Waters 717plus User manual

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Waters 717plus Autosampler
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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Attention: The Waters 717plus Autosampler may be used for IN VITRO diagnostic
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
responsible for compliance could void the user’s authority to operate the equipment.
Attention: This equipment has been tested and found to comply with the limits for a Class
A digital device, pursuant to Part 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 covers.
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 receives its electrical power from a local level, such
as an electrical wall outlet.
STOP
STOP
STOP
STOP
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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 5
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
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6 Table of Contents
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
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Table of Contents 7
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
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8 Table of Contents
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
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Table of Contents 9
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 Tables........................................................ 147
6.4 Troubleshooting Procedures ............................................... 155
6.4.1 Manual Syringe Purge............................................. 155
6.4.2 Valve 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
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10 Table of Contents
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
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Table of Contents 11
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 andVoltage 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
List of Figures
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12 Table of Contents
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
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Table of Contents 13
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
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Table of Contents 14
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 Autosampler 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
List of Tables
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How To Use This Guide 15
How to Use This Manual
Purpose of This Manual
The Waters 717plus Operator’s Manual describes the features and use of the Waters 
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.
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 Provides procedures for starting up, calibrating,
configuring, verifying, and powering down.
Chapter 4, Operating the
Autosampler Provides procedures for preparing and loading
samples, programming and using the automatic
features, and making a stat run.
Chapter 5, Maintenance Provides procedures for defrosting the
heater/cooler and for replacing the syringe, seal
pak, and in-line filters.
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16 How to Use This Guide
Related Adobe™ Acrobat Reader Documentation
For detailed information about using the Adobe Acrobat Reader, refer to the Adobe
Acrobat Reader Online Guide .This Online Guide covers procedures such as viewing,
navigating and printing electronic documentation from Adobe Acrobat Reader.
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.
• PurpleText 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 tells the software how to acquire data.
Chapter 6, Troubleshooting Provides troubleshooting tables to aid in problem
diagnosis and information about error messages.
Appendix A, Specifications Lists Waters 717plus specifications.
Appendix B, Spare Parts Lists spare parts.
Appendix C, Warranty
Information Contains the warranty and a key to serial number
interpretation.
Appendix D,
Reproducibility and
Solvent Degassing
Provides information about the factors affecting
reproducibility and the theory and methods of
solvent degassing.
Appendix E, Selecting
Sample Vials Provides information about selecting sample
vials.
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How To Use This Guide 17
•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.
• 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.
STOP
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18 Introduction
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.
Figure 1-1 Waters 717plus Autosampler
123
456
789
0
Home
Clear Enter
Display
Contrast
Waters 717plus Autosampler
O I
MILLIPORE
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1
Features 19
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.
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.
• AutoTransfer - 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.
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