Varian ProStar 400 Instrucciones de operación

Tipo
Instrucciones de operación
Varian, Inc.
2700 Mitchell Drive
Walnut Creek, CA 94598-1675/usa
©Varian, Inc. 2000 - 2004 Printed in U.S.A. 03-914786-00:Rev. 3
ProStar 400
AutoSampler
Operation Manual
03-914451-00:4 1 of 1
Quality Systems At Varian, Inc.
The ISO 9000 series standards were created in Geneva in 1987 to cut through a morass of conflicting
quality definitions. These standards define a model for quality assurance systems in product design,
development, manufacturing, installation, service, and customer support. They are now the worldwide quality
assurance benchmark used to gauge the strength of a company's commitment to quality, and the value of its
quality systems.
Various organizations around the world, such as the British Standards Institution (BSI), provide
certified, objective auditors to scrutinize quality procedures, product development, manufacturing processes,
and customer satisfaction programs. No company can claim ISO 9000 series registration unless it receives a
stamp of approval from the demanding quality assessors of BSI or similar accredited examining body. ISO
9000 series registration constitutes an objective third-party report to determine the level of a supplier's
commitment to quality.
In 1992, Varian, Inc., Analytical Instruments became registered to the most comprehensive of the ISO
9000 series standards — ISO 9001. ISO 9001 registration means that every stage of our quality system,
including product development, manufacturing, final test, shipping, and parts and supplies has been rigorously
examined against the most exacting set of internationally recognized standards. It means we live up to a
standard of quality that you can count on today, and into the future. Our Quality System has received ISO
9001 certification number FM21797.
The quality systems that earned us ISO 9001 registration have direct benefits for our customers:
We can speed instruments to you faster than ever before. Emergency orders can
be processed even faster.
We fill your orders promptly and completely.
We have implemented a system of continuous feedback from our customers —
we are aware of your needs today and tomorrow.
We have improved your productivity by cutting systems failure rates in half and
speeding service response time.
We have embedded continuous improvement into the fabric of our organization
so that we can achieve even higher levels of quality in the future.
We are embedding GLP requirements into our products and services to help you
meet your regulatory compliance requirements.
ISO 9001 registration is not enough. For us, quality is defined by our customers. We are not satisfied
unless you are satisfied. We are striving to understand customer needs, using independent surveys, user
groups, customer advisory boards, and our “Hallmark of Quality” response program, in addition to individual
face-to-face customer contact. Our products and our processes are configured to meet those needs.
We know that you are seeking more than the most advanced processes and top-notch applications expertise.
You want to join forces with a partner committed to delivering world-class quality, reliability, and value — on
time, every time.
Our overriding aim is to be that partner.
Varian, Inc. Analytical Instrument Warranty
03-914412-00:2
1 of 1
Hardware Products
All analytical instruments sold by Varian, Inc. are
warranted to be free from defects in material and
workmanship for the periods specified and in
accordance with the terms on the face of Varian's
quotation or as otherwise agreed upon in writing
between Varian and the Customer. The warranty
period begins on the date of shipment from Varian to
the original Customer. However, where installation is
paid for by the Customer or included in the purchase
price, the warranty period begins upon completion of
installation. If the Customer schedules installation to
start later than 30 days after delivery or if such delay
is caused through the Customer's inability to provide
adequate facilities or utilities or through failure to
comply with Varian's reasonable pre-installation
instructions or through other omissions by Customer,
then the warranty period starts on the 31st day from
date of shipment. Moreover Varian will charge the
Customer for labor and other expenses involved in
making multiple or follow-up installation service calls.
Software Products
Where software is provided within the frame of a
license agreement concluded between the Customer
and Varian, any warranty shall be strictly in
accordance with the terms of such agreement.
In the absence of a license agreement and unless an
alternate warranty period is agreed upon in writing
between Varian and the Customer, the warranty
period is as specified on the face of Varian's
quotation. Varian warrants such software products, if
used with and properly installed on Varian hardware
or other hardware as specified by Varian to perform
as described in the accompanying Operator's Manual
and to be substantially free of those defects which
cause failure to execute respective programming
instructions; however, Varian does not warrant
uninterrupted or error-free operation.
Remedies
The sole and exclusive remedy under hardware
warranty shall be repair of instrument malfunctions
which in Varian's opinion are due or traceable to
defects in original materials or workmanship or, at
Varian's option, replacement of the respective
defective parts, provided that Varian may as an
alternative elect to refund an equitable portion of the
purchase price of the instrument or accessory.
Repair or replacement under warranty does not
extend the original warranty period.
Repair or replacement under warranty claims shall be
made in Varian's sole discretion either by sending a
Customer Support Representative to the site or by
authorizing the Customer to return the defective
accessory or instrument to Varian or to send it to a
designated service facility. The Customer shall be
responsible for loss or damage in transit and shall
prepay shipping cost. Varian will return the accessory
or instrument to the Customer prepaid and insured.
Claims for loss or damage in transit shall be filed by
the Customer. To correct software operation
anomalies, Varian will issue software revisions where
such revisions exist and where, in Varian's opinion,
this is the most efficient remedy.
Limitation of Warranty
This warranty does not cover software supplied by
the Customer, equipment and software warranted by
another manufacturer or replacement of expendable
items and those of limited life, such as but not limited
to: Filters, glassware, instrument status lamps, source
lamps, septa, columns, fuses, chart paper and ink,
nebulizers, flow cells, pistons, seals, fittings, valves,
burners, sample tubes, probe inserts, print heads,
glass lined tubing, pipe and tube fittings, variable
temperature dewars, transfer lines, flexible discs,
magnetic tape cassettes, electron multipliers,
filaments, vacuum gaskets, seats and all parts
exposed to samples and mobile phases.
This warranty shall be void in the event of accident,
abuse, alteration, misuse, neglect, breakage,
improper operation or maintenance, unauthorized or
improper modifications or tampering, use in an
unsuitable physical environment, use with a marginal
power supply or use with other inadequate facilities or
utilities. Reasonable care must be used to avoid
hazards.
This warranty is expressly in lieu of and excludes
all other express or implied warranties, including
but not limited to warranties of merchantability
and of fitness for particular purpose, use or
application, and all other obligations or liabilities
on the part of Varian, unless such other
warranties, obligations or liabilities are expressly
agreed to in writing by Varian.
Limitation of Remedies and Liability
The remedies provided herein are the sole and
exclusive remedies of the Customer. In no case
will Varian be liable for incidental or
consequential damages, loss of use, loss of
production or any other loss incurred.
03-914603-00:10 1 of 4
Safety
Information
Operating Instructions
This instruction manual is provided to help you establish operating conditions which will permit safe and efficient use
of your equipment. Special considerations and precautions are also described in the manual, which appear in the form
of
NOTES, CAUTIONS, and WARNINGS as described below. It is important that you operate your equipment in
accordance with this instruction manual and any additional information which may be provided by Varian. Address
any questions regarding the safe and proper use of your equipment to your local Varian office.
NOTE
Information to aid you in obtaining
optimal performance from your
instrument.
Alerts you to situations that may
cause moderate injury and/or
equipment damage, and how to
avoid these situations.
Alerts you to potentially hazardous
situations that could result in
serious injury, and how to avoid
these situations.
Warning Symbol Warning Description
Hazardous voltages are present inside instrument. Disconnect from
main power before removing screw-attached panels.
Hazardous chemicals may be present. Avoid contact, especially
when replenishing reservoirs. Use proper eye and skin protection.
Very hot or cryogenically cold surfaces may be exposed. Use proper
skin protection.
Eye damage could occur either from flying particles, chemicals, or
UV radiation. Use proper eye and face protection.
The potential for fire may be present. Follow manual instructions for
safe operation.
The potential for explosion may exist because of type of gas or
liquid used.
Ionizing radiation source is present. Follow manual instructions for
safe operation.
Keep hands and fingers away.
2 of 4 03-914603-00:10
General Safety Precautions
Follow these safety practices to ensure safe equipment operation.
Perform periodic leak checks on all supply lines and pneumatic plumbing.
Do not allow gas lines to become kinked or punctured. Place lines away from foot traffic
and extreme heat or cold.
Store organic solvents in fireproof, vented and clearly labeled cabinets so they are easily
identified as toxic and/or flammable materials.
Do not accumulate waste solvents. Dispose of such materials through a regulated disposal
program and not through municipal sewage lines.
NOTICE:
This instrument has been tested per applicable requirements of EMC Directive as required to
carry the European Union CE Mark. As such, this equipment may be susceptible to
radiation/interference levels or frequencies which are not within the tested limits.
This instrument is designed for chromatographic analysis of appropriately prepared samples. It
must be operated using appropriate gases and/or solvents and within specified maximum
ranges for pressure, flows, and temperatures as described in this manual. If the equipment is
used in a manner not specified by the manufacturer, the protection provided by the equipment
may be impaired.
It is the responsibility of the Customer to inform Varian Customer Support Representatives if
the instrument has been used for the analysis of hazardous biological, radioactive, or toxic
samples, prior to any instrument service being performed or when an instrument is being
returned to the Service Center for repair.
Electrical Hazards
Disconnect the instrument from all power sources before removing protective panels to avoid
exposure to potentially dangerous voltages.
When it is necessary to use a non-original power cord plug, make sure the replacement cord adheres
to the color coding and polarity described in the manual and all local building safety codes.
Replace blown fuses with fuses of the size and rating stipulated on the fuse panel or in the manual.
Replace faulty or frayed power cords immediately with the same type and rating.
Make sure that voltage sources and line voltage match the value for which the instrument is wired.
Compressed Gas Cylinders
Store and handle compressed gases carefully and in strict adherence to safety codes.
Secure cylinders to an immovable structure or wall.
Store and move cylinders in an upright, vertical position. Before transport, remove regulators
and install cylinder cap.
Store cylinders in a well-ventilated area away from heat, direct sunshine, freezing
temperatures, and ignition sources.
Mark cylinders clearly so there is no doubt as to their contents.
Use only approved regulators and connections.
Use only connector tubing that is chromatographically clean (Varian Part Number 03-918326-00)
and has a pressure rating significantly greater than the highest outlet pressure from the regulator.
03-914603-00:10 3 of 4
GC Safety Practices
Exhaust System
No special exhaust ducting is necessary for GC
detectors installed in a well-ventilated room except
when the detectors are used to test hazardous
chemicals. If you do install ducting:
Use only fireproof ducting.
Install a blower at the duct outlet.
Locate duct intakes such that their vibration or air
movement does not effect detector operation.
Check periodically for proper operation of the duct.
Ensure proper ventilation in lab area.
Radioactive Source Detectors
Read carefully and comply with all NOTES,
CAUTIONS, and WARNINGS in the Ni
63
ECD
manual.
Perform the tests for removable radioactive
contamination described in the Ni
63
ECD manual.
Comply with leak test schedules and procedures.
Burn Hazard
Heated or cryogenically cooled zones of gas
chromatographs can remain hot or cold for a
considerable time after instrument power is turned off.
To prevent painful burns, ensure that all heated or
cooled areas have returned to room temperature or wear
adequate hand protection before you touch potentially
hot or cold surfaces.
LC Safety Practices
High Pressure Hazard
If a line ruptures, a relief device opens, or a
valve opens accidentally under pressure,
potentially hazardous high liquid pressures can
be generated by the pump causing a high
velocity stream of volatile and/or toxic liquids.
Wear face protection when you inject samples or
perform routine maintenance.
Never open a solvent line or valve under pressure.
Stop the pump first and let the pressure drop to
zero.
Use shatter-proof reservoirs capable of operating at
50-60 psi.
Keep the reservoir enclosure closed when the
reservoir is under pressure.
Read and adhere to all NOTES, CAUTIONS, and
WARNINGS in the manual.
Flash Chromatography
The operator should be familiar with the physico-
chemical properties of the components of the mobile
phase.
Keep solvents from direct contact with the
polyurethane supply tubing as certain solvents will
cause weakening and leaks with possible bursting.
All components of the system should be connected to a
common power supply and common ground. This
ground must be a true ground rather than a floating
ground.
Non-polar solvents can develop a static charge when
pumped through the system. All vessels that contain
mobile phase (including tubing and collection vessels)
must be grounded to dissipate static electricity.
Employ static measuring and static discharge devices
(e.g., air ionizers) to safeguard against the buildup of
static electricity.
Ultraviolet Radiation
Liquid chromatograph detectors that use an ultraviolet
light source have shielding to prevent radiation
exposure to personnel.
For continued protection:
Ensure that protective lamp covers of variable and
fixed wavelength detectors are in place during
operation.
Do not look directly into detector fluid cells or at
the UV light source. When inspecting the light
source or fluid cell, always use protective eye
covering such as borosilicate glass or polystyrene.
The following is a Federal Communications
Commission advisory: This equipment has been
tested and found to comply with the limits of a Class A
computing device, pursuant to part 15 of the FCC
Rules. These limits are designed to provide reasonable
protection against harmful interference when the
equipment is operated in a commercial environment.
This equipment generates, uses, and can radiate radio
frequency energy and, if not installed and used in
accordance with the instruction manual, may cause
harmful interference to radio communications.
Operation of this equipment in a residential area is
likely to cause harmful interference in which case the
user will be required to correct the interference at his
own expense.
4 of 4 03-914603-00:10
Spare Parts Availability
It is the policy of Varian to provide operational spare parts for any
instrument and major accessory for a period of five (5) years after
shipment of the final production run of that instrument. Spare parts will
be available after this five (5) year period but on an as available basis.
Operational spare parts are defined as those individual electrical or
mechanical parts that are susceptible to failure during their normal
operation. Examples include relays, lamps, temperature probes, detector
elements, motors, etc. Sheet metal parts, structural members or
assemblies and castings, printed circuit boards, and functional modules
are normally capable of being rebuilt to like-new condition throughout
their useful life and therefore will be supplied only on an as available
basis after the final production run of the instrument.
Service Availability
Varian provides a variety of services
to support its customers after
warranty expiration. Repair service
can be provided by attractively priced
service contracts or on a time and
material basis. Technical support and
training can be provided by qualified
personnel on both a contractual or as-
needed basis.
Varian, Inc. Analytical Instruments Sales Offices
For Sales or Service assistance and to order Parts and Supplies, contact your local Varian office.
Argentina
Buenos Aires
Tel. +54.11.4.783.5306
Australia
Mulgrave, Victoria
Tel. +61.3.9566.1134
Austria
Vösendorf bei Wien
Tel. +43.1.699.9669
Benelux
Bergen Op Zoom
Tel. +31.164.282.800
Brazil and Latin America (S)
São Paulo
Tel. +55.11.820.0444
Canada
Mississauga, Ontario
Tel. 800.387.2216
China
Beijing
Tel. +86.106209.1727
Europe
Middelburg, The Netherlands
Tel. +31.118.671.000
France
Les Ulis Cédex
Tel. +33.1.6986.3838
Germany
Darmstadt
Tel. +49.6151.7030
India
Mumbai
Tel. +91.22.857.0787/88/89
Italy
Torino
Tel. +39.011.997.9111
Japan
Tokyo
Tel. +81.3.5232.1211
Korea
Seoul
Tel. +82.2.345.22452
Mexico and Latin America (N)
Mexico City
Tel. +52.5.523.9465
Russian Federation
Moscow
Tel. +7.095.937.4280
Spain
Madrid
Tel. +34.91.472.7612
Sweden
Solna
Tel. +46.8.445.1620
Switzerland
Varian AG
Tel. +41.848.803.800
Taiwan
Taipei Hsien
Tel. +886.2.698.9555
United Kingdom and
Ireland
Walton-on-Thames
Tel. +44.1932.898000
Venezuela
Valencia
Tel. +58.41.257.608
United States
Walnut Creek, California, USA
Tel. +1.800.926.3000
(GC and GC/MS)
Tel. +1.800.367.4752
(LC)
www.varianinc.com
03-914603-81:10 1 of 4
Sicherheitsinformationen
Arbeitsanleitungen
Diese Arbeitsanleitung will Ihnen bei der Aufstellung solcher Arbeitsbedingungen helfen, die einen sicheren und
wirkungsvollen Gebrauch Ihrer Geräte ermöglichen. Besondere Überlegungen und Vorsichtsmaßnahmen erscheinen
in diesem Handbuch in Form von
HINWEIS, ACHTUNG und WARNUNG, wie unten beschrieben. Es ist wichtig, daß
Sie Ihr Gerät in Übereinstimmung mit dieser Arbeitsanleitung und allen möglichen zusätzlichen Informationen von
Varian betreiben. Alle Fragen bezüglich Sicherheit und Handhabung Ihres Gerätes richten Sie an Ihr Varian Büro.
HINWEIS
ACHTUN
G
WARNUN
G
Eine Information, um einen optimalen
Wirkungsgrad Ihres Instruments zu
erzielen.
Weist auf Situationen, die zu mäßiger
Beeinträchtigung und/oder zu
Geräteschäden führen und auf die
Vermeidung dieser Situationen hin.
Weist auf mögliche Gefahrensituationen,
die zu ernsthaften Verletzungen führen
können und auf die Vermeidung dieser
Situationen hin.
Warnungssymbol Warnungsbeschreibung
WARNUNG
ELEKTRISCHER
SCHL
A
G
Gefährliche Spannungen bestehen innerhalb des Instruments. Trennen Sie das
Gerät vom Netz, bevor Sie abschraubbare Paneele entfernen.
Gefährliche Chemikalien können vorhanden sein. Vermeiden Sie jeden Kon-
takt, besonders beim Auffüllen der Reservoirs. Benutzen Sie wirksamen
Augen und Hautschutz.
WARNUNG
VERBRENNUNGSGEFAHR
Sehr heiße oder tiefstgekühlte Oberflächen können freigelegt sein. Benutzen
Sie einen wirksamen Hautschutz.
Herumfliegende Partikel, Chemikalien oder UV-Strahlung können
Augenschäden verursachen. Tragen Sie deshalb einen geeigneten Schutz für
Augen und Gesicht.
WARNUNG
FEUERGEFAHR
Es besteht eine mögliche Feuergefahr. Beachten Sie die Vorschriften im
Handbuch für eine gefahrlose Benutzung.
WARNUNG
EXPLOSIONSGEFAH
R
Eine mögliche Explosionsgefahr besteht infolge der benutzten Gas- oder
Flüssigkeitsart.
WARNUNG
STRAHLUNGSQUELLE
Es besteht eine ionisierende Strahlungsquelle. Beachten Sie die Vorschriften
im Handbuch für eine gefahrlose Benutzung.
WARNUNG
BEWEGTE TEIL
E
Bleiben Sie mit Ihren Händen und Fingern weg.
2 of 4 03-914603-81:10
Allgemeine Sicherheitsmaßnahmen
Befolgen Sie diese Sicherheitspraktiken für eine gefahrlose Gerätebenutzung.
Prüfen Sie regelmäßig alle Versorgungs und Pneumatikleitungen auf Lecks.
Gasleitungen dürfen nicht geknickt oder angestochen werden. Verlegen Sie die Leitungen außer-
halb von Laufwegen und abseits von extremer Hitze oder Kälte.
Lagern Sie organische Lösungsmittel in feuerfesten, belüfteten und eindeutig bezeichneten
Schränken, damit sie leicht als toxische und/oder brennbare Materialien erkannt werden.
Sammeln Sie keine Lösungsmittelabfälle. Entsorgen Sie solche Materialien über ein geregeltes Ent-
sorgungsprogramm und nicht über die öffentlichen Abwasserleitungen.
HINWEIS:
Dies Instrument wurde nach den zutreffenden Vorschriften der EMC Direktive getestet, die
zum Führen des CE Zeichens der Europäischen Union berechtigen. Dieses Gerät kann an sich
auf Strahlungs-/Störpegel oder Frequenzen außerhalb der getesteten Grenzen reagieren.
WARNUNG
Dies Instrument ist für chromatographische Analysen entsprechend präparierter Proben ge-
dacht. Es muß mit geeigneten Gasen und/oder Lösungsmitteln und innerhalb der im Handbuch
spezifizierten maximalen Werte für Druck, Flüsse und Temperaturen betrieben werden.
WARNUNG
Der Kunde ist vor der Durchführung irgendeines Geräteservices verpflichtet den Varian
Kundendienstvertreter zu informieren, wenn das Instrument für Analysen gefährlicher
biologischer, radioaktiver oder toxischer Proben benutzt worden ist.
Elektrische Gefahren
Lösen Sie das Instrument von allen Stromquellen, bevor Sie Schutzpaneele entfernen, damit Sie nicht mit
potentiell gefährlichen Spannungen in Berührung kommen.
Wenn ein Nicht-Original Netzkabelstecker benutzt werden muß, muß das Austauschkabel die im Handbuch
beschriebene Farbcodierung und Polarität beibehalten und alle örtlichen Sicherheitsvorschriften erfüllen.
Ersetzen Sie durchgebrannte Sicherungen nur mit Sicherungen der Werte, die am Sicherungspaneel oder im
Handbuch angegeben sind.
Ersetzen Sie fehlerhafte oder durchgescheuerte Netzkabel sofort durch Kabel gleicher Art.
Sorgen Sie dafür, daß Spannungsquellen und die Netzspannung den gleichen Wert haben, für den das In-
strument verdrahtet ist.
Gasdruckflaschen
Lagern und handhaben Sie komprimierte Gase vorsichtig und in strikter Einhaltung der
Sicherheitsvorschriften.
Befestigen Sie die Gasflaschen an feststehenden Aufbauten oder an Wänden.
Lagern und transportieren Sie Gasflaschen in aufrechter Stellung. Druckregler zuvor abnehmen.
Lagern Sie Gasflaschen in gut durchlüfteten Räumen, weit genug weg von Heizungen, direktem
Sonnenschein, Frosttemperaturen und Entzündungszonen.
Kennzeichnen Sie die Flaschen so eindeutig, daß kein Zweifel über deren Inhalt bestehen kann.
Benutzen Sie nur geprüfte Druckminderer und Verbindungsstücke.
Benutzen Sie nur chromatographisch reines Verbindungsrohr (Varian Part Number 03-918326-00), das
wesentlich höheren Druck als den höchsten Ausgangsdruck des Druckminderers aushält.
03-914603-81:10 3 of 4
GC Sicherheitspraktiken
Abgassystem
Für GC Detektoren, die in einem gut durchlüfteten
Raum installiert sind, ist keine spezielle Abgasführung
erforderlich, außer wenn die Detektoren zum Testen
gefährlicher Chemikalien benutzt werden. Wenn Sie
eine Abgasführung installieren:
Benutzen Sie nur feuerfeste Führungen.
Installieren Sie ein Gebläse am Ausgang.
Ordnen Sie die Ansaugöffnung so an, daß ihre Er-
schütterungen oder Luftströmungen nicht die De-
tektorfunktion beeinträchtigen.
Prüfen Sie regelmäßig die einwandfreie Arbeits-
weise der Abgasführung.
Sorgen Sie für gute Entlüftung im Laborbereich.
Radioaktive Detektoren
Lesen Sie sorgfältig und befolgen Sie alle
HINWEISE, ACHTUNGEN und WARNUNGEN im
Ni
63
ECD Handbuch.
Führen Sie die Tests für zu beseitigende radioak-
tive Kontamination durch, die im Ni
63
ECD Hand-
buch beschrieben sind.
Erfüllen Sie die Zeitpläne und Verfahren zur Di-
chtigkeitsprüfung.
Verbrennungsgefahr
Beheizte oder tieftemperaturgekühlte Zonen des Gas-
chromatographen können beträchtlich lange heiß oder
kalt bleiben, nachdem das Instrument bereits ab-
geschaltet ist. Zur Vermeidung schmerzhafter Verbren-
nungen müssen Sie darauf achten, daß alle beheizten
oder gekühlten Zonen auf Raumtemperatur zurück-
gegangen sind oder Sie müssen ausreichenden Hand-
schutz benutzen, bevor Sie möglicherweise heiße oder
kalte Oberflächen berühren.
LC Sicherheitspraktiken
Gefahr durch hohen Druck
Wenn eine Leitung bricht, eine Entlüftungseinheit sich
öffnet oder ein Ventil sich unbeabsichtigt unter Druck
öffnet, kann durch die Pumpe möglicherweise ein ge-
fährlich hoher Flüssigkeitsdruck entstehen, der einen
Strahl flüchtiger und/oder toxischer Flüssigkeiten von
hoher Stömungsgeschwindigkeit verursacht.
Tragen Sie einen Gesichtsschutz, wenn Sie Proben
injizieren oder Routinewartungen durchführen.
Öffnen Sie niemals eine unter Druck stehende
Lösungsmittelleitung oder ein Ventil. Halten Sie
zuerst die Pumpe an und lassen Sie den Druck auf
Null abfallen.
Benutzen Sie splittersichere Reservoirs, die für
einen Druck von 3,4 bis 4,1 bar ausgelegt sind.
Halten Sie die Reservoirverkleidung geschlossen,
wenn die Reservoirs unter Druck stehen.
Lesen Sie und befolgen Sie alle HINWEISE,
ACHTUNGEN und WARNUNGEN im Handbuch.
Blitzlicht-Chromatographie
Der Bediener sollte mit den physikalisch-chemischen
Eigenschaften der Komponenten vertraut sein, aus
denen sich die mobile Phase zusammensetzt.
Vermeiden Sie direkten Kontakt der Lösungsmittel mit
den Zuführungsleitungen aus Polyurethan, da einige
Lösungsmittel das Material der Leitungen schwächen
und damit Undichtigkeiten oder Brüche hervorrufen
können.
Alle Systemkomponenten sollten an der gleichen
Netzstromquelle und einer gemeinsamen Erdung
angeschlossen sein. Dabei muss es sich um eine echte,
nicht um eine schwebende Erdung handeln.
Nicht-polare Lösungsmittel können sich beim Pumpen
durch das System statisch aufladen. Alle Gefäße, die
mobile Phase enthalten (einschließlich Leitungen und
Sammelgefäße), müssen zur Ableitung elektro-
statischer Aufladungen geerdet sein.
Setzen Sie Geräte zur Messung und Ableitung
elektrostatischer Aufladungen (z.B. Geräte zur
Luftionisierung) als Maßnahmen gegen den Aufbau
statischer Elektrizität ein.
Ultraviolette Strahlung
Detektoren in Liquidchromatographen, die eine
ultraviolette Lichtquelle benutzen, besitzen eine
Abschirmung, die das Bedienungspersonal gegen
Abstrahlungen schützt. Zum ständigen Schutz:
Achten Sie darauf, daß die schützende Lampenab-
deckung der Detektoren mit variablen und festen
Wellenlängen während des Betriebs an ihrem Platz
ist.
Schauen Sie nicht direkt in die Flüssigkeitszellen
im Detektor oder in die UV Lampe. Zum In-
spizieren der Lichtquelle oder der Flüssigkeitszelle
benutzen Sie immer einen wirksamen Augenschutz,
wie er durch Borsilikatglas oder Polystyrol gewähr-
leistet wird.
4 of 4 03-914603-81:10
Verfügbarkeit von Ersatzteilen
Es ist Varian’s Grundsatz, Ersatzteile für alle Instrumente und die wichtig-
sten Zubehöre für einen Zeitraum von fünf (5) Jahren nach dem Fertigung-
sauslauf dieser Geräteserie verfügbar zu haben. Nach diesem Zeitraum von
fünf (5) Jahren können Ersatzteile auf der Basis solange vorhanden be-
zogen werden. Als Ersatzteil werden hier solche elektrischen und mecha-
nischen Einzelteile verstanden, die unter normalen Bedingungen ausfallen
können. Beispiele sind Relais, Lampen, Temperaturfühler, Detektorele-
mente, Motore usw. Metallbleche, Formteile oder Baugruppen und
Gußteile, PC Boards und Funktionsmodule können normalerweise neu-
wertähnlich für eine brauchbare Lebensdauer instandgesetzt werden und
werden deshalb nur auf der Basis solange vorhanden nach dem Produk-
tionsauslauf des Instruments geliefert werden.
Serviceverfügbarkeit
Varian bietet seinen Kunden auch
nach dem Auslaufen der Garantie
eine Vielfalt von Serviceleistungen
an. Reparaturservice kann zu attrak-
tiven Preisen über eine Wartungs-
vereinbarung oder nach Zeit- und
Materialaufwand zur Verfügung
gestellt werden. Technische Unter-
stützung und Training bieten wir
Ihnen durch qualifizierte Chemiker
sowohl auf einer Kontraktbasis als
auch nach Ihren Erfordernissen an.
Varian Analytical Instruments Verkaufsbüros
Für Verkaufs oder Servicehilfe und zum Bestellen von Teilen und Zubehören setzen Sie sich bitte mit Ihrem
Varian Büro in Verbindung.
Argentina
Buenos Aires
Tel. +54.11.4.783.5306
Australia
Mulgrave, Victoria
Tel. +61.3.9566.1134
Austria
Vösendorf bei Wien
Tel. +43.1.699.9669
Benelux
Bergen Op Zoom
Tel. +31.164.282.800
Brazil and Latin America (S)
São Paulo
Tel. +55.11.820.0444
Canada
Mississauga, Ontario
Tel. 800.387.2216
China
Beijing
Tel. +86.106209.1727
Europe
Middelburg, The Netherlands
Tel. +31.118.671.000
France
Les Ulis Cédex
Tel. +33.1.6986.3838
Germany
Darmstadt
Tel. +49.6151.7030
India
Mumbai
Tel. +91.22.857.0787/88/89
Italy
Torino
Tel. +39.011.997.9111
Japan
Tokyo
Tel. +81.3.5232.1211
Korea
Seoul
Tel. +82.2.345.22452
Mexico and Latin America (N)
Mexico City
Tel. +52.5.523.9465
Russian Federation
Moscow
Tel. +7.095.937.4280
Spain
Madrid
Tel. +34.91.472.7612
Sweden
Solna
Tel. +46.8.445.1620
Switzerland
Varian AG
Tel. +41.848.803.800
Taiwan
Taipei Hsien
Tel. +886.2.698.9555
United Kingdom and
Ireland
Walton-on-Thames
Tel. +44.1932.898000
Venezuela
Valencia
Tel. +58.41.257.608
United States
Walnut Creek, California, USA
Tel. +1.800.926.3000
(GC and GC/MS)
Tel. +1.800.367.4752
(LC)
www.varianinc.com
03-914603-82:10 1 of 4
Informations et mesures de sécurité
Instructions de fonctionnement
Ce manuel d’instruction est conçu pour aider l’utilisateur à créer des conditions opératoires lui permettant de faire
fonctionner le matériel efficacement et en toute sécurité. Il contient entre autres certaines observations spéciales
présentées sous forme de
NOTES, MISES EN GARDE et AVERTISSEMENTS. Il est important de faire fonctionner ce
matériel conformément aux instructions du présent manuel et à toute autre information émanant de Varian. S’adresser
au bureau régional Varian pour toute question relative à la sécurité ou à l’utilisation correcte du matériel.
NOTE
Information destinée à tirer le
meilleur parti du matériel sur le plan
des performances
Attire l’attention sur une situation
pouvant occasionner des dommages
corporels légers et/ou des dégâts
mineurs à l’appareil et indique
comment remédier à cette situation
Attire l’attention sur une situation
potentiellement dangereuse pouvant
occasionner des dommages corporels
importants et indique comment
remédier à cette situation
Symboles d’avertissement Description
A
TTENTION
RISQUE
D'ELECTROCUTION
Exposition à des tensions dangereuses. Débrancher le matériel du secteur avant de
dévisser les panneaux protecteurs.
Présence éventuelle de substances chimiques dangereuses. Eviter tout contact, en
particulier lors du remplissage des réservoirs. Prendre les mesures de protection
adéquates pour les yeux et la peau.
ATTENTION
RISQUE DE BRÛLURE
S
Exposition à des surfaces chaudes ou traitées cryogéniquement. Prendre les
mesures de protection adéquates pour la peau.
Les dommages causées aux yeux sont de deux natures différentes : jet de
particules et de produits chimiques ou radiations UV. Utiliser des protections du
visage et des yeux appropriées.
ATTENTION
RISQUE D'INCENDI
E
Risque potentiel d’incendie. Se conformer aux instructions du manuel pour faire
fonctionner le matériel en toute sécurité.
ATTENTION
RISQUE D'EXPLOSION
Risque potentiel d’explosion en raison du type de gaz ou de liquide utilisé.
ATTENTION
SOURCE DE RADIATION
Présence d’une source de radiation ionisante. Se conformer aux instructions du
manuel pour faire fonctionner le matériel en toute sécurité.
ATTENTION
PIECES EN MOUVEMENT
Garder les mains et les doigts hors de portée.
2 of 4 03-914603-82:10
Précautions générales en matière de sécurité
Les pratiques suivantes garantissent une utilisation sans risques du matériel:
Effectuer régulièrement des essais d’étanchéité de tous les conduits d’alimentation et de tous les tuyaux du
système pneumatique.
Ne pas travailler avec des conduits de gaz déformés ou percés. Installer les conduits de gaz à l’écart des allées
et venues et à l’abri du chaud ou du froid.
Conserver les solvants organiques dans des récipients à l’épreuve du feu, bien ventilés et portant mention de la
nature de leur contenu, en particulier lorsque lesdits solvants sont toxiques et/ou inflammables.
Ne pas accumuler les solvants de rebut. Les éliminer conformément à un programme agréé d’élimination des
déchets et non via les égouts municipaux.
NOTE:
Ce matériel a été testé conformément aux dispositions de la directive CME afin de
pouvoir porter le sigle CE de l’Union européenne. Il en résulte qu’il peut être sensible à
des niveaux de radiation/d’interférence ou à des fréquences se situant hors des limites
testées.
ATTENTIO
N
Ce matériel est conçu pour effectuer des analyses chromatographiques d’échantillons
préparés selon des méthodes appropriées. Il convient de le faire fonctionner avec les gaz
et/ou les solvants adéquats et dans les limites des pressions, des débits et des températures
maximales spécifiées dans le présent manuel.
ATTENTIO
N
Le client est tenu d’informer le service Varian d’assistance à la clientèle que son matériel
a été utilisé pour l’analyse d’échantillons biologiques dangereux, radioactifs ou toxiques
avant que n’en soit effectué la maintenance.
Risques de chocs électriques
Déconnecter le matériel de toute source d’alimentation avant d’en démonter les panneaux de protection, sous
peine de s’exposer à des tensions dangereuses.
En cas d’utilisation d’un cordon d’alimentation n’étant pas d’origine, s’assurer que celui-ci soit conforme à la
polarité et au codage des couleurs décrits dans le manuel d’utilisation ainsi qu’à toutes les normes régionales
de sécurité régissant le secteur de la construction.
Remplacer les fusibles sautés par des fusibles de même type que ceux stipulés sur le panneau des fusibles ou
dans le manuel d’utilisation.
Remplacer les cordons d’alimentation défectueux ou dénudés par des cordons d’alimentation de même type.
S’assurer que les sources de tension et la tension de secteur correspondent à la tension de fonctionnement du
matériel.
Bouteilles à gaz comprimé
Ranger et manipuler les bouteilles à gaz comprimé avec précaution et conformément aux normes de sécurité.
Fixer les bouteilles à gaz comprimé à un mur ou à une structure inamovible.
Ranger et déplacer les bouteilles à gaz comprimé en position verticale. Avant de transporter les bouteilles à
gaz comprimé, retirer leur régulateur.
Ranger les bouteilles dans un endroit bien ventilé et à l’abri de la chaleur, des rayons directs du soleil, du gel
ou des sources d’allumage.
Marquer les bouteilles de manière à n’avoir aucun doute quant à leur contenu.
N’utiliser que des connexions et régulateurs agréés.
N’utiliser que des tuyaux de raccordement propres sur le plan chromatographique (Varian P/N 03-918326-00) et
pouvant supporter des pressions sensiblement plus élevées que la plus haute pression de sortie du régulateur.
03-914603-82:10 3 of 4
Mesures de sécurité en CPG
Système d’échappement
Les détecteurs CPG installés dans une pièce bien
ventilée ne nécessitent pas de conduits spéciaux
d’échappement excepté lorsqu’ils sont destinés à
analyser des substances chimiques dangereuses. Lors
de l’installation de tels conduits:
N’utiliser que des conduits à l’épreuve du feu
Installer un ventilateur à la sortie du conduit.
Placer les orifices d’aspiration de manière à ce que
les vibrations ou les mouvements d’air n’affectent
pas le fonctionnement du détecteur.
Vérifier périodiquement l’état du conduit.
S’assurer que le laboratoire est correctement
ventilé.
Détecteurs à source radioactive
Se conformer au manuel d’utilisation de l’ECD
Ni
63
, en particulier à ses NOTES, MISES EN
GARDE ET AVERTISSEMENTS.
Effectuer les tests de décontamination radioactive
décrits dans le manuel d’utilisation de l’ECD Ni
63
.
Se conformer aux procédures et au calendrier des
essais d’étanchéité.
Risque de brûlures
Les zones des chromatographes à gaz chauffées ou
traitées cryogéniquement peuvent rester très chaudes ou
très froides durant une période plus ou moins longue
après la mise hors tension du matériel. Pour éviter les
brûlures, s’assurer que ces zones sont revenues à
température ambiante ou utiliser un dispositif adéquat
de protection des mains avant de les toucher.
Mesures de sécurité en CPL
Risques liés aux hautes pressions
En cas de rupture d’un tuyau ou en cas d’ouverture
accidentelle d’une vanne alors que le système est sous
pression, la pompe peut occasionner des dommages en
expulsant à grande vitesse des jets de liquides volatiles
et/ou toxiques.
Mettre un masque de protection lors de l’injection
des échantillons ou en effectuant les opérations de
maintenance de routine.
Ne jamais déconnecter un conduit de solvant ou
une vanne sous pression. Arrêter préalablement la
pompe et laisser la pression descendre à zéro.
Utiliser des réservoirs incassables à 50-60 psi.
Laisser l’enceinte du réservoir fermée lorsque le
réservoir est sous pression.
Se conformer aux NOTES, MISES EN GARDE ET
AVERTISSEMENTS du manuel d’utilisation.
Chromatographie Flash
L’utilisateur aura la connaissance des propriétés
physico-chimiques des constituants de la phase mobile.
Eviter le contact direct des solvants avec les tuyaux en
polyuréthane : certains solvants sont susceptibles de
provoquer des faiblesses et des fuites avec risques
d’explosion.
Tous les constituants du système devront être connectés
à une source de courant commune et à une prise de
terre commune. Cette prise de terre devra être fixe et
non mobile.
Les solvants non-polaires peuvent produire de
l’électricité statique lorsqu’ils passent au travers du
système. Les bouteilles qui contiennent la phase mobile
(incluant les tuyaux et les flacons de collecte de
fractions) doivent être mises à la terre pour éliminer
l’électricité statique.
Utiliser des appareils de mesure et de décharge
d’électricité statique (par exemple des ionisateurs d’air)
pour combattre la formation d’électricité statique.
Radiations ultraviolettes
Les détecteurs CPL utilisant une source lumineuse
ultraviolette comportent un écran destiné à se prémunir
contre les expositions aux rayonnements.
Pour s’assurer une protection permanente:
Vérifier que le couvercle de protection de la lampe
des détecteurs opérant à des longueurs d’onde
variables et fixes soit bien en place durant le
fonctionnement du matériel.
Ne pas regarder directement les cellules du
détecteur ou la source d’UV. Se protéger
systématiquement les yeux lors du contrôle de la
source lumineuse ou des cellules, par exemple au
moyen de verres borosilicatés ou en polystyrène.
4 of 4 03-914603-82:10
Disponibilité des pièces de rechange
La politique de Varian consiste à fournir des pièces de rechange pour
tous les appareils et accessoires majeurs durant une période de cinq (5)
ans après livraison de leur production finale. Les pièces de rechange ne
sont fournies au terme de cette période de cinq (5) ans que suivant les
disponibilités. Il faut entendre par pièces de rechange les pièces
individuelles électriques ou mécaniques susceptibles de défaillance au
cours de leur utilisation normale. Par exemple, les relais, les lampes, les
sondes thermiques, les éléments de détecteur, les moteurs, etc. Les
parties en tôles, les éléments ou assemblages structurels et les pièces de
fonderie, les cartes à circuits imprimés et les modules fonctionnels sont
normalement susceptibles d’être remis à l’état neuf pendant toute la
durée de leur vie utile et ne sont dès lors fournies, au terme de la
production finale des appareils, que suivant les disponibilités.
Service d’assistance à
la clientèle
Varian fournit divers services
destinés à aider sa clientèle après
expiration de la garantie: service de
réparation sur base de contrats de
maintenance à prix attractifs ou sur
base d’accords à durée limitée
portant sur du matériel spécifique;
support technique et service de
formation assurés par des chimistes
qualifiés sur base contractuelle ou
en fonction des besoins spécifiques.
Points de vente des instruments analytiques Varian
Contactez votre point de vente régional Varian pour toute question commerciale ou de service d’assistance à
la clientèle ou pour passer commande de pièces et de fournitures.
Argentina
Buenos Aires
Tel. +54.11.4.783.5306
Australia
Mulgrave, Victoria
Tel. +61.3.9566.1134
Austria
Vösendorf bei Wien
Tel. +43.1.699.9669
Benelux
Bergen Op Zoom
Tel. +31.164.282.800
Brazil and Latin America (S)
São Paulo
Tel. +55.11.820.0444
Canada
Mississauga, Ontario
Tel. 800.387.2216
China
Beijing
Tel. +86.106209.1727
Europe
Middelburg, The Netherlands
Tel. +31.118.671.000
France
Les Ulis Cédex
Tel. +33.1.6986.3838
Germany
Darmstadt
Tel. +49.6151.7030
India
Mumbai
Tel. +91.22.857.0787/88/89
Italy
Torino
Tel. +39.011.997.9111
Japan
Tokyo
Tel. +81.3.5232.1211
Korea
Seoul
Tel. +82.2.345.22452
Mexico and Latin America (N)
Mexico City
Tel. +52.5.523.9465
Russian Federation
Moscow
Tel. +7.095.937.4280
Spain
Madrid
Tel. +34.91.472.7612
Sweden
Solna
Tel. +46.8.445.1620
Switzerland
Varian AG
Tel. +41.848.803.800
Taiwan
Taipei Hsien
Tel. +886.2.698.9555
United Kingdom and
Ireland
Walton-on-Thames
Tel. +44.1932.898000
Venezuela
Valencia
Tel. +58.41.257.608
United States
Walnut Creek, California, USA
Tel. +1.800.926.3000
(GC and GC/MS)
Tel. +1.800.367.4752
(LC)
www.varianinc.com
03-914603-83:10 1 of 4
Informazioni sulla Sicurezza
Instruzioni per l’Uso
Questo manuale ha lo scopo di aiutare l’operatore ad utilizzare lo strumento in modo sicuro ed efficiente. Le
considerazioni e le precauzioni speciali vengono presentate in questo manuale sotto forma di avvisi di
NOTA,
CAUTELA e ATTENZIONE. E’ importante che lo strumento venga utilizzato rispettando le istruzioni fornite in questo
manuale o che verranno fornite successivamente dalla Varian. Per ogni eventuale chiarimento sull’uso o sulla
sicurezza, si prega di contattare la Varian di Leinì (TO).
NOTA
Sono informazioni utili ad ottenere
le prestazioni migliori da parte
dello strumento.
ATTENZION
Allerta l’operatore su situazioni che
potrebbero causare ferite leggere e
danni limitati allo strumento ed il
modo di evitarle.
ATTENZION
Allerta l’operatore su situazioni
potenzialmente pericolose che
possono causare danni molto seri ed
il modo di evitarle.
Segnali di ATTENZIONE Descrizione del Pericolo
ATTENZIONE
Pericolo di folgorazion
i
Nello strumento sono presenti tensioni pericolose. Scollegare il cavo
di alimentazione prima di togliere il pannello fissato con le viti.
Possono essere presenti composti chimici pericolosi. Evitare il
contatto, specialmente quando si riempiono i contenitori. Usare
protezioni opportune per la pelle e per gli occhi.
ATTENZIONE
Pericolo di scottature
Pericolo di esposizione a superfici molto calde o raffreddate
criogenicamente. Usare protezioni opportune per la pelle.
Particelle volanti, agenti chimici o radiazioni UV possono
danneggiare gli occhi. Vanno quindi utilizzate le opportune
protezioni per gli occhi e per il volto.
ATTENZIONE
Pericolo di incendi
Pericolo potenziale di incendio. Seguire le istruzioni del manuale per
lavorare con una maggiore sicurezza.
ATTENZIONE
Pericolo di esplosioni
C’è pericolo di esplosioni a causa del tipo di gas o liquido utilizzato.
ATTENZIONE
Pericolo di radiazion
i
E’ presente una radiazione ionizzante. Seguire le istruzioni del
manuale per lavorare con una maggiore sicurezza.
Parti in movimento
ATTENZIONE
Non tenere le mani o le dita vicino.
2 of 4 03-914603-83:10
Norme di Sicurezza
Per lavorare in modo sicuro sullo strumento, Vi consigliamo si adottare le seguenti procedure.
Verificare periodicamente che non ci siano perdite sulle linee e sui raccordi pneumatici.
Evitare che le linee dei gas vengano piegate o forate. Le linee vanno posizionate in modo tale
da non essere calpestate e lontane da sorgenti o troppo calde o troppo fredde.
I solventi organici vanno conservati in armadi speciali antiincendio, ventilati e con indicazioni
chiare sul contenuto di materiali tossici e/o infiammabili.
Non accumulare i solventi utilizzati. Adottare un programma regolare di smaltimento, ma mai
nelle acque di scarico.
AVVERTENZA:
Questo strumento è stato testato secondo le Direttive EMC allo scopo di poter utilizzare il
Marchio CE della Comunità Europea. Questo strumento può essere suscettibile a
radiazioni/interferenze o frequenze che non sono entro i limiti collaudati.
ATTENZION
E
Questo strumento è progettato per l’analisi cromatografica di campioni opportunamente
preparati. Deve essere utilizzato usando gas e solventi adatti a questo scopo ed entro i limiti
massimi di pressione, flusso e temperatura riportati in questo manuale. Se lo strumento non
viene utilizzato secondo le modalità specificate dal costruttore, le condizioni di sicurezza
previste potranno non essere sufficienti.
ATTENZION
E
E’ responsabilità del Cliente informare il Servizio Tecnico Varian, prima di qualsiasi
intervento di riparazione, se lo strumento è stato utilizzato per l’analisi di campioni
biologicamente pericolosi, radioattivi o tossici.
Pericoli Elettrici
Prima di togliere i pannelli di protezione, scollegare lo strumento da tutte le alimentazioni
elettriche in modo da evitare l’esposizione a voltaggi potenzialmente pericolosi.
Quando si rende necessario sostituire il cavo di alimentazione, assicurarsi che il nuovo cavo
rispetti sia le codifiche di colore e di polarità riportate nel manuale di istruzioni che quelle
stabilite dalle norme di sicurezza del laboratorio.
Sostituire i fusibili bruciati solo con fusibili che abbiano le stesse caratteristiche; queste ultime sono
riportate sul pannello dei fusibili e/o nel manuale di istruzioni.
Sostituire immediatamente i cavi di alimentazione difettosi o consumati con cavi dello stesso
tipo e con le stesse caratteristiche.
Assicurarsi che il voltaggio del pannello di alimentazione corrisponda a quello dello
strumento da collegare.
Bombole dei Gas
Occorre prestare molta attenzione quando si spostano bombole di gas compressi. Rispettare tutte le
norme di sicurezza.
Assicurare le bombole ad una parete o ad una struttura fissa.
Spostare e conservare le bombole sempre in posizione verticale. Togliere i manometri prima di
spostare le bombole.
Conservare le bombole in un’area ben ventilata, non infiammabile, lontana da sorgenti di calore,
non esposta a temperature troppo fredde o alla luce diretta del sole.
Evidenziare in modo chiaro e che non lasci dubbi il contenuto di ogni bombola.
Usare solo manometri e raccordi di qualità.
Usare solo tubazioni cromatograficamente pulite (Numero di Parte Varian 03-918326-00) e calibrate
per pressioni superiori a quella massima di uscita dal manometro.
03-914603-83:10 3 of 4
Procedure di Sicurezza in GC
Scarico dei Gas
Per i rivelatori GC non è richiesto alcun sistema
particolare di scarico dei gas, se lo strumento è
installato in una stanza ben ventilata e se non viene
utilizzato per l’analisi di sostanze chimiche pericolose.
Se si deve installare un sistema di scarico dei gas:
Usare condutture non infiammabili
Installare un aspiratore in uscita
Posizionare la presa d’aria in modo che le
vibrazioni e il movimento dell’aria non disturbino
il rivelatore.
Eseguire verifiche periodiche per garantire un
funzionamento corretto.
Garantire una buona ventilazione nel laboratorio.
Rivelatori a Sorgente Radioattiva
Leggere e rispettare tutte gli avvisi di NOTA,
CAUTELA e ATTENZIONE riportati nel manuale
del rivelatore ECD al Ni
63
.
Eseguire tutti i test di contaminazione radioattiva
rimovibile descritti nel manuale dell’ECD al Ni
63
.
Rispettare tutte le procedure e le scadenze di
verifica per eventuali perdite.
Pericolo di Scottature
Le zone calde o raffreddate criogenicamente del
gascromatografo possono mantenere la loro
temperatura per parecchio tempo, dopo aver spento lo
strumento. Per evitare scottature, assicurarsi che le
zone riscaldate o raffreddate siano a temperatura
ambiente oppure indossare delle protezioni adeguate
prima di toccare tali superfici.
Procedure di Sicurezza in LC
Pericolo di Alte Pressioni
In caso di rottura di una linea o di apertura accidentale
di una valvola, quando il sistema è sotto pressione, la
pompa può liberare liquidi tossici e/o volatili molto
pericolosi.
E’ opportuno adottare un sistema di protezione del
viso quando si inietta il campione o si esegue una
manutenzione routinaria del sistema.
Non smontare mai una linea del solvente od una
valvola quando il sistema è sotto pressione.
Fermare prima la pompa ed aspettare che la
pressione scenda a zero.
Usare dei contenitori per solventi infrangibili ed in
grado di lavorare a 50-60 psi.
Quando i contenitori sono sotto pressione, usare
una protezione esterna.
Leggere e rispettare tutti gli avvisi di NOTA,
CAUTELA e ATTENZIONE.
Cromatografia Flash
L’operatore deve conoscere le proprietà fisico-
chimiche delle componenti della fase mobile.
I solventi non vanno messi in contatto diretto con il
tubo di erogazione in poliuretano, dal momento che
alcuni solventi possono causare indebolimento e perdite
con possibili scoppi.
Tutte le componenti del sistema vanno collegate ad una
fonte di alimentazione e ad una messa a terra comuni.
E’ meglio che per quest’ultima venga utilizzata una
spina con polo di terra.
I solventi non-polari possono sviluppare una carica
statica quando vengono pompati attraverso il sistema.
Tutti i recipienti che contengono la fase mobile (inclusi
i tubi e i recipienti di raccolta) devono avere una messa
a terra per disperdere l’elettricità statica.
Vanno utilizzati dispositivi di misurazione e scarico (ad
esempio ionizzatori d’aria) per evitare l’aumento di
elettricità statica.
Radiazioni Ultraviolette
I rivelatori di cromatografia liquida che usano sorgenti
a luce ultravioletta montano degli schermi di protezione
per evitare che gli operatori siano esposti a radiazioni
pericolose.
Per una protezione sicura:
Assicurarsi che i coperchi delle lampade dei
rivelatori a lunghezza fissa e variabile siano sempre
al loro posto, quando si lavora.
Non guardare mai direttamente dentro le celle o
alla sorgente di luce UV. Quando si vuole
ispezionare la lampada o le celle, usare sempre
delle protezioni adatte per gli occhi, quali vetro in
borosilicato e polistirolo.
4 of 4 03-914603-83:10
Disponibilità delle Parti di Ricambio
E’ politica della Varian il fornire le parti di ricambio per lo strumento ed
i suoi accessori per un periodo di cinque (5) anni a partire dalla data di
produzione dell’ultima unità della serie. Le parti di ricambio saranno
disponibili anche dopo questo periodo di cinque (5) anni ma solo in base
alla disponibilità delle stesse. Per parti di ricambio si intendono i
componenti elettrici e meccanici soggetti ad usura durante l’uso, in
condizioni normali, dello strumento. Come esempio, citiamo i relay, le
lampade, i probe di temperatura , i componenti del rivelatore, i motorini,
ecc. Le parti strutturali o da fusione, le schede elettroniche ed i moduli
funzionali possono essere ricostruiti e rimessi a nuovo durante tutto il
loro periodo di vita e perciò sarà possibile acquistarli, dopo la
produzione dell’ultima unità delle serie, solo in base alla loro
disponibilità.
Servizi Tecnico
La Varian, alla scadenza del periodo
di garanzia, è in grado di fornire ai
suoi clienti un’ampia scelta di
opzioni. Le riparazioni possono
essere effettuate sulla base di
contratti di manutenzione particolar-
mente vantaggiosi od in base ad una
tariffa oraria piu’ il costo delle parti.
A richiesta, si possono avere corsi
per operatori sia sotto forma di
contratto che a tariffe da
concordare.
Uffici Vendite della Divisione Strumenti Analitici della Varian
Per informazioni relative alla Vendita, al Servizio Tecnico o all’acquisto di Parti di ricambio, si prega di
contattare l’ufficio Varian piu’ vicino.
Argentina
Buenos Aires
Tel. +54.11.4.783.5306
Australia
Mulgrave, Victoria
Tel. +61.3.9566.1134
Austria
Vösendorf bei Wien
Tel. +43.1.699.9669
Benelux
Bergen Op Zoom
Tel. +31.164.282.800
Brazil and Latin America (S)
São Paulo
Tel. +55.11.820.0444
Canada
Mississauga, Ontario
Tel. 800.387.2216
China
Beijing
Tel. +86.106209.1727
Europe
Middelburg, The Netherlands
Tel. +31.118.671.000
France
Les Ulis Cédex
Tel. +33.1.6986.3838
Germany
Darmstadt
Tel. +49.6151.7030
India
Mumbai
Tel. +91.22.857.0787/88/89
Italy
Torino
Tel. +39.011.997.9111
Japan
Tokyo
Tel. +81.3.5232.1211
Korea
Seoul
Tel. +82.2.345.22452
Mexico and Latin America (N)
Mexico City
Tel. +52.5.523.9465
Russian Federation
Moscow
Tel. +7.095.937.4280
Spain
Madrid
Tel. +34.91.472.7612
Sweden
Solna
Tel. +46.8.445.1620
Switzerland
Varian AG
Tel. +41.848.803.800
Taiwan
Taipei Hsien
Tel. +886.2.698.9555
United Kingdom and
Ireland
Walton-on-Thames
Tel. +44.1932.898000
Venezuela
Valencia
Tel. +58.41.257.608
United States
Walnut Creek, California, USA
Tel. +1.800.926.3000
(GC and GC/MS)
Tel. +1.800.367.4752
(LC)
www.varianinc.com
03-914603-84:10 1 of 4
Instrucciones de
Seguridad
Instrucciones de Operación
Este Manual de Instrucciones está diseñado para ayudarle a establecer las condiciones de operación que le permitan
operar su instrumento de forma segura y eficaz. Así mismo, se describen consideraciones especiales ó precauciones,
que aparecen en forma de
NOTA, PRECAUCION, y ATENCION como se indica más abajo.Es importante que utilice
el instrumento de acuerdo con este Manual de Operación y cualquier otra información que le proporcione Varian.
Remita a la Oficina Local de Varian cualquier cuestión que tenga respecto al correcto uso de su equipo.
NOTA
Información para ayudarle a
obtener unas prestaciones óptimas
de su instrumento.
¡PRECAUCION
!
Le alerta de situaciónes que pueden
causar daños moderados a la salud
ó al equipo, y cóm evitar esas
situaciones.
ATENCI
N
Ó
Le alerta de potenciales situaciones
peligrosas que pueden causar serios
daños, y cómo evitar esas
situaciones.
Símbolo Descripción
ATENCIÓN
PELIGRO DE
DE
S
C
A
R
G
A
ELÉ
C
TRI
C
A
El instrumento utiliza voltages peligrosos. Desconecte el interruptor
general antes de retirar los paneles atornillados.
Peligro de productos químicos. Evite el contacto, especialmente cuando
rellene los depósitos. utilice protección de ojos y piel.
ATENCIÓN
PELIGRO DE
QUEM
A
DUR
A
S
Superficies posiblemente calientes ó frías (criogénico). Utilice
protección para la piel.
Las partículas volátiles, productos químicos o radiación UV pueden
causar daños en los ojos. Usar las debidas protecciones para la cara y
los ojos.
ATENCIÓN
PELIGRO DE FUEG
O
Peligro potencial de fuego. Siga las instrucciones del Manual de
Operación para su seguro funcionamiento.
ATENCI
Ó
N
PELIGRO DE EXPLOSIÓN
Peligro potencial de explosión debido al tipo de gas ó líquido empleado.
ATENCIÓN
PELIGRO DE RADIACIÓN
Peligro por Fuente de radiación. Siga las instrucciones del Manual de
Operación para su seguro funcionamiento.
ATENCIÓN
PARTES EN MOVIMIENT
O
Mantenga alejados los dedos y las manos.
2 of 4 03-914603-84:10
Precauciones Generales de Seguridad
Siga estas indicaciones de seguridad para una correcta operación del equipo.
Realice verificaciones periódicas de fugas en todas las líneas de suministro y tuberías.
No permita que las líneas de gas se doblen ó pinchen. Manténgalas alejadas de zonas de
paso y del calor ó frío excesivo.
Guarde los disolventes orgánicos en cabinas ventiladas, a prueba de fuego, y etiquetadas
para que puedan ser fácilmente identificadas como material tóxico y/ó inflamable.
No acumule disolventes inservibles. Deseche todo el material inservible a través de un
programa especial de desechos y no a través del sistema convencional.
NOTA:
Este instrumento ha sido testado bajo las normas de la Directiva EMC según requerimientos
de la Marca CE de la Unión Europea. Por lo tanto, este equipo puede ser sensible a niveles
de radiaciones / interferencias ó frecuencias que no estén incluidas dentro de los límites
testados.
ATENCI
N
Ó
Este instrumento está diseñado para análisis cromatográfico de muestras preparadas
apropiadamente. Debe ser operado usando gases y/ó disolventes apropiados y con unos
niveles máximos de presión, flujos y temperaturas, según se describe en este manual.
ATENCI
N
Ó
El Usuario tiene la obligación de informar al Servicio Técnico de Varian cuando el
instrumento vaya a ser empleado para análisis de muestras peligrosas de origen biológico,
radioactivo ó tóxico, antes de comenzar a realizar cualquier análisis.
Peligros Eléctricos
Desconecte el instrumento de todos las conexiones eléctricas a la red antes de retirar los
paneles para evitar la posible exposición a peligrosos voltages.
Cuando sea necesario emplear una clavija eléctrica no original, asegurese de colocar los
cables de acuerdo con el código de colores y polaridades descritos en el manual y los
códigos de seguridad de la red eléctrica.
Sustituya los fusibles fundidos con fusibles del tipo y tamaño estipulados en el panel de fusibles
ó en el manual.
Sustituya los cables deteriorados inmediatamente con cables del mismo tipo y
graduación.
Asegureses de que los valores de las líneas de electricidad se ajustan a los valores para
los que el Instrumento ha sido preparado.
Botellas de Gas Comprimido
Guarde y maneje las botellas de gas con cuidado y de acuerdo con las normas de seguridad.
Asegure las botellas a una estructura inmovil ó a la pared.
Guarde y mueva las botellas en posición vertical. Retire los reguladores antes de
transportarlas.
Guarde las botellas en un área ventilada, lejos de fuentes de calor, de luz solar directa y de
temperaturas extremadamente bajas.
Identifique las botellas claramente para evitar cualquier duda sobre su contenido.
Utilice sólamente reguladores y conexiones aprobadas.
Utilice sólo tubos de conexión cromatográficamente límpios (Varian p/n 03-918326-00) y que
tengan una graduación de presión significativamente mayor que la mayor presión del regulador.
03-914603-84:10 3 of 4
GC Prácticas de Seguridad
Sistema de Extracción
No se necesita un sistema de extracción para los
detectores GC instalados en un laboratorio bien
ventilado, excepto cuando se analicen muestras
químicas peligrosas. Si instala un sistema de
extracción:
Utilice conductos a prueba de fuego.
Instale un ventilador al final del sistema.
Instale entradas de aire cuya vibración no afecte al
trabajo del detector.
Compruebe periódicamente el correcto
funcionamiento del sistema.
Asegurese de una correcta ventilación del
laboratorio.
Detectores con fuentes radioctivas
Lea con cuidado y cumpla todas las NOTAS,
PRECAUCION, y ATENCION del Manual del
Detector Ni
63
ECD.
Realice los test de contaminación radioactiva
descritos en el Manual del Detector Ni
63
ECD.
Cumpla con los plazos y procedimientos de test de
fugas.
Peligro de Quemaduras
Las zonas de calor ó frío (criogénicas) del
Cromatógrafo de Gases pueden permanecer calientes ó
frías durante bastante tiempo después de apagar el
instrumento. Para evitar quemaduras asegureses de que
todas las áreas que se calienten ó enfríen han vuelto a la
temperatura ambiente, ó protejase adecuadamente las
manos, antes de tocar las superficies potencialmente
calientes ó frías.
LC Prácticas de Seguridad
Peligro de Alta Presión
Si se rompe una línea de presión, ó se abre una válvula
de seguridad accidentalmente bajo presión, la bomba
puede generar líquidos a alta presión potencialmente
peligrosos, produciendo un chorro a alta velocidad de
líquidos volátiles y/ó tóxicos.
Lleve protección facial cuando inyecte muestras ó
realice mantenimiento de rutina.
Nunca abra una línea ó una válvula bajo presión.
Apague la bomba antes y deje que la presión baje a
cero.
Utilice depósitos irrompibles que sean capaces de
operar a 50-60 psi.
Mantenga cerrada la junta del depósito cuando se
haye bajo presión.
Lea y cumpla todas las NOTA, PRECAUCION, y
ATENCION del manual.
Cromatografía Flash
El operador debe familiarizarse con las propiedades
físico-químicas de los componentes de la fase móvil.
Alejar los disolventes del contacto directo con los tubos
de poliuretano ya que ciertos disolventes pueden causar
reblandecimiento de los tubos o posibles fugas con
riesgo de explosión.
Todos los componentes del sistema deben estar
conectados a un enchufe común con toma de tierra
común. Esta toma de tierra debe ser una toma de tierra
verdadera en lugar de flotante.
Los disolventes no-polares pueden originar carga
estática cuando son bombeados por el sistema. Todos
los recipientes que contienen fase móvil (incluyendo
los tubos y los recipientes de recogida) deben estar
conectados a tierra para disipar la electricidad estática.
Utilizar medidores de carga estática y los debidos
dispositivos de descarga (por Ej., ionizadores de aire)
para salvaguardarse contra la creación de electricidad
estática.
Radiación Ultravioleta
Los detectores del Cromatógrafo de Líquidos que
utilizan una fuente de luz ultravioleta disponen de
protección para prevenir exposiciones radioactivas al
personal.
Para una correcta protección:
Asegurese de que las cubiertas de protección de la
lámpara de los detectores está correctamente
situada durante su funcionamiento.
No mire directamente a las celdas del detector ó a
la fuente de luz UV. Cuando inspeccione la fuente
de luz ó la celda, utilice siempre una protección
para los ojos como gafas de borosilicato ó
poliestireno.
4 of 4 03-914603-84:10
Disponibilidad de Recambios
Es Política de Varian disponer de Recambios para cualquier instrumento y
la mayoría de los accesorios por un periodo de cinco (5) años después del
último instrumento fabricado. Los recambios durante esos cinco años
estarán disponibles, pero siempre bajo el sistema “Según disponibilidad”.
Los Recambios están definidos como todas aquellas partes individuales
mecánicas ó eléctricas que son susceptibles de fallo durante su normal
proceso de operación. Por ejemplo, relés, lámparas, sondas de temperatura,
elementos del detector, motores, etc. Las planchas de metal, partes de la
estructura, placas de circuitos integrados, y otros módulos funcionales son
normalmente susceptibles de reparación y por lo tanto sólo estarán
disponibles bajos el sistema “Según disponibilidad” después del último
instrumento fabricado.
Disponibilidad de
Servicio
Varian ofrece una gran variedad de
sistemas de Servicio para mantener
el soporte a sus usuarios tras el
periodo de garantía. El Soporte de
Servicio se ofrece a través de
atractivos Contratos de Servicio ó
bajo un sistema de facturación de
mano de obra y materiales. El
mantenimiento y el entrenamiento
se realiza por ingenieros
cualificados bajo Contrato ó
petición.
Oficinas de Instrumentación Analítica Varian
Para cualquier consulta sobre Instrumentación Analítica, Servicio Técnico ó Recambios y Accesorios,
contacte con su oficina local:
Argentina
Buenos Aires
Tel. +54.11.4.783.5306
Australia
Mulgrave, Victoria
Tel. +61.3.9566.1134
Austria
Vösendorf bei Wien
Tel. +43.1.699.9669
Benelux
Bergen Op Zoom
Tel. +31.164.282.800
Brazil and Latin America (S)
São Paulo
Tel. +55.11.820.0444
Canada
Mississauga, Ontario
Tel. 800.387.2216
China
Beijing
Tel. +86.106209.1727
Europe
Middelburg, The Netherlands
Tel. +31.118.671.000
France
Les Ulis Cédex
Tel. +33.1.6986.3838
Germany
Darmstadt
Tel. +49.6151.7030
India
Mumbai
Tel. +91.22.857.0787/88/89
Italy
Torino
Tel. +39.011.997.9111
Japan
Tokyo
Tel. +81.3.5232.1211
Korea
Seoul
Tel. +82.2.345.22452
Mexico and Latin America (N)
Mexico City
Tel. +52.5.523.9465
Russian Federation
Moscow
Tel. +7.095.937.4280
Spain
Madrid
Tel. +34.91.472.7612
Sweden
Solna
Tel. +46.8.445.1620
Switzerland
Varian AG
Tel. +41.848.803.800
Taiwan
Taipei Hsien
Tel. +886.2.698.9555
United Kingdom and
Ireland
Walton-on-Thames
Tel. +44.1932.898000
Venezuela
Valencia
Tel. +58.41.257.608
United States
Walnut Creek, California, USA
Tel. +1.800.926.3000
(GC and GC/MS)
Tel. +1.800.367.4752
(LC)
www.varianinc.com
ProStar 400 AutoSampler i
Table of Contents
Introduction.............................................................................................. 1
Installation................................................................................................ 3
Unpacking............................................................................................................................3
Connections.........................................................................................................................3
Power Connections.......................................................................................................4
Communication Connectors..........................................................................................4
Control I/O Connector.............................................................................................5
Vial Number Output Connector ..............................................................................6
RS485 Connector...................................................................................................6
Fluid Connections .........................................................................................................6
Sample Loop...........................................................................................................7
Digital Dispenser System (DDS)............................................................................7
Sample Drain for Loopfilling by Headspace Pressure............................................8
Sample Consumption..........................................................................................................8
Rest volume ..................................................................................................................8
Pre-flush volume...........................................................................................................8
Injection volume......................................................................................................9
Sample consumption formula (dispenser controlled).............................................9
Sample consumption for headspace pressure controlled loopfill...........................9
Filling and Sealing the Vials ..............................................................................................10
Loading the Sample Tray ..................................................................................................10
Positioning of vials................................................................................................10
Needle wash vials.................................................................................................11
Large Volume Samples.....................................................................................................11
Description ..................................................................................................................11
Installation...................................................................................................................12
Instrument Description ......................................................................... 13
General Description...........................................................................................................13
Injection Principle ..............................................................................................................14
Dispenser-controlled Injection.....................................................................................14
Pressure-controlled Injections.....................................................................................15
Digital Dispenser System (DDS).................................................................................16
Operating Principle...............................................................................................16
ii 03-914786-00:3
Operation................................................................................................ 17
Principle.............................................................................................................................17
Different Programming Modes....................................................................................17
Other Modes ...............................................................................................................17
READY Status.............................................................................................................18
Key Functions....................................................................................................................18
Function Codes .................................................................................................................19
Programming Chart...........................................................................................................20
Programming.....................................................................................................................21
System Settings..........................................................................................................21
RUN Parameters.........................................................................................................22
Cooling Control (optional)...........................................................................................23
RUN...................................................................................................................................23
HOLD ..........................................................................................................................24
Priority Sample............................................................................................................25
Remote Control..................................................................................................................25
PC Workstation Interface...................................................................................................26
Varian 4400 Integrator Interface........................................................................................27
Special Display Messages.................................................................................................27
After Use............................................................................................................................28
Maintenance/Service............................................................................. 29
Needle Penetration Depth.................................................................................................30
Needle Pair Replacement..................................................................................................30
Sample Needle............................................................................................................30
Air Needle ...................................................................................................................32
Dispenser Pump Tubing....................................................................................................32
Appendix................................................................................................ 33
Specifications.....................................................................................................................33
Accessories .......................................................................................................................35
ProStar 400 AutoSampler 1
Introduction
The ProStar 400 AutoSampler is dedicated to routine analyses
of large series of samples in an environment where zero sample
loss and injection flexibility are of little significance but where
reliability, stability, and reproducibility are mandatory. The
ProStar 400 therefore makes use of flushed loop injection, with
reproducibility of injection better than 0.5%.
2 03-914786-00:3
ProStar 400 AutoSampler 3
Installation
Unpacking
Inspect the shipping container for indications of damage.
Damage occurring during transit is the responsibility of the
carrier and should be reported immediately to the carrier and to:
Varian, Inc.
2700 Mitchell Drive
Walnut Creek, California 94598-1675
Attention: Customer Service
1-800-FOR-HPLC or your local Varian office
For contents of shipping container see the Standard Accessory
Kit list in the shipping box.
Unpack the ProStar 400 AutoSampler carefully.
Connections
5
4
3
1
2
9
6
8
Figure 1 ProStar 400 AutoSampler Rear Panel
1 Fuses and voltage selector
2 Main power input
3 Power switch
4 Cooling fan, only in case of tray
cooling
5 Standard RS232 connector
6 Connector vial number output
7 Connector control I/O
8 Optional communication connector
9 Serial Number Label
4 03-914786-00:3
Power Connections
Before plugging in the power cable, check voltage settings of
the modules at the input socket on the rear panel.
Make sure that the voltage settings of the modules are
identical with the voltage of your local power supply.
Use only a supply appliance with protective grounding.
If the indicated voltage is not correct, select the proper
voltage by removing, inverting, and then re-inserting the
voltage selector.
When the voltage selection and fuses are correct for your
power source, plug in the power cable.
The correct fuses should be installed.
WARNING:
FIRE HAZARD
For continued protection replace only with same type and rating of fuse.
If a new voltage was selected, check the fuses and change
appropriately with the following specifications:
For ... Use ... Part Number
115 Vac ±10% Two 5.0 amp T-type (slo-blo) 55-500338-00
230 Vac ±10% Two 2.5 amp T-type (slo-blo) 55-500344-00
Communication Connectors
For connection to Varian ProStar and Star LC modules, use
Cable Kit Part Number 03-909126-90. Follow the Installation
Instructions included with that cable. Information in the following
paragraphs is provided for users who wish to develop custom
interfaces to other devices.
INSTALLATION
ProStar 400 AutoSampler 5
Control I/O Connector
Table 1 Control I/O Connector
Pin No. I/O Description
1 24 volt DC
2 Auxiliary output 2 inverted (open collector, max. 250 mA)
3 Auxiliary output 2 (open collector, max. 250 mA)
4 Auxiliary output 1 inverted (open collector, max. 250 mA)
5 Auxiliary output 1 (open collector, max. 250 mA)
6 Inject marker output (N.O. contact)
7 Inject marker output (N.C. contact)
8 Inject marker common (for N.O./N.C. contacts)
Note: Starting at the moment of injection, Inject marker contacts are
closed/openproducing a 1.0 sec. switch closure.
9 Inject marker output (TTL, active low)
10 Stop I/O (TTL, pulled up); output is low when the ProStar 400 AutoSampler ends
processing (READY); pull low input will stop processing (ProStar 400 goes to READY).
11 Spare (open collector)
12 Next vial input (active low, pulled up, TTL)
This input triggers a next vial to be processed when the ProStar 400 AutoSampler is in REMOTE
CONTROL mode.
13 Freeze (HOLD) input (active low, pulled up, TTL)
This input has the same function as the HOLD/CONT key (see Operation on page 17).
14 Next injection input (active low, pulled up, TTL)
This input triggers a next injection when the
ProStar 400 AutoSampler is in REMOTE CONTROL
mode. It can also be used as a START input when the ProStar 400 is not in REMOTE CONTROL
mode.
15 Ground
16 Ground
NOTE: The duration of inputs 10, 12, and 14 must be at least 20 msec.
6 03-914786-00:3
Vial Number Output Connector
8-bit BCD-coded VIAL NUMBER OUTPUT (True logic),
representing vial numbers 1-96; active when corresponding vial
is processed.
Table 2 Vial Number Output Connector
Pin No. Output Pin No. Output
1 Bit 0 units 1 9 Bit 1 units 2
2 Bit 2 units 4 10 Bit 3 units 8
3 Bit 4 units x 10 11 Bit 5 units x 20
4 Bit 6 units x 40 12 Bit 7 units x 80
8 Ground 15 Inject marker (TTL, active low)
RS485 Connector
The ProStar 400 can be controlled by a PC using the RS485
interface.
Fluid Connections
The instrument has been tested with isopropanol. Make sure
that the mobile phase of your HPLC system is miscible with
isopropanol. If not, start up with an intermediate solvent as
mobile phase which is compatible with your column.
To gain access to the high pressure valve, remove the keyboard
cover of the ProStar 400
AutoSampler.
WARNING:
MOVING PARTS
Moving parts and sharp needle. Keep hands clear.
Remove the safety screw on the left hand side of the ProStar
400 AutoSampler. Lift the cover and place it on the top of the
AutoSampler.
Connect the HPLC pump to port 5 and the column to port 6 of
the injection valve.
INSTALLATION
ProStar 400 AutoSampler 7
Figure 2 Keyboard Cover Removal
Sample Loop
The ProStar 400 is factory-equipped with a 20 µL sample loop.
If a different volume is to be injected, the sample loop must be
replaced. Please note that to fill the loop quantitatively, three
times the loop volume is withdrawn from the sample vial for
loops smaller than 100 µL and twice the loop volume for loops
larger than 100 µL.
Loops ranging from 5 µL to 1 mL are available from Varian.
Digital Dispenser System (DDS)
The DDS pump tubing cassette is factory-installed and
connected to the injection valve. Fasten the pump tubing
cassette before use with the screw on top of the pump tubing
cassette. If the AutoSampler is not to be used for two days or
more, be sure to loosen this screw to prevent permanently
deforming the tubing. If the pump tubing cassette needs
replacement, refer to Maintenance/Service on page 29.
8 03-914786-00:3
Sample Drain for Loopfilling by Headspace Pressure
Time-based loopfilling by sample headspace pressure can be
selected (see Operation on page 17) to shorten loopfill time for
larger loop volumes (see Injection Principle on page 14).
To allow time-based loopfilling and to prevent hydrostatic sample
loss, the special sample drain for headspace pressure loopfill
must be connected at the injection valve, replacing the dispenser
connection at the valve.
Sample Consumption
Rest volume
Since the sample needle is always at some (very short) distance
above the bottom of the sample vial, a certain volume of sample
always remains in the vial, out of reach of the sample needle.
This volume is called the rest volume.
For standard 1.5 mL vials, the rest volume is approximately
200 µL. For a conical vial, the rest volume is only a few µL.
Refer to page 30 for adjustment of needle penetration depth.
Pre-flush volume
Prior to the FIRST injection, the sample needle and tubing
(needleinjection valve) are flushed with sample (for dispenser
controlled loopfill, see page 14, Injection Principle).
Depending on the concentration differences between samples
and the cross-contamination allowed, this so-called pre-flush
volume may range between 30-999 µL (programmable). Only
dispenser controlled loopfilling uses a pre-flush.
If sample loss greater than 30 µL for pre-flush is not acceptable,
select NEEDLE WASH between sample vials in SYSTEM
SETTINGS to avoid cross-contamination. See Operation on
page 17.
INSTALLATION
ProStar 400 AutoSampler 9
Injection volume
Due to the reduced solvent velocity near the wall of the tubing
(loop), it takes more than the nominal loopvolume to fill the loop
reproducibly. For flushed loop injections the ProStar 400
takes
twice the loop volume from the sample vial for a sample loop
equal to or larger than 100 µL and three times the loop volume
for a sample loop smaller than 100 µL.
Sample consumption formula (dispenser controlled)
The minimum amount of sample needed for N injections per vial:
Flushed loop injections for 100 µL loop or larger:
rest volume + pre-flush volume + 2N x loopvolume + (N-1) x 4 (µL)
Flushed loop injections for loop smaller than 100 µL:
rest volume + pre-flush volume + 3N x loopvolume + (N-1) x 4 (µL)
Example: 3 flushed loop injections out of a standard sample vial
using a 20 µL loop and 30 µL pre-flush volume, minimum sample
volume needed is:
200 µL + 30 µL + 3 x 3 x 20 µL + 2 x 4 µL = 418 µL
Sample consumption for headspace pressure controlled loopfill
If the sample loop is filled on a time basis by sample headspace
pressure (see Injection Principle on page 14 and Operation on
page 17), sample consumption has to be determined
experimentally since the flow is dependent on the viscosity. (For
water, the flow rate is approximately 1 mL/min.) Make sure that
programmed fill time is sufficient to flush the loop with at least
twice its volume.
If more injections are to be taken from the same vial, please note
that a volume equal to max. 20% of the headspace in the vial
after loopfill may flow to waste during analysis time due to
expansion of the headspace back to atmospheric pressure.
10 03-914786-00:3
Filling and Sealing the Vials
The 1.5 mL vials, as well as the conical vials, can best be filled
by means of a narrow-end pipette to allow air to escape while
filling the vial.
NOTE: Do not fill vials past the shoulder. Sample will be forced into the air
needle, risking extra cross-contamination of samples.
It is important that the seal be airtight to maintain a constant
pressure on the vial for air bubble prevention and reproducible
injections.
Leaking vial septa will impair reproducibility when doing loop
overfill with headspace pressure.
NOTE: Do not reuse a vial without replacing its septum.
Loading the Sample Tray
To allow remote loading of the sample tray, the sample tray
consists of four removable segments that fit in one unique
position of the tray holder.
Use the STEP key (see Operation on page 17) to rotate the tray
(functioning only when the ProStar 400 is in READY status).
CAUTIO
N
Do not rotate the tray manually; you may damage the tray drive mechanism.
Positioning of vials
Sample vials should be placed in sequential positions on the
tray. Empty spaces between vials of a sample series are
allowed, since the ProStar 400 can detect empty positions. After
detecting an empty place, the AutoSampler will continue with the
next position.
INSTALLATION
ProStar 400 AutoSampler 11
Additional samples can be placed during RUN since the LAST
VIAL value can be changed during RUN (see Operation on page
17).
Needle wash vials
If needle wash is programmed (see Operation on page 17),
place 4 vials with washing solvent (1.5 mL each, usually mobile
phase) on positions 93-96. You must use all four vials as they
will be used alternately.
Large Volume Samples
Description
The large volume sample tray is an option of the ProStar 400
AutoSampler. This option allows the user to inject large volumes
of sample with the DDS or by headspace pressure.
The option consists of:
4 LSV sample tray segments
500 µL loop
a serum needle with serum air-needle
special sample tubing (0.5 mm ID)
sample drain
12 03-914786-00:3
Installation
Install the LSV option according to the following procedure:
Replace the standard installed tubing and needles with the
tubing and needles of the LSV option. Follow the procedure
described in Maintenance/Service, page 29.
Replace the standard tray by the LSV tray.
Install the 500 µL loop to port 1 and 4.
Check the needle penetration depth and if necessary adjust
it. See page 29, Needle Pair Replacement.
Connect the drain to port 3 if the loop will be filled on a time
basis by headspace pressure. It is also possible to fill the
loop with the DDS. This will take less sample, but more time.
NOTE: If the loop is filled using the DDS, a larger preflush volume (minimum
50 µL) must be programmed to avoid cross contamination due to the
larger internal diameters of the tubing and needle.
ProStar 400 AutoSampler 13
Instrument Description
General Description
Figure 3 ProStar 400
1 Sample tray, consisting of 4 removable segments
2 Keyboard
3 Display
4 Removable cover
5 Needle arm with sample needle
6 Injection valve with sample loop
7 Dispenser cassette screw
8 Dispenser
9 Outlet tubing holder
10 Common leakage/condensation water drain for injection valve,
sample tray and DDS
14 03-914786-00:3
Injection Principle
A six-port high pressure switching valve can perform the
injections based on the flushed loop principle. Loopfilling can
be done on a volume basis, controlled by the digital dispenser
system, or on a time basis by headspace pressure on the
sample to shorten filling time for larger loop volumes. See
Operation on page 17. The switching patterns of the valve in
“LOAD” and “INJECT” positions are shown in Figure 4. An
injection is performed as described in the following paragraphs.
Dispenser-controlled Injection
1. Dispenser aspirates an approximately 10 µL air bubble in the
sample needle for more efficient removal of the previous
sample.
2. With the injection valve in inject position, the coaxial needle
pair is inserted into the sample. Air pressure, applied to the
sample through the outer air needle, ensures that no air or
vapor bubbles are formed during sample withdrawal.
3. Dispenser withdraws “preflush volume” from sample vial to
fill the sample line with sample and to remove previous
sample (30 - 999 µL, programmable).
4. Injection valve switches into load position with flushed-loop
injections; dispenser transports 2 or 3 X loopvolume through
the loop to fill the loop quantitatively.
2 X loopvolume for loops equal to or larger than 100 µL
3 X loopvolume for loops smaller than 100 µL
5. Injection valve switches into inject position. The sample loop
is now part of the HPLC mobile phase flow path. The
sample is transported to the column, and the analysis time
starts.
If one injection is to be made out of each sample vial, the needle
pair withdraws after analysis time and sequence 1-5 is repeated
for the next vial. If more than one injection is to be made out of
the same sample vial, the needles remain in the vial and after
INSTRUMENT DESCRIPTION
ProStar 400 AutoSampler 15
the analysis time is completed, the next injection is made starting
the sequence at step 3 with a fixed preflush of 4 µL.
Figure 4 Dispenser-controlled Injection
Pressure-controlled Injections
1. With the injection valve in load position, the coaxial needle
pair is inserted into the sample. Air pressure, applied on the
sample through the outer (air-) needle, will force the sample
via the inner (sample-) needle through the sample loop. The
duration of the headspace pressure is programmable;
appropriate duration has to be determined experimentally.
2. Injection valve switches into inject position. Sample loop is
now part of the HPLC mobile phase flow path: sample is
transported to the column. Analysis time starts.
NOTE: A special sample drain that prevents siphoning must be connected to the
injection valve (replacing the dispenser connection). Refer to Installation
on page 3.
16 03-914786-00:3
If one injection is to be made out of each sample vial, the needle
pair withdraws after the analysis time is complete and sequence
steps 1-2 starts for the next vial. If more than one injection is to
be made out of the same sample vial, the needles remain in the
vial.
Figure 5 Pressure-controlled Injection
Digital Dispenser System (DDS)
Operating Principle
The DDS is a miniature “finger pump”. The operating principle is
shown below. Fingers 1 and 3 act as inlet and outlet pinch valve,
respectively, finger 2 provides the fluid displacement. The stroke
of finger 2 is factory adjusted to provide 2 µL per stroke. Since
the volume dispensed is always a multiple of one stroke volume
(digital dispensing), i.e., 2, 4, 6 µL, etc., odd values for volumes
will be rounded down to even values.
Figure 6 Operating Principle of Digital Dispensing System (DDS)
ProStar 400 AutoSampler 17
Operation
Operating the ProStar 400 AutoSampler is easy. After
programming the system SETTINGS, only a few parameters
need to be programmed for regular automatic processing of a
series of samples.
All parameter values are saved in memory when power is
switched off or during power failure, except the tray temperature
setting, if the tray cooling option is installed. Tray cooling is
always turned off at power up.
Principle
Different Programming Modes
To simplify regular operation, common injection parameters like
“analysis time” and “first/last vial” are programmed in the RUN
PARAMETER mode. Less frequently altered parameters like
“auxiliaries YES/NO” are programmed in the SYSTEM
SETTINGS mode. An additional COOLING CONTROL mode
takes care of the sample tray temperature, when the option is
installed.
Other Modes
RUN mode for automatic processing of samples.
REMOTE CONTROL mode for autosampler control via I/O
contacts.
SERIAL RS485 mode for autosampler control via serial
interface.
18 03-914786-00:3
READY Status
READY status is the “ground state” of the ProStar 400
AutoSampler which is initiated automatically after power UP.
Every mode can be entered from READY status, except
PRIORITY mode, which can be entered only when the
ProStar 400 AutoSampler is in RUN mode.
In addition, RUN PARAMETER and COOLING CONTROL
mode can be entered when the ProStar 400 AutoSampler is
in the RUN mode.
Function codes are used to enter any specific mode, except for
the RUN PARAMETER mode which can be entered directly via
the PROG/END key, and RUN mode (entered by the START
command).
Every mode uses the same function code (F,0) to exit, except for
RUN PARAMETER mode and RUN mode which are left via
PROG/END and STOP respectively.
Key Functions
STEP key; used to step through the parameter list. The STEP key is also used to
rotate the sample tray (in READY status only.).
START/STOP
Start/Stop automatic processing of samples.
HOLD/CONT
Hold/Continue countdown of analysis time. Analysis time is extended with the time
that hold is active.
PROG/END
Enables/Ends programming of parameters in the selected mode. Note that the
PROG/END key selects the RUN PARAMETER mode and enables the
programming of its parameters at the same time.
CL
Clears the value of the parameter on display.
F
Function key; used in combination with a numerical key to select or exit the
various modes.
0-9
Numerical keys; used to enter values for programmable parameters. Values are
stored when going to the next parameter (STEP) or when ending programming
(PROG/END).
OPERATION
ProStar 400 AutoSampler 19
Function Codes
The following table shows all the possible modes of the
ProStar 400 AutoSampler.
Function code Selected mode
F,9 Selects SYSTEM SETTINGS mode.
F,7 Selects COOLING CONTROL mode (only if
cooling option is installed)
F,2 Selects PRIORITY mode (only accessible
during sample run).
F,3 Selects REMOTE CONTROL mode.
F,4 Selects SERIAL RS485 mode.
F,0 To exit all modes, selected by a function code
Refer to the following Programming Chart.
20 03-914786-00:3
Programming Chart
Use to step.
1. FIRST VIAL (1—>48/92/96)
2. LAST VIAL (1—>48/92/96)
3. NO OF INJ'S/VIAL (1—>9)
4. PREFLUSH VOLUME (30—>999µL)
FLUSH TIME (1—> 999 SEC)
5. ANALYSIS TIME (0:00—> 99:59)
6. TIME AUX 1 ON (0:00—> 99:59)
7. TIME AUX 1 OFF (0:00—> 99:59)
8. TIME AUX 2 ON (0:00—> 99:59)
9. TIME AUX 2 OFF (0:00—> 99:59)
Use to step.
1. LOOPVOLUME (0->999µL)
2. SAMPLE VOLUME (STD/LSV)
3. FLUSH (VOL/TIME)
4. NEEDLE WASH (YES/NO)
5. AUXILIARIES (YES/NO)
TRAY COOLING (ON / OFF)
PRESS TO ADVANCE SAMPLE TRAY REMOTE CONTROL MODE SERIAL RS485 MODE
DEVICE IDENTIFIER (10 —> 19)
RUN MODE
ANALYSIS TIME
Accessible: Run parameters, Temperature control.
PRIORITY MODE
default vial no 00!
FREEZE ANALYSIS TIME
Accessible:
Run parameters,
Temperature control.
Enter number to activate
OPERATION
ProStar 400 AutoSampler 21
Programming
Only three modes contain programmable parameters:
SYSTEM SETTINGS mode to “set” system parameters.
RUN PARAMETER mode for regular programming of
sample processing.
COOLING CONTROL mode to program the tray cooling, if
installed.
System Settings
With the ProStar 400 in READY status, key in F,9 to select
SYSTEM SETTINGS mode. Press PROG/END to enable
programming of the following parameters (use STEP key to go to
the next parameter):
LOOP VOLUME
Enter volume of the installed loop: 0-999 µL. If using dispenser
controlled loopfill, this will set the loop overfill volume to 3X
loopvolume if loop <100 µL and 2X loopvolume for loops
>100 µL.
SAMPLE VOLUME
(STD/LSV)
Enter 0 to select STANDARD sample tray. Enter 1 if the optional
Large Sample Volume tray has been installed (48 vials of 5 mL
each).
FLUSH (VOL/TIME)
Enter 0 to select dispenser controlled loopfilling on a volume
basis. Enter 1 to select loop filling by sample headspace
pressure on a time basis. Filling on a time basis may be used for
large injection volumes (>500 µL) to shorten loopfill time.
For loopfilling on a time basis, mount the special drain
included in the Accessory Kit to allow for pressure
controlled sample transport and to prevent hydrostatic
sample flow which may empty your sample vial during
analysis time.
22 03-914786-00:3
NEEDLE WASH
(YES/NO)
Enter 1 to select needle wash.
Positions 93-96 are now used as containers for washing solvent.
After every sample vial the needle and connecting tubing is
flushed with solvent from one of the “wash vials” (alternating
between 93 and 96).
Enter 0 if no needle wash is wanted (position 93-96 can now be
used for sample vials).
AUXILIARIES (YES/NO)
Enter 1 if time programmable auxiliary output(s) are to be used.
Parameters will appear in the RUN PARAMETER mode.
Enter 0 if no auxiliaries are to be used.
RUN Parameters
With the ProStar 400 in READY status, press PROG/END to
select RUN PARAMETER mode and to enable programming at
the same time.
The following parameters can be programmed (use STEP key to
go to next parameter):
FIRST VIAL
Enter position number of the first vial of the sample series in the
sample tray.
1-96 without needle wash
1-92 with needle wash
1-48 with LSV
LAST VIAL
Enter position number of the last vial of the sample series in the
tray. (See FIRST VIAL for valid numbers.)
INJ/VIAL
Up to 9 injections can be taken from the same vial. Enter number
0-9.
PRE FLUSH VOLUME
Parameter shows up for flush on a volume basis only; enter
volume (of sample) which is to be used to flush needle and
connecting tubing prior to filling the loop: 30-999 µL.
FLUSH TIME
Parameter shows for flush on a time basis only. Enter duration of
headspace pressure for loopfilling: 1-999 sec.
ANALYSIS TIME
Enter the time interval needed before the next injection takes
place: 0-99'59". Time countdown starts at moment of injection.
OPERATION
ProStar 400 AutoSampler 23
TIME AUX 1 ON
Parameter shows only when auxiliaries are enabled in System
settings. Enter time at which auxiliary 1 must switch ON: 0-
99'59".
TIME AUX 1 OFF
Parameter shows only when auxiliaries are enabled in System
settings.
Enter time at which auxiliary 1 must switch OFF: 0-99'59".
TIME AUX 2 ON
See AUX 1.
TIME AUX 2 OFF
See AUX 1.
Cooling Control (optional)
Sample tray temperature control is switched ON/OFF in the
COOLING CONTROL mode.
With the ProStar 400 in READY status, key in F,7 to select
COOLING CONTROL mode. Press PROG/END to switch ON or
OFF the cooling control.
The sample tray cooling has a fixed temperature of 4°C.
TRAY COOLING
(ON/OFF)
Enter 0 to switch OFF the sample tray cooling.
Enter 1 to switch ON the sample tray cooling.
NOTE: After power up, the sample tray cooling is always off.
RUN
When programming is complete, system is ready and the
ProStar 400 AutoSampler is in READY status, press
START/STOP key to start automatic processing of the samples.
During RUN, the ProStar 400 will show information relevant to
the actual process such as: SEARCH VIAL 45, LOOPFILL,
WASHING, etc. During analysis time the display will show the
following information continuously (example):
0 VIAL:15 82 2'INJ 4 C
pTIME 03:45 AUX 1 2
24 03-914786-00:3
The first line shows that the second injection from vial 15 is
being processed, vial 82 is the last vial to be processed. The
temperature of the cooling tray shown at the end of the first line
will only be displayed if the option is present.
The second line shows the time since the injection in minutes,
seconds format, and the status of the auxiliaries. The number
will be displayed if the auxiliary is ON (only shown when enabled
in the settings).
The first character of the second line will be a blinking R if the
ProStar 400 is under remote control or a blinking p if a priority
sample is programmed.
It is possible to reprogram RUN PARAMETERS during RUN;
simply press PROG/END to enter the RUN PARAMETER mode.
Press PROG/END to exit RUN PARAMETER mode and to
continue the RUN program.
NOTE: If you do not return to RUN mode, RUN will stop after finishing the
current injection.
Changes in the RUN parameters will be executed immediately
after returning to RUN mode, although an injection will not be
interrupted.
COOLING CONTROL can also be reprogrammed during RUN;
press F,7 to enter COOLING CONTROL mode.
Return to RUN (F,0) to continue RUN.
HOLD
HOLD (press HOLD/CONT) can be used to freeze the time
base. During HOLD, the RUN PARAMETER mode, COOLING
CONTROL mode and PRIORITY mode are accessible to
reprogram/check parameters. Exit any of these modes (if
entered) and press HOLD/CONT key to continue RUN. Analysis
time of the current injection has then been extended with the
time that HOLD was active.
OPERATION
ProStar 400 AutoSampler 25
Priority Sample
A sample run can be interrupted to process an emergency
sample prior to the next sample of the programmed samples
series: press F,2 to enter the priority mode, press PROG/END
key and enter the number of the tray position where the priority
vial has been placed. Press PROG/END to end programming.
Return to RUN (F,0). Priority vial will be processed immediately
after the current vial. A blinking “P” (first position of lower display
line) indicates that a priority vial is to be/being processed. After
processing the priority vial, RUN will continue where it was
interrupted.
NOTE: Priority mode can only be entered during sample run. It cannot be
entered during pre flush or loopfill.
Remote Control
When used with Varian ProStar or Star LC modules, the ProStar
400 is interfaced using Cable Kit Part Number 03-909126-90.
Remote control mode is not necessary to use this cable.
However, using remote control mode, the ProStar 400 will wait
for a “ready” signal from the other modules of the Star system
before starting its injection cycle. See the installation instructions
enclosed with the cable for details of these modes of operation.
When the ProStar 400 is in REMOTE CONTROL mode it can
only be controlled using the “next injection” and “next vial” inputs.
RUN is executed as programmed, but analysis time is now
infinite. Only a “next injection” input signal will initiate the next
injection from the same vial (or from the next vial when the
programmed number of injections per vial have been executed).
A “next vial” input signal will initiate the first injection from the
next vial.
With the
ProStar 400 in READY status, REMOTE CONTROL
mode is entered with F,3; display will show:
0 REMOTE CONTROL
READY
26 03-914786-00:3
A “next injection” input signal will start the RUN.
A blinking R (first position of the lower display line) indicates that
the ProStar 400 is under remote control. All other relevant RUN
information will be displayed as usual.
When all programmed vials have been processed, the display
will show:
0 REMOTE CONTROL
F,0 TO EXIT
Next injection or next vial inputs will no longer have any effect.
Exit REMOTE CONTROL mode (F,0) to return to READY status.
PC Workstation Interface
Up to four ProStar 400 AutoSamplers can be simultaneously
controlled from the Varian Star Chromatography Workstation.
Control requires purchase of the Star LC Control Software Kit.
Contact your local Varian representative for more information or
to order communication kits.
Figure 7 shows the connection cabling and the kit part numbers
for the Star Workstation control of ProStar 400 AutoSamplers.
Complete installation instructions are included with these kits.
OPERATION
ProStar 400 AutoSampler 27
Figure 7 Star Workstation Communication for Single ProStar 400 AutoSampler
Varian 4400 Integrator Interface
The ProStar 400 outputs the vial location number through a BCD
port. Varian Cable Kit Part Number 03-919938-90 provides a
cable to connect the BCD output to the Varian 4400 Integrator.
The instructions enclosed with this cable describe how to
interface to the 4400 such that the AutoSampler vial number is
printed on each 4400 report. Full synchronization cable
operation of the ProStar 400 with the 4400 Integrator and other
Varian Star modules requires this cable plus Cable Kit P/N
03-909126-90 described above.
Special Display Messages
During operation several messages may appear on the display
to make you aware of errors, system malfunctions or other
uncommon events. These special display messages are listed
below together with the appropriate actions to take.
28 03-914786-00:3
MEMORY ERROR
ALL VALUES DEFAULT
Press any key; if the ProStar 400 goes to READY status, all
parameters are set to default values. Reprogram RUN and
TEMP.CONTROL parameters and check SYSTEM SETTINGS.
If message remains, call Varian.
TRAY ROTATION
FAILURE
Tray movement is obstructed; check/remove obstruction. Press
any key to continue; if message remains: call Varian.
NEEDLE MOVEMENT
FAILURE
Needle arm movement is obstructed; check/remove obstruction.
Press any key to continue; if message remains, call Varian.
DISPENSER FAILURE
Call Varian.
PROGRAM VIALS
SYSTEM SETTING STD/LSV was changed: FIRST VIAL and
LAST VIAL are reset to 0; reprogram (RUN PARAMETER
mode). Press any key to continue.
NEEDLE WASH was switched ON (SYSTEM SETTINGS) with
FIRST or LAST vial programmed on WASH positions. FIRST
VIAL and LAST VIAL are reset to 0; reprogram (RUN
PARAMETER mode). Press any key to continue.
ERROR.(.............)
An erratic value has been entered; limits for this parameter are
shown in parenthesis on display. Enter correct value.
After Use
If the ProStar 400 AutoSampler is not to be used for more than
two days, flush needle and valve with water and isopropanol
(can be placed as last vials of a sample series) and loosen pump
tubing cassette screw one turn. Never leave the AutoSampler
out of use with a buffer or salt solution in the tubing; crystals may
block the flow path and may damage the rotor seal of the
injection valve. Power can be switched OFF since all parameter
values are saved in memory (long-life non-chargeable battery
back-up). Only sample tray cooling is changed to OFF after
power UP.
ProStar 400 AutoSampler 29
Maintenance/Service
Figure 8 Injection System
1 Side-port sample needle
2 Air needle
3 Air tubing to provide sample headspace pressure
4 Needle penetration depth adjustment screw
5 Injection valve
6 Digital Dispenser System
7 Pump tubing Cassette
8 Dispenser drain
9 Sample tubing needle --> valve (port 2)
10 Sample tubing valve (port 3) --> dispenser
11 Sample loop
12 Sample drain for loopfilling by sample headspace
pressure. Replaces sample tubing (10)
13 Vial stripper
14 The silicon tubing connector with air inlet hole must be
approximately at the same level as the liquid in the sample
vial to prevent hydrostatic sample flow during analysis
time.
15 Air inlet hole in connector to prevent emptying of sample
vial by hydrostatic suction.
16 Needle connection nut
17 Ferrule (PTFE)
18 Sample needle connection hub
19 Air seal
30 03-914786-00:3
Needle Penetration Depth
To keep rest volume small, the sample needle should stop close
to the bottom of the sample vial. If penetration depth requires
adjustment, proceed as follows (see Figure 8):
Remove keyboard cover.
Place an uncapped vial in the tray.
Program an injection from that vial with injection volume 0 µL
in case of partial loopfill injections or a loopvolume of 0 µL in
case of flushed loop injections. Press START and
disconnect the power supply as soon as the needle is in the
vial.
Loosen adjustment screw one turn (counterclockwise).
Using the needle connection nut as a grip, adjust needle
penetration depth: Needle should stop not less than 1 mm
above the bottom of a standard vial and not less than 2 mm
above the bottom of a conical vial.
Fasten adjustment screw (clockwise).
VIAL SENSOR MUST BE AROUND THE NEEDLE.
CLOSE KEYBOARD COVER.
Connect power.
Needle Pair Replacement
Sample Needle
To replace sample needle proceed as follows:
Remove keyboard cover.
MAINTENANCE/SERVICE
ProStar 400 AutoSampler 31
WARNING:
MOVING PARTS
Moving parts and sharp needle. Keep hands clear.
Place an uncapped vial in the tray.
Program an injection from that vial with injection volume 0 µL
in case of partial loopfill injections or a loopvolume of 0 µL in
case of flushed loop injections. Press START and
disconnect the power supply as soon as the needle is in the
vial.
Loosen needle connection nut (Figure 8) that connects
PTFE tubing to sample needle.
Move needle arm down manually.
Remove sample needle by pulling it out of its fitting with the
PTFE tubing that usually sticks to the needle.
Put in new needle (watch the air seal around the needle).
When needle connection tubing needs replacement, loosen
the nut that connects the tubing to the injection valve.
Cut the appropriate length of a 0.25 mm ID tubing taking
care that cuts are made perfectly rectangular to avoid dead
volumes.
Connect tubing to needle.
Connect loose end of needle connection tubing to port 2 of
injection valve (use a Rheodyne ferrule
.). Do not tighten
excessively; it may close the tubing.
Check needle penetration depth and adjust if necessary.
Connect main power supply.
CLOSE KEYBOARD COVER.
32 03-914786-00:3
Air Needle
To replace air needle, proceed as follows:
Remove sample needle.
Unscrew air needle and install new air needle.
Reinstall sample needle.
Dispenser Pump Tubing
Loosen fitting that connects PTFE inlet tubing of dispenser to
injection valve.
Remove pump tubing cassette including PTFE connection
tubing, by loosening the screw that attaches the cassette to
the dispenser.
Install new pump tubing cassette.
Check length of PTFE tubing.
Connect PTFE tubing to injection valve.
ProStar 400 AutoSampler 33
Appendix
Specifications
ANALYTICAL
Sample capacity 96 samples (92, when needle wash is used)
Injection volume Flushed loop:
5 - 500 µL (dispenser controlled)
5 - >5000 µL (by headspace pressure)
Injections per vial max 9
Analysis time max 99 min 59 sec
Needle wash Selectable, 50 µL fixed volume between vials
Headspace pressure Built-in compressor (0.5 atm or 7 psi)
Switching time injection valve Electrically <100 msec
PERFORMANCE
Reproducibility Flushed loop injections:
RSD 0.5 %
Memory effect Better than 0.2 %
ELECTRICAL
Power requirements 115 Vac; ±10%; 50/60 Hz; 100 VA
230 Vac; ±10%; 50/60 Hz; 100 VA
34 03-914786-00:3
COMMUNICATION
OUTPUTS Inject marker (Relays & TTL)
Stop I/O (TTL)
Vial number BCD output (TTL)
Auxiliary 1 (open collector)
Auxiliary 1 inverted (open collector)
Auxiliary 2 (open collector)
Auxiliary 2 inverted (open collector)
INPUTS Next injection input (TTL)
Next vial input (TTL)
Freeze runtime (TTL)
Stop I/O (TTL)
OPTIONS
Sample tray cooling Built-in Peltier cooling
Temperature: 4°C (fixed)
Accuracy: ± 2°C
Operation range: Ambient - 25°C
Ring temperature at relative humidity of 80% and
ambient temperature of 31°C, decreasing to 50% at
40°C.
Large Volume tray 48 positions for 5 mL vials (specify cool or no-
cool)
PHYSICAL
Dimensions ( W × D × H ) 300 mm × 440 mm × 283 mm
11.8 in × 17.3 in × 11.1 in
Weight 15.5 kg (34 lbs.)
18.5 kg (41 lbs.), with cooling option
APPENDIX
ProStar 400 AutoSampler 35
Accessories
Part Number Description
0391969190 ProStar 400 Startup Kit
Includes: PEEK Tubing (10ft. x 0.01" ID), Package of 10 fingertight fittings and
2 mL Sample Vials (3 x 144)
0391968900 ProStar 400 Large Volume Option
Allows injection volumes up to 4 mL. 48 Sample Vial Capacity Includes:
Racks for 4 mL Vials, Serum Needle, Air Serum Needle, 500 µL sample loop,
and PTFE tubing.
0392604590 Sync Cable Kit
0391993890 Integrator Interface Cable Kit
0190000804 Serum Needle for Standard Vials, Package of 3
0190000805 Air Serum Needle for Standard Vials
0190000836 Serum Needle for Large Volume Option, Package of 3
0190000837 Air Serum Needle for Large Volume Option
0392602714 ProStar 400 Plexiglas Tray Cover
0190000850 Pump Tubing Cassette, Single Channel
R000088016 Air Needle
R000088018 Liquid Sampling Needle, Package of 3
SAMPLE LOOPS
0190018200 5 µL SS Loop for Valco Valve
0190018202 20 µL SS Loop for Valco Valve
0392611011 50 µL SS Loop for Valco Valve
0190018204 100 µL SS Loop for Valco Valve
0392611012 250 µL SS Loop for Valco Valve
0190018205 500 µL SS Loop for Valco Valve
0392611013 1000 µL SS Loop for Valco Valve
36 03-914786-00:3
Part Number Description
0392611014 2000 µL SS Loop for Valco Valve
0392611015 5000 µL SS Loop for Valco Valve
0392611016 10 mL SS Loop for Valco Valve
0392611017 20 µL PEEK Loop for Valco Valve
0392611018 50 µL PEEK Loop for Valco Valve
0190018208 100 µL PEEK Loop for Valco Valve
0392611019 250 µL PEEK Loop for Valco Valve
0392611020 500 µL PEEK Loop for Valco Valve
0392611021 1000 µL PEEK Loop for Valco Valve
0392611022 2000 µL PEEK Loop for Valco Valve
2869450201 Package of 10 Valco Ferrules
2869450101 Package of 10 Valco Nuts
0392607983 Valco fingertight PEEK Nut
0392607984 Valco fingertight PEEK Ferrule
VIALS, SEALS AND CAPS
R0000542CV Standard clear crimptop 2-CV vial (pck/100)
R005411AC6 Crimpcap for standard 2-CV and 1.1-CTVG vials. (pck/100)
R05411CTVG Chromacol 1.1-CTVG conical vial with crimptop. (pck/100)
R054TTS312 Chromacol TTS-312 support for 1.1-CTVG vial. (pck/100)
R0000542SV Standard screwtop 2-SV vial. (pck/100)
R0000548SC Screwcap for standard 2-SV vial. (pck/100)
R005486RTI Septum for standard 2-SV vial. (pck/100)
R05406PPCV Polypropylene crimptop vial 0.6 mL (pck/100)
R000541201 Polypropylene septum caps for polypropylene vials (pck/100)
R005402MTV 0.2 mL Insert to fit inside standard 2 mL crimptop vial, requires support sleeve
R00054MTSA
R00054MTSA Support sleeve for 0.2 mL insert
APPENDIX
ProStar 400 AutoSampler 37
Part Number Description
RK60827510 Chromacol 10-CV, 10 mL vial. (pck/100)
R0K7382420 Chromacol 20-ACB crimpcap and seal for 10-CV vial (pck/100)
R0K6990111 Handcrimper 11 mm OD vials (standard)
R0K6990120 Handcrimper 20 mm OD vials
FOR STANDARD SAMPLE TRAYS
Part Number Description Quantity
0394983500
0394983501
Disposable 2 mL Vials, Screw Caps and Septa 1 gross
12 gross
0390619590
0390619591
Glass 2 mL Vials, Screw Caps and Septa 1 gross
12 gross
6600010400 Amber Glass 2 mL Vials 1 gross
0099743106
0099743105
Tapered Glass 1.1 mL Vials
(requires Teflon Support Sleeve)
500
50
6600012101 Precision 100 µL Vials 12
0099750301
8830024200
Glass 200 µL inserts for 2 mL Vials
Glass 100 µL inserts for 2 mL Vials
1000
1 gross
1600069800
0390614901
0390614902
Caps for all Vial Types
Septa for all Vial Types
1 gross
1 gross
12 gross
FOR LARGE VOLUME SAMPLE TRAYS
0190000839
4 mL Vials
0190000840
Caps for 4 mL Vials
0190000841
Septa for 4 mL Vials
NOTE: The use of Eppendorf microcentrifuge tubes may cause malfunctioning
of the ProStar 400 vial sensor.

Transcripción de documentos

Varian, Inc. 2700 Mitchell Drive Walnut Creek, CA 94598-1675/usa ProStar 400 AutoSampler Operation Manual ©Varian, Inc. 2000 - 2004 Printed in U.S.A. 03-914786-00:Rev. 3 Quality Systems At Varian, Inc. The ISO 9000 series standards were created in Geneva in 1987 to cut through a morass of conflicting quality definitions. These standards define a model for quality assurance systems in product design, development, manufacturing, installation, service, and customer support. They are now the worldwide quality assurance benchmark used to gauge the strength of a company's commitment to quality, and the value of its quality systems. Various organizations around the world, such as the British Standards Institution (BSI), provide certified, objective auditors to scrutinize quality procedures, product development, manufacturing processes, and customer satisfaction programs. No company can claim ISO 9000 series registration unless it receives a stamp of approval from the demanding quality assessors of BSI or similar accredited examining body. ISO 9000 series registration constitutes an objective third-party report to determine the level of a supplier's commitment to quality. In 1992, Varian, Inc., Analytical Instruments became registered to the most comprehensive of the ISO 9000 series standards — ISO 9001. ISO 9001 registration means that every stage of our quality system, including product development, manufacturing, final test, shipping, and parts and supplies has been rigorously examined against the most exacting set of internationally recognized standards. It means we live up to a standard of quality that you can count on today, and into the future. Our Quality System has received ISO 9001 certification number FM21797. The quality systems that earned us ISO 9001 registration have direct benefits for our customers: ♦ We can speed instruments to you faster than ever before. Emergency orders can be processed even faster. ♦ We fill your orders promptly and completely. ♦ We have implemented a system of continuous feedback from our customers — we are aware of your needs today and tomorrow. ♦ We have improved your productivity by cutting systems failure rates in half and speeding service response time. ♦ We have embedded continuous improvement into the fabric of our organization so that we can achieve even higher levels of quality in the future. ♦ We are embedding GLP requirements into our products and services to help you meet your regulatory compliance requirements. ISO 9001 registration is not enough. For us, quality is defined by our customers. We are not satisfied unless you are satisfied. We are striving to understand customer needs, using independent surveys, user groups, customer advisory boards, and our “Hallmark of Quality” response program, in addition to individual face-to-face customer contact. Our products and our processes are configured to meet those needs. We know that you are seeking more than the most advanced processes and top-notch applications expertise. You want to join forces with a partner committed to delivering world-class quality, reliability, and value — on time, every time. Our overriding aim is to be that partner. 03-914451-00:4 1 of 1 Varian, Inc. Analytical Instrument Warranty Hardware Products All analytical instruments sold by Varian, Inc. are warranted to be free from defects in material and workmanship for the periods specified and in accordance with the terms on the face of Varian's quotation or as otherwise agreed upon in writing between Varian and the Customer. The warranty period begins on the date of shipment from Varian to the original Customer. However, where installation is paid for by the Customer or included in the purchase price, the warranty period begins upon completion of installation. If the Customer schedules installation to start later than 30 days after delivery or if such delay is caused through the Customer's inability to provide adequate facilities or utilities or through failure to comply with Varian's reasonable pre-installation instructions or through other omissions by Customer, then the warranty period starts on the 31st day from date of shipment. Moreover Varian will charge the Customer for labor and other expenses involved in making multiple or follow-up installation service calls. Software Products Where software is provided within the frame of a license agreement concluded between the Customer and Varian, any warranty shall be strictly in accordance with the terms of such agreement. In the absence of a license agreement and unless an alternate warranty period is agreed upon in writing between Varian and the Customer, the warranty period is as specified on the face of Varian's quotation. Varian warrants such software products, if used with and properly installed on Varian hardware or other hardware as specified by Varian to perform as described in the accompanying Operator's Manual and to be substantially free of those defects which cause failure to execute respective programming instructions; however, Varian does not warrant uninterrupted or error-free operation. Remedies The sole and exclusive remedy under hardware warranty shall be repair of instrument malfunctions which in Varian's opinion are due or traceable to defects in original materials or workmanship or, at Varian's option, replacement of the respective defective parts, provided that Varian may as an alternative elect to refund an equitable portion of the purchase price of the instrument or accessory. Repair or replacement under warranty does not extend the original warranty period. 03-914412-00:2 Repair or replacement under warranty claims shall be made in Varian's sole discretion either by sending a Customer Support Representative to the site or by authorizing the Customer to return the defective accessory or instrument to Varian or to send it to a designated service facility. The Customer shall be responsible for loss or damage in transit and shall prepay shipping cost. Varian will return the accessory or instrument to the Customer prepaid and insured. Claims for loss or damage in transit shall be filed by the Customer. To correct software operation anomalies, Varian will issue software revisions where such revisions exist and where, in Varian's opinion, this is the most efficient remedy. Limitation of Warranty This warranty does not cover software supplied by the Customer, equipment and software warranted by another manufacturer or replacement of expendable items and those of limited life, such as but not limited to: Filters, glassware, instrument status lamps, source lamps, septa, columns, fuses, chart paper and ink, nebulizers, flow cells, pistons, seals, fittings, valves, burners, sample tubes, probe inserts, print heads, glass lined tubing, pipe and tube fittings, variable temperature dewars, transfer lines, flexible discs, magnetic tape cassettes, electron multipliers, filaments, vacuum gaskets, seats and all parts exposed to samples and mobile phases. This warranty shall be void in the event of accident, abuse, alteration, misuse, neglect, breakage, improper operation or maintenance, unauthorized or improper modifications or tampering, use in an unsuitable physical environment, use with a marginal power supply or use with other inadequate facilities or utilities. Reasonable care must be used to avoid hazards. This warranty is expressly in lieu of and excludes all other express or implied warranties, including but not limited to warranties of merchantability and of fitness for particular purpose, use or application, and all other obligations or liabilities on the part of Varian, unless such other warranties, obligations or liabilities are expressly agreed to in writing by Varian. Limitation of Remedies and Liability The remedies provided herein are the sole and exclusive remedies of the Customer. In no case will Varian be liable for incidental or consequential damages, loss of use, loss of production or any other loss incurred. 1 of 1 Safety Information Operating Instructions This instruction manual is provided to help you establish operating conditions which will permit safe and efficient use of your equipment. Special considerations and precautions are also described in the manual, which appear in the form of NOTES, CAUTIONS, and WARNINGS as described below. It is important that you operate your equipment in accordance with this instruction manual and any additional information which may be provided by Varian. Address any questions regarding the safe and proper use of your equipment to your local Varian office. NOTE Information to aid you in obtaining optimal performance from your instrument. Warning Symbol Alerts you to situations that may cause moderate injury and/or equipment damage, and how to avoid these situations. Alerts you to potentially hazardous situations that could result in serious injury, and how to avoid these situations. Warning Description Hazardous voltages are present inside instrument. Disconnect from main power before removing screw-attached panels. Hazardous chemicals may be present. Avoid contact, especially when replenishing reservoirs. Use proper eye and skin protection. Very hot or cryogenically cold surfaces may be exposed. Use proper skin protection. Eye damage could occur either from flying particles, chemicals, or UV radiation. Use proper eye and face protection. The potential for fire may be present. Follow manual instructions for safe operation. The potential for explosion may exist because of type of gas or liquid used. Ionizing radiation source is present. Follow manual instructions for safe operation. Keep hands and fingers away. 03-914603-00:10 1 of 4 General Safety Precautions Follow these safety practices to ensure safe equipment operation. „ Perform periodic leak checks on all supply lines and pneumatic plumbing. „ Do not allow gas lines to become kinked or punctured. Place lines away from foot traffic and extreme heat or cold. „ Store organic solvents in fireproof, vented and clearly labeled cabinets so they are easily identified as toxic and/or flammable materials. „ Do not accumulate waste solvents. Dispose of such materials through a regulated disposal program and not through municipal sewage lines. NOTICE: This instrument has been tested per applicable requirements of EMC Directive as required to carry the European Union CE Mark. As such, this equipment may be susceptible to radiation/interference levels or frequencies which are not within the tested limits. This instrument is designed for chromatographic analysis of appropriately prepared samples. It must be operated using appropriate gases and/or solvents and within specified maximum ranges for pressure, flows, and temperatures as described in this manual. If the equipment is used in a manner not specified by the manufacturer, the protection provided by the equipment may be impaired. It is the responsibility of the Customer to inform Varian Customer Support Representatives if the instrument has been used for the analysis of hazardous biological, radioactive, or toxic samples, prior to any instrument service being performed or when an instrument is being returned to the Service Center for repair. Electrical Hazards „ Disconnect the instrument from all power sources before removing protective panels to avoid exposure to potentially dangerous voltages. „ When it is necessary to use a non-original power cord plug, make sure the replacement cord adheres to the color coding and polarity described in the manual and all local building safety codes. „ Replace blown fuses with fuses of the size and rating stipulated on the fuse panel or in the manual. „ Replace faulty or frayed power cords immediately with the same type and rating. „ Make sure that voltage sources and line voltage match the value for which the instrument is wired. Compressed Gas Cylinders 2 of 4 „ Store and handle compressed gases carefully and in strict adherence to safety codes. „ Secure cylinders to an immovable structure or wall. „ Store and move cylinders in an upright, vertical position. Before transport, remove regulators and install cylinder cap. „ Store cylinders in a well-ventilated area away from heat, direct sunshine, freezing temperatures, and ignition sources. „ Mark cylinders clearly so there is no doubt as to their contents. „ Use only approved regulators and connections. „ Use only connector tubing that is chromatographically clean (Varian Part Number 03-918326-00) and has a pressure rating significantly greater than the highest outlet pressure from the regulator. 03-914603-00:10 GC Safety Practices Flash Chromatography Exhaust System The operator should be familiar with the physicochemical properties of the components of the mobile phase. No special exhaust ducting is necessary for GC detectors installed in a well-ventilated room except when the detectors are used to test hazardous chemicals. If you do install ducting: „ Use only fireproof ducting. „ Install a blower at the duct outlet. „ Locate duct intakes such that their vibration or air movement does not effect detector operation. „ Check periodically for proper operation of the duct. „ Ensure proper ventilation in lab area. Radioactive Source Detectors „ „ „ Read carefully and comply with all NOTES, CAUTIONS, and WARNINGS in the Ni63 ECD manual. Perform the tests for removable radioactive contamination described in the Ni63 ECD manual. Comply with leak test schedules and procedures. Burn Hazard Heated or cryogenically cooled zones of gas chromatographs can remain hot or cold for a considerable time after instrument power is turned off. To prevent painful burns, ensure that all heated or cooled areas have returned to room temperature or wear adequate hand protection before you touch potentially hot or cold surfaces. LC Safety Practices Keep solvents from direct contact with the polyurethane supply tubing as certain solvents will cause weakening and leaks with possible bursting. All components of the system should be connected to a common power supply and common ground. This ground must be a true ground rather than a floating ground. Non-polar solvents can develop a static charge when pumped through the system. All vessels that contain mobile phase (including tubing and collection vessels) must be grounded to dissipate static electricity. Employ static measuring and static discharge devices (e.g., air ionizers) to safeguard against the buildup of static electricity. Ultraviolet Radiation Liquid chromatograph detectors that use an ultraviolet light source have shielding to prevent radiation exposure to personnel. For continued protection: „ „ Ensure that protective lamp covers of variable and fixed wavelength detectors are in place during operation. Do not look directly into detector fluid cells or at the UV light source. When inspecting the light source or fluid cell, always use protective eye covering such as borosilicate glass or polystyrene. High Pressure Hazard • „ „ „ „ „ If a line ruptures, a relief device opens, or a valve opens accidentally under pressure, potentially hazardous high liquid pressures can be generated by the pump causing a high velocity stream of volatile and/or toxic liquids. Wear face protection when you inject samples or perform routine maintenance. Never open a solvent line or valve under pressure. Stop the pump first and let the pressure drop to zero. Use shatter-proof reservoirs capable of operating at 50-60 psi. Keep the reservoir enclosure closed when the reservoir is under pressure. Read and adhere to all NOTES, CAUTIONS, and WARNINGS in the manual. 03-914603-00:10 The following is a Federal Communications Commission advisory: This equipment has been tested and found to comply with the limits of a Class A computing device, pursuant to part 15 of the FCC Rules. These limits are designed to provide reasonable protection against harmful interference when the equipment is operated in a commercial environment. This equipment generates, uses, and can radiate radio frequency energy and, if not installed and used in accordance with the instruction manual, may cause harmful interference to radio communications. Operation of this equipment in a residential area is likely to cause harmful interference in which case the user will be required to correct the interference at his own expense. 3 of 4 Spare Parts Availability Service Availability It is the policy of Varian to provide operational spare parts for any instrument and major accessory for a period of five (5) years after shipment of the final production run of that instrument. Spare parts will be available after this five (5) year period but on an as available basis. Operational spare parts are defined as those individual electrical or mechanical parts that are susceptible to failure during their normal operation. Examples include relays, lamps, temperature probes, detector elements, motors, etc. Sheet metal parts, structural members or assemblies and castings, printed circuit boards, and functional modules are normally capable of being rebuilt to like-new condition throughout their useful life and therefore will be supplied only on an as available basis after the final production run of the instrument. Varian provides a variety of services to support its customers after warranty expiration. Repair service can be provided by attractively priced service contracts or on a time and material basis. Technical support and training can be provided by qualified personnel on both a contractual or asneeded basis. Varian, Inc. Analytical Instruments Sales Offices For Sales or Service assistance and to order Parts and Supplies, contact your local Varian office. Argentina Buenos Aires Tel. +54.11.4.783.5306 France Les Ulis Cédex Tel. +33.1.6986.3838 Spain Madrid Tel. +34.91.472.7612 Australia Mulgrave, Victoria Tel. +61.3.9566.1134 Germany Darmstadt Tel. +49.6151.7030 Sweden Solna Tel. +46.8.445.1620 Austria Vösendorf bei Wien Tel. +43.1.699.9669 India Mumbai Tel. +91.22.857.0787/88/89 Switzerland Varian AG Tel. +41.848.803.800 Benelux Bergen Op Zoom Tel. +31.164.282.800 Italy Torino Tel. +39.011.997.9111 Taiwan Taipei Hsien Tel. +886.2.698.9555 Brazil and Latin America (S) São Paulo Tel. +55.11.820.0444 Japan Tokyo Tel. +81.3.5232.1211 Canada Mississauga, Ontario Tel. 800.387.2216 Korea Seoul Tel. +82.2.345.22452 United Kingdom and Ireland Walton-on-Thames Tel. +44.1932.898000 China Beijing Tel. +86.106209.1727 Mexico and Latin America (N) Mexico City Tel. +52.5.523.9465 Europe Middelburg, The Netherlands Tel. +31.118.671.000 Russian Federation Moscow Tel. +7.095.937.4280 4 of 4 Venezuela Valencia Tel. +58.41.257.608 United States Walnut Creek, California, USA Tel. +1.800.926.3000 (GC and GC/MS) Tel. +1.800.367.4752 (LC) www.varianinc.com 03-914603-00:10 Sicherheitsinformationen Arbeitsanleitungen Diese Arbeitsanleitung will Ihnen bei der Aufstellung solcher Arbeitsbedingungen helfen, die einen sicheren und wirkungsvollen Gebrauch Ihrer Geräte ermöglichen. Besondere Überlegungen und Vorsichtsmaßnahmen erscheinen in diesem Handbuch in Form von HINWEIS, ACHTUNG und WARNUNG, wie unten beschrieben. Es ist wichtig, daß Sie Ihr Gerät in Übereinstimmung mit dieser Arbeitsanleitung und allen möglichen zusätzlichen Informationen von Varian betreiben. Alle Fragen bezüglich Sicherheit und Handhabung Ihres Gerätes richten Sie an Ihr Varian Büro. HINWEIS Eine Information, um einen optimalen Wirkungsgrad Ihres Instruments zu erzielen. Warnungssymbol WARNUNG ELEKTRISCHER SCHLAG ACHTUNG Weist auf Situationen, die zu mäßiger Beeinträchtigung und/oder zu Geräteschäden führen und auf die Vermeidung dieser Situationen hin. WARNUNG Weist auf mögliche Gefahrensituationen, die zu ernsthaften Verletzungen führen können und auf die Vermeidung dieser Situationen hin. Warnungsbeschreibung Gefährliche Spannungen bestehen innerhalb des Instruments. Trennen Sie das Gerät vom Netz, bevor Sie abschraubbare Paneele entfernen. Gefährliche Chemikalien können vorhanden sein. Vermeiden Sie jeden Kontakt, besonders beim Auffüllen der Reservoirs. Benutzen Sie wirksamen Augen und Hautschutz. WARNUNG Sehr heiße oder tiefstgekühlte Oberflächen können freigelegt sein. Benutzen VERBRENNUNGSGEFAHR Sie einen wirksamen Hautschutz. Herumfliegende Partikel, Chemikalien oder UV-Strahlung können Augenschäden verursachen. Tragen Sie deshalb einen geeigneten Schutz für Augen und Gesicht. WARNUNG FEUERGEFAHR WARNUNG EXPLOSIONSGEFAHR WARNUNG STRAHLUNGSQUELLE WARNUNG BEWEGTE TEILE 03-914603-81:10 Es besteht eine mögliche Feuergefahr. Beachten Sie die Vorschriften im Handbuch für eine gefahrlose Benutzung. Eine mögliche Explosionsgefahr besteht infolge der benutzten Gas- oder Flüssigkeitsart. Es besteht eine ionisierende Strahlungsquelle. Beachten Sie die Vorschriften im Handbuch für eine gefahrlose Benutzung. Bleiben Sie mit Ihren Händen und Fingern weg. 1 of 4 Allgemeine Sicherheitsmaßnahmen Befolgen Sie diese Sicherheitspraktiken für eine gefahrlose Gerätebenutzung. „ Prüfen Sie regelmäßig alle Versorgungs und Pneumatikleitungen auf Lecks. „ Gasleitungen dürfen nicht geknickt oder angestochen werden. Verlegen Sie die Leitungen außerhalb von Laufwegen und abseits von extremer Hitze oder Kälte. „ Lagern Sie organische Lösungsmittel in feuerfesten, belüfteten und eindeutig bezeichneten Schränken, damit sie leicht als toxische und/oder brennbare Materialien erkannt werden. „ Sammeln Sie keine Lösungsmittelabfälle. Entsorgen Sie solche Materialien über ein geregeltes Entsorgungsprogramm und nicht über die öffentlichen Abwasserleitungen. HINWEIS: Dies Instrument wurde nach den zutreffenden Vorschriften der EMC Direktive getestet, die zum Führen des CE Zeichens der Europäischen Union berechtigen. Dieses Gerät kann an sich auf Strahlungs-/Störpegel oder Frequenzen außerhalb der getesteten Grenzen reagieren. Dies Instrument ist für chromatographische Analysen entsprechend präparierter Proben ge- WARNUNG dacht. Es muß mit geeigneten Gasen und/oder Lösungsmitteln und innerhalb der im Handbuch spezifizierten maximalen Werte für Druck, Flüsse und Temperaturen betrieben werden. Der Kunde ist vor der Durchführung irgendeines Geräteservices verpflichtet den Varian WARNUNG Kundendienstvertreter zu informieren, wenn das Instrument für Analysen gefährlicher biologischer, radioaktiver oder toxischer Proben benutzt worden ist. Elektrische Gefahren „ Lösen Sie das Instrument von allen Stromquellen, bevor Sie Schutzpaneele entfernen, damit Sie nicht mit potentiell gefährlichen Spannungen in Berührung kommen. „ Wenn ein Nicht-Original Netzkabelstecker benutzt werden muß, muß das Austauschkabel die im Handbuch beschriebene Farbcodierung und Polarität beibehalten und alle örtlichen Sicherheitsvorschriften erfüllen. „ Ersetzen Sie durchgebrannte Sicherungen nur mit Sicherungen der Werte, die am Sicherungspaneel oder im Handbuch angegeben sind. „ Ersetzen Sie fehlerhafte oder durchgescheuerte Netzkabel sofort durch Kabel gleicher Art. „ Sorgen Sie dafür, daß Spannungsquellen und die Netzspannung den gleichen Wert haben, für den das Instrument verdrahtet ist. Gasdruckflaschen „ Lagern und handhaben Sie komprimierte Gase vorsichtig und in strikter Einhaltung der Sicherheitsvorschriften. „ Befestigen Sie die Gasflaschen an feststehenden Aufbauten oder an Wänden. „ Lagern und transportieren Sie Gasflaschen in aufrechter Stellung. Druckregler zuvor abnehmen. „ Lagern Sie Gasflaschen in gut durchlüfteten Räumen, weit genug weg von Heizungen, direktem Sonnenschein, Frosttemperaturen und Entzündungszonen. „ Kennzeichnen Sie die Flaschen so eindeutig, daß kein Zweifel über deren Inhalt bestehen kann. „ Benutzen Sie nur geprüfte Druckminderer und Verbindungsstücke. „ Benutzen Sie nur chromatographisch reines Verbindungsrohr (Varian Part Number 03-918326-00), das wesentlich höheren Druck als den höchsten Ausgangsdruck des Druckminderers aushält. 2 of 4 03-914603-81:10 GC Sicherheitspraktiken „ Öffnen Sie niemals eine unter Druck stehende Lösungsmittelleitung oder ein Ventil. Halten Sie zuerst die Pumpe an und lassen Sie den Druck auf Null abfallen. „ Benutzen Sie splittersichere Reservoirs, die für einen Druck von 3,4 bis 4,1 bar ausgelegt sind. „ Halten Sie die Reservoirverkleidung geschlossen, wenn die Reservoirs unter Druck stehen. „ Lesen Sie und befolgen Sie alle HINWEISE, ACHTUNGEN und WARNUNGEN im Handbuch. Abgassystem Für GC Detektoren, die in einem gut durchlüfteten Raum installiert sind, ist keine spezielle Abgasführung erforderlich, außer wenn die Detektoren zum Testen gefährlicher Chemikalien benutzt werden. Wenn Sie eine Abgasführung installieren: „ Benutzen Sie nur feuerfeste Führungen. „ Installieren Sie ein Gebläse am Ausgang. „ Ordnen Sie die Ansaugöffnung so an, daß ihre Erschütterungen oder Luftströmungen nicht die Detektorfunktion beeinträchtigen. „ Prüfen Sie regelmäßig die einwandfreie Arbeitsweise der Abgasführung. „ Sorgen Sie für gute Entlüftung im Laborbereich. Radioaktive Detektoren „ Lesen Sie sorgfältig und befolgen Sie alle HINWEISE, ACHTUNGEN und WARNUNGEN im Ni63 ECD Handbuch. „ Führen Sie die Tests für zu beseitigende radioaktive Kontamination durch, die im Ni63 ECD Handbuch beschrieben sind. „ Erfüllen Sie die Zeitpläne und Verfahren zur Dichtigkeitsprüfung. Verbrennungsgefahr Beheizte oder tieftemperaturgekühlte Zonen des Gaschromatographen können beträchtlich lange heiß oder kalt bleiben, nachdem das Instrument bereits abgeschaltet ist. Zur Vermeidung schmerzhafter Verbrennungen müssen Sie darauf achten, daß alle beheizten oder gekühlten Zonen auf Raumtemperatur zurückgegangen sind oder Sie müssen ausreichenden Handschutz benutzen, bevor Sie möglicherweise heiße oder kalte Oberflächen berühren. LC Sicherheitspraktiken Gefahr durch hohen Druck Wenn eine Leitung bricht, eine Entlüftungseinheit sich öffnet oder ein Ventil sich unbeabsichtigt unter Druck öffnet, kann durch die Pumpe möglicherweise ein gefährlich hoher Flüssigkeitsdruck entstehen, der einen Strahl flüchtiger und/oder toxischer Flüssigkeiten von hoher Stömungsgeschwindigkeit verursacht. „ Tragen Sie einen Gesichtsschutz, wenn Sie Proben injizieren oder Routinewartungen durchführen. 03-914603-81:10 Blitzlicht-Chromatographie Der Bediener sollte mit den physikalisch-chemischen Eigenschaften der Komponenten vertraut sein, aus denen sich die mobile Phase zusammensetzt. Vermeiden Sie direkten Kontakt der Lösungsmittel mit den Zuführungsleitungen aus Polyurethan, da einige Lösungsmittel das Material der Leitungen schwächen und damit Undichtigkeiten oder Brüche hervorrufen können. Alle Systemkomponenten sollten an der gleichen Netzstromquelle und einer gemeinsamen Erdung angeschlossen sein. Dabei muss es sich um eine echte, nicht um eine schwebende Erdung handeln. Nicht-polare Lösungsmittel können sich beim Pumpen durch das System statisch aufladen. Alle Gefäße, die mobile Phase enthalten (einschließlich Leitungen und Sammelgefäße), müssen zur Ableitung elektrostatischer Aufladungen geerdet sein. Setzen Sie Geräte zur Messung und Ableitung elektrostatischer Aufladungen (z.B. Geräte zur Luftionisierung) als Maßnahmen gegen den Aufbau statischer Elektrizität ein. Ultraviolette Strahlung Detektoren in Liquidchromatographen, die eine ultraviolette Lichtquelle benutzen, besitzen eine Abschirmung, die das Bedienungspersonal gegen Abstrahlungen schützt. Zum ständigen Schutz: „ Achten Sie darauf, daß die schützende Lampenabdeckung der Detektoren mit variablen und festen Wellenlängen während des Betriebs an ihrem Platz ist. „ Schauen Sie nicht direkt in die Flüssigkeitszellen im Detektor oder in die UV Lampe. Zum Inspizieren der Lichtquelle oder der Flüssigkeitszelle benutzen Sie immer einen wirksamen Augenschutz, wie er durch Borsilikatglas oder Polystyrol gewährleistet wird. 3 of 4 Verfügbarkeit von Ersatzteilen Serviceverfügbarkeit Es ist Varian’s Grundsatz, Ersatzteile für alle Instrumente und die wichtigsten Zubehöre für einen Zeitraum von fünf (5) Jahren nach dem Fertigungsauslauf dieser Geräteserie verfügbar zu haben. Nach diesem Zeitraum von fünf (5) Jahren können Ersatzteile auf der Basis solange vorhanden bezogen werden. Als Ersatzteil werden hier solche elektrischen und mechanischen Einzelteile verstanden, die unter normalen Bedingungen ausfallen können. Beispiele sind Relais, Lampen, Temperaturfühler, Detektorelemente, Motore usw. Metallbleche, Formteile oder Baugruppen und Gußteile, PC Boards und Funktionsmodule können normalerweise neuwertähnlich für eine brauchbare Lebensdauer instandgesetzt werden und werden deshalb nur auf der Basis solange vorhanden nach dem Produktionsauslauf des Instruments geliefert werden. Varian bietet seinen Kunden auch nach dem Auslaufen der Garantie eine Vielfalt von Serviceleistungen an. Reparaturservice kann zu attraktiven Preisen über eine Wartungsvereinbarung oder nach Zeit- und Materialaufwand zur Verfügung gestellt werden. Technische Unterstützung und Training bieten wir Ihnen durch qualifizierte Chemiker sowohl auf einer Kontraktbasis als auch nach Ihren Erfordernissen an. Varian Analytical Instruments Verkaufsbüros Für Verkaufs oder Servicehilfe und zum Bestellen von Teilen und Zubehören setzen Sie sich bitte mit Ihrem Varian Büro in Verbindung. Argentina Buenos Aires Tel. +54.11.4.783.5306 France Les Ulis Cédex Tel. +33.1.6986.3838 Spain Madrid Tel. +34.91.472.7612 Australia Mulgrave, Victoria Tel. +61.3.9566.1134 Germany Darmstadt Tel. +49.6151.7030 Sweden Solna Tel. +46.8.445.1620 Austria Vösendorf bei Wien Tel. +43.1.699.9669 India Mumbai Tel. +91.22.857.0787/88/89 Switzerland Varian AG Tel. +41.848.803.800 Benelux Bergen Op Zoom Tel. +31.164.282.800 Italy Torino Tel. +39.011.997.9111 Taiwan Taipei Hsien Tel. +886.2.698.9555 Brazil and Latin America (S) São Paulo Tel. +55.11.820.0444 Japan Tokyo Tel. +81.3.5232.1211 Canada Mississauga, Ontario Tel. 800.387.2216 Korea Seoul Tel. +82.2.345.22452 United Kingdom and Ireland Walton-on-Thames Tel. +44.1932.898000 China Beijing Tel. +86.106209.1727 Mexico and Latin America (N) Mexico City Tel. +52.5.523.9465 Europe Middelburg, The Netherlands Tel. +31.118.671.000 Russian Federation Moscow Tel. +7.095.937.4280 4 of 4 United States Walnut Creek, California, USA Tel. +1.800.926.3000 (GC and GC/MS) Tel. +1.800.367.4752 (LC) www.varianinc.com Venezuela Valencia Tel. +58.41.257.608 03-914603-81:10 Informations et mesures de sécurité Instructions de fonctionnement Ce manuel d’instruction est conçu pour aider l’utilisateur à créer des conditions opératoires lui permettant de faire fonctionner le matériel efficacement et en toute sécurité. Il contient entre autres certaines observations spéciales présentées sous forme de NOTES, MISES EN GARDE et AVERTISSEMENTS. Il est important de faire fonctionner ce matériel conformément aux instructions du présent manuel et à toute autre information émanant de Varian. S’adresser au bureau régional Varian pour toute question relative à la sécurité ou à l’utilisation correcte du matériel. NOTE Information destinée à tirer le meilleur parti du matériel sur le plan des performances Symboles d’avertissement ATTENTION RISQUE D'ELECTROCUTION Attire l’attention sur une situation pouvant occasionner des dommages corporels légers et/ou des dégâts mineurs à l’appareil et indique comment remédier à cette situation Attire l’attention sur une situation potentiellement dangereuse pouvant occasionner des dommages corporels importants et indique comment remédier à cette situation Description Exposition à des tensions dangereuses. Débrancher le matériel du secteur avant de dévisser les panneaux protecteurs. Présence éventuelle de substances chimiques dangereuses. Eviter tout contact, en particulier lors du remplissage des réservoirs. Prendre les mesures de protection adéquates pour les yeux et la peau. ATTENTION RISQUE DE BRÛLURES Exposition à des surfaces chaudes ou traitées cryogéniquement. Prendre les mesures de protection adéquates pour la peau. Les dommages causées aux yeux sont de deux natures différentes : jet de particules et de produits chimiques ou radiations UV. Utiliser des protections du visage et des yeux appropriées. RISQUE D'INCENDIE Risque potentiel d’incendie. Se conformer aux instructions du manuel pour faire fonctionner le matériel en toute sécurité. ATTENTION Risque potentiel d’explosion en raison du type de gaz ou de liquide utilisé. ATTENTION RISQUE D'EXPLOSION ATTENTION SOURCE DE RADIATION ATTENTION PIECES EN MOUVEMENT 03-914603-82:10 Présence d’une source de radiation ionisante. Se conformer aux instructions du manuel pour faire fonctionner le matériel en toute sécurité. Garder les mains et les doigts hors de portée. 1 of 4 Précautions générales en matière de sécurité Les pratiques suivantes garantissent une utilisation sans risques du matériel: „ „ „ „ Effectuer régulièrement des essais d’étanchéité de tous les conduits d’alimentation et de tous les tuyaux du système pneumatique. Ne pas travailler avec des conduits de gaz déformés ou percés. Installer les conduits de gaz à l’écart des allées et venues et à l’abri du chaud ou du froid. Conserver les solvants organiques dans des récipients à l’épreuve du feu, bien ventilés et portant mention de la nature de leur contenu, en particulier lorsque lesdits solvants sont toxiques et/ou inflammables. Ne pas accumuler les solvants de rebut. Les éliminer conformément à un programme agréé d’élimination des déchets et non via les égouts municipaux. NOTE: Ce matériel a été testé conformément aux dispositions de la directive CME afin de pouvoir porter le sigle CE de l’Union européenne. Il en résulte qu’il peut être sensible à des niveaux de radiation/d’interférence ou à des fréquences se situant hors des limites testées. Ce matériel est conçu pour effectuer des analyses chromatographiques d’échantillons ATTENTION préparés selon des méthodes appropriées. Il convient de le faire fonctionner avec les gaz et/ou les solvants adéquats et dans les limites des pressions, des débits et des températures maximales spécifiées dans le présent manuel. Le client est tenu d’informer le service Varian d’assistance à la clientèle que son matériel ATTENTION a été utilisé pour l’analyse d’échantillons biologiques dangereux, radioactifs ou toxiques avant que n’en soit effectué la maintenance. Risques de chocs électriques „ „ „ „ „ Déconnecter le matériel de toute source d’alimentation avant d’en démonter les panneaux de protection, sous peine de s’exposer à des tensions dangereuses. En cas d’utilisation d’un cordon d’alimentation n’étant pas d’origine, s’assurer que celui-ci soit conforme à la polarité et au codage des couleurs décrits dans le manuel d’utilisation ainsi qu’à toutes les normes régionales de sécurité régissant le secteur de la construction. Remplacer les fusibles sautés par des fusibles de même type que ceux stipulés sur le panneau des fusibles ou dans le manuel d’utilisation. Remplacer les cordons d’alimentation défectueux ou dénudés par des cordons d’alimentation de même type. S’assurer que les sources de tension et la tension de secteur correspondent à la tension de fonctionnement du matériel. Bouteilles à gaz comprimé „ „ „ „ „ „ „ 2 of 4 Ranger et manipuler les bouteilles à gaz comprimé avec précaution et conformément aux normes de sécurité. Fixer les bouteilles à gaz comprimé à un mur ou à une structure inamovible. Ranger et déplacer les bouteilles à gaz comprimé en position verticale. Avant de transporter les bouteilles à gaz comprimé, retirer leur régulateur. Ranger les bouteilles dans un endroit bien ventilé et à l’abri de la chaleur, des rayons directs du soleil, du gel ou des sources d’allumage. Marquer les bouteilles de manière à n’avoir aucun doute quant à leur contenu. N’utiliser que des connexions et régulateurs agréés. N’utiliser que des tuyaux de raccordement propres sur le plan chromatographique (Varian P/N 03-918326-00) et pouvant supporter des pressions sensiblement plus élevées que la plus haute pression de sortie du régulateur. 03-914603-82:10 Mesures de sécurité en CPG „ Ne jamais déconnecter un conduit de solvant ou une vanne sous pression. Arrêter préalablement la pompe et laisser la pression descendre à zéro. „ Utiliser des réservoirs incassables à 50-60 psi. „ Laisser l’enceinte du réservoir fermée lorsque le réservoir est sous pression. „ Se conformer aux NOTES, MISES EN GARDE ET AVERTISSEMENTS du manuel d’utilisation. Système d’échappement Les détecteurs CPG installés dans une pièce bien ventilée ne nécessitent pas de conduits spéciaux d’échappement excepté lorsqu’ils sont destinés à analyser des substances chimiques dangereuses. Lors de l’installation de tels conduits: „ N’utiliser que des conduits à l’épreuve du feu „ Installer un ventilateur à la sortie du conduit. „ Placer les orifices d’aspiration de manière à ce que les vibrations ou les mouvements d’air n’affectent pas le fonctionnement du détecteur. Chromatographie Flash „ Vérifier périodiquement l’état du conduit. „ S’assurer que le laboratoire est correctement ventilé. Eviter le contact direct des solvants avec les tuyaux en polyuréthane : certains solvants sont susceptibles de provoquer des faiblesses et des fuites avec risques d’explosion. Détecteurs à source radioactive „ Se conformer au manuel d’utilisation de l’ECD Ni63, en particulier à ses NOTES, MISES EN GARDE ET AVERTISSEMENTS. „ Effectuer les tests de décontamination radioactive décrits dans le manuel d’utilisation de l’ECD Ni63. „ Se conformer aux procédures et au calendrier des essais d’étanchéité. Risque de brûlures Les zones des chromatographes à gaz chauffées ou traitées cryogéniquement peuvent rester très chaudes ou très froides durant une période plus ou moins longue après la mise hors tension du matériel. Pour éviter les brûlures, s’assurer que ces zones sont revenues à température ambiante ou utiliser un dispositif adéquat de protection des mains avant de les toucher. Mesures de sécurité en CPL Risques liés aux hautes pressions En cas de rupture d’un tuyau ou en cas d’ouverture accidentelle d’une vanne alors que le système est sous pression, la pompe peut occasionner des dommages en expulsant à grande vitesse des jets de liquides volatiles et/ou toxiques. „ Mettre un masque de protection lors de l’injection des échantillons ou en effectuant les opérations de maintenance de routine. 03-914603-82:10 L’utilisateur aura la connaissance des propriétés physico-chimiques des constituants de la phase mobile. Tous les constituants du système devront être connectés à une source de courant commune et à une prise de terre commune. Cette prise de terre devra être fixe et non mobile. Les solvants non-polaires peuvent produire de l’électricité statique lorsqu’ils passent au travers du système. Les bouteilles qui contiennent la phase mobile (incluant les tuyaux et les flacons de collecte de fractions) doivent être mises à la terre pour éliminer l’électricité statique. Utiliser des appareils de mesure et de décharge d’électricité statique (par exemple des ionisateurs d’air) pour combattre la formation d’électricité statique. Radiations ultraviolettes Les détecteurs CPL utilisant une source lumineuse ultraviolette comportent un écran destiné à se prémunir contre les expositions aux rayonnements. Pour s’assurer une protection permanente: „ Vérifier que le couvercle de protection de la lampe des détecteurs opérant à des longueurs d’onde variables et fixes soit bien en place durant le fonctionnement du matériel. „ Ne pas regarder directement les cellules du détecteur ou la source d’UV. Se protéger systématiquement les yeux lors du contrôle de la source lumineuse ou des cellules, par exemple au moyen de verres borosilicatés ou en polystyrène. 3 of 4 Disponibilité des pièces de rechange La politique de Varian consiste à fournir des pièces de rechange pour tous les appareils et accessoires majeurs durant une période de cinq (5) ans après livraison de leur production finale. Les pièces de rechange ne sont fournies au terme de cette période de cinq (5) ans que suivant les disponibilités. Il faut entendre par pièces de rechange les pièces individuelles électriques ou mécaniques susceptibles de défaillance au cours de leur utilisation normale. Par exemple, les relais, les lampes, les sondes thermiques, les éléments de détecteur, les moteurs, etc. Les parties en tôles, les éléments ou assemblages structurels et les pièces de fonderie, les cartes à circuits imprimés et les modules fonctionnels sont normalement susceptibles d’être remis à l’état neuf pendant toute la durée de leur vie utile et ne sont dès lors fournies, au terme de la production finale des appareils, que suivant les disponibilités. Service d’assistance à la clientèle Varian fournit divers services destinés à aider sa clientèle après expiration de la garantie: service de réparation sur base de contrats de maintenance à prix attractifs ou sur base d’accords à durée limitée portant sur du matériel spécifique; support technique et service de formation assurés par des chimistes qualifiés sur base contractuelle ou en fonction des besoins spécifiques. Points de vente des instruments analytiques Varian Contactez votre point de vente régional Varian pour toute question commerciale ou de service d’assistance à la clientèle ou pour passer commande de pièces et de fournitures. Argentina Buenos Aires Tel. +54.11.4.783.5306 France Les Ulis Cédex Tel. +33.1.6986.3838 Spain Madrid Tel. +34.91.472.7612 Australia Mulgrave, Victoria Tel. +61.3.9566.1134 Germany Darmstadt Tel. +49.6151.7030 Sweden Solna Tel. +46.8.445.1620 Austria Vösendorf bei Wien Tel. +43.1.699.9669 India Mumbai Tel. +91.22.857.0787/88/89 Switzerland Varian AG Tel. +41.848.803.800 Benelux Bergen Op Zoom Tel. +31.164.282.800 Italy Torino Tel. +39.011.997.9111 Taiwan Taipei Hsien Tel. +886.2.698.9555 Brazil and Latin America (S) São Paulo Tel. +55.11.820.0444 Japan Tokyo Tel. +81.3.5232.1211 Canada Mississauga, Ontario Tel. 800.387.2216 Korea Seoul Tel. +82.2.345.22452 United Kingdom and Ireland Walton-on-Thames Tel. +44.1932.898000 China Beijing Tel. +86.106209.1727 Mexico and Latin America (N) Mexico City Tel. +52.5.523.9465 Europe Middelburg, The Netherlands Tel. +31.118.671.000 Russian Federation Moscow Tel. +7.095.937.4280 4 of 4 United States Walnut Creek, California, USA Tel. +1.800.926.3000 (GC and GC/MS) Tel. +1.800.367.4752 (LC) www.varianinc.com Venezuela Valencia Tel. +58.41.257.608 03-914603-82:10 Informazioni sulla Sicurezza Instruzioni per l’Uso Questo manuale ha lo scopo di aiutare l’operatore ad utilizzare lo strumento in modo sicuro ed efficiente. Le considerazioni e le precauzioni speciali vengono presentate in questo manuale sotto forma di avvisi di NOTA, CAUTELA e ATTENZIONE. E’ importante che lo strumento venga utilizzato rispettando le istruzioni fornite in questo manuale o che verranno fornite successivamente dalla Varian. Per ogni eventuale chiarimento sull’uso o sulla sicurezza, si prega di contattare la Varian di Leinì (TO). NOTA Sono informazioni utili ad ottenere le prestazioni migliori da parte dello strumento. Segnali di ATTENZIONE ATTENZIONE Pericolo di folgorazioni ATTENZIONE Allerta l’operatore su situazioni che potrebbero causare ferite leggere e danni limitati allo strumento ed il modo di evitarle. ATTENZIONE Allerta l’operatore su situazioni potenzialmente pericolose che possono causare danni molto seri ed il modo di evitarle. Descrizione del Pericolo Nello strumento sono presenti tensioni pericolose. Scollegare il cavo di alimentazione prima di togliere il pannello fissato con le viti. Possono essere presenti composti chimici pericolosi. Evitare il contatto, specialmente quando si riempiono i contenitori. Usare protezioni opportune per la pelle e per gli occhi. ATTENZIONE Pericolo di scottature Pericolo di esposizione a superfici molto calde o raffreddate criogenicamente. Usare protezioni opportune per la pelle. Particelle volanti, agenti chimici o radiazioni UV possono danneggiare gli occhi. Vanno quindi utilizzate le opportune protezioni per gli occhi e per il volto. ATTENZIONE Pericolo di incendio Pericolo potenziale di incendio. Seguire le istruzioni del manuale per lavorare con una maggiore sicurezza. ATTENZIONE C’è pericolo di esplosioni a causa del tipo di gas o liquido utilizzato. Pericolo di esplosioni ATTENZIONE Pericolo di radiazioni E’ presente una radiazione ionizzante. Seguire le istruzioni del manuale per lavorare con una maggiore sicurezza. ATTENZIONE Parti in movimento 03-914603-83:10 Non tenere le mani o le dita vicino. 1 of 4 Norme di Sicurezza Per lavorare in modo sicuro sullo strumento, Vi consigliamo si adottare le seguenti procedure. „ Verificare periodicamente che non ci siano perdite sulle linee e sui raccordi pneumatici. „ Evitare che le linee dei gas vengano piegate o forate. Le linee vanno posizionate in modo tale da non essere calpestate e lontane da sorgenti o troppo calde o troppo fredde. „ I solventi organici vanno conservati in armadi speciali antiincendio, ventilati e con indicazioni chiare sul contenuto di materiali tossici e/o infiammabili. „ Non accumulare i solventi utilizzati. Adottare un programma regolare di smaltimento, ma mai nelle acque di scarico. AVVERTENZA: Questo strumento è stato testato secondo le Direttive EMC allo scopo di poter utilizzare il Marchio CE della Comunità Europea. Questo strumento può essere suscettibile a radiazioni/interferenze o frequenze che non sono entro i limiti collaudati. Questo strumento è progettato per l’analisi cromatografica di campioni opportunamente ATTENZIONE preparati. Deve essere utilizzato usando gas e solventi adatti a questo scopo ed entro i limiti massimi di pressione, flusso e temperatura riportati in questo manuale. Se lo strumento non viene utilizzato secondo le modalità specificate dal costruttore, le condizioni di sicurezza previste potranno non essere sufficienti. E’ responsabilità del Cliente informare il Servizio Tecnico Varian, prima di qualsiasi ATTENZIONE intervento di riparazione, se lo strumento è stato utilizzato per l’analisi di campioni biologicamente pericolosi, radioattivi o tossici. Pericoli Elettrici „ Prima di togliere i pannelli di protezione, scollegare lo strumento da tutte le alimentazioni elettriche in modo da evitare l’esposizione a voltaggi potenzialmente pericolosi. „ Quando si rende necessario sostituire il cavo di alimentazione, assicurarsi che il nuovo cavo rispetti sia le codifiche di colore e di polarità riportate nel manuale di istruzioni che quelle stabilite dalle norme di sicurezza del laboratorio. „ Sostituire i fusibili bruciati solo con fusibili che abbiano le stesse caratteristiche; queste ultime sono riportate sul pannello dei fusibili e/o nel manuale di istruzioni. „ Sostituire immediatamente i cavi di alimentazione difettosi o consumati con cavi dello stesso tipo e con le stesse caratteristiche. „ Assicurarsi che il voltaggio del pannello di alimentazione corrisponda a quello dello strumento da collegare. Bombole dei Gas 2 of 4 „ Occorre prestare molta attenzione quando si spostano bombole di gas compressi. Rispettare tutte le norme di sicurezza. „ Assicurare le bombole ad una parete o ad una struttura fissa. „ Spostare e conservare le bombole sempre in posizione verticale. Togliere i manometri prima di spostare le bombole. „ Conservare le bombole in un’area ben ventilata, non infiammabile, lontana da sorgenti di calore, non esposta a temperature troppo fredde o alla luce diretta del sole. „ Evidenziare in modo chiaro e che non lasci dubbi il contenuto di ogni bombola. „ Usare solo manometri e raccordi di qualità. „ Usare solo tubazioni cromatograficamente pulite (Numero di Parte Varian 03-918326-00) e calibrate per pressioni superiori a quella massima di uscita dal manometro. 03-914603-83:10 Procedure di Sicurezza in GC „ Non smontare mai una linea del solvente od una valvola quando il sistema è sotto pressione. Fermare prima la pompa ed aspettare che la pressione scenda a zero. „ Usare dei contenitori per solventi infrangibili ed in grado di lavorare a 50-60 psi. „ Quando i contenitori sono sotto pressione, usare una protezione esterna. „ Leggere e rispettare tutti gli avvisi di NOTA, CAUTELA e ATTENZIONE. Scarico dei Gas Per i rivelatori GC non è richiesto alcun sistema particolare di scarico dei gas, se lo strumento è installato in una stanza ben ventilata e se non viene utilizzato per l’analisi di sostanze chimiche pericolose. Se si deve installare un sistema di scarico dei gas: „ Usare condutture non infiammabili „ Installare un aspiratore in uscita „ Posizionare la presa d’aria in modo che le vibrazioni e il movimento dell’aria non disturbino il rivelatore. „ Eseguire verifiche periodiche per garantire un funzionamento corretto. „ Garantire una buona ventilazione nel laboratorio. Rivelatori a Sorgente Radioattiva „ Leggere e rispettare tutte gli avvisi di NOTA, CAUTELA e ATTENZIONE riportati nel manuale del rivelatore ECD al Ni63. „ Eseguire tutti i test di contaminazione radioattiva rimovibile descritti nel manuale dell’ECD al Ni63. „ Rispettare tutte le procedure e le scadenze di verifica per eventuali perdite. Pericolo di Scottature Le zone calde o raffreddate criogenicamente del gascromatografo possono mantenere la loro temperatura per parecchio tempo, dopo aver spento lo strumento. Per evitare scottature, assicurarsi che le zone riscaldate o raffreddate siano a temperatura ambiente oppure indossare delle protezioni adeguate prima di toccare tali superfici. Cromatografia Flash L’operatore deve conoscere le proprietà fisicochimiche delle componenti della fase mobile. I solventi non vanno messi in contatto diretto con il tubo di erogazione in poliuretano, dal momento che alcuni solventi possono causare indebolimento e perdite con possibili scoppi. Tutte le componenti del sistema vanno collegate ad una fonte di alimentazione e ad una messa a terra comuni. E’ meglio che per quest’ultima venga utilizzata una spina con polo di terra. I solventi non-polari possono sviluppare una carica statica quando vengono pompati attraverso il sistema. Tutti i recipienti che contengono la fase mobile (inclusi i tubi e i recipienti di raccolta) devono avere una messa a terra per disperdere l’elettricità statica. Vanno utilizzati dispositivi di misurazione e scarico (ad esempio ionizzatori d’aria) per evitare l’aumento di elettricità statica. Radiazioni Ultraviolette Procedure di Sicurezza in LC I rivelatori di cromatografia liquida che usano sorgenti a luce ultravioletta montano degli schermi di protezione per evitare che gli operatori siano esposti a radiazioni pericolose. Pericolo di Alte Pressioni Per una protezione sicura: In caso di rottura di una linea o di apertura accidentale di una valvola, quando il sistema è sotto pressione, la pompa può liberare liquidi tossici e/o volatili molto pericolosi. „ Assicurarsi che i coperchi delle lampade dei rivelatori a lunghezza fissa e variabile siano sempre al loro posto, quando si lavora. „ Non guardare mai direttamente dentro le celle o alla sorgente di luce UV. Quando si vuole ispezionare la lampada o le celle, usare sempre delle protezioni adatte per gli occhi, quali vetro in borosilicato e polistirolo. „ E’ opportuno adottare un sistema di protezione del viso quando si inietta il campione o si esegue una manutenzione routinaria del sistema. 03-914603-83:10 3 of 4 Disponibilità delle Parti di Ricambio Servizi Tecnico E’ politica della Varian il fornire le parti di ricambio per lo strumento ed i suoi accessori per un periodo di cinque (5) anni a partire dalla data di produzione dell’ultima unità della serie. Le parti di ricambio saranno disponibili anche dopo questo periodo di cinque (5) anni ma solo in base alla disponibilità delle stesse. Per parti di ricambio si intendono i componenti elettrici e meccanici soggetti ad usura durante l’uso, in condizioni normali, dello strumento. Come esempio, citiamo i relay, le lampade, i probe di temperatura , i componenti del rivelatore, i motorini, ecc. Le parti strutturali o da fusione, le schede elettroniche ed i moduli funzionali possono essere ricostruiti e rimessi a nuovo durante tutto il loro periodo di vita e perciò sarà possibile acquistarli, dopo la produzione dell’ultima unità delle serie, solo in base alla loro disponibilità. La Varian, alla scadenza del periodo di garanzia, è in grado di fornire ai suoi clienti un’ampia scelta di opzioni. Le riparazioni possono essere effettuate sulla base di contratti di manutenzione particolarmente vantaggiosi od in base ad una tariffa oraria piu’ il costo delle parti. A richiesta, si possono avere corsi per operatori sia sotto forma di contratto che a tariffe da concordare. Uffici Vendite della Divisione Strumenti Analitici della Varian Per informazioni relative alla Vendita, al Servizio Tecnico o all’acquisto di Parti di ricambio, si prega di contattare l’ufficio Varian piu’ vicino. Argentina Buenos Aires Tel. +54.11.4.783.5306 France Les Ulis Cédex Tel. +33.1.6986.3838 Spain Madrid Tel. +34.91.472.7612 Australia Mulgrave, Victoria Tel. +61.3.9566.1134 Germany Darmstadt Tel. +49.6151.7030 Sweden Solna Tel. +46.8.445.1620 Austria Vösendorf bei Wien Tel. +43.1.699.9669 India Mumbai Tel. +91.22.857.0787/88/89 Switzerland Varian AG Tel. +41.848.803.800 Benelux Bergen Op Zoom Tel. +31.164.282.800 Italy Torino Tel. +39.011.997.9111 Taiwan Taipei Hsien Tel. +886.2.698.9555 Brazil and Latin America (S) São Paulo Tel. +55.11.820.0444 Japan Tokyo Tel. +81.3.5232.1211 Canada Mississauga, Ontario Tel. 800.387.2216 Korea Seoul Tel. +82.2.345.22452 United Kingdom and Ireland Walton-on-Thames Tel. +44.1932.898000 China Beijing Tel. +86.106209.1727 Mexico and Latin America (N) Mexico City Tel. +52.5.523.9465 Europe Middelburg, The Netherlands Tel. +31.118.671.000 Russian Federation Moscow Tel. +7.095.937.4280 4 of 4 United States Walnut Creek, California, USA Tel. +1.800.926.3000 (GC and GC/MS) Tel. +1.800.367.4752 (LC) www.varianinc.com Venezuela Valencia Tel. +58.41.257.608 03-914603-83:10 Instrucciones de Seguridad Instrucciones de Operación Este Manual de Instrucciones está diseñado para ayudarle a establecer las condiciones de operación que le permitan operar su instrumento de forma segura y eficaz. Así mismo, se describen consideraciones especiales ó precauciones, que aparecen en forma de NOTA, PRECAUCION, y ATENCION como se indica más abajo.Es importante que utilice el instrumento de acuerdo con este Manual de Operación y cualquier otra información que le proporcione Varian. Remita a la Oficina Local de Varian cualquier cuestión que tenga respecto al correcto uso de su equipo. NOTA Información para ayudarle a obtener unas prestaciones óptimas de su instrumento. Símbolo ATENCIÓN PELIGRO DE DESCARGA ELÉCTRICA ¡PRECAUCION! Le alerta de situaciónes que pueden causar daños moderados a la salud ó al equipo, y cóm evitar esas situaciones. ATENCIÓN Le alerta de potenciales situaciones peligrosas que pueden causar serios daños, y cómo evitar esas situaciones. Descripción El instrumento utiliza voltages peligrosos. Desconecte el interruptor general antes de retirar los paneles atornillados. Peligro de productos químicos. Evite el contacto, especialmente cuando rellene los depósitos. utilice protección de ojos y piel. ATENCIÓN PELIGRO DE QUEMADURAS Superficies posiblemente calientes ó frías (criogénico). Utilice protección para la piel. Las partículas volátiles, productos químicos o radiación UV pueden causar daños en los ojos. Usar las debidas protecciones para la cara y los ojos. ATENCIÓN PELIGRO DE FUEGO ATENCIÓN PELIGRO DE EXPLOSIÓN ATENCIÓN PELIGRO DE RADIACIÓN Peligro potencial de fuego. Siga las instrucciones del Manual de Operación para su seguro funcionamiento. Peligro potencial de explosión debido al tipo de gas ó líquido empleado. Peligro por Fuente de radiación. Siga las instrucciones del Manual de Operación para su seguro funcionamiento. ATENCIÓN PARTES EN MOVIMIENTO 03-914603-84:10 Mantenga alejados los dedos y las manos. 1 of 4 Precauciones Generales de Seguridad Siga estas indicaciones de seguridad para una correcta operación del equipo. „ Realice verificaciones periódicas de fugas en todas las líneas de suministro y tuberías. „ No permita que las líneas de gas se doblen ó pinchen. Manténgalas alejadas de zonas de paso y del calor ó frío excesivo. „ Guarde los disolventes orgánicos en cabinas ventiladas, a prueba de fuego, y etiquetadas para que puedan ser fácilmente identificadas como material tóxico y/ó inflamable. „ No acumule disolventes inservibles. Deseche todo el material inservible a través de un programa especial de desechos y no a través del sistema convencional. NOTA: Este instrumento ha sido testado bajo las normas de la Directiva EMC según requerimientos de la Marca CE de la Unión Europea. Por lo tanto, este equipo puede ser sensible a niveles de radiaciones / interferencias ó frecuencias que no estén incluidas dentro de los límites testados. ATENCIÓN Este instrumento está diseñado para análisis cromatográfico de muestras preparadas apropiadamente. Debe ser operado usando gases y/ó disolventes apropiados y con unos niveles máximos de presión, flujos y temperaturas, según se describe en este manual. ATENCIÓN El Usuario tiene la obligación de informar al Servicio Técnico de Varian cuando el instrumento vaya a ser empleado para análisis de muestras peligrosas de origen biológico, radioactivo ó tóxico, antes de comenzar a realizar cualquier análisis. Peligros Eléctricos „ „ „ „ „ Desconecte el instrumento de todos las conexiones eléctricas a la red antes de retirar los paneles para evitar la posible exposición a peligrosos voltages. Cuando sea necesario emplear una clavija eléctrica no original, asegurese de colocar los cables de acuerdo con el código de colores y polaridades descritos en el manual y los códigos de seguridad de la red eléctrica. Sustituya los fusibles fundidos con fusibles del tipo y tamaño estipulados en el panel de fusibles ó en el manual. Sustituya los cables deteriorados inmediatamente con cables del mismo tipo y graduación. Asegureses de que los valores de las líneas de electricidad se ajustan a los valores para los que el Instrumento ha sido preparado. Botellas de Gas Comprimido „ „ „ „ „ „ „ 2 of 4 Guarde y maneje las botellas de gas con cuidado y de acuerdo con las normas de seguridad. Asegure las botellas a una estructura inmovil ó a la pared. Guarde y mueva las botellas en posición vertical. Retire los reguladores antes de transportarlas. Guarde las botellas en un área ventilada, lejos de fuentes de calor, de luz solar directa y de temperaturas extremadamente bajas. Identifique las botellas claramente para evitar cualquier duda sobre su contenido. Utilice sólamente reguladores y conexiones aprobadas. Utilice sólo tubos de conexión cromatográficamente límpios (Varian p/n 03-918326-00) y que tengan una graduación de presión significativamente mayor que la mayor presión del regulador. 03-914603-84:10 GC Prácticas de Seguridad „ Nunca abra una línea ó una válvula bajo presión. Apague la bomba antes y deje que la presión baje a cero. „ Utilice depósitos irrompibles que sean capaces de operar a 50-60 psi. „ Mantenga cerrada la junta del depósito cuando se haye bajo presión. „ Lea y cumpla todas las NOTA, PRECAUCION, y ATENCION del manual. Sistema de Extracción No se necesita un sistema de extracción para los detectores GC instalados en un laboratorio bien ventilado, excepto cuando se analicen muestras químicas peligrosas. Si instala un sistema de extracción: „ Utilice conductos a prueba de fuego. „ Instale un ventilador al final del sistema. „ Instale entradas de aire cuya vibración no afecte al trabajo del detector. „ Compruebe periódicamente el correcto funcionamiento del sistema. „ Asegurese de una correcta ventilación del laboratorio. Detectores con fuentes radioctivas „ Lea con cuidado y cumpla todas las NOTAS, PRECAUCION, y ATENCION del Manual del Detector Ni63 ECD. „ Realice los test de contaminación radioactiva descritos en el Manual del Detector Ni63 ECD. „ Cumpla con los plazos y procedimientos de test de fugas. Peligro de Quemaduras Las zonas de calor ó frío (criogénicas) del Cromatógrafo de Gases pueden permanecer calientes ó frías durante bastante tiempo después de apagar el instrumento. Para evitar quemaduras asegureses de que todas las áreas que se calienten ó enfríen han vuelto a la temperatura ambiente, ó protejase adecuadamente las manos, antes de tocar las superficies potencialmente calientes ó frías. Cromatografía Flash El operador debe familiarizarse con las propiedades físico-químicas de los componentes de la fase móvil. Alejar los disolventes del contacto directo con los tubos de poliuretano ya que ciertos disolventes pueden causar reblandecimiento de los tubos o posibles fugas con riesgo de explosión. Todos los componentes del sistema deben estar conectados a un enchufe común con toma de tierra común. Esta toma de tierra debe ser una toma de tierra verdadera en lugar de flotante. Los disolventes no-polares pueden originar carga estática cuando son bombeados por el sistema. Todos los recipientes que contienen fase móvil (incluyendo los tubos y los recipientes de recogida) deben estar conectados a tierra para disipar la electricidad estática. Utilizar medidores de carga estática y los debidos dispositivos de descarga (por Ej., ionizadores de aire) para salvaguardarse contra la creación de electricidad estática. Radiación Ultravioleta Los detectores del Cromatógrafo de Líquidos que utilizan una fuente de luz ultravioleta disponen de protección para prevenir exposiciones radioactivas al personal. LC Prácticas de Seguridad Para una correcta protección: Peligro de Alta Presión „ Si se rompe una línea de presión, ó se abre una válvula de seguridad accidentalmente bajo presión, la bomba puede generar líquidos a alta presión potencialmente peligrosos, produciendo un chorro a alta velocidad de líquidos volátiles y/ó tóxicos. Asegurese de que las cubiertas de protección de la lámpara de los detectores está correctamente situada durante su funcionamiento. „ No mire directamente a las celdas del detector ó a la fuente de luz UV. Cuando inspeccione la fuente de luz ó la celda, utilice siempre una protección para los ojos como gafas de borosilicato ó poliestireno. „ Lleve protección facial cuando inyecte muestras ó realice mantenimiento de rutina. 03-914603-84:10 3 of 4 Disponibilidad de Recambios Es Política de Varian disponer de Recambios para cualquier instrumento y la mayoría de los accesorios por un periodo de cinco (5) años después del último instrumento fabricado. Los recambios durante esos cinco años estarán disponibles, pero siempre bajo el sistema “Según disponibilidad”. Los Recambios están definidos como todas aquellas partes individuales mecánicas ó eléctricas que son susceptibles de fallo durante su normal proceso de operación. Por ejemplo, relés, lámparas, sondas de temperatura, elementos del detector, motores, etc. Las planchas de metal, partes de la estructura, placas de circuitos integrados, y otros módulos funcionales son normalmente susceptibles de reparación y por lo tanto sólo estarán disponibles bajos el sistema “Según disponibilidad” después del último instrumento fabricado. Disponibilidad de Servicio Varian ofrece una gran variedad de sistemas de Servicio para mantener el soporte a sus usuarios tras el periodo de garantía. El Soporte de Servicio se ofrece a través de atractivos Contratos de Servicio ó bajo un sistema de facturación de mano de obra y materiales. El mantenimiento y el entrenamiento se realiza por ingenieros cualificados bajo Contrato ó petición. Oficinas de Instrumentación Analítica Varian Para cualquier consulta sobre Instrumentación Analítica, Servicio Técnico ó Recambios y Accesorios, contacte con su oficina local: Argentina Buenos Aires Tel. +54.11.4.783.5306 France Les Ulis Cédex Tel. +33.1.6986.3838 Spain Madrid Tel. +34.91.472.7612 Australia Mulgrave, Victoria Tel. +61.3.9566.1134 Germany Darmstadt Tel. +49.6151.7030 Sweden Solna Tel. +46.8.445.1620 Austria Vösendorf bei Wien Tel. +43.1.699.9669 India Mumbai Tel. +91.22.857.0787/88/89 Switzerland Varian AG Tel. +41.848.803.800 Benelux Bergen Op Zoom Tel. +31.164.282.800 Italy Torino Tel. +39.011.997.9111 Taiwan Taipei Hsien Tel. +886.2.698.9555 Brazil and Latin America (S) São Paulo Tel. +55.11.820.0444 Japan Tokyo Tel. +81.3.5232.1211 Canada Mississauga, Ontario Tel. 800.387.2216 Korea Seoul Tel. +82.2.345.22452 United Kingdom and Ireland Walton-on-Thames Tel. +44.1932.898000 China Beijing Tel. +86.106209.1727 Mexico and Latin America (N) Mexico City Tel. +52.5.523.9465 Europe Middelburg, The Netherlands Tel. +31.118.671.000 Russian Federation Moscow Tel. +7.095.937.4280 4 of 4 United States Walnut Creek, California, USA Tel. +1.800.926.3000 (GC and GC/MS) Tel. +1.800.367.4752 (LC) www.varianinc.com Venezuela Valencia Tel. +58.41.257.608 03-914603-84:10 Table of Contents Introduction.............................................................................................. 1 Installation................................................................................................ 3 Unpacking............................................................................................................................3 Connections.........................................................................................................................3 Power Connections .......................................................................................................4 Communication Connectors..........................................................................................4 Control I/O Connector.............................................................................................5 Vial Number Output Connector ..............................................................................6 RS485 Connector ...................................................................................................6 Fluid Connections .........................................................................................................6 Sample Loop...........................................................................................................7 Digital Dispenser System (DDS) ............................................................................7 Sample Drain for Loopfilling by Headspace Pressure............................................8 Sample Consumption ..........................................................................................................8 Rest volume ..................................................................................................................8 Pre-flush volume ...........................................................................................................8 Injection volume......................................................................................................9 Sample consumption formula (dispenser controlled) .............................................9 Sample consumption for headspace pressure controlled loopfill...........................9 Filling and Sealing the Vials ..............................................................................................10 Loading the Sample Tray ..................................................................................................10 Positioning of vials................................................................................................10 Needle wash vials.................................................................................................11 Large Volume Samples .....................................................................................................11 Description ..................................................................................................................11 Installation ...................................................................................................................12 Instrument Description ......................................................................... 13 General Description...........................................................................................................13 Injection Principle ..............................................................................................................14 Dispenser-controlled Injection.....................................................................................14 Pressure-controlled Injections.....................................................................................15 Digital Dispenser System (DDS).................................................................................16 Operating Principle ...............................................................................................16 ProStar 400 AutoSampler i Operation................................................................................................ 17 Principle .............................................................................................................................17 Different Programming Modes ....................................................................................17 Other Modes ...............................................................................................................17 READY Status.............................................................................................................18 Key Functions ....................................................................................................................18 Function Codes .................................................................................................................19 Programming Chart ...........................................................................................................20 Programming .....................................................................................................................21 System Settings ..........................................................................................................21 RUN Parameters.........................................................................................................22 Cooling Control (optional) ...........................................................................................23 RUN ...................................................................................................................................23 HOLD ..........................................................................................................................24 Priority Sample............................................................................................................25 Remote Control..................................................................................................................25 PC Workstation Interface...................................................................................................26 Varian 4400 Integrator Interface........................................................................................27 Special Display Messages.................................................................................................27 After Use............................................................................................................................28 Maintenance/Service ............................................................................. 29 Needle Penetration Depth .................................................................................................30 Needle Pair Replacement..................................................................................................30 Sample Needle............................................................................................................30 Air Needle ...................................................................................................................32 Dispenser Pump Tubing ....................................................................................................32 Appendix ................................................................................................ 33 Specifications.....................................................................................................................33 Accessories .......................................................................................................................35 ii 03-914786-00:3 Introduction The ProStar 400 AutoSampler is dedicated to routine analyses of large series of samples in an environment where zero sample loss and injection flexibility are of little significance but where reliability, stability, and reproducibility are mandatory. The ProStar 400 therefore makes use of flushed loop injection, with reproducibility of injection better than 0.5%. ProStar 400 AutoSampler 1 2 03-914786-00:3 Installation Unpacking Inspect the shipping container for indications of damage. Damage occurring during transit is the responsibility of the carrier and should be reported immediately to the carrier and to: Varian, Inc. 2700 Mitchell Drive Walnut Creek, California 94598-1675 Attention: Customer Service 1-800-FOR-HPLC or your local Varian office For contents of shipping container see the Standard Accessory Kit list in the shipping box. Unpack the ProStar 400 AutoSampler carefully. Connections 6 5 4 3 8 2 9 1 2 3 4 5 6 7 8 9 Fuses and voltage selector Main power input Power switch Cooling fan, only in case of tray cooling Standard RS232 connector Connector vial number output Connector control I/O Optional communication connector Serial Number Label 1 Figure 1 ProStar 400 AutoSampler Rear Panel ProStar 400 AutoSampler 3 Power Connections • Before plugging in the power cable, check voltage settings of the modules at the input socket on the rear panel. • Make sure that the voltage settings of the modules are identical with the voltage of your local power supply. • Use only a supply appliance with protective grounding. • If the indicated voltage is not correct, select the proper voltage by removing, inverting, and then re-inserting the voltage selector. • When the voltage selection and fuses are correct for your power source, plug in the power cable. The correct fuses should be installed. WARNING: FIRE HAZARD For continued protection replace only with same type and rating of fuse. If a new voltage was selected, check the fuses and change appropriately with the following specifications: For ... Use ... Part Number 115 Vac ±10% Two 5.0 amp T-type (slo-blo) 55-500338-00 230 Vac ±10% Two 2.5 amp T-type (slo-blo) 55-500344-00 Communication Connectors For connection to Varian ProStar and Star LC modules, use Cable Kit Part Number 03-909126-90. Follow the Installation Instructions included with that cable. Information in the following paragraphs is provided for users who wish to develop custom interfaces to other devices. 4 03-914786-00:3 INSTALLATION Control I/O Connector Table 1 Control I/O Connector Pin No. I/O Description 1 24 volt DC 2 Auxiliary output 2 inverted (open collector, max. 250 mA) 3 Auxiliary output 2 (open collector, max. 250 mA) 4 Auxiliary output 1 inverted (open collector, max. 250 mA) 5 Auxiliary output 1 (open collector, max. 250 mA) 6 Inject marker output (N.O. contact) 7 Inject marker output (N.C. contact) 8 Inject marker common (for N.O./N.C. contacts) Note: Starting at the moment of injection, Inject marker contacts are closed/openproducing a 1.0 sec. switch closure. 9 Inject marker output (TTL, active low) 10 Stop I/O (TTL, pulled up); output is low when the ProStar 400 AutoSampler ends processing (READY); pull low input will stop processing (ProStar 400 goes to READY). 11 Spare (open collector) 12 Next vial input (active low, pulled up, TTL) This input triggers a next vial to be processed when the ProStar 400 AutoSampler is in REMOTE CONTROL mode. 13 Freeze (HOLD) input (active low, pulled up, TTL) This input has the same function as the HOLD/CONT key (see Operation on page 17). 14 Next injection input (active low, pulled up, TTL) This input triggers a next injection when the ProStar 400 AutoSampler is in REMOTE CONTROL mode. It can also be used as a START input when the ProStar 400 is not in REMOTE CONTROL mode. 15 Ground 16 Ground NOTE: The duration of inputs 10, 12, and 14 must be at least 20 msec. ProStar 400 AutoSampler 5 Vial Number Output Connector 8-bit BCD-coded VIAL NUMBER OUTPUT (True logic), representing vial numbers 1-96; active when corresponding vial is processed. Table 2 Vial Number Output Connector Pin No. Output Pin No. Output 1 Bit 0 units 1 9 Bit 1 units 2 2 Bit 2 units 4 10 Bit 3 units 8 3 Bit 4 units x 10 11 Bit 5 units x 20 4 Bit 6 units x 40 12 Bit 7 units x 80 8 Ground 15 Inject marker (TTL, active low) RS485 Connector The ProStar 400 can be controlled by a PC using the RS485 interface. Fluid Connections The instrument has been tested with isopropanol. Make sure that the mobile phase of your HPLC system is miscible with isopropanol. If not, start up with an intermediate solvent as mobile phase which is compatible with your column. To gain access to the high pressure valve, remove the keyboard cover of the ProStar 400 AutoSampler. WARNING: MOVING PARTS Moving parts and sharp needle. Keep hands clear. Remove the safety screw on the left hand side of the ProStar 400 AutoSampler. Lift the cover and place it on the top of the AutoSampler. Connect the HPLC pump to port 5 and the column to port 6 of the injection valve. 6 03-914786-00:3 INSTALLATION Figure 2 Keyboard Cover Removal Sample Loop The ProStar 400 is factory-equipped with a 20 µL sample loop. If a different volume is to be injected, the sample loop must be replaced. Please note that to fill the loop quantitatively, three times the loop volume is withdrawn from the sample vial for loops smaller than 100 µL and twice the loop volume for loops larger than 100 µL. Loops ranging from 5 µL to 1 mL are available from Varian. Digital Dispenser System (DDS) The DDS pump tubing cassette is factory-installed and connected to the injection valve. Fasten the pump tubing cassette before use with the screw on top of the pump tubing cassette. If the AutoSampler is not to be used for two days or more, be sure to loosen this screw to prevent permanently deforming the tubing. If the pump tubing cassette needs replacement, refer to Maintenance/Service on page 29. ProStar 400 AutoSampler 7 Sample Drain for Loopfilling by Headspace Pressure Time-based loopfilling by sample headspace pressure can be selected (see Operation on page 17) to shorten loopfill time for larger loop volumes (see Injection Principle on page 14). To allow time-based loopfilling and to prevent hydrostatic sample loss, the special sample drain for headspace pressure loopfill must be connected at the injection valve, replacing the dispenser connection at the valve. Sample Consumption Rest volume Since the sample needle is always at some (very short) distance above the bottom of the sample vial, a certain volume of sample always remains in the vial, out of reach of the sample needle. This volume is called the rest volume. For standard 1.5 mL vials, the rest volume is approximately 200 µL. For a conical vial, the rest volume is only a few µL. Refer to page 30 for adjustment of needle penetration depth. Pre-flush volume Prior to the FIRST injection, the sample needle and tubing (needle→injection valve) are flushed with sample (for dispenser controlled loopfill, see page 14, Injection Principle). Depending on the concentration differences between samples and the cross-contamination allowed, this so-called pre-flush volume may range between 30-999 µL (programmable). Only dispenser controlled loopfilling uses a pre-flush. If sample loss greater than 30 µL for pre-flush is not acceptable, select NEEDLE WASH between sample vials in SYSTEM SETTINGS to avoid cross-contamination. See Operation on page 17. 8 03-914786-00:3 INSTALLATION Injection volume Due to the reduced solvent velocity near the wall of the tubing (loop), it takes more than the nominal loopvolume to fill the loop reproducibly. For flushed loop injections the ProStar 400 takes twice the loop volume from the sample vial for a sample loop equal to or larger than 100 µL and three times the loop volume for a sample loop smaller than 100 µL. Sample consumption formula (dispenser controlled) The minimum amount of sample needed for N injections per vial: Flushed loop injections for 100 µL loop or larger: rest volume + pre-flush volume + 2N x loopvolume + (N-1) x 4 (µL) Flushed loop injections for loop smaller than 100 µL: rest volume + pre-flush volume + 3N x loopvolume + (N-1) x 4 (µL) Example: 3 flushed loop injections out of a standard sample vial using a 20 µL loop and 30 µL pre-flush volume, minimum sample volume needed is: 200 µL + 30 µL + 3 x 3 x 20 µL + 2 x 4 µL = 418 µL Sample consumption for headspace pressure controlled loopfill If the sample loop is filled on a time basis by sample headspace pressure (see Injection Principle on page 14 and Operation on page 17), sample consumption has to be determined experimentally since the flow is dependent on the viscosity. (For water, the flow rate is approximately 1 mL/min.) Make sure that programmed fill time is sufficient to flush the loop with at least twice its volume. If more injections are to be taken from the same vial, please note that a volume equal to max. 20% of the headspace in the vial after loopfill may flow to waste during analysis time due to expansion of the headspace back to atmospheric pressure. ProStar 400 AutoSampler 9 Filling and Sealing the Vials The 1.5 mL vials, as well as the conical vials, can best be filled by means of a narrow-end pipette to allow air to escape while filling the vial. NOTE: Do not fill vials past the shoulder. Sample will be forced into the air needle, risking extra cross-contamination of samples. It is important that the seal be airtight to maintain a constant pressure on the vial for air bubble prevention and reproducible injections. Leaking vial septa will impair reproducibility when doing loop overfill with headspace pressure. NOTE: Do not reuse a vial without replacing its septum. Loading the Sample Tray To allow remote loading of the sample tray, the sample tray consists of four removable segments that fit in one unique position of the tray holder. Use the STEP key (see Operation on page 17) to rotate the tray (functioning only when the ProStar 400 is in READY status). CAUTION Do not rotate the tray manually; you may damage the tray drive mechanism. Positioning of vials Sample vials should be placed in sequential positions on the tray. Empty spaces between vials of a sample series are allowed, since the ProStar 400 can detect empty positions. After detecting an empty place, the AutoSampler will continue with the next position. 10 03-914786-00:3 INSTALLATION Additional samples can be placed during RUN since the LAST VIAL value can be changed during RUN (see Operation on page 17). Needle wash vials If needle wash is programmed (see Operation on page 17), place 4 vials with washing solvent (1.5 mL each, usually mobile phase) on positions 93-96. You must use all four vials as they will be used alternately. Large Volume Samples Description The large volume sample tray is an option of the ProStar 400 AutoSampler. This option allows the user to inject large volumes of sample with the DDS or by headspace pressure. The option consists of: ProStar 400 AutoSampler • 4 LSV sample tray segments • 500 µL loop • a serum needle with serum air-needle • special sample tubing (0.5 mm ID) • sample drain 11 Installation Install the LSV option according to the following procedure: NOTE: 12 • Replace the standard installed tubing and needles with the tubing and needles of the LSV option. Follow the procedure described in Maintenance/Service, page 29. • Replace the standard tray by the LSV tray. • Install the 500 µL loop to port 1 and 4. • Check the needle penetration depth and if necessary adjust it. See page 29, Needle Pair Replacement. • Connect the drain to port 3 if the loop will be filled on a time basis by headspace pressure. It is also possible to fill the loop with the DDS. This will take less sample, but more time. If the loop is filled using the DDS, a larger preflush volume (minimum 50 µL) must be programmed to avoid cross contamination due to the larger internal diameters of the tubing and needle. 03-914786-00:3 Instrument Description General Description Figure 3 ProStar 400 1 Sample tray, consisting of 4 removable segments 2 Keyboard 3 Display 4 Removable cover 5 Needle arm with sample needle 6 Injection valve with sample loop 7 Dispenser cassette screw 8 Dispenser 9 Outlet tubing holder 10 Common leakage/condensation water drain for injection valve, sample tray and DDS ProStar 400 AutoSampler 13 Injection Principle A six-port high pressure switching valve can perform the injections based on the flushed loop principle. Loopfilling can be done on a volume basis, controlled by the digital dispenser system, or on a time basis by headspace pressure on the sample to shorten filling time for larger loop volumes. See Operation on page 17. The switching patterns of the valve in “LOAD” and “INJECT” positions are shown in Figure 4. An injection is performed as described in the following paragraphs. Dispenser-controlled Injection 1. Dispenser aspirates an approximately 10 µL air bubble in the sample needle for more efficient removal of the previous sample. 2. With the injection valve in inject position, the coaxial needle pair is inserted into the sample. Air pressure, applied to the sample through the outer air needle, ensures that no air or vapor bubbles are formed during sample withdrawal. 3. Dispenser withdraws “preflush volume” from sample vial to fill the sample line with sample and to remove previous sample (30 - 999 µL, programmable). 4. Injection valve switches into load position with flushed-loop injections; dispenser transports 2 or 3 X loopvolume through the loop to fill the loop quantitatively. 2 X loopvolume for loops equal to or larger than 100 µL 3 X loopvolume for loops smaller than 100 µL 5. Injection valve switches into inject position. The sample loop is now part of the HPLC mobile phase flow path. The sample is transported to the column, and the analysis time starts. If one injection is to be made out of each sample vial, the needle pair withdraws after analysis time and sequence 1-5 is repeated for the next vial. If more than one injection is to be made out of the same sample vial, the needles remain in the vial and after 14 03-914786-00:3 INSTRUMENT DESCRIPTION the analysis time is completed, the next injection is made starting the sequence at step 3 with a fixed preflush of 4 µL. Figure 4 Dispenser-controlled Injection Pressure-controlled Injections 1. With the injection valve in load position, the coaxial needle pair is inserted into the sample. Air pressure, applied on the sample through the outer (air-) needle, will force the sample via the inner (sample-) needle through the sample loop. The duration of the headspace pressure is programmable; appropriate duration has to be determined experimentally. 2. Injection valve switches into inject position. Sample loop is now part of the HPLC mobile phase flow path: sample is transported to the column. Analysis time starts. NOTE: A special sample drain that prevents siphoning must be connected to the injection valve (replacing the dispenser connection). Refer to Installation on page 3. ProStar 400 AutoSampler 15 If one injection is to be made out of each sample vial, the needle pair withdraws after the analysis time is complete and sequence steps 1-2 starts for the next vial. If more than one injection is to be made out of the same sample vial, the needles remain in the vial. Figure 5 Pressure-controlled Injection Digital Dispenser System (DDS) Operating Principle The DDS is a miniature “finger pump”. The operating principle is shown below. Fingers 1 and 3 act as inlet and outlet pinch valve, respectively, finger 2 provides the fluid displacement. The stroke of finger 2 is factory adjusted to provide 2 µL per stroke. Since the volume dispensed is always a multiple of one stroke volume (digital dispensing), i.e., 2, 4, 6 µL, etc., odd values for volumes will be rounded down to even values. Figure 6 Operating Principle of Digital Dispensing System (DDS) 16 03-914786-00:3 Operation Operating the ProStar 400 AutoSampler is easy. After programming the system SETTINGS, only a few parameters need to be programmed for regular automatic processing of a series of samples. All parameter values are saved in memory when power is switched off or during power failure, except the tray temperature setting, if the tray cooling option is installed. Tray cooling is always turned off at power up. Principle Different Programming Modes To simplify regular operation, common injection parameters like “analysis time” and “first/last vial” are programmed in the RUN PARAMETER mode. Less frequently altered parameters like “auxiliaries YES/NO” are programmed in the SYSTEM SETTINGS mode. An additional COOLING CONTROL mode takes care of the sample tray temperature, when the option is installed. Other Modes ProStar 400 AutoSampler • RUN mode for automatic processing of samples. • REMOTE CONTROL mode for autosampler control via I/O contacts. • SERIAL RS485 mode for autosampler control via serial interface. 17 READY Status • READY status is the “ground state” of the ProStar 400 AutoSampler which is initiated automatically after power UP. Every mode can be entered from READY status, except PRIORITY mode, which can be entered only when the ProStar 400 AutoSampler is in RUN mode. • In addition, RUN PARAMETER and COOLING CONTROL mode can be entered when the ProStar 400 AutoSampler is in the RUN mode. Function codes are used to enter any specific mode, except for the RUN PARAMETER mode which can be entered directly via the PROG/END key, and RUN mode (entered by the START command). Every mode uses the same function code (F,0) to exit, except for RUN PARAMETER mode and RUN mode which are left via PROG/END and STOP respectively. Key Functions STEP key; used to step through the parameter list. The STEP key is also used to rotate the sample tray (in READY status only.). START/STOP Start/Stop automatic processing of samples. HOLD/CONT Hold/Continue countdown of analysis time. Analysis time is extended with the time that hold is active. PROG/END Enables/Ends programming of parameters in the selected mode. Note that the PROG/END key selects the RUN PARAMETER mode and enables the programming of its parameters at the same time. CL Clears the value of the parameter on display. F Function key; used in combination with a numerical key to select or exit the various modes. 0-9 Numerical keys; used to enter values for programmable parameters. Values are stored when going to the next parameter (STEP) or when ending programming (PROG/END). 18 03-914786-00:3 OPERATION Function Codes The following table shows all the possible modes of the ProStar 400 AutoSampler. Function code Selected mode F,9 Selects SYSTEM SETTINGS mode. F,7 Selects COOLING CONTROL mode (only if cooling option is installed) F,2 Selects PRIORITY mode (only accessible during sample run). F,3 Selects REMOTE CONTROL mode. F,4 Selects SERIAL RS485 mode. F,0 To exit all modes, selected by a function code Refer to the following Programming Chart. ProStar 400 AutoSampler 19 Programming Chart Use 1. 2. 3. 4. 5. 6. 7. 8. 9. to step. FIRST VIAL (1—>48/92/96) LAST VIAL (1—>48/92/96) NO OF INJ'S/VIAL (1—>9) PREFLUSH VOLUME (30—>999µL) FLUSH TIME (1—> 999 SEC) ANALYSIS TIME (0:00—> 99:59) TIME AUX 1 ON (0:00—> 99:59) TIME AUX 1 OFF (0:00—> 99:59) TIME AUX 2 ON (0:00—> 99:59) TIME AUX 2 OFF (0:00—> 99:59) PRESS TO ADVANCE SAMPLE TRAY Use 1. 2. 3. 4. 5. to step. LOOPVOLUME SAMPLE VOLUME FLUSH NEEDLE WASH AUXILIARIES TRAY COOLING (ON / OFF) (0->999µL) (STD/LSV) (VOL/TIME) (YES/NO) (YES/NO) REMOTE CONTROL MODE SERIAL RS485 MODE DEVICE IDENTIFIER (10 —> 19) RUN MODE ANALYSIS TIME Accessible: Run parameters, Temperature control. PRIORITY MODE default vial no 00! FREEZE ANALYSIS TIME Accessible: Run parameters, Temperature control. Enter number to activate 20 03-914786-00:3 OPERATION Programming Only three modes contain programmable parameters: • SYSTEM SETTINGS mode to “set” system parameters. • RUN PARAMETER mode for regular programming of sample processing. • COOLING CONTROL mode to program the tray cooling, if installed. System Settings With the ProStar 400 in READY status, key in F,9 to select SYSTEM SETTINGS mode. Press PROG/END to enable programming of the following parameters (use STEP key to go to the next parameter): LOOP VOLUME Enter volume of the installed loop: 0-999 µL. If using dispenser controlled loopfill, this will set the loop overfill volume to 3X loopvolume if loop <100 µL and 2X loopvolume for loops >100 µL. SAMPLE VOLUME (STD/LSV) Enter 0 to select STANDARD sample tray. Enter 1 if the optional Large Sample Volume tray has been installed (48 vials of 5 mL each). FLUSH (VOL/TIME) Enter 0 to select dispenser controlled loopfilling on a volume basis. Enter 1 to select loop filling by sample headspace pressure on a time basis. Filling on a time basis may be used for large injection volumes (>500 µL) to shorten loopfill time. For loopfilling on a time basis, mount the special drain included in the Accessory Kit to allow for pressure controlled sample transport and to prevent hydrostatic sample flow which may empty your sample vial during analysis time. ProStar 400 AutoSampler 21 NEEDLE WASH (YES/NO) Enter 1 to select needle wash. Positions 93-96 are now used as containers for washing solvent. After every sample vial the needle and connecting tubing is flushed with solvent from one of the “wash vials” (alternating between 93 and 96). Enter 0 if no needle wash is wanted (position 93-96 can now be used for sample vials). AUXILIARIES (YES/NO) Enter 1 if time programmable auxiliary output(s) are to be used. Parameters will appear in the RUN PARAMETER mode. Enter 0 if no auxiliaries are to be used. RUN Parameters With the ProStar 400 in READY status, press PROG/END to select RUN PARAMETER mode and to enable programming at the same time. The following parameters can be programmed (use STEP key to go to next parameter): FIRST VIAL Enter position number of the first vial of the sample series in the sample tray. 1-96 without needle wash 1-92 with needle wash 1-48 with LSV LAST VIAL Enter position number of the last vial of the sample series in the tray. (See FIRST VIAL for valid numbers.) INJ/VIAL Up to 9 injections can be taken from the same vial. Enter number 0-9. PRE FLUSH VOLUME Parameter shows up for flush on a volume basis only; enter volume (of sample) which is to be used to flush needle and connecting tubing prior to filling the loop: 30-999 µL. FLUSH TIME Parameter shows for flush on a time basis only. Enter duration of headspace pressure for loopfilling: 1-999 sec. ANALYSIS TIME Enter the time interval needed before the next injection takes place: 0-99'59". Time countdown starts at moment of injection. 22 03-914786-00:3 OPERATION TIME AUX 1 ON Parameter shows only when auxiliaries are enabled in System settings. Enter time at which auxiliary 1 must switch ON: 099'59". TIME AUX 1 OFF Parameter shows only when auxiliaries are enabled in System settings. Enter time at which auxiliary 1 must switch OFF: 0-99'59". TIME AUX 2 ON See AUX 1. TIME AUX 2 OFF See AUX 1. Cooling Control (optional) Sample tray temperature control is switched ON/OFF in the COOLING CONTROL mode. With the ProStar 400 in READY status, key in F,7 to select COOLING CONTROL mode. Press PROG/END to switch ON or OFF the cooling control. The sample tray cooling has a fixed temperature of 4°C. Enter 0 to switch OFF the sample tray cooling. TRAY COOLING (ON/OFF) NOTE: Enter 1 to switch ON the sample tray cooling. After power up, the sample tray cooling is always off. RUN When programming is complete, system is ready and the ProStar 400 AutoSampler is in READY status, press START/STOP key to start automatic processing of the samples. During RUN, the ProStar 400 will show information relevant to the actual process such as: SEARCH VIAL 45, LOOPFILL, WASHING, etc. During analysis time the display will show the following information continuously (example): 0 VIAL:15 82 2'INJ pTIME 03:45 AUX 1 2 ProStar 400 AutoSampler 4 C 23 The first line shows that the second injection from vial 15 is being processed, vial 82 is the last vial to be processed. The temperature of the cooling tray shown at the end of the first line will only be displayed if the option is present. The second line shows the time since the injection in minutes, seconds format, and the status of the auxiliaries. The number will be displayed if the auxiliary is ON (only shown when enabled in the settings). The first character of the second line will be a blinking R if the ProStar 400 is under remote control or a blinking p if a priority sample is programmed. It is possible to reprogram RUN PARAMETERS during RUN; simply press PROG/END to enter the RUN PARAMETER mode. Press PROG/END to exit RUN PARAMETER mode and to continue the RUN program. NOTE: If you do not return to RUN mode, RUN will stop after finishing the current injection. Changes in the RUN parameters will be executed immediately after returning to RUN mode, although an injection will not be interrupted. COOLING CONTROL can also be reprogrammed during RUN; press F,7 to enter COOLING CONTROL mode. Return to RUN (F,0) to continue RUN. HOLD HOLD (press HOLD/CONT) can be used to freeze the time base. During HOLD, the RUN PARAMETER mode, COOLING CONTROL mode and PRIORITY mode are accessible to reprogram/check parameters. Exit any of these modes (if entered) and press HOLD/CONT key to continue RUN. Analysis time of the current injection has then been extended with the time that HOLD was active. 24 03-914786-00:3 OPERATION Priority Sample A sample run can be interrupted to process an emergency sample prior to the next sample of the programmed samples series: press F,2 to enter the priority mode, press PROG/END key and enter the number of the tray position where the priority vial has been placed. Press PROG/END to end programming. Return to RUN (F,0). Priority vial will be processed immediately after the current vial. A blinking “P” (first position of lower display line) indicates that a priority vial is to be/being processed. After processing the priority vial, RUN will continue where it was interrupted. NOTE: Priority mode can only be entered during sample run. It cannot be entered during pre flush or loopfill. Remote Control When used with Varian ProStar or Star LC modules, the ProStar 400 is interfaced using Cable Kit Part Number 03-909126-90. Remote control mode is not necessary to use this cable. However, using remote control mode, the ProStar 400 will wait for a “ready” signal from the other modules of the Star system before starting its injection cycle. See the installation instructions enclosed with the cable for details of these modes of operation. When the ProStar 400 is in REMOTE CONTROL mode it can only be controlled using the “next injection” and “next vial” inputs. RUN is executed as programmed, but analysis time is now infinite. Only a “next injection” input signal will initiate the next injection from the same vial (or from the next vial when the programmed number of injections per vial have been executed). A “next vial” input signal will initiate the first injection from the next vial. With the ProStar 400 in READY status, REMOTE CONTROL mode is entered with F,3; display will show: 0 ProStar 400 AutoSampler REMOTE CONTROL READY 25 A “next injection” input signal will start the RUN. A blinking R (first position of the lower display line) indicates that the ProStar 400 is under remote control. All other relevant RUN information will be displayed as usual. When all programmed vials have been processed, the display will show: 0 REMOTE CONTROL F,0 TO EXIT Next injection or next vial inputs will no longer have any effect. Exit REMOTE CONTROL mode (F,0) to return to READY status. PC Workstation Interface Up to four ProStar 400 AutoSamplers can be simultaneously controlled from the Varian Star Chromatography Workstation. Control requires purchase of the Star LC Control Software Kit. Contact your local Varian representative for more information or to order communication kits. Figure 7 shows the connection cabling and the kit part numbers for the Star Workstation control of ProStar 400 AutoSamplers. Complete installation instructions are included with these kits. 26 03-914786-00:3 OPERATION Figure 7 Star Workstation Communication for Single ProStar 400 AutoSampler Varian 4400 Integrator Interface The ProStar 400 outputs the vial location number through a BCD port. Varian Cable Kit Part Number 03-919938-90 provides a cable to connect the BCD output to the Varian 4400 Integrator. The instructions enclosed with this cable describe how to interface to the 4400 such that the AutoSampler vial number is printed on each 4400 report. Full synchronization cable operation of the ProStar 400 with the 4400 Integrator and other Varian Star modules requires this cable plus Cable Kit P/N 03-909126-90 described above. Special Display Messages During operation several messages may appear on the display to make you aware of errors, system malfunctions or other uncommon events. These special display messages are listed below together with the appropriate actions to take. ProStar 400 AutoSampler 27 Press any key; if the ProStar 400 goes to READY status, all MEMORY ERROR ALL VALUES DEFAULT parameters are set to default values. Reprogram RUN and TEMP.CONTROL parameters and check SYSTEM SETTINGS. If message remains, call Varian. TRAY ROTATION FAILURE Tray movement is obstructed; check/remove obstruction. Press any key to continue; if message remains: call Varian. NEEDLE MOVEMENT FAILURE Needle arm movement is obstructed; check/remove obstruction. Press any key to continue; if message remains, call Varian. DISPENSER FAILURE Call Varian. PROGRAM VIALS SYSTEM SETTING STD/LSV was changed: FIRST VIAL and LAST VIAL are reset to 0; reprogram (RUN PARAMETER mode). Press any key to continue. NEEDLE WASH was switched ON (SYSTEM SETTINGS) with FIRST or LAST vial programmed on WASH positions. FIRST VIAL and LAST VIAL are reset to 0; reprogram (RUN PARAMETER mode). Press any key to continue. ERROR.(.............) An erratic value has been entered; limits for this parameter are shown in parenthesis on display. Enter correct value. After Use If the ProStar 400 AutoSampler is not to be used for more than two days, flush needle and valve with water and isopropanol (can be placed as last vials of a sample series) and loosen pump tubing cassette screw one turn. Never leave the AutoSampler out of use with a buffer or salt solution in the tubing; crystals may block the flow path and may damage the rotor seal of the injection valve. Power can be switched OFF since all parameter values are saved in memory (long-life non-chargeable battery back-up). Only sample tray cooling is changed to OFF after power UP. 28 03-914786-00:3 Maintenance/Service 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 Figure 8 Injection System ProStar 400 AutoSampler 16 17 18 19 Side-port sample needle Air needle Air tubing to provide sample headspace pressure Needle penetration depth adjustment screw Injection valve Digital Dispenser System Pump tubing Cassette Dispenser drain Sample tubing needle --> valve (port 2) Sample tubing valve (port 3) --> dispenser Sample loop Sample drain for loopfilling by sample headspace pressure. Replaces sample tubing (10) Vial stripper The silicon tubing connector with air inlet hole must be approximately at the same level as the liquid in the sample vial to prevent hydrostatic sample flow during analysis time. Air inlet hole in connector to prevent emptying of sample vial by hydrostatic suction. Needle connection nut Ferrule (PTFE) Sample needle connection hub Air seal 29 Needle Penetration Depth To keep rest volume small, the sample needle should stop close to the bottom of the sample vial. If penetration depth requires adjustment, proceed as follows (see Figure 8): Remove keyboard cover. • Place an uncapped vial in the tray. • Program an injection from that vial with injection volume 0 µL in case of partial loopfill injections or a loopvolume of 0 µL in case of flushed loop injections. Press START and disconnect the power supply as soon as the needle is in the vial. • Loosen adjustment screw one turn (counterclockwise). • Using the needle connection nut as a grip, adjust needle penetration depth: Needle should stop not less than 1 mm above the bottom of a standard vial and not less than 2 mm above the bottom of a conical vial. • Fasten adjustment screw (clockwise). • VIAL SENSOR MUST BE AROUND THE NEEDLE. • CLOSE KEYBOARD COVER. • Connect power. Needle Pair Replacement Sample Needle To replace sample needle proceed as follows: • 30 Remove keyboard cover. 03-914786-00:3 MAINTENANCE/SERVICE WARNING: MOVING PARTS Moving parts and sharp needle. Keep hands clear. ProStar 400 AutoSampler • Place an uncapped vial in the tray. • Program an injection from that vial with injection volume 0 µL in case of partial loopfill injections or a loopvolume of 0 µL in case of flushed loop injections. Press START and disconnect the power supply as soon as the needle is in the vial. • Loosen needle connection nut (Figure 8) that connects PTFE tubing to sample needle. • Move needle arm down manually. • Remove sample needle by pulling it out of its fitting with the PTFE tubing that usually sticks to the needle. • Put in new needle (watch the air seal around the needle). • When needle connection tubing needs replacement, loosen the nut that connects the tubing to the injection valve. • Cut the appropriate length of a 0.25 mm ID tubing taking care that cuts are made perfectly rectangular to avoid dead volumes. • Connect tubing to needle. • Connect loose end of needle connection tubing to port 2 of injection valve (use a Rheodyne ferrule.). Do not tighten excessively; it may close the tubing. • Check needle penetration depth and adjust if necessary. • Connect main power supply. • CLOSE KEYBOARD COVER. 31 Air Needle To replace air needle, proceed as follows: • Remove sample needle. • Unscrew air needle and install new air needle. • Reinstall sample needle. Dispenser Pump Tubing 32 • Loosen fitting that connects PTFE inlet tubing of dispenser to injection valve. • Remove pump tubing cassette including PTFE connection tubing, by loosening the screw that attaches the cassette to the dispenser. • Install new pump tubing cassette. • Check length of PTFE tubing. • Connect PTFE tubing to injection valve. 03-914786-00:3 Appendix Specifications ANALYTICAL Sample capacity 96 samples (92, when needle wash is used) Injection volume Flushed loop: 5 - 500 µL (dispenser controlled) 5 - >5000 µL (by headspace pressure) Injections per vial max 9 Analysis time max 99 min 59 sec Needle wash Selectable, 50 µL fixed volume between vials Headspace pressure Built-in compressor (0.5 atm or 7 psi) Switching time injection valve Electrically <100 msec PERFORMANCE Reproducibility Flushed loop injections: RSD ≤ 0.5 % Memory effect Better than 0.2 % ELECTRICAL Power requirements 115 Vac; ±10%; 50/60 Hz; 100 VA 230 Vac; ±10%; 50/60 Hz; 100 VA ProStar 400 AutoSampler 33 COMMUNICATION OUTPUTS INPUTS Inject marker Stop I/O Vial number BCD output Auxiliary 1 Auxiliary 1 inverted Auxiliary 2 Auxiliary 2 inverted Next injection input Next vial input Freeze runtime Stop I/O (Relays & TTL) (TTL) (TTL) (open collector) (open collector) (open collector) (open collector) (TTL) (TTL) (TTL) (TTL) OPTIONS Sample tray cooling Built-in Peltier cooling Temperature: 4°C (fixed) Accuracy: ± 2°C Operation range: Ambient - 25°C Ring temperature at relative humidity of 80% and ambient temperature of 31°C, decreasing to 50% at 40°C. Large Volume tray 48 positions for 5 mL vials (specify cool or nocool) PHYSICAL Dimensions ( W × D × H ) 300 mm × 440 mm × 283 mm 11.8 in × 17.3 in × 11.1 in Weight 15.5 kg (34 lbs.) 18.5 kg (41 lbs.), with cooling option 34 03-914786-00:3 APPENDIX Accessories Part Number Description 0391969190 ProStar 400 Startup Kit Includes: PEEK Tubing (10ft. x 0.01" ID), Package of 10 fingertight fittings and 2 mL Sample Vials (3 x 144) 0391968900 ProStar 400 Large Volume Option Allows injection volumes up to 4 mL. 48 Sample Vial Capacity Includes: Racks for 4 mL Vials, Serum Needle, Air Serum Needle, 500 µL sample loop, and PTFE tubing. 0392604590 Sync Cable Kit 0391993890 Integrator Interface Cable Kit 0190000804 Serum Needle for Standard Vials, Package of 3 0190000805 Air Serum Needle for Standard Vials 0190000836 Serum Needle for Large Volume Option, Package of 3 0190000837 Air Serum Needle for Large Volume Option 0392602714 ProStar 400 Plexiglas Tray Cover 0190000850 Pump Tubing Cassette, Single Channel R000088016 Air Needle R000088018 Liquid Sampling Needle, Package of 3 SAMPLE LOOPS 0190018200 5 µL SS Loop for Valco Valve 0190018202 20 µL SS Loop for Valco Valve 0392611011 50 µL SS Loop for Valco Valve 0190018204 100 µL SS Loop for Valco Valve 0392611012 250 µL SS Loop for Valco Valve 0190018205 500 µL SS Loop for Valco Valve 0392611013 1000 µL SS Loop for Valco Valve ProStar 400 AutoSampler 35 Part Number Description 0392611014 2000 µL SS Loop for Valco Valve 0392611015 5000 µL SS Loop for Valco Valve 0392611016 10 mL SS Loop for Valco Valve 0392611017 20 µL PEEK Loop for Valco Valve 0392611018 50 µL PEEK Loop for Valco Valve 0190018208 100 µL PEEK Loop for Valco Valve 0392611019 250 µL PEEK Loop for Valco Valve 0392611020 500 µL PEEK Loop for Valco Valve 0392611021 1000 µL PEEK Loop for Valco Valve 0392611022 2000 µL PEEK Loop for Valco Valve 2869450201 Package of 10 Valco Ferrules 2869450101 Package of 10 Valco Nuts 0392607983 Valco fingertight PEEK Nut 0392607984 Valco fingertight PEEK Ferrule VIALS, SEALS AND CAPS R0000542CV Standard clear crimptop 2-CV vial (pck/100) R005411AC6 Crimpcap for standard 2-CV and 1.1-CTVG vials. (pck/100) R05411CTVG Chromacol 1.1-CTVG conical vial with crimptop. (pck/100) R054TTS312 Chromacol TTS-312 support for 1.1-CTVG vial. (pck/100) R0000542SV Standard screwtop 2-SV vial. (pck/100) R0000548SC Screwcap for standard 2-SV vial. (pck/100) R005486RTI Septum for standard 2-SV vial. (pck/100) R05406PPCV Polypropylene crimptop vial 0.6 mL (pck/100) R000541201 Polypropylene septum caps for polypropylene vials (pck/100) R005402MTV 0.2 mL Insert to fit inside standard 2 mL crimptop vial, requires support sleeve R00054MTSA R00054MTSA Support sleeve for 0.2 mL insert 36 03-914786-00:3 APPENDIX Part Number Description RK60827510 Chromacol 10-CV, 10 mL vial. (pck/100) R0K7382420 Chromacol 20-ACB crimpcap and seal for 10-CV vial (pck/100) R0K6990111 Handcrimper 11 mm OD vials (standard) R0K6990120 Handcrimper 20 mm OD vials FOR STANDARD SAMPLE TRAYS Part Number Description Quantity 0394983500 Disposable 2 mL Vials, Screw Caps and Septa 1 gross 12 gross Glass 2 mL Vials, Screw Caps and Septa 1 gross 12 gross 6600010400 Amber Glass 2 mL Vials 1 gross 0099743106 0099743105 Tapered Glass 1.1 mL Vials (requires Teflon Support Sleeve) 500 50 6600012101 Precision 100 µL Vials 12 0099750301 Glass 200 µL inserts for 2 mL Vials Glass 100 µL inserts for 2 mL Vials 1000 1 gross Caps for all Vial Types Septa for all Vial Types 1 gross 1 gross 12 gross 0394983501 0390619590 0390619591 8830024200 1600069800 0390614901 0390614902 FOR LARGE VOLUME SAMPLE TRAYS 0190000839 4 mL Vials 0190000840 Caps for 4 mL Vials 0190000841 Septa for 4 mL Vials NOTE: The use of Eppendorf microcentrifuge tubes may cause malfunctioning of the ProStar 400 vial sensor. ProStar 400 AutoSampler 37
  • Page 1 1
  • Page 2 2
  • Page 3 3
  • Page 4 4
  • Page 5 5
  • Page 6 6
  • Page 7 7
  • Page 8 8
  • Page 9 9
  • Page 10 10
  • Page 11 11
  • Page 12 12
  • Page 13 13
  • Page 14 14
  • Page 15 15
  • Page 16 16
  • Page 17 17
  • Page 18 18
  • Page 19 19
  • Page 20 20
  • Page 21 21
  • Page 22 22
  • Page 23 23
  • Page 24 24
  • Page 25 25
  • Page 26 26
  • Page 27 27
  • Page 28 28
  • Page 29 29
  • Page 30 30
  • Page 31 31
  • Page 32 32
  • Page 33 33
  • Page 34 34
  • Page 35 35
  • Page 36 36
  • Page 37 37
  • Page 38 38
  • Page 39 39
  • Page 40 40
  • Page 41 41
  • Page 42 42
  • Page 43 43
  • Page 44 44
  • Page 45 45
  • Page 46 46
  • Page 47 47
  • Page 48 48
  • Page 49 49
  • Page 50 50
  • Page 51 51
  • Page 52 52
  • Page 53 53
  • Page 54 54
  • Page 55 55
  • Page 56 56
  • Page 57 57
  • Page 58 58
  • Page 59 59
  • Page 60 60
  • Page 61 61
  • Page 62 62
  • Page 63 63

Varian ProStar 400 Instrucciones de operación

Tipo
Instrucciones de operación