Waters 2690 Quick Start Manual

W aters 2690
Separations Modul e
Quick Star t Guid e
34 Maple Street
Milford, MA 01757
WAT553-03TP, Revision 3
NOTICE
The information in this document is subject to change without notice and should not be construed as a commitment by Waters Corporation. Waters Corporation assumes no responsibility for any errors that may appear in this document. This manual 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 manual.
© 1996, 1998, 2000 WATERS CORPORAT ION. PRINTED IN THE UNITED STATES OF AMERICA. ALL RIG H TS RESERVED. THIS BO OK OR PARTS THERE OF MAY NOT BE REPRODUCED IN ANY FORM WITHOUT THE WRITTEN PERMISSION OF THE PUBLISHER.
Alliance , M il len n iu m, an d Waters are t r ad emar k s o f Waters Corpor at io n . All other trad em a rk s a re the sol e p r op er ty of thei r re s pe ctive owners.
Quick Summary
The figure below summarizes the information contained in this Quick Start Guide. Use it as a reference after you have read the entire document.
Start
Power on the
Separations
Module
Configure the
Separations
Module
Degas or
Sparge Eluents
Prime the Solvent
Management
System
Prime the Plunger
Seal Wash Pump
(If Insta lle d )
Purge the Sample
Management
System
Prime the Needle
Was h Pum p
Adjust the Seal Pack
Load the
Carousels
Perform
an Automatic
Run?
Yes
Press the
Samples
on the Main Screen
Select the Separation
Method, Sample Set , or
Template to Run, then
Press
Enter Data Required by the Separation Method,
Sample Template
Press the Screen Key to Start
Screen Key
Screen Key
Run
Sample Set, or
the Run
Run
Routine
No
Set Flow Rate and
Composition
Set Sparge Rate
(if Applicable)
Set Control
Switches
Direct
Press
Function
Screen Key
Select Direct
Function to Perform
Enter Function
Parameters
The Function
Begins to Run
The Run Ends as
Programmed
Conventions Used in This Guide
This Quick Start Guide uses the following conventions:
• Bold text indicates user input or action. For example, press
• When you are instructed to “press the X key”, pre ss the indica ted keypad k ey.
• When you are instructed to “press the X screen key,” press the keypad key directly below the key name displayed on the screen.
Notes and Warnings
This guide uses the following note and warning conventions:
• Notes call out information that is important to the operator. For example:
Record your result before you proceed to the next step.
Note:
• Attentions provide information about preventing possible damage to the system or equipment. For example:
Enter
.
STOP
Attention:
cell window.
• Cautions provide information essential to the safety of the operator. For example:
Caution:
laboratory practices when you operate your system.
Caution:
cord from the rear panel of the instrument before you perform the procedures in this section.
To avoid damaging the detector flow cell, do not touch the flow
To avoid chemical or electrical hazards, always observe safe
To avoid electrical shock and possible injury, remove the power
1

Introduction

The
Waters 2690 Separations Module Quick Start Guide
features of the Waters 2690 Separations Module and describes how to make a run.
Who Should Use This Guide?
This guide is intended for both novice and experienced chromatographers who need to operate the Waters 2690 Separations Module.
What Is In This Guide?
The
Waters 2690 Separations Module Quick Start Guide
information to help you set up the Waters 2690 Separations Module and make a run. In addition, this guide contains detailed flow charts that provide Waters-recommended steps to prime, equilibrate, and purge both degasser and sparge-based 2690 Separations Modules. Refer to Chapter 6,
This guide is not designed to teach you chemistry and does not contain background
Note:
or reference information.
Recommended Preparation Procedures .
introduces you to the basic
contains basic procedural
For additional information, or if you want to learn how to modify any of the procedures in this guide, refer to the
With the purchase of the 2690 Separations Module, Waters supplies both this guide
Note:
and the Waters 2690 Separations Module Operator’s Guide in electronic format on a CD-ROM. To install and view these guides on your computer, refer to the Readme file on the CD-ROM. To purchase a printed version of the Operator’s Guide, contact W aters Sales Support at 800-252-4752, extension 8101.
Waters 2690 Separations Module Operator’s Guide
.
Before You Begin
This guide assumes that:
• Your system is properly installed (refer to the
Operator’s Guide
• Your separation methods, sample sets, and/or sample templates are already created and stored (refer to the Chapter 6, Creating Methods, Sample Sets, and Sample Templates).
, Chapter 2, Installing the Separations Module).
Waters 2690 Separations Module Operator’s Guide
Waters 2690 Separations Module
Introduction 5
,
System Description
The Waters™ 2690 Separations Module (Figure 1-1) is an integrated solvent and sample management platform. This integration of two traditional high performance liquid chromatography (HPLC) components streamlines all critical separation functions.
Solvent Bot tle Tray
Detector Drip Tray
Fr ont P anel Displa y
and Keyboard
Floppy Disk Drive
Sample
Compartment
Access Door
Solvent Delivery
Tray Access Door
Syringe Access Door
Column Heater Module
Solvent Conditioning
Tray Access Door
TP01354
Figure 1-1 Waters 2690 XE Separations Module (Front View)
The sample management system in the Waters 2690 Separations Module uses five carousels with a total capacity of 120 vials. A carrier rotates the carousels to the injection station in the sample compart men t.
The Waters 2690 Separations Module is available from Waters in a number of configurations, differing from each other by the options that are included.
The two primary configurations are designated:
2690
• helium sparge for solvent conditioning, integral plunger seal-wash system, 120-vial capacity sample management system, liquid-crystal display and keyboard user interface, and floppy disk drive.
2690 XE
• sparge system with a four-channel in-line vacuum degasser , and adds a column heater and a sample heater/cooler.
6 Introduction
– Provides quaternary solvent, high-performance solvent delivery, integral
– Provides the capabilities of the 2690 base product, replaces the helium

2 Preparing the Se parations Module for Operation

Before you can prepare the Separations Module for operation, you need to power on the
2690 Separations Module by moving the power switch (located at the top of the left side
panel) to the I (On) position. The startup diagnostics routine begins.

2.1 Powering On

Startup Diagnostics
The startup diagnos tics routine performs the following functions and tests:
• CPU board
• Memory (RAM and ROM)
• Keypad
•Display
• External communicat ion
• Digital signal processor (DSP)
• Floppy disk drive
Once the electronic part of the diagnostics test is complete, the front-panel screen
displays the results of the tests, as shown in Figure 2-1
STARTUP DIAGNOSTICS CPU
ROM RAM KEYPAD
Figure 2-1 Diagnostic Test Results Screen
OK OK OK OK
DISPLAY DMA GPIB FLASH
OK OK OK OK
Preparing the Separations Module for Operation 7
.
DSP FLOPPY CLOCK
OK OK OK
The Main Screen
When the initial part of the start up diag nos tics routine is successful, the Main screen
appears in the front panel display (Figure 2-2
by initializing the:
• Needle, syringe, and valves
• Carousel carrier
• Solvent management system
The statuses of these mechanical diagnostics tests appear in the banner area of the Main
screen (Figure 2-2
not successful, refer to the
) while the diagnostics are running. If the startup diagnostics routine is
Waters 2690 Separations Module Operator’s Guide
8.5, Troubleshooting. When the startup diagnostics routine is complete, the Separations
Module enters the Idle mode.
Banner Area
Data Area
). The startup diagnostics routine cont inues
, Section
Screen Keys
Figure 2-2 Main Screen
8 Preparing the Separations Module for Ope ration

2.2 Configuring the Separations Module

Before you can operate the Separations Module, you need to configure the Separations
Module for stand-alone or remote control and for a variety of other operating parameters.
No Interaction Mode
In this standalone mode, the Separations Module is not connected to the IEEE-488
interface bus. The Separations Module controls other non-IEEE devices in the HPLC
system using the I/O connections on the rear panel. Refer to the
Module Operator’s Guide
make I/O connections. Use this mode if you want to suspend communication with a
connected Millennium Chromatography Manager workstation and operate the Separations
Module and the other HPLC system components from their front panels.
To set the Separations Module to the No Interaction mode:
, Section 2.7.1, I/O Signal Connections, for the procedure to
Waters 2690 Separations
1. Press the (Figure 2-3
2. Select the
3. Sel ect
4. Press
Config
No interaction
Exit
screen key in the Main screen. The Configuration screen appears
).
System
.
field, then press
, then press
Enter
Enter
to display a list of choices.
.
System Controller Mode
In this standalone mode, the Separations Module controls up to three detector channels on the I EEE-488 b us. This can include two UV detector channels (Waters 2487 and/or 486 Tunable Absorbance Detectors) and one RI detector channel (Waters 2410 or 410 Differential Refractometer). You can also control other HPLC modules using the I/O connections.
To set the Separations Module to the System Controller mode:
1. Press the (Figure 2-3
Config
).
screen key in the Main screen. The Configuration screen appears
Preparing the Separations Module for Operation 9
Figure 2-3 Configuration Screen
2. Select the
3. Sel ect
System Controller
4. Press the
System
field, then press
Detectors
, then press
screen key. A list of active devices (with their IEEE-488
Enter
to display a list of choices.
Enter
.
interface bus addresses) appears.
a. Press the
Scan
screen key to update the list.
b. P ress t he OK screen key to return to the Configuration screen.
5. Press
Exit.
The Separations Module is ready to control Waters detectors using
separation methods, sample sets, or sample templates.
Controlled by Millennium32 Mode
In this remote-control mode, a Millen nium Ch romat ography Manager work station r unning Millenn iu m system using the IEEE-488 interface bus.
To set the Separations Module to the Controlled by Millennium
1. S ele ct the
2. Select
3. Press
4. Select an address that is unused by other chromatographic components connected
5. Press
32
software (Windows 95, 98, or NT) controls the operation of your HPLC
32
mode:
System
field in the Configuration screen, then press
Enter
list of choices.
Controlled by Millennium
32
, then press
Enter
. The IEEE 488 Address
field is highlighted.
Enter
to display a list of addresses.
to the Millennium C hromatography Manager workstation, then press
Exit.
The Separations Module is ready to be controlled from the
Millennium Chromatography Manager workstation.
to display a
Enter
.
10 Preparing the Sepa rations Module for Operation
Controlled by MassLynx Mode
In this remote-control mode, Micromass MassLynx NT software (Version 3.1 Build 004 or higher) controls the 2690 Separations Module. MassLynx software is used with Micromass mass spectrometry (MS) detectors, using the IEEE-488 interface between the Micromass computer and the 2690 Separations Module.
To set the Separations Module to the Controlled by MassLynx mode:
1. S ele ct the list of choices.
2. Select is highlighted.
3. Press
4. Select an address that is unused by other chromatographic components connected to the Micromass computer, then press
5. Press computer.
System
Controlled by MassLynx
Enter
Exit.
The Separations Module i s r eady to be controlled from the M ass Lynx
field in the Configuration screen, then press
, then press
to display a list of addresses.
Enter
Enter
.
. The IEEE 488 Address field
Enter
to display a
Controlled by Millennium 2.xx Mode
In this remote-control mode, a Millen nium Ch romat ography Manager work station r unning Millennium 2.xx soft ware (Wi ndows 3 .1) cont rols the oper ati on of y our HPLC syst em using the IEEE-488 interface bus.
To set the Separations Module to the Controlled by Millennium 2.xx mode:
1. S ele ct the list of choices.
2. Select field is highlighted.
3. Press
System
Controlled by Millennium 2.xx
Enter
field in the Configuration screen, then press
, then press
to display a list of address pairs.
Ente r
Enter
to display a
. The IEEE 488 Address
4. Select an address pair that is unused by other chromatographic components connected to the Millennium Chromatography Manager, then press
5. Press
The Separations Module appears as two devices in the Millennium System view:
Exit.
The Separations Module is ready to be controlled from the
Millennium Chromatography Manager workstation.
The solvent and sample manageme nt systems The optional sample heater/cool er
– With an odd address.
Preparing the Separations Module for Operation 11
– With an even address.
Enter
.
Refer to the Automatic Runs Under Millennium Control, for details on making runs under Millennium control.
Waters 2690 Separations Module Operator’s Guide
, Section 5.2, Making
Controlled by Operate Gradient by Event In
In the Operate Gradient by Event In mode, an external autosampler (a Waters 2700 Sample Manager, for example) signals the Solvent Management System of the Separations Module to begin a gradient. In this mode, the Separations Module has no
can
control of IEEE-488 devices, however, the Separations Module devices using the I/O connections on the rear panel.
To set the Separations Module to the Operate Gradient by Event In mode:
control non-IEEE
1. S ele ct the list of choices.
2. Select
3. Press the more detailed steps on defining Events In conditions, refer to the
Separations Module Operator’s Guide
Setting Configuration Parameters.
4. Set the Stop Flow field to the appropriate condition ( press
• Choose
• Choose
• Choose
5. Set the Hold 1 field to the appropriate condition (
• Choose
• Choose
System
Operate Gradient by Event In
Events In
Enter
not used.
Stop Flow I/O terminals of the Separations Module changes to a high (more positive) TTL-level.
Flow I/O terminals of the Separations Module changes to a low (more negative) TTL-level.
Hold 1 Inject terminals of the Separations Module changes to a high (more positive) TTL-lev el to initiate a chromatographic run (and prevent an injection by the Separations Module).
1 Inject terminals of the Separations Module changes to a low (more negative) TTL-level to initiate a chromatographic run (and prevent an injection by the Separations Module).
field in the Configuration screen, then press
, then press
screen key to display the Events In dialog box. If you need
Events In
,
.
Ignore
High
Low
High
Low
if the Stop Flow I/O terminals of the Separations Module are
if the output connection from the external autosampler to the
if the output connection from the external autosampler to the Stop
if the output connection from the external autosampler to the
if the output connection from the external autosampler to the Hold
Enter
.
discussion, Section 3.2.1,
Ignore, High
High
or
Low
Enter
to display a
Waters 2690
Low
, or
), then press
), then
Enter
.
If you are configuring the Separations Module with a Waters 2700 Sample
Note:
Manager, choose
12 Preparing the Sepa rations Module for Operation
Low
.
6. Set the Logic field to Or, then press
7. Set the Hold 2 field to
8. Press the OK screen key to save your selections and exit from the Events In dialog box.
Ignore
, then press
Enter
.
Enter
.
Controlled via RS-232 (ASCII) or (Binary) Modes
In these remote-control modes, a non-Waters data system (a mass spectrometry system, for example) controls the Separations Module using RS-232 ASCII or binary communications. The Separations Module disconnects from the IEEE-488 interface bus when either of these modes is selected. The Separations Module can control other non-IEEE devices in the HPLC system using the I/O connections on the rear panel.
To set the Separations Module to the Controlled via RS-232 (ASCII) or (Binary) mode:
1. S ele ct the list of choices.
2. Select press
3. Press system using RS-232 communications.
System
Cont roll e d vi a RS23 2 (ASCI I )
Enter
Exit.
The Separations Module is ready to be controlled by a remote data
field in the Configuration screen, then press
.
Controlled via RS232 (Binary),
or
Enter
to display a
Setting Report Options
Use the Report Options dialog box to define the information that is sent to the printer, integrator, and/or floppy disk. (Before you print a report, select the printer in the Printer section of the Configuration screen. You select the destination of the repor t in the print dialog box that appears when you press the Print screen key. )
To define the information sent to a printer, integrator, and/or floppy disk:
1. Press the Options dialog box (Figure 2-4
Reports
screen key on the Configuration screen to display the Report
).
then
Preparing the Separations Module for Operation 13
Figure 2-4 Report Options Dialog Box
2. Select the destination for the report in the drop-down list.
3. Select any option and press any numeric key to enable or disable the option, then press include:
Gradient ta ble
I/O event ta bl e
Detector table
Event overview
Misc. parameters
System config
Per-inject data
• values for temperature, pressure, the time and date of each injection, and so on.
Alarms
4. Press the OK screen key to exit from the Report Options dialog box.
5. Press
Enter
. An “X” in the box means the option is enabled. The options
– Generates the gradient table
– Generates the I/O events table
– Generates the detector table
– Generates an overview of all merged tables
– Generates a list of all parameters not included in tables – Generates a list of the instrument configuration parameters – Generates a list of the minimum, maximum, and average
– Generates a list of the error conditions that occurred during the run
Exit
to return to the Main scr ee n
Programming for Auto Shutdown
You can set up the Separations Module to shut down automatically after a specified period of inactivity. Inactivity is defined as:
• No keyboard use
• No injections performed
14 Preparing the Sepa rations Module for Operation
• No changes sent to the Separations Module from a remotely connected Millennium Chromatography Manager workstation, MassLynx computer, or external autosampler
• An error condition that suspends the operation of the Separations Module
You can leave the Separations Module in the shutdown state indefinitely. The separation method you specify in the Auto Shutdown dialog box defines the initial conditions that are applied after the specified period of inactivity. Use the auto shutdown function:
• When there is a long delay between injections
• To minimize solvent flow after an unattended or long run
• To minim ize sparge gas consumption
• To disable the vacuum degasser
• To disable temperature controls
• To turn off detector lamps
To enable the auto shutdown function:
1. Press the
Config
screen key in the Main screen, then press the
More
screen key
once.
2. Press the (Figure 2-5
Auto Shutdown
).
screen key. The Auto-Shutdown dialog box appears
Figure 2-5 Auto-Shutdown Dialog Box
3. Select the separation method to be used while the Separations Module is shut down. Only the
initial
conditions in the method you select are used.
Preparing the Separations Module for Operation 15
4. Enter a time period (in minutes) after which you want the Separations Module to shut down (or press
5. Press
6. Press
Note:
OK.
The Separations Module shuts down when there has been no activity
for the specified period.
Exit
to return to the Main screen.
If you want to use Auto Shutdown to turn off the lamp of a 2487 or 486 detector,
Clear
to disable the Auto Shutdown function).
program a Lamp Off event and specify a time of INIT in the I/O Events Timed Table screen (see Section 6.2.5, Setting I/O Parameter Value s in the Waters 2690 Separations Module Operator’s Guide).
16 Preparing the Sepa rations Module for Operation

2.3 Preparing the Solvent Management System

For optimal performance of your Separations Module, perform the steps identified in
Figure 2-6
Note:
Modules for operation, refer to
.
For details on how to prepare both degasser and sparge-based 2690 Separations
Chapter 6, Recomme nded P reparation Procedures
Start
.
Degas or Sparge
Solvents
Prepare Solvent
Reservoirs
Figure 2-6 Preparing the Solvent Management System for Operation
Caution:
Observe safe laboratory practices when you handle solvents. Refer to the
Material Safety Data Sheet for each solvent you use.

2.3.1 Degassing S olvents

In-Line Vacuum Degassing
Prime the Solv ent
Management
System
Prime the Plunger
Seal Wash Pump
Solvent
Management
System is Ready to
Operate
In-line vacuum degassing reduces the total dissolved gas in the mobile phase. For more information on vacuum degassing, refer to Section 1.5, the “Degasser Considerations” discussion in the
Waters 2690 Separations Module Operator’s Guide
Preparing the Separations Module for Operation 17
.
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