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Waters 600e User Manual

Multisolvent delivery system
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Waters 600E
Multisolvent Delivery System
User's Guide
View More Waters Manuals at
www.Chromatography.co
34 Maple Street
Milford, MA 01757
WAT174-02TP, Revision 3

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Summary of Contents for Waters 600e

  • Page 1 Waters 600E Multisolvent Delivery System User’s Guide View More Waters Manuals at www.Chromatography.co 34 Maple Street Milford, MA 01757 WAT174-02TP, Revision 3...
  • Page 2 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, the use of this document.
  • Page 3 Note: When you use the instrument, follow generally accepted procedures for quality control and methods development. If you observe a change in the retention of a particular compound, in the resolution between two compounds, or in peak shape, immediately determine the reason for the changes.
  • Page 4 Caution: Use caution when working with any polymer tubing under pressure: • Always wear eye protection when near pressurized polymer tubing. • Extinguish all nearby flames. • Do not use tubing that has been severely stressed or kinked. • Do not use nonmetallic tubing with tetrahydrofuran (THF) or concentrated nitric or sulfuric acids.
  • Page 5 Attenzione: prestare attenzione durante l’utilizzo dei tubi di polimero pressurizzati: • Indossare sempre occhiali da lavoro protettivi nei pressi di tubi di polimero pressurizzati. • Estinguere ogni fonte di ignizione circostante. • Non utilizzare tubi soggetti che hanno subito sollecitazioni eccessive o son stati incurvati.
  • Page 7 Caution: The user shall be made aware that if the equipment is used in a manner not specified by the manufacturer, the protection provided by the equipment may be impaired. Attention : L’utilisateur doit être informé que si le matériel est utilisé d’une façon non spécifiée par le fabricant, la protection assurée par le matériel risque d’être défectueuses.
  • Page 8 Caution: To protect against fire hazard, replace fuses with those of the same type and rating. Attention : Remplacez toujours les fusibles par d’autres du même type et de la même puissance afin d’éviter tout risque d’incendie. Vorsicht: Zum Schutz gegen Feuergefahr die Sicherungen nur mit Sicherungen des gleichen Typs und Nennwertes ersetzen.
  • Page 9 Caution: To avoid possible electrical shock, disconnect the power cord before servicing the instrument. Attention : Afin d’éviter toute possibilité de commotion électrique, débranchez le cordon d’alimentation de la prise avant d’effectuer la maintenance de l’instrument. Vorsicht: Zur Vermeidung von Stromschlägen sollte das Gerät vor der Wartung vom Netz getrennt werden.
  • Page 10 Commonly Used Symbols Direct current Courant continu Gleichstrom Corrente continua Corriente continua Alternating current Courant alternatif Wechselstrom Corrente alternata Corriente alterna Protective conductor terminal Borne du conducteur de protection Schutzleiteranschluss Terminale di conduttore con protezione Borne del conductor de tierra...
  • Page 11 Commonly Used Symbols (Continued) Frame or chassis terminal Borne du cadre ou du châssis Rahmen- oder Chassisanschluss Terminale di struttura o telaio Borne de la estructura o del chasis Caution or refer to manual Attention ou reportez-vous au guide Vorsicht, oder lesen Sie das Handbuch Prestare attenzione o fare riferimento alla guida Actúe con precaución o consulte la guía Caution, hot surface or high temperature...
  • Page 12 Commonly Used Symbols (Continued) Caution, risk of electric shock (high voltage) Attention, risque de commotion électrique (haute tension) Vorsicht, Elektroschockgefahr (Hochspannung) Attenzione, rischio di scossa elettrica (alta tensione) Precaución, peligro de descarga eléctrica (alta tensión) Caution, risk of needle-stick puncture Attention, risques de perforation de la taille d’une aiguille Vorsicht, Gefahr einer Spritzenpunktierung Attenzione, rischio di puntura con ago...
  • Page 13 Commonly Used Symbols (Continued) Fuse Fusible Sicherung Fusibile Fusible Electrical power on Sous tension Netzschalter ein Alimentazione elettrica attivata Alimentación eléctrica conectada Electrical power off Hors tension Netzschalter aus Alimentazione elettrica disattivata Alimentación eléctrica desconectada...
  • Page 14 United States – FCC Emissions Notes This device complies with Part 15 of the FCC Rules. Operation is subject to the following two conditions: (1) this device may not cause harmful interference, and (2) this device must accept any interference received, including interference that may cause undesired operation.

  • Page 15: Intended Use

    600E Pump Information Intended Use When you develop methods, follow the “Protocol for the Adoption of Analytical Methods in the Clinical Chemistry Laboratory,” American Journal of Medical Technology, 44, 1, pages 30–37 (1978). This protocol covers good operating procedures and techniques necessary to validate system and method performance.

  • Page 17: Table Of Contents

    Basic Operation ......................13 Powering Up the System ................. 13 2.1.1 Powering Up IEEE-488 Components ..........13 2.1.2 Powering Up the Stand-Alone 600E System ........16 Running Diagnostics ..................16 2.2.1 Powerup Self-Diagnostics ..............16 2.2.2 Running Extended Diagnostics ............17 Using the Controller Front Panel ..............
  • Page 18 4.1.2 Selecting an Integrator ..............51 4.1.3 Selecting the Report Type ..............54 Verifying that PowerLine Devices Are Active..........61 Setting Up the 600E Pump ................63 4.3.1 Accessing the Pump Setup Screen ............ 65 4.3.2 Setting Pump Setup Parameters ............66 4.3.3 Exiting the Pump Setup Screen ............
  • Page 19 Setting Up Dissolution Control ............... 76 Setting Up the Detectors ................. 76 4.6.1 Accessing the Detector Setup Screen ..........79 4.6.2 Setting Detector Setup Parameters ........... 80 4.6.3 Exiting the Detector Setup Screen ............ 83 Chapter 5 Running PowerLine in Direct Control Mode ..........
  • Page 20 Creating an Event Table ................111 6.2.1 Documenting the Event Table ............112 6.2.2 Programming the Event Table ............115 6.2.3 Entering Parameter Values in the Event Table ........ 118 6.2.4 Editing the Event Table ..............119 Creating a Detector Table................119 6.3.1 Documenting the Detector Table ............
  • Page 21 Setting Up the 600 as a Gradient Controller ..........150 8.1.1 Configuring the Controller Type ............. 152 8.1.2 Communicating with a Data System ..........154 Setting Up the 600E Pump ................157 8.2.1 Accessing the Pump Setup Screen ..........158 8.2.2 Setting Pump Setup Parameters ............160 8.2.3 Exiting the Pump Setup Screen ............
  • Page 22 10.1.3 Entering Parameter Values into the Gradient Table ......179 10.1.4 Editing the Gradient Table .............. 180 10.2 Creating an Event Table ................182 10.2.1 Documenting the Event Table ............182 10.2.2 Programming the Event Table ............185 10.2.3 Entering Parameter Values into the Event Table ......188 10.2.4 Editing the Event Table ..............
  • Page 23 Appendix B Eluent Considerations ..................207 Eluent Compatibility with the 600E System ..........207 Clean Eluent ....................211 Eluent Miscibility..................212 B.3.1 Eluent Properties Table ..............213 B.3.2 Using Miscibility Numbers (M-Numbers) ........214 Head Height....................215 Eluent Viscosity..................... 215 Eluent Degassing...................
  • Page 24 xxiv Table of Contents...

  • Page 25: Preface

    Preface The Waters 600E Multisolvent Delivery System User’s Guide describes the features and ® use of the Waters 600E Multisolvent Delivery System. This guide also includes information on the use of these systems with other Waters components, including autosamplers, detectors, and computer control/data management systems.
  • Page 26 Online Help A convenient way to look up information while using the 600E System. You access Help by pressing the Help screen key whenever it appears on the controller screens. Printed Documentation for the Base Product Waters 600E System Quick Start Guide: Provides concise setup and operational information that is designed to get you up and running right away.
  • Page 27 Convention Usage Keys The word key refers to a computer key on the keypad or keyboard. Screen keys see the keys on the instrument located immediately below the screen. For example, “The A/B screen key on the 2414 Detector displays the selected channel.” …...
  • Page 28 xxviii...

  • Page 29: Chapter 1 Introduction

    600E Multisolvent Delivery System. It describes the system and each individual system module. 1.1 Waters 600E System Overview The Waters 600E system is a high-performance liquid chromatography (HPLC) multisolvent delivery system that includes the following features: • 225 µL pump head volume at 45 mL/min flow rate or 100 µL pump head volume at 20 mL/min flow rate •...
  • Page 30 Optional shelf unit to house system modules • Polymeric and stainless steel flow path with low-permeability CO tubing • Optional column heater Figure 1-1 illustrates the 600E system. Table 1-1 describes its major modules. Figure 1-1 Waters 600E System Introduction...

  • Page 31: Waters 600E System Modules

    Allows variable-volume injections from a fraction of a µL Load/Inject Handle to 20 µ L without changing loops. 1.2 Waters 600E System Modules This section discusses the major modules of the Waters 600E system: • Waters 600 Controller •...
  • Page 32 Figure 1-2 Waters 600 Controller Front Panel The 600 Controller rear panel (Figure 1-3) provides connection terminals and communication ports for operation with external devices. Figure 1-3 Waters 600 Controller Rear Panel Introduction...
  • Page 33 Stop Flow/Hold Both the Stop Flow and the Hold terminals on the controller rear panel are TTL-compatible. • Stop Flow input switch - Allows you to stop the pump unit with a signal from an external device Waters 600E System Modules...

  • Page 34: Waters 600E Pump

    1.2.2 Waters 600E Pump The Waters 600E pump (Figure 1-4 Figure 1-5) contains the components required to blend and deliver eluents from the reservoir bottles to the injector. The Waters 600E pump features: • Four-eluent blending (Auto•Blend) • Manual, variable-volume injector (optional) •...
  • Page 35 Figure 1-4 Waters 600E Pump (Front View) Figure 1-5 600E Pump Rear Panel Waters 600E System Modules...
  • Page 36 It produces predictable gradient segments regardless of eluent compressibility and system backpressure. Eluent selection and proportioning take place on the low-pressure (intake) side of the 600E system. Flow Path The pump flow path begins with the eluent reservoirs and ends with the column as follows: 1.

  • Page 37: Powerline Controller Features

    Dissolution bath • Hanson Transfer Controller (including volumetric manifold and transfer/air vacuum source) For information on using the Waters 600E dissolution control, see the Waters Dissolution System Operator’s Manual. 1.4 Gradient Controller Features The 600 Gradient Controller allows you to: •...

  • Page 38: Options And Accessories

    Fraction Collector You can configure the Waters Fraction Collector with the Waters 600E system. You can program event outputs to control fraction collector operation, or you can program the fraction collector directly.
  • Page 39 Automatic Switching Valves Allow automatic column selection, large-volume sample injection, or flow-path diversion. 746 Data Module The Waters 746 Data Module (integrator) provides documentation of PowerLine system programs, a permanent annotated chromatographic record, and integrated data. Reference Valve Routes eluent to the reference cell of a detector. Replaces the mixing tee on the front of the pump.
  • Page 40 Introduction...

  • Page 41: Chapter 2 Basic Operation

    Chapter 2 Basic Operation This chapter introduces you to the operation of the Waters 600E Multisolvent Delivery System. This chapter assumes that you are using the system with other Waters system components. 2.1 Powering Up the System Before You Begin This section provides instructions on powering up your Waters 600E system, including: •...
  • Page 42 (for example, a non-IEEE-488 detector): 3. Power up all equipment controlled through the IEEE-488 bus. To power up the 600E system, press the On/Off switch on the front panel of the 600 controller to the 1 (On) position. The Powerup screen appears (Figure 2-1).
  • Page 43 1. Power up all equipment not controlled through the IEEE-488 bus (non-PowerLine). 2. Power up all equipment controlled through the IEEE-488 bus (PowerLine). 3. Power up the 600E system by pressing the On/Off switch on the front panel of the 600 controller to the 1 (On) position. The Powerup screen appears (Figure 2-2).

  • Page 44: Powering Up The Stand-Alone 600E System

    Gradient Controller configuration. To power up your stand-alone system: 1. Power up all external equipment (chart recorder, injector). 2. Power up the 600E system by pressing the On/Off switch on the front panel of the 600 controller to the 1 (On) position.

  • Page 45: Running Extended Diagnostics

    If any failure occurs, turn the controller Off, then On again. If the diagnostics fail a second time, contact Waters Technical Service. To reach Waters Technical Service, contact your local Waters sales/service representative. 2.2.2 Running Extended Diagnostics In addition to the powerup self-diagnostics, your 600E system contains extended diagnostic routines.

  • Page 46: Keypad

    The specific function for a given screen key appears at the bottom of the screen above the key. Figure 2-3 Waters 600 Controller Front Panel 2.3.1 Keypad The Waters 600 controller main keypad (see Figure 2-3) includes: •...

  • Page 47: Function Keys

    2. Type a value for the selected parameter. Press the Help screen key to display the allowable range for the field. 3. Press Enter. The system checks the new value to see if it is the correct type of entry and within the proper range.

  • Page 48: Screen Keys

    Gradient Controller Keys In Gradient Controller mode, function keys access different screens: Accesses Function Setup Pump Setup screen Sets up pump hardware Direct Isocratic screen Programs conditions for attended operation Operate Method Operate Gradient screen Starts a gradient run Program Program Gradient screen Sets up/stores gradient tables Method...

  • Page 49: Comparing Controller Types

    • Gradient controller configuration Note: After you have decided upon a controller type, continue with Chapter 3, Preparing Your 600E System for Operation, before proceeding to the controller-specific chapters outlined in the table below. Using PowerLine or Gradient Controller Mode...

  • Page 50: Powerline Controller Configuration

    Control external PowerLine devices (such as, autosamplers, detectors and integrators) from the Waters 600E system through the IEEE-488 bus. • Develop complex multi-method applications. Note: Your Waters 600 controller was preconfigured at the factory as a PowerLine Controller. PowerLine Description The PowerLine Controller: •...
  • Page 51 PowerLine Operation The PowerLine controller provides product-specific setup and operating parameters for PowerLine detectors and autoinjectors. Detector parameters inlude: • Detector filter constant • Autozero (except for 431/432 detector) • Polarity • Absorbance Units Full Scale (AUFS) • UV wavelength (λ) •...

  • Page 52: Gradient Controller Configuration

    When to Use Gradient Controller Mode Use the Gradient Controller configuration to: • Control the 600E system from an IEEE-based data system, such as the Waters Empower or Millennium Chromatography Manager Data System. • Operate the 600E system in stand-alone mode.

  • Page 53: Powering Down The System

    2.5 Powering Down the System If you do not plan to use the Waters 600E system for a long period of time (overnight or longer), power down the system.
  • Page 54 Basic Operation...

  • Page 55: Preparing Your 600E System For Operation

    Figure 3-2). You can perform the procedures listed in this chapter when the 600E system is in Gradient Controller mode. However, when you press the Direct key, the Isocratic screen appears. Set the parameters on the Isocratic screen as instructed in the procedures for the Direct Control screen.

  • Page 56: Sparging Eluents

    3.1 Sparging Eluents Use the Waters 600E system helium sparge feature to sparge all enabled reservoirs at a flow rate between 0 and 100 mL/min. At 100 mL/min, the sparge valves are On at all times. At flow rates less than 100 mL/min, the sparge valves turn on and off periodically to achieve an average flow rate over time.
  • Page 57 1. Confirm that sparge and eluent tubing are properly assembled and connected (see the Waters 600E Multisolvent Delivery System Installation and Maintenance Guide, Chapter 2, making Fluidic Connections to the 600E Pump). 2. Press the Setup function key. The Pump Setup screen appears (Figure 3-1).
  • Page 58 • 10 to 15 mL/min for aqueous mobile phases • 20 to 30 mL/min for aqueous-acetonitrile mobile phases • 50 mL/min for aqueous-methanol mobile phases Maintain these helium flow conditions continuously while the system is running. Preparing Your 600E System for Operation...

  • Page 59: Priming The Pump

    100 µ L pump heads may require additional priming after you introduce eluent into the inlet manifold. • You must prime with a suitable syringe (such as the one available from Waters). During priming, do not apply excessive force to the syringe by injecting eluent more quickly than the pumps can accept.
  • Page 60 • If you are using a Waters 717plus Autosampler, put the autosampler in purge mode. Initiating Flow 1. Rotate the inlet manifold valve handle located on the front of the pump to the Run...
  • Page 61 Drawing Off Eluent Once you have initiated flow, draw off eluent as follows: 1. Move the cursor to the %A field for the first eluent and type 100 in the New column. Press Enter. 2. Type 0 and press Enter for the remaining eluent composition fields. 3.

  • Page 62: Daily Routine Operation

    2. Press the Direct function key. The Direct Control screen appears. 3. Move the cursor to the Flow Rate field and type a flow rate of 2.00 mL/min. Preparing Your 600E System for Operation...

  • Page 63: Flushing The System

    4. Flush for 2 to 5 minutes. 5. If your system backpressure fluctuates more than 100 psi (7 kg/cm ) once the system has reached the operating flow rate, prime the system again as described in Section 3.2, Priming the Pump.

  • Page 64: Flushing The System Fluid Lines

    3. Fill a syringe (fitted with a 22-gauge, 90° point needle) with the new or intermediate eluent. 4. Set the injector handle to the Load position (Figure 3-5). Figure 3-5 Injector Handle in the Load Position Preparing Your 600E System for Operation...

  • Page 65: Purging The Autoinjector

    9. Allow the eluent to flow for several minutes at 1.0 mL/min. 3.4.3 Purging the Autoinjector Perform the following steps to purge a Waters autoinjector. If you are using a non-Waters autoinjector, see the documentation provided with the autoinjector for the appropriate steps to flush the autoinjector flow path.

  • Page 66: Equilibrating The System

    Equilibrate both the eluent and the system at ambient temperature before pump operation. Cold eluents that flow through a system at room temperature outgas as they warm up. • If you are operating in a cold room, equilibrate the system at the reduced temperature. Preparing Your 600E System for Operation...
  • Page 67 Procedure To equilibrate the system: 1. Press the Direct function key to access the Direct Control screen (see Figure 3-2). Sparging 2. If desired, set the sparging conditions as follows: a. Move the cursor to the Sparge field. b. Type in the maintenance rate for your eluents. Press Enter. All reservoirs that are enabled for sparging on the Pump Setup screen sparge at that rate.
  • Page 68 • At the l field, type the required detector operating wavelength. Press Enter. Valid entries are 190 to 600 nm. For a PowerLine refractive index detector (Waters 410), at the Sens field, type the required sensitivity. Press Enter. Valid values are 1, 2, 4, 8, 16, 32, 64, 128, 256, 512, and 1024.

  • Page 69: Changing Eluents

    Eluent Compatibility All eluents are compatible with the 600E system. However, long-term static exposure to halide salts (for example, fluoride, bromide, chloride, and iodide) will cause pitting and corrosion of stainless steel parts. Flush the system thoroughly with water if the pump will be idle for more than two days.

  • Page 70: Changing Between Incompatible Eluents

    Before you begin, take into account the following considerations: • If organic eluents and aqueous buffers are used together, be careful not to precipitate salt in the pump heads and check valves during eluent changes. Preparing Your 600E System for Operation...
  • Page 71 • Changes involving two miscible eluents can be made immediately, without an intermediate eluent. • To prevent eluent contamination, use the same container to prepare, supply, and store an eluent. Once a container is used for one eluent, it should not be used for any other eluent without a thorough cleansing.
  • Page 72 4. Flush the system with 20 to 40 mL of eluent at a flow rate of 2.0 mL/min for 10 to 20 minutes or until the detector signal is constant. Adding the Final Eluent to the System To add the final eluent to the system, follow the instructions in Section 3.6.1, Adding Fresh Eluent. Preparing Your 600E System for Operation...

  • Page 73: Setting Powerline Controller Operating Parameters

    Section 2.4.2, Gradient Controller Configuration. For instructions on configuring and using your Waters 600 Controller as a Gradient Controller, see Chapters 8 through 11. When to Use the PowerLine Controller Use PowerLine Controller mode when you want to control other devices (such as, detectors, autosamplers, and integrators) from the 600E system.
  • Page 74 Screen Layout Figure 4-1 illustrates the relationship of the screens associated with the Waters 600 controller in its PowerLine configuration. See Figure 4-1 when you set PowerLine parameters in preparation for a run. Figure 4-1 PowerLine Controller Screens Setting PowerLine Controller Operating Parameters...

  • Page 75: Setting Up The 600 As A Powerline Controller

    4.1 Setting Up the 600 as a PowerLine Controller This section describes how to use the Pump Configuration screen to configure the Waters 600 Controller as a PowerLine Controller. It includes procedures for: • Configuring the controller type • Communicating with a data module (integrator) •...
  • Page 76 Figure 4-2 Pump Configuration Flowchart Setting PowerLine Controller Operating Parameters...

  • Page 77: Configuring The Controller Type

    Press the Cancel screen key to return to the Pump Setup screen without saving any changes made to the Pump Configuration screen. 4.1.1 Configuring the Controller Type This section describes how to configure the Waters 600 Controller as a PowerLine Controller. Waters preconfigures the 600 controller as a PowerLine Controller at the manufacturing site.
  • Page 78 It is not necessary to set any parameters on this screen right now. A description of this screen and parameters appears in Section 4.3, Setting Up the 600E Pump. 4. Press the Pump Config screen key to display the Gradient Controller Pump...

  • Page 79: Selecting An Integrator

    Section 4.3, Setting Up the 600E Pump 4.1.2 Selecting an Integrator This section describes how to set the parameters for an optional Waters 745B/746 Data Module (integrator). An integrator allows you to print out a report at the conclusion of a run.
  • Page 80 Accessing the Pump Configuration Screen 1. Press the Set Up function key from the PowerLine Controller Powerup screen. The PowerLine Controller Pump Setup screen appears (Figure 4-6). Figure 4-6 PowerLine Controller Pump Setup Screen 2. Press the Pump Config screen key. The PowerLine Controller Pump Configuration screen appears (Figure 4-7).
  • Page 81 2. Type the number for the module you want to use: • 0 for no device connected • 1 for a Waters 745B Data Module • 2 for a Waters 746 Data Module 3. Press Enter. The system automatically displays the default RS-232 communication parameters in the fields at the bottom of the screen.

  • Page 82: Selecting The Report Type

    Section 4.3, Setting Up the 600E Pump 4.1.3 Selecting the Report Type If you connected a Waters 745B/746 Data Module to the RS-232 port, specify the type of report to print as follows: 1. Move the cursor to the Print field.
  • Page 83 Figure 4-8 Example of a Short Report (First Injection) Setting Up the 600 as a PowerLine Controller...
  • Page 84 Figure 4-8 Example of a Short Report (First Injection) (Continued) Setting PowerLine Controller Operating Parameters...
  • Page 85 Figure 4-9 Example of an Abridged Report (First Injection) Setting Up the 600 as a PowerLine Controller...
  • Page 86 Figure 4-9 Example of an Abridged Report (First Injection) (Continued) Setting PowerLine Controller Operating Parameters...
  • Page 87 Figure 4-10 Example of a Full Report (All Injections) Setting Up the 600 as a PowerLine Controller...
  • Page 88 Figure 4-10 Example of a Full Report (All Injections) (Continued) Setting PowerLine Controller Operating Parameters...

  • Page 89: Verifying That Powerline Devices Are Active

    600E Multisolvent Delivery System Installation and Maintenance Guide, Section 3.3, Making IEEE-488 Interface Connections. Verifying PowerLine Devices To verify that the PowerLine devices in your 600E system are active on the IEEE-488 bus: 1. Press the Setup function key to display the Pump Setup screen (Figure 4-6).
  • Page 90 Connections, for the PowerLine device connection procedure. Note: If you do not set a PowerLine device IEEE-488 address correctly, the controller will not recognize the device. See the Waters 600E Multisolvent Delivery System Installation and Maintenance Guide, Section 3.3, Making IEEE-488 Interface Connections, for information on setting addresses and powerup sequences.

  • Page 91: Setting Up The 600E Pump

    4.3 Setting Up the 600E Pump This section describes how to access and use the Pump Setup screen in PowerLine Control mode. It includes the following information: • Accessing the Pump Setup screen • Setting Pump Setup screen parameters •...
  • Page 92 Figure 4-12 PowerLine Controller Pump Setup Flowchart Setting PowerLine Controller Operating Parameters...

  • Page 93: Accessing The Pump Setup Screen

    Table 4-2. Table 4-2 Pump Setup Screen Keys Function Next Setup Displays the configuration screens for the autoinjector and detectors. System Config Identifies the PowerLine modules active in the system. Setting Up the 600E Pump...

  • Page 94: Setting Pump Setup Parameters

    Table 4-2 Pump Setup Screen Keys (Continued) Function Pump Config Displays additional configuration parameters related to the pump and controller. Lock Keyboard Locks or unlocks the keyboard. Help Displays the Help screen for the Pump Setup screen. 4.3.2 Setting Pump Setup Parameters This section describes the pump parameters on the Pump Setup screen (see Figure 4-13)
  • Page 95 3. Press Enter. Press Limits Defines the high and low operating-pressure limits of the Waters 600E pump. Your system column and packing chemistry determine the low and high values. See the Care and Use Manual supplied with the column to determine the maximum pressure to which you can expose the column.
  • Page 96 This time delay is the system, or delay, volume. The 600E system has been optimized to reduce the delay volume. The detector signal is further delayed by the volume of the column. At a low flow rate, with a column attached, the delay between an eluent changeover instruction and its subsequent detection may be several minutes.
  • Page 97 4. At the Step field, type the step number of the Method Table where program execution will start. Press Enter. 5. At the Vial field, type the vial number in the specified step number where sample analysis will start. Press Enter. Setting Up the 600E Pump...
  • Page 98 Sample Method Table For example, your Method table may appear as shown in Figure 4-14. FIRST LAST STEP # INJ INJ VOL TABLE # VIAL VIAL TIME PRG 1 EQUIL PRG 1 EQUIL Figure 4-14 Example of a Method Table If you want to equilibrate your system 12 hours from now and start on vial 15, type the following in the Autostart field: In 12 Hrs 0 Min Step 3 Vial 15...

  • Page 99: Exiting The Pump Setup Screen

    • Pump Config - Displays the Pump Configuration screen 2. Press one of the function keys to enter a different mode. 4.4 Setting Up the Autoinjector Refer to this section when using a PowerLine autosampler (Waters 717plus) in your system. This section describes: •...
  • Page 100 Figure 4-15 Autoinjector Setup Flowchart Setting PowerLine Controller Operating Parameters...

  • Page 101: Accessing The Autoinjector Setup Screen

    4.4.1 Accessing the Autoinjector Setup Screen You set up the autoinjector through the Autoinjector Setup screen. To access the Autoinjector Setup screen (Figure 4-16): 1. Press the Set Up key to display the Pump Setup screen (Figure 4-13). 2. Press the Next Setup screen key to display the Autoinjector Setup screen (Figure 4-16).

  • Page 102: Setting Autoinjector Setup Parameters

    (see Table 5-1). Standards can occupy up to the first five consecutive vial positions in the Waters autoinjector carousel and must start with Vial 1. If you are using fewer than five standards, samples can start in the next vial position after the last standard.

  • Page 103: Exiting The Autoinjector Setup Screen

    • Injection Volume - Type the volume in µL (0 to 2000) for a standard injection and press Enter. Dissolution Specifies whether you will be using a dissolution bath with your Waters WISP 712D Autoinjector. To set the Dissolution parameter: 1.

  • Page 104: Setting Up Dissolution Control

    4. Press the Next Setup screen key. The Dissolution Setup screen appears. When you use the 600E system for dissolution control, the collection of dissolution samples becomes the highest-priority function of the system. When the 712D is not in the process of collecting dissolution samples, you can run chromatography on previously collected samples or calibration standards.
  • Page 105 Using Multiple Detectors You may use up to three PowerLine detectors in the system at one time: • Two UV/Vis absorbance detectors (two Waters 486 detectors, two channels of a Waters 490E detector, or one 486 and one 490E channel) and •...
  • Page 106 Figure 4-17 Detector Setup Flowchart Setting PowerLine Controller Operating Parameters...

  • Page 107: Accessing The Detector Setup Screen

    4. If the Dissolution Control screen appeared in step 3, press the Next Setup screen key again to display the Detector Setup screen. Figure 4-18 Detector Setup Screen (with 410 Detector Parameters) The Detector Setup screen also supports setup of a Waters 431/432 Conductivity detector as an alternate Det #3 (Figure 4-19).

  • Page 108: Setting Detector Setup Parameters

    Figure 4-19 Detector Setup Screen (with 431/432 Detector Parameters) In addition to the parameters shown on the screen, the Detector Setup screen displays the screen keys described in Table 4-4. Table 4-4 Detector Setup Screen Keys Function Next Setup Displays the Pump Setup screen. Help Displays the Help screen for the Detector Setup screen.
  • Page 109 Data Chan Assigns an identifying number to a channel of data when using an integrator or data system (for example, the Waters Millennium Chromatography Manager or the Waters ExpertEase 845/860 Data System) with your Waters 600E system. Note: The channel number is arbitrary and is for documentation purposes only.
  • Page 110 Specifies whether the data output of the detector is positive or negative. Note: This parameter affects only the detector 10 mV full scale output, except for the Waters 431/432 in which case both the 1 V output and the 10 mV output are affected. To set polarity: 1.

  • Page 111: Exiting The Detector Setup Screen

    3. Press Enter. Ext temp 1, Ext temp 2 Specifies the set temperature of up to two external column heaters connected to the Waters 410 detector. To set the Ext Temp parameters: 1. Move the cursor to the appropriate Ext Temp field for Det #3.
  • Page 112 Setting PowerLine Controller Operating Parameters...

  • Page 113: Running Powerline In Direct Control Mode

    Running PowerLine in Direct Control Mode Once you have familiarized yourself with your system and prepared your system according to the procedures in Chapters 1 through 4, you can run your Waters 600E Multisolvent Delivery System in the direct control mode. Direct Control All direct-control operations are isocratic.

  • Page 114: Setting Run Conditions

    External event switches • Autoinjector parameters • Detector parameters Figure 5-1 illustrates the steps involved in using the Direct Control screen. Use this figure for quick reference once you become familiar with the 600E system. Running PowerLine in Direct Control Mode...
  • Page 115 Figure 5-1 Direct Control Flowchart Setting Run Conditions...

  • Page 116: Setting Pump Parameters

    Accessing the Direct Control Screen You set the run conditions from the Direct Control screen. To access the Direct Control screen, press the Direct function key. The PowerLine Controller Direct Control screen appears (Figure 5-2). Figure 5-2 PowerLine Controller Direct Control Screen Exiting the Direct Control Screen To exit the Direct Control screen, press any function key to select another mode.
  • Page 117 Flow Specifies the eluent flow rate. To set the Flow Rate: 1. Move the cursor to the Flow field if necessary. 2. Type the appropriate eluent flow rate (0.00 to 20.0 or 45.00 mL/min) for the application and press Enter. The system immediately sets the pump to the flow rate you entered.

  • Page 118: Setting External Event Switches

    (see Section 4.3.2, Setting Pump Setup Parameters). Note: If there is no column heater installed in the 600E system, the Temp field displays a value of None. To set the optional column heater temperature: 1. At the Temp field, type the appropriate temperature for the chromatography that you wish to run.

  • Page 119: Setting Autoinjector Parameters

    Before setting any of the event switches, ensure that all external devices are connected to the appropriate switch terminals on the rear panel of the controller. See the Waters 600E Multisolvent Delivery System Installation and Maintenance Guide for more information on making connections.
  • Page 120 Equilibrate Equilibrates the system at initial conditions for the specified run time. Purge 410 Purges the Waters 410 detector by placing its flow path in the purge mode and running initial condi- tions for the specified run time. Purge Inj Purges the PowerLine autoinjector (Waters 717plus) for 4.5 minutes using the autoinjector...

  • Page 121: Setting Detector Parameters

    Section 4.2, Verifying that PowerLine Devices Are Active. Controlling the 486 Detector Lamp Note: Waters recommends that in order to conserve lamp life, do not turn the lamp off for less than 4 hours. To turn On/Off the 486 detector lamp: 1.

  • Page 122: Performing A Direct Control Run

    2. Press the Lamp On/Lamp Off screen key for the desired function. The key toggles between the two functions. Waters 486 lamp status is checked at the beginning of each run. If the lamp is off at the start of a run, the system returns to IDLE and the error message Unable to Set Up appears.
  • Page 123 In addition to the parameters shown on the screen, the Direct Control screen displays the screen keys described in Table 5-2. Table 5-2 Direct Control Screen Keys Function Setup Sends the operating parameters (displayed on the setup screens) to the PowerLine modules. Toggles with Start Run and Abort. Start Run Starts the isocratic run and the run time clock.

  • Page 124: Setting The Run Time

    5.2.1 Setting the Run Time Use the Direct Control screen (see Figure 5-2) to set the Run Time parameter. Run Time Specifies the duration of the analysis after the injection is made. The system does not recognize another Inject signal while a run is in progress. To set the run time: 1.

  • Page 125: Equilibrating The System

    5.2.3 Equilibrating the System When the system status displays , the system is running with the conditions Initial displayed on the Direct Control screen and with the downloaded PowerLine module operating parameters. The system runs at these conditions until you equilibrate the system. For more details, see Section 3.5, Equilibrating the System.

  • Page 126: Stopping The Pump

    3. The autoinjector draws the sample and makes the injection. The autoinjector sends a contact closure signal to the Inject input terminal on the rear panel of the controller. Using the Start Run Screen Key with a Non-PowerLine Autoinjector For methods development and for runs that are not time-sensitive, you may also use the Start Run screen key to start a run with a non-PowerLine autoinjector.

  • Page 127: Aborting A Run

    5.2.6 Aborting a Run 1. Press the Abort screen key. The Caution screen appears (Figure 5-3). Figure 5-3 Caution Screen 2. Press either the: • Abort screen key to immediately abort the run • Direct function key to continue running 5.2.7 Changing Parameters During a Run The pump, external switch, injector, and detector conditions displayed on the Direct Control screen can be changed while a run is in progress.
  • Page 128 Accessing the Operate Method Screen To run a method from the Direct Control screen: 1. Press the Operate Method function key. The initial Operate Method screen appears with the current direct control flow conditions shown in the Current field (Figure 5-4).

  • Page 129: Creating Powerline Methods

    Waters 600E Multisolvent Delivery System. You can combine these tables to compose a method. A method is a set of instructions that controls how and when a run is made. In the Waters 600E system, a method comprises a set of timed-based tables consisting of: •...

  • Page 130: Creating A Gradient Table

    Chapter 7, Running PowerLine Methods. 6.1 Creating a Gradient Table This section provides the information you need to create the first element of a method table, the gradient table. Use the gradient table to control the 600E pump. Creating PowerLine Methods...

  • Page 131: Documenting The Gradient Table

    This section describes: • Documenting the gradient table • Programming the gradient table Note: When creating gradient, event, and detector tables, be sure that you design the time-related parameters specified in each table to work effectively with the time-related parameters in the other two tables of the same set. 6.1.1 Documenting the Gradient Table Define the information you want in a gradient table before you actually program a gradient table.
  • Page 132 This line in the gradient table should: • Be executed by the controller after the separation is complete (run time has elapsed) and allow enough time for the column to equilibrate • Change the flow rate to that used in the Initial line of the gradient table •...

  • Page 133: Programming The Gradient Table

    Editing the gradient table Figure 6-4 illustrates the steps involved in using the Program Gradient screen to create a gradient table. Use this flowchart for quick reference once you become familiar with your Waters 600E system. Creating a Gradient Table 105...
  • Page 134 Figure 6-4 Program Gradient Flowchart Creating PowerLine Methods...
  • Page 135 Accessing the Program Gradient Screen Press the Program Table function key to display the PowerLine Controller Program Gradient screen (Figure 6-5). Figure 6-5 PowerLine Controller Program Gradient Screen In addition to the gradient table parameters, there are five active screen keys. These screen keys have the functions described in Table 6-1.

  • Page 136: Entering Parameter Values In The Gradient Table

    Exiting the Program Gradient Screen To exit the Program Gradient screen, press either: • The Next Table screen key to access the Program Event screen • Any function key, except the Program Table key, to enter another mode 6.1.3 Entering Parameter Values in the Gradient Table To enter the parameter values into the Program Gradient table (see Figure 6-5):...

  • Page 137: Editing The Gradient Table

    7. At the Curve field, type the gradient curve profile number for the gradient segment. Figure 6-6 shows the gradient curve profiles. Figure 6-6 Gradient Curve Profiles 8. Repeat steps 3 through 7 for each line in the gradient table. 9.
  • Page 138 Deleting Lines To delete individual lines from a table: 1. Move the cursor to any field on the line you want to delete. 2. Press the Clear Line screen key. This immediately clears the line the cursor is on and moves succeeding lines in the table up one line.

  • Page 139: Creating An Event Table

    To save the new table, repeat steps 1 and 2, and assign a different table number to the table. Continue this process until you locate a table that can be replaced with the new table. Replacing Existing Tables A maximum of 15 tables of one type can be stored in permanent memory in the controller. Once 15 tables are saved, you must replace one of these tables to save a new table.

  • Page 140: Documenting The Event Table

    Note: When creating gradient, event, and detector tables, be sure that you design the time-related parameters specified in each table to work effectively with the time-related parameters in the other two tables of the same set. 6.2.1 Documenting the Event Table Define the information you want in an event table before you actually program the event table.
  • Page 141 • Waters 486 lamp status is checked at the beginning of each run. If the lamp is turned off via Event 10 at the start of a run, the system returns to IDLE and the error message appears.
  • Page 142 • Waters 486 lamp status is checked at the beginning of each run. If the lamp is turned off via Event 10 at the start of a run, the system returns to IDLE and the error message appears.

  • Page 143: Programming The Event Table

    6.2.2 Programming the Event Table Figure 6-8 illustrates the steps involved in using the Program Event screen to create an event table. Use this flowchart for quick reference once you become familiar with the Waters 600E system. Creating an Event Table 115...
  • Page 144 Figure 6-8 Program Event Flowchart Creating PowerLine Methods...
  • Page 145 The remainder of this section describes how to access the Program Event screen and enter an event table. Accessing the Program Event Screen 1. Press the Program Table function key to display the Program Gradient screen (see Figure 6-5). 2. Press the Next Table screen key. The PowerLine Controller Program Event screen appears (Figure 6-9).

  • Page 146: Entering Parameter Values In The Event Table

    Table 6-3 Program Event Screen Keys (Continued) Function Save Saves the table currently displayed and erases the previous values. You must save the table before leaving this screen. Otherwise, you lose any changes that you made. Help Displays the Help screen associated with the Program Event screen.

  • Page 147: Editing The Event Table

    Table. 6.3 Creating a Detector Table Skip this section if you are not using PowerLine detectors in your Waters 600E system. This section provides the information you need to create the third and last component of a method table, the detector table.

  • Page 148: Programming The Detector Table

    3. When the table entries are complete, keep the Analysis Plan and File Sheet as a permanent record of your table. Detector table entries affect the two UV/Vis detectors (Waters 486 and 490E). There is a separate sensitivity parameter for the Waters 410 RI detector and Waters 431/432 Conductivity detector.
  • Page 149 Figure 6-11 Detector Table Flowchart Creating a Detector Table 121...
  • Page 150 Accessing the Detector Tables Screen 1. Press the Program Table function key to display the Program Gradient screen (see Figure 6-5). 2. Press the Next Table screen key to display the Program Event screen (see Figure 6-9). 3. Press the Next Table screen key. The Detector Tables screen appears (Figure 6-12).

  • Page 151: Entering Parameter Values In The Detector Table

    Table 6-4 Detector Table Screen Keys (Continued) Function Save Saves the table currently displayed and erases the previous values. You must save the table before leaving this screen. Help Displays the Help screen associated with the Detector Tables screen. 6.3.3 Entering Parameter Values in the Detector Table To enter the parameter values into the Detector Table (see Figure 6-12):...

  • Page 152: Editing The Detector Table

    c. At the Det/Chan field, type a value to specify which UV/Vis detector (1 = Det #1 or 2 = Det #2) or channel to change. Press Enter. d. At the l field, type a wavelength value between 190 and 600 nm. Press Enter. Note: By default, wavelength changes are accompanied by an Autozero, unless you disable this feature using the detector diagnostics.

  • Page 153: Programming The Method Table

    6.4.2 Programming the Method Table Figure 6-13 illustrates the steps involved in using the Program Methods screen to create a Method Table. Use this flowchart for quick reference once you become familiar with your Waters 600E system. Creating a Method Table 125...
  • Page 154 Figure 6-13 Program Methods Flowchart Creating PowerLine Methods...
  • Page 155 Accessing the Program Methods Screen To access the Program Methods screen, press the Program Method function key. The Program Methods screen appears with the cursor at the Step field (Figure 6-14). Figure 6-14 Program Methods Screen In addition to the methods table parameters, the Program Methods screen displays seven active screen keys that function as described in Table 6-5.

  • Page 156: Entering Parameter Values In The Method Table

    2. Type the number of the vial from which you want to make the first injection. Press Enter. The system automatically assigns a step number. • When using a Waters PowerLine autoinjector, the vial number can be any value between 1 and 48 or 1 and 96, depending on the autoinjector carousel.
  • Page 157 Table 6-6 Special Vial Codes (Continued) Vial Code Function Description Purge 410 Purges the Waters 410 detector by placing its flow path in the purge mode and running initial conditions for the specified run time. Purge Inj Purges the PowerLine autoinjector (Waters 717plus) for 4.5 minutes using the autoin-...

  • Page 158: Editing The Method Table

    5. At the Inj Vol field, type the sample volume for all injections. Press Enter. • When using a Waters autosampler (717plus), the maximum volume is determined by the loop size (200 µ L or 2000 µL) installed in the autosampler.
  • Page 159 2. Press the Insert Line screen key. This copies the line the cursor is presently on to the new line and reorders the step numbers. 3. Edit the information on the new line as necessary. Saving Tables Whenever you change a table, you must save the changes before powering down the system.
  • Page 160 Creating PowerLine Methods...

  • Page 161: Running Powerline Methods

    If you have not performed these tasks, please take the time to do them now. 7.1 Using an Injector The Waters 600E system supports three methods for injecting samples. The following sections present programming instructions for each method and a description of how to make injections using: •...
  • Page 162 Caution: Always follow safe laboratory practices when handling eluents. Know the physical and chemical properties of the eluents. See the Material Safety Data Sheets for the eluents in use. Caution: When using sample loops larger than 100-µL, protect yourself from the rapid ejection of mobile phase from the needle port when you turn the valve from Inject to Load.

  • Page 163: Using A Powerline Autoinjector

    Note: For complete information on the Waters 717plus Autosampler, see the Waters 717plus Autosampler Operator’s Manual. You configure a PowerLine autoinjector such as the Waters 717plus Autosampler on the IEEE-488 bus. The autoinjector is under the control of the Waters 600 Controller.

  • Page 164: Setting Initial Operating Parameters

    (see Chapter 6, Creating PowerLine Methods). Figure 7-2 summarizes the steps involved in using the Operate Methods screens. Use this flowchart for quick reference once you become familiar with your Waters 600E system. Running PowerLine Methods...
  • Page 165 Figure 7-2 Operate Method Flowchart Setting Initial Operating Parameters 137...
  • Page 166 Accessing Initial Operate Method Screen Press the Operate Method function key. The initial Operate Method screen appears with the cursor at the Step # field (Figure 7-3). Figure 7-3 Initial Operate Method Screen This screen displays the following: • Step number, vial number, and injection number at which the run will start, and the keyboard status (locked or unlocked) during the run.

  • Page 167: Starting A Run

    If Autostart is active at this time, the keyboard will be locked. To abort the Autostart, unlock the keyboard on the Pump Setup screen (see Section 4.3.2, Setting Pump Setup Parameters). After the keyboard is unlocked, make your changes to the Initial Operate Method screen as follows: 1.
  • Page 168 2. Press the Operate Method function key again. The Operate Methods screen appears (Figure 7-4). Figure 7-4 Operate Methods Screen Operate Methods Screen Keys In addition to the current system conditions, the Operate Methods screen displays the screen keys described in Table 7-1 Table 7-1 Operate Methods Screen Keys Function...

  • Page 169: Downloading Operating Parameters

    Running Analysis in progress. Reporting Report is printing on the Waters 746 integrator. 7.3.2 Downloading Operating Parameters When you press the Operate Method function key to display the Operate Methods screen, the controller automatically downloads to the PowerLine modules the parameters that you...

  • Page 170: Running A Method

    7.3.3 Running a Method Note: The 600 controller examines the status of the 490E detector before initiating a run. If the detector is in the standby state, the controller automatically turns on the lamp. Using the Rheodyne 7725i Manual Injector To begin a run with the Rheodyne 7725i manual injector: 1.

  • Page 171: Modifying Conditions While Running

    2. Program and start the autoinjector. 3. Press the Start Run key as soon as possible after the injection occurs. Note: An Autostart method can override a method that you started with the Start Run screen key. Starting the Run-Time Clock When the controller receives an Inject signal from an injector, the system status changes to Running and the run-time clock begins counting at 0.00.

  • Page 172: Changing Parameters

    7.4.1 Changing Parameters You can change the following parameters during a run: • Sparge rate • Column heater temperature • Event switch status (On/Off) • Operating parameters for any of the detectors Note: You can change parameters only if the keyboard is unlocked. To change a parameter on the Operate Methods screen: 1.

  • Page 173: Modifying Gradient, Event, And Detector Tables

    Flow causes switch S4 to default to the Off position. This action provides an additional level of control for non-IEEE devices. Note: The receipt of the Stop Flow signal (at the 600 controller’s Stop Flow rear panel terminal) suspends the controller’s run, gradient, and event clocks. The three clocks resume operation when the Stop Flow signal terminates.

  • Page 174: Modifying The Method Table

    To modify a table that is currently running: 1. Stop the run by pressing the Abort screen key from the Operate Methods screen. The Caution I screen appears. 2. Press the Abort screen key from the Caution I screen (Figure 7-5).
  • Page 175 Figure 7-5 Caution I Screen 2. Take one of the following actions: • To cancel the abort and resume monitoring the method, press the Operate Method function key. The Operate Methods screen appears. • To immediately abort the run, press the Abort function key. This action also stops dissolution acquisition.
  • Page 176 Figure 7-6 Caution II Screen 2. Take one of the following actions: • To cancel the abort and continue monitoring the method, press the Operate Method function key. The Operate Methods screen appears. • To abort the method immediately and enter the direct control mode, press the Direct function key.

  • Page 177: Setting Gradient Controller Operating Parameters

    Use Gradient Controller mode when you want to control the Waters 600E Multisolvent Delivery System from a data system (Millennium Chromatography Manager or ExpertEase 845/860 Data System), or when you want to run the 600E system in stand-alone operation. For a detailed description of Gradient Controller mode, see Section 2.4.2, Gradient...

  • Page 178: Setting Up The 600 As A Gradient Controller

    Keys. Figure 8-1 Gradient Controller Screens 8.1 Setting Up the 600 as a Gradient Controller This section describes how to use the Pump Configuration screen to configure the Waters 600 Controller as a Gradient controller. It includes procedures for: •...
  • Page 179 Figure 8-2 illustrates the steps involved in using the Pump Configuration screen. Use this flowchart as a quick reference for setting the parameters on the Pump Configuration screen. Figure 8-2 Pump Configuration Flowchart Setting Up the 600 as a Gradient Controller 151...

  • Page 180: Configuring The Controller Type

    Pump Configuration screen, press the Cancel screen key. 8.1.1 Configuring the Controller Type This section describes how to configure the Waters 600 Controller as a Gradient Controller. Waters preconfigures the 600 controller as a PowerLine Controller at the manufacturing site.
  • Page 181 It is not necessary to set any parameters on the Pump Setup screen now. For a description of the gradient controller version of the Pump Setup screen and pump parameters, see Section 8.2, Setting Up the 600E Pump. 4. Press the Pump Config screen key to display the PowerLine Controller Pump...

  • Page 182: Communicating With A Data System

    Section 8.2, Setting Up the 600E Pump 8.1.2 Communicating with a Data System Use this section only if you intend to use the Waters Millennium Chromatography Manager (PC-based) or the Waters ExpertEase 845/860 Data System (VAX/VMS-based) to control the 600E system. Otherwise, proceed to Section 8.2, Setting Up the 600E...
  • Page 183 IEEE-488 cable connections to the data system. Setting the IEEE-488 Address To configure the 600E system to communicate with a data system, you must set the IEEE-488 address of the 600E system on the Gradient Controller Pump Configuration screen as follows: 1.
  • Page 184 IEEE-488 address selection. The controller reboots and returns to the Gradient Controller Powerup screen. If you are setting up your system for the first time or you want to change one or more pump parameter values, proceed to Section 8.2, Setting Up the 600E Pump. Otherwise, proceed to: •...

  • Page 185: Setting Up The 600E Pump

    8.2 Setting Up the 600E Pump This section describes how to access and use the Pump Setup screen in Gradient Control mode. It includes the following information: • Accessing the Gradient Controller Pump Setup screen • Setting Gradient Controller Pump Setup parameters •...

  • Page 186: Accessing The Pump Setup Screen

    Figure 8-8 illustrates the steps for using the Pump Setup screen. Use Figure 8-8 as a quick reference for setting the parameters on the Pump Setup screen. Enter Flow Compensation Factor Figure 8-8 Pump Setup Flowchart 8.2.1 Accessing the Pump Setup Screen To access the Gradient Controller Pump Setup screen (Figure 8-9):...
  • Page 187 Table 8-1 Pump Setup Screen Keys Function Pump Config Displays additional configuration parameters related to the pump and controller. Lock Keyboard Locks or unlocks the keyboard. Help Displays the Help screen for the Pump Setup screen. Setting Up the 600E Pump 159...

  • Page 188: Setting Pump Setup Parameters

    8.2.2 Setting Pump Setup Parameters This section describes the pump parameters and provides procedures for setting each parameter on the Pump Setup screen. The pump parameters are: • Reservoirs to sparge • Pump col. temp. heater limit • Press limits •...
  • Page 189 3. Press Enter. Press Limits Defines the high and low operating-pressure limits of the Waters 600E pumps. Your system, column, and packing chemistry determine the low- and high-pressure limits. See the Care and Use Manual supplied with the column to determine the maximum pressure to which you can expose the column.
  • Page 190 This time delay is the system volume or delay volume. The 600E system has been optimized to reduce the delay volume. The detector signal is further delayed by the volume at the column. At a low flow rate, with a column attached, the delay between an eluent changeover instruction and its subsequent detection may be several minutes.
  • Page 191 Press Enter. Sample Gradient Table For example, your Gradient Table may appear as shown in Figure 8-10. Time Flow Curve Initial 1.00 30.00 1.00 35.00 1.00 50.00 1.00 Figure 8-10 Example of a Gradient Table Setting Up the 600E Pump 163...

  • Page 192: Exiting The Pump Setup Screen

    If you want to run your system 12 hours from now and start on Table 1, type the following in the Autostart field: Min Start Run of Table 1 6. Activate Autostart by pressing the Lock Keyboard screen key. The countdown time displays on the Pump Setup screen.

  • Page 193: Running Gradient Controller In Isocratic Mode

    Running Gradient Controller in Isocratic Mode Once you have familiarized yourself with the Waters 600E Multisolvent Delivery System and prepared it according to the procedures in Chapters 1 through 3 and 8, you may make a run in the isocratic mode.

  • Page 194: Setting Run Conditions

    • Prepared your system as outlined in Chapter 3, Preparing Your 600E System for Operation • Set operating parameters as described in Chapter 8, Setting Gradient Controller Operating Parameters 9.1 Setting Run Conditions Before you make a run with the PowerLine controller in the Isocratic mode, you must first set the run conditions.
  • Page 195 Figure 9-1 illustrates the steps involved in using the Isocratic screen. Use Figure 9-1 quick reference once you become familiar with your 600E system. Figure 9-1 Isocratic Control Flowchart Setting Run Conditions 167...

  • Page 196: Setting Pump Parameters

    Accessing the Isocratic Screen To access the Isocratic screen (Figure 9-2), press the Direct function key on the controller front panel. Figure 9-2 Isocratic Screen In addition to the parameters shown on the screen, the Isocratic screen displays the screen keys described in Table 9-1.
  • Page 197 • Sparge • Temperature Flow Rate Specifies the eluent flow rate. Note: Some columns require a flow ramp up. See the column Care and Use Manual for guidelines. Be sure that the values for the maximum and minimum operating pressures programmed on the Pump Setup screen are appropriate for your column.

  • Page 198: Setting External Event Switches

    The sparge method you use depends on your analytical requirements. Appendix B, Eluent Considerations, and Chapter 3, Preparing Your 600E System for Operation, for more information. Temperature Controls and maintains a stable column-operating temperature. This value must be less than or equal to the high-temperature limit programmed on the Pump Setup screen (see Section 8.2.3, Exiting the Pump Setup...

  • Page 199: Performing An Isocratic Run

    Connecting External Devices Before setting any of the event switches, connect the external device to the switch terminals on the rear panel of the controller. See the Waters 600E Multisolvent Delivery System Installation and Maintenance Guide for more information on these connections.

  • Page 200: Starting A Run

    9.2.2 Starting a Run Using the Rheodyne 7725i Manual Injector 1. Load the injector loop with sample. See Section 11.1.1, Using the Rheodyne 7725i Manual Injector. 2. Turn the injector handle to the Inject position to make the injection. Using a Non-PowerLine Autoinjector Note: If you are using an autoinjector, see the documentation provided with that product for information on sample loading and operation.

  • Page 201: Creating Gradient Controller Time-Based Tables

    600 controller. Each time-based table has an identification number. When the system executes a table number, the gradient and event tables with that number run simultaneously. The 600E system can store up to 15 sets of tables that allow you to: • Run a series of samples •...

  • Page 202: Documenting The Gradient Table

    10.1.1 Documenting the Gradient Table Define the information you want in a gradient table before you actually program a gradient table. This minimizes the need for you to reprogram the table later. Using the Analysis Plan and File Sheet Appendix C, Analysis Plan, contains an Analysis Plan and File Sheet to assist you in defining and documenting gradient-table information.
  • Page 203 Reducing Flow Include a final line in the gradient table to reduce the flow rate after the last injection to conserve eluent when the sample set completes. This final line in the gradient table should: • Appear as the last line in the table. •...

  • Page 204: Programming The Gradient Table

    10.1.2 Programming the Gradient Table Figure 10-3 illustrates the steps involved in using the Program Gradient screen to create a gradient table. Use this flowchart for quick reference once you become familiar with the Waters 600E system. Creating Gradient Controller Time-Based Tables...
  • Page 205 Figure 10-3 Program Gradient Flowchart Creating a Gradient Table 177...
  • Page 206 Accessing the Program Gradient Screen To display the Gradient Controller Program Gradient screen (Figure 10-4), press the Program Method function key. Figure 10-4 Gradient Controller Program Gradient Screen In addition to the gradient table parameters, the Program Gradient screen displays four active screen keys, as described in Table 10-1.

  • Page 207: Entering Parameter Values Into The Gradient Table

    Exiting the Program Gradient Screen To exit the Program Gradient screen and enter another mode, press any function key except the Program Method key. 10.1.3 Entering Parameter Values into the Gradient Table To enter the parameter values into the table displayed on the Program Gradient screen: 1.

  • Page 208: Editing The Gradient Table

    8. Repeat steps 3 through 7 for each line in the gradient. When entering information for subsequent lines in the table, enter the time value for each line and press Enter. This action copies the values from the previous line to the new line.
  • Page 209 If the new line appears at the end of the table, the values from the previous line are copied into the new line when you enter the time for that line. Edit the copied conditions as necessary. Saving Tables Whenever you change a table, you must save the changes before powering down the system.

  • Page 210: Creating An Event Table

    3. If desired, clear the table by pressing the Clear Table screen key. 4. Enter the new information. 5. When you have entered all information, save the table by pressing the Save screen key. This replaces the preexisting table with the new table in permanent memory. Deleting Tables To delete a table without replacing it with a new table: 1.
  • Page 211 2. Before you program the event table (see Section 10.2.2, Programming the Event Table), develop the table by writing each change as an individual line on the Analysis Plan and File Sheet. On each line of the Analysis Plan and File Sheet, write: •...
  • Page 212 • Waters 486 lamp status is checked at the beginning of each run. If the lamp is turned off via Event 10 at the start of a run, the system returns to IDLE and the error message appears.

  • Page 213: Programming The Event Table

    10.2.2 Programming the Event Table Figure 10-7 illustrates the steps involved in using the Program Event screen to create an Event table. Use this flowchart for quick reference once you become familiar with your Waters 600E system. Creating an Event Table 185...
  • Page 214 Figure 10-7 Program Event Flowchart Creating Gradient Controller Time-Based Tables...
  • Page 215 Accessing the Program Event Screen Press the Program Table function key to display the Program Event screen (Figure 10-8). Figure 10-8 Gradient Controller Program Event Screen In addition to the event table parameters, the Program Event screen displays four active screen keys as described in Table 10-3.

  • Page 216: Entering Parameter Values Into The Event Table

    Exiting the Program Event Screen To exit the Program Event screen, press any function key except the Program Table key to enter another mode. 10.2.3 Entering Parameter Values into the Event Table To enter the parameter values into the Program Event table (see Figure 10-8): 1.

  • Page 217: Chapter 11 Running Gradients

    If you have not performed these tasks, please take the time to do them now. 11.1 Using an Injector The Waters 600E systems supports two methods for injecting samples in the Operate Gradient mode: manual injection and autoinjection. This section provides instructions for using: •...
  • Page 218 Caution: Always follow safe laboratory practices when handling eluents. Know the physical and chemical properties of the eluents. See the Material Safety Data Sheets for the eluents in use. Caution: When using sample loops larger than 100-µL, protect yourself from the rapid ejection of mobile phase from the needle port when you turn the valve from Inject to Load.

  • Page 219: Using A Non-Powerline Autoinjector

    Injecting Sample 1. Ensure that you have connected the injector according to the instructions in the Waters 600E Multisolvent Delivery System Installation and Maintenance Guide (see Section 3.5.2, Connecting a Non-IEEE-488 Autosampler). 2. Load the sample vials into the autoinjector.
  • Page 220 Figure 11-2 summarizes the steps involved in running gradients. Use this flowchart for quick reference once you become familiar with your Waters 600E system. Figure 11-2 Operate Gradient Flowchart Running Gradients...
  • Page 221 Accessing the Initial Operate Gradient Screen To access the initial Operate Gradient screen, press the Operate Method function key. The initial Operate Gradient screen appears (Figure 11-3). Figure 11-3 Initial Operate Gradient Screen This screen displays: • Gradient and events table numbers (sets) to be run from the Operate Gradient screen •...

  • Page 222: Starting A Run

    Canceling the Run To cancel the run, press any function key, except the Operate Method key, to select another mode. 11.3 Starting a Run This section assumes that you have already set your initial operating parameters. If you have not, review Section 11.2, Setting Initial Operating Parameters, for requirements.

  • Page 223: Running A Gradient

    In addition to the current system conditions, the Operate Gradient screen displays the screen keys described in Table 11-1. Table 11-1 Second Operate Gradient Screen Keys Function Start Run Starts the gradient and the run-time clock at 0.00 minutes. Initial Starts the pump at the initial conditions of the table.
  • Page 224 To begin a run with an external non-PowerLine autoinjector: 1. Load the sample vials into the autoinjector. 2. Program and start the autoinjector. See the autoinjector manual. 3. When the autoinjector makes the injection, it sends a contact closure signal to the Inject input terminal on the rear panel of the controller.

  • Page 225: Modifying Conditions While Running

    11.4 Modifying Conditions While Running This section describes how to modify conditions during a run, including: • Changing parameters • Holding conditions constant • Stopping flow • Modifying gradient and event tables • Switching to another table • Aborting the run Note: If the keyboard is locked, unlock it by pressing the Unlock Keyboard screen key on the Pump Setup screen (see Section 8.2.3, Exiting the Pump Setup...

  • Page 226: Stopping Flow

    When you press Hold: • Gradient clock stops • Run-time clock stops 2. To continue system operation from the point at which you suspended it, press the Resume Run screen key. The gradient and run-time clocks continue from where they stopped. 11.4.3 Stopping Flow You generally use the Stop Flow screen key at the end of an analysis.

  • Page 227: Switching To Another Table

    To modify a table during a run: 1. Press the Program Method function key to display the gradient table or the Program Table function key to display the event table. 2. Move the cursor to the Table # field and type the number of the table to modify. Press Enter.

  • Page 228: Aborting The Run

    11.4.6 Aborting the Run Using the Direct Function Key 1. Press the Direct function key. The Caution screen appears (Figure 11-5). The Caution screen prompts you to immediately abort the gradient or cancel the abort. Figure 11-5 Caution Screen 2. Take one of the following actions: •...

  • Page 229: Appendix A Specifications

    Appendix A Specifications This appendix contains 600E system specifications for the following areas: • Operational • Electrical • Environmental • Physical • Optional Rheodyne 7725i manual injector Table A-1 Operational Specifications Item Specification Number of eluents One to four. Modes of operation...
  • Page 230 Table A-1 Operational Specifications (Continued) Item Specification Program storage Storage for 15 sets of tables (gradient, program event, and detector), with a maximum of 15 steps per table. Storage for a time-based multi-method program with up to 48 individual steps. EEPROM stores setup parameters and tables, and preserves memory indefinitely following power loss or extended shutdown.
  • Page 231 Table A-2 Electrical Specifications Item Specification Power Requirements Maximum power: 250 VA Frequency 47 to 63 Hz Fuse Nominal Voltage Fuse Fuse Voltage Range (North America) (Europe) 2 A, 250 V 1.6, 250 V UL/CSA, IEC, Time Time Delay Delay 2 A, 250 V 1.6, 250 V UL/CSA,...
  • Page 232 Receives a signal from an external injector (autosampler or manual injector) to initiate the chromatographic run. The Inject terminal also provides a signal to start a Waters 745B/746 Data Module (integrator). The Inject terminal accepts signals from several outputs, including TTL signals, open collector outputs, and contact closures.
  • Page 233 Table A-4 Physical Specifications Item Specification Wetted Surface Material 316 stainless steel, ruby, sapphire, fluorocarbon polymer Controller Height: 7.19 inches (18.26 cm) Depth: 21.75 inches (55.25 cm) Width: 11.32 inches (28.75 cm) Weight: 33 lb (15 kg) Pump Height: 9.625 inches (24.4 cm) Depth: 20.5 inches (52.1 cm) Width: 11.125 inches (28.3 cm) Weight: 60.2 lb (27.3 kg)
  • Page 234 Specifications...

  • Page 235: Appendix B Eluent Considerations

    The Waters 600E System is constructed of high-quality, 316 stainless steel components that, with some minor restrictions, can be used with all eluents. This section lists the eluents that have, and have not, been approved for use with the 600E System.
  • Page 236 Materials of construction used in the 600E system are nonreactive with most acids, bases, salts, and organic eluents. The following list of eluents has been approved for use with the 600E system. These include salts, acids and bases in concentrations up to 1 M (unless otherwise noted), and organic eluents in concentrations of up to 100% (unless otherwise noted).
  • Page 237 Tartrate • Trilithium citrate • Tris • 4-(2-pyridylazo)resorcinol monosodium salt monohydrate Acids The following is a list of acids that may be used with the 600E system: • Acetic acid, glacial • Benzoic acid • Chromic acid • Citric acid •...
  • Page 238 • NaOH, up to 10 M • OH, up to 3 M • Tetramethylammonium hydroxide pentahydrate Organic Eluents The following is a list of organic eluents that may be used with the 600E system: • 4-cyanophenol • Acetone • Acetonitrile •...

  • Page 239: Clean Eluent

    Phenol • Tetrahydrofuran (THF) • Toluene • Waters PIC Reagents • Xylene B.2 Clean Eluent Using Clean Eluents Use clean eluents to obtain reproducible results and for operation with minimal maintenance. An unclean eluent can cause baseline noise and drift. Purchase only the highest quality HPLC-grade eluents.

  • Page 240: Eluent Miscibility

    Using Clean Filters The 600E system contains an eluent filter. To avoid drawing foreign particles into the pump where they can accumulate and affect pump operation, the eluent reservoir filter should be kept clean.

  • Page 241: Eluent Properties Table

    • When using a high-ionic-strength buffer, flush all fluid pathways with distilled water before shutting down the system. Leave distilled water in the system (flush with 10% methanol in water for shutdowns scheduled to be more than one day). See Section 2.5, Powering Down the System.

  • Page 242: Using Miscibility Numbers (M-Numbers)

    Table B-1 Physical Properties of Eluents (Continued) Polarity Viscosity [η] CP, Boiling Point °C Miscibility Eluent Index 20 °C (1 atm) Number (M) Cyclohexanone 2.24 155.7 Nitrobenzene 2.03 210.8 14, 20 Benzonitrile 1.22 191.1 15, 19 p-Dioxane 1.54 101.3 Ethanol 1.20 78.3 Pyridine...

  • Page 243: Head Height

    B.4 Head Height The 600E system allows you flexibility in the placement of the eluent reservoirs. Ideally, the eluent elevation should be close to that of the pump heads or higher. Avoid placing eluents on top of the system unless the bottles are in a container that can hold the total volume of all of the eluents in case bottle leakage occurs.

  • Page 244: Eluent Degassing

    For example, a 1:1 mixture of water and methanol produces twice the pressure of either water or methanol alone. If the extent to which the pressure changes affect the analysis is not known, monitor the pressure during the run using the controller Chart output terminal provided for this purpose (select %A or %B).
  • Page 245 Temperature Temperature affects the solubility of gases in two ways: • The higher the boiling point of a gas, the more soluble the gas is in a given eluent. • Increasing the temperature of the gas-liquid solution affects the percentage of gas in solution.

  • Page 246: Eluent Degassing Methods

    Sparging combines the convenience of short initial degassing time, ease of maintaining the eluent condition during operation, and complete control within the framework of the 600E system. Sparging Sparging, or bubbling a gas through eluent, removes unwanted gas from solution while saturating the eluent with the sparging gas.
  • Page 247 Heat Heating to remove dissolved gas is usually not effective unless you boil the eluent, and this is not practical for mixed eluents. However, low levels of heat will raise the partial pressure of the eluent and thereby reduce the rate of resolubilization of a gas. This may affect the separation on the column.
  • Page 248 Eluent Considerations...

  • Page 249: Appendix C Analysis Plan

    Appendix C Analysis Plan Use the Analysis Plan and File Sheet that follows to help you define and document: • The gradient, event, and detector tables that compose a method table in PowerLine Control mode (see Chapter 6, Creating PowerLine Methods) •...
  • Page 250 Analysis Plan and File Sheet Analysis Name:___________________________ Memory Location (Table Number):____ Gradient Table Event Table Detector Table 410 Sensitivity Time Flow Curve Time Event Action 431/432 Sensitivity Time Det Chan Sens AUFS Choice of Gradient Curves: Choice of Events: Go to end condition 1-4 = Switches 1-4 immediately 5 = Alarm...

  • Page 251: Index

    Index Numerics 600E System, features 1–2 Cancelling a run 139, 140, 141, 600S Controller, See Controller Changing eluents 41–44 parameters Chart out 68, Column heater, setting temperature 67, 90, Aborting a run 146–148 160, Accessing the Pump Setup Screen Communications...
  • Page 252 downloading parameters eluent composition event switches Daily operation flow rate Data channel injection volume Data system overview communicating with 154–156 pump parameters 88–90 Degassing 28–30, 216–219 run conditions 86–94 Deleting lines in a table run time Detector Table running a method from creating 119–124 running in...
  • Page 253 compatibility 207–211 immiscible incompatible Gas dissolution 216–218 miscibility 28, 212–215 Good operating practices organic Gradient properties 213–214 aborting a run sparging 28–30 cancelling a run unacceptable changing parameters using clean completing viscosity holding conditions constant Equilibrating the system 38–40, 97, modifying conditions 197–200 Error messages, clearing...
  • Page 254 Gradient Table equilibrating the system creating 102–111, 173–182 event switches curve profile 109, flow rate description pump parameters 168–170 documenting 103–105, 174–176 run requirements editing 109–111, 180–182 running in 171–172 entering parameter values 108–109, sparging 179–180 stopping the pump example 104, 163, Isocratic screen initial conditions line 103, exiting...
  • Page 255 function keys starting with a non-Powerline autoinjector IEEE-488 interface starting with an Autosampler RS-232 interface stopping flow 144, setting up 47–60 Method Table unit type clearing tables verifying active devices 61–62 creating 124–131 PowerLine Controller Program Event screen, deleting lines screen keys description PowerLine Controller Program Gradient...
  • Page 256 Pump holding conditions constant Auto•Blend modifying conditions 143–148 description 3, 6–8 modifying tables 145–146 flow factor 68, 70, 162, starting with a manual injector flow rate 1, 89, 108, 169, starting with a non-PowerLine head volume autoinjector pressure 1, 40, 67, starting with an Autosampler priming 28, 31–34...
  • Page 257 PowerLine Controller Pump Setup 52, PowerLine Program Event Vial codes 92, 128–129 PowerLine screen layout Viscosity Program Methods Pump Setup System Configure Screw terminals Water, using clean Aux +12 V Wavelength Chart WISP 712D Hold Pressure Sensitivity Sparging eluents 28–30, flow rate 28, in Direct Control mode in Isocratic Control mode...
  • Page 258 Index...

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