Waters 717plus User manual

Waters 717plus Autosampler
Operator’s Manual
34 Maple Street
Milford, MA 01757
173-02TP, Revision 3

NOTICE
The information in this document is subject to change without notice and should not be
construed as a commitment by Waters Corporation. Waters Corporation assumes no
responsibility for any errors that may appear in this document. This manual is believed to
be complete and accurate at the time of publication. In no event shall Waters Corporation
be liable for incidental or consequential damages in connection with or arising from the
use of this manual.
1993–2002 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.
Millennium and Waters are registered trademarks, and ExpertEase, LAC/E, Maxima,
PowerLine, SAT/IN, and WISP are trademarks of Waters Corporation.
Millex is a trademark of Millipore Corporation.
Torx is a registered trademark of Camcar, Division of Textron, Inc.
All other trademarks or registered trademarks are the sole property of their respective
owners.

Note: When you use the instrument, follow generally accepted procedures for quality
control and methods development.
If you observe a change in the retention of a particular compound, in the resolution
between two compounds, or in peak shape, immediately determine the reason for the
changes. Until you determine the cause of a change, do not rely on the separation results.
Note: 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
Atención: 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.
Important : Toute modification sur cette unité n’ayant pas été expressément approuvée
par l’autorité responsable de la conformité à la réglementation peut annuler le droit de
l’utilisateur à exploiter l’équipement.
Achtung: Jedwede Änderungen oder Modifikationen an dem Gerät ohne die
ausdrückliche Genehmigung der für die ordnungsgemäße Funktionstüchtigkeit
verantwortlichen Personen kann zum Entzug der Bedienungsbefugnis des Systems
führen.
Avvertenza: eventuali modifiche o alterazioni apportate a questa unità e non
espressamente approvate da un ente responsabile per la conformità annulleranno
l’autorità dell’utente ad operare l’apparecchiatura.
Atención: cualquier cambio o modificación realizado a esta unidad que no haya sido
expresamente aprobado por la parte responsable del cumplimiento puede anular la
autorización de la que goza el usuario para utilizar el equipo.

Caution: Use caution when working with any polymer tubing under pressure:
•Always wear eye protection when near pressurized polymer tubing.
•Extinguish all nearby flames.
•Do not use Tefzel tubing that has been severely stressed or kinked.
•Do not use Tefzel tubing with tetrahydrofuran (THF) or concentrated nitric or
sulfuric acids.
•Be aware that methylene chloride and dimethyl sulfoxide cause Tefzel tubing to
swell, which greatly reduces the rupture pressure of the tubing.
Attention : soyez très prudent en travaillant avec des tuyaux de polymères sous
pression :
•Portez toujours des lunettes de protection quand vous vous trouvez àproximitéde
tuyaux de polymères.
•Eteignez toutes les flammes se trouvant àproximité.
•N'utilisez pas de tuyau de Tefzel fortement abîméou déformé.
•N'utilisez pas de tuyau de Tefzel avec de l'acide sulfurique ou nitrique, ou du
tétrahydrofurane (THT).
•Sachez que le chlorure de méthylène et le sulfoxyde de diméthyle peuvent
provoquer le gonflement des tuyaux de Tefzel, diminuant ainsi fortement leur
pression de rupture.
Vorsicht: Bei der Arbeit mit Polymerschläuchen unter Druck ist besondere Vorsicht
angebracht:
•In der Nähe von unter Druck stehenden Polymerschläuchen stets Schutzbrille
tragen.
•Alle offenen Flammen in der Nähe löschen.
•Keine Tefzel-Schläuche verwenden, die stark geknickt oder überbeansprucht sind.
•Tefzel-Schläuchenichtfür Tetrahydrofuran (THF) oder konzentrierte Salpeter- oder
Schwefelsäure verwenden.
•Durch Methylenchlorid und Dimethylsulfoxid können Tefzel-Schläuche quellen;
dadurch wird der Berstdruck des Schlauches erheblich reduziert.

Precauzione: prestare attenzione durante le operazioni con i tubi di polimero sotto
pressione:
•Indossare sempre occhiali da lavoro protettivi nei pressi di tubi di polimero
pressurizzati.
•Estinguere ogni fonte di ignizione circostante.
•Non utilizzare tubi Tefzel soggetti a sollecitazioni eccessive o incurvati.
•Non utilizzare tubi Tefzel contenenti tetraidrofurano (THF) o acido solforico o nitrico
concentrato.
•Tenere presente che il cloruro di metilene e il dimetilsolfossido provocano
rigonfiamento nei tubi Tefzel, che riducono notevolmente il limite di pressione di
rottura dei tubi stessi.
Advertencia: manipular con precaución los tubos de polimero bajo presión:
•Protegerse siempre los ojos a proximidad de tubos de polimero bajo presión.
•Apagar todas las llamas que estén a proximidad.
•No utilizar tubos Tefzel que hayan sufrido tensiones extremas o hayan sido
doblados.
•No utilizar tubos Tefzel con tetrahidrofurano o ácidos nítrico o sulfúrico
concentrados.
•No olvidar que el cloruro de metileno y el óxido de azufre dimetilo inflan los tubos
Tefzel lo que reduce en gran medida la presión de ruptura de los tubos.

Caution: The user shall be made aware that if the equipment is used in a manner not
specified by the manufacturer, the protection provided by the equipment may be impaired.
Attention : L’utilisateur doit être informéque si le matériel est utiliséd’une façon non
spécifiée par le fabricant, la protection assurée par le matériel risque d’être défectueuses.
Vorsicht: Der Benutzer wird darauf aufmerksam gemacht, dass bei unsachgemäßer
Verwenddung des Gerätes unter Umständen nicht ordnungsgemäß funktionieren.
Precauzione: l’utente deve essere al corrente del fatto che, se l’apparecchiatura viene
usta in un modo specificato dal produttore, la protezione fornita dall’apparecchiatura
potràessere invalidata.
Advertencia: El usuario deberásaber que si el equipo se utiliza de forma distinta a la
especificada por el fabricante, las medidas de protección del equipo podrían ser
insuficientes.

Caution: To protect against fire hazard, replace fuses with those of the same type and
rating.
Attention : Remplacez toujours les fusibles par d’autres du même type et de la même
puissance afin d’éviter tout risque d’incendie.
Vorsicht: Zum Schutz gegen Feuergefahr die Sicherungen nur mit Sicherungen des
gleichen Typs und Nennwertes ersetzen.
Precauzione: per una buona protezione contro i rischi di incendio, sostituire i fusibili con
altri dello stesso tipo e amperaggio.
Precaución: sustituya los fusibles por otros del mismo tipo y características para evitar
el riesgo de incendio.

Caution: To avoid possible electrical shock, power off the instrument and disconnect the
power cord before servicing the instrument.
Attention : Afin d’éviter toute possibilitéde commotion électrique, mettez hors tension
l’instrument et débranchez le cordon d’alimentation de la prise avant d’effectuer la
maintenance de l’instrument.
Vorsicht: Zur Vermeidung von Stromschlägen sollte das Gerät vor der Wartung
abgeschaltet und vom Netz getrennt werden.
Precauzione: per evitare il rischio di scossa elettrica, spegnere lo strumento e
scollegare il cavo di alimentazione prima di svolgere la manutenzione dello strumento.
Precaución: para evitar choques eléctricos, apague el instrumento y desenchufe el
cable de alimentación antes de realizar cualquier reparación en el instrumento.

Commonly Used Symbols
Direct current
Courant continu
Gleichstrom
Corrente continua
Corriente continua
Alternating current
Courant alternatif
Wechselstrom
Corrente alternata
Corriente alterna
Protective conductor terminal
Borne du conducteur de protection
Schutzleiteranschluss
Terminale di conduttore con protezione
Borne del conductor de tierra

Frame or chassis terminal
Borne du cadre ou du châssis
Rahmen- oder Chassisanschluss
Terminale di struttura o telaio
Borne de la estructura o del chasis
Caution or refer to manual
Attention ou reportez-vous au guide
Vorsicht, oder lesen Sie das Handbuch
Prestare attenzione o fare riferimento alla guida
Actúe con precaución o consulte la guía
Caution, hot surface or high temperature
Attention, surface chaude ou température élevée
Vorsicht, heiße Oberfläche oder hohe Temperatur
Precauzione, superficie calda o elevata temperatura
Precaución, superficie caliente o temperatura elevada
Commonly Used Symbols (Continued)

Caution, risk of electric shock (high voltage)
Attention, risque de commotion électrique (haute tension)
Vorsicht, Elektroschockgefahr (Hochspannung)
Precauzione, rischio di scossa elettrica (alta tensione)
Precaución, peligro de descarga eléctrica (alta tensión)
Caution, risk of needle-stick puncture
Attention, risques de perforation de la taille d’une aiguille
Vorsicht, Gefahr einer Spritzenpunktierung
Precauzione, rischio di puntura con ago
Precaución, riesgo de punción con aguja
Caution, ultraviolet light
Attention, rayonnement ultrviolet
Vorsicht, Ultraviolettes Licht
Precauzione, luce ultravioletta
Precaución, emisiones de luz ultravioleta
Commonly Used Symbols (Continued)
UV

717plus Autosampler Information
Intended Use
The Waters 717plus Autosampler can be used for in-vitro diagnostic testing to analyze
many compounds, including diagnostic indicators and therapeutically monitored
compounds. When you develop methods, follow the “Protocol for the Adoption of
Analytical Methods in the Clinical Chemistry Laboratory,”American Journal of Medical
Technology, 44, 1, pages 30–37 (1978). This protocol covers good operating procedures
and techniques necessary to validate system and method performance.
Biological Hazard
When you analyze physiological fluids, take all necessary precautions and treat all
specimens as potentially infectious. Precautions are outlined in “CDC Guidelines on
Specimen Handling,”CDC –NIH Manual, 1984.
Calibration
Follow acceptable methods of calibration with pure standards to calibrate methods. Use a
minimum of five standards to generate a standard curve. The concentration range should
cover the entire range of quality-control samples, typical specimens, and atypical
specimens.
Quality Control
Routinely run three quality-control samples. Quality-control samples should represent
subnormal, normal, and above-normal levels of a compound. Ensure that quality-control
sample results are within an acceptable range,and evaluate precision from day to day and
run to run. Data collected when quality-control samples are out of range may not be valid.
Do not report this data until you ensure that chromatographic system performance is
acceptable.

Table of Contents 14
Preface ....................................................................................... 24
Chapter 1
Introduction ...................................................................................... 27
1.1 Description............................................................................ 27
1.2 Features................................................................................ 28
1.3 Components and Subsystems.............................................. 31
Chapter 2
Installation ....................................................................................... 33
2.1 Site Requirements ................................................................ 33
2.2 Unpacking and Inspection..................................................... 35
2.3 Making the Power Supply Connection .................................. 36
2.4 Connecting Fluid and Drain Lines ........................................ 36
2.5 Connecting Communication Cables ..................................... 39
2.5.1 Making Terminal Strip Connections........................... 40
2.5.2 Making IEEE-488 Network Connections.................... 45
2.5.3 Connecting RS-232 Output to Data Module.............. 46
2.6 Changing the Hardware Configuration.................................. 47
2.6.1 Removing/Replacing the 717plus Cover.................... 47
2.6.2 Installing the Heater/Cooler....................................... 49
2.6.3 Installing the Large Sample Loop.............................. 52
Table of Contents

Table of Contents 15
Chapter 3
Startup and Configuration ................................................................ 55
3.1 Powering Up the Autosampler............................................... 55
3.2 Using the Front Panel............................................................ 56
3.2.1 Accessing Menus....................................................... 57
3.2.2 Entering Operating Parameters................................. 58
3.3 Flushing the Autosampler ..................................................... 59
3.4 Calibrating the Seal Pak........................................................ 59
3.4.1 Purging the Autosampler ........................................... 59
3.4.2 Auto Zeroing the Transducer...................................... 60
3.4.3 Calibrating the Seal Pak ............................................ 62
3.5 Priming the Needle Wash Pump........................................... 64
3.6 Configuring the Autosampler ................................................ 65
3.6.1 Overview of Configuration ......................................... 65
3.6.2 Setting Parameters for LC System Operation............ 68
3.6.3 Entering Hardware Changes ..................................... 72
3.7 System Verification ............................................................... 74
3.8 Power Down and Storage ..................................................... 75
3.8.1 Removing Buffered Mobile Phase ............................. 75
3.8.2 Powering Down.......................................................... 75
3.8.3 Storage...................................................................... 76
Chapter 4
Operating the Autosampler .............................................................. 77
4.1 Overview of Operation .......................................................... 77
4.2 Preparing Samples ............................................................... 79
4.2.1 Preparing Samples.................................................... 79

Table of Contents 16
4.2.2 Selecting Sample Vials.............................................. 81
4.3 Selecting a Needle Wash Solvent......................................... 82
4.4 Loading the Carousel............................................................ 84
4.5 Ensuring Reproducibility....................................................... 86
4.5.1 Overview of Reproducibility....................................... 86
4.5.2 Performing a Purge.................................................... 87
4.5.3 Performing a Compression Check............................. 89
4.6 Running Autosampling.......................................................... 91
4.6.1 Programming Auto Run ............................................. 92
4.6.2 Programming Step Functions .................................... 96
4.6.3 Using Auto Standards ............................................... 98
4.6.4 Using Auto Addition ................................................ 102
4.6.5 Using Auto Transfer ................................................. 106
4.6.6 Programming the Event Output ............................... 113
4.6.7 Starting and Stopping an Auto Run......................... 114
4.6.8 Monitoring Auto Run Status..................................... 115
4.7 Making a Stat Run .............................................................. 116
4.8 Sampling Considerations.................................................... 119
4.8.1 Temperature Control................................................ 119
4.8.2 Microbore/Semiprep Injections................................ 120
4.8.3 Injecting Viscous Samples ...................................... 123
4.8.4 Purging During an Auto Run.................................... 124
4.8.5 Using Buffered Mobile Phase .................................. 125

Table of Contents 17
Chapter 5
Maintenance .................................................................................. 127
5.1 Defrosting the Heater/Cooler .............................................. 127
5.2 Replacing the Syringe......................................................... 129
5.2.1 Removing the Syringe ............................................. 129
5.2.2 Installing the New Syringe....................................... 132
5.3 Replacing the Seal Pak....................................................... 135
5.3.1 Removing the Injector.............................................. 136
5.3.2 Removing the Seal Pak ........................................... 137
5.3.3 Replacing the Needle .............................................. 138
5.3.4 Installing a New Seal Pak........................................ 139
5.3.5 Installing the Injector................................................ 139
5.3.6 Calibrating the Seal Pak .......................................... 140
5.4 Replacing In-Line Filters..................................................... 140
Chapter 6
Troubleshooting ............................................................................. 143
6.1 Safety and Handling............................................................ 143
6.2 Error Messages................................................................... 144
6.2.1 Informational Error Messages.................................. 145
6.2.2 Calibration (CAL) Error Messages........................... 145
6.2.3 Carousel (CAR) Error Messages............................. 146
6.2.4 Heater/Cooler (H/C) Error Messages ...................... 147
6.2.5 Injector (INJ) Error Messages.................................. 147
6.2.6 Syringe (SYR) Error Messages ............................... 148
6.3 Troubleshooting Tables........................................................ 148

Table of Contents 18
6.4 Troubleshooting Procedures ............................................... 154
6.4.1 Manual Syringe Purge............................................. 154
6.4.2 Valve Leak Test........................................................ 155
6.4.3 Manual Transducer Adjustment ............................... 158
Appendix A
Specifications ................................................................................. 161
Appendix B
Spare Parts..................................................................................... 164
Appendix C
Reproducibility and Solvent Degassing.......................................... 167
C.1 Factors Affecting Reproducibility ....................................... 167
C.1.1 Chemical Factors Affecting Reproducibility ............ 167
C.1.2 Instrument Factors Affecting Reproducibility........... 168
C.2 Solvent Degassing ............................................................ 169
C.2.1 Theory of Solvent Degassing ................................. 169
C.2.2 Solvent Degassing Methods ................................... 170
C.2.3 Solvent Degassing Considerations......................... 171
Appendix D
Selecting Sample Vials................................................................... 173
Index ..................................................................................... 175

List of Figures 19
1-1 Waters 717plus Autosampler.........................................................27
1-2 Waters 717plus Autosampler Subsystems....................................32
2-1 Waters 717plus Autosampler Site Requirements..........................34
2-2 Fluid Line Connections..................................................................37
2-3 Drain Line Connections .................................................................38
2-4 Autosampler Rear Panel................................................................39
2-5 Terminal Strip.................................................................................42
2-6 IEEE-488 Connections ..................................................................46
2-7 Removing the Autosampler Cover.................................................48
2-8 Installing Heater/Cooler................................................................. 50
2-9 Connecting the Heater/Cooler Power Cord and
Temperature Probe........................................................................51
2-10 Installing the Temperature Probe...................................................52
2-11 Disconnecting the Sample Loop....................................................53
3-1 Power Switch Location...................................................................55
3-2 Main Menu.....................................................................................56
3-3 Front Panel ....................................................................................57
3-4 717plus Autosampler Menu Flowchart .......................................... 58
3-5 Path to Auto Zero Pressure Page..................................................61
3-6 Path to Seal Pak Calibration Page.................................................63
3-7 Priming the Needle Wash Pump.................................................... 64
3-8 Autosampler Configuration Flowchart............................................66
3-9 Setting the Integrator Report Delay...............................................69
3-10 Setting Terminal Signal Parameters...............................................70
3-11 Setting IEEE-488 Address.............................................................72
3-12 Configuration Page 3.....................................................................73
3-13 Purge Menu...................................................................................74
List of Figures

List of Figures 20
4-1 Overview of Operations .................................................................78
4-2 Preparing Samples........................................................................80
4-3 Sample Vial Assembly...................................................................82
4-4 Improper Needle Wash Solvent Location ......................................84
4-5 Inserting the Carousel ...................................................................85
4-6 Purging the Autosampler ...............................................................87
4-7 Purge and Compressibility Page ................................................... 88
4-8 Running a Compressibility Test .....................................................90
4-9 Overview of Programming.............................................................92
4-10 Edit: Auto Run Screen...................................................................93
4-11 Edit: Step Function Screen............................................................ 96
4-12 Edit: Auto Standards Screen .........................................................99
4-13 Example Auto Standard Run 1 ....................................................101
4-14 Example Auto Standard Run 2 ....................................................101
4-15 Auto Addition Screen................................................................... 104
4-16 Auto Addition Example ................................................................ 106
4-17 Auto Transfer Screen ................................................................... 108
4-18 Transfer Before Step.................................................................... 111
4-19 Transfer Before Vial......................................................................112
4-20 Transfer Before Injection.............................................................. 113
4-21 Edit: Step Function Screen.......................................................... 114
4-22 Auto Run Status Screen ..............................................................115
4-23 Edit Stat Run Screen................................................................... 117
4-24 Status: Stat Run........................................................................... 118
4-25 Setting Sample Chamber Temperature ....................................... 120
4-26 Changing Syringe Configuration.................................................. 121
4-27 Entering the Semiprep Configuration...........................................122
4-28 Setting Sample Draw Rate .......................................................... 124
4-29 Enabling Auto Purge.................................................................... 125
4-30 Enabling Purge in Idle.................................................................126