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W aters 717plus A utosampler
Operator’s Manual
34 Maple Street
Milford, MA 01757
173-02TP, Revision 2
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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.
1993 WATERS CORPORATION. PRINTED IN THE UNITED STATES OF AMERICA.
ALL RIGHTS RESERVED. THIS BOOK OR PARTS THEREOF MAY NOT BE
REPRODUCED IN ANY FORM WITHOUT THE WRITTEN PERMISSION OF THE
PUBLISHER.
LAC/E, PowerLine, and Waters are trademarks of Waters Corporation.
Millex is a trademark of Millipore Corporation.
Torx is a trademark of Camcar, Division of Textron, Inc.
The quality management systems of Waters manufacturing facilities comply with
the International Organization for Standardization International Standard ISO 9001
Quality Management and Quality Assurance Standards. Waters quality
management systems are periodically audited by the registering body to ensure
compliance.
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STOP
Attention: The Waters 717plus Autosampler may be used for IN VITRO diagnostic
STOP
applications. This is a highly sensitive instrument. Read the accompanying operator's
manual before using.
When using 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 take steps to determine the
reason for the changes. Until you determine the cause of a change, do not rely upon the
results of the separations.
Attention: Changes or modifications to this unit not expressly approved by the party
STOP
responsible for compliance could void the user’s authority to operate the equipment.
STOP
Attention:
This equipment has been tested and found to comply with the limits for a Class
A digital device, pursuant to P art 15 of the FCC rules. These limits are designed to provide
reasonable protection against harmful interference when the equipment is operated in a
commercial environment. This equipment generates, uses, and can radiate radio
frequency energy, and, if not installed and used in accordance with the instruction manual,
may cause harmful interference to radio communications . Operation of this equipment in a
residential area is likely to cause harmful interference, in which case you must correct the
interference at your own expense.
Shielded cables must be used with this unit to ensure compliance with the Class A FCC
limits.
Caution: For continued protection against fire hazard, replace fuses with those of the
same type and rating.
Caution:
To avoid the possibility of electric shock, do not remove the power supply co vers .
The power supply does not contain user-serviceable components.
Attention: To meet the regulatory requirements of immunity from external electrical
disturbances that may affect the performance of this instrument, do not use cables longer
than 9.8 feet (3 meters) when you make connections to the screw-type barrier terminal
strips. In addition, ensure you always connect the shield of the cable to chassis ground at
one instrument only.
The Installation Category (Overvoltage Category) for this instrument is Level II. The Level
II category pertains to equipment that receiv es its electrical power from a local level, such
as an electrical wall outlet.
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Canadian Emissions Notice
This digital apparatus does not exceed the Class A limits for radio noise
emissions from digital apparatus set forth in the Radio Interference
Regulations of the Canadian Department of Communications.
Le présent appareil numérique n’émet pas de bruits radioélectriques
dépassant les limites applicables aux appareils numériques de la classe A
prescrites dans les règlements sur le brouillage radioélectrique édictés par le
Ministère des Communications du Canada.
Symbols Used on 717plus Autosampler
Direct current
Alternating current
Protective conductor
terminal
Frame or chassis terminal
Caution, risk of electric
shock (high voltage)
Caution or refer to
manual
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Table of Contents
How to Use This Manual................................................................... 15
Chapter 1
Introduction ...................................................................................... 18
1.1 Description............................................................................ 18
1.2 Features................................................................................ 19
1.3 Components and Subsystems.............................................. 21
Chapter 2
Installation ....................................................................................... 23
2.1 Site Requirements ................................................................ 23
2.2 Unpacking and Inspection..................................................... 25
2.3 Changing Voltage Configuration ........................................... 26
2.4 Connecting Fluid and Drain Lines ........................................ 29
2.5 Connecting Communication Cables ..................................... 32
2.5.1 Making Terminal Strip Connections........................... 33
2.5.2 Making IEEE-488 Network Connections.................... 39
2.5.3 Connecting RS-232 Output to Data Module.............. 40
2.6 Changing the Hardware Configuration.................................. 41
2.6.1 Removing/Replacing the 717plus Cover.................... 41
2.6.2 Installing the Heater/Cooler....................................... 44
Table of Contents 5
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2.6.3 Installing the Large Sample Loop.............................. 47
Chapter 3
Startup and Configuration ................................................................ 50
3.1 Powering Up the Autosampler............................................... 50
3.2 Using the Front Panel ........................................................... 51
3.2.1 Accessing Menus....................................................... 52
3.2.2 Entering Operating Parameters................................. 54
3.3 Flushing the Autosampler..................................................... 54
3.4 Calibrating the Seal Pak........................................................ 54
3.4.1 Purging the Autosampler........................................... 55
3.4.2 Auto Zeroing the Transducer...................................... 55
3.4.3 Calibrating the Seal Pak ............................................ 56
3.5 Priming the Needle Wash Pump........................................... 59
3.6 Configuring the Autosampler ................................................ 60
3.6.1 Overview of Configuration ......................................... 60
3.6.2 Setting Parameters for LC System Operation............ 63
3.6.3 Entering Hardware Changes ..................................... 67
3.7 System Verification................................................................ 69
3.8 Power Down and Storage..................................................... 70
3.8.1 Removing Buffered Mobile Phase............................. 70
3.8.2 Powering Down.......................................................... 70
3.8.3 Storage...................................................................... 71
6 Table of Contents
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Chapter 4
Operating the Autosampler .............................................................. 72
4.1 Overview of Operation.......................................................... 72
4.2 Preparing Samples ............................................................... 74
4.2.1 Preparing Samples.................................................... 74
4.2.2 Selecting Sample Vials.............................................. 76
4.3 Selecting a Needle Wash Solvent......................................... 77
4.4 Loading the Carousel............................................................ 79
4.5 Ensuring Reproducibility....................................................... 81
4.5.1 Overview of Reproducibility....................................... 81
4.5.2 Performing a Purge.................................................... 81
4.5.3 Performing a Compression Check............................. 84
4.6 Running Autosampling.......................................................... 87
4.6.1 Programming Auto Run ............................................. 88
4.6.2 Programming Step Functions.................................... 92
4.6.3 Using Auto Standards ............................................... 94
4.6.4 Using Auto Addition .................................................. 99
4.6.5 Using Auto Transfer ................................................. 103
4.6.6 Programming the Event Output............................... 110
4.6.7 Starting and Stopping an Auto Run......................... 111
4.6.8 Monitoring Auto Run Status..................................... 112
4.7 Making a Stat Run .............................................................. 113
4.8 Sampling Considerations.................................................... 116
4.8.1 Temperature Control................................................ 116
4.8.2 Microbore/Semiprep Injections................................ 117
Table of Contents 7
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4.8.3 Injecting Viscous Samples ...................................... 120
4.8.4 Purging During an Auto Run.................................... 121
4.8.5 Using Buffered Mobile Phase.................................. 122
Chapter 5
Maintenance .................................................................................. 124
5.1 Defrosting the Heater/Cooler.............................................. 124
5.2 Replacing the Syringe......................................................... 126
5.2.1 Removing the Syringe ............................................. 126
5.2.2 Installing the New Syringe....................................... 129
5.3 Replacing the Seal Pak....................................................... 132
5.3.1 Removing the Injector.............................................. 133
5.3.2 Removing the Seal Pak ........................................... 134
5.3.3 Replacing the Needle .............................................. 135
5.3.4 Installing a New Seal Pak........................................ 136
5.3.5 Installing the Injector................................................ 137
5.3.6 Calibrating the Seal Pak .......................................... 137
5.4 Replacing In-Line Filters..................................................... 138
Chapter 6
Troubleshooting ............................................................................. 141
6.1 Safety and Handling............................................................ 141
6.2 Error Messages................................................................... 142
6.2.1 Informational Error Messages.................................. 143
6.2.2 Calibration (CAL) Error Messages........................... 143
8 Table of Contents
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6.2.3 Carousel (CAR) Error Messages............................. 144
6.2.4 Heater/Cooler (H/C) Error Messages ...................... 146
6.2.5 Injector (INJ) Error Messages.................................. 146
6.2.6 Syringe (SYR) Error Messages ............................... 147
6.3 Troubleshooting Tab les........................................................ 147
6.4 Troubleshooting Procedures ............................................... 155
6.4.1 Manual Syringe Purge............................................. 155
6.4.2 V alve Leak Test........................................................ 156
6.4.3 Manual Transducer Adjustment ............................... 159
Appendix A
Specifications ................................................................................. 162
Appendix B
Spare Parts..................................................................................... 165
Appendix C
Warranty Information...................................................................... 169
C.1 Limited Product Warranty................................................... 169
C.2 Shipments, Damages, Claims, Returns.............................. 172
Appendix D
Reproducibility and Solvent Degassing.......................................... 174
D.1 Factors Affecting Reproducibility........................................ 174
D.1.1 Chemical Factors Affecting Reproducibility............. 174
Table of Contents 9
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D.1.2 Instrument Factors Affecting Reproducibility........... 175
D.2 Solvent Degassing.............................................................. 176
D.2.1 Theory of Solvent Degassing .................................. 176
D.2.2 Solvent Degassing Methods.................................... 177
D.2.3 Solvent Degassing Considerations.......................... 178
Appendix E
Selecting Sample Vials................................................................... 180
Index .......................................................................................... 182
10 Table of Contents
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List of Figures
1-1 Waters 717plus Autosampler......................................................... 18
1-2 Waters 717plus Autosampler Subsystems.................................... 22
2-1 Waters 717plus Autosampler Site Requirements.......................... 24
2-2 Fuse Block and Voltage Selector Card .......................................... 26
2-3 Voltage Selector Card.................................................................... 27
2-4 Removing the Fuse Block..............................................................28
2-5 Fuse Installation............................................................................. 28
2-6 Fluid Line Connections..................................................................30
2-7 Drain Line Connections ................................................................. 32
2-8 Autosampler Rear Panel................................................................ 33
2-9 Terminal Strip................................................................................. 36
2-10 IEEE-488 Connections ................................................................. 40
2-11 Removing the Autosampler Cover................................................. 43
2-12 Installing Heater/Cooler.................................................................45
2-13 Connecting the Heater/Cooler Power Cord and Temperature
Probe.............................................................................................46
2-14 Installing the Temperature Probe................................................... 47
2-15 Disconnecting the Sample Loop.................................................... 48
3-1 Power Switch Location...................................................................50
3-2 Main Menu..................................................................................... 51
3-3 Front Panel ....................................................................................52
3-4 717plus Autosampler Menu Flowchart .......................................... 53
3-5 Path to Auto Zero Pressure Page.................................................. 56
3-6 Path to Seal Pak Calibration Page................................................. 58
3-7 Priming the Needle Wash Pump.................................................... 59
3-8 Autosampler Configuration Flowchart............................................ 61
3-9 Setting the Integrator Report Delay...............................................64
Table of Contents 11
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3-10 Setting Terminal Signal Parameters...............................................65
3-11 Setting IEEE-488 Address............................................................. 67
3-12 Configuration Page 3..................................................................... 68
3-13 Purge Menu...................................................................................69
4-1 Overview of Operations................................................................. 73
4-2 Preparing Samples........................................................................75
4-3 Sample Vial Assembly................................................................... 77
4-4 Improper Needle Wash Solvent Location ......................................79
4-5 Inserting the Carousel................................................................... 80
4-6 Purging the Autosampler...............................................................82
4-7 Purge and Compressibility Page ................................................... 83
4-8 Running a Compressibility Test...................................................... 86
4-9 Overview of Programming............................................................. 88
4-10 Edit: Auto Run Screen ................................................................... 89
4-11 Edit: Step Function Screen............................................................ 93
4-12 Edit: Auto Standards Screen.......................................................... 96
4-13 Example Auto Standard Run 1......................................................98
4-14 Example Auto Standard Run 2......................................................99
4-15 Auto Addition Screen................................................................... 101
4-16 Auto Addition Example ................................................................ 103
4-17 Auto Transfer Screen ...................................................................105
4-18 Transfer Before Step.................................................................... 108
4-19 Transfer Before Vial...................................................................... 109
4-20 Transfer Before Injection.............................................................. 110
4-21 Edit: Step Function Screen.......................................................... 111
4-22 Auto Run Status Screen..............................................................112
4-23 Edit Stat Run Screen...................................................................114
4-24 Status: Stat Run........................................................................... 115
4-25 Setting Sample Chamber Temperature........................................117
4-26 Changing Syringe Configuration..................................................118
4-27 Entering the Semiprep Configuration .......................................... 119
12 Table of Contents
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4-28 Setting Sample Draw Rate .......................................................... 121
4-29 Enabling Auto Purge....................................................................122
4-30 Enabling Purge in Idle................................................................. 123
5-1 Defrost Menu Flowchart .............................................................. 125
5-2 Syringe Assembly Components................................................... 127
5-3 Positioning the Syringe for Removal............................................ 128
5-4 Installing the Syringe ................................................................... 129
5-5 Changing Syringe Volume........................................................... 131
5-6 Removing the Injector (shown with Safety Shield Removed) ...... 134
5-7 Bottom View of Injector................................................................135
5-8 Needle Removal.......................................................................... 136
5-9 Locating In-Line Filters ................................................................ 139
5-10 Assembling In-Line Filters ........................................................... 139
6-1 Positioning the Syringe for Manual Purge....................................156
6-2 Valve and Motor Operations........................................................ 157
6-3 Accessing the Auto Zero Pressure Page.....................................160
6-4 Adjusting the Transducer ............................................................. 161
Table of Contents 13
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List of Tables
2-1 Terminal Strip Signals ............................................................. 34
2-2 System Controller Connections .............................................. 37
2-3 Auto Zero Connections............................................................ 38
2-4 Chart Mark Connections ........................................................ 38
2-5 RS-232 Parameters................................................................. 41
3-1 Menu Functions ..................................................................... 52
3-2 Configuration Parameters ....................................................... 62
3-3 Hold Logic............................................................................... 65
4-1 Suggested Needle Wash Solvents .......................................... 77
4-2 A utosampler Volume .............................................................. 83
4-3 Purge Time Examples............................................................. 84
4-4 Sample Draw Rate................................................................ 120
6-1 Error Message Type ............................................................. 142
6-2 Informational Error Messages ............................................... 143
6-3 CAL Error Messages ............................................................ 143
6-4 CAR Error Messages ........................................................... 145
6-5 H/C Error Messages ............................................................. 146
6-6 INJ Error Messages ............................................................. 146
6-7 Autosampler Troubleshooting ..................................................... 148
A-1 Operational Specifications .......................................................... 162
A-2 Mechanical Specifications ......................................................... 163
A-3 Environmental Specifications ................................................ 163
A-4 Power Requirements ........................................................... 164
A-5 Communications .................................................................. 164
B-1 Spare Parts .......................................................................... 165
C-1 Autosampler Warranty Periods ............................................. 171
E-1 Sample Vials for 48-Vial Carousel ........................................ 180
E-2 Sample Vials for 96-Vial Carousel......................................... 181
Table of Contents 14
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How to Use This Manual
Purpose of This Manual
The
Waters 717plus Operator’s Manual
717plus Autosampler. It also includes installation, maintenance, and troubleshooting
procedures.
Audience
The audience for this operator’s manual includes chemists and technicians who will use
the autosampler to make injections for chromatographic analysis.
describes the features and use of the Waters
Structure of This Manual
This manual is divided into chapters. Each chapter page is marked with a tab and a footer
facilitating access to information within the chapter.
The table below describes the material covered in each chapter.
Chapter 1, Introduction Describes the Waters 717plus Autosampler.
Chapter 2, Installation Provides procedures for installing the Waters
717plus and making fluidic and electrical
connections.
Chapter 3, Startup and
Configuration
Chapter 4, Operating the
Autosampler
Chapter 5, Maintenance Provides procedures for defrosting the
Provides procedures for starting up, calibrating,
configuring, verifying, and powering down.
Provides procedures for preparing and loading
samples, programming and using the automatic
features, and making a stat run.
heater/cooler and for replacing the syringe, seal
pak, and in-line filters.
How To Use This Guide 15
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Chapter 6, Troubleshooting Provides troubleshooting tables to aid in prob lem
diagnosis and information about error messages.
Appendix A, Specifications Lists Waters 717plus specifications.
Appendix B, Spare Parts Lists spare parts.
Appendix C, Warranty
Information
Appendix D,
Reproducibility and
Solvent Degassing
Appendix E, Selecting
Sample Vials
Contains the warranty and a key to serial number
interpretation.
Provides information about the factors affecting
reproducibility and the theory and methods of
solvent degassing.
Provides information about selecting sample
vials.
Related Adobe™ Acrobat Reader Documentation
For detailed information about using the Adobe Acrobat Reader, refer to the
Acrobat Reader Online Guide
navigating and printing electronic documentation from Adobe Acrobat Reader.
. This Online Guide covers procedures such as viewing,
Adobe
Printing From This Electronic Document
Adobe Acrobat Reader lets you easily print pages, pages ranges, or the entire electronic
document by selecting Print from the File menu. For optimum print quantity, Waters
recommends that you specify a Postscript printer driver for your printer. Ideally, use a
printer that supports 600 dpi print resolution.
Conventions Used in This Guide
This guide uses the following conventions to make text easier to understand.
• Purple Te xt indicates user action. For example:
Press 0 , then press Enter for the remaining fields.
•
Italic
text denotes new or important words, and is also used for emphasis. For
example:
An
instrument method
16 How to Use This Guide
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tells the software how to acquire data.
• Underlined, Blue Color text indicates hypertext cross-references to a specific
chapter, section, subsection, or sidehead. Clicking this topic using the hand symbol
automatically brings you to this topic within the electronic document. Right-clicking
and selecting Go Back from the popup context menu brings you back to the
originating topic. For example:
For details on selecting a needle wash solution for a specific sample, refer to
Section 4.3, Selecting a Needle Wash Solvent.
Notes, Attentions, and Cautions
• Notes call out information that is important to the operator. For example:
Note: Record your results before you proceed to the next step.
STOP
• Attentions provide information about preventing possible damage to the system or
equipment. For example:
Attention: To avoid damaging the detector flow cell, do not touch the flow cell
window.
• Cautions provide information essential to the safety of the operator. For example:
Caution: To avoid chemical or electrical hazards, always observe safe laboratory
practices when operating the system.
Caution: To avoid the possibility of electrical shock and possible injury, always turn
off the detector and unplug the power cord before performing maintenance
procedures.
How To Use This Guide 17
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1
1
Introduction
This chapter introduces you to the Waters 717plus Autosampler. The autosampler’s
operational features are summarized and its components described.
1.1 Description
The Waters 717plus Autosampler injects samples into a high performance liquid
chromatography (HPLC) system. The Waters 717plus automates sampling by storing up
to 96 sampling methods or “steps”. Each method controls all injection parameters for a
sequence of vials.
The Waters 717plus (Figure 1-1) may be used as either a stand-alone unit or as a
component in a Waters IEEE-488 based HPLC system. As part of an IEEE-488 based
system, the autosampler may be controlled by Waters PowerLine System Controllers or
Waters Data Workstations.
Waters 717plus Autosampler
Home
123
4
56
8
7
0
Display
Contrast
9
Clear
Enter
O I
18 Introduction
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MILLIPORE
Figure 1-1 Waters 717plus Autosampler
1.2 Features
Sample Carousels and Vials
The Waters 717plus autosampler features:
Two carousel sizes:
• 48-vial carousel - Holds 4 mL sample vials
• 96-vial carousel - Holds 1 mL sample vials
A variety of sample vials are available. For details, refer to Appendix E, Selecting Sample
Vials.
Multi-method Automatic Sampling
An auto sampling multi-method may contain:
• Up to 96 steps, with each step containing a different sampling method
• Random access to any single or series of vials
Priority (Stat) Sampling
The Stat function:
• Interrupts a programmed sampling method.
• Performs injections from a single vial or a series of vials.
• Returns to the interrupted sampling method, and continues auto sampling from the
interruption point.
1
Automated Options
The 717plus allows you to program the following options:
• Auto Addition - Allows you to inject a common solution with each sample.
• Auto Standards - Allows you to run standards automatically during a run.
• Auto T ransfer - Allows you to program the 717plus to transfer solutions from
specified vials to your sample vial; to mix the solution; and to inject.
Interaction with Other LC Modules
The Waters 717plus sends and receives signals from other LC modules, including:
• Inject Start - Occurs when the sample is injected into the mobile phase stream.
Initiates data acquisition, fraction collection, and detector autozero. Contact closure
is initiated by the autosampler.
Features 19
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1
•
Inject Stop - Occurs when the programmed run time expires. Signals data
integrators that the chromatography run is complete. Contact closure is initiated by
the autosampler.
• Hold - Halts the autosampler until the signal changes. Can be used to prevent
sample injections if an LC system module fails or while a data acquisition system is
preparing for the next run. Signal is received from external devices.
• Report Delay - Delays the next injection until a data integrator can complete a
report for the previous run. The delay is a programmable interval that occurs after
the Inject Stop signal.
• Programmable Event - The 717plus includes a programmable event output that
can control external devices during a run.
IEEE-488 Bus Communication
As part of a Waters IEEE-488 system, the Waters 717plus autosampler accepts
programming and control signals from an LC system controller.
RS-232 Communications
The Waters 717plus autosampler sends data over an RS-232 communication line. The
data is in ASCII format and contains:
VIAL # nn INJ # n OF n
INJ VOL nnnn RUN TIME nnnnn
Purge and Compression
Purge and compression testing capability includes:
• Purge - Fills the sample loop and injection syringe with fresh mobile phase.
• Compression - Tests the sample loop for gas content (compressibility).
Compressibility limits may be set for specific mobile phases. Testing may be
automatic or operator initiated.
Needle Wash System
The needle wash system:
• Prevents cross-contamination of samples
• Extends seal life by removing the mobile phase and the sample from the sampling
needle
20 Introduction
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Semiprep Chromatography
For semiprep chromatography (up to 2 mL injections), the 717plus autosampler may be
configured with optional:
• 2000 µL sample loop - Required for injections greater than 200 µL
• 2500 µL syringe - Speeds pre-injection sequence for samples greater than 150 µL
Microbore (< 1 µL) Chromatography
For microbore chromatography, the 717plus autosampler may be configured with:
• 25 µL syringe for improved injection volume precision below 1.0 µL
• Low volume sample vials
1
Syringe Speed
The autosampler syringe speed is adjustable for each syringe size and allows you to
adjust for sample viscosity.
Heater/Cooler
The Waters 717plus Autosampler may be configured with a heater/cooler to maintain
constant sample compartment temperature from 4 to 40°C.
1.3 Components and Subsystems
717plus Components
This section describes the components and subsystems of the Waters 717plus
Autosampler (Figure 1-2):
• Front Panel - Contains a display screen, keypad, and function keys, and provides
access to the control system.
• Autosampler Controller - Contains a microprocessor and memory for controlling
all autosampler components.
• Sample T ransport System - Positions sample vials under the injector.
• Fluid Pack - Contains all components involved in directing mobile phase and
sample to the column. Performs purges and mobile phase compression tests.
• Injector - Withdraws the sample (aliquot) from the sample vial, and performs an
injection into the mobile phase.
• Syringe - Draws samples and compresses the mobile phase during testing.
• Needle Wash System - Cleans the outside of the needle to prevent
cross-contamination of samples.
Components and Subsystems 21
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1
Front Panel
Display
IEEE-488 Network
Connector
Keypad
RS-232
Connector
Contact Closure Terminal Strip
Inject Stop
End-of-Run Inject Start Hold
Needle Wash
Out In
(Yellow) (Green)
Needle Wash
Valve (v4)
Needle Wash
Pump
Injector Drive
(Stepper Motor)
Injector Top
and Bottom
Sensors
Outlet Line to
Column (Red)
Autosampler
microprocessor
Sample Loop
Pressure
Transducer
Syringe
Valve (v2)
Sample Loop
Valve (v1)
Carousel lift
sensors
Syringe empty
and full position
sensors
Figure 1-2 Waters 717plus Autosampler Subsystems
Carousel lift
Drive
Carousel reader
Purge Waste Line (Clear)
Waste
Valve (v3)
Syringe Drive
(stepper motor)
Inlet Line from
Pump (Blue)
22 Introduction
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Installation
This chapter describes 717plus installation and setup. It includes procedures for making
connections, voltage selection, and configuring optional hardware.
2.1 Site Requirements
2
2
•
•
•
Required Space
Before beginning the installation procedure, note the following autosampler site and utility
requirements (Figure 2-1):
Note: The autosampler site requires room for a waste bottle and a needle wash solvent
reservoir.
Bench space - Allow 21 x 23.5 inches (53 x 72 cm) for the autosampler. This space
includes ventilation sides 2.5 inches (6.3 cm) and back 3.5 inches (8.75 cm).
Note: Ensure the bench top must be level to ensure proper drainage of the solvent
spill lines.
Bench space with heater/cooler installed - Allow an additional three inches on
the back and on each side next to the air vents.
Note: To avoid heater/cooler performance degradation, do not place the rear of the
unit in an enclosed space, under a shelf, or near a heat source.
Column location - Ensure the red fluid line reaches the column. Lengthening this
line may result in peak broadening.
• Waste and solvent container location - Place the needle wash reservoir at bench
level to prevent siphoning.
Site Requirements 23
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1
4
7
Home
2
56
8
0
Display
Contrast
3
9
Clear
Enter
Rear
Ventilation
3.5 inches
(8.8 cm)
2
23.5 inches
(59 cm)
21 inches (53 cm)
Side Ventilation
2.5 inches (6 cm)
Figure 2-1 Waters 717plus Autosampler Site Requirements
Operating Conditions
Locate the Waters 717plus in a clean area free from extremes in temperature, humidity,
strong radio frequency radiation, appreciable shock or vibration. The Waters 717plus
operates within the following ranges:
Temperature
Humidity
Do not locate the Waters 717plus in direct sunlight, near heat registers, or under air
conditioning vents.
4 to 40 °C
Note that cooler performance is derated above 27 °C
80% maximum relative humidity, non-condensing
Weight
Requires a bench capable of supporting at least 75 lbs.
24 Installation
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Power Requirements
Requires 5 Amps at 110 Vac (nominal) or 4 Amps at 220 Vac (nominal) from a grounded
outlet.
2.2 Unpacking and Inspection
Unpacking
To unpack your unit:
1. Remove the straps and open the top of the shipping carton.
2. Remove the Startup Kit.
3. Remove the packing material from the carton.
4. Lift the carton sides from the base of the carton to expose the autosampler.
Caution: The autosampler weighs approximately 63 pounds (28.6 kg). Two
people are required to safely lift the autosampler; use care when lifting.
5. Grasp the autosampler from the bottom to lift. Do not lift by holding the front
panel.
6. Place the 717plus securely on the bench top. Allow clearance for the power cord
and ventilation.
List of Components
The autosampler shipping carton contains:
• Waters 717plus autosampler
• Startup Kit
Reporting Damage
Check the packing list against the contents as you unpack, and confirm that all items are
included. If you find any damage or discrepancy, immediately report any damage to both
the shipping carrier and to your Technical Service representative. You can contact Waters
Technical Service at (800) 252-4752,
customers, call your local Waters subsidiary or your local Waters Technical Service
Representative, or call Waters corporate headquarters for assistance at (508) 478-2000
(U.S.).
U.S. and Canadian customers only
. Other
2
If any items are damaged, use the shipping container for subsequent claim purposes.
Unpacking and Inspection 25
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2.3 Changing Voltage Configuration
The Waters 717plus autosampler is shipped in a 120 V/60 Hz configuration. If you require
a different voltage setting, change the configuration.
Tools required:
• One small-blade screwdriver
• One Phillips-head screwdriver
• One pair of needlenose pliers
2
Caution: Disconnect the autosampler power cord before continuing this procedure.
For continued protection, use only fuses of the approved type and rating, as
indicated by the label on the rear panel near the power cord connector
Selecting V oltage
To select the voltage configuration:
1. Disconnect the power cord from the back of the Waters 717plus Autosampler.
2. Insert a small-blade screwdriver into the notch just to the right of the power cord
connector and pry off the fuse block cover (Figure 2-2).
Notch
Fuse Block
Voltage Selector
Card
Voltage indicated
by white pin
100 v
USE ONLY WITH
250 V FUSES
120 V
220 V
240 V
3. Grasp the voltage selector card and pull it straight out of the housing.
26 Installation
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Fuse Block Cover
Figure 2-2 Fuse Block and Voltage Selector Card
Attention: Do not use the voltage selector card to compensate for low line
STOP
voltage. Always use a selection that equals the nominal line voltage, or power
surges may damage the instrument.
4. The edge of the voltage card is labeled with four voltages (Figure 2-3). Position
the voltage indicator pin on the opposite side of the card from the required
voltage. Seat the indicator in the notch on the edge of the card.
Indicator pin
2
4
0
0
1
240 V
2
0
0
2
0
100V 120 V 220 V
1
0
0
1
2
2
2
0
0
1
2
0
0
2
2
2
2
4
2
2
1
0
2
0
0
4
Notch for indicator pin
Figure 2-3 Voltage Selector Card
5. Insert the voltage selector card into the housing until it is firmly seated.
Changing Fuses
Change the fuse block arrangement if the fuse requirements change from single 1/4-inch x
1 1/4-inch to dual 5 mm x 20 mm.
To change the fuse configuration:
1. Loosen the Phillips screw two turns and remove the fuse block by tilting it up and
sliding it away from the screw (Figure 2-4).
2
Changing Voltage Configuration 27
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1. Loosen retaining screw.
Screw
Mount Shoulder
2. Push clip.
3. Tilt up and slide
away from screw.
2
Figure 2-4 Removing the Fuse Block
2. Or ient the fuse block for the desired voltage (Figure 2-5) as follows:
• For single 1/4-inch x 1 1/4-inch fuse arrangements, install the fuse block with
the fuse and jumper bar facing away from the cover.
• For dual 5 mm x 20 mm fuse arrangements, install the fuse block with the two
fuses facing away from the cover.
100/120 Fuse
220/240 Fuse
Dual
Configuration
Figure 2-5 Fuse Installation
3. Install the appropriate fuse or fuses as labeled on the rear panel near the power
cord connector.
4. Ensure that the assembly is seated against the shoulder of the screw mount and
tighten the Phillips screw.
5. Install the fuse block and cover in the rear panel of the autosampler. Make sure
that the indicator pin fits through the appropriate opening on the left end of the
cover.
Single
Configuration
28 Installation
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2.4 Connecting Fluid and Drain Lines
Caution: Observe safe laboratory practices when handling solvents. Refer to the
Material Safety Data sheets for the solvents in use.
The Waters 717plus Autosampler fluid lines are:
• Green - Plastic tubing for needle wash inlet
• Yellow - Plastic tubing for needle wash waste
• Clear - Plastic tubing for purging the sample loop waste
• Blue - High pressure steel tubing, 0.04-inch (1 mm) I.D., connects the autosampler
to the pump
• Red - High pressure steel tubing, 0.009-inch (0.2 mm) I.D., connects the
autosampler to the column
• Drain - Two 1/4-inch clear lines attached to the drip trays on bottom of the
autosampler. One line drains solvent and sample spills. The other line drains water
when the heater/cooler is defrosted.
2
Connecting Fluid and Drain Lines 29
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Connecting Fluid Lines
To connect the fluid lines (Figure 2-6):
Red Line to Column
2
Green Line to
Needle Wash Solvent
Home
Display
Contrast
2
3
1
4
56
8
9
7
Clear
Enter
0
O I
Blue Line to Pump
Yellow and Clear Lines
to Waste
Figure 2-6 Fluid Line Connections
1. Cut the plastic tie securing the coil of tubing located at the rear of the autosampler.
The coil consists of yellow, clear, and green tubing.
2. Fill a flask with a filtered solution of 90 percent methanol/10 percent water. Use
this solution for the needle wash during installation. Place the flask at bench
level, and put the end of the green line in the solution.
Note: For details on selecting a needle wash solution for a specific sample, refer to
Section 4.3, Selecting a Needle Wash Solvent.
3. Place the ends of the yellow (needle wash waste), and clear (purge waste) lines
in appropriate containers.
4. Connect the blue line to the pump. Do not connect the red line to the column
inlet until you flush the system (see Section 3.3, Flushing the Autosampler).
30 Installation
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Attention: Ensure that the red and blue fluid lines are in the side panel slots and not
STOP
pinched between the cover and side panels.
Installing Drain Lines
Using parts from the 717plus Startup Kit, connect the two drain lines to the drain pans
located on the bottom of the autosampler (Figure 2-7) as follows:
1. Place an appropriate waste container for solvent and sample leaks below bench
level.
2. Cut a length of 1/4-inch tubing long enough to reach the waste container from
the autosampler.
3. Slip the tubing strain relief onto the tubing and push it onto the fitting for the
solvent drain pan (located on left side).
4. Use the elbows to facilitate bends in the tubing.
5. If you have a heater/cooler, connect a drain line for condensation/defrosting
following steps 1 through 4.
2
Connecting Fluid and Drain Lines 31
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2
Strain Relief 1/4-inch Tubing
Bottom View
Solvent/Sample
Drain Pan
Figure 2-7 Drain Line Connections
Defrost
Drain Pan
2.5 Connecting Communication Cables
The 717plus autosampler communicates with other LC system components via the
following connections on the rear panel of the autosampler (Figure 2-8):
• Terminal Strip - Contact closure signals from the terminal on the back panel
provide communication with non-IEEE-488 LC components.
• IEEE-488 - Communicates with a system controller over the IEEE network.
• RS-232 - Provides information to RS-232 based data systems such as the Waters
746 Data Integrator.
This section describes the communication connections listed above.
32 Installation
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Terminal Strip
(removable)
INJECT STOP
PROG EVENT
INJECT START
INJECT START
HOLD
HOLD
RS-232
RANGE
85-130 VAC
185-265 VAC
INPUT VOLTAGE
FUSE
6.0 A
3.0 A
IEEE-488
Figure 2-8 Autosampler Rear Panel
1 2 3 4 5 6 7 8 9 1 0 11 1 2 1 3 1 4 1 5
NEEDLE WASH IN (1/16") GREEN
NEEDLE WASH OUT (1/16") YELLOW
WASTE LINE OUT (1/16") CLEAR
RS-232
IEEE-488
2
2.5.1 Making Terminal Strip Connections
This section covers:
• Terminal strip signals
• Electrical specifications
• Making cable connections
• Making system controller connections
• Making detector connections
• Making pump connections
• Making programmable event output connections
Refer to Figure 2-8
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while performing the following procedures.
Connecting Communication Cables 33
Terminal Strip Signals
The signals available on the back panel terminal strip include:
Table 2-1 Terminal Strip Signals
2
Terminal
Numbers
1, 2 Hold Input signals the autosampler to hold (pause) the
4, 5 Hold Input signals the autosampler to hold (pause) the
6, 7 Inject Start Output signals the start of an injection
9, 10 Inject Start Output signals the start of an injection
11, 12 Prog Event Programmable event output signal
14, 15 Inject Stop Output signals the end of the programmed run
3, 8, 13 Ground Signal ground for cable shields
For specific information on signal use with other Waters equipment, refer to the
appropriate manual.
Signal
Name
Description
injection sequence
injection sequence
time
Electrical Specifications
Input (Hold) terminal specifications are:
• TTL or switch closure
• Low trigger < 1.8 V
• High trigger > 3.0 V
• Protected to ±30 V
• Minimum pulse width: 30 milliseconds
• Maximum current: 5 milliamps
34 Installation
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Output (Inject Start/Inject Stop) specifications are:
STOP
STOP
• Contact closure
• Maximum power 10 watts
• Maximum current: 0.5 amps at 20 V
• Maximum voltage: 40 Vdc at 0.25 amps
Attention: Do not connect two cables to the same autosampler terminal on the terminal
strip.
Attention: To meet the regulatory requirements of immunity from external electrical
disturbances that may affect the performance of this instrument, do not use cables longer
than 9.8 feet (3 meters) when you make connections to the screw-type barrier terminal
strips. In addition, ensure you always connect the shield of the cable to chassis ground at
one instrument only.
Making Cable Connections
Tools required:
• One small-blade screwdriver
• One electrical insulation stripping tool
• Signal cable from 717plus Startup Kit
2
Connecting Communication Cables 35
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2
Removable Terminal Strip
Event Out
STOP
EVENT
START
START
connection
Label
(on side)
INJ
13
PROG
10 11 12 13 14 15
INJECT
8
INJECT
HOLDHOLD
3
1 2 3 4 5 6 7 8 9
Figure 2-9 Terminal Strip
To connect cables from other LC devices to the terminal strip on the back panel
(Figure 2-9):
1. To facilitate making connections, remove the terminal strip from the rear panel (see
Figure 2-8).
2. Strip 1/4 inch (5 mm) of insulation from each wire at one end of the signal cable.
3. Insert the bare wire into the appropriate connector, and secure it by screwing
down the connector.
Note: If multiple components require an injection start signal, use separate INJECT
START terminals for each component. Do not exceed the 0.5 A and 20 V maximum open
circuit limit for a terminal.
System Controller Connections
Note: Some system controllers do not allow injections of less than 1 µL. To make
injections of less than 1 µL, do not operate the Waters 717plus autosampler o v er the IEEE
bus.
36 Installation
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Using a signal (contact closure) from the Waters 717plus autosampler, a Waters system
controller can coordinate the start of detectors, pumps, and computers. F or specific details
on programming a system controller, refer to the system controller operator’s manual.
To connect a system controller, connect the Inject Start terminal on the autosampler as
outlined in Table 2-2.
Table 2-2 System Controller Connections
Autosampler
Terminal
Inject Start Millennium Chromatography Manager Event In for
Inject Start ExpertEase SAT/IN Event In for
Inject Start ExpertEase SIM Start Inject and
Inject Start 600 Series INJ and GND
Inject Start Maxima Watch Dog Event Box IN 1 or IN 2
Controller
Controller
channel 1 or 2
channel 1 or 2
COM
Making LAC/E Connections
Use the Inject Start signal from the Waters 717plus:
• If the LAC/E system contains components such as detectors that are not connected
to the IEEE-488 bus.
• If the ExpertEase multi-method is set to “Start by Injector.”
Terminal
2
Making Detector Connections
Waters detectors use the start of the injection for:
• Auto zeroing
• Start of data transfer
• Detector chart marking
For specific details on programming a detector for an auto zero, refer to the detector
operator’s manual.
Connecting Communication Cables 37
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Auto Zero
To enable an auto zero, connect the Inject Start terminal on the autosampler as outlined in
Table 2-3.
Table 2-3 Auto Zero Connections
2
Autosampler
Terminal
Inject Start 490E Event In 1
Inject Start 996 Event In 1
Inject Start Other Waters detectors Auto Zero
Detector Data Transfer and Chart marking
Using the Inject Start signal from the Waters 717plus autosampler, a Waters detector can:
• Start data transfer over the IEEE-488 bus when the autosampler initiates an
injection
Note: If you specify start by LAC/E, you do not need the Inject Start signal.
• Indicate the start of an injection on a chart recorder
For specific details on connecting a chart recorder to the detector, refer to the detector
operator’s manual.
To enable a detector to mark a chart recorder, connect the Inject Start terminal on the
autosampler as outlined in Table 2-4.
Detector
Detector
Terminal
Table 2-4 Chart Mark Connections
Autosampler
Terminal
Inject Start 490E Event In 1
Inject Start 996 Event In 1
38 Installation
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Detector
Detector
Terminal
Table 2-4 Chart Mark Connections (Continued)
STOP
Autosampler
Terminal
Inject Start Other Waters detectors Chart Mark
Detector
Detector
Terminal
Making Pump Connections
Waters 600 series gradient controllers provide a Hold signal to stop the next injection.
Connect the Waters 717plus autosampler to the 600 series pump as follows:
Autosampler 600 Series
HOLD HOLD and GRN
Making Event Output Connections
Connect a signal cable to the Prog Event terminals (pins 11 and 12, pin 13 for ground) on
the 717plus autosampler terminal strip (Figure 2-9).
2.5.2 Making IEEE-488 Network Connections
2
The IEEE-488 bus provides a communication link between the Waters 717plus
autosampler and system controllers such as the Millennium Chromatography Manager,
ExpertEase data systems (through a LAC/E module), and 600 series system controllers.
Making IEEE-488 Bus Connections
With all instruments powered down, make the following cable connections (Figure 2-10):
Attention: Power down all instruments on the IEEE-488 bus before making connections.
1. Connect one end of the IEEE-488 cable to the IEEE connector of the 717plus
autosampler.
2. Connect the other end of the IEEE-488 cable to a system controller or to any
one of your IEEE-488 components.
Ensure that all IEEE cable screws are fastened securely.
Connecting Communication Cables 39
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IEEE-488
Network Cable
Data System or
System Controller
2
Waters 717plus
Autosampler
Figure 2-10 IEEE-488 Connections
Waters Detector
Equipped with IEEE-488
Setting IEEE-488 Addresses
In order to interact with the PowerLine system controller or LAC/E, each device on the
IEEE-488 communications bus must have a unique individual address.
Note: To use the autosampler on the IEEE-488 network, change the autosamplers
IEEE-488 address (refer to Section 3.6.2, Setting Parameters for LC System Operation).
2.5.3 Connecting RS-232 Output to Data Module
The RS-232 connector on the rear panel allows the autosampler to transfer injection
parameters to a data integrator such as the Waters 746 Data Integrator.
You may use the RS-232 port with any device that can read ASCII code.
To connect to the RS-232 port, plug the cable into the modified phone jack connector on
the rear panel of the Waters 717plus autosampler.
40 Installation
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RS-232 Parameters
Note: RS-232 parameters are not user-configurable.
Table 2-5 RS-232 Parameters
Parameter Value
Baud rate 1200
Number of bits 8
Number of stop bits 1
Parity none
2.6 Changing the Hardware Configuration
This section covers:
• Removing the autosampler cover
• Installing the heater/cooler
• Installing the auxiliary sample loop
2
2.6.1 Removing/Replacing the 717plus Cover
Caution: To avoid the possibility of electric shock, disconnect the autosampler pow er cord
before continuing this procedure.
Removing the Cover
To remove the autosampler cover (Figure 2-11):
1. Turn off the autosampler and disconnect the power cord.
2. Remove the syringe cover, and unscrew the cover retaining screw located to the
right of the magnetic latch.
3. Slide back the cover until it clears the posts on the rear panel.
4. Ensure that the red and blue fluid lines are free of the side cover slots.
5. Lift the cover up and back.
Changing the Hardware Configuration 41
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2
STOP
Attention: Always replace the 717plus autosampler cover to maintain RFI and EMI
shielding integrity.
Caution: To avoid the possibility of electric shock, do not remove the power supply cover.
The power supply does not contain user-serviceable components.
42 Installation
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Front Flanges
Side Slots
(for fluid lines)
Side Flanges
INPUT VOLTAGE
FUSE
RANGE
6.0 A
85-130 VAC
3.0 A
185-265 VAC
END OF RUN
INJECT START
INJECT START
INJECT START
HOLD
HOLD
RS-232
IEEE-488
1 2 3 4 5 6 7 8 9 10 1 1 1 2 1 3 1 4 1 5
NEEDLE WASH IN (1/16") GREEN
NEEDLE WASH OUT (1/16") YELLOW
WASTE LINE OUT (1/16") CLEAR
1. Lift up syringe
cover
to remove.
2
2. Remove
cover
retaining
screw.
3. Pull cover
back to clear
posts, fluid
lines, and
front flanges.
4. Lift up
cover.
Posts
Figure 2-11 Removing the Autosampler Cover
Changing the Hardware Configuration 43
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2
Replacing the Cover
To replace the autosampler cover:
1. Lower the cover onto the autosampler leaving a 2-inch space between the cover
and the front panel.
2. Before sliding the cover forward, ensure that the red and blue fluid lines are in
the side slots and that the flanges fit over the sides of the base.
3. Slide the cover forward until it seats on the rear panel posts.
4. Secure the cover retaining screw on the right of the magnetic latch, and replace
the syringe cover.
5. Reconnect the power cord.
2.6.2 Installing the Heater/Cooler
Caution: To avoid the possibility of electric shock, disconnect the autosampler pow er cord
before continuing this procedure.
This section describes the following procedures:
• Remove the rear chamber assembly
• Install the heater/cooler
• Connect the heat/cooler power cord
• Install the temperature probe
To install the heater/cooler:
1. Disconnect the power cord and remove the autosampler cover (see Section 2.6.1,
Removing/Replacing the 717plus Cover).
2. Remove the rear chamber assembly by unlatching the side clips, and pulling the
assembly back.
3. Slide the heater/cooler into the autosampler until the side clip latches are in
position to close. Take care not to damage the insulation.
4. Clamp the heater/cooler to the autosampler using the two side clips
(Figure 2-12).
44 Installation
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1 2 3 4 5 6 7 8 9 1 0 11 12 1 3 1 4 1 5
Side Clips
Heater/Cooler
Power Cable
Figure 2-12 Installing Heater/Cooler
5. Feed the power cable up through the opening in the chassis and attach it to the
J20 connector on the main circuit board (Figure 2-13).
2
Changing the Hardware Configuration 45
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2
Heater/Cooler
Power Connector
(J20)
Temperature
Probe
Connector
Figure 2-13 Connecting the Heater/Cooler Power Cord and Temperature Probe
Opening For
Heater/Cooler
Power Cable
6. Push the temperature probe through the grommet located on the floor of the unit
behind the carousel drive (Figure 2-14). Push the probe down until it reaches the
stop.
46 Installation
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Carousel Drive
2
Figure 2-14 Installing the Temperature Probe
7. Attach the temperature probe connector to the main circuit board. The
temperature probe connects to the main circuit board at J18, located to the lower
right of the battery (see Figure 2-13).
8. Replace the autosampler cover (see Section 2.6.1, Removing/Replacing the
717plus Cover) and reconnect the power cord.
2.6.3 Installing the Large Sample Loop
To inject sample volumes greater than 200 µL, you must install the auxiliary loop.
Caution: To avoid the possibility of electric shock, disconnect the autosampler pow er cord
before continuing this procedure.
Temperature Probe
Changing the Hardware Configuration 47
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2
Required tools:
• One 5/16-inch wrench
• One adjustable wrench
• Auxiliary loop from 717plus Startup Kit
• Union from 717plus Startup Kit
To install the loop:
1. From the 717plus front panel, set system flow to 0 mL/min.
2. Turn off the autosampler, disconnect the power cord, and remove the
autosampler cover (see Section 2.6.1, Removing/Replacing the 717plus Cover).
3. Disconnect the sample loop at the filter using the 5/16-inch wrench (Figure 2-15).
Disconnect at outlet side
of in-line filter.
4. Connect the auxiliary loop to the filter.
5. Using a union from the Startup Kit, connect the auxiliary loop to the sample loop.
6. Replace the cover, reconnect the power cord, and turn on the autosampler.
48 Installation
Sample
Loop
Figure 2-15 Disconnecting the Sample Loop
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7. Complete the configuration procedures discussed in Section 3.6.3, Entering
Hardware Changes.
If the auxiliary loop was added to a previously configured autosampler, perform the
procedures in:
• Section 3.3, Flushing the Autosampler
• Section 3.7, System Verification
• Section 4.5.2, Performing a Purge
1
Changing the Hardware Configuration 49
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3
Startup and Configuration
This chapter provides procedures for starting up, calibrating, configuring, verifying, and
powering down the Waters 717plus autosampler.
3.1 Powering Up the Autosampler
Note: If the 717plus autosampler is part of an IEEE-488 system, power up the 717plus
autosampler before powering up the system controller.
Powerup
To power up the 717plus autosampler:
1. Press the 1/0 (on/off) switch (Figure 3-1) on the front panel.
Waters 717plus Autosampler
Home
123
4
56
8
7
0
9
Clear
MILLIPORE
Power Switch
Display
Contrast
Enter
O I
Figure 3-1 Power Switch Location
3
Powering Up the Autosampler 50
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2. Wait for the initializing sequence to complete and the IDLE message to appear
in the upper left corner (Figure 3-2).
IDLE
Menu: Main
Waters 717plus Autosampler
Rev. 2.0C 2/12/93
Copyright (C) 1991, 93
Waters Corporation
Heater/Cooler Not Installed
3
Auto
Page
Stat
Page
Purge
Figure 3-2 Main Menu
Adjusting Display Contrast
If you do not see the Main menu, or need to improve readability, adjust the screen display
contrast as follows:
• If the screen appears blue in color, press the Display Contrast Up arrow (see
Figure 3-3) until the screen text is in focus.
• If the screen appears white in color, press the Display Contrast Down arrow (see
Figure 3-3) until the screen text is in focus.
3.2 Using the Front Panel
Use the front panel (Figure 3-3) to configure the 717plus system and perform injection
programming.
This section describes:
• Accessing menus using menu function keys
• Entering operating parameters using the keypad
Page
Contig
Page
Diag
Page
51 Startup and Configuration
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INIT
Arrow Keys
Carousel
Homing syringe
Waters 717plus Autosampler
Copyright(C) 1991, 93
Heater / Cooler Not Installed
Stat
Auto
Page
Page
Menu: Main
Rev 2.0 2/1/93
Waters Corporation
Purge
Page
(Cursor control)
Diag
Config
Page
Page
1
4
7
0
Release/Engage
Home
2
3
56
8
9
Clear
Enter
CAROUSEL
Release
Engage
Menu Function Keys Numeric Keys
3.2.1 Accessing Menus
The Main Menu (see Figure 3-2) provides access to the main system operations:
Table 3-1 Menu Functions
Function Key Menu Function
Auto Page Auto run Program and run sampling
Stat Page Stat run Interrupt a programmed run for
Purge Page Purge and
compressibility
Clear Key
3
Figure 3-3 Front Panel
methods
priority samples
Purge sample loop and test
compressibility of mobile phase
Using the Front Panel 52
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Table 3-1 Menu Functions (Continued)
Function Key Menu Function
Config Page Configuration Set hardware and LC system
configuration parameters
Diag Page Diagnostics Calibrate injector, test valves,
perform maintenance
Access additional menus using the function keys below the screen. Menus are arranged
as shown in the System Menu Flowchart (Figure 3-4).
3
Main Menu
Status: Auto Run
Edit: Auto Run
Edit: Stat Run
Edit: Purge &
Compressibility
Edit:
Configuration
Page 1
Menu:
Diagnostics
Edit: Step
Function
Status: Stat Run
Status: Purge
Edit:
Configuration
Page 2
Diagnostic: Service Entry
Status: Error Log
Menu: User Maintenance
Edit: Auto Standards
Edit: Auto Addition
Edit: Auto Transfer
Edit:
Configuration
Page 3
Diagnostic: Valve & Motor Operations
Edit:
Configuration
Page 4
Diagnostic: Defrost
Diagnostic: Prime Needle Wash
Menu: Calibration Pages
Status: Defrost
Status: Needle Wash Prime
Diagnostic: Injector Calibration
Diagnostic: Auto Zero Pressure
Figure 3-4 717plus Autosampler Menu Flowchart
53 Startup and Configuration
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3.2.2 Entering Operating Parameters
To enter operating parameters:
1. Access the appropriate menu by pressing the screen function key.
2. Use the arrow keys (see Figure 3-2) to highlight the parameter you want to
change.
3. If the parameter has two or more values, highlight the desired value and press
Enter.
4. If there is one value, use the number keys to type a value and press Enter to
record the new value.
5. If you make a mistake, press Clear to erase the value in the current parameter
field.
3.3 Flushing the Autosampler
Solvent Considerations
When flushing or purging your 717plus, make sure the solvent is properly degassed and
miscible with the previous mobile phase in the autosampler.
Flushing
To flush the 717plus autosampler:
1. Place the red line in a waste container to catch the solvent.
2. Set the mobile phase pump to deliver 1 mL/min of 100 percent methanol.
3. Continue pumping mobile phase for 10 minutes or until all air is forced out of the
autosampler (no bubbles appear in the waste container).
3.4 Calibrating the Seal Pak
The Waters 717plus autosampler seal pak must be calibrated upon startup or after
installation or service.
Injector calibration involves:
• Purging the autosampler
• Auto zeroing the transducer
• Calibrating the seal pak
3
Flushing the Autosampler 54
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3.4.1 Purging the Autosampler
Before calibrating the seal pak, run a purge to ensure that there is no air in the
autosampler, the mobile phase is fresh, and there are no bubbles in the syringe.
1. Using a degassed solution of 100 percent methanol, set the solvent delivery pump
to 1 mL/min.
2. Remove the syringe cover panel to examine the syringe for bubbles.
3. From the Main Menu, press Edit Purge. The Purge and Compressibility menu
appears (Figure 3-13), listing the default parameter values.
4. Use the arrow keys to set Compression Check to No, then press Enter. Press
Start Purge.
5. Run at least 2 purges before calibrating the seal pak.
6. If the purging fails to remove bubbles from the syringe, perform a manual purge
(Section 6.4.1, Man
ual Syringe Purge).
3.4.2 Auto Zeroing the Transducer
Auto zeroing the transducer ensures that pressure readings are accurate.
3
To zero the transducer:
1. Ensure that the system pressure is at 0 psi.
2. Set pump flow to 0 mL/min.
3. To auto zero the transducer, press the keys as outlined in the flowchart below
(Figure 3-5).
After pressing Auto zero Pressure, the system requires approximately 2 minutes to auto
zero the pressure.
If the system is unable to auto zero , manually adjust the transducer (Section 6.4.3, Man ual
Transducer Adjustment).
55 Startup and Configuration
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Main Page
Menu: Diagnostic
Menu: User
Maintenance
Menu: Calibration
DIAG
Diagnostic: Auto Zero Pressure
Ambient pressure with no correction
must be between -90 psi and 750 psi.
Otherwise, manually adjust transducer.
Pressure Correction -72
Pressure (psi) 0
Diag
Page
UserMaint
Page
Cal
Page
AutoZero
Page
3
Autozero
Pressure
Autozero
Pressure
Figure 3-5 Path to Auto Zero Pressure Page
3.4.3 Calibrating the Seal Pak
The autosampler must be calibrated after:
• Initial installation
• Replacing the seal pak and needle
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Cal
Page
Calibrating the Seal Pak 56
3
Before Calibrating
Before running the seal pak calibration, ensure that:
• Two purges have occurred
• Pump pressure is 400 to 600 psi and flow at least 0.5 mL/min
• Solvent is 100 percent degassed methanol
• Mobile phase pump is free of pressure fluctuations
• Remove your column if it is sensitive to sudden pressure changes
To calibrate the seal pak:
1. Adjust the pump flow to achieve a pump pressure of between 400 and 600 psi.
Note: To attain sufficient backpressure without a column, it may be necessary to
partially cap the red line with the union and fitting plug assembly included in the
717plus Startup Kit.
2. To access and run the seal pak calibration, press the keys indicated in the
flowchart below (Figure 3-6).
57 Startup and Configuration
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Menu: Main
Menu: Diagnostic
Menu: User
Maintenance
Menu: Calibration
DIAG
Diagnostic: Injector Calibration
Set system pressure to 400 to 600 psi.
Down Seal Counts
Up Seal Counts
Seal Width Counts
Pressure
96
327
88
498
Diag
Page
UserMaint
Page
Cal
Page
Cal
Page
3
Cal
Page
Start
Cal
Start
Cal
Figure 3-6 Path to Seal Pak Calibration Page
Calibrating the Seal Pak 58
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3
3.5 Priming the Needle Wash Pump
To prime the needle wash pump:
1. Ensure that the needle wash supply line (green) is in the solvent bottle and the
waste line (yellow) is in an appropriate container.
2. To prime the needle wash, press the keys outlined in the flowchart below
(Figure 3-7).
Main Page
Diag
Page
Diagnostic Menu
Page
UserMaint
Page
User Maintenance
Page
Figure 3-7 Priming the Needle Wash Pump
3. If, after 30 seconds, the solvent does not flow out of the waste line, press Start
NdlWash again.
59 Startup and Configuration
NdlWash
Page
Start
NdlWash
Prime Needle
Wash Page
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3.6 Configuring the Autosampler
Configuring the Waters 717plus Autosampler requires:
• Setting parameters to enable the autosampler to communicate with other modules
in the LC system
• Recording changes to autosampler hardware (syringe size and sample loop
volume)
3.6.1 Overview of Configuration
Refer to the Autosampler Configur ation flowchart (Figure 3-8) for a 717plus configur ation
overview.
Table 3-2 provides a summary of parameters from the Configuration Pages.
3
Configuring the Autosampler 60
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Configure
autosampler
3
Connect to IEEE-488
system controller?
No
Connect to
data integrator
or workstation?
Allow other
LC components
to hold next
injection?
Do other
LC components
require start of
injection signal?
Yes
Yes
Yes
Yes
Attach cable
(Section 2.5.2)
and set IEEE-488 address
(Section 3.3.1).
3.6.2).
Attach RS-232 cable
(Section 2.5).
Enter delay required to set
up data files (Section 3.3.1).
Connect cables to HOLD
terminals (Section 2.5.1).
Enable Hold input and
set sense (Section 3.3.1).
Connect cables to INJECT
START terminals
(Section 2.5.1).
Set inject pulse output
interval (Section 3.3.1).
3.6.2).
3.6.2).
3.6.2).
Do other
LC components
require end-of-run
signal?
Autosampler
configured
Figure 3-8 Autosampler Configuration Flowchart
61 Startup and Configuration
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Yes
Connect cables to
END OF RUN terminal
(Section 2.5.1).
Set End of Run pulse
interval (Section 3.3.1).
3.6.2).
Configuration parameters are shown in Table 3-2.
Table 3-2 Configuration Parameters
Parameter
Purge In Idle? 1 Enables purging every 60 minutes while the
Vials Between Purges 1 Enables automatic purging during an auto
Halt Bad Comp
Check?
Report Delay 1 Delays the next injection to allow a data
Hold Input? 2 Enables other LC components to stop the
Hold Contact Sense? 2 Sets polarity of signal arriving at the terminal
Configuration
Page
717plus is idle. See Section 4.8.5, Using
Buffered Mobile Phase.
run. See Section 4.8.4, Purging During an
Auto Run.
1 Prevents the next injection when a
compression check (auto purge) fails. See
Section 4.8.4, Purging Dur
integrator to complete the processing of the
previous run. See Section 3.6.2, Setting
Parameters for LC System Operation.
injector. See Section 3.6.2, Setting
Parameters for LC System Operation.
strip. See Section 3.6.2, Setting Parameters
for LC System Operation.
Description
ing an Auto Run.
3
Inject Start Pulse 2 Sets length of pulse used to signal other LC
components that an injection occurred. See
Section 3.6.2, Setting Parameters for LC
System Operation.
Inject Stop Pulse 2 Sets length of pulse used to signal other LC
components that the run has ended. See
Section 3.6.2, Setting Parameters for LC
System Operation.
Configuring the Autosampler 62
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Table 3-2 Configuration Parameters (Continued)
3
Parameter
Temp Setpoint 2 Sets temperature for sample compartment
Temp Control? 2 Enables temperature control for units with
Draw Rate 3 Sets syringe draw rate. See Section 4.8.3,
Syringe Volume? 3 Set equal to installed syringe size. See
Loop V olume? 3 Set equal to installed sample loop size. See
Installed IEEE
Address
Desired IEEE
Address
Configuration
Page
heater/cooler. See Section 4.8.1,
Temperature Control.
heater/cooler. See Section 4.8.1,
Temperature Control.
Injecting Viscous Samples.
Section 4.8.2, Microbore/Semiprep Injections.
Section 4.8.2, Microbore/Semiprep Injections.
4 Displays current address. See Section 3.6.2,
Setting Parameters for LC System Operation.
4 Sets new IEEE address. See Section 3.6.2,
Setting Parameters for LC System Operation.
Description
3.6.2 Setting Parameters for LC System Operation
To communicate with other LC system components:
• Set Report Delay for data integrators
• Set terminal strip signal parameters for Hold, Injection Start, and Injection Stop
• Set IEEE-488 address
Setting Report Delay
The Report Delay provides time for the data integrator to process data from a run bef ore a
new injection begins.
If a data integrator is attached to the LC system, set the delay as follows:
1. From the 717plus Main Menu, press Config Page.
63 Startup and Configuration
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2. On Configuration Page 1 (Figure 3-9), highlight the Report Delay field and enter
the delay time in minutes.
IDLE
Edit: Configuration Page 1 of 4
Use Door Sensor?
Purge In Idle?
Vials Between Purges:
Halt Bad Comp Check?
Report Delay (min):
LCD Contrast Adjust?
PrevCfg
Page
Yes
Yes
0
Yes
3.0
25
NextCfg
Page
No
No
No
Main
Page
Figure 3-9 Setting the Integrator Report Delay
Setting Terminal Strip Signal Parameters
To set the contact closure parameters for LC components connected through the terminal
strip on the rear panel:
1. From the Main Menu, press Config Page.
2. Press NextCfg Page to access Configuration Page 2 (Figure 3-10).
3
Configuring the Autosampler 64
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IDLE
Edit Configuration Page 2 of 4
Hold Contat Sense? + Hold Input On Off
Inject Start Pulse (sec): 0.5
Inject Stop Pulse (sec): 0.5
Temp Setpoint (¡C): 20
Temp Control? On Off
3
PrevCfg
Page
NextCfg
Page
Figure 3-10 Setting Terminal Signal Parameters
Hold Contact Sense and Hold Input
3. To enable other instruments to stop an injection sequence:
• Set the Hold Contact Sense parameter to the polarity of the incoming hold
signal.
Table 3-3 Hold Logic
Hold Inputs Positive Sense Negative Sense
LOW LOW RUN HOLD
LOW HIGH HOLD HOLD
HIGH LOW HOLD HOLD
HIGH HIGH HOLD RUN
• Set the Hold Input parameter to On.
Main
Page
Note: Set Hold Input to Off for PowerLine control.
65 Startup and Configuration
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Inject Start Pulse
4. The Inject Start default pulse width is 0.5 seconds. Change the pulse width if the
instrument connected to the autosampler requires a different setting.
Inject Stop Pulse
5. The Inject Stop Pulse signal default pulse width is 0.5 seconds. Change the
pulse width if the instrument connected to the autosampler requires a different
setting.
Setting IEEE-488 Address
To ensure that the autosampler is correctly identified when it is part of an IEEE-488
network, verify that the address is a unique number from 2 to 29. The default IEEE-488
address is set to 30.
Note: To use the Waters 717plus Autosampler in an IEEE-488 network, you must change
the address.
To change the address:
1. From the 717plus Main Menu, press Config Page.
2. From Configuration Page 1, press Next Cfg Page three times to view Page 4 of
the Configuration Pages.
3. On Configuration Page 4 (Figure 3-11), highlight the desired IEEE Address field,
type the new address, and press Enter.
3
Note: The address must be unique to the system and must be a number between 2
and 29.
4. Press Reboot System to configure and store the new address.
Note: If the system controller is powered up, rescan the system to view the new
717plus Autosampler address. Refer to the system controller operator's manual for
details.
Configuring the Autosampler 66
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IDLE
Edit: Configuration Page 4 of 4
IEEE Address Assignment
3
Installed IEEE Address:
Desired IEEE Address:
Press REBOOT SYSTEM softkey to
install desired IEEE address.
REBOOT
SYSTEM
PrevCfg
Page
Figure 3-11 Setting IEEE-488 Address
3.6.3 Entering Hardware Changes
To enable the autosampler to adjust to changes in hardware configuration (syringe and
sample loop size), you must enter the changes on Configuration Page 3 (Figure 3-12).
30
20
NextCfg
Page
Main
Page
67 Startup and Configuration
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IDLE
Edit: Configuration Page 3 of 4
Draw Rate ( l/sec):
Syringe Volume ( l)?
Loop Volume ( l)?
Figure 3-12 Configuration Page 3
Entering Syringe Size
To record a change in the syringe size:
1. From the 717plus Main Menu, press Config Page.
2. Press Next Page twice to access Configuration Page 3.
3. Select the appropr iate Syr inge Volume, and press Enter.
The autosampler automatically updates the draw rate to adjust to changes in
syringe volume. If you require a different draw rate, change the rate on
Configuration Page 3 (see Section 4.8.3, Injecting Viscous Samples).
PrevCfg
Page
2.50
25 250 2500
200 2000
NextCfg
Page
Main
Page
3
Entering Sample Loop Size
To record a change in the sample loop volume:
1. From the Main Menu, press Config Page.
2. Press Next Page twice to access Configuration Page 3.
3. Select the applicable Loop Volume and press Enter.
Configuring the Autosampler 68
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3
3.7 System Verification
Perform system verification:
• After installation
• Daily to test the autosampler sample loop
To perform system verification:
1. Using a degassed solution of 100 percent methanol, set the solvent delivery pump
to 1 mL/min.
Note: For daily verification, use the mobile phase that you normally run.
2. From the 717plus Main Menu, press Edit Purge (Figure 3-13).
PURGE
Edit: Purge and Compressibility
Purge Time (min):
Compression Check?
Compression Pressure (psi):
Pressure Decay Time (min):
Compressible Volume ( l):
1.0
Yes
30
0.2
20
No
Pressure Change (psi)
Compressed Volume (psi)
Start
Purge
3. Set Compression Check to Yes and press Enter.
4. Press Start Purge.
5. Record the pressure change and compressed volume. Use these values as a
basis for evaluating mobile phase degassing and sample loop integrity.
69 Startup and Configuration
Main
Page
Figure 3-13 Purge Menu
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6. If the compression exceeds the default compressible volume, degas the mobile
phase and run the compression check again.
7. If the compression check still fails, perform a leak test (Section 6.4.2, Valve Leak
Test).
3.8 Power Down and Storage
If the mobile phase contains buffers, remove the buffers before power down and storage.
This section describes:
• Removing the buffered mobile phase
• Powering down the 717plus Autosampler
• Long-term storage
3.8.1 Removing Buffered Mobile Phase
Remove the mobile phase containing buffer salts as described below:
1. Replace the buffered mobile phase with a solution of 100 percent water, and flush
the sampling system for 10 minutes at 1 mL/min.
2. Run three purges to ensure that the syr inge is well-purged (see Section 3.4.1,
Purging the Autosampler).
3. Replace the needle wash solvent with 90 percent methanol 10 percent water,
and perform a needle wash prime (Section 3.5, Priming the Needle Wash Pump).
4. Replace the water with a solution of 90 percent methanol and 10 percent water.
Flush the sampling system for 3 minutes at 1 mL/min.
5. Purge the autosampler.
3
3.8.2 Powering Down
This section covers procedures for powering down the Waters 717plus autosampler for 1
to 14 days.
1. If the current mobile phase is water, replace the water with a solution of 90 percent
methanol and 10 percent water. Flush the sampling system for 3 minutes at
1 mL/min.
2. Purge the autosampler (see Section 3.4.1, Purging the Autosampler).
3. To power down the autosampler, press 1/0 (on/off).
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Power Down and Storage 70
3
3.8.3 Storage
This section covers procedures for long-term storage of the Waters 717plus autosampler.
If the autosampler will be stored for more than two weeks:
1. Remove buffered mobile phases (see Section 3.8.1, Removing Buffered Mobile
Phase).
2. Power down the autosampler (see Section 3.8.2, Powering Down).
3. Remove the waste lines and needle wash line from their containers.
4. Disconnect the red and blue lines.
5. Disconnect the power line.
71 Startup and Configuration
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4
Operating the Autosampler
This chapter covers 717plus autosampler operation. Provided are procedures for
preparing and loading samples, programming and using the automatic features, and
making a stat run.
4.1 Overview of Operation
Figure 4-1 provides an overview of autosampling.
Note: If the Waters 717plus autosampler is part of an IEEE-488 network, power up the
autosampler before powering up the system controller.
Overview of Operation 72
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4
Operating the
autosampler
Power up autosampler,
detectors, and other
LC components before
system controller.
Prepare samples
and load carousel.
Select needle wash
based on sample
and mobile chemistry.
4
Changing
mobile
phase?
NO
Purge autosampler.
Program auto run.
Equilibrate.
Start auto run.
YES
Flush system.
Perform purge and
compression check.
Figure 4-1 Overview of Operations
73 Operating the Autosampler
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4.2 Preparing Samples
To prepare and load samples into the autosampler, you must:
• Prepare the sample
• Select and fill a sample vial
4.2.1 Preparing Samples
Minimum sample preparation consists of dissolving the sample:
• In a solvent that is compatible with the mobile phase and column chemistry
• At a concentration that permits detection of the analyte
• In a solution that is particle-free and homogeneous
Figure 4-2 details the procedure for preparing a sample.
Preparing Samples 74
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4
Preparing samples
(Section 4.2.1).
4
Normal phase
column?
No
Reverse phase
column?
Ion exchange?
GPC?
Filter samples
with 0.5 µ filter.
Yes
Yes
Yes
Yes
Dissolve in
mobile phase.
Same or weaker
organic component
as mobile phase.
Use a low salt
concentration.
Dissolve in mobile
phase (from the same
bottle).
Load sample vials.
75 Operating the Autosampler
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Figure 4-2 Preparing Samples
Selecting a Solvent
STOP
Note: Prevent precipitation of buffered salts or of sample through careful consideration of
solvent concentration and pH. Whenever possible, use mobile phase as the solvent for
dissolving samples.
Observe the following guidelines when selecting a sample solvent:
• Normal phase column - Use the same solvent that is used for the mobile phase.
• Reverse phase column - Use the same or weaker concentration of the mobile
phase organic component.
• Ion exchange - Use a low salt concentration.
• GPC - Dissolve in the mobile phase (preferably from the same bottle).
Filtering Samples
Unless restricted by sample chemistry, filter prepared samples before placing them in the
sample vials. Filtering with a 0.5 µ filter, such as a Millipore Millex filter unit, prevents
particulate accumulation on internal filters or the column inlet fitting which would result in
an increase in backpressure.
4.2.2 Selecting Sample Vials
The Waters 717plus autosampler is compatible with the complete line of Waters
chromatography sample vials.
Attention: Use only sample vials and supplies from Waters. Use of non-Waters sample
vials, low-volume inserts, or septa may result in damage to the needle.
Selecting Sample Vials
Select a sample vial based on:
• Chemistry of the sample
• Volume of sample
• Volume of injection
• Number of injections
• Volatility of sample
For detail on sample vials, see Appendix E, Selecting Sample Vials.
Assembling Sample Vials
Assemble the sample vials as shown in Figure 4-3.
Preparing Samples 76
4
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STOP
Attention:
dimples in) may cause the cap to fit incorrectly. Also, the use of self-sealing septa may
cause variable injector volumes on multiple injections due to vacuum buildup.
Do not overtighten the cap with a self-sealing septum. Ov ertightening (septum
Screw Cap
Limited Volume
Insert
Snap-on Cap
Septum
Figure 4-3 Sample Vial Assembly
4
4.3 Selecting a Needle Wash Solvent
The needle wash prevents cross-contamination of samples by wiping the needle with
porous, wetted frits. Select a needle wash solvent based on the sample and mobile phase
chemistry . Table 4-1 lists some suggested needle wash solvents. High sample
concentrations may require stronger needle wash solvents.
Attention: Do not use buffers in the needle wash solvent. Buffers decreases seal life.
STOP
Table 4-1 Suggested Needle Wash Solvents
Mobile Phase Needle Wash
Buffered aqueous, reverse phase 50% H2O 50% MeOH
Non aqueous, reverse phase 100% MeOH
77 Operating the Autosampler
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Table 4-1 Suggested Needle Wash Solvents (Continued)
Mobile Phase Needle Wash
Normal phase Mobile phase
GPC Mobile phase
Ion exchange Paired ion reagent in H2O
To use a needle wash:
1. Select a needle wash solvent based on the chemistry of the mobile phase.
2. Place the green line in the needle wash solvent reservoir and place the reservoir
on the same level as the autosampler (Figure 4-4).
Note: To avoid siphoning, do not place the needle wash reservoir above bench height.
For extended storage, replace the needle wash solvent with a recommended storage
solvent (see Section 3.8, Power Down and Storage).
Selecting a Needle Wash Solvent 78
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4
4
STOP
Needle
Wash
Solvent
Home
Display
Contrast
2
3
1
4
Needle wash
pump location
7
0
56
8
9
Clear
Enter
O I
Figure 4-4 Improper Needle Wash Solvent Location
3. With the 717plus autosampler powered on, prime the needle wash pump (see
Section 3.5, Priming the Needle Wash Pump).
4.4 Loading the Carousel
Attention: Use only Waters grey carousels. The Waters 717plus autosampler does not
work with WISP white or brown carousels.
To load the carousel:
1. With the power on, open the sample compartment door. If the door sensor is
enabled (default condition), the autosampler releases the carousel.
79 Operating the Autosampler
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Note: The carousel release is not active when the autosampler is performing a
STOP
purge or a pre-injection sequence.
2. Before loading the sample vials into the carousel, ensure that the carousel is
clean and the holes on top are not blocked.
3. Place the assembled sample vials in the carousel and note the location. The vial
number is located on the rim of the carousel.
Attention: Use of non-Waters sample vials, low-volume inserts, and septa may
result in damage to the needle.
4. Slide the carousel into the sample compartment until it reaches the two
positioning stops on the compartment floor (Figure 4-5).
Home
Display
Contrast
2
1
3
4
56
8
9
7
Clear
0
Enter
O I
Positioning
Stops
Figure 4-5 Inserting the Carousel
5. Close the sample compartment door. The autosampler homes the carousel.
Loading the Carousel 80
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4
4.5 Ensuring Reproducibility
This section covers:
• Overview of Reproducibility
• Purging the Autosampler
• Performing a Compression Check
4.5.1 Overview of Reproducibility
Reproducibility depends on:
• Purity of the mobile phase in the autosampler
• Compressibility of the mobile phase due to dissolved gas
• Integrity of the autoinjector sample loop
Ensuring Reproducibility
1. Run a purge and a compression check:
• To remove mobile phase that has been sitting in the system during a shutdown.
• To check the system on a daily basis for air or solvent leaks.
• To remove the previous mobile phase when changing to a new mobile phase.
• To establish the compressibility for a new mobile phase.
2. Run a purge and a compression check (see Section 4.5.3, Performing a
Compression Check) on the degassed mobile phase.
3. If the mobile phase fails the compression check, degas the solvent (see
Appendix D, Reproducibility and Solvent Degassing).
4. If the degassed mobile phase again fails the compression check, run a leak test
(see Section 6.4.2, Valve Leak Test) to verify the integrity of the sample loop.
4.5.2 Performing a Purge
Perform a purge from the Purge and Compressibility Page.
Purging the Autosampler
To perform a purge using the default values, press the Waters 717plus autosampler keys
as indicated below (Figure 4-6):
81 Operating the Autosampler
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Start
Purge
Figure 4-6 Purging the Autosampler
Changing Purge Time
Change the Purge Time if:
• System flow rates are less than 1 mL/min
• The auxiliary loop is installed
The purge time setting depends on:
• Flow rate of the mobile phase
• Sample loop size
Main Page
Purge
Page
Purge and
Compressibility
Page
To change the Purge Time:
1. From the 717plus Main Page, press Purge Page to display the Purge and
Compressibility page (Figure 4-7).
Ensuring Reproducibility 82
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PURGE
Edit: Purge and Compressibility
4
Purge Time (min):
Compression Check?
Compression Pressure (psi):
Pressure Decay Time (min):
Compressible Volume ( l):
Pressure Change (psi)
Compressed Volume (psi)
Start
Purge
1.0
Yes
30
0.2
20
Main
Page
No
Figure 4-7 Purge and Compressibility Page
2. Calculate the purge time based on the flow rate and sample loop size. The time
must be sufficient to allow three volume changes of the autosampler. The
autosampler volume in Table 4-2 includes the inlet and outlet lines.
Table 4-2 Autosampler Volume
Sample Loop Autosampler Volume
Normal (200 µL) 836 µL
Auxiliary (2.4 mL) 3236 µL
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Table 4-3 lists sample purge times for the two sample loops at selected flow rates.
Table 4-3 Purge Time Examples
Sample
Loop
Normal 0.2 12.5
Auxiliary 0.5 19.4
Flow Rate
(mL/min)
0.5 5.0
>1 2.5
1 9.7
2 4.8
Purge Time
(min)
4.5.3 Performing a Compression Check
The compression check tests for gas in the mobile phase, and, when enabled, occurs
immediately after a purge. For most mobile phases, use the default parameters.
Note: The compression check is only valid using the standard 250 µL syringe and 200 µL
sample loop.
Change the default parameters if:
• Mobile phase is highly compressible (see Appendix D, Reproducibility and Solvent
Degassing).
• Testing for leaks (see Section 6.4.2, Valve Leak Test).
4
Compression Parameters
When enabled, the compression check is executed immediately after a purge. The
parameters are:
• Compression PressureComression Pressure
• Pressure Decay Time
• Compressible V olume
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Compression Pressure
For testing the compressibility of the mobile phase, use 30 psi. For leak testing, use the
maximum pressure.
Range 30 to 350 psi
Default 30
Pressure Decay Time
Sets the length of time the system pauses before recompressing the mobile phase in the
sample loop. The default value is sufficient for most applications. The longer the decay
time, the more rigorous the test.
Range 0.0 to 3.0 min
Default 0.2 min
Compressible V olume
4
The default value is sufficient for most applications. Changes to the compression limit are
dependent on the solvent used for the mobile phase. If the mobile phase is highly
compressible, increase the compression limit setting (see Appendix D, Reproducibility and
Solvent Degassing).
Range 5 to 30 µL
Default 20 µL
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Performing a Compression Check
To perform a compression check, press the keys indicated in Figure 4-8:
Main Page
Purge
Page
PURGE
Edit Purge and
Compressibility Page
Purge Time (min):
Compression Check?
Compression Pressure (psi):
Pressure Decay Time (min):
Compressible Volume ( l):
Pressure Change (psi)
Compressed Volume (psi)
1.0
Yes
30
0.2
20
No
Yes No
Start
Purge
Main
Page
Start
Purge
Figure 4-8 Running a Compressibility Test
• If the compression limit is exceeded, the following message appears:
Compressibility check failed
• If the compression check fails, re vie w Section 4.1, Ov erview of Operation, for further
testing.
4
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4
4.6 Running Autosampling
This section describes:
• Programming an auto run
• Programming step functions
• Using Auto Standards
• Using Auto Addition
• Using Auto Transfer
• Programming the Event Output
• Starting and stopping an auto run
• Monitoring auto run status
Features of Auto Run
Use Auto Run mode to program, run, and monitor sample injections. Auto Run mode
allows:
• Multi-method programming - Allows programming of up to 96 different steps
(methods). Each step can use different numbers of injections, volumes, run times,
and optional functions.
• Unattended operation - Provides injection start and stop output signals for
controlling external devices.
• Programmable output signal - Allows the 717plus to control external devices
during a run.
• Auto Standard, Auto Addition, and Auto Transfer functions - Allow automated
operation for standards, pre-injection addition of samples, and automatic
pre-injection transfer and mixing.
Overview of Programming
Figure 4-9 is an overview of the steps involved in programming and running an auto run.
87 Operating the Autosampler
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Load samples
P
(
1)
P
(
2)
P
:
5)
P
(
6)
rogram the step on the
Auto Run page
Section 4.6.
rogram step functions
for the step
Section 4.6.
rogram the option for the step
Auto Standards (Section 4.6.3)
Auto Addition (Section 4.6.4)
Transfer (Section 4.6.
Auto
rogram the event
output for the step
Section 4.6.
Figure 4-9 Overview of Programming
4
4.6.1 Programming Auto Run
Program and start an Auto Run from the Edit: Auto Run screen (Figure 4-10).
This section describes:
• Using the Auto Run screen
• Entering step parameters
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4.6.1.1 Using the Auto Run Screen
Display the Edit: Auto Run screen by pressing the Auto Page key on the Main Menu.
The Edit: Auto Run screen (see Figure 4-10) lets you program up to 96 steps.
IDLE
Edit: Auto Run
Step
From
Vial
1
2
3
4
11
End of Table.
Start
Auto
2
5
8
To
Vial
4
7
10
13
Insert
Line
Inj
Delete
Options
#
Inj
Vol
1
15.0
1
15.0
1
15.0
1
15.0
Run
Time
10.0
10.0
10.0
10.0
Step
Function
Trns
Main
Page
4
Figure 4-10 Edit: Auto Run Screen
Moving Through the T able
To move through the table you can:
Press: To:
Home once Move the cursor to the
top of the page
Home twice Move the cursor to
step 1
Arrow keys Moves the cursor up
and down lines and
between parameters
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Enter: To:
Step number Advance to a step
96 for step number Move the cursor to the
last step (whether or not
there are 96 steps
programmed)
Note: To move through the table a screen at a time (10 lines), enter step numbers in
increments of 10. For example, enter 11, 21, 31, and so on.
Inserting a Line
To insert a line:
1. Use the arrow keys to move to a step number where the new line will be inserted.
2. Press Insert Line. The 717plus duplicates the previous line, and renumbers all
subsequent lines.
Deleting a Line
To delete a line:
1. Use the arrow keys to move to a step number to delete.
2. Press Delete Options, and the Delete Line function key appears.
3. Press Delete Line. The 717plus removes the line , and renumbers all subsequent
lines.
Deleting a Table
4. To delete a table:
1. Press Delete Options, and the Delete Table function key appears.
2. Press Delete Table. After you confirm your intention to clear the table, the
autosampler removes all data on the page.
Options
If you have enabled an option for a step, the option is listed after the Run Time field.
Note: If you have disabled an option, it is not listed for the step.
Running Autosampling 90
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4.6.1.2 Entering Step Parameters
You must enter a value for each parameter in a step. Parameters you enter are saved in
permanent memory.
Before Programming
Load the required vials in the carousel, noting the carousel positions.
Note: Standard vials and common vials do not ha ve to be loaded in consecutive positions.
Programming
To program:
Step
1. Place the cursor on a blank line, then press Enter.
The 717plus inserts a new line and copies the information, including step
function and option settings, from the previous line.
You can program up to 96 different steps. Each vial included in the step shares
the same number of injections, injection volume, run time, step functions, and
options. By changing steps and step parameters, you can run a different method
using the same set of vials.
4
Vial From/To
2. Enter a vial number in the From Vial and To Vial fields. Vial number defaults to
the values you entered on the previous line. Valid entries are 1 to 48 or 1 to 96,
depending on the type of carousel in use.
When injecting from a single vial, enter the same vial number in the From and To
fields. When injecting from a sequence of vials, enter the starting vial in the From
Vial field and the last vial in the To Vial field.
STOP
# Inj
91 Operating the Autosampler
Attention: The vial injection sequence entered in the From/To field is continuous. If
a vial is missing, the autosampler will inject air into the LC system.
3. Enter the number of injections to make from each vial. Valid entries are 1 to 99.
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Inj V ol
4. Enter the injection volume. The maximum injection volume depends on the size
of the sample loop.
Sample Loop Size Range (µL)
Standard 0 to 200
Auxiliary 0 to 2000
Run Time
5. Enter the r un time in minutes. Valid entries are 0 to 999.9.
The run time clock starts when the sample enters the mobile phase stream. At
the same time, the autosampler closes the Inject Start contact. When the run
time clock expires, the autosampler closes the Inject Stop contact and begins
another injection sequence unless a Report Delay has been configured.
Note: You can delay the next injection in order to complete an integration printout.
Use the Report Delay or External Hold input signal (see Section 3.6.2, Setting
Parameters for LC System Operation).
Step Functions
6. Program step functions (described in Section 4.6.2, Programming Step
Functions).
Note: You can program only one set of step functions and one option per step.
4.6.2 Programming Step Functions
Use the Step Function screen to select the following parameters for each Auto Run step:
• Needle Position
• Purge After Step
• Options for an Auto Run step
• Programmable Event outputs
This section describes the Step Function screen (Figure 4-11).
4
Running Autosampling 92
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IDLE
Edit: Step Function 1 of 1 Trns
Editing Step: 1
Needle Position (%)? 25 50 75 100
Purge After Step? Yes No
Option? None Stds Addn Trns
Run Event (0=Off 1=On)
Time Time Prog Event
10.0 1.0
2.0
3.0
4.0
1
0
1
0
Trns
Page
Auto
Page
Figure 4-11 Edit: Step Function Screen
Note: Figure 4-11 is an example of the Edit: Step Function screen with the Auto Transfer
option selected. When other options are selected, keys for the selected function appear.
4
If no option is enabled, the option field displays “None”, and no option key appears.
Programming Step Functions
To program step functions:
1. Display the Edit: Step Function screen by pressing Step Function on the Edit:A uto
Run screen.
The currently selected step number appears on the Edit: Step Function screen.
Editing Step
2. To change the step number, enter a new number on the keypad and press Enter .
Needle Position
3. Move the cursor to the Needle Position% line. This determines needle
withdrawal position. Use the right/left arrow keys to select the desired position of
25, 50, 75, or 100%. Default is 100%.
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The picture of the vial displayed in the upper-right corner of the screen shows
the selected needle position.
Purge After Step
4. If desired, move the cursor to Purge After Step?, and select Yes. Default is No.
Step function purges use the Purge Parameters set on the Purge and
Compressibility screen. For information on setting the Purge Time, refer to
Section 4.5.2, Performing a Purge.
Option
5. Move the cursor to the Option? field, then use the arrow keys to select the
option for the step. The default is None.
Note: If you select None to disable an option, you delete all information
programmed for the option. To disable the option without deleting, display the option
screen and set the option to No.
6. Program the option for the step. For information on programming the options,
refer to:
• Section 4.6.3, Using Auto Standards
• Section 4.6.4, Using Auto Addition
• Section 4.6.5, Using Auto Transfer
Note: You can program a different option for each step (not multiple options per
step).
Event Output
7. Program the event output for the step (see Section 4.6.6, Programming the Event
Output).
4.6.3 Using Auto Standards
This section describes:
• Overview of Auto Standards
• Programming and Running Auto Standards
• Example Auto Standard Run
4
Running Autosampling 94
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4.6.3.1 Overview of Auto Standards
Auto Standards
Use the Auto Standards routine to program standard vials to run automatically during an
Auto Run.
Use the Auto Standards menu routine to enter standard vial parameters, along with the
number of sample vials to run between standard vials.
The Auto Standards table is saved in permanent memory.
Standard Vials
You can specify up to five standard vials for each Auto Run step. Standard vials:
• Can be unique or repeated
• Do not have to be in consecutive positions in the carousel
• Can be different for each step
Auto Standards Sequence
During an Auto Standards run, the 717plus:
• Injects standards (specified on Auto Standards screen)
• Injects samples (specified on Auto Run screen)
• Re-injects the same standards (specified on Auto Standards screen)
4
Section 4.6.3.3, Example Auto Standard Run, includes an example of an
Auto Standards run.
4.6.3.2 Programming and Running Auto Standards
Before Programming
Before programming:
• Place your samples in the carousel, noting each position (usually in sequential
order)
• Place your standards in the carousel, noting each position (usually in sequential
order)
• Program the step on the Auto Run screen (see Section 4.6.1, Programming Auto
Run)
• Program the step functions for the step (see Section 4.6.2, Programming Step
Functions)
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Programming Auto Standards
To program Auto Standards:
1. From the Edit: Auto Run screen (see Figure 4-10), select a step, then press Step
Function to display the Edit: Step Function screen.
Note: For instructions on setting Needle Position and Purge, refer to Section 4.6.2,
Programming Step Functions.
2. From the Edit: Step Function screen (see Figure 4-11), press the down-arrow
key to move the cursor to the Option? field.
3. Press the right-arrow key to move the cursor to the Stds selection. The Stds
Page key appears on the screen.
4. Press Stds Page to display the Edit: Auto Standards screen (Figure 4-12).
IDLE
Edit: Auto Standards 1 of 1 Stds
Editing Step:
Run Standards? Yes No
Vials Between: 1
Vial
Delete
Table
1
Delete
Inj
Vol
15.0
Line
#
Inj
1
Run
Time
1.0
Step
Function
Figure 4-12 Edit: Auto Standards Screen
5. At the Run Standards? field, select Yes (default).
6. Move the cursor to the Vials Between field. Enter the number of sample vials to
run between standards (1 to 48 or 1 to 96, depending on carousel type).
Running Autosampling 96
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7. Press the down-arrow key to move the cursor to the Vial field. Enter the
following parameters for each standard vial. You can enter up to five standard
vials for each Auto Run step.
Parameter Description/Range
Vial Carousel number, 1 to 96
4
Inj V ol 0.0 to 200.0 µL or
0.0 to 2000.0 µL
# Inj Number of injections for standard vial,
1 to 99
Run Time Total run time from injection to Inject
Stop signal, 0.0 to 999.9 min
1
Dependent on sample loop installed in Waters 717plus
1
Running Auto Standards
To start the Auto Run:
1. When programming is complete, press Step Function, then Auto Page to return to
the Edit: Auto Run screen.
2. Press Start Auto. The Auto Standards routine runs as part of each programmed
step. A message appears indicating that Auto Standards is running. You cannot
change screen settings of the currently running step.
Turning off Auto Standards
To turn off Auto Addition on the Edit Auto Addition screen, select No at the Run Addition?
field. The information programmed f or A uto Standards is sa ved, b ut A uto Standards do not
run.
When Auto Standards are turned off, the Stds notation is not displayed on the Auto Run
screen.
Note: If you turn off Auto Standards on the Edit: Step Function screen (by setting the
Option field to None), you delete the information programmed for Auto Standards.
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4.6.3.3 Example Auto Standard Run
V
V
V
V
V
V
V
V
V
V
V
In an Auto Standards run, standards always run at the beginning of a step, and may run
during or at the end of a step.
Whether standards run during or at the end of a step is determined by the number of vials
in a step and the number of vials specified to run between standards.
Note: If you run a stat sample during an Auto Standard run, the stat sample is not
considered to be one of the sample vials running between standards.
Standards During or at End of Run
If the number of vials in the step is
equal
to the Vials Between value, standards run at the
beginning and at the end of the step.
If the number of vials in the step is a
multiple
of the Vials Between v alue , standards run at
the beginning, during, and at the end of the step (Figure 4-13).
Step
1
ial
1
ial
1
Auto Run
From
2
ial
2
3
To
7
ial
1
ial
ial
ial
4
1
Auto Standards
Vials Between = 3
Standard Vial = 1
ial
5
6
Figure 4-13 Example Auto Standard Run 1
No Standards at End of Run
Standards do not run after the last sample if (Figure 4-14):
• The number of vials in the step is
• The number of vials in the step is
not
equal to the Vials Between value.
not
a multiple of Vials Between value.
ial
ial
ial
1
7
4
Running Autosampling 98
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V
V
V
V
V
V
V
V
V
V
Step
A
1
uto Run
From
2
Auto Standards
To
7
Vials Between =4
Standard Vial = 1
4
ial
1
ial
ial
ial
1
2
ial
3
4
Figure 4-14 Example Auto Standard Run 2
4.6.4 Using Auto Addition
This section describes:
• Overview of Auto Addition
• Programming and Running Auto Addition
• Example Auto Addition Run
4.6.4.1 Overview of Auto Addition
Auto Addition
Auto Addition withdraws specified volumes from common vials, then withdraws from a
sample vial. The common solutions and the sample are all contained
before injection. You can set a time delay for the injection of the sample and common
solutions.
Auto Addition is useful for applications requiring automatic addition of derivatizing agents ,
standards, or reference peaks.
ial
1
ial
5
1
ial
ial
ial
6
7
in the sample loop
The Auto Addition table is saved in permanent memory.
Common Vials
You can specify up to five common vials for each Auto Run step. Common vials:
• Can be unique or repeated
• Do not have to be in consecutive positions in the carousel
• Can be different for each step
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