keypad not Keypad defective Recycle power to the 2414 functioning detector and run the keypad diagnostic. Contact Waters Technical Service. Analog output RIU-FS setting...

  • Page 144: Chromatography Troubleshooting

    “Troubleshooting” on page 142. If you need further help, contact Waters Technical Service. Abnormal baseline Drift, noise, and cycling are common symptoms of an abnormal baseline. Baseline drift – Can be flow-related or result from changing ambient conditions, especially temperature.
  • Page 145 Troubleshooting Use the following table to troubleshoot baseline problems. Abnormal baseline troubleshooting: Symptom Possible cause Corrective action Baseline drift, rapid Column not Equilibrate column. equilibrated Detector not allowed to Allow detector to warm warm up up until baseline is stable. Warmup time varies based on sensitivity.
  • Page 146 Dirty flow cell Clean flow cell (see “Decontaminating the fluid path” on page 124). Baseline drift, Leaky flow cell Call Waters Technical descending Service. Flow cell can possibly Properly purge the contain an air bubble system. May 31, 2017, 71500241402 Rev. C...
  • Page 147 Troubleshooting Abnormal baseline troubleshooting: (Continued) Symptom Possible cause Corrective action Short-term noise Pump pulsing Add pulse dampener cycling and shut off flow to (30 sec to 60 sec) confirm if this is the cause. Inadequate solvent Connect high-flow blending in pump pulse dampener.
  • Page 148 7 Error Messages, Diagnostic Functions, and Troubleshooting Abnormal baseline troubleshooting: (Continued) Symptom Possible cause Corrective action Long-term noise cycling Ambient temperature Stabilize ambient (approximately 1 hour) fluctuations temperature. Integrator or recorder Examine integrator or faulty recorder for excessive baseline noise. Faulty check valve Clean/replace/rebuild pump check valves.
  • Page 149 Symptom Possible cause Corrective action Baseline noise, random Analog output cable not Properly connect cable. (Continued) properly connected between 2414 and data system or recorder System improperly Plug into different grounded outlet on different electrical circuit. Use power conditioner. Recorder voltage...
  • Page 150 7 Error Messages, Diagnostic Functions, and Troubleshooting Use the following table to troubleshoot problems with retention times. Troubleshooting problems with retention times: Symptom Possible cause Corrective action Erratic retention Air bubble in pump head Degas all solvents, times prime pump (see “Solvent degassing methods”...

  • Page 151: Poor Peak Resolution

    Troubleshooting Troubleshooting problems with retention times: (Continued) Symptom Possible cause Corrective action Reduced retention Incorrect flow rate Verify flow rate. times Incorrect solvent Change composition. composition High column temperature Reduce column temperature. Incorrect column See column manual. pretreatment Column contaminated Clean/replace column.
  • Page 152 Resolution troubleshooting: Symptom Possible cause Corrective action Straight baseline, no No pump flow Set pump flow rate. peaks LED not on Call Waters Technical Service. Detector not zeroed Auto zero detector baseline. Improper connection between detector and Inspect cabling between recorder unit and recorder.

  • Page 153: Incorrect Qualitative/Quantitative Results

    Troubleshooting Resolution troubleshooting: (Continued) Symptom Possible cause Corrective action Flat-topped peaks Detector not zeroed Auto zero detector baseline. Incorrect recorder Adjust recorder input input voltage voltage, or adjust detector output cable to correct position. Sensitivity too high Select a lower sensitivity.
  • Page 154 7 Error Messages, Diagnostic Functions, and Troubleshooting Incorrect results troubleshooting: (Continued) Symptom Possible cause Corrective action Change in mobile phase Correct mobile phase composition pH or ionic composition. Incorrect flow rate Change flow rate. Dirty flow cell Clean the fluid path (see “Decontaminating Electronic noise...

  • Page 155: A Safety Advisories

    Safety Advisories Waters instruments display hazard symbols designed to alert you to the hidden dangers of operating and maintaining the instruments. Their corresponding user guides also include the hazard symbols, with accompanying text statements describing the hazards and telling you how to avoid them.

  • Page 156: Warning Symbols

    Heed all warnings when you install, repair, and operate Waters instruments. Waters assumes no liability for the failure of those who install, repair, or operate its instruments to comply with any safety precaution.

  • Page 157: Specific Warnings

    The following warnings can appear in the user manuals of particular instruments and on labels affixed to them or their component parts. Burst warning This warning applies to Waters instruments fitted with nonmetallic tubing. Pressurized nonmetallic, or polymer, tubing can burst. Warning: Observe these precautions when working around such tubing: •...

  • Page 158: Notices

    A Safety Advisories Biohazard warning This warning applies to Waters instruments that can be used to process material that can contain biohazards: substances that contain biological agents capable of producing harmful effects in humans. Waters instruments and software can be used to analyze or...

  • Page 159: Bottles Prohibited Symbol

    Bottles Prohibited symbol Bottles Prohibited symbol The Bottles Prohibited symbol alerts you to the risk of equipment damage caused by solvent spills. To avoid equipment damage caused by spilled solvent, do Prohibited: not place reservoir bottles directly atop an instrument or device or on its front ledge.

  • Page 160: Warnings That Apply To All Waters Instruments

    A Safety Advisories Warnings that apply to all Waters instruments When operating this device, follow standard quality-control procedures and the equipment guidelines in this section. Changes or modifications to this unit not expressly approved by the Attention: party responsible for compliance could void the user’s authority to operate the equipment.
  • Page 161 Warnings that apply to all Waters instruments Use caution when working with any polymer tubing under pressure: Warning: • Always wear eye protection when near pressurized polymer tubing. • Extinguish all nearby flames. • Do not use tubing that has been severely stressed or kinked.
  • Page 162 A Safety Advisories fare attenzione quando si utilizzano tubi in materiale polimerico Attenzione: sotto pressione: • Indossare sempre occhiali da lavoro protettivi nei pressi di tubi di polimero pressurizzati. • Spegnere tutte le fiamme vive nell'ambiente circostante. • Non utilizzare tubi eccessivamente logorati o piegati. •...
  • Page 163 Warnings that apply to all Waters instruments 警告：当有压力的情况下使用管线时，小心注意以下几点： • 当接近有压力的聚合物管线时一定要戴防护眼镜。 • 熄灭附近所有的火焰。 • 不要使用已经被压瘪或严重弯曲的管线。 • 不要在非金属管线中使用四氢呋喃或浓硝酸或浓硫酸。 • 要了解使用二氯甲烷及二甲基亚枫会导致非金属管线膨胀，大大降低管线的耐压能力。 경고: 가압 폴리머 튜브로 작업할 경우에는 주의하십시오. • 가압 폴리머 튜브 근처에서는 항상 보호 안경을 착용하십시오. • 근처의 화기를 모두 끄십시오. • 심하게 변형되거나 꼬인 튜브는 사용하지 마십시오.
  • Page 164 A Safety Advisories The user shall be made aware that if the equipment is used in a Warning: manner not specified by the manufacturer, the protection provided by the equipment may be impaired. L’utilisateur doit être informé que si le matériel est utilisé d’une Attention: façon non spécifiée par le fabricant, la protection assurée par le matériel risque d’être défectueuses.

  • Page 165: Electrical And Handling Symbols

    Electrical and handling symbols Electrical and handling symbols Electrical symbols These can appear in instrument user manuals and on the instrument’s front or rear panels. Symbol Description Electrical power on Electrical power off Standby Direct current Alternating current Alternating current (3 phase) Safety ground Frame, or chassis, terminal Fuse...

  • Page 166: Handling Symbols

    A Safety Advisories Handling symbols These handling symbols and their associated text can appear on labels affixed to the outer packaging of Waters instrument and component shipments. Keep upright! Keep dry! Fragile! Use no hooks! May 31, 2017, 71500241402 Rev. C...

  • Page 167: B Specifications

    2414 refractive index detector specifications Specifications 2414 refractive index detector specifications Refer to the following tables for 2414 detector specifications. Operational specifications: Condition Specification RI Range 1.00 to 1.75 RIU Measurement –4 5 × 10 Range –9 7 × 10 Flow Rate 0.1 to 10 mL/min...
  • Page 168 B Specifications Operational specifications: (Continued) Condition Specification Analog Outputs –2.0 to +2.0 V Temperature Internal oven: 30 to 55 °C (86 to 131 °F) Control One external column heater: Ambient to 150 °C (302 °F), steel a. Measurement taken after a minimum 2-hour warmup time or longer for equilibration, depending on column heater.
  • Page 169 2414 refractive index detector specifications Electrical specifications: Conditions Specifications Line Frequency 50 Hz, 47 to 53 Hz 60 Hz, 57 to 63 Hz Fuse Rating Fast 3.15 A, 250 VAC Power 145 VA (Nominal) Consumption Power source specification: Nominal Voltage 100 to 240 V, 50/60 Hz May 31, 2017, 71500241402 Rev.
  • Page 170 B Specifications May 31, 2017, 71500241402 Rev. C...

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