SpectraSYSTEM P1000 Isocratic Pump

SpectraSYSTEM P1000 Isocratic Pump
SpectraSYSTEM
P1000 Isocratic Pump
User Guide
A0099-97003 Revision A
August 2008
© 2008 Thermo Fisher Scientific Inc. All rights reserved.
Kel-F is a registered trademark of the 3M Co. Luer-LOK is a registered trademark of Becton-Dickinson and
Company. Teflon and Tefzel are registered trademarks of E.I. du Pont de Nemours & Co. Tygon is a
registered trademark of Norton Co.
Thermo Fisher Scientific Inc. provides this document to its customers with a product purchase to use in the
product operation. This document is copyright protected and any reproduction of the whole or any part of this
document is strictly prohibited, except with the written authorization of Thermo Fisher Scientific Inc.
The contents of this document are subject to change without notice. All technical information in this
document is for reference purposes only. System configurations and specifications in this document supersede
all previous information received by the purchaser.
Thermo Fisher Scientific Inc. makes no representations that this document is complete, accurate or errorfree and assumes no responsibility and will not be liable for any errors, omissions, damage or loss that might
result from any use of this document, even if the information in the document is followed properly.
This document is not part of any sales contract between Thermo Fisher Scientific Inc. and a purchaser. This
document shall in no way govern or modify any Terms and Conditions of Sale, which Terms and Conditions of
Sale shall govern all conflicting information between the two documents.
Release history: Revision A August 2008
For Research Use Only. Not regulated for medical or veterinary diagnostic use by U.S. Federal Drug
Administration or other competent authorities.
Regulatory Compliance
Thermo Fisher Scientific performs complete testing and evaluation of its products to ensure full compliance with
applicable domestic and international regulations. When the system is delivered to you, it meets all pertinent
electromagnetic compatibility (EMC) and safety standards as described below.
EMC Directive 2004/108/EC
EMC compliance has been evaluated by TUV Rheinland of North America.
CISPR 11: 1998
EN 61000-4-4: 2004
EN 55011: 1998, A1:1999, A2, 2002
EN 61000-4-5: 2001
EN 61000-3-2: 2000
EN 61000-4-6: 2003
EN 61000-3-3: 1995, A1: 2001
EN 61000-4-11: 2001
EN 61000-4-2: 2001
EN 61326-1: 1997, A1: 1998, A2: 2001, A3: 2003
EN 61000-4-3: 2002
CFR 47: 2007
Low Voltage Safety Compliance
Low voltage safety compliance has been evaluated by TUV Rheinland of North America.
This device complies with Low Voltage Directive 2006/95/EC, harmonized standard EN 61010-1: 2001,
IEC 61010-1: 2002, UL 61010A-1: 2004, and CAN/CSA 22.2 61010-1: 2004.
Changes that you make to your system may void compliance with one or more of these EMC and safety standards.
Changes to your system include replacing a part or adding components, options, or peripherals not specifically
authorized and qualified by Thermo Fisher Scientific. To ensure continued compliance with EMC and safety standards,
replacement parts and additional components, options, and peripherals must be ordered from Thermo Fisher Scientific
or one of its authorized representatives.
FCC Compliance Statement
THIS DEVICE COMPLIES WITH PART 15 OF THE FCC RULES. OPERATION IS SUBJECT TO
THE FOLLOWING TWO CONDITIONS: (1) THIS DEVICE MAY NOT CAUSE HARMFUL
INTERFERENCE, AND (2) THIS DEVICE MUST ACCEPT ANY INTERFERENCE RECEIVED,
INCLUDING INTERFERENCE THAT MAY CAUSE UNDESIRED OPERATION.
CAUTION Read and understand the various precautionary notes, signs, and symbols contained inside
this manual pertaining to the safe use and operation of this product before using the device.
Notice on Lifting and Handling of
Thermo Scientific Instruments
For your safety, and in compliance with international regulations, the physical handling of this Thermo Fisher Scientific
instrument requires a team effort to lift and/or move the instrument. This instrument weighs 18 kg (40 lbs) and is too
heavy for one person alone to handle safely.
Notice on the Proper Use of
Thermo Scientific Instruments
In compliance with international regulations: Use of this instrument in a manner not specified by Thermo Fisher
Scientific could impair any protection provided by the instrument.
Notice on the Susceptibility
to Electromagnetic Transmissions
Your instrument is designed to work in a controlled electromagnetic environment. Do not use radio frequency
transmitters, such as mobile phones, in close proximity to the instrument.
For manufacturing location, see the label on the instrument.
WEEE Compliance
This product is required to comply with the European Union’s Waste Electrical & Electronic
Equipment (WEEE) Directive 2002/96/EC. It is marked with the following symbol:
Thermo Fisher Scientific has contracted with one or more recycling or disposal companies in each
European Union (EU) Member State, and these companies should dispose of or recycle this product.
See www.thermo.com/WEEERoHS for further information on Thermo Fisher Scientific’s compliance
with these Directives and the recyclers in your country.
WEEE Konformität
Dieses Produkt muss die EU Waste Electrical & Electronic Equipment (WEEE) Richtlinie 2002/96/EC
erfüllen. Das Produkt ist durch folgendes Symbol gekennzeichnet:
Thermo Fisher Scientific hat Vereinbarungen mit Verwertungs-/Entsorgungsfirmen in allen EUMitgliedsstaaten getroffen, damit dieses Produkt durch diese Firmen wiederverwertet oder entsorgt
werden kann. Mehr Information über die Einhaltung dieser Anweisungen durch Thermo Fisher
Scientific, über die Verwerter, und weitere Hinweise, die nützlich sind, um die Produkte zu
identifizieren, die unter diese RoHS Anweisung fallen, finden sie unter www.thermo.com/
WEEERoHS.
Conformité DEEE
Ce produit doit être conforme à la directive européenne (2002/96/EC) des Déchets d'Equipements
Electriques et Electroniques (DEEE). Il est marqué par le symbole suivant:
Thermo Fisher Scientific s'est associé avec une ou plusieurs compagnies de recyclage dans chaque état
membre de l’union européenne et ce produit devrait être collecté ou recyclé par celles-ci. Davantage
d'informations sur la conformité de Thermo Fisher Scientific à ces directives, les recycleurs dans votre
pays et les informations sur les produits Thermo Fisher Scientific qui peuvent aider la détection des
substances sujettes à la directive RoHS sont disponibles sur www.thermo.com/WEEERoHS.
CAUTION Symbol
CAUTION
VORSICHT
ATTENTION
PRECAUCION
AVVERTENZA
Electric Shock: This instrument uses
high voltages that can cause personal
injury. Before servicing, shut down the
instrument and disconnect the instrument
from line power. Keep the top cover on
while operating the instrument. Do not
remove protective covers from PCBs.
Elektroschock: In diesem Gerät werden
Hochspannungen verwendet, die
Verletzungen verursachen können. Vor
Wartungsarbeiten muß das Gerät
abgeschaltet und vom Netz getrennt
werden. Betreiben Sie Wartungsarbeiten
nicht mit abgenommenem Deckel. Nehmen
Sie die Schutzabdeckung von Leiterplatten
nicht ab.
Choc électrique: L’instrument utilise des
tensions capables d’infliger des blessures
corprelles. L’instrument doit être arrêté et
débranché de la source de courant avant
tout intervention. Ne pas utiliser
l’instrument sans son couvercle. Ne pas
elensver les étuis protecteurs des cartes de
circuits imprimés.
Descarga eléctrica: Este instrumento
utiliza altas tensiones, capaces de
producir lesiones personales. Antes de
dar servicio de mantenimiento al
instrumento, éste debera apagarse y
desconectarse de la línea de alimentacion
eléctrica. No opere el instrumento sin sus
cubiertas exteriores quitadas. No remueva
las cubiertas protectoras de las tarjetas
de circuito impreso.
Shock da folgorazione. L’apparecchio è
alimentato da corrente ad alta tensione
che puo provocare lesioni fisiche. Prima di
effettuare qualsiasi intervento di
manutenzione occorre spegnere ed isolare
l’apparecchio dalla linea elettrica. Non
attivare lo strumento senza lo schermo
superiore. Non togliere i coperchi a
protezione dalle schede di circuito
stampato (PCB).
Chemical: This instrument might contain
hazardous chemicals. Wear gloves when
handling toxic, carcinogenic, mutagenic,
or corrosive or irritant chemicals. Use
approved containers and proper
procedures to dispose waste oil.
Chemikalien: Dieses Gerät kann
gefährliche Chemikalien enthalten. Tragen
Sie Schutzhandschuhe beim Umgang mit
toxischen, karzinogenen, mutagenen oder
ätzenden/reizenden Chemikalien.
Entsorgen Sie verbrauchtes Öl
entsprechend den Vorschriften in den
vorgeschriebenen Behältern.
Chimique: Des produits chemiques
dangereux peuven se trouver dans
l’instrument. Proted dos gants pour
manipuler tous produits chemiques
toxiques, cancérigènes, mutagènes, ou
corrosifs/irritants. Utiliser des récipients
et des procédures homologuées pour se
débarrasser des déchets d’huile.
Química: El instrumento puede contener
productos quimicos peligrosos. Utilice
guantes al manejar productos quimicos
tóxicos, carcinogenos, mutagenos o
corrosivos/irritantes. Utilice recipientes y
procedimientos aprobados para
deshacerse del aceite usado.
Prodotti chimici. Possibile presenza di
sostanze chimiche pericolose
nell’apparecchio. Indossare dei guanti per
maneggiare prodotti chimici tossici,
cancerogeni, mutageni, o
corrosivi/irritanti. Utilizzare contenitori
aprovo e seguire la procedura indicata per
lo smaltimento dei residui di olio.
Heat: Before servicing the instrument,
allow any heated components to cool.
Hitze: Warten Sie erhitzte Komponenten
erst nachdem diese sich abgekühlt haben.
Haute Temperature: Permettre aux
composants chauffés de refroidir avant
tout intervention.
Altas temperaturas: Permita que lop
componentes se enfríen, ante de efectuar
servicio de mantenimiento.
Calore. Attendere che i componenti
riscaldati si raffreddino prima di
effetturare l’intervento di manutenzione.
Fire: Use care when operating the system
in the presence of flammable gases.
Feuer: Beachten Sie die einschlägigen
VorsichtsmaBnahmen, wenn Sie das
System in Gegenwart von entzündbaren
Gasen betreiben.
Incendie: Agir avec précaution lors de
l’utilisation du système en présence de
gaz inflammables.
Fuego: Tenga cuidado al operar el
sistema en presencia de gases
inflamables.
Incendio. Adottare le dovute precauzioni
quando si usa il sistema in presenza di gas
infiammabili.
Eye Hazard: Eye damage could occur
from splattered chemicals or flying
particles. Wear safety glasses when
handling chemicals or servicing the
instrument.
Verletzungsgefahr der Augen:
Verspritzte Chemikalien oder kleine
Partikel können Augenverletzungen
verursachen. Tragen Sie beim Umgang mit
Chemikalien oder bei der Wartung des
Gerätes eine Schutzbrille.
Danger pour les yeux: Dex projections
chimiques, liquides, ou solides peuvent
être dangereuses pour les yeux. Porter des
lunettes de protection lors de toute
manipulationde produit chimique ou pour
toute intervention sur l’instrument.
Peligro par los ojos: Las salicaduras de
productos químicos o particulas que
salten bruscamente pueden causar
lesiones en los ojos. Utilice anteojos
protectores al mnipular productos
químicos o al darle servicio de
mantenimiento al instrumento.
Pericolo per la vista. Gli schizzi di
prodotti chimici o delle particelle presenti
nell’aria potrebbero causare danni alla
vista. Indossare occhiali protettivi quando
si maneggiano prodotti chimici o si
effettuano interventi di manutenzione
sull’apparecchio.
General Hazard: A hazard is present that
is not included in the above categories.
Also, this symbol appears on the
instrument to refer the user to instructions
in this manual.
Allgemeine Gefahr: Es besteht eine
weitere Gefahr, die nicht in den
vorstehenden Kategorien beschrieben ist.
Dieses Symbol wird im Handbuch
auBerdem dazu verwendet, um den
Benutzer auf Anweisungen hinzuweisen.
Danger général: Indique la présence
d;un risque n’appartenant pas aux
catégories citées plus haut. Ce symbole
figure également sur l’instrument pour
renvoyer l’utilisateur aux instructions du
présent manuel.
Peligro general: Significa que existe un
peligro no incluido en las categorias
anteriores. Este simbolo también se utiliza
en el instrumento par referir al usuario a
las instrucciones contenidas en este
manual.
Pericolo generico. Pericolo non
compreso tra le precedenti categorie.
Questo simbolo è utilizzato inoltre
sull’apparecchio per segnalare all’utente
di consultare le istruzioni descritte nel
presente manuale.
When the safety of a procedure is
questionable, contact your local Technical
Support organization for Thermo Fisher
Scientific San Jose Products.
Wenn Sie sich über die Sicherheit eines
Verfahrens im unklaren sind, setzen Sie
sich, bevor Sie fortfahren, mit Ihrer
lokalen technischen
Unterstützungsorganisation für Thermo
Fisher Scientific San Jose Produkte in
Verbindung.
Si la sûreté d’un procédure est incertaine,
avant de continuer, contacter le plus
proche Service Clientèle pour les produits
de Thermo Fisher Scientific San Jose.
Cuando la certidumbre acerca de un
procedimiento sea dudosa, antes de
proseguir, pongase en contacto con la
Oficina de Asistencia Tecnica local para
los productos de Thermo Fisher Scientific
San Jose.
Quando e in dubbio la misura di sicurezza
per una procedura, prima di continuare, si
prega di mettersi in contatto con il
Servizio di Assistenza Tecnica locale per i
prodotti di Thermo Fisher Scientific San
Jose.
CAUTION Symbol
CAUTION
Electric Shock: This instrument uses
high voltages that can cause personal
injury. Before servicing, shut down the
instrument and disconnect the instrument
from line power. Keep the top cover on
while operating the instrument. Do not
remove protective covers from PCBs.
Chemical: This instrument might contain
hazardous chemicals. Wear gloves when
handling toxic, carcinogenic, mutagenic,
or corrosive or irritant chemicals. Use
approved containers and proper
procedures to dispose waste oil.
Heat: Before servicing the instrument,
allow any heated components to cool.
Fire: Use care when operating the system
in the presence of flammable gases.
Eye Hazard: Eye damage could occur
from splattered chemicals or flying
particles. Wear safety glasses when
handling chemicals or servicing the
instrument.
General Hazard: A hazard is present that
is not included in the above categories.
Also, this symbol appears on the
instrument to refer the user to instructions
in this manual.
When the safety of a procedure is
questionable, contact your local Technical
Support organization for Thermo Fisher
Scientific San Jose Products.
C
Contents
Preface . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . xi
Safety and Special Notices . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .xi
Manual Conventions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . xii
Good Laboratory Practices . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .xiii
Contacting Us . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . xv
Installation and Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
Start-up Checklist . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
Unpacking. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
Installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
LC System Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
Performance Verification. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
Specifications. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
A Quick Example . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .21
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
Learning Your Way Around . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
Instrument Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
Practice Examples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
Basic Operations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .31
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
Theory of Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
SpectraSYSTEM P1000 Isocratic Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
Instrument Startup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33
Some Routine Operations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
The File Menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
Purging Solvent Lines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
Starting a Run . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40
Status . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
Monitoring Pump Performance. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43
Shutting Down at the End of the Day . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
Thermo Scientific
SpectraSYSTEM P1000 Isocratic Pump User Guide
iii
Contents
Advanced Operations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .45
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
The Options Menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
The Tests Menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
Required Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .67
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 67
Maintenance Schedule. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 68
Maintenance Log. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 68
Extending the Maintenance Period . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 72
Maintenance Procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73
Maintenance Tips . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 92
Repair Instructions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94
Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 95
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 95
Theory of Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 95
Troubleshooting Your Pump. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 96
Glossary
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .105
Kits and Parts Lists . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .111
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 111
Accessory Kit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 111
Standard Maintenance Kit. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 112
Standard LC Fittings Kit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 112
Piston Flush Seal Kit (10 mL) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 113
Piston Seal Kit (30 mL) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 113
Solvent Inlet Tube Kit. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 113
Solvent Tube Extension Kit. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 113
Manual Injection Valve Bracket Kit. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 114
Narrow-bore Upgrade Kit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 117
iv
SpectraSYSTEM P1000 Isocratic Pump User Guide
Thermo Scientific
P
Preface
This guide describes how to install and maintain the SpectraSYSTEM P1000 isocratic pump,
as well as how to control the gradient pump from the front panel keypad.
Safety and Special Notices
Caution!
A caution alerts you to situations that could result in personal injury. It also tells you how to
avoid them.
High Voltage!
A high voltage caution alerts you to the presence of high voltage and to the potential injury
that could occur from electrical shock were you to come in contact with a specific
instrument area or component. It also tells you how to avoid contact with the high-voltage
areas in your instrument.
Hot Surface!
A hot surface caution alerts you to potential injury that could occur from coming in contact
with a heated surface or area on or in an instrument. It also tells you how to avoid contact
with the heated surfaces in your instrument.
Note
Notes alert you to the correct operating or maintenance procedures needed to prevent
equipment or data damage. They also alert you to important exceptions, side effects, or
unexpected occurrences that may result from certain action(s).
Hint
Hints call out general rules or shortcuts. They specify ways to obtain the best performance
and results from your instrument.
Thermo Scientific
SpectraSYSTEM P1000 Isocratic Pump User Guide
xi
Preface
Manual Conventions
This manual uses several conventions. Among them are menu displays, text conventions
(brackets, slashes, and so on), and standard words.
Displays
We will depict the two-line display as shown below. Note that in menu illustrations, the
triangular cursor location is indicated by a caret (>).
>FILES
QUEUE
COMMANDS
TESTS
OPTIONS
A two-line menu display
Frequently the two lines shown on the display are only part of a longer menu which you
would see by pressing the down-arrow key. In this manual, menus having more than two lines
are represented as follows:
Edit File
1
File Name
-------------------------------------------------------->Solvent Program
Options
Timed Events
A menu longer than two lines
Text Conventions
Three typographic conventions are used to differentiate between keys, menus, and fields.
Brackets
Brackets, [ ], indicate instrument keys, For example: Press the [MENU] key.
Slashes
Slashes, / /, are text conventions used around menu choices. For example: From the Main
Menu, select /FILES/, /Edit/.
Capitalization
Capitalization is used to make field and menu names appear just as they do on the display.
Generally the first letters of field names are capitalized. For example: In /Solvent Program/ go
to the Flow field.
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SpectraSYSTEM P1000 Isocratic Pump User Guide
Thermo Scientific
Preface
Standard Words
We have also standardized the meanings of two words: “select” and “enter.”
Select
The word “select” is used when you need to choose from among available options. For
example, to select a particular menu choice, you would move the cursor to the appropriate
choice and press [ENTER]. To “select” a field entry, move the cursor to the appropriate field
and use the [+] and [–] keys to scroll to the desired choice.
Enter
The word “enter” is used when you need to specify individual alphanumeric digits. To “enter”
a particular value, move the cursor to the field and use the [+] and [–] keys to increment or
decrement each digit in the field until the desired value or letter appears.
Good Laboratory Practices
To obtain optimal performance from your LC system and to prevent personal injury or injury
to the environment, do the following:
• Keep good records
• Read the manufacturers’ Material Safety Data Sheets for the chemicals being used in your
laboratory
• Remove particulate matter from your samples before you inject them into the liquid
chromatograph
• Use HPLC grade solvents
• Connect the drainage tubes from the pump, autosampler, and detector to an appropriate
waste receptacle. Dispose of solvents as specified by local regulations
Keep Good Records
To help identify and isolate problems with either your equipment or your methodology, keep
good records of all system conditions (for example,% RSDs on retention times and peak areas,
peak shape and resolution). At a minimum, keep a chromatogram of a typical sample and
standard mixture, well documented with system conditions, for future reference. Careful
comparison of retention times, peak shapes, peak sensitivity, and baseline noise can provide
valuable clues to identifying and solving future problems.
Thermo Scientific
SpectraSYSTEM P1000 Isocratic Pump User Guide
xiii
Preface
Chemical Toxicity
Although the large volume of toxic and flammable solvents used and stored in laboratories can
be quite dangerous, do not ignore the potential hazards posed by your samples. Take special
care to read and follow all precautions that ensure proper ventilation, storage, handling, and
disposal of both solvents and samples. Become familiar with the toxicity data and potential
hazards associated with all chemicals by referring to the manufacturers’ Material Safety Data
Sheets (MSDS).
Sample Preparation
Always consider the solubility of your sample in the solvent/mobile phase. Sample
precipitation can plug the column, tubing or flowcell causing flow restriction. This
obstruction can result in irreparable damage to the system. To avoid damage caused by
particulate matter, filter samples through 0.45 or 0.2 micron (or less) filters.
Solvent Requirements
Many chemical manufacturers provide a line of high-purity or HPLC-grade reagents that are
free of chemical impurities. Routine filtration of all solvents or eluents through a 0.45 or
0.2 micron (or less) fluorocarbon filter before placing them in the solvent reservoir
significantly prolongs the life and effectiveness of the inlet filters, check valves and seals,
injector, and column. Typically, HPLC-grade solvents do not require filtration.
Choose a mobile phase that is compatible with the sample and column you have selected for
your separation. Remember that some solvents are corrosive to stainless steel.
Solvent Disposal
Make sure you have a solvent waste container or other kind of drain system available at or
below the benchtop level. Most solvents have special disposal requirements and should not be
disposed of directly down a drain. Follow all governmental regulations when disposing of any
chemical.
High-pressure Systems and Leaks
LC systems operate at high pressures. Because liquids are not highly compressible they do not
store much energy. Accordingly, there is little immediate danger from the high pressures in an
LC system. However, if a leak occurs, correct it as soon as possible. Always wear eye and skin
protection when operating or maintaining an LC system. Always shut down the system and
return it to atmospheric pressure before attempting any maintenance.
xiv
SpectraSYSTEM P1000 Isocratic Pump User Guide
Thermo Scientific
Preface
Contacting Us
There are several ways to contact Thermo Fisher Scientific for the information you need.
Y To contact Technical Support
Phone
Fax
E-mail
Knowledge base
800-532-4752
561-688-8736
[email protected]
www.thermokb.com
Y Find software updates and utilities to download at mssupport.thermo.com.
Y To contact Customer Service for ordering information
Phone
Fax
E-mail
Web site
800-532-4752
561-688-8731
[email protected]
www.thermo.com/ms
Y To copy manuals from the Internet
Go to mssupport.thermo.com and click Customer Manuals in the left margin of the
window.
Y To suggest changes to documentation or to Help
• Fill out a reader survey online at www.thermo.com/lcms-techpubs.
• Send an e-mail message to the Technical Publications Editor at
[email protected]
Thermo Scientific
SpectraSYSTEM P1000 Isocratic Pump User Guide
xv
1
Installation and
Specifications
Introduction
This chapter contains information necessary to install your Thermo
Scientific, SpectraSYSTEM™ P1000 isocratic pump properly. The
step-by-step instructions describe how to set the voltage for your area,
how to connect tubing, and how to prime and purge the pump. Use
the checklist on the next page to complete pump installation. Be sure
you read the Safety Information at the front of this manual before
proceeding with any installation.
Thermo Scientific
1
Start-up Checklist
This list is a brief summary of tasks that should be completed to
install your pump. Complete installation information is contained in
this chapter.
Inspect your instrument
Check for parts shortages
Set the voltage
Place the pump
Connect the power cord
Check initial response to power-on
Hardwire to eight-pin port, using external
function connector, making electrical connection
to other SpectraSYSTEM instruments
Install kits or accessories
Prepare and connect solvents
Connect inlet lines
Prime with solvent
Purge solvent lines
Connect to system
This pump was installed by:
(Name)
2
(Date)
Thermo Scientific
Unpacking
INSPECT YOUR
INSTRUMENT
Your pump was shipped in a special container designed to provide
excellent protection from routine wear and tear encountered in transit.
After unpacking, inspect your pump and its accessories for missing
parts and/or physical damage. If damage is found, notify both the
carrier and your sales representative. DO NOT return any goods
without prior authorization from Thermo Fisher Scientific.
NOTE: Narrow-bore pumps will have a 3μL static mixer included.
The contents of your package varies with the model and options
purchased. A basic accessory kit is supplied with each pump and
includes the following tools and parts.
The contents of your ship kit is as follows:
1
1
1
1
1
Pump
Accessory Kit
Tubing Kit
SpectraSYSTEM documentation CD
Declaration of Conformity
OPTIONS
AVAILABLE
A variety of options, kits, and accessories are available for your
pump. Refer to Appendix A, Kits and Parts Lists for a full
description and parts list of each. If you purchased an
inert/biocompatible pump, the correct tubing and liquid ends were
installed at the factory before shipment.
For a list of all available accessories, upgrades, and kits, see the insert
at the front of this manual or contact your Thermo Fisher Scientific
sales representative. Note that all upgrades require installation by
Thermo Fisher Scientific.
NOTE: The pump features a bypass valve pre-installed as standard
equipment.
Thermo Scientific
3
Installation
LIFTING AND
CARRYING THE
PUMP
The correct way to carry the pump is to use the two hand holds, one
located underneath the front of the pump, and the other at the top of
the back, near the power switch. Grasp the pump well underneath the
front when lifting and carrying.
SETTING THE
VOLTAGE
All pumps are configured at shipment for 230 VAC (50/60 Hz)
operation. Depending upon the country of use, you might need to
change the voltage setting.
NOTE: Check the position of the voltage select barrel located on the rear
panel (Figure 1.2). If the indicated voltage setting is not consistent with
your area, DO NOT CONNECT THE POWER CORD!
The voltage setting can be easily modified as follows:
1. Remove the tape label covering the power entry receptacle.
2. Ensure that the power cord is not connected to the pump.
3. Use a small, flat-blade screwdriver to pry open the power
selector/fuse cover to expose the voltage selector barrel. You
will probably hear the top edge of the cover snap as it is pried
open.
4. Remove the plastic selector barrel by pulling it straight out.
5. Rotate the barrel until you see the desired voltage (either
115 VAC or 230 VAC) and insert the barrel back into the
housing with the desired voltage visible.
6. Firmly snap the housing cover back in place. Be sure that the
selected voltage is visible in the voltage window (Figure 1.2).
HINT: Use two thumbs to push up on the top half of the cover as you push
in. The voltage selected will be visible through the window.
4
Thermo Scientific
Lift Point
I
ON
O
OFF
Communication
Port (COMM)
Power Switch
TERMINAL CONFIGURATION
8-Pin Port
Fan
Power Input
Voltage Selector/
Fuse Cover
230Vac
PU-Z033E/DT
Power Cord
Connection
Figure 1.1 Rear panel
Thermo Scientific
5
PRY OPEN HERE
REMOVE, TURN
& REPLACE
TO CHANGE VOLTAGE
115Vac
230Vac
PU-Z006E/FM
230Vac
230Vac
Figure 1.2 Power selector/fuse cover, closed, with "voltage window." The opened
power selector/fuse cover, with barrel selector removed
PLACING THE
PUMP
The pump weighs approximately 38 pounds (18 kg) and requires at
least 6 inches (16 cm) of bench width and at least 19 inches (48 cm)
of bench depth. If used with a manual injector bracket, the pump
requires 9 inches (23 cm) of bench width. The pump needs a space at
least 15 inches (38 cm) high.
Place the pump on a level surface. Leave 2 inches (6 - 7 cm) behind
the instrument for good air flow and access to electrical connections.
Keep the pump away from heating and cooling ducts, and avoid
exposing the pump to direct sunlight. The pump should be placed to
the far left of your LC system if it is used with a SpectraSYSTEM
autosampler or detector.
CONNECTING THE
POWER CORD
Attach the AC power cord. (see the insert at the front of this manual.)
Plug the power connector into an appropriately grounded power
outlet.
NOTE: For safe operation and optimum performance, the pump must be
connected to a properly grounded power receptacle.
6
Thermo Scientific
CHECKING INITIAL
RESPONSE TO
POWER ON
Turn on the power by pressing the power switch (Figure 1.1). With
the pump's front panel facing you, the power switch is located in the
back, on the upper right-hand side. The fan starts and a display
similar to Figure 1.3 appears for one second.
VERSION x.yy.zz
Figure 1.3 A brief power-up message
If this message does not appear, double-check the electrical
connections and try turning on the pump once more, watching the
screen closely. If the message still does not appear, contact your
Thermo Fisher Scientific representative.
Next, the display shows the Status Screen, similar to Figure 1.4.
Status
Flow
PSI
STOP
1.00
154T
Figure 1.4 P1000 Status Screen
HARDWIRING
EXTERNAL EVENTS
Pin 6 of the eight-pin port on the back of the pump (Figure 1.1)
allows you to control another device, such as a column switching
valve or fraction collector. If you plan to control such a device or
instrument using the pump's Timed Events feature, insert the external
function connector into the eight-pin port.
The pins are labeled both on the port and on the external function
connector. Ensure that the pin numbers match whenever plugging the
connector into the port.
Hardwire your device using the 4-connection cable. Loosen pin 6's
small screw, insert the wire, then tighten the screw.
You must also insert the external function connector if you use a
SpectraSYSTEM autosampler. More information about making
hardwire connections to an autosampler is found on page 16, and in
the SpectraSYSTEM AS3000 Autosampler User Guide.
Pin assignments for the eight-pin port are shown in Table 1.1.
Thermo Scientific
7
Table 1.1 Eight-pin port pin assignments
Pin #
Assignment
1
READY (Output)
2
+5 VDC 100 mA MAX
3
GROUND
4
PRESSURE 0.1 V/1000 PSI
5
STOP (Input)
6
7
RUN (Input)
8
INJ HOLD (Output)
All outputs (pin 1, pin 6, and pin 8) are open-collector type, capable
of sinking up to 30 mA at a maximum of 30 VDC.
INSTALLING KITS
OR ACCESSORIES
Refer to Appendix C for complete instructions for installing the
Manual Injection Valve Bracket (column holder).
PREPARING AND
CONNECTING
SOLVENTS
If you did not purchase a solvent degassing apparatus or solvent
bottles from Thermo Fisher Scientific, skip this section. Continue
with Connecting Inlet Lines on the next page.
Solvent Bottles
Prepare your solvent bottle(s) as follows:
1. Rinse the bottle(s) with LC-grade solvent to remove any dust.
2. Fill the bottle(s) with appropriate LC-grade solvent(s).
3. The bottle caps are pre-assembled to include an inlet line and
filter. Ensure that each filter is tightly assembled to its fitting,
and the filter fitting is firmly attached to the inlet line. Place
the solvent filter/inlet line into each bottle, making sure that the
inlet filter rests on the bottom of the bottle. Cap the bottle.
4. Attach the appropriate label to each solvent bottle cap to
identify it.
5. Run vent lines from each bottle to an appropriate exhaust
apparatus.
8
Thermo Scientific
Degassing
There are two recommended methods for degassing solvents for use
with your pump: vacuum degassing and helium degassing.
NOTE: Solvent degassing is recommended for isocratic applications
because it results in improved detector performance.
If you purchased a Thermo Scientific degasser, set up your degasser
as described in the degasser manual and continue the pump
installation when you have a supply of degassed solvent available.
CONNECTING
INLET LINES
Refer to Figure 1.5 when connecting the inlet lines. The P1000 has
one inlet. Connect the pump's inlet line (Figure 1.5) to your solvent
supply.
Thermo Scientific
9
R UN
S TATUS
MENU
S TOP
Purge key
E NTER
Purge
Spectr
aSY ST EM
P1000
Crossover tube
Pressure
transducer
Outlet
liquid
end
Bypass valve
Bypass valve tube
Transducer
check valve
Transducer
tube
Bypass valve knob
Inlet
liquid
end
Solvent
inlet
Outlet port
(to autosampler or
manual injection valve)
Inlet check valve
Solvent inlet tube
Waste tube
Lift point
Drip tray
Figure 1.5 Front panel, cover removed
10
Thermo Scientific
BYPASS VALVE
The bypass valve is shown in Figure 1.6. Do not attach a line to the
waste/prime port (the middle port) now, but have the solvent waste
tube (provided in the accessory kit) ready. You will attach the tube to
the waste/prime port after priming the pump.
PRIMING AND
PURGING
The P1000 pump is shipped with methanol in the pump heads and
connecting tubing. If the first solvent you'll use is not miscible with
methanol, first prime the pump with an intermediary solvent. Once
primed, you should purge the pump to remove any air bubbles.
HINT: It is best to prime the pump initially with methanol to fully wet all
internal surfaces. Priming with 100% water can often result in trapped air
due to the high surface tension of the water. Trapped air affects flow
stability.
Priming the Pump
To prime the pump with your solvent and simultaneously flush the
methanol out, you will need the 20 mL priming syringe and
Luer adapter found in the accessory kit. You will also need a solvent
waste container.
1. Remove the waste line from the waste/prime port of the bypass
valve, if connected.
2. Install the Luer adapter to the waste/prime port (Figure 1.6).
Tighten to finger-tight, then wrench tighten approximately
1/4-turn. (This allows the priming syringe to be attached and
detached conveniently.)
Thermo Scientific
11
Open
Closed
Bracket
Mounting
Screws
Bypass Valve
Luer Adapter
Waste/Prime
Port
Bypass Inlet
Tube
PU-Z007E/FM
Bypass Outlet
Tube
Figure 1.6 Bypass valve with Luer adapter connected
3. Make sure that the 20 mL Luer-tip priming syringe is fully
depressed. Connect the syringe to the adapter in the
waste/prime port twisting the syringe slightly to make a leakfree connection.
4. Position a solvent waste container nearby to collect the syringe
discharge, since two or three syringe volumes might be needed
to prime the pump. Make sure that all tube connections are
airtight.
12
Thermo Scientific
P U-Z008/DT
Figure 1.7 Bypass valve with syringe attached
5. Open the bypass valve by turning the knob fully
counterclockwise.
NOTE: Solvents flow through the pump when the pump is purging or
when a file is initialized (loaded as a run file).
6.
Turn on power to the pump (if it not already on)
7.
Press [PURGE]. See Figure 1.5.
NOTE: Purging starts whenever the cursor is moved out of the Purge
Menu Time field by pressing [ENTER].
Purge
Flow
Time
1.00
0.0
Figure 1.8 The Purge Menu (P1000)
NOTE: The Flow field might be labeled Pres instead of Flow, depending
on the purge mode that is set.
7. For analytical applications: Move the cursor to the Flow field.
Set the flow rate to 10 mL/min. If the purge mode is pressure,
set the pressure to 1000 psi (69 bars, 7 Mpa).
For narrow-bore applications: Move the cursor to the Flow
field. If the purge mode is pressure, set the pressure to
1000 psi (69 bars, 7 Mpa).
Thermo Scientific
13
8. Move the cursor to the Time field, then press [ENTER]. You
will hear the pump's motor start.
9. Slowly pull the syringe plunger back to create a small vacuum
in the solvent lines that will draw the solvent from the solvent
bottles (or the vacuum degasser) into the pump heads. Do not
draw back so far as to remove the plunger from the syringe
barrel!
If more than one draw is necessary to prime the pump, (i.e., the
syringe fills with air before solvent enters the pump heads),
press [STOP], close the bypass valve (turn clockwise), remove
the syringe, and depress the plunger. Reconnect the syringe,
open the bypass valve, press [PURGE], enter a flow rate or
time, press [ENTER], and finish drawing the solvents into the
pump as described at the beginning of this step.
If you notice a leak in one of the fittings, or need to stop the
solvent flow, press [STOP]. This will immediately stop flow
through the pump.
10. When solvent steadily appears in the syringe and no air bubbles
are present, press [STOP], then close the bypass valve.
11. Gently remove the syringe and empty it into the solvent waste
container.
12. Remove the Luer adapter from the valve port and store it, along
with the priming syringe, for later use.
13. Connect the solvent waste line to the waste/prime port of the
valve and tighten to finger-tight. Route the waste tubing to an
appropriate solvent waste container.
Purging the Pump
With the pump primed, purge the lines containing your chosen
solvents as follows:
1. Ensure that the solvent inlet filters inside each solvent bottle
are in a vertical position so that air within the filter will not be
trapped.
2. Fully open the bypass valve.
3. We suggest that you initially purge the lines with a volume of
10 mL.
Follow the steps below to begin the purge operation:
a) Press [PURGE] to reach the Purge Menu. If desired,
change the purge mode by pressing [MENU], /OPTIONS/,
/More/, Purge Mode. (The words in the top line of the
display will change, depending on your purge mode
preference.)
b) Move the cursor to the Flow or Pressure field.
14
Thermo Scientific
For analytical applications: If the purge mode is Flow,
enter a flow of 10.00 mL/min. [If pressure, set to 1000 psi
(69 bars, 7 Mpa).]
For narrow-bore applications: If the purge mode is Flow,
enter a flow of 5.00 mL/min. [If pressure, set to 1000 psi
(69 bars, 7 MPa).]
c) Press [ENTER] and enter a time of 1.00 minute.
d) Press [ENTER], the pumps motor will start. The pump
will automatically stop purging after one minute and then
initialize. After you have completed the purge, be sure to
close the purge valve.
Purge
Flow
Time
1.00
1.00
Figure 1.9 The Purge Menu with flow and time values entered
4. When you complete the purge and the pump stops, close
the bypass valve.
Thermo Scientific
15
LC System Connections
Once the pump is purged, you can plumb it to the rest of your
chromatographic system. Figure 1.5 and Figure 1.6 illustrate the
bypass valve, showing the pump's outlet. Using a pre-cut piece of
stainless steel tubing (or PEEK tubing if inert/biocompatible), connect
the outlet to your autosampler or manual injection apparatus.
If you are using a manual injector valve from Thermo Fisher
Scientific, refer to Appendix C for complete information for installing
the injector valve bracket.
If you are using a SpectraSYSTEM autosampler, the pump sends a
ready signal to the autosampler through pin 1, and receives a stop
signal from the autosampler through pin 5. In addition, the ground
contact (pin 3) must also be connected to the autosampler's ground
contact. For complete information on how to make these
connections, refer to the SpectraSYSTEM Autosampler User Guide,
Chapter 1. The table below summarizes the hardwire connections
necessary between a SpectraSYSTEM autosampler and pump.
Table 1.2 Pump connections to a SpectraSYSTEM autosampler
AUTOSAMPLER
PUMP
READY (Output)
GROUND
STOP (Input)
RUN (Input)
INJ HOLD (Output)
16
Pin 1
Pin 3
Pin 5
Pin 7
Pin 8
Thermo Scientific
to
to
to
to
to
Pin 5
Pin 1
Pin 3
Pin 4
Pin 7
PUMP READY
GROUND
PUMP STOP
GRAD START
INJ HOLD
Performance Verification
After installing your SpectraSYSTEM pump, it is suggested that you
run a performance test to verify that the instrument is working
properly. Common tests for pumps include flow accuracy and
precision. Procedures for these performance tests are described
below.
FLOW ACCURACY
There are many ways to test pump flow accuracy: graduated cylinder
vs. time, calibrated flow meter, or gravimetric vs. time. The
procedure below describes how to measure the flow accuracy and
precision using a gravimetric procedure. In general, you will set the
pump to a flow rate, collect eluant for a specified time in a weighed
flask, and determine the flow rate and accuracy. The actual flow rate
can also be used to calibrate your pump. This test will take
approximately 20 minutes.
Test Setup
Column or flow restrictor: To deliver c.a. 1000 psi backpressure
Flow Rate: Any flow rate to be tested for accuracy
Mobile phase: MeOH or other appropriate mobile phase
Experimental
Use the following steps to calculate the flow rate accuracy:
1. Prepare the desired mobile phase for the accuracy test.
2. Filter and degas the mobile phase.
3. Purge the pump and the column or flow restrictor being used.
4. Set the pump at the desired flow rate and start.
HINT: A volumetric flask is ideal because it helps to minimize evaporation.
Also, wrap tube and top of flask with aluminum foil to help eliminate
evaporation.
5. Weigh a clean flask capable of holding approximately
10 minutes of volume at the set flow rate. Include top and any
other items attached to flask.
6. Record this weight.
7. Place the flask under the flow stream from the pump and start
timing.
HINT: Use a stopwatch for the timing portion of the test. The more
accurate the stopwatch the better the results.
8. Collect the pump's eluant for 20 minutes.
9. Re-weigh the flask and record.
Thermo Scientific
17
10. Calculate the actual flow rate:
[(Weightfull - Weightempty) / Density] / Time = Flow Rate
11. Set a flow rate of 0.5 mL/min using MeOH as the mobile
phase.
Flow Rate = [(22.8577 g - 14.8858 g) / 0.7894 g/mL] / 19.9687 min
Flow Rate = [(7.9719 g) / 0.7894 g/mL] / 19.9687 min
Flow Rate = 10.0987 mL / 19.9687 min
Flow Rate = 0.506 mL / min
12. Calculate the flow accuracy of the pump:
Flow Accuracy = 100 × ⎢(FRset - FRactual) / FRset⎟
Flow Accuracy = 100 × 0.006mL / min
Example
Using the data from step 10 gives the following results:
Flow Accuracy = 100 × ⎢(0.5 mL/min - 0.506 mL/min)/0.5 mL/min ⎢
Flow Accuracy = 100 × (0.006 mL / 0.5 mL/min)
Flow Accuracy = 1.2%
HINT: For flow rates above 0.5 mL/min, it is best to install an in-line
100 μL mixer replacing the 3 μL mixer.
Specification
Typical results for flow precision are less than 1% (absolute).
However, results can vary based on temperature, mobile phase, and
flow rate.
HINT: When using gravimetric measurements, other correction factors
might be used to increase the accuracy of the measurements. These include
evaporation rate and the net buoyant effect.
FLOW PRECISION
Flow precision checks the reproducibility of the flow rate. This
procedure is simply running the accuracy test 7 or more times and
calculating a percent relative standard deviation. This procedure will
require at least a couple of hours.
18
Thermo Scientific
Test Setup
Set up the flow precision test above to perform 7 or more replicate
runs.
Column or flow restrictor: To deliver c.a. 1000 psi backpressure
Flow rate: Any flow rate that accuracy is to be tested
Mobile phase: MeOH or other appropriate mobile phase
HINT: For flow rates above 0.5 mL/min, it is best to install a 100 μL mixer
in-line replacing the 3 μL mixer.
Experimental
1. Repeat the flow accuracy test above for 7 or more replicate
runs.
2. Determine the flow rate for each replicate.
3. Determine the average flow rate for the replicate runs.
4. Determine the standard deviation for the replicate runs.
5. Determine the relative standard deviation for the replicate runs.
Using the following example values:
Average = 0.502 mL/min
Standard Deviation = 0.004
Relative Standard Deviation (RSD) = 100 × SD/Average
Yields:
RSD = 100 × (0.004/0.502 mL/min)
RSD = 100 × 0.00797
RSD = 0.797%
Specification
Typical results for flow precision are less than 1% (absolute).
However, results can vary based on temperature, mobile phase, and
flow rate.
Thermo Scientific
19
Specifications
P1000:
Isocratic pump using a dual in-line and floating piston design,
bayonet-mounted liquid ends, and patented ceramic check valves.
Physical:
14.5” (37 cm) × 6” (15 cm) × 18.5” (47 cm) (H × W × D)
38.6 lb. (18 kg)
Wetted Surfaces:
316 stainless steel, analytical and narrow-bore
PEEK, semi-prep
other surfaces for all pumps: Teflon®, Tefzel®, sapphire,
polyethylene
Delay Volume:
< 800 μL, analytical
< 500 μL, narrow-bore
Flow Rate Range:
0.01 - 10.00 mL/min, analytical or narrow-bore pumps
0.01 - 30.00 mL/min, semi-prep PEEK pumps
Flow Accuracy:
< 1% at 1.0 and 4.0 mL/min, analytical or semi-prep
< 1% at 0.2 and 1.0 mL/min, narrow-bore
Flow Precision:
Typically < 0.2% at 0.5 mL/min or greater
Pressure Range:
42 MPa or 420 bar or 6000 psi, analytical or narrow-bore
28 MPa or 280 bar or 4000 psi, semi-prep
Pressure Pulsation:
Typically < 1.0% at 1 mL/min
Method Files:
1 method + 1 Shutdown
Communications:
Remote Inputs: Ready, Run, Stop
Timed Events
Analog Pressure output
RS-232
Power:
115/230 VAC, 50/60 Hz
1.2/0.6A 200 VA
Safety/EMC Compliance: CSA, TÜV, FCC, CE Mark, EMC and Low Voltage Directives
20
Thermo Scientific
2
A Quick Example
Introduction
This chapter gives you the chance to become familiar with your
pump's screens and menus. It provides you with the three basic rules
you'll need for using your pump menus. It also introduces you to the
instrument's command center and describes the conventions we'll use
in this manual. In this chapter you will set up a few typical options,
purge your solvent lines, and run a flow stability test.
If you already feel comfortable with how to move through menus and
displays, just scan this chapter and proceed to Chapter 3. If you want
more practice with the pump menus, follow the instructions in this
chapter closely. Since the object of this chapter is to become familiar
with the keypad and menus, we won't provide detailed explanations
of the examples shown. More information can be found in one of the
succeeding chapters.
If you haven't installed your pump, be sure that you read the Safety
Information at the front of this manual and follow the procedure in
Chapter 1.
Throughout our explanations, we encourage you to explore the
general architecture of the instrument's menus and screens.
Learning Your
Way Around
AS EASY AS 1-2-3!
It's easy to learn your way around a SpectraSYSTEM or
SpectraSERIES pump. Just remember these three easy rules:
1. The ([∧], [∨], [<], [>]) move the cursor in the direction printed
on the key.
HINT: Press [MENU] to jump quickly to the top of the menu structure.
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2. The shape of the cursor determines how you make a selection:
•
If a triangular cursor appears, press [ENTER]
•
If a blinking square cursor appears, press the [+] or [-] keys
to scroll up or down through preset choices, or to increase
or decrease alphanumeric entries.
3. There are four ways to accept (and automatically save) an
entry. Just move the cursor out of the field by any of the
following methods:
•
Pressing [ENTER]
•
Using the arrow keys
•
Pressing [MENU]
•
Pressing [STATUS]
NOTE: If you can't leave a menu, either errors are present or you haven't
filled in all the necessary entries.
VISUAL CLUES
ON DISPLAY
Several visual clues help you move through the pump's menus and
enter values.
1. Top-level menu choices are displayed in all-capital letters;
lower-level menu choices are displayed in upper- and lowercase letters.
2. A field's square cursor changes to an underscore cursor when
you're scrolling through preset choices or entering numerical
values and characters.
3. A solid down-arrow (T) on the right side of some displays
indicates that the current menu continues on additional screens.
To access additional menu lines, press the down-arrow key,
[∨].
4. The last line of a longer menu is frequently a blank line
(without a solid down-arrow).
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Instrument Control
Take a look at the keypad and two-line display located on the front
panel (Figure 2.1). This is the command center from which you'll
access menus and control the instrument's operations. A brief
explanation of the keys and the main menus and screens follows.
RUN
STATUS
MENU
STOP
ENTER
SpectraSYSTEM
P1000
PU-Z032/DT
Purge
Figure 2.1 The P1000 pump keypad
The keypad of each SpectraSYSTEM instrument consists of twelve
keys. Four keys directly control the instrument's operation: [RUN],
[STOP], [STATUS], and, on the pump, a blank key called [Purge].
The remaining keys ([MENU], [ENTER], [∧], [∨], [<], [>], [+], [-])
either access commands or are used to set parameters and move
around the display. The function of each is explained below.
[RUN]
Generally, pressing [RUN] starts a run or sets up the conditions
specified for the beginning of a run.
The specific [RUN] operation depends on the instrument's state:
If the pump's state is STOP, pressing [RUN] automatically prepares
the last file loaded (the P1000 has only one file) to be run and sets the
pump to the conditions specified for the start of the run (t0
conditions).
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[STOP]
Pressing [STOP] halts an operation in progress. (Specifically, the
[STOP] key stops a run in progress by stopping solvent flow through
the pump.)
[STATUS]
Pressing [STATUS] displays the Status Screen. From the Status
Screen, you can monitor the run in progress. You can also access the
Status Menu. See page 26 for more information.
[Purge]
The unlabeled key is the only variable key in the whole
SpectraSYSTEM family. On the pump, the blank key is the [Purge]
key. The key's name appears on the nameplate below the key.
The [Purge] key brings the PURGE Screen to the display. Purge
parameters can be changed and the purge operation started from this
display. Refer to Purging Solvent Lines in Chapter 3 and to Priming
and Purging the Pump in Chapter 1 for complete information.
[MENU]
Pressing [MENU] displays the Main Menu. Each Main Menu item is
explained in detail in the rest of this manual. For FILE(s) and
COMMANDS, see Chapter 3. For OPTIONS and TESTS, see
Chapter 4.
NOTE: The P1000 Main Menu choices are FILE, OPTIONS,
and TESTS.
[ENTER]
Pressing [ENTER] accepts a selected choice or menu entry. The
[ENTER] key also advances the cursor to a new field, either on the
same line of the display or in the line below.
[∧], [∨], [<], and [>]
Pressing any arrow key (up, down, left, or right) moves the cursor in
the direction indicated on the key. If the cursor is on the first or the
last line of a menu, the up- and down-arrow keys move you "up" or
"down" in the menu structure.
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[+] and [-]
Pressing the [+] and [-] keys scrolls you through a field's available
choices or changes the value of alphanumeric entries. Holding down
either key will continuously scroll the list of choices forward or
backward until you release the key.
In fields that require numeric entries, the value of the selected digit is
increased or decreased by one unit each time you press the [+] or [-]
key. In fields that accept either numeric or alphabetic entries, such as
the File Name field, the [+] and [-] key scroll through the alphabet
from A to Z, then through the numbers 0 to 9, and finally to a slash,
hyphen and blank space.
In other fields, the [+] key advances you through a preset list of
choices while the [-] key takes you back through the list.
MENUS
AND SCREENS
Your pump has two kinds of displays: menus and screens. Menus
require you to make selections or enter specific values. Screens
display information that cannot be edited. The Menu Tree in from
pocket of your manual illustrates the structure and content of the
pump's menus and screens.
Main Menu
The Main Menu is the top level of the menu structure. The Main
Menu gives you access to several other menus. In the P1000 there are
three menus: FILE, TESTS, and OPTIONS. To see the Main Menu,
press the [MENU] key at any time.
>FILE
TESTS
OPTIONS
Figure 2.2 Main Menu (P1000)
From the File Menu you can edit, load, or delete a file. In the Options
Menu, you can set up or change your instrument's configuration. The
Tests Menu provides access to performance-related diagnostic tests
and maintenance-related menus. Refer to Chapters 3 and 4 for more
information on any of the instrument menus.
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Status Screen
The status screen automatically appears whenever you turn on the
instrument or press the [STATUS] key. The P1000 Status Screens
(Figure 2.3) show the pump's state (or purge time), flow, and
pressure. Below either Status Screen is the Status Menu, described
next.
Status
Flow
PSI
READY
1.00
1250
T
Figure 2.3 The Status Screen (P1000)
Status Menu
Just below the Status Screen is the Status Menu. To access the Status
Menu, press the down-arrow key from the Status Screen. The Status
Menu lets you review and edit run parameters during a run (Chapter 3).
MESSAGES
Three kinds of messages can appear on the pump's display: user
messages, confirmation messages, and error messages.
User messages
User messages (Figure 2.4) tell you about an existing instrument
condition or ask for further action. Some of these will only appear on
the display for three seconds. An example of a message requiring
further action is shown in Figure 2.4.
To install or remove liquid ends, press ENTER
Figure 2.4 An example of a user message
Confirmation messages
Confirmation messages (Figure 2.5) indicated on the display by
asterisks appear for one second after an operation has been carried out
successfully.
* *
File Loaded
* *
Figure 2.5 An example of a confirmation message
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Error messages
Error messages (Figure 2.6), indicated on the display by exclamation
points, are displayed whenever an undesirable condition exists that
prevents the instrument from carrying out an operation. Error
messages remain on the display until you press a key.
!!
MAX PRESSURE
!!
EXCEEDED
Figure 2.6 An example of an error message
Practice Examples
This section will take you step-by-step through four operations:
1. Setting a display option.
2. Creating a file.
3. Purging a solvent line.
4. Running a flow stability test.
These examples assume that the pump is properly installed using the
procedures in Chapter 1 and that the bypass valve's outlet is routed to
a solvent waste container.
SETTING A DISPLAY
OPTION (CHANGING
PRESSURE UNITS)
The pump’s default display can be changed to suit your own needs.
For example, you can use the steps below to change the pressure units
from the default in PSI to megapascals.
1.
Press [MENU]. Press [>] to move the cursor to /Options/, then
press [ENTER] to access the Options Menu.
2.
Press the down-arrow key [∨] until you see the /More/
selection. With the cursor next to /More/, press [ENTER] to
access the More Menu.
3.
The display now looks similar to Figure 2.7:
Pressure Units
PSIν
Purge Mode
Flow
Figure 2.7 The More Menu
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4. The cursor should be to the right of the value in the Pressure
Units field (PSI). Press [+] until the field shows MPa.
You have just changed the display so that all pressures will be
shown in megapascals. If you prefer other units, press [+] until
you see another preset choice that suits you.
5. You’ll also need to move the cursor between fields to set
method parameters. For example, move the cursor down to the
Purge Mode field. Use [+] to see the Pressure selection
(pressure). Press [+] once more, to change the Purge Mode
selection back to Flow.
6. You can exit the More Menu in several ways. This time, press
[STATUS] to exit the menu.
7. Press [∨] to display the Status Menu, which shows the run file.
EDITING A FILE
Editing a simple file is a good way to become familiar with entering
values and moving the cursor between menus.
1. Press [MENU].
2. With the caret (>) next to /FILE(S)/, press [ENTER] to access
the File Menu.
3. The cursor should be on the /Edit/ selection. Press [ENTER] to
access the Edit Menu. The cursor is in the Flow Rate field
(P1000).
4. For the P1000 (Figure 2.8), use the [+] key to enter a flow rate
of 1.50 mL/min in the Flow Rate field.
Flow Rate
1.50
Maximum Pressure
6000
---------------------------------------------------Minimum Pressure
Figure 2.8 The Edit Menu (P1000)
5. Press [∧] until you return to the File(s) Menu.
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0
PURGING A
SOLVENT LINE
You might already be familiar with the purge operation from
Appendix A. If so, skip this example and go on to Running a Flow
Stability Test.
In this example, you will purge a solvent line.
1. Open the bypass valve on the pump. Make sure that the bypass
valve outlet is routed to a solvent waste container.
2. Press [STATUS]. The Status Screen should show that the
pump is stopped (Figure 2.9)
Status
Flow
MPa
STOP
1.50
1
----------------------------------------------------Flow
MaxP
MinP
1.50
21
0
Figure 2.9 Status Screen and Status Menu (P1000)
3. Leave the Status Screen and go to the Purge Menu by pressing
[PURGE] (the blank key). The cursor should be in the Purge
field. Note that the screen displays the flow rate in mL/min
and the purge time in min. See Figure 2.10.
Purge
Flow
Time
1.50
0.0
Figure 2.10 The Purge Menu (P1000)
Now you will actually begin the purge cycle.
4. Move the cursor to the Time field either by pressing [ENTER]
or [>]. Enter 2.00 minutes in the Time field, then press
[ENTER].
The pump motor will start. The pump will purge solvent for two
minutes at the flow rate shown in the Flow field. You can stop the
purge operation at any time by pressing [STOP]. After the purge is
complete, the pump will automatically initialize the run file.
Remember to close the bypass valve immediately following the purge
so that solvent flow returns to the LC.
RUNNING A FLOW
STABILITY TEST
The flow stability test is a common test of the pump's performance.
The pump must be running, or be in a READY or EQUIL state for
this test to be initiated, and the flow rate must be greater than
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0 mL/min. If you need to change the flow rate, edit the flow setting
from the Status Menu, then proceed with the steps below.
NOTE: The Flow Stability test can be completed only when the pump is in a
READY state although it might be initiated while the pump is in any of the
states mentioned above.
1. When the Status Screen shows READY, press [MENU] and
select /TESTS/.
2. Select /Diagnostics/ from the Tests Menu.
3. The cursor should be on /Flow Stability/. Press [ENTER].
After a short time, the flow stability rating followed by a numerical
value will appear. STABLE flow corresponds to a reading between 0
and 25, ACCEPTABLE is between 26 and 90, and UNSTABLE is a
value greater than 90.
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3
Basic Operations
Introduction
This chapter contains a general theory of LC pump operations,
recommended laboratory practices, and how to perform routine
operations on your SpectraSYSTEM P1000 pump. Specifically
included are procedures for editing, loading and running a file, and
reviewing the pump operations status.
Before beginning this chapter, be sure that you have properly
installed the pump using the procedures in Chapter 1 and that you are
familiar with the pump keypad and menus as discussed in Chapter 2.
Theory of Operation
The pump is typically the second of five components in an LC system
(degasser is the first). A pump delivers a steady flow of one or more
solvents to a sample-injection instrument (generally an autosampler).
This solvent flow continues through the column and on to a detector.
From the detector, a signal is passed to an integrator, a recorder, or
another kind of data system capable of collecting the data and
allowing the data of the injected sample to be analyzed. The P1000
isocratic pump precisely and accurately delivers a mobile phase to
the LC.
Solvent flow rate is specified in the run file. The solvent travels to
the pump head where a piston meters the flow of the mixture to an
outlet tube. The pump's outlet tubing then connects the solvent
stream to an automatic or manual injector.
SpectraSYSTEM P1000 Isocratic Pump
The SpectraSYSTEM pump has been designed for ease of use and
unsurpassed performance. Any one of them can be used as a standalone pump or as a module in a totally automated LC system.
The P1000 is a single-solvent isocratic pump. Rugged, reliable, and
easy to use, it features a Shutdown option and Maintenance Log. The
P1000 can be connected to other SpectraSYSTEM modules through
RS-232 communication.
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The SpectraSYSTEM P1000 pump is engineered for reliability and
ease of maintenance. Easy maintenance helps to ensure that your
chromatography results are accurate and remain accurate. The builtin, patented Maintenance Log (Chapter 5) allows you to follow the
life span and use of seals, pistons, and check valves. If service is ever
required, the resident diagnostics and modular design of the pump
will keep downtime to a minimum. The simplicity and durability of
the pump means that a minimum of spare parts needs to be kept on
hand.
Table 3.1 File Characteristics for P1000 Pump
File Characteristics
Time Lines/File
Total Number Files
Total Time Lines
P1000
0
1
N/A
(flow rate only)
OPTIONS
Narrow-bore
LC refers to the use of narrow-ID, 2.0-3.0 mm columns for LC
separations. To optimize LC instruments for narrow-bore LC,
standard LC hardware must be modified to reduce extra-column
volume. Specific hardware modifications include minimizing the
pump’s dead volume, the detector flowcell’s volume, and the volume
contained in any interconnecting tubing and fittings. The lower
system volume of narrow-bore LC increases sample concentration,
which results in greatly improved sensitivity. Decreased solvent
consumption reduces operating costs as compared to standard
(4.0-4.6 mm ID) LC separation techniques.
NOTE: For narrow-bore applications we recommend you use a 20 μL
sample loop in Thermo Scientific autosamplers.
Hardware Modifications
Autosamplers: For the SpectraSYSTEM narrow-bore autosamplers
the pump-to-autosampler tubing (~ 6 inches long) and pre-heat tubing
(~ 24 inches long) has been changed from 0.020-inch ID to
0.007-inch ID.
Operational Considerations
Injection Mode: We recommend that you consider the following in
setting up your methods and LC instrumentation. Due to the manner
in which the pump firmware stores certain values and references the
hardware, the minimum operating pressure for the P1000 pump is
200 psi.
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We recommend that you use the PushLoop® mode for most narrowbore applications; however, depending on your sample volume, other
injection modes might be more beneficial in some cases (see below).
The following algorithms define the amount of sample needed for
your injection volume:
PushLoop (Injection Volume + 15 μL)
Pull Loop (Injection Volume + 1.1 μL)
Full Loop (Injection Volume x 1.33) + 70 μL
In PushLoop mode, the smallest settable sample volume is 0.1 μL.
Allowed volume increments are also 0.1 μL. You should not inject
more than 10 μL without changing the standard 20 μL loop. The
autosampler is supplied with a 20 μL loop.
Reducing Extra Column Volume: Minimizing extra column
volume maximizes analytical efficiency. Band-broadening can occur
in several ways. With narrow-bore columns, it is vital that good
plumbing connections are made. Otherwise, a dead volume created
by a bad fitting can result in much lower than expected efficiency and
peak resolution. Use zero dead volume (ZDV) fittings only with the
proper nuts and ferrules. Cut and debur tubing with the proper tools.
For polymer tubing (for example PEEK), use a "guillotine" cutter to
ensure straight, right-angle cuts.
The flowcell volume is probably the single largest contributor to extra
column volume in a narrow-bore system. Use the smallest internal
volume cell you can find, subject to path length requirements.
Instrument Startup
Be sure you have installed the pump according to Chapter 1 and have
completed the Startup Checklist.
When you turn on the pump, the Status display appears. This allows
you to check the instrument settings before entering your parameters.
As described in Chapter 2, it is possible to edit a file under the Status
Menu. If you have turned on the pump before, and have used this
editing capability, the Status Menu will contain the parameters last
saved.
At powerup, there are no messages to alert you that a file is being
loaded, but you can check the file number and name by pressing the
[STATUS] key. Then use the down-arrow key to scroll to the file
listing. (Both the [STATUS] key and the creation of files are
discussed later in this chapter.)
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Some Routine Operations
Ordinarily, you perform these operations with your pump every day:
•
Edit a file (or create a new file) and load a file to run
•
Run your samples
•
Purge the solvent lines
•
Check the pump's status
•
Monitor pump performance
•
Shut down the pump at the end of the day
The rest of this chapter is devoted to explaining these basic
operations. If you need to, refer to the keypad “rules” in Chapter 2.
You might also want to refer to the basic menu structure presented on
the quick reference cards in the front pocket of your manual.
The File Menu
In this section we describe how to set up the files that control
pressures, flow rates, and run times. Each of the file operations
accessed from the File Menu is briefly defined, then described in
detail.
To access the File Menu, press [MENU] and select /FILE/. The File
Menu is shown in Figure 3.1.
>Edit
·Load
·Delete
Figure 3.1 The File Menu (P1000)
Edit
Select /Edit/ if you want to change the parameters in an existing file,
or create a new file.
Load
Select /Load/ to load the file you want the pump to use when in
operation. The loaded file is referred to as the run file.
Delete
Select /Delete/ to return all file parameters to their default values. An
information message allows you to cancel the delete operation before
the file is deleted. The default file parameters are as follows:
• Flow rate = 1.00 mL/min
• Maximum Pressure = 6000 (depending on the selected
pressure units)
• Minimum Pressure = 0
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EDITING A FILE
The P1000 contains only one file and its Edit Menu (Figure 3.2)
consists of three fields.
Flow Rate
1.00
Maximum Pressure
6000
-----------------------------------------------------Minimum Pressure
0
Figure 3.2 The Edit Menu (P1000)
Flow Rate: Enter a flow rate in mL/min. The maximum flow rate is
determined by the liquid ends and head type. The head type is preset
in the Maintenance Log Head Type field by Thermo Fisher Scientific.
The flow range of your liquid ends was preset by Thermo Fisher
Scientific.
NOTE: If you change the liquid ends, refer to the Maintenance Log
description in Chapter 5.
Maximum, Minimum Pressures: Change the pressure levels as
desired. The maximum value is 6000 psi, the minimum is 0 psi. (The
allowed values depend on the pressure units.) The maximum pressure
value must be greater than the minimum pressure. The pump will not
allow you to set maximum and minimum pressures to values that are
inconsistent. If you are unable to edit one value, try to edit the
maximum valve first.
NOTE: Select pressure units (psi, bar, or MPa) from the Main Menu. Press
/Menu /OPTIONS/, /More/ as described in Chapter 4.
Creating the Run File - A P1000 Example
Enter run parameters in the P1000 by first selecting /FILE/, /Edit/.
The Edit Menu is shown in Figure 3.3.
Flow Rate
2.50
Maximum Pressure
4000
-----------------------------------------------------Minimum Pressure
0
Figure 3.3 Example P1000 Edit Menu
Simply enter a flow rate, and the maximum and minimum operating
pressures.
NOTE: Parameters are also easily changed from the Status Menu. Press
[STATUS], then [∨] to access active fields.
SHUTDOWN FILE
The Shutdown file in the P1000 is accessed from /OPTIONS/,
/Shutdown/.
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Making use of the Shutdown file assists you with the proper
maintenance of the pump. Since your pump and column should never
be allowed to sit idle with salts or corrosive materials in them
(including water), the Shutdown file lets you automatically flush the
pump and the column at the completion of a series of samples.
Whenever the pump detects that it has been in a READY state,
without a run being initiated for a specified period of time, it
automatically loads, initializes, and runs the Shutdown file when time
from Ready has been reached.
NOTE: The pump's clock is reset any time the [STOP] key is pressed.
Some instances when you might want to use a shutdown file are:
•
to keep solvent at a very low flow rate flowing through the LC
•
to clean the column and keep the pump running
•
to clean the column, then stop solvent flow through the LC
NOTE: If the pump will be operated unattended for an extended period of
time, ensure that the solvent reservoir and waste containers have sufficient
capacity.
If you use an autosampler, specify the time interval to be longer than
the cycle time on the autosampler (for example., [1.5 × cycle time], or
[cycle time + 20 minutes]). If you perform manual injections, set the
time interval to the maximum time likely between injections.
Depending on your own circumstances, you might want to turn the
Time from Ready to "Off."
The P1000 Shutdown Menu is shown in Figure 3.4. The Flow field
contains the flow rate parameter. The Time field contains 11 preset
choices: Off, and ten time values, ranging from 5 to 480 minutes.
The value selected in the Time field is the length of time the pump
will remain in a READY state before it automatically loads and runs a
shutdown file. So, for example, if you select 60 minutes, then
whenever the pump senses that it has been READY for 60 minutes
without a run being started, it will load and run the Shutdown
parameters.
Flow
Time
1.00
20
Figure 3.4 The Shutdown Menu (File), accessed from /OPTIONS/,
/Shutdown/
When the Shutdown File Loads Automatically
If the Shutdown file is loaded automatically, when it reaches the last
time line of the Shutdown file, the pump will maintain (Hold) the last
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Thermo Scientific
time line's flow rate indefinitely if the flow rate is greater than zero (>
0.0).
LOADING A FILE
For the P1000, select /LOAD/ and the file is loaded. A message will
confirm that the file was loaded. A loaded file is referred to as the
run file.
As soon as a file is loaded, the pump will initialize the file, that is,
bring the pump to the conditions specified on the zero (0.0) time line
of the file. The Status Screen shows INIT. If an equilibration has
been specified, the pump will then show EQUIL until the
equilibration time has been reached.
After initialization and equilibration, the Status Screen then shows
that the pump is READY. The pump's clock will not start unless a
run is triggered either manually by pressing [RUN] or from a properly
connected (hardwired) autosampler.
DELETING A FILE
For the P1000, selecting /DELETE/ will delete the file.
When you delete a file you are actually returning all parameters in the
file to their default values.
Purging Solvent Lines
If the solvent line contains air, refer to Priming the Pump in
Chapter 1.
Air will slowly diffuse through the thin-wall Teflon inlet tubing, and
into the solvent. If the pump flow has been turned off or if the
solvent line has not been used in the past several hours, the line
should be purged with degassed solvent before use.
The purge operation can be activated when the pump is in any state.
NOTE: Open the bypass valve prior to purging, or else ensure that your
chromatographic column can withstand the purge parameters you set
before performing any purge.
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THE PURGE MENU
Pressing the [PURGE] key displays the Purge Menu.
NOTE: DO NOT move the cursor out of the Time field using the
[ENTER] key unless your LC is ready to start a purge.
Purge
Flow
Time
1.00
0.0
Figure 3.5 The Purge Menu (P1000)
Purging can be accomplished in any of three purge modes: Flow,
Pressure, or Both. Table 3.2 describes purging across the three
modes.
Table 3.2 Purging mechanisms for the three purge modes
Modes
Purging requirements
Flow Mode
Regulated by the flow rate from the pump
Pressure Mode
Accomplished at a specific pressure
Both Mode
Uses both flow and pressure parameters
Internal limits are designed to protect your LC system: in flow mode,
the pump will accept rates of 0.01 to 10.0 mL/min. The maximum
pressure the pump allows in flow mode is the maximum pressure
value from the current run file; in pressure mode, the maximum flow
the pump will reach in attaining the set pressure is 6 mL/min.
NOTE: Purging in Pressure or Both modes with the bypass valve open
might not allow sufficient pressure to be generated in the system. The pump
will operate at maximum flow, but the target purge pressure might not be
achieved. Ensure that your analytical column can withstand the purge
pressure (or use a flow restrictor or old column), and do not open the
bypass valve.
The purge mode is changed from /OPTIONS/, /More/, Purge Mode.
The top line of the Purge Menu will show either Flow or pressure
units (PSI, BAR, MPa), depending on the purge mode you select.
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Thermo Scientific
Flow or pressure (PSI, BAR, or MPa)
The flow rate is taken from the last time line of the run file. Use this
field to select a flow rate. If the purge mode is pressure, the pressure
is automatically set to one-half (50%) of the maximum pressure level
set in the run file.
NOTE: To change the purge mode you must go to /OPTIONS/, /More/,
Purge Mode. Refer to Chapter 4 for complete information.
Time
The Time field is used to set the length of time you want the pump to
purge. If the field remains 0.0, purging, once started, will continue
until you press the [STOP] key.
NOTE: When you check the purge operation from the Status Screen, the
time remaining to complete the purge is shown below the word Status.
Starting a Purge
To initiate a purge cycle, move the cursor out of the Time field by
using the [ENTER] key.
The pump will begin to purge solvent. If the time stays set to 0.0,
purging will continue until you press [STOP], or a file is initialized.
If a time is entered, the pump will purge until the time set. After
completing a purge, the pump automatically initializes the run file.
When running in a timed purge mode, the Status Screen will indicate
the time remaining to purge (that is, counts backwards toward 0.0). If
the [PURGE] key is pressed once more, the Purge Menu is again
displayed and the time countdown continues, uninterrupted, unless
the cursor is moved out of the Time field by pressing [ENTER], at
which point the timer will be reset and purging will restart.
The pump will retain the selections made in the PURGE display as
long as the power to the pump is on.
Stopping a Purge
There are three ways to stop a purge cycle:
•
Press the [STOP] key
•
Load (initialize) a file by selecting a file using /FILE(S)/,
/Load/
•
Allow the pump to complete the purge (if a time has been
specified), at which point the pump will automatically initialize
the last run file.
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Starting a Run
To perform a run:
•
Purge the solvent lines if necessary
•
Load a file or press [RUN] to establish a READY state,
•
Inject the sample, and
•
Press [RUN].
•
If you are performing a manual injection, fill the injection
loop, check that the Status Screen shows READY, inject
the sample, and press [RUN] in succession.
•
If an autosampler is hardwired to the pump, simply initiate
the autosampler run sequence.
NOTE: Generally, when operated manually, if the pump is stopped (i.e., the
Status Screen shows STOP), the run file can be initialized by pressing
[RUN], and then started by pressing [RUN] again when the Status Screen
shows READY.
ESTABLISHING
READY
The READY state means that the pump has reached the conditions
specified on the first line of the solvent program and is ready to start a
run.
Initializing a File
To achieve the READY state, initialize a run file, by any of the
following methods:
•
Load a file by selecting /FILE/, /Load/, and then pressing
[ENTER]. .
•
If the pump is stopped (Status Screen shows STOP), press
[RUN]. This initializes the run file, without starting the
run.
Wait for the pump to reach zero time line conditions. If an
equilibration time was specified in the file, the Status Screen will
show EQUIL for this period of time.
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PRESSING [RUN]
As soon as the pump shows READY, begin the run by pressing the
[RUN] key. This starts the pump's clock.
NOTE: Even though the pump might be ready, your column and the rest
of your LC system might not be! Take into account your own LC
application and ensure that your column is at chemical equilibrium and
that the other instruments in your system are ready before you proceed
with any injection.
STOPPING THE
PUMP
There are a number of ways to stop the pump, depending on what you
want to do next.
By Pressing [STOP]
If you want to completely stop the pump, press [STOP]. This stops
the run and stops solvent flow through the pump. If you want to
resume with the same file, you must initialize the run file by pressing
[RUN], waiting for the pump to show [READY], then pressing
[RUN] again.
While the Pump is
Running
There are several messages which can appear in the Status field.
These are discussed in detail in the Status section below.
While the pump is running you can do several things without
disturbing pump operation:
•
Edit files (/FILE(S)/, /Edit/).
•
Check some pump performance parameters.
•
Edit the run file from the Status Menu. (This has an effect
on the current run. See page 42 for more information.)
Status
The Status Screen appears whenever the pump is powered on, a file is
initialized, or the [STATUS] key is pressed. The Status Screen,
consisting of two lines, shows the pump's current operating values.
Below the Status Screen is the Status Menu, where you can view and,
if necessary, edit the run file parameters.
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STATUS
MESSAGES
The P1000 can show any of the following messages:
Table 3.3 Status Messages
(time) The time into the run (or time remaining if a timed purge).
INIT The pump is initializing a file.
READY The pump has achieved the conditions on the first line of the
run file, and the equilibration time has elapsed (if set). A run
can be started. READY, shown in Status
RUN Appears briefly when the pump begins a run.
STOP All mobile-phase flow through the pump is stopped.
SYNC This is a remote communications message that appears
briefly whenever a run is started. At lower flow rates, it
might be seen for longer periods of time.
STATUS EXAMPLES
Shown below are two examples of an entire Status Screen and Status
Menu.
P1000
Status
Flow
PSI
READY
1.00
1250
------------------------------------------------------Flow
MaxP
MinP
1.00
6000
0
Figure 3.6 Example Status Screen and Status Menu
The first and second lines of the display show the state, flow, and
pressure.
EDITING A RUN
FILE
The remaining lines, which comprise the Status Menu, show the
parameters and options of the run file. If the run file and options do
not appear, the Status Lock feature has been turned on. (Status Lock
is described in Chapter 4, under the OPTIONS, More Menu.)
All time lines of the run file's solvent program can be edited while the
pump is running, as can the maximum and minimum pressures, and
the equilibration time. Any changes take effect as soon as the cursor
leaves each field. However, the changes are saved only when the
/Save File/ command is selected from the Status Menu.
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Monitoring Pump Performance
SpectraSYSTEM pumps can automatically monitor their own
performance and warn you if a flow problem exists. These options
(not to be confused with File Options), are described in detail in
Chapter 4.
Certain flow conditions are monitored continuously. For example, if
a time line with a zero flow rate has been encountered, the pump
responds with the appropriate error message shown below. As
mentioned earlier, you can select the pump's response to certain
conditions.
! !
ZERO FLOW RATE
! !
! !
MAX PRESSURE EXCEEDED
! !
Figure 3.7 Example error messages resulting from flow problems
To choose a pump response, select /OPTIONS/, /Error Recovery/.
(See Chapter 4, Options section.)
The pump can also initiate a Flow Stability Test. This test is run by
selecting /TESTS/, /Diagnostics/, /Flow Stability/. The results are
continuously displayed until another key is pressed. The results
consist of two parts. The first is a summary of the performance
evaluation (STABLE, ACCEPTABLE, or UNSTABLE) and the
second is a number that indicates a position in each range. Further
explanation of this test can be found in Chapter 4.
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Shutting Down at the End of the Day
Some shut down suggestions when you conclude your work with the
pump for the day:
44
•
Do not leave buffers in the pump or in your LC; purge the
pump (water is a good solvent) if it has just concluded a run
using buffered solutions. (Don't leave water in your LC.)
•
Leave the column full of a solvent recommended by the
column manufacturer.
•
Open the column bypass valve and purge using the same
solvent as in the column so that the liquid ends are filled with
that solvent.
•
Make use of the Shutdown file. The pump will automatically
maintain the conditions specified in the last or only line of the
file. This is particularly useful if you prefer to have a small but
continuous flow of solvent through your LC system while it is
idle.
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4
Advanced Operations
Introduction
This chapter focuses on three top-level menus: Options, used to set
important, yet seldom changed features, and Tests, used to run the
built-in diagnostics.
The Options Menu
The Options Menu (accessed from the Main Menu, not from
/FILES/), contains seldom-changed features such as the pump's
response to certain electrical and flow conditions it detects, userselected display and operational preferences, and file protection.
>FILE
·TESTS
•OPTIONS
Figure 4.1 The P1000's Main Menu with /OPTIONS/ selected
The P1000 Options Menu is shown in Figure 4.2.
>Shutdown
·Error Recovery
---------------------------------------------------·More
Figure 4.2 The Options Menu (P1000)
ERROR RECOVERY
MENU
The pump continuously checks pressure so that problems can be
indicated immediately on the display. The pump can also sense a
power failure or power interruption. The Error Recovery Menu
(Figure 4.3) is used to preset the pump's response to detecting error
conditions in any of these three operating parameters.
AC Power Fail
Stop
@Maximum Pres
Stop
Figure 4.3 The Error Recovery Menu
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Each field in the Error Recovery Menu can be set to one of three
selections:
Selection
Pump’s Response
Stop
The pump stops immediately if the
condition is encountered.
The pump continues as if the condition
had not occurred.
The pump immediately stops, then loads
and runs the Shutdown file.
Continue
Shutdown
AC Power Fail
The pump might sense a power interruption at any time. Select Stop,
Continue, or Shutdown in the AC Power Fail field to stop, continue,
or shut down the pump as soon as power is restored.
NOTE: If the power switch is turned off while the motor is running, the
pump considers this a power failure and will respond accordingly as soon
as power is restored.
@Maximum Pres
In a file's Options Menu, you can change the maximum pressure level
(the default is 6000 psi). If the pump's operating pressure ever
exceeds this value, the pump will operate based on your selection in
the @Maximum Pres field. Select Stop, Continue, or Shutdown to set
the pump's response to sensing operation at maximum pressure.
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MORE MENU
To access other options, select /More/ (Figure 4.4).
·Error Recovery
>More
Figure 4.4 Selecting /More/
The More Menu (Figure 4.5) contains additional, miscellaneous, user
preferences, such as the units the pressure is displayed in and how
quickly field choices scroll when the [+] and [-] keys are pressed and
held.
Pressure Units
Purge Mode
PSI
Flow
------------------------------------------------------Cursor Speed
Status Lock
Ready Output Active
Medium
Off
H
Figure 4.5 The P1000's More Menu
Pressure Units
Select either PSI, BAR, or MPa as your preferred units. All menus
and screens that show pressure units will reflect the selection.
Purge Mode
Select either Flow, Pressure, or Both in the Purge Mode field. Your
selection is reflected on the Purge Menu and is used as the primary
purge parameter. Select Flow if you want to purge based on a flow
rate, Pressure if you want to purge based on an operating pressure, or
Both if you want both flow and pressure parameters to govern
purging.
Purging in Pressure or Both mode requires a certain amount of back
pressure in the system. Ensure that your analytical column can
withstand the purge pressure (or use a flow restrictor or old column),
and do not open the bypass valve.
NOTE: You can select the P1000 purge modes from the Purge Menu.
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Cursor Speed
Cursor Speed is used to change how quickly choices scroll on the
display when the [+] and [-] keys are pressed and held, and how
quickly a menu scrolls (up and down) when the arrow keys are
pressed and held. Select Fast, Medium, or Slow.
Status Lock
Status Lock prevents a run file from being edited from the Status
Menu.
The Status Screen is unaffected by Status Lock; it can always be
viewed.
Ready Output Active
The Ready output, located on the back of the pump, continuously
sends an electrical signal to any device hardwired to it. Use the
Ready Output Active field to choose whether the signal is either a 5V
signal (Hi) or a 0V signal (Lo) whenever the pump is in a READY
state. If the pump is not READY the other signal is output.
Whenever the pump's Ready Output is hardwired to a
SpectraSYSTEM autosampler to coordinate injections, it should be
set to provide "Hi" voltage in the READY state.
Shutdown Option (P1000)
The Shutdown Menu (Figure 4.6) contains the parameters the pump
uses after it has been in a READY state, without a run being started,
for a specified length of time after time from READY has been
reached. More information about the Shutdown Menu is found in
Chapter 3 on page 35.
Flow
Time
1.00
20
Figure 4.6 The Shutdown Menu
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The Tests Menu
The Tests Menu allows you to access the pump’s built-in diagnostics,
part of the pump’s advanced features. This section assumes that the
source of the problem is known to be the SpectraSYSTEM pump. If
you are not certain that the pump is the source of trouble, refer to
General LC System Troubleshooting, on page 97.
To access the Tests Menu, select /TESTS/ from the Main Menu
(Figure 4.7):
·
FILE
>TESTS
·OPTIONS
Figure 4.7 Main Menu with /TESTS/ selected
The Tests Menu (Figure 4.8) consists of five items. Tests are divided
into three specific menus, for convenience: diagnostic tests,
calibration tests, and service tests. The Maintenance Log is described
fully in Chapter 5.
>Software Version
·Diagnostics
-------------------------------------------------------·Maintenance Log
·Calibration
·Service
Figure 4.8 Tests Menu
ABOUT RUNNING
TESTS
Tests are internal computer programs that exercise the pump's
hardware and circuitry and verify operation. If any abnormal
behavior is found it is reported as a message or an electronic circuit
board failure code. In most cases the test isolates the problem to the
failed module or component.
Active and Passive
Tests
There are active and passive tests. Passive tests can be initiated at any
time as they do not affect either file memory or pump performance.
Passive tests are usually initiated by pressing [ENTER]. Active tests
require that the pump be idle before being initiated, since the pump's
valves and motor might be engaged during the test. Usually, active
tests are initiated by pressing [RUN], and are stopped by pressing
[STOP]. Some tests stop by themselves. An active test should not be
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49
performed while the pump is in operation, as it will interfere with
pump operation.
NOTE: Pressing [STOP] during a passive test can interrupt pump
operation.
Initiating Tests
To initiate a test, move the cursor to the test's name and press
[ENTER]. Always follow the instructions displayed on the pump
when you initiate a test. In some cases the message, "Pump must be
stopped to run test" might be displayed if you attempt to run an active
test while the pump is in RUN. Alternately, if the pump is stopped
when you initiate a test you might see the message, "The Pump Must
Be Running to Perform This Test." In most cases, the pump will
initiate an active test if the pump is in INIT, EQUIL, or READY.
Usually you will press [ENTER] to initiate a passive test, or [RUN] to
initiate an active test. Some tests display instructions. In these cases,
follow the instructions in the message to proceed.
Test Results
After each test is run a message appears advising you of the results of
the test. In most cases, if trouble is found, the message indicates the
failure or failed component. Specific test menu descriptions begin
below.
Flow Stability and
Hardware Series
Test Routines
Under most circumstances the Flow Stability and Hardware Series
tests will provide a thorough evaluation of the condition of your
pump. We recommended that these two tests be used first if the
performance of the pump is in question. The Flow Stability test is
described on page 51 and the Hardware Series Tests is described on
page 61.
SOFTWARE
VERSION
(PASSIVE)
Selecting /Software Version/ displays the version of software
contained in the pump. The particular version of software resident in
your pump will vary depending upon the date of manufacture or upon
the date of software upgrade.
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THE DIAGNOSTICS
MENU
The Diagnostics Menu (Figure 4.9) contains three items commonly
used to evaluate the pump and an additional selection to allow the
pressure transducer's output to be zeroed.
>Flow Stability
·Measured Parameters
-------------------------------------------------------·Check Valve Test
·Zero Pressure
Figure 4.9 The Diagnostics Menu
Flow Stability
Your pump is constantly monitoring its flow stability while pumping.
An internal software program allows the pump to determine when
flow stability has been adversely affected by leaking check valves,
out-gassing solvents, or other abnormal conditions.
The Flow Stability test (a passive test) evaluates how even the solvent
flow is through the pump. The pump must be pumping solvent for
this test to be run. The test can be initiated when the Status Screen
shows any one of these states: EQUIL, or READY (all pumps.
Completion of the test however, is dependent on the pump being in a
READY state. When the pump is not in a ready state the Flow
Stability screen will read, "Not Ready". When flow stability is being
evaluated, the screen will read, "Test in Progress. Please Wait."
The pump's cam must go through at least 10 pump cycles (cam
revolutions) to accurately assess stability. The value displayed is
affected by the compressibility of the solvent being pumped and the
compliancy of the hardware (tubing, column, etc.). Therefore, the
results are reported in two ways: a) an overall judgment of the pump
performance which appears in the upper left-hand corner of the
display and b) a number indicating where, within the range, the result
lies. This number is shown in the upper right-hand corner of the
display. Three flow stability readings are possible:
Stable
Acceptable
Unstable
( 0- 25)
(25 - 90)
( > 90)
Unless a very volatile or compressible solvent is being pumped, for
example hexane, a number near the higher end of the range (60-90)
probably indicates that the system is not ideal, and the results of
further troubleshooting might improve the flow stability.
NOTE: The Flow Stability Test might show unstable flow during column
equilibration.
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If the results of the flow stability test are abnormal for your LC
application, follow these steps to locate the problem:
1. Test the integrity of the inlet and transducer check valves by
running a Check Valve test. (See page 52.)
2. Verify that the mobile phase solvents are adequately degassed.
3. Refer to the recommendations of General LC System
Troubleshooting Techniques in Appendix A, page 97.
The flow stability assessment will remain displayed until you stop the
test by pressing any one of the following keys: [ENTER], [∧],
[MENU], or [STATUS].
Measured Parameters
Measured Parameters (a passive test) shows the measured flow rate
(Figure 4.10). The number in parentheses indicates the flow rate
setting in the run file. The calculated flow is based on the flow
calculated during the last 360° of motor rotation.
Calc Flow
(2.00)
1.95
Figure 4.10 An example of the Measured Parameters Menu
The measured parameters will remain on the display until the test is
stopped by pressing any one of the following keys: [ENTER], [∧],
[MENU], or [STATUS].
Check Valve Test
The Check Valve test (an active test) can help you further diagnose
the source of flow stability problems. If the results indicate a
defective check valve, the test should be repeated to ensure the results
were not due to an isolated transient condition, such as a single air
bubble.
This test affects flow accuracy while the test is running. Do not run
the test during an analysis. The pump can be in EQUIL, or READY
and the flow rate must be 2.5 mL/min or less (for standard liquid
ends). If the test is activated and the current flow rate is greater than
2.5 mL/min, a message will be displayed, prompting you to reset the
flow rate. In general, the flow rate must be set to one-quarter or less
of the maximum flow rate of the liquid ends.
HINT: Defective check valves tend to perform better at higher column
pressures. Lowering the column pressure by decreasing the flow rate
increases the test's sensitivity of marginally operating check valves.
NOTE: The inlet check valve is located at the base of the inlet liquid end.
The transducer check valve is located at the base of the pressure transducer.
To activate the test select /Check Valve Test/. Follow the displayed
instructions. A message will inform you of the 8 - 10 pump cycle
delay before test completion. During this time, the condition of the
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inlet and transducer check valves of the pump are monitored. When
the monitoring period is complete, pumping returns to normal
constant flow control and a message is displayed, showing the results.
Messages are listed in Table 4.1.
NOTE: Changing mobile phase concentration might cause the test to report
a good check valve as defective. Stabilize composition before running the
test.
Pressing [RUN] after the results are displayed will rerun the test.
Stop the test by pressing [ENTER] or [∧].
Table 4.1 Check Valve Test Results
Both check valves good
Both check valves are performing well.
Transducer check valve
is defective
The transducer check valve should be replaced. See Chapter 5, Required
Maintenance for instructions.
Inlet check valve might
be defective
The inlet check valve might be defective. An air bubble lodged in the check
valve or piston seal or a slight leak in an inlet fitting might cause this
message to be displayed. Verify that solvents are adequately degassed and
that fittings are tight. Purge the pump and rerun the test to verify the
message. If this same message is displayed, replace the inlet check valve.
See Chapter 5, Required Maintenance for instructions.
Bubbles or leaks likely.
Check degas
The check valves are not the cause of flow problems. Verify that solvents
are adequately degassed and that fittings are tight. Observe the inlet tubing
while purging the pump. If air bubbles are seen, increase the helium flow
rate (if helium degassing), or tighten the leaking fitting. Tighten bottle caps.
Ensure solvent supply is vented.
NOTE: Pulse dampeners should not be used with SpectraSYSTEM pumps.
The flow is dynamically controlled and will be adversely affected by
compliant loads.
Test aborted, Pump not
referenced in 10 Cycles
The pump is not able to establish a reference column pressure within 10
pump cycles. The pump has serious flow problems. Verify that the solvents
used are miscible in all concentrations encountered. If possible for your
column, increase the column pressure by raising the flow rate. The check
valves require more than 100 psi column pressure to operate properly.
Defective check valves will usually operate well enough at higher pressures
to allow the test to run.
Test aborted
By Operator
The test was stopped before the pump could count 8 cycles.
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Zero Pressure
The pump allows the pressure transducer's output to be zeroed
automatically without the need for adjustment of potentiometers. The
pump should be stopped before selecting /Zero Pressure/. The display
will show:
Release system pressure,
then press ENTER key.
Figure 4.11 Release system pressure prior to zeroing the pressure
transducer's output
Release the system pressure by opening the bypass valve or removing
the column from the system to ensure that the transducer is actually
sensing zero system pressure. Otherwise, a message showing
"Unable to Zero" will appear. Follow the instructions to complete
zeroing the pressure. To abort the test, press [ENTER], or [∧], or
[STOP]. This will return the zero setting to its previous value.
THE MAINTENANCE
LOG
The Maintenance Log is fully described in Chapter 5, Required
Maintenance.
THE CALIBRATION
MENU
The Calibration Menu (Figure 4.12) contains a Flow Calibration
"test". The flow Calibration can be run in one of three modes.
·Flow Calibration
Figure 4.12 The Calibration Menu
Flow Calibration
The Flow Calibration Menu performs some internal calculations
based on user-measured values. This is a passive test but it uses the
[RUN] key. Unless run incorrectly, this test will not interfere with
pump operation. Select /Flow Calibration/ to access the flow
calibration menus.
The test is run in one of three modes. Select either Meter, Fixed
Volume or Fixed Time from the Flow Calibration Menu (Figure 4.13).
Depending on your selection, the display will allow you to enter values
that enable the test to be completed.
These are described in Figure 4.13.
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·Fixed Time
·Meter
·Fixed Volume
Figure 4.13 Flow Calibration Menu
Table 4.2 Flow Calibration Modes
Calibration Mode
Value to Enter
Fixed Time
Measured Volume (mL)
Fixed Volume
Measured Time (min)
Meter
Measured Flow
Fixed Time: Measured Vol (mL)
This calibration mode assumes that you have collected and measured
a specific volume pumped during a fixed time period. Selecting
Fixed Time displays the Fixed Time Menu (Figure 4.14).
·Calculated Vol.
·10.0 mL
·Measured Vol.
9.5 mL
Figure 4.14 The Fixed Time Menu
(NOTE: The Measured Vol. value was artificially input to
demonstrate the menu function.)
1. Enter the theoretical volume for the fixed time period in the
Calculated Vol. field.
2. Enter the measured volume for the fixed time period in the
Measured Vol. field.
3. Press [RUN] to initiate the test. During the test, the pump
determines a new flow correction factor to compensate for the
inaccuracy in the flow rate. The Flow Correction Menu
displays the results of the test. Figure 4.15 shows example
results.
OLD
Flow Correction
100.00%
Use
NEW
101.00%
Figure 4.15 The Flow Correction Menu with example fixed time
calibration results
OLD: The previous flow rate correction factor default or from
a previous flow calibration test.
NEW: The new flow rate correction factor based on the
Measured Vol. value.
Flow Correction: Use the [+]/[-] keys and press [ENTER] to
select one of three choices:
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55
Use:
Use NEW flow correction factor. The factor remains in
effect until you turn off the pump or initiated the
NOVRAM.
Save: Save NEW flow correction factor to NOVRAM. This
factor remains in effect until you save a different value
over it, or until you reinitialize the NOVRAM
(TESTS/SERVICE/Test 271). Test 271 replaces this
value with the default flow correction factor.
Scrap: Discard the NEW (previous) flow calibration factor and
keep the current value.
Press [RUN] to complete the test.
Fixed Volume: Measured Time (min).
This calibration mode assumes that you have externally timed the
period in which a specific volume has been pumped.
Selecting Fixed Volume displays the Fixed Volume Menu
(Figure 4.16).
·Calculated Time.
·10.00 min
·Measured Time
9.50 min
Figure 4.16 The Fixed Volume Menu
(NOTE: The Measured Time value was artificially input to
demonstrate the menu function.)
1. Enter the theoretical time period for the fixed volume in the
Calculated time field.
2. Enter the measured time for the fixed volume in the Measured
Time field.
3. Press [RUN] to initiate the test. During the test the pump
determines a new flow correction factor to compensate for the
flow rate inaccuracy.
OLD
Flow Correction
100.00%
Use
NEW
101.00%
Figure 4.17 The Flow Correction Menu with example fixed volume
calibration results
OLD: The previous flow rate correction factor default or from
a previous flow calibration test.
NEW: The new flow rate correction factor based on the
Measured Vol. value.
Flow Correction: Use the [+]/[-] keys and press [ENTER] to
select Use, Save, or Scrap as described above.
4. Use the [+]/[-] keys to choose Use, Save, or Scrap.
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Thermo Scientific
5. Press [RUN] to complete the test.
Meter: Measured Flow (mL/min)
This calibration mode assumes that you have externally measured the
precise flow rate that the pump is operating at while set at a specific
flow rate.
Selecting /Meter/ displays the Meter Menu (Figure 4.18).
·Selected Flow.
·1.00 Mn
·Measured Flow
1.00 Mn
Figure 4.18 The /Meter/ Menu
(NOTE: The Measured Time value was artificially input to
demonstrate the menu function.)
1. Enter the set flow in the Selected Flow field.
2. Enter the measured flow in the Measured Flow field.
3. Press [RUN] to initiate the test. During the test the pump
determines a new flow correction factor to compensate for the
inaccuracy in the flow. The Flow Correction Menu displays
the results of the test. Figure 4.19 shows example results.
OLD
Flow Correction
100.00%
Use
NEW
101.00%
Figure 4.19 The Flow Correction Menu with example fixed volume
calibration results
4. Use the [+]/[-] keys to choose Use, Save or Scrap as described
for the Fixed Time Menu.
5. Press [RUN] to complete the test.
To exit the flow calibration menus without entering any values, press
[∧] until you return to the Calibration Menu.
NOTE: Do not press [STOP] unless you have already entered a new value
in one of the flow calibration menus. If the pump is in RUN, doing so will
interfere with your analysis. Use [∧] to exit the flow calibration menus
instead.
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THE SERVICE
MENU
The Service Menu (Figure 4.20) contains several service-related tests,
including the Hardware Series test.
>Current History
·Lifetime History
------------------------------------------------------·ROM Test
(200)
·RAM Test
(201)
·Cycle Step Count
(205)
·External Inputs
(206)
·Display Test
(208)
·Transducer Range
(209)
·Motor Step/Valve
(211)
·Hardware Series
(220)
·Initialize NOVRAM
(271)
Figure 4.20 The Service Menu
The numbers in parentheses refer to a similar test found in earlier
SpectraSYSTEM pumps. They are included for the convenience of
users and service personnel familiar with this previously-used
numbering scheme.
Current History
By selecting /Current History/ you access a chronological list of
operating state changes. The negative number on the far left indicates
the time (in minutes) between the time the Current History Menu was
accessed and the state change occurred. More specific information
about reading the Current History Menu is found in the
SpectraSYSTEM Pumps Field Repair Manual.
To exit the Current History, press [ENTER].
Lifetime History
By selecting /Lifetime History/ you access a log of five measured
items relating to the entire time the pump has been in operation. An
example Lifetime History Menu is shown in Figure 4.21.
The top line shows 1) the total time that the pump's motor has been
running in hours (Hr) and 2) the total number of strokes in thousands
(kSt) taken by the cam; the bottom line shows 3) the number of times
the pump has been powered-on (on), 4) the number of times the pump
has been powered-down (off), and 5) the number of times an error
occurred when NOVRAM was written to upon power-down (bad).
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Thermo Scientific
Press any one of the following keys to exit the Lifetime History
screen: [ENTER], [∧], [MENU], or [STATUS].
1.2 Hr
24on
2.3kSt
23off
0bad
Figure 4.21 The Lifetime History Menu
ROM Test
(Passive)
The ROM test (200) verifies the integrity of the ROM (Read Only
Memory) in your pump. The ROM is where all of the built-in
programs for the pump operation are stored. If faults are found in any
part of ROM, a message indicating that the test has failed will be
displayed. Press [STOP] to stop this test. Do not to press [STOP]
more than once or else pump operation will be interfered with.
If a failure is indicated, contact Thermo Fisher Scientific.
RAM Test
(Active)
The RAM test (201) verifies the integrity of the RAM (Random
Access Memory) in your pump. The RAM is where your pump files
are stored and where temporary calculations are performed. The
pump must be stopped (STOP) for this test to be implemented. If any
faults are found with RAM, the message shown in Figure 4.22 is
displayed.
RAM TEST failed
Figure 4.22 RAM Test failure message
Contact Thermo Fisher Scientific if this test indicates a failure.
Cycle Step
Count (Passive)
Normally, 12,800 motor drive pulses are required for one revolution
of the pump motor, as detected by the cam sensor. The Cycle Step
Count test (205) displays a count of the number of pulses required for
the last complete motor revolution.
The Cycle Step Count test is a dynamic measurement of the number
of steps counted, the lag amount (the number of steps the count has
shifted since the last revolution), and the number of seconds required
for the last revolution.
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59
Generally, the number of steps should be 12,800 ± 64. The lag value
varies due to the load on the pump. This number should be steady, or
fluctuate no more than ±120 steps.
Start the test by selecting /Cycle Step Count/. To stop the test, press
any one of the following keys: [ENTER], [∧], [MENU], or
[STATUS].
NOTE: The Cycle Step Count test requires that a full cam revolution has
occurred.
External Inputs
(Passive)
The External Inputs test (206) allows you to conveniently monitor the
status of two of the external input lines, STOP and RUN. The STOP
line causes the pump to stop pumping when momentarily grounded.
A momentary ground at the RUN input line causes the run time clock
to begin. Use this test if you are having difficulty interfacing your
pump to a controlling device, such as a SpectraSYSTEM
autosampler.
To run the test, select /External Inputs/. The display continuously
shows the current state of the STOP and RUN inputs (updates every
0.5 second). "Lo" means the input is grounded (active) and "Hi"
means the input is "high" (inactive).
To stop the test, press either [ENTER], [∧], [MENU], or [STATUS].
Display Test
(Passive)
The Display test (208) exercises the pump's display. When initiated,
the display shows staggered alphanumeric characters that scroll from
left to right. Pressing [STOP] freezes the display; pressing [RUN]
resumes movement.
This test is also a keyboard test. Pressing the cursor keys will cause
the alphanumeric display to scroll in that direction.
Other keys can be tested by first pressing [ENTER] to access the key
test. The display will verify other keys such as [STATUS] or
[MENU], as soon as each is pressed.
To return to the scrolling alphanumeric characters, press [RUN],
[RUN]. To stop the test, and return to the Service Test Menu, press
[STOP], [STOP].
Contact your representative if the display appears unusual.
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Thermo Scientific
Transducer Range
(Active)
Transducer Range is not truly a test. It contains a field where you
must enter the calibration value (in mV) for a replaced pressure
transducer. The range is located on the replacement transducer wire.
Your pump features advanced circuit designs which allow the
pressure transducer range adjustment to be set by entering a value
from the keyboard. No adjustment of potentiometers is necessary.
Your pump comes from the factory preset to the proper range. The
value is stored in a NOVRAM. Do not change the transducer
calibration setting unless the pressure transducer or System PCB are
replaced. The calibration number is recorded on a tag attached to the
transducer cable. The System PCB and pressure transducer are not
user-serviceable parts. A qualified service representative must
perform any repair or replacement.
Motor Step
(Active)
The Motor Step/Valve test (211) exercises the pump motor. When
activated, the pump motor is continuously stepped and each switching
valve is sequentially opened and closed at a rate of 1 valve per 0.512
seconds. This test is useful for detecting an intermittently failing
switching valve or pump motor.
Select /Motor Step Valve/ to initiate the test. Follow the instructions.
Each open valve is shown dynamically on the display. The test will
continue until one of the following keys is pressed: [ENTER], [∧],
[STOP], [MENU], or [STATUS].
Hardware Series
(Active)
The Hardware Series test (220) is an extensive evaluation of the
System Printed Circuit Board (PCB), switching valve, pump motor,
and pressure transducer. The System PCB contains all of the circuitry
for the operation of the pump, except for the display functions. Once
activated, the test exercises and diagnoses the condition of various
circuits. The pump must be idle (not pumping) before activating the
test. This test will not affect pump files.
NOTE: The external events connector (if present) must be removed from the
rear of the pump before initiating the Hardware Series test. Otherwise,
"Board Failure: Code 8" might occur.
To activate the test, select /Hardware Series/. Follow the instructions
given on the display. Typically, the display will show:
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61
Release system pressure
Then press ENTER.
Figure 4.23 Initial Hardware Series test message
Open the column bypass valve or otherwise remove column pressure
from the transducer since the pump will operate during the test and an
excessively high column pressure might be generated if not bypassed.
Press [ENTER] to continue the test.
Once the test is activated the display will appear as in Figure 4.24.
Test in Progress
Figure 4.24 Hardware Series test message, after pressing [ENTER]
The pump's components are tested in the following order.
1. Pressure transducer and circuitry
2. Input/output ports
3. Motor drive circuitry
4. Cam marker and circuitry
5. Motor revolution and sine/cosine circuitry
As each portion of the test is completed a message is displayed. If all
components and circuitry are within specifications, the messages
shown in Figure 4.25 are displayed during the test.
If a failure is detected during the test, the failure message is
displayed. It remains displayed until [ENTER] is pressed (the test
resumes).
To stop the test, press [STOP], or press [∧] to return to the Service
Menu.
TRANSDUCER TEST PASSED
------------------------------------------------------PORT TEST PASSED
------------------------------------------------------MOTOR DRIVE TEST PASSED
------------------------------------------------------CAM MARKER TEST PASSED
------------------------------------------------------REVOLUTION TEST PASSED
------------------------------------------------------Hardware series tests completed - PASSED
Figure 4.25 No problems found during the Hardware Series test.
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If problems are found during the test, a message suggesting the most
likely failure is displayed, although in some cases other failures are
possible. The messages shown in Table 4.3 indicate a possible
System PCB failure.
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63
Table 4.3 Errors indicating possible System PCBA failure
BOARD FAILURE: CODE XXX
If the failure is identified as a component on the system printed circuit
board or if the test cannot determine the failed component, a message is
reported where XXX is a 1-, 2- or 3- digit number.
8
Remove the external events connector from the rear of the pump. This
test exercises the input lines and might be affected by attached cabling.
1-100
Pertains to failures of the system printed circuit board. Contact your
service representative.
104, 105
Possible broken or loose pump motor cable wire.
124
Too many motor steps were needed to complete a cam revolution. You
might have a loose motor coupler or faulty System PCB. Contact your
local sales/service representative for service information.
125
Too few motor steps were needed to complete a cam revolution. You
might have a faulty cam sensor or System PCB. Contact your local
sales/service representative for service information.
TRANSDUCER UNPLUGGED
The pressure transducer was not detected. The connector going to the
pressure transducer should be checked. Access to this connector requires
the removal of the pump's outer protective cover. Because there are safety
issues involved in its removal, this should only be performed by a
qualified service technician. The location of this connector as well as the
proper procedure for removing the outer cover are outlined in the Field
Repair Manual.
CANNOT ZERO TRANSDUCER
The transducer circuitry is not able to compensate for the zero offset of
the transducer. Make sure that the system is at zero column pressure
(column bypassed) before starting the test. If so, replace the transducer.
Contact your local sales/service representative for assistance.
CAM MARKER NOT FOUND
This message indicates that the sensor that detects cam revolutions is not
operational. Either the motor coupling is loose or the cam sensor is
defective. This requires tightening of the motor-to cam coupler if loose,
or replacement of the cam sensor. Both of these actions require the
removal of the top cover. Because of safety issues involved in the
removal of this cover a trained service technician should perform this
evaluation.
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Thermo Scientific
Table 4.3 Errors indicating possible System PCBA failure, continued
CAM SENSOR FAILURE
The cam sensor cable is disconnected or defective and needs to be
replaced. Correction of this problem requires the removal of the top
cover. Because of safety issues involved in the removal of this cover a
trained service technician should perform corrective action. Contact your
local sales/service representative for service information.
NO CURRENT TO MOTOR
The test has detected no current flow through the pump motor. Either the
motor cable is unplugged on the System PCB or the entire drive circuitry
is defective. Correction of this problem requires the removal of the top
cover. Because of safety issues involved in the removal of this cover a
trained service technician should perform corrective action. Contact your
local sales/service representative for information on obtaining a
replacement.
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65
Initialize NOVRAM
(Active)
The pump must be stopped for /Initialize NOVRAM/ to be
completed.
NOTE: Initialize NOVRAM (271) has a profound effect upon the pump's
non-volatile RAM. Do not initialize the NOVRAM unless you fully
understand all consequences associated with this action.
By initializing the NOVRAM all files are reset to their default values,
with the exception of the run file. All user-preferences set in
/OPTIONS/ are also returned to their default values. In addition, any
changes that had been made to the Liquid End Type and Flow
Calibration parameters are erased, and these selections are returned to
their default values.
In general, any field value or selection that is normally retained when
the pump is turned off and then on will be reset to its default value
when the NOVRAM is initialized.
NOTE: The pressure transducer's range value is not reset when the
NOVRAM is initialized.
HINT: To retain a single file while initializing the NOVRAM: load it (so
that it becomes the run file), stop the pump, initialize NOVRAM, make a
change to a value within the run file from Status, then select /Save File/ at
the bottom of the Status Menu.
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5
Required Maintenance
Introduction
When properly maintained, your Thermo Scientific pump will
provide years of trouble-free operation. It is important that your
pump receive routine preventive maintenance to ensure reliability and
optimum performance. Properly performed routine, preventive
maintenance also helps keep your warranty valid. Your pump is
designed to encourage proper maintenance by making maintenance
parts easy to access, replace and record.
This chapter describes the Maintenance Log Menu and how to use it.
Some hints to help you extend the maintenance period of your pump
are also included. Easy-to-follow, step-by-step required maintenance
procedures are also contained in this chapter so that you can keep
your pump in optimum working condition. A few maintenance tips
for parts of the pump not directly involved with solvent flow follow
the maintenance procedures. The last section contains replacement
procedures for two user-serviceable parts: fuses and the solvent
switching valve.
NOTE: Maintenance of the pump is the responsibility of the user. Routine
maintenance is not provided under warranty. However, planned
maintenance contracts are generally available. Please contact your local
representative if you are interested in purchasing a planned maintenance
contract.
THE BENEFITS OF
PROPER
MAINTENANCE
As with most things, there is tremendous benefit in doing things right
the first time. For example, an unusually fast seal failure might
indicate either incorrect installation or a scratched piston. A
scratched piston might be caused by improper installation of the seal
or piston, by allowing the pump to sit idle with a buffered eluant in it,
or by failing to filter your eluants.
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Maintenance Schedule
Table 5.1 Gradient Pump Preventative Maintenance Schedule
Frequency
Procedure
Performed By
Daily
Check waste reservoir.
Empty as required.
User
Check solvent reservoir.
Replenish as required.
User
Replace piston seals.
User
Replace backflush seal.
User
Annually
Check pistons and Kel-F seals.
Sonicate any parts as required.
Maintenance Log
The Maintenance Log provides a convenient way for you to record
maintenance performed on the liquid ends and set intervals for
periodic maintenance. When a maintenance interval has been
exceeded the pump will automatically display a message indicating
that maintenance might need to be performed.
MAINTENANCE
LOG MENU
The Maintenance Log is accessed by selecting /TESTS/ from the
Main Menu, then selecting /Maintenance Log/ (Figure 5.1 and Figure
5.2).
FILE
•TESTS
OPTIONS
Figure 5.1 Main Menu with TESTS selected
·Software Version
·Diagnostics
--------------------------------------------------->Maintenance Log
·Calibration
·Service
Figure 5.2 Tests Menu with Maintenance Log selected
The Maintenance Log Menu (See Figure 5.3) consists of a table, used
to record dates and volumes, followed by one field used to enter a
value relating to flow, and two additional menu items. All of these
are described in this section.
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Thermo Scientific
ITEM
Seal1
DATE
DUE
VOL
8 AUG95
200
201
-------------------------------------------------------Seal2
8 AUG95
200
201
Piston1
18AUG95
600
400
Piston2
18AUG95
600
400
Inlet
8 AUG95
600
201
X-ducer
8 AUG95
600
201
·Maintenance Position
·Liquid End Type
Figure 5.3 Maintenance Log Menu
The Maintenance
Table
The top half of the Maintenance Log Menu is a table. (Figure 5.3)
ITEM, DATE, DUE, and VOL
The ITEM field remains fixed. "Seal 1" and "Seal 2" should be
paired with "Piston 1" and "Piston 2", respectively, to identify the
inlet and outlet liquid ends. "Inlet" refers to the inlet check valve,
while "X-ducer" refers to the transducer check valve.
Enter the date (day/month/year) in the DATE field for the last time
maintenance was performed on each item.
The pump keeps "liters pumped" counters, in the VOL (volume) field,
for each major maintenance item (the pump seals, pistons, and check
valves). You might set a DUE volume in liters for each item. When
the DUE volume is exceeded by the volume of liters pumped (VOL),
the reminder "MAINTENANCE DUE - SEE PUMP LOG" is
displayed. This message will appear each time a file is initialized.
You might choose to use this feature to set regular intervals for
maintenance, such as seal changes, pump/column cleaning, or simply
to serve as a reminder to verify that the system is operating properly.
The interval remains set until either the date has been updated or the
DUE value has been increased.
In the example shown in Figure 5.3, a fairly complete maintenance
was done on 8 Aug 95, when both seals and check valves were
replaced.
Setting Intervals
The volume of mobile phase that you can expect to pump before the
pump requires maintenance is very dependent upon the eluant being
pumped and your adherence to good chromatographic practices. To
obtain the maximum lifetime and best performance from your pump,
read Extending the Maintenance Period on page 72. Pump pistons
and check valves have been known to last for years. Even the seals
themselves can last more than a year for some applications.
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69
An initial guideline for setting up your Maintenance Log for the first
time is to set both seal DUE counters to 200 liters, and the check
valve and piston DUE counters to 600 liters. Setting a value of zero
(0) for any DUE interval inactivates the Maintenance Log for that
specific item. To inactivate the entire Log, a zero (0) must be entered
for all DUE intervals. Your specific maintenance interval can be
determined by observing pump performance over time.
When a Maintenance Message is Displayed
Whenever the interval has been exceeded, and the message
"MAINTENANCE DUE - SEE PUMP LOG" is displayed, you
should either verify that the pump needs maintenance or that the
pump is operating properly. If a maintenance interval is exceeded
and you find that the pump does not require maintenance, increase the
DUE interval by another 50 liters from the previous setting. Once you
have established an expected interval for your system, use that
interval for routine preventive care.
If you find that the interval before component failure is either
unacceptable or variable, then the source of the problem must be
identified. Read this chapter and Appendix A. Poor chromatographic
practices are by far the most common source of problems. Specific
procedures for inspecting and changing parts begin on page 73.
Maintenance
Position
Selecting /Maintenance Position/ prepares the pump for liquid end
removal or replacement. The display shown in Figure 5.4 appears:
To install or remove
liquid ends press ENTER
Figure 5.4 Maintenance position message
The maintenance position puts the pump's cam into a position to
facilitate liquid end removal.
Liquid End Type
The Liquid End Type Menu allows you to select the proper liquid end
for a specific application.. Do not change the flow range unless you
are installing liquid ends with capacities different from those
purchased with the pump.
Liquid End Type
Flow Range
Normal
0 - 10 mL/Min
Figure 5.5 Liquid End Type Menu
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Thermo Scientific
Selecting Normal, Bio, or SemiPrp
If you select Normal, Bio, or SemiPrp (semi prep) in the Liquid End
Type field, the Flow Range field changes automatically to
corresponds to the preset ranges for these liquid ends.
(Normal = 0 - 10 mL/min, SemiPrp = 0 - 30 mL/min,
Bio = 0 - 10 mL/min, and Other.
Selecting Other
If you select Other in the Liquid End Type field, the Flow Range field
becomes active, allowing you to enter your own flow range.
After changing the liquid end type on the display, press [ENTER]. A
message (Figure 5.6) will prompt you to write down the old values in
the Maintenance Log which correspond to the liquid ends you
presumably just removed. It is important to keep records for each set
of liquid ends you use. If you reinstall the "old" liquid ends, you will
need to reenter the dates and statistics for the "old" ends into the
Maintenance Log table. You are also reminded to enter new values
into the log's VOL field, which correspond to the newly installed
liquid ends. Normally the VOL field is not edited, but when new
liquid ends are installed, ensure that the VOL fields for the
appropriate maintenance items are reset to 0.
Write down old values
ENTER new values in log
Figure 5.6 Reminder to keep proper records when liquid ends are
changed
Flow Correction
An additional menu appears whenever you press an arrow key,
[ENTER], or [+]/ [-] from the display shown in Figure 5.7. This
menu allows you to set a Flow Correction, if desired. OLD and NEW
values are displayed. For no Flow Correction, enter 100.00%.
NOTE: The Flow Correction menu is the same as the menu displayed when
a flow calibration (/TESTS/, /Calibration/, /Flow Calibration/) has been
initiated, except that it does not include the Use, Save, or Scrap option.
OLD
Flow Correction
100.00%
NEW
100.00%
Figure 5.7 Flow Correction Menu
Flow correction is a value, in percent, which adjusts the actual
volume that the pump delivers. As you use the pump, you might feel
that although the pump is set at a specific flow rate, for example
2 mL/min, the pump actually delivers slightly more or less than this
volume per minute. This can be due to a variety of maintenance- or
LC-related reasons (seals, valves, and so on).
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71
If desired, manually enter a flow correction value. This value can be
entered automatically, based on the result of the flow calibration test,
initiated from /TESTS/, /Calibration/, /Flow Calibration/. This test
[which requires you to enter an accurately measured operation value
(time, volume or flow rate)] is fully explained in Chapter 4.
If no correction to the flow is desired, enter a value of 100% in this
field. Values from 90% to 110% are valid. For example, if you pump
for one minute at 1 mL/min and collect 0.95 mL, then the pump is
actually delivering 5% less solvent than expected. To compensate,
enter 105.26% in the Flow Correction field. The pump's Status
Screen will still display a flow rate of 1.0 mL/min, but the pump will
actually deliver 105.26% of what it normally delivers at 1.0 mL/min.
Press [ENTER] to save the value, or simply leave the menu by
pressing an arrow key.
Extending the Maintenance Period
As mentioned earlier, the volume of mobile phase you can expect to
pump before maintenance is due is very much dependent on the way
that the pump is being used. Following these guidelines helps you
extend the life and improve the performance of your pump.
• Use high quality, spectro-grade or HPLC-grade solvents.
These solvents do not usually need to be filtered before use.
• Filter water and prepared solvents through at least a 0.45micron filter before placing them in the solvent reservoirs to
remove particulate matter and organic contamination.
• Avoid pH extremes. Thermo Fisher Scientific offers an
inert/biocompatible pump for mobile phases that are outside
the pH range of 2.2 to 8.0.
• Verify that the solvents used are miscible in all proportions.
This is very important for a buffered mobile phase.
Precipitation of salts quickly damages maintenance parts.
• Never leave the pump filled with buffered solvent when not
pumping. Either lower the flow to 0.1 mL/min. or thoroughly
flush the pump. Flush with at least 25 mL of pure filtered
water.
• The pump should be filled with methanol if it is to be left idle
for more than two days. This avoids the possible growth of
organisms in aqueous solvent systems.
• Never use hydrochloric acids solutions.
• Avoid metal ions that can cause corrosion due to
electrochemical processes. Typical metal ions to avoid:
manganese, chromium, nickel, copper, iron, molybdenum.
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Thermo Scientific
Maintenance Procedures
SAFETY
PRECAUTIONS
Observe the following safety precautions whenever performing
periodic maintenance.
Caution!
A caution alerts you to situations that could result in personal injury.
It also tells you how to avoid them.
High Voltage!
This icon alerts you to the presence of high voltage and to the
potential injury that could occur from electrical shock were you to
come in contact with a specific instrument area or component. It also
tells you how to avoid contact with the high-voltage areas in your
instrument.
Hot Surface!
This icon alerts you to potential injury that could occur from coming
in contact with a heated surface or area on or in an instrument. It also
tells you how to avoid contact with the heated surfaces in your
instrument.
This section includes procedures for:
•
Complete liquid end maintenance (includes disassembly
and assembly)
•
Check valve replacement
•
Passivating stainless steel parts
Also included are maintenance tips for pump parts that are not
involved with pump flow.
TOOLS
The following tools are useful to have on-hand as you perform
maintenance procedures.
•
Tweezers
•
Open-end wrenches (1/4-inch, 5/16-inch, 1/2-inch)
•
Loupe or magnifying glass
•
Allen wrench (Hex head) 9/64-inch
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73
PREPARATION
Prepare the pump for maintenance before performing any
maintenance procedure.
To prepare the pump for maintenance, flush the pump with 25 mL of
methanol. If an incompatible solvent is resident in the pump, flush
with appropriate intermediate solvents before flushing with methanol.
For example, if chloroform is being used as the mobile phase solvent,
an intermediate flush of 25 mL methylene chloride would be
appropriate before flushing with methanol.
LIQUID END
MAINTENANCE
Complete liquid end maintenance includes procedures for seal and
piston maintenance:
•
Removal
•
Disassembly
— inspection for contamination
— cleaning
— piston inspection
— cleaning/replacing parts if necessary
•
Assembly
•
Installation
For thorough cleaning, piston replacement, or total liquid end
reconditioning, the liquid ends must be removed.
Having a second set of reconditioned liquid ends on hand for quick
replacement will save additional time and allow maintenance to be
performed at your convenience. Contact your local Thermo Fisher
Scientific representative if you are interested in obtaining spare
components. Part numbers are included in Appendix C.
NOTE: Keep the liquid end components as clean as possible.
Contamination decreases seal life significantly.
Preparation
1. Flush your pump with 25 mL prior to disassembling your
liquid ends. If methanol is not compatible with the mobile
phase in your pump, flush the system with 25 mL of an
intermediate solvent before flushing with methanol.
2. Remove the front cover, exposing the liquid ends (Figure 5.8).
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Thermo Scientific
R UN
S TATUS
MENU
S TOP
Purge key
E NTER
Purge
Spectr
aSY ST EM
P1000
Crossover tube
Pressure
transducer
Outlet
liquid
end
Bypass valve
Bypass valve tube
Transducer
check valve
Transducer
tube
Bypass valve knob
Inlet
liquid
end
Solvent
inlet
Outlet port
(to autosampler or
manual injection valve)
Inlet check valve
Solvent inlet tube
Waste tube
Lift point
Drip tray
Figure 5.8 Pump with front cover removed
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75
Liquid End Removal
To remove the liquid ends from the pump:
PU-Z016E/DT
1. Remove all tubing attached to the pump heads. Turn the nuts
counter-clockwise to remove (Figure 5.9).
Crossover Tube
Outlet
Liquid
End
Pressure
Transducer
Bracket
BypassValve
Tube
Pressure
Transducer
Inlet
Liquid
End
Transducer
Tube
Solvent Inlet
Tube
Inlet
Check
Valve
Figure 5.9 Liquid ends and tubing
2. Position the pump cam to enable the liquid ends to be removed.
To do this, press [MENU], and select /TESTS/, /Maintenance
Log/. Then move the cursor to /Maintenance Position/ and
press [ENTER]. The display shown in Figure 5.10 appears.
To install or remove
liquid ends, press ENTER
Figure 5.10 Maintenance position message
Press [ENTER] to continue. The pump motor rotates for a few
seconds and then is electrically locked into position. While the
motor rotates the display appears as in Figure 5.11. When the
cam is in the maintenance position, the display in Figure 5.12
appears.
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Thermo Scientific
Install or remove liquid
ends when motor stops
Figure 5.11 The display when the motor moves cam to maintenance
position
X-ducer
(date)
(due)
(vol)
· Maintenance Position
Figure 5.12 The display after the motor moves the
cam to the maintenance position
The pump is now in its maintenance position. It will hold this
position (if power is maintained) until a file is initialized or a
purge is started.
3. Remove the inlet check valve (Figure 5.13) from the inlet
pump head.
NOTE: It is not necessary to remove the check valve to replace a piston,
however, it is easier to remove at this time if total liquid end reconditioning
is to be performed.
PU-Z009E/DT
Inlet
check
valve
Figure 5.13 Inlet check valve
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77
4. Push in the outlet (upper) liquid end and rotate it (90 degrees
counter clockwise) until it releases from the pump module.
Remove the liquid end and set it aside.
5. Push in the inlet (lower) liquid end and rotate it (90 degrees
clockwise) until it releases from the pump module. Remove it
and set it aside.
Liquid End
Disassembly
To disassemble the liquid ends:
1. Separate the pump head from the piston holder housing by
removing the two 9/64-inch hex cap screws. Turn the screws
counter-clockwise.
2. Examine the Kel-F® seal in the cylinder bore. If the seal is
damaged (scratched, warped or torn) it must be removed. Use
tweezers to remove it by pulling gently on the seal's inner
circumference. (Be careful not to scratch the cylinder surface!)
3. Examine the pump head for contamination. Flush the pump
head with methanol or place it into an ultrasonic bath.
PU-Z050E/DT
4. Remove the seal holder from the piston holder housing by
grasping both ends of the exposed tube, and pulling gently
(Figure 5.14).
Seal Holder
Piston Seal
(Spring Side Up)
Pump Head
Cylinder
Figure 5.14 Removing the seal holder from the piston holder housing
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Thermo Scientific
5. Carefully remove the piston seals from the seal holders using
the seal removal tool supplied in the accessory kit. Insert the
tool and wiggle it in a circular manner to remove the seal. (See
Figure 5.15). Flush the holders with methanol if contamination
is present.
Seal Removal
Tool
Piston Seal
(Spring Side Up)
PU-Z025E/DT
Seal Holder
Figure 5.15 Using the seal removal tool
6. While retaining the piston holder, remove the 9/64-inch
retaining cap screw (Figure 5.15). This allows the piston
holder to be removed from the piston holder housing. Separate
the holder, piston, spring and housing.
NOTE: The piston components are spring loaded and might shoot out!
(Figure 5.17)
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79
PU-Z130E/ST
Gently press the piston holder while
you remove the retaining cap screw.
Then slowly let the piston holder out
of the piston holder housing.
Figure 5.16 Retaining the piston holder
7. Examine all parts for wear, corrosion or contamination. Clean
all deposits. Look for wear marks on the stainless steel shaft of
the piston and corresponding wear marks on the inner aspects
of the spring which indicate bending or bowing. If these wear
marks are present, replace the spring (Figure 5.17).
NOTE: It is normal for the piston holder to produce a small amount of
wear particles.
8. Examine the piston carefully under a low-power microscope or
magnifying glass for fine scratches, ridges, or scoring which
can reduce seal life (Figure 5.18). Some apparent scratches are
actually cleanable deposits. The piston can be cleaned by
wiping it gently with a laboratory towlette or cotton swab that
has been immersed in methanol. Replace the piston if
scratched or pitted. The new piston should also be cleaned
prior to installation.
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Thermo Scientific
Bushing
Backup Seal
Bushing
Cap Screws (2x)
Inlet
Check Valve
Pump Head
Kel-F Seal
Piston Seal
Standard Version
Seal Holder
Piston Flush Seal
Retaining
Cap Screw
Lock
Washer
Piston Holder
Housing
Piston
Spring
PU-Z164E/ST
Piston Holder
Figure 5.17 Liquid end components
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81
PU-Z024E/DT
Look for Scratches
in this Portion
of the Piston
Figure 5.18 Piston scratches (under magnification)
9. Thoroughly flush all components with methanol.
Liquid End
Assembly
To replace the piston seal and reassemble the liquid end:
1. Place the seal holder on end on a clean, flat surface. Place the
seal holder into the pump head with the seal down (spring
should face the inside of the pump head.) Install new piston
seals by setting them in position on the seal holder (spring side
up) and gently pressing them into place with the pump head
(Figure 5.19).
NOTE: It is possible to install the seal in the wrong end of the seal holder.
If installed in the wrong end, the seal will not be flush with the top of the
holder. The opposite end of the seal holder is deeper, to accommodate the
piston flush seal. Install the piston seal only in the end closest to the tubes.
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Pump Head
Cylinder
Seal Holder
PU-Z021E/DT
Piston Seal
(Spring Side Up)
Piston Flush Seal
Figure 5.19 Seal installation
2. A piston flush seal (part of a Piston Flush Seal Kit and
normally used with buffers), might be located at the opposite
end of the seal holder. If you use a piston flush seal it should
be replaced once a year. The piston flush seal is not subject to
the higher pressures seen by the piston seal, so maintenance of
this part is only occasionally necessary.
The piston guide bushings do not need replacement. Retain them for
new seal replacement.
To replace the piston flush seal:
a. Use the seal removal tool to remove the piston flush seal.
b. Insert a new piston flush seal into the seal holder (spring
side down). The piston flush seal is thicker than a piston
seal. The seal holder's cavity on the piston flush seal side
is deeper to accommodate the larger size.
c. Ensure that the piston flush seal is flush with the edge of
the seal holder. Use the large end of the seal removal tool
to push the seal into the holder.
3. Place the seal holder into the piston holder housing spring side
up (Figure 5.20).
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83
Inlet Check
Valve
Cap
Screws
Figure 5.20 Seal holder alignment
4. If the Kel-F seal is being replaced, put the new seal in the
pump head cavity now.
5. Install the pump head onto the housing using the two 9/64-inch
Allen head screws.
a) For the inlet liquid end, the pump head must be connected
to the piston holder housing as shown in Figure 5.21 (Inlet
check valve down, retaining cap screw to the left).
b) For the outlet liquid end, the pump head must be oriented
as shown in Figure 5.22.
Evenly tighten the screws to forty inch-pounds (tight).
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PU-Z020E/DT
Piston Holder
Housing
PU-Z029E/DT
Piston Holder
Piston Holder
Housing
Pump
Head
Retaining
Cap Screw
Cap Screws
Inlet Check
Valve
PU-Z049E/ST
Figure 5.21 Installing the retaining cap screw
(inlet liquid end)
Piston Holder
Piston Holder
Housing
Pump Head
Retaining
Cap Screw
Cap Screws
Bypass Valve
Tube Connection
(Hidden from View))
Figure 5.22 Installing the retaining cap screw
(outlet liquid end)
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85
6. Install the piston into the piston spring and then place them
both into the piston holder housing (Figure 5.23). Do not press
the piston through the seal at this time.
7. Compress the piston holder into the holder housing and install
the retaining cap screw with its washer as shown in Figure 5.21
and Figure 5.22, so that the screw enters the slot in the piston
holder. This action pushes the piston through the seal. Tighten
the screw until snug.
NOTE: Make sure the retaining cap screw is oriented on the left-hand side
of the piston holder housing for both the inlet and outlet liquid ends.
Piston Holder
Housing
E-Ring
Piston
PU-Z022E/S
Piston Spring
Figure 5.23 Piston installation
Liquid End
Installation
To install the liquid end assemblies into the pump, the pump must be
in the maintenance position. If the pump has not been switched off
since the liquid ends were removed, the pump motor should still be in
its maintenance position.
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Thermo Scientific
To place the liquid end assemblies in the maintenance position:
1. Press [MENU], /TESTS/, /Maintenance Log/ then move the
cursor to /Maintenance Position/ and press [ENTER]. The
display shows:
To install or remove
liquid ends, press ENTER
Figure 5.24 Maintenance position message
2. Press [ENTER] to continue. The pump motor rotates for a few
seconds and then is electrically locked into position. While the
motor rotates the display shows:
Install or remove liquid
ends when motor stops
Figure 5.25 Pump rotating cam to maintenance position
The pump is now in its maintenance position. The display will appear
as shown in Figure 5.26. The liquid ends can be installed.
X-ducer
(date)
(due)
(vol)
· Maintenance Position
Figure 5.26 The display after the motor moves
cam to the maintenance position
To install the liquid ends:
1. Replace the inlet liquid end first. This liquid end contains
tapped holes for the inlet check valve and the transducer tube.
Install it by pressing in and turning it approximately 90 degrees
counter-clockwise, until it locks into position. Be sure that the
check valve (or the check valve hole, if the valve is not
installed) is pointed down, and the transducer tube hole is
pointed to the upper left-hand side (10 o'clock) (Figure 5.27).
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87
Inlet
Liquid
End
Figure 5.27 Inlet liquid end
2. Replace the outlet (upper) liquid end. This liquid end contains
tapped holes for the crossover tube and the bypass valve tube.
This liquid end is installed by pressing in and turning it
approximately 90 degrees clockwise, until it locks into
position. Be sure that the crossover tube hole is pointed up,
and the bypass valve tube is pointed to the lower right-hand
side (4 o'clock).
3. Replace the check valve and tubing. (Do not over-tighten
fittings.) Generally, a 1/16-turn beyond finger-tight is
sufficient to make a leak-free connection.
HINT: If the transducer check valve has been removed you can distinguish
the two check valves: the inlet check valve has a wider fitting opening than
the transducer check valve (connected to the pressure transducer).
4. After replacing the liquid ends, reset the VOL values in the
Maintenance Log for all replaced components to zero (0).
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POST-INSTALLATION
SEAL CONDITIONING
Follow the procedure below each time you replace liquid end seals.
1. Open the column bypass valve and purge with methanol to
clear air from the solvent lines and liquid ends.
2. Purge the pump through an old column or flow restrictor at
4000 psi for a minimum of 20 minutes. Reduce the flow to
1 mL/min and continue pumping for 15 minutes.
3. Check for solvent leaks. Do not return the pump to every-day
service unless you are sure that no leaks are present.
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89
CHECK VALVE
MAINTENANCE
If the pump has notified you that it is time to replace check valves or
if check valve replacement was recommended in Appendix A,
Troubleshooting, then follow these steps. Check valve maintenance
consists of:
•
Inlet check valve removal and installation
•
Transducer check valve removal and installation
NOTE: The factory-supplied replacement check valves are manufactured
in a clean-room environment and capped to protect them from
contamination. It is very important to maintain a clean environment when
installing them.
Inlet Check Valve
(bottom position)
To remove the existing inlet check valve and install a new one:
1. Remove the solvent inlet tube (Figure 5.27) from the check
valve.
2. Remove the defective check valve by rotating the valve
counter-clockwise with a 1/2-inch open-end wrench.
3. Install the new check valve by rotating clockwise until the
valve is snug against the liquid end cylinder. Reconnect the
inlet tubing. Tighten to finger-tight.
Transducer Check
Valve
To remove the existing transducer check valve (connected to the
Pressure Transducer) and install a new one:
1. Remove the transducer tubing from the transducer check valve
and the inlet pump head (Figure 5.28).
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PU-Z015E/DG
Pressure
Transducer
Transducer
Tube
Transducer
Check Valve
Figure 5.28 Transducer check valve
2. Remove the defective check valve by rotating it counter
clockwise with a 1/2-inch open-end wrench.
3. Install the new check valve by rotating it clockwise until snug,
and tighten with a 1/2-inch open-end wrench. Replace the
connecting tubing. Tighten fittings only enough to stop leaks.
Generally, this is 1/16-turn beyond finger-tight.
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91
Maintenance Tips
This section contains useful maintenance tips for pump parts not
directly related to solvent flow.
DRIP TRAY
A removable, white plastic solvent drip tray is located underneath the
inlet bracket of your pump.
To remove the tray squeeze the top, front-edge of both sides of the
tray together and carefully pull the tray out. You might need to
wiggle the tray as you pull. If you see solvents in the tray, be
particularly careful not to spill them as the tray is removed.
PU-Z017E/DG
HINT: It might be easiest to use the index finger of each hand to push the
sides together.
Drip Tray
Solvent Value
Mounting Plate
Figure 5.29 Drip tray installed
PASSIVATION OF
STAINLESS STEEL
COMPONENTS
All the major type 316 stainless steel components used in the
SpectraSYSTEM pumps are passivated prior to assembly to ensure
the removal of porous particles from the surface and to coat the
surface with a layer of chromium oxide, which is highly resistant to
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Thermo Scientific
corrosion. All stainless steel replacement parts purchased from
Thermo Fisher Scientific are also passivated.
However, stainless steel components are subject to corrosion from
strong acid solutions (in particular, materials containing halides),
organic acids, and sometimes even water. Resistance to corrosion of
the stainless steel components can be enhanced by using the
following procedures.
CAUTION—Chemical Hazard! Take care when passivating with
strong acids. Wear protective eye covering and protective clothing.
NOTE: Before installing any new parts not supplied from the Factory such
as stainless steel tubing, the parts should first be passivated using the
methods below.
NOTE: DO NOT expose a column to the passivation mixture. Remove the
column before pumping if it is necessary to pump passivation solvents
through the pump. It is preferable, however, to remove the components
from the pump and then passivate them apart from the system.
1. When the surface area to be passivated is thoroughly clean, it is
passivated by wetting the surface with a 20% nitric acid
solution in deionized water for about 10 minutes at room
temperature.
2. After passivation, thoroughly clean the parts to remove any
residual nitric acid. Wash with deionized water until the
system is neutral to pH paper. Follow up with another wash
using 50-50 water/methanol followed by methanol. When
thoroughly clean, blow dry using nitrogen. (Do not use the
laboratory air system or air from a compressor that might
contain an oily residue.)
If frequent passivation is required to protect your pump from
aggressive solvent systems, you might want to consider using the
inert version of SpectraSYSTEM pumps. The inert pump parts do not
require passivation.
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93
Repair Instructions
If troubleshooting has pointed to a blown fuse in the power entry
module, use the procedures below to make repairs.
POWER ENTRY MODULE
FUSE REPLACEMENT
Instrument power is supplied by two 4.0-amp fuses housed in the fuse
compartment of the power entry module, above the power cord
receptacle.
To replace the fuses:
1. Ensure that the power cord is not connected to the pump.
2. Use a small, flat blade screwdriver to pry open the power
selector/fuse cover. You will probably hear the top edge of the
cover snap as it is pried open.
3. Pull out the fuse holder and discard the bad fuse. Place the
new fuse into the holder with the metal end visible.
4. Snap the fuse holder back into place.
NOTE: If the power selector barrel accidentally comes out, be sure to
replace it so that the correct voltage for your area shows through the
voltage window.
5. Firmly snap the housing cover back in place. Be sure that the
correct voltage is visible in the voltage window.
HINT: Use two thumbs to push up on the top half of the cover as you
push in.
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Thermo Scientific
A
Troubleshooting
Introduction
Your SpectraSYSTEM pump is designed to operate trouble-free for
many years when properly maintained. Most pump problems can be
avoided by simple, periodic maintenance, as described in Chapter 5.
However, in the event that an error message is displayed or if a
mechanical or electrical failure is suspected, the problem can be
easily diagnosed. Further, if the diagnosis indicates that a problem
exists with non user-serviceable parts inside the pump, a qualified
Thermo Fisher Scientific service representative can quickly and easily
replace most malfunctioning parts.
This appendix contains information on:
•
Theory of operation
•
General LC system troubleshooting
•
Pump-specific hardware troubleshooting
•
Error Messages
•
Display Messages
A quick-reference hardware troubleshooting guide is included at the
end of this appendix that includes tips for diagnosing and remedying
hardware problems. This guide can save you time in diagnosing
problems when the symptoms are known.
Theory of Operation
An isocratic pump works by first pulling a solvent into a valve.
Solvent travels to the pump head, where a piston regulates the flow of
the mixture to an outlet tube. The solvent is routed through the
pressure transducer, into a second pump head, then through a bypass
valve (closed during normal operation), and finally out to the LC
system. The pump's outlet tubing is then generally connected to an
automatic injector, such as an autosampler.
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95
Troubleshooting Your Pump
SAFETY
PRECAUTIONS
Observe the following safety precautions whenever troubleshooting
hardware difficulties.
Caution!
A caution alerts you to situations that could result in personal injury.
It also tells you how to avoid them.
High Voltage!
This icon alerts you to the presence of high voltage and to the
potential injury that could occur from electrical shock were you to
come in contact with a specific instrument area or component. It also
tells you how to avoid contact with the high-voltage areas in your
instrument.
Hot Surface!
This icon alerts you to potential injury that could occur from coming
in contact with a heated surface or area on or in an instrument. It also
tells you how to avoid contact with the heated surfaces in your
instrument.
TROUBLESHOOTING
TIPS
Eliminate all other possible sources of trouble
Before you spend any time trying to diagnose a suspected pump
problem you should verify that the pump is the only source of
difficulty. Systematically eliminate all other instruments in your LC
system as the source of trouble. If you are not sure which component
of your chromatography system is responsible for poor system
performance the General LC System Troubleshooting section
beginning on page 97 of this appendix provides useful suggestions.
When you're sure it’s the pump
Once you have isolated the pump as the only remaining source of
difficulty, a variety of self-tests are built into the pump to help you
determine if your pump is operating correctly.
The next section describes the tests found in the /TESTS/ menu item.
Instructions for the built-in hardware and electronics diagnostics are
contained within the description of the Test Menu.
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Thermo Scientific
Table A.1 General Troubleshooting Table
Symptom
Cause/Remedy
1. No flow.
a) Check mobile phase connections,
b) Check for leaks,
c) Check pump troubleshooting guide.
2. High back pressure.
a) Check flow rate and system/column
specifications,
b) Check for tubing or column blockage,
c) Check pump troubleshooting guide.
3. Unstable baseline or
drift.
a) System/column not equilibrated; allow more
time,
b) Check detector troubleshooting guide,
c) Check pump troubleshooting guide.
4. Baseline noise.
a) Check for air bubbles in system, degas
solvents,
b) Check for system/solvent contamination,
c) Check pump troubleshooting guide,
d) Check PC1000 troubleshooting guides.
5. No peaks.
a) Check detector and data system connections,
b) Check autosampler troubleshooting guide,
c) Check sample retention with
chromatographic conditions.
6. Contaminating/ghost
peaks.
a) Clean system and column,
b) Check autosampler troubleshooting guide,
c) Check pump troubleshooting guide.
7. Poor peak shape.
a) Check system for leaks,
b) Check fittings and tubing lengths,
c) Check column performance,
d) Check autosampler troubleshooting guide,
e) Check pump troubleshooting guide,
f) Check detector troubleshooting guide.
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Table A.1 General Troubleshooting Table, continued
Symptom
Cause/Remedy
8. Poor retention time
reproducibility.
a) Check system for leaks and bubbles,
b) System/column not equilibrated, allow more
time,
c) Check column performance,
d) Check pump troubleshooting guide,
e) Check autosampler troubleshooting guide,
f) Check ISM or data system troubleshooting
guide.
a) Check column performance,
9. Poor peak area
reproducibility.
b) Check autosampler troubleshooting guide,
c) Check data system troubleshooting guide.
10. Non-integrated or too
many peaks.
a) Check integrator or data system
troubleshooting guide.
11. No instrument of device
control.
a) Check cable connections,
b) Check system configuration,
c) Check individual instrument troubleshooting
guide,
d) Check integrator or data system
troubleshooting guide.
For more detailed chromatographic troubleshooting, refer to any
HPLC troubleshooting reference book or call your local sales or
service representative.
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Table A.2 Pump-specific Hardware Problems
Symptom
Possible Cause
Diagnostic/Remedy
1. No response when
power is switched on.
a) Power cord not firmly
installed.
a) Re-seat cord.
b) Power cord defective.
b) None. Replace cord.
c) Power entry module fuse
blown.
c) None. Refer to page 94 for fuse
replacement.
a) Display contrast needs
adjustment.
a) Press [STATUS]. Press and hold the
right-arrow key. Press the [+] or [-]
key to adjust the display contrast.
Press [STATUS] again.
b) Internal fuse blown.
b) None. Contact Thermo Fisher
Scientific representative for service.
3. No display.
a) System PCB defective.
a) None. Contact Thermo Fisher
Scientific representative for service.
4. Only fan runs with
power on.
a) Internal fuse blown.
a) None. Contact Thermo Fisher
Scientific representative for service.
b) Display cable
loose/unplugged.
b) None. Contact Thermo Fisher
Scientific representative for service.
5. No response to keypad
entry. Display OK.
a) Keypad defective or
System PCB defective.
a) None. Contact Thermo Fisher
Scientific representative for service.
6. Random display.
a) Display defective.
a) Run Display Test page 60. Contact
Thermo Fisher Scientific
representative for service.
7. Pump motor will not run.
a) Max pressure set to zero.
a) Press [STATUS]. Set Maximum
Pressure to a value > 100 psi.
b) Motor defective.
b) Run Hardware Series Test page 61.
Contact Thermo Fisher Scientific
representative for service.
c) Motor cable unplugged.
c) Hardware Series Test page 61.
Contact Thermo Fisher Scientific
representative for service.
d) Drive circuit.
d) Hardware Series Test page 61.
Contact Thermo Fisher Scientific
representative for service.
2. No display. Fan and
pump run OK.
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99
Table A.2 Pump-specific Hardware Problems, continued
Possible Cause
Diagnostic/Remedy
e) Internal fuse blown.
e) Hardware Series Test page 61.
Contact Thermo Fisher Scientific
representative for service.
f) Target pressure low.
f) None. Press [PURGE] and then
reinitialize file.
8. Oil found on inlet
bracket.
a) Main bearing overlubricated.
a) None. Small amount of oil is
normal.
9. Solvent not switching.
a) Switching valve cable loose.
a) Hardware Series Test page 61.
Reconnect cable.
b) Switching valve defective.
b) Hardware Series Test page 61.
Replace solvent switching valve.
c) Switching valve drive
defective.
c) Hardware Series Test page 61.
Contact Thermo Fisher Scientific
representative for service.
d) Cam marker failure.
d) Hardware Series Test page 61.
Contact Thermo Fisher Scientific
representative for service.
a) Internal fuse defective.
a) Hardware Series Test page 61.
Contact Thermo Fisher Scientific
representative for service.
b) Switching valve drive
failure.
b) Hardware Series Test page 61.
Contact Thermo Fisher Scientific
representative for service.
a) Check valve failure.
a) Flow Stability Test page 51. Replace
Check Valve Test page 52. Replace
check valve Appendix A, page 90.
b) Immiscible solvents.
b) Flow Stability Test page 51. Run
Check Valve Test page 52. Change
solvent system.
c) Unstable load (column).
c) Flow Stability Test page 51. Check
Valve Test page 52. Pump must see
stable, non-compressible load.
d) Insufficient degas.
d) Flow Stability Test page 51. Check
Valve Test page 52. Increase helium
rate (if helium degas) or decrease
flow rate (if vacuum degas). Use
vent line and good bottle cap seal.
Symptom
10. Switching valve does not
click open.
11. Flow unstable (will not
go READY).
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Thermo Scientific
Table A.2 Pump-specific Hardware Problems, continued
Possible Cause
Diagnostic/Remedy
e) Circuitry failure.
e) Hardware series Test page 61.
Contact Thermo Fisher Scientific
representative for service.
f) Partially clogged frit or filter
on high pressure side of
pump.
f) Hardware Series Test page 61.
Replace filter or frit.
a) Pressure transducer failure.
a) None. Contact Thermo Fisher
Scientific representative for service.
b) Circuitry failure.
b) Hardware Series Test page 61.
Contact Thermo Fisher Scientific
representative for service.
13. Pump goes from RUN
immediately to READY
(will not maintain RUN
state).
a) Run file has only one time
line.
a) View run file. Add time line and
reload file.
14. Pump will not start or
stop remotely.
a) Incorrect wiring.
a) External Inputs Test page 60.
Correct wiring.
Symptom
12. Sudden shift in pressure
display with no flow.
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101
Table A.3 Error Messages
BELOW MINIMUM
PRESSURE;
CHECKSUM ERROR
BAD PROGRAM;
CODE ERROR
PROGRAM LOST;
CODE ERROR
STACK UNDERFLOW;
CODE ERROR
STACK OVERFLOW;
CODE ERROR
FALSE POWER FAIL;
EXCEEDS FLOW RANGE
MAX PRESSURE
EXCEEDED;
MOTOR STALLED
OVER MAXIMUM
TEMPERATURE;
POWER FAILURE
CONTINUE;
POWER FAILURE
STOP;
POWER FAILURE
SHUTDOWN;
ZERO FLOW RATE
102
The column pressure has fallen below the file's Minimum Pressure setting.
Check for mobile phase leaks.
The program memory might have been corrupted. Make a note of the
circumstances which preceded the message and contact Thermo Fisher
Scientific.
The program code has errors. Make a note of the software version and the
circumstances which preceded the message. Contact Thermo Fisher
Scientific.
The program code has errors. Make a note of the software version and the
circumstances which preceded the message. Contact Thermo Fisher
Scientific.
The program code has errors. Make a note of the software version and the
circumstances which preceded the message. Contact Thermo Fisher
Scientific.
You might have experienced low line voltage ("brown-out") or there might
be hardware problems. Note the circumstances which preceded the
message and contact Thermo Fisher Scientific.
A flow rate was entered in the pump file which exceeded the flow rate
capabilities of the pump. The maximum flow rate for standard
SpectraSYSTEM pumps is 10 mL/min. If higher flow rates are needed,
inert/biocompatible liquid ends are available to increase the flow rate to 30
mL/min. Contact your local sales representative for information.
The column pressure of the system has exceeded the MaxP (maximum
pressure) value entered into the pump file. The file's Maximum Pressure
value might need to be increased. The default value is 3000 psi for
10 mL/min liquid ends (the maximum is 6000 psi). If your operating
column pressure is increasing, check for column plugging.
The motor is unable to maintain the combination of requested flow rate and
needed pressure for operation. Reduce flow rate or check for flow
restriction or plugged column frit.
The pump has overheated. This might be due to blocked ventilation slots
or to a hardware malfunction.
A power failure has occurred or the pump was switched off with the motor
running. The pump has automatically resumed operation. ("Continue" was
selected in /OPTIONS/, /Error Recovery/, AC Power Fail.)
A power failure has occurred or the pump was switched off with the motor
running. The pump has automatically stopped. ("Stop" was selected in
/OPTIONS/, /Error Recovery/, AC Power Fail.)
A power failure has occurred or the pump was switched off with the motor
running. The pump has automatically loaded and run the shutdown file.
("Shutdown" was selected in /OPTIONS/, /Error Recovery/, AC Power
fail.)
A time line (other than Time = 0.0 min) with a zero flow rate was
encountered. To remedy, enter a valid flow rate in the first line of the
pump file. Rates between 0.01 and 10 mL/min are valid for standard
SpectraSYSTEM Pumps. The optional inert/biocompatible liquid ends
extend the maximum flow rate to 30 mL/min.
Thermo Scientific
Table A.4 Display Messages
Maintenance Due
See Log
A volume milestone has been reached. Consult the Maintenance Log for
component by pressing the [MENU] key and selecting /TESTS/,
/Maintenance Log/. For more information, refer to Chapter 5.
Memory Nearly Full
Data Might Not Be Saved
There might not be enough memory available. Double-check the file to
ensure that no parameters or settings were lost. Free memory by deleting
an old or unused file, or by reducing the number of time lines in a file. Try
to save the file again.
Not Enough Room
File Not Saved
The run file changes cannot be saved to the file. Free memory by deleting
an old or unused file, or by reducing the number of time lines in a file. Try
to save the run file once more from the Status Menu.
Run In Progress
No Testing Allowed
The test cannot be initiated because the pump is in RUN or is in HOLD.
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Table A.5 Solvent Compatibility for Pump Wetted Surfaces
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Thermo Scientific
B
Glossary
A
autosampler
an instrument designed to automatically inject samples into the sample flow
path with a high degree of precision and reproducibility; sometimes called
an injector
B
baseline
the reference line at the bottom of a chromatogram from which
measurements are made; a baseline represents the chromatogram that would
be drawn if only the mobile phase (with no sample) were run through the
column
binary
capable of mixing or switching between two solvents
biocompatible
describes components that are inert when used with biological samples;
biocompatible components are usually made from titanium, Teflon®, PEEK,
quartz, or sapphire
buffer
a medium the resists changes in acidity and alkalinity
C
channel
the path along which something (solvent or information) flows
chromatogram
a plot depicting the separated components in a sample (absorbance units
versus time); each component is shown as a separate peak whose
concentration can be determined by studying the area under the peak
chromatograph
the basic set of instruments needed to perform chromatography: a pump,
injector (manual or automatic), a column, and a detector; various recording
and data handling instruments are common additions
chromatography
a means of separating and analyzing mixtures of chemical substances
column
the packed tube through which a sample is passed for separation; the sample
separates according to the way in which it adheres to the column's packing
material
component
an "ingredient" in a chemical mixture, also the individual parts of a liquid
end assembly
conditioning
the process of preparing the surface of the column wall and introducing the
buffer pH conditions into the column before a run
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105
configuration
the way instruments are interconnected to form a system
cursor
a moving or blinking symbol on the display which indicates where
information is entered
D
default
a value or choice built into a system; if no specific choice is made,
instruments will run (or data analyzed) using the default settings
degassing
removal of dissolved gas (i.e., oxygen) from the solvent to prevent bubbles
from forming in the pump; degassing can be done by vacuum or by sparging
detector
the instrument used to detect the presence of a chemical compound
diagnostics
ways of detecting and isolating instrument or software problems
digit
an editable space within a field
display
the backlit LCD screen on all SpectraSYSTEM instruments
E
elution time
the length of time needed to pass a particular sample through a packed LC
column
equilibration
the process used to bring a system (solvent, column, etc.) to a point of
equilibrium, where all thermal and chemical reactions occur at equal rates; a
stable baseline is a good sign of a well-equilibrated system
error message
a printed or displayed message that notifies the user of an error condition
error recovery
user-selectable responses to error conditions detected by the instrument,
such as a power interruption or over-pressure
external event
an action performed by an external device that is under the control of the
current instrument (see also timed event)
F
field
an area in a display, screen, or menu where an entry is required or a choice
must be made
flow parameters
flow rate, solvent, and run time
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Thermo Scientific
flow rate
the rate at which solvent flows through a system
G
ground terminal
a terminal used to connect the ground or earth lead of a signal or contact
closure cable; generally green and/or black
H
helium manifold
a pneumatic assembly containing valves and switches for regulating helium
sparging
helium sparging
see sparging
I
inert
see biocompatible
injection
the manual or automatic introduction of a sample into a chromatography
system
integrator
the instrument used to analyze data and produce a chromatogram
isocratic
constant solvent composition
K
Kel-F seal
the translucent seal, made of Kel-F material, inside the pump head which
faces the piston seal
keypad
all of the keys by which you can communicate with an instrument or
computer
L
LC
Liquid Chromatography
linear
a gradient curve that follows a straight line
liquid end
the inlet or outlet assemblies of the pump consisting of the head, piston,
seals, and sometimes a check valve
Thermo Scientific
107
M
maintenance log
a place to record dates, service, and cumulative solvent volume pumped
menu
a list of choices
method
the set of parameters that define how one or more analyses will be
accomplished
method development
the process of specifying the parameters under which an instrument will
perform a particular function
N
NOVRAM
Non-volatile RAM (random access memory). Computer memory into which
the user can enter information and instructions and from which the user can
recall information. Data in NOVRAM are saved even when the instrument
is switched off.
P
parameter
a value or set of values used to define the characteristics or behavior of an
instrument or system
PEEK
polyetheretherketone; a material frequently used in fabricating
inert/biocompatible components
piston
the short cylinder piece that moves inside the sealed cylindrical opening and
is used to pressurize fluid
piston holder housing
the shaft into which the piston and its holder are housed
piston flush seal
the low-pressure spring seal inside the liquid ends, facing the piston
assembly
piston seal
also called pump seal, a high-pressure spring seal located inside the pump
head
plot
the presentation of analytical data in a graphical manner; typical plots
include chromatogram traces and calibration curves
prime
to flush the solvents contained in a new pump in order to prepare the pump
for solvents chosen by the user
pump
the instrument used to push a liquid solvent through a chromatography
system
purge
to flush the system with fresh, degassed solvent
108
Thermo Scientific
Q
queue
a set of files in a prearranged order
R
RAM
Random Access Memory (computer)
real-time
the current, actual time
reproducibility
the precision with which a piece of data can be repeated; a good measure of
a system's overall performance
retaining screw
also retaining cap screw; the screw which holds the piston assembly into the
piston holder housing
run
a complete analytical operation cycle of the chromatographic system
run file
the file that has been loaded and that the pump is currently operating by
run time
the duration of a sample run, from injection to separation
S
sample
a known or unknown substance in a small quantity
seal holder
a metal part used for pumps fitted with standard parts which contains two
seals, (piston seal and piston flush seal) and allows the pump head and
piston holder housing to be joined
shutdown file
a special file used by the pump after the pump has been in a READY state
for a period of time set by the user
solvent
a substance that can completely dissolve another; the mobile phase of an LC
system
solvent filter
a small cylindrical attachment for inlet tubing used to filter a solvent prior to
the solvent entering a pump
solvent program
a set of time lines indicating a time, selected solvent, and flow rate
sparging
a degassing technique in which solvent gases are replaced with an inert gas
such as helium or nitrogen
status
the current condition
status lock
a feature used to prevent a run file from being changed from the Status
Menu
Thermo Scientific
109
stroke
one complete revolution of the pump's cam which displaces both pistons
system
a set of chromatography instruments that operate together in a concerted
manner to produce an analytical result
T
timed event
an instrument action triggered to occur at a specific, preset time during a run
or analysis
trace
a chromatogram
transducer check valve
the valve which attached to the inlet of the pressure transducer
V
vacuum degassing
the technique of removing dissolved gasses from solvents by passing the
solvent through tubing made of gas-permeable membrane, and creating a
vacuum around the tubing, thus allowing gasses to be evacuated out of the
solvent and into the surrounding chamber
viscosity
the degree to which a fluid resists flow
110
Thermo Scientific
C
Introduction
Kits and Parts Lists
This chapter contains unpacking lists and information for several kits
and accessories available from Thermo Fisher Scientific for use with
your SpectraSYSTEM pump. Described in this chapter are:
• Accessory Kit
p/n A4070-010
• Standard Maintenance Kit
p/n A4050-010
• Standard LC Fittings Kit
p/n A4051-010
• Piston Flush Seal Kit (10 mL)
p/n A4114-010
• Piston Seal Kit (30 mL)
p/n A4084-010
• Solvent Inlet Tube Kit
p/n A4074-010
• Solvent Tube Extension Kit
p/n A4117-010
• Manual Injection Valve Bracket Kit
p/n A4054-010
• Narrow-bore Upgrade Kit
p/n A5190-060
Accessory Kit
Your kit consists of:
2
1
2
2
1
2
1
1
1
1
1
1
1
1
1
3
4 amp, 250V fuse
12-inch piece stainless steel tubing
(0.06 OD x 0.02 ID) (27.5 cm length)
nuts, 0.06 OD
ferrules
seal removal tool
piston seals
hex/ball wrench
4-connection cable
external function connector
20 mL (cc) priming syringe with Luer LOK® tip
Luer adapter
waste tube kit:
48-inch Teflon tubing, 0.031 ID (123 cm)
washer and finger-tight fitting
solvent bottle label
stainless steel tubing, 0.06 OD x 0.007 ID
Thermo Scientific
111
Standard Maintenance Kit
The Standard Maintenance Kit contains the following:
4
1
1
2
1
1
1
6
2
6
1
1
inlet filter cartridges
inlet check valve
transducer check valve
sapphire pistons (0.125 inch-diameter)
barbed fitting (nylon)
piece piston flush tube (Tygon®), 0.0655 ID (approx. 76 cm
long)
syringe (20 cc)
piston seals
piston flush seals
Kel-F seals
seal removal tool
seal insertion tool
Standard LC Fittings Kit
Your kit consists of:
1
1
2
4
4
3
1
storage/carrying case
120-inch piece Teflon tubing, 0.063-inch ID
adapter fittings (10-32M)
Rheodyne nuts/ferrules
Parker type nuts/ferrules
wrenches (sizes: 1/4" - 5/16", 3/8" - 7/16", 1/2" - 9/16")
1/8-inch tube adapter for gas regulator assorted tubing:
stainless steel 0.020-inch ID
stainless steel 0.010-inch ID
Fittings kits contain tubing and fittings commonly needed for LC
systems. These fittings can be used for several different instruments.
If you change your LC configuration or damage connections, the
fittings provided in this kit should allow you to make changes or
replacements quickly and easily. All fittings can be kept in the
compartmentalized storage box.
112
Thermo Scientific
Piston Flush Seal Kit (10 mL)
Your kit consists of:
1
1
2
1
1
1
piece tubing, 30-inch, Tygon (76 cm length)
barbed fitting (nylon)
piston flush seals
seal removal tool
seal insertion tool
syringe, 20 cc
Piston Seal Kit (30 mL)
Your kit consists of:
1
3
1
1
piston (with small O-ring, high pressure)
PEEK wash rings
large O-ring
Piston flush seal (low-pressure)
Solvent Inlet Tube Kit
Your kit consists of:
1
1
bottle cap
tubing, Teflon, 0.063 ID
Solvent Tube Extension Kit
Your kit consists of:
4
1
60-inch extension tubing, with washer and union
(152 cm length)
tubing Teflon, 0.063 ID
Thermo Scientific
113
Manual Injection Valve Bracket Kit
Your kit contains:
1
2
2
2
1
4
2
2
2
1
1
11-3/16 inch steel mounting rod
rod brackets
short column brackets
long column brackets
manual injector valve mount
short set screws (6-32 x 1/4-inch)
flat-head screws (8-32 x 3/8-inch)
screws (6-32 x 7/16-inch)
long set screws (6-32 x 5/8-inch)
Allen wrench (1/16-inch)
12 inches stainless steel tubing, 0.06 OD × 0.01 ID, 12 inches
If you purchased a Rheodyne valve (standard), you also received the
valve, accompanied by Rheodyne's documentation.
Installing the Holder
onto the Valve
To install the valve onto the bracket, do the following:
1. Move the injector valve handle to the "LOAD" position. Using
the Allen wrench supplied with your Rheodyne valve, loosen
the two set screws and remove the injection valve handle.
2. Hold the valve mounting bracket so that the two set screw
holes are on the left. Place the injector valve into the bracket
from the rear. If your injector valve has a remote start cable
attached to it, place the cable into the cut-out on the left side of
the bracket. When aligned correctly the "V" made by the two
flats of the valve shaft will point to the upper left-hand
mounting hole.
3. Fasten the valve securely with the two flat-head (Phillips)
screws.
4. Attach the handle to the valve by tightening the two set screws,
making sure that each screw is positioned over a flat edge of
the valve shaft.
5. Install a long (5/8-inch) set screw into each of the valve
bracket's mounting holes.
6. Install the rod through the valve bracket so that the notched
portion of the rod faces you, as you look at the front of the
injection valve.
114
Thermo Scientific
7. Slide the valve bracket so that it is within the top quarter of the
rod. Tighten the two set screws, securing the valve bracket to
the rod.
8. Brackets for long (22 cm - 25 cm) and short (3 cm - 10 cm)
columns are provided. Choose the bracket size that matches
the type of column you use. Both brackets can be mounted, if
desired.
9. Install a short (1/4-inch) set screw into each column bracket
you want to use. Slide the brackets onto the rod for
positioning. Temporarily tighten the set screws to hold the
brackets in place (Figure C.1).
10. Remove the two top cover screws from the right side of your
SpectraSYSTEM pump or detector. Install a rod bracket into
the lower hole, using a 7/16-inch Phillips-head screw.
11. Rest the rod in the lower rod bracket (with the injector valve
facing toward the front) and place the upper rod bracket on top
of the rod. Attach the upper rod bracket to the pump or
detector, using the other 7/16-inch screw.
12. Re-position the column brackets or manual injector valve as
needed, and tighten the set screws.
Thermo Scientific
115
Slotted Rod
Valve Holder
RUN
STATUS
MENU
STOP
ENTER
SpectraSYSTEM
UV2000
Wrench
Column
Bracket
Rod Bracket
Figure C.1 Manual Injection Valve/Column Bracket mounted to a SpectraSYSTEM instrument
116
Thermo Scientific
DT-Z018/FM
ZERO
Narrow-bore Upgrade Kit
Your kit consists of:
• 0.01” ID bypass, crossover, and transducer stainless steel tubes
• 0.03” ID Teflon solvent inlet tube
• Low-volume outlet liquid-end assembly
• 3 μL static mixer
• 0.007” stainless steel tubing
• Nuts and ferrules for all tubes
• Instruction sheet
Thermo Scientific
117
INDEX
KEYS
@Maximum Pres, 46
[+] and [-] keys, 22, 25
[ENTER] key, 24
[PURGE] key, 24
[RUN] key, 23, 40
[STOP] key, 24, 41
[ ] key, 24
A
AC Power Fail, 46
Accessory Kit, basic, 3, 111
active tests, 49
alphanumeric entries, 25
increasing and decreasing, 22
arrow keys
illustrated, 23
rules, 21
asterisks, 26
B
BELOW MINIMUM, 102
blank key, see PURGE key, 24
Bypass valve, 11
C
Calibration Menu, 54
illustration, 54
cautions
maintenance, 73
troubleshooting, 96
check valves
inlet, illustration, 77
inlet, maintenance, 90
maintenance, 90
test, 52
transducer, illustration, 91
transducer, maintenance, 90
Checklist vii:, 21
CHECKSUM ERROR, 102
CODE ERROR, 102
commands
Hold, 41
Software Version, 50
Commands Menu, 25
Confirmation messages, 26
Current History, 58
cursor
movement, 22
speed, 48
square, 22
underscore, 22
Cycle Step Count test, 59
D
damage
shipping, 3
Degassing, 9
Diagnostics Menu
illustration, 51
display
contrast adjustment, 99
Display test, 60
down-arrow (t), right side of display, 22
drip tray, 92
E
Edit Menu (FILE), 35
Editing parameters during a run, 42
ENTER
KEY DEFINED, 24
Error messages, 27
Error Recovery Menu, 45
EXCEEDS FLOW RANGE, 102
exclamation points, 27
external events
connection for, 7
External Inputs Test, 60
F
fields
@ Maximum Pres, 46
AC Power Fail, 46
Cursor Speed, 48
DATE, 69
DUE, 69
Edit File, 35
Flow (Purge), 39
Flow Range, 70
ITEM, 69
Liquid End Type, 70
Maximum Pressure, 35
Measured Time, 57
Measured Vol, 56, 57
Minimum Pressure, 35
Pressure Units, 47
PSI, BAR, or MPa, 39
Thermo Scientific
index-i
[ENTER], 24
[MENU], 24
[PURGE], 24
[RUN], 23
[STATUS], 24
[STOP], 24
BLANK, 24
kits, 111
maintenance, 10 mL/min piston flush seal, 113
maintenance, standard, 112
manual injection valve bracket
illustration, 116
Manual Injection Valve Bracket, 114
Piston Flush Seal, 113
Solvent Inlet Tube, 113
Solvent Tube Extension, 113
Standard LC Fittings, 112
Purge, 39
Purge Mode, 47
Ready Output Active, 48
Status Lock, 48
Time (Purge), 39
Time (Shutdown), 36
Transducer Range, 61
VOL, 69
FILE
Edit, 34, 35
initializing, 40
Menu, 34
Flow
field of [PURGE] Menu, 39
Flow Calibration Test, 54
Flow Correction, 71
Flow Stability test, 29, 51
front panel
illustration, 23
fuse, power entry module replacement, 94
L
Lifetime History, 58
lifting, 4
liquid end
piston seal, 82
Liquid End Type, 70
liquid ends
assembly, 82
components, illustration, 81
disassembly, 78
inlet, illustration, 88
installation, 86
maintenance, 74
removal, 76
H
Hardware modifications
autosampler, 32
Hardware Series test, 61
results, 62, 64
high voltage, defined, 73, 96
hot surface
defined, 73, 96
I
Increment (+) and decrement (-)
keys
DEFINED, 25
illustrated, 23
INIT, 42
initializing a file, 40
injection valve/column bracket, see kits, manual injection
valve bracket:, 114
inlet bracket, 100
installation
bench space needed, 6
external events connection, 7
power-on response, 7
unpacking, 3
instrument control, 23
K
Kel-F seal, 78
keypad
illustrated, 23
instrument control, 23
moving around, 21
keys
[+] and [-], 22, 25
index-ii
M
maintenance
check valves, see also check valves, 90
drip tray, 92
kits
contents of 10 mL/min piston flush seal, 113
contents of standard, 112
liquid end, see also Liquid Ends, 74
period, extending, 72
piston, 80
piston flush seal, 83
preparing the pump for, 74
tips, 92
Maintenance Log, 68
DATE, 69
DUE, 69
ITEM, 69
menu, 68
illustration, 69
message, 68, 70
setting intervals, 69
table, 69
using, 69
VOL, 69
Thermo Scientific
Maintenance Position, 70
Manual Injection Valve Bracket, 114
MAX PRESSURE, 102
Measured Parameters, 52
MENU
KEY DEFINED, 24
menus
Calibration, 54
Current History, 58
Diagnostics, 51
Edit (FILE), 35
Error Recovery, 45
FILE, 34
FILES, 34
Flow Correction, 71
Lifetime History, 58
Liquid End Type, 70
More (OPTIONS), 47
OPTIONS, 45
Service, 58
Shutdown, 36, 48
TESTS, 49
Menus and Screens, general description of
File Menu, 25
Files Menu, 25
Main Menu, 25
Options Menu, 25
Status Screen, 26
Tests Menu, 25
menusDiagnostics, 51
messages, 26
confirmation, 26
error, 27
user, 26
More Menu (OPTIONS), 47
MOTOR STALLED, 102
Motor Step/Valve test, 61
N
narrow-bore
pump operation, 32
specifications, 20
narrow-bore applications, 32
numeric entries, 25
O
Options Menu, 25, 45
OVER MAXIMUM, 102
P
P1000 Shutdown Menu, 36
passivation of stainless steel parts, 93
passive tests, 49
piston
flush seal, 83, 113
holder housing, 78
scratches, 67
illustration, 82
seal, 82
Piston flush seal kit, 113
power entry module
fuse replacement, 94
POWER FAILURE, 102
power selection
see voltage selection, 4
power-on response, 7
preset choices
scrolling through, 25
selecting from, 25
pressure
setting limits, 35
pressure units, 47
example of changing, 27
Priming the Pump, 11
Program Version, 50
pump
front panel, illustration of, 23
illustration with front cover removed, 75
isocratic basics, 31
LC basics, 31
lifting and carrying, 4
list of routine operations, 34
operating statistics, 58
P1000
description, 31
placement, 6
pressure, 35
rear panel, illustration of, 5
repair, 94
rules for operation, 21
state changes, 58
stopping, 41
theory of operation, 95
Pumps
carrying, 4
narrow-bore, 32
purge
mode
example of changing, 28
starting, 39
stopping, 39
PURGE
internal limits, 38
key defined, 24
Menu, 38
Purge Mode, 47
purging
after priming the pump, 14
example, 29
solvents, 37
R
RAM test, 59
READY, 40
Thermo Scientific
index-iii
Ready Output Active, 48
READY, shown in Status, 42
Rear panel
illustration, 5
repair
fuse replacement, 94
ROM test, 59
RUN, 40
KEY DEFINED, 23
shown in Status, 42
S
safety
icons, 73, 96
safety certification
see Safety Information:, 73
safety precautions
for troubleshooting, 96
saving an entry, 22
scrolling, 25
seals
Kel-F, 78
piston, 82
piston flush, 83, 113
Service Menu, 58
illustration, 58
shipping
damage, 3
Shutdown Menu (P1000), 36, 48
Software Version, 50
solvents
connecting, 8
drip tray, 92
purging, 37
spare parts, list of ix:, 21
stainless steel
passivation, 93
state changes, chronological list of, 58
statistics, operating, 58
status display, 42
STATUS
KEY DEFINED, 24
Status Lock, 48
Status Menu
described, 26
P1000 illustrated, 42
Status Messages, 42
Status Screen
described, 26
P1000 illustrated, 42
STOP
KEY DEFINED, 24
shown in Status, 42
SYNC, 42
index-iv
T
tests
active and passive, 49
Calibration, 54
Check Valve Test, 52
Cycle Step Count, 59
Display, 60
External Inputs, 60
Flow Stability, 51
Hardware Series, 61
initiating, 50
Measured Parameters, 52
Motor/Step Valve, 61
RAM, 59
results, 50
ROM, 59
Service, 58
Software Version, 50
Transducer Range, 61
Tests Menu, 25, 49
illustration, 49
theory of operation, 95
time
shown in Status, 42
Time
field of [PURGE] display, 39
Transducer Range, 61
troubleshooting, 95
isolating the source of problem, 96
safety precautions for, 96
U
unpacking, 3
V
Visual clues on display, 22
voltage select barrel, 4
voltage selection, 4
barrel, 4
illustration, 6
instructions for, 4
Z
ZERO FLOW RATE, 102
Zero Pressure, 54
Thermo Scientific
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