NOTICE: Varian, Inc. was acquired by Agilent
Technologies in May 2010. This document is provided
as a courtesy but is no longer kept current and thus
will contain historical references to Varian. For more
information, go to www.agilent.com/chem.
2700 Mitchell Drive
Walnut Creek, CA 94598-1675/usa
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.
03-914451-00:41 of 1
Page 4
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.
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.
03-914412-00:2
1 of 1
Page 5
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 Warning Description
Alerts you to situations that may
cause moderate injury and/or
equipment damage, and how to
avoid these situations.
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.
Alerts you to potentially hazardous
situations that could result in
serious injury, and how to avoid
these situations.
Very hot or cryogenically cold surfaces may be exposed. Use proper
03-914603-00:101 of 4
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.
Page 6
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.
2 of 4 03-914603-00:10
Page 7
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
manual.
Perform the tests for removable radioactive
contamination described in the Ni
Comply with leak test schedules and procedures.
63
ECD
63
ECD manual.
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 physicochemical 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.
03-914603-00:103 of 4
Page 8
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
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.
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, 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
4 of 4 03-914603-00:10
Page 9
Sicherheitsinformationen
G
G
A
R
E
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
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, ACHTUNG und WARNUNG, wie unten beschrieben. Es ist wichtig, daß
HINWEIS
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.
ACHTUN
Warnungssymbol Warnungsbeschreibung
WARNUNG
ELEKTRISCHER
G
SCHL
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
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
WARNUNG
EXPLOSIONSGEFAH
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.
Weist auf mögliche Gefahrensituationen,
die zu ernsthaften Verletzungen führen
können und auf die Vermeidung dieser
Situationen hin.
WARNUN
WARNUNG
STRAHLUNGSQUELLE
WARNUNG
BEWEGTE TEIL
03-914603-81:101 of 4
Es besteht eine ionisierende Strahlungsquelle. Beachten Sie die Vorschriften
im Handbuch für eine gefahrlose Benutzung.
Bleiben Sie mit Ihren Händen und Fingern weg.
Page 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.
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 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.
2 of 4 03-914603-81:10
Page 11
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 Detektorfunktion 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
63
Ni
ECD Handbuch.
Führen Sie die Tests für zu beseitigende radioak-
tive Kontamination durch, die im Ni
buch beschrieben sind.
Erfüllen Sie die Zeitpläne und Verfahren zur Di-
chtigkeitsprüfung.
63
ECD Hand-
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.
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 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 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 Inspizieren der Lichtquelle oder der Flüssigkeitszelle
benutzen Sie immer einen wirksamen Augenschutz,
wie er durch Borsilikatglas oder Polystyrol gewährleistet wird.
03-914603-81:103 of 4
Page 12
Verfügbarkeit von Ersatzteilen
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.
Serviceverfügbarkeit
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
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
4 of 4 03-914603-81:10
Page 13
Informations et mesures de sécurité
A
S
E
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
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.
NOTES,MISESENGARDEetAVERTISSEMENTS.Il est important de faire fonctionner ce
NOTE
Information destinée à tirer le
meilleur parti du matériel sur le plan
des performances
Symboles d’avertissement Description
TTENTION
RISQUE
D'ELECTROCUTION
ATTENTION
RISQUE DE BRÛLURE
ATTENTION
RISQUE D'INCENDI
ATTENTION
RISQUE D'EXPLOSION
ATTENTION
SOURCE DE RADIATION
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
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.
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 potentiel d’incendie. Se conformer aux instructions du manuel pour faire
fonctionner le matériel en toute sécurité.
Risque potentiel d’explosion en raison du type de gaz ou de liquide utilisé.
Présence d’une source de radiation ionisante. Se conformer aux instructions du
manuel pour faire fonctionner le matériel en toute sécurité.
Attire l’attention sur une situation
potentiellement dangereuse pouvant
occasionner des dommages corporels
importants et indique comment
remédier à cette situation
ATTENTION
PIECES EN MOUVEMENT
03-914603-82:101 of 4
Garder les mains et les doigts hors de portée.
Page 14
Précautions générales en matière de sécurité
N
N
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
ATTENTIO
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
ATTENTIO
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.
2 of 4 03-914603-82:10
Page 15
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
63
Ni
, en particulier à ses NOTES, MISES EN
GARDEET AVERTISSEMENTS.
Effectuer les tests de décontamination radioactive
décrits dans le manuel d’utilisation de l’ECD Ni
Se conformer aux procédures et au calendrier des
essais d’étanchéité.
63
.
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, MISESENGARDEET
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.
03-914603-82:103 of 4
Page 16
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
4 of 4 03-914603-82:10
Page 17
Informazioni sulla Sicurezza
E
E
i
o
i
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
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,
NOTA
Sono informazioni utili ad ottenere
le prestazioni migliori da parte
dello strumento.
Segnali di ATTENZIONE Descrizione del Pericolo
ATTENZIONE
Pericolo di folgorazion
ATTENZIONE
Pericolo discottature
ATTENZIONE
Pericolo di incendi
ATTENZIONE
Pericolo di esplosioni
Allerta l’operatore su situazioni che
potrebbero causare ferite leggere e
danni limitati allo strumento ed il
modo di evitarle.
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.
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.
Pericolo potenziale di incendio. Seguire le istruzioni del manuale per
lavorare con una maggiore sicurezza.
C’è pericolo di esplosioni a causa del tipo di gas o liquido utilizzato.
ATTENZION
Allerta l’operatore su situazioni
potenzialmente pericolose che
possono causare danni molto seri ed
il modo di evitarle.
ATTENZION
ATTENZIONE
Pericolo di radiazion
E’ presente una radiazione ionizzante. Seguire le istruzioni del
manuale per lavorare con una maggiore sicurezza.
ATTENZIONE
Parti in movimento
03-914603-83:101 of 4
Non tenere le mani o le dita vicino.
Page 18
Norme di Sicurezza
E
E
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
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
Questo strumento è progettato per l’analisi cromatografica di campioni opportunamente
ATTENZION
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.
2 of 4 03-914603-83:10
Page 19
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
Eseguire tutti i test di contaminazione radioattiva
rimovibile descritti nel manuale dell’ECD al Ni
Rispettare tutte le procedure e le scadenze di
verifica per eventuali perdite.
63
.
63
.
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 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
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.
03-914603-83:103 of 4
Page 20
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
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 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.
disponibilità.
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
4 of 4 03-914603-83:10
Page 21
Instrucciones de
!
SCARG
A
C
A
A
A
S
O
O
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
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, PRECAUCION, y ATENCIONcomo se indica más abajo.Es importante que utilice
NOTA
Información para ayudarle a
obtener unas prestaciones óptimas
de su instrumento.
Símbolo Descripción
ATENCIÓN
PELIGRO DE
DE
ELÉCTRI
ATENCIÓN
PELIGRO DE
DUR
QUEM
ATENCIÓN
PELIGRO DE FUEG
ATENCIÓN
PELIGRO DEEXPLOSIÓN
ATENCIÓN
PELIGRO DE RADIACIÓN
Le alerta de situaciónes que pueden
causar daños moderados a la salud
ó al equipo, y cóm evitar esas
situaciones.
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.
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.
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.
¡PRECAUCION
Le alerta de potenciales situaciones
peligrosas que pueden causar serios
daños, y cómo evitar esas
situaciones.
ATENCIÓN
PARTES EN MOVIMIENT
Mantenga alejados los dedos y las manos.
ATENCINÓ
03-914603-84:101 of 4
Page 22
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.
ATENCINÓ
ATENCINÓ
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.
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.
2 of 403-914603-84:10
Page 23
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 ATENCIONdel Manual del
Detector Ni
Realice los test de contaminación radioactiva
descritos en el Manual del Detector Ni
Cumpla con los plazos y procedimientos de test de
fugas.
63
ECD.
63
ECD.
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
ATENCIONdel 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.
03-914603-84:103 of 4
Page 24
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)
This is a brief summary of the steps that must be completed for
the proper installation of your ProStar 345 detector. Complete
installation information is provided in the next section.
• Unpack and inspect your instrument
• Read the Safety Information at the front of this manual
• Position the detector appropriately
• Select voltage and check fuses
• Connect the power cord
• Complete rear panel connections
• Connect the flowcell
• Switch on the instrument
• Check initial response to power-on
• Check operation with a test sample
Manual Conventions
This manual uses several conventions. Among them are menu
displays, text conventions (brackets, slashes, etc.), standard
words, and several different icons.
ProStar 345 UV-Vis Detector 1
Page 30
Displays
Text
Displays with two lines or less are shown in the manual as they
appear on the instrument. Frequently the two lines shown on the
display are only part of a longer display. In this manual, displays
having more than two lines are represented as in the screen
below.
Zero on λ change Yes
Cursor Speed Medium
-----------------------------------------
Status Lock Off
READY Output Active Hi
Three typographic conventions are used to differentiate between
keys, menus, and fields.
Brackets, Slashes, and Capitalization
Brackets, [ ], indicate instrument keys. For example: Press
[MENU].
Slashes, / /, are used around menu choices, e.g.,
Menu, select /FILES/.
From the Main
Capitalization is used to make field and menu names appear just
as they do on the display. Generally the first letters of field
names are capitalized. For example:
Select /FILES/, /Copy/, Copy File #.
Standard Words
For the purposes of this manual, the meanings of two words:
“select” and “enter” have been standardized.
Select is used when you need to choose from among available
options. For example, to “select” a particular menu choice, you
would move the cursor to the appropriate choice and press
[ENTER]. To “select” a field entry, move the cursor to the
03-914784-00:2
2
Page 31
I
appropriate field and use the [+] and [-] keys to scroll to the
desired preset value.
is used when you need to specify individual alphanumeric
Enter
digits. To “enter” a particular value, move the cursor to the
desired field and use the [+] and [-] keys to increment or
decrement each digit in the field until the desired value or letter
appears.
NTRODUCTION
ProStar 345 UV-Vis Detector
3
Page 32
03-914784-00:2
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Page 33
Installation
Unpacking
Carefully remove the detector from the shipping container and
inspect both the detector and packing for any signs of damage.
Keep the shipping container as it provides excellent protection
for your detector for any future transit or storage.
Any evidence of damage should be reported immediately to the
carrier and to:
Varian Chromatography Systems
2700 Mitchell Drive
Walnut Creek, CA 94598-1675
Attention: Customer Service
1-800-FOR HPLC or your local Varian office
Check the contents against the enclosed packing list. Any
discrepancies or missing items should be reported to the carrier
and to Varian.
Installation
The following tools are required for installation:
• narrow-tip screwdriver (2 mm wide)
• #2 Phillips screwdriver
The ProStar 345 detector is a sensitive instrument and should
always be handled with the degree of care appropriate to
ProStar 345 UV-Vis Detector 5
Page 34
laboratory instrumentation. After unpacking, place the detector
near the column outlet to minimize the length of tubing
necessary for connection to the flowcell inlet. The flow cell
compartment is on the left when facing the front of the ProStar
345. For normal operation, the detector should be located on a
firm flat surface away from:
• heat sources (such as direct sunlight or a heater vent)
• drafts (such as an open doorway, window, or air-conditioner
• smoke or other vapor
• corrosive or dusty atmosphere
• vibration
• potential liquid spills
Allow at least five inches of clear space at the back of the
instrument to allow a free flow of cooling air through the detector
and access to the rear panel.
Voltage Selection
The detector is shipped with the voltage and fuses preset for 110
Vac. Verify the setting by looking through the cut-out window on
the voltage selector cover, Figure 1. The cover is located at the
bottom left of the detector rear panel. If the voltage setting
satisfies your local site requirements, skip to Fuses, page 9. If
not, proceed to the next section
vent)
WARNING
Do not plug in the instrument without first verifying that the voltage is properly set for
your location. Never run the detector at more than 10% below the nominal line voltage.
Ensure that the voltage selector at the back of the instrument is
set correctly before making electrical connections. Turn the
detector so that you are facing the rear panel.
03-914784-00:2
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Page 35
I
The connector for the power cord is at the lower left corner. The
voltage selector cover panel, above the power connector,
displays the current voltage setting through a cut-out panel. The
voltage selector was factory set to the for the line voltage at the
detector destination. If the voltage setting is not correct for your
area, you must set it correctly before proceeding.
Insert screwdriver blade into slot. Pry open.
NSTALLATION
120Vac
A. Power Connector/Voltage Selector with access
panel closed.
Figure 1 Power Connector/Voltage Selector
1. Insert a small screwdriver blade into the slot at the top
of the voltage selector access panel and gently pry the
panel downward. Once unlatched, the panel will swing
downward to reveal the voltage selector barrel and the
two fuses.
100 Vac
120Vac
220 Vac
B. Power Connector/Voltage Selector with access
panel open.
ProStar 345 UV-Vis Detector
7
Page 36
Current
Voltage
Selection
VoltageSelector
Drum
Fuse
Holder
Figure 2 Voltage Selector and Fuse Holders
2. Remove the voltage selector barrel from the detector.
The selector resembles a drum imprinted with four
settings: 100, 120, 220, and 240V.
3. Rotate the barrel such that the desired voltage setting
will be visible through the cut-out in the cover when
replaced.
DT-Z026E/DG
4. Replace the barrel in the detector. Before closing the
cover, check the fuses according to the procedure
below.
03-914784-00:2
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Page 37
I
Fuses
Verify that your detector is fitted with the correct fuses.
1. Pull each fuse holder straight toward you. The fuse
holders are the black squares with arrows located
directly beneath the voltage selector.
2. Remove each fuse from its holder. Check the fuse
amperage, voltage, and type according to the following
description. You should have either:
two 2-amp, sloblow fuses (for 100/120V), or
two 1-amp, sloblow fuses (for 220/240V)
3. Assuming that you have the proper fuses, reinsert them
and the fuse holders, making sure that the arrows on
the holders point the same direction as the arrow on the
cover panel.
NSTALLATION
4. Close the cover panel by swinging it upward and
pressing it in until it snaps shut. The correct voltage
should appear in the cut-out opening.
CAUTION
To avoid damaging the instrument, verify that the new voltage setting (displayed in the
cut-out window) is correct before you switch on power.
Rear Panel Connections
Attach the power cord at the lower left of the detector rear panel.
Do not switch on the power yet. Locate the two in-line
connectors (8-pin and 12-pin) in your accessory kit and insert
them in the appropriate sockets on the detector rear panel,
Figure 3 or Figure 4. Note that the connectors are both keyed to
their sockets, making it impossible to insert them incorrectly.
ProStar 345 UV-Vis Detector
9
Page 38
Figure 3 ProStar 345 Analog-Input Connections
The larger connector (Figure 3) is for analog inputs. It allows the
detector to communicate with other devices in your liquid
chromatographic system. The smaller connector (Figure 4)
delivers two analog outputs (CH1 and CH2). Use the cables
supplied with your detector to complete the connections
described in this section. For each connection, loosen the small
setscrew located next to the appropriate terminal, insert the
cable bare wire, and hold it in place while you tighten the screw.
Figure 4 ProStar 345 Analog-Output Connections
03-914784-00:2
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Page 39
I
NSTALLATION
Connecting an Integrator, Workstation, or Recorder
Connect your integrator/workstation to the 1.0V F/S and
corresponding ANALOG GND terminals.
NOTE: The 0.01 and 0.10V F/S terminals are provided for recorders and special
applications. We recommend that you use only the 1.0V F/S terminal for
an integrator or workstation.
Connect the positive input from your recorder to the full-scale
voltage (0.01, 0.10, or 1.0V) appropriate for your recorder.
Connect the recorder floating-ground input to the corresponding
ANALOG GND terminal.
NOTE: Do not connect the detector ANALOG GND to any earth ground on your
recorder. This would lead to creation of a ground loop resulting in an
increased noise level and a decrease in sensitivity.
Remote Communications Connections
The ProStar 345 can accept inputs from, and send inputs to,
remote devices through the Analog Output connector, Figure 4.
If your chromatographic system has programmable timed events
you can use one to zero the detector signal automatically during
a run.
The terminals available on the ProStar 345 remote
communications connector are labeled STOP, RUN/START, and
ZERO (each with a ground terminal), and Accessory Relay.
STOP You can use a timed event from your
chromatographic system to take the detector out
of run by connecting the system event to the
detector STOP and ANALOG GND terminals.
RUN/START You can use the remote-start event on your
injector or autosampler to put the detector into
run automatically whenever an injection occurs
by connecting the event to the detector
ProStar 345 UV-Vis Detector
11
Page 40
ZERO You can zero the detector signal automatically
NOT READY The detector is capable of driving one TTL load
Flowcell Connections
1. Although the flowcell assembly is located behind the forward
enclosure (Figure 5) you need not remove the enclosure to
connect your inlet and outlet lines.
2. Using finger-tight nut and ferrule sets connect the column
outlet directly to the detector fluid inlet on the left side of the
flowcell, Figure 5. If additional tubing is required to reach
the inlet, use a zero dead-volume union.
RUN/START and ANALOG GND terminals.
by connecting a timed event on your
chromatograph to the detector ZERO and
ANALOG GND terminals.
through the NOTREADY terminals each time it
goes to its READY state. This ability to signal
other instruments is particularly useful with
autosamplers, where the detector can signal
that it is ready for the next injection in an
automated series of runs. To hook up the
NOTREADY terminals, connect the one input
lead from the other instrument to the detector
NOTREADY and GROUND terminals.
3. Connect the detector fluid outlet to the supplied lowpressure union and waste tubing.
NOTE: If you have several detectors hooked up in series, place the ProStar 345
closest to the column outlet; its flowcell can withstand high pressure.
4. Replace the side enclosure of the detector, making sure that
the tubing passes through the slots without being pinched.
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Photodiode Mount
Flowcell
NSTALLATION
DT-Z065E\DT
Figure 5 ProStar 345, Inside the Side Enclosure
Optional Flowcells
Several different flowcells are available for use in different
applications. Each flowcell has distinct design characteristics
and performance specifications. These characteristics are
compiled in Table 1.
ProStar 345 UV-Vis Detector
13
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Table 1 Design and performance specifications for optional flowcells
Flowcell Path length
(mm)
Analytical LC 6 9 .01 SS 50 68
Analytical LC 10 15 .01 SS 50 68
Microbore 3 1.2 .005 SS 10 68
Microbore 6 7 .007 SS 20 68
Semi-Prep 3 4.5 0.02 SS 100 68
* All cells have sapphire windows. All but the prep cells have a heat exchanger.
Volume
(µL)
Tubing Dia
(in.)
Material* Max Flow
(mL/min)
Max Press
(bar)
Flowcell Orientation
The flowcell shipped with your ProStar 345 detector is properly
oriented on its black-anodized backing plate. However, should
you subsequently order one or more additional cells to enhance
the versatility of your instrument, the cell(s) you receive may be
configured for vertically-oriented applications. As shown in
Figure 6, this orientation is characterized by the photodiode
standoffs being positioned at the upper right and lower left
corners of the flowcell assembly and the tapered cut-away areas
being positioned at the top and the right of the assembly.
In order to use any of the vertically-oriented flowcells with your
ProStar 345, you must remove the two flowcell mounting screws
and rotate the flowcell 90° on the flowcell holder as described in
the following instructions.
Figure 7 shows the vertically-oriented flowcell as shipped. Note
the vertical orientation of the flowcell inlet and outlet connections
relative to the photodiode standoffs and the tapered cut-aways at
the top and right of the cell holder.
NOTE:
Figure 6
and
Figure 7 show the tubing clamp as an aid
to the proper
positioning of the inlet and outlet tubes. The tubing clamp is actually
mounted on the detector and is not part of the flowcell assembly. To
ensure proper alignment, always hold the cell holder and flowcell in the
orientation shown in the illustrations.
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NSTALLATION
Inlet Tube
Tubing Clamp
(on
verticallyoriented
detectors)
Mounting
Screws
Figure 6 Alignment of vertically-oriented flowcells
Re-orienting the Flowcell
Use the following steps to re-orient a flowcell:
1. Remove the two Phillips-head mounting screws that secure
the flowcell to the black-anodized flowcell holder and set
them aside.
2. Maintaining the flowcell in the vertical position shown in
Figure 6 and Figure 7, rotate the black cell-holder 90°
clockwise. Don’t rotate the flowcell body itself. Part B of
Figure 7 shows the cell holder in its new horizontallyoriented position. Note, in particular, the new position of the
photodiode standoffs and the tapered cut-aways.
Outlet Tube
Photodiode
Standoffs
A.
DET\Z014\FM
3. Reattach the flowcell body by replacing and securing the
4. Bend the inlet and outlet tubes gently as shown in Part C of
ProStar 345 UV-Vis Detector
mounting screws.
Figure 7. The inlet tube (wound around the cell body) should
always enter at the bottom of the flowcell; the outlet tube
should always exit at the top of the flowcell.
15
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Photodiode
Standoffs
Tubing Clamp
(on horizontallyoriented detectors)
Cell Holder
Outlet Tube
Inlet Tube
B.C.
Mounting Screw
Holes
Figure 7 Changing the Alignment of a Vertically-Oriented Flowcell
Turn the cell holder as shown in Part B. Align the inlet and outlet
tubes with the tubing clamp as shown in Part C.
Using the ProStar 345
This section describes the three basic rules for using your
ProStar 345 detector. It also introduces the instrument and
describes the conventions in this manual. Before you start this
section, read the Safety Information located at the beginning of
this manual and install your detector as described on the
previous pages. While you read these descriptions, you can
explore the general architecture of the ProStar 345 menus and
screens, using the Menu Tree, page 103.
Finding Your Way Around
When using your ProStar 345 detector, remember these three
rules:
1. The arrow keys, [] [] [] [] move the cursor in the
direction printed on the key.
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NSTALLATION
NOTE: Press [MENU] to move quickly to the top of the menu structure.
2. The shape of the cursor determines how a selection is
made:
If a
triangular
If a
blinking square
cursor appears, press [ENTER]
cursor appears, press [+] or [-] to change
values. Depending on the field, you will scroll up or down
through preset choices, or change alphanumeric entries one
letter or digit at a time.
3. There are four ways to accept (and automatically save) an
entry. Just move the cursor out of the field by any of the
following methods:
• Pressing [ENTER].
• Using the arrow keys: [] [] [] []
• Pressing [MENU].
• Pressing [STATUS].
NOTE: You cannot leave a menu if there are errors present or if all necessary
entries are not completed.
Visual Clues
The following conventions are used on the ProStar 345 display:
ProStar 345 UV-Vis Detector
1. Top-level menu choices are displayed in CAPITAL
letters.
2. A square cursor in a field () changes to an underscore
cursor (_) when you scroll through preset choices or
enter numerical values and characters.
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Instrument Control
START
STOP
ZERO
STATUS
+
_
MENU
ENTER
Menus and control operations are accessed from the key pad
and two-line display on the front panel. A brief explanation of the
keys and the main menus and screens follows.
The keypad of each ProStar 345 detector consists of twelve keys
Four keys directly control the ProStar 345 operation: [START],
[STOP], [STATUS], and [ZERO]. The remaining keys either
access commands, [MENU] and [ENTER], or are used to set
parameters and move around the display: [] [] [] [] [+] [-].
3. A solid down-arrow () on the right side of some
displays indicates that the current menu continues on
additional screens. To access additional menu lines,
press the down-arrow key, [].
4. The last line of a longer menu is frequently a blank
display line without a solid down-arrow, ().
Figure 8 The ProStar 345 Keypad
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NSTALLATION
[START]
[STOP]
[STATUS]
[ZERO]
[MENU]
[ENTER]
[] [] [] []
[+] [-]
Pressing [START] begins a run. The detector must be in the READY state (or
QREADY if a queue is loaded), indicating that the detector is stabilized and
waiting to begin a run.
Pressing [STOP] halts a run, stops the internal clock, and returns the detector
to a READY state. If a wavelength program is operating, pressing [STOP] halts
the program and returns the detector to its initial conditions.
Pressing [STATUS] displays the Status Screen. From the Status Screen you
can monitor the run in progress. You can also access the Status Menu.
Pressing [ZERO] resets the detector output to zero volts, plus or minus any
offset.
Pressing [MENU] displays the Main Menu
Pressing [ENTER] accepts a selected choice or menu entry. The [ENTER] key
also advances the cursor to a new field, either on the same line of the display
or in the line below.
Pressing any arrow key moves the cursor in the direction indicated on the key.
The up and down arrow keys also move the cursor between menus and
displays.
Pressing the [+] and [-] keys scrolls the available choices in a field or changes
the value of alphanumeric entries. Holding down either key will continuously
scroll the list of choices forward or backward until you release the key.
In fields that require numerical entries, the value of each digit is increased or
decreased by one unit each time you press the [+] or [-] key. In fields that
accept either numeric or character entries, the [+] and [-] keys scroll through
the alphabet from A to Z, then through the numbers 0 to 9, and finally to a
slash, hyphen, and blank space.
In other fields, the [+] key advances you through a preset list of choices while
the [-] key takes you backward through the list.
ProStar 345 UV-Vis Detector
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Menus, Screens, and Messages
The ProStar 345 display shows three kinds of information:
menus, screens, and messages. Menus require you to make
selections or enter specific values. Screens display information
that cannot be edited. Messages confirm actions and point out
errors. The Menu Tree on page 103 outlines the structure and
content of the detector menus and screens, three of which are
discussed here.
Main Menu
The Main Menu is the top level of the menu structure. It gives
you access to five menus: FILES, QUEUE, TESTS,
COMMANDS, and OPTIONS. To see the Main Menu, press the
[MENU] key at any time.
FILES QUEUE TESTS
COMMANDS OPTIONS
From the Files Menu you can edit, load, copy, or delete files. The
Commands Menu lets you insert an event mark onto your
chromatogram, short outputs, or shut down the detector. The
Tests Menu lets you run built-in instrument tests and diagnostics.
In the Options Menu you can set up or change your instrument
configuration. From the Queue Menu you can edit or change the
order of files in the sample queue. See the sections on
Operations, Advanced Operations
Troubleshooting
for more information on menus.
and
Maintenance
Basic
and
Status Screen
The Status Screen displays the detector status, wavelength
setting, and the absorbance reading. It appears automatically
whenever the instrument is powered on or the [STATUS] key is
pressed. No entries are made on the Status screen.
Status λ AU
READY 250 0.00001
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Status Menu
Just below the Status Screen is the Status Menu. To access the
Status Menu, press [] from the Status Screen. The Status
Menu lets you review and edit run parameters during a run. See
Basic Operations
for more infomration on Status Menus.
Messages
There are three kinds of messages that can appear on the
display: user messages, confirmation messages, and error
messages.
User Messages
User messages, indicated on the display by two sets of double
asterisks, tell you about an existing instrument condition or ask
for further actions. Some of these messages will only appear on
the display for three seconds. An example of a message
requiring further action is shown below.
NSTALLATION
** Protected File **
No Editing Allowed
Confirmation Messages
Confirmation messages also indicated on the display by two sets
of double asterisks, appear for one second after an operation
has been carried out successfully.
** File Loaded **
Error Messages
Error messages are indicated on the display with capital letters
and two sets of double exclamation points. Error messages are
shown when a condition exists that prevents completion of an
operation. Error messages remain on the display until you press
a key.
!! RAM ERROR !!
ProStar 345 UV-Vis Detector
21
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Basic Operation
A Quick Example
This example shows how to prepare a file and how to load the
file into the detector operating parameters. After a practice run,
we will add a stop-time. To keep the instructions simple, we will
use the single-wavelength mode.
You may wish to keep the Menu Tree in the Appendix on hand
as you work through this example. If you lose your place at any
time, you can:
1. Press [] to move back to a previous screen.
2. Or, press [STATUS] to return to the Status Screen and
retrace your steps.
Startup
Set the power switch (on the rear panel) to On. After a series of
power-up tests, the Status Screen appears on the display. The
Status Screen is discussed after operating parameters have
been set up.
Status λ AU
READY 250 0.00001
Setting Parameters
Parameters are set in an edit file. To access the Edit Menu and
prepare the file:
ProStar 345 UV-Vis Detector 23
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1. Press the [MENU] key. The Main Menu is displayed.
FILES QUEUE TESTS
COMMANDS OPTIONS
2. Select /FILES/ to display the Files Menu.
Edit Load
Copy Delete
3. Select /Edit/ to display the Edit Menu .
Edit File 1
File name
---------------------------------------
Wavelength Program
Options
This example uses a file designation of 1 and the File Name field
is left blank.
Wavelength
Wavelength is an example of a field that requires a numeric
entry. To set each wavelength:
1. From the Edit Menu select /Wavelength Program/ to display
the Wavelength Program.
Time Wavelength
0.00 254
2. Scroll to the Wavelength field. Using the [+] and [-] keys, set
each wavelength field to the desired setting for your
analysis. Each digit must be edited individually.
3. Press [ENTER] to accept the new wavelength settings.
Range
Range is an example of a field with a preset list of choices. Note
that Range 1 and Range 2 correspond to the Analog Outputs 1
and 2 on the rear panel. To set Range:
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1. Select /Options/ from the Edit Menu to display the Options
Menu.
Rise Time 1.0
Autozero Time 0.00
---------------------------------------
Range 1 1.0
Range 2 1.0
2. Move the cursor to Range 1 using []. With the [+] or [-]
key, select the desired setting from the list of choices.
3. Press [ENTER] to accept the new Range 1 setting.
For this example, default settings are used for the remaining
parameters. You will learn more about setting these parameters
in
Basic Operations
.
Loading the File
ASIC OPERATION
You are now ready to load the settings from File 1 into the
ProStar 345 operating parameters. To load the file:
1. Return to the Files Menu using [].
2. Select /Load/. The screen following appears.
Load File 1: (filename)
3. You will be able to select from several files in the Load File
** File Loaded **
The Status Screen is displayed, ready to run the detector.
ProStar 345 UV-Vis Detector
field. Depending on whether or not your detector has ever
been used before, these files will either contain previouslystored settings or default settings. Use [+] and [-] to move
the cursor through the available choices. When the file you
wish to load appears, (we are using the default settings for
this example), press [ENTER] to execute the load command.
The confirmation message shown below appears for one
second.
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Practice Run
The Status Screen now displays your wavelength setting, the
detector status, and the absorbance reading. If the Status reads
READY, the detector is stabilized and ready to run. If NRDY (Not
Ready) appears, the detector lamp may need additional time to
warm up.
When the detector is stabilized:
1. Press the [ZERO] key to zero the detector analog output
signal.
2. Inject your sample.
During this setup, there was no stop time entered in the detector
parameters. In this case, the detector stays in the READY state
and continually monitors the column eluant. You do not need to
manually start or stop a run with this set-up.
Adding a Stop Time
To add a stop-time, you need to use the following steps to
modify the detector operating parameters. Then start and stop a
run with the new setting.
1. From the Status Screen, press the [] key to move down to
the Status Menu which is the programming area below the
Status Screen.
File 1:
---------------------------------------
Time λ1 λ2
0.00 250 280
Rise Time 1.0
Autozero Time 0.00
Range 1 1.0
Range 2 1.0
2. Using the [] key, move the cursor to the blank line below
the 0.00 time line and press [+]. This adds a second line,
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with a time of 1.00 and the same wavelength settings as the
first. Change 1.00 to the desired stop-time for the run, and
leave the wavelengths unchanged.
3. To save your changes to the file, scroll down to the words
“Save File” (which now appear below PMT Voltage), and
press [ENTER].
The message shown below appears and the Status Screen is
displayed.
** File Saved **
Once a stop time is entered, the run is started with each
injection. To do this:
1. Zero the detector analog output signal by pressing the
[ZERO] key.
2. When the detector is stabilized, inject sample and press
[START].
ASIC OPERATION
Notice that Status now shows the run time. To stop your run
before the set stop-time, press [STOP].
NOTE: Your display values may differ from those presented in this manual,
especially if the detector has been programmed previously.
Single and Dual Wavelength Operation
You can operate the detector in either single or a dual
wavelength mode. In the dual-wavelength mode, the detector
simultaneously monitors two wavelengths in a single run in either
the UV range or the visible range.
To perform a single or dual wavelength operation, you need to
be able to identify and enter a file, load that file into the detector
current operating parameters, and start and stop a run. This
section will also show you how to modify the detector current
operating parameters.
ProStar 345 UV-Vis Detector
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Setting Parameters
File Identification
Before setting any detector parameters, the file to be edited must
be identified. To do this, access the Files Menu by first pressing
[MENU].
The Main Menu is displayed. Select /FILES/.
Edit Load
Copy Delete
Select /Edit/ from the Files Menu to display the Edit Menu.
Edit File 1
File name
--------------------------------------
Wavelength Program
Options
Enter the number of the file to be edited in the Edit File field. The
ProStar 345 can store up to four files in memory, so file numbers
from 1 to 4 are allowed. You may also enter a name of up to
eight characters in the File Name field.
In /Edit File/, the file choices of “S” and “D” represent Scan and
Develop files, respectively. These files are some of the
advanced features described in
Advanced Operations
.
Wavelength Program
From the Edit Menu, select/Wavelength Program/. The
Wavelength Program designates dual or single wavelength
operation, and also contains a table of time and wavelength. A
wavelength program for dual-wavelength operation appears
below.
Program Dual λ (190-450)
----------------------------------------
Time λ1 λ2
0.00 250 280
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Select Single λ, Dual λ (190-450) or Dual λ (366-700) in the
Program field. The table for time and wavelength(s) will appear.
(For single-wavelength operation, there is only one wavelength
field.)
You can operate with either a one-line or a two-line wavelength
program. Using a one-line program, the detector is always in the
READY state and you can monitor the chromatographic eluant
continually. Using a two-line program, you can add a stop-line
and you can start and stop the detector during a
chromatographic run. (Stop-lines are useful, for example, in a
series of automated runs where you want to autozero the
detector baseline after each injection.)
For a one-line program, enter the wavelength(s) for your analysis
in the λ1 and λ2 (or Wavelength) fields that correspond to the
time of 0.00.
For a two-line program, add an additional line (the stop-line) by
scrolling down to the blank line below the time 0.00 line and
pressing. [+]. The second line automatically will have a time
setting of 1.00 and the same wavelength setting(s) as the first.
Change 1.00 to the desired stop-time for the run, and leave the
wavelength value(s) unchanged.
ASIC OPERATION
An example of a dual-wavelength, nine-minute run at 254 and
283 nm is shown.
Time λ1 λ2
0.00 254 283
-----------------------------------------
9.00 254 283
Options
Select /Options/ from the Edit Menu to display the Options Menu.
Use this menu to set the detector rise time, autozero time, and
ranges.
ProStar 345 UV-Vis Detector
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Rise Time 1.0
Autozero Time 0.00
-----------------------------------------
Range 1 1.0
Range 2 1.0
Rise Time
This field affects the detector response time. Rise time is
inversely proportional to the amount of baseline noise. For
example, the longer the rise time, the less noise detected. The
two-second default value is appropriate for most applications.
NOTE: To minimize baseline noise while retaining maximum resolution, select a
rise time at least one-tenth of the peak width at the base of the narrowest
peak of interest.
Autozero Time
This parameter tells the detector when to perform an automatic
zero of the baseline. If you don’t want to set an automatic
autozero and you are using a stop-line in your wavelength
program, simply set the autozero time to a value greater than
your stop-time.
NOTE: It is good practice to zero the detector automatically at the start of each
run. This will keep the detector output in range throughout an automated
series of runs.
Range 1 and 2
These parameters range the signal from Analog Output 1 and
Analog Output 2 (shown as CH 1 and CH 2 on the detector rear
panel). Set each range to an appropriate full-scale absorbance
for your sample.
NOTE: We recommend a range of 1.0 when you are using an integrator or data
system.
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Loading a File
When you’re ready to load a file, select /Load/ from the Files
Menu. The screen will display the words “Load File 1:(filename).”
Enter the desired file number and press [ENTER]. The message
shown below will appear for one second. You are then returned
to the Status Screen.
** File Loaded **
Running The ProStar 345
Once detector parameters have been set in the designated file
and the file loaded into the detector operating parameters, you’re
ready to run your analysis. First check the detector status by
pressing [STATUS] to view the Status Screen. If you’re using a
stop-line in your wavelength program, you’ll start and stop the
run with each injection.
Status Screen
ASIC OPERATION
You can check the detector status, wavelength setting(s), and
absorbance reading(s) by pressing [STATUS] to view the Status
Screen. The Status Screen for the Model 205 in dual-wavelength
mode appears.. Note that, in the single-wavelength mode, the
third line does not appear.
Status λ AU
READY 250 +0.00001
-----------------------------------------
280 -0.00001
If the Status reads READY, the detector is stabilized and ready
to run. If NRDY appears, the detector lamps may need additional
time to warm up, or a wavelength outside the selected lamp
range may have been chosen.
Inject Sample
When the detector is stabilized and you are ready to inject
sample, manually zero the detector by pressing [ZERO].
ProStar 345 UV-Vis Detector
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Starting a Run
If you are not using a stop-line in the wavelength program, the
detector remains in the READY state throughout your
chromatographic runs. When using a stop-line, you must start
and stop the run with each injection, following the procedures in
the next few pages.
When using a stop-line in your wavelength program, you need to
start the run with each injection. There are two ways to start a
run using the ProStar 345:
1. Manually, by pressing [START] each time you make an
injection.
2. Automatically, by interfacing the detector with a remote runsignal from the injector (see
scenario, a signal equivalent to pressing the START button
is sent from the injector to the detector automatically with
each injection.
Installation
for details). In this
During the run, you can monitor the run time from the Status
Screen.
Stopping a Run
There are two ways to stop a run:
1. Manually, by pressing [STOP] before the programmed stop
time.
2. Automatically, by allowing the run to finish at the preset
time.
If you are conducting a dual-wavelength run, you can also stop
the run by loading a single-wavelength file.
Regardless of how you stop the run, the detector returns to
READY.
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Changing Run Parameters
There are two ways to change the detector run parameters:
1. You can use the Files Menu and follow the procedures
Status Menu
outlined under
Setting Parameters
2. You can use the Status Menu, which is the programming
area below the Status Screen.
Each has a distinct advantage. Programming in the Status Menu
allows you to change the detector current operating parameters,
even while the detector is running. Programming in the Files
Menu allows you to prepare a file containing the changes without
altering the current detector settings. The file may then be
loaded at a later time.
on page 23.
ASIC OPERATION
From the Status Screen, move the cursor down to the Status
Menu. The Status Menu contains the loaded file identification (its
number and name), Wavelength Program, Rise Time, Autozero
Time, and Ranges.
File 1:
-----------------------------------------
Time λ1 λ2
0.00 250 280
Rise Time 1.0
Autozero Time 0.00
Range 1 1.0
Range 2 1.0
The detector parameters are set following the same instructions
previously given under
Options
identification or wavelength mode while in the Status Menu.
ProStar 345 UV-Vis Detector
Wavelength Program
on page 28 and
on page 29. However, you cannot modify the file
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NOTE: When you modify file parameters from the Status Menu, you do not
change the contents of the same file number stored in the detector
memory. Only the copy of the active file is modified.
Saving the File
When you change settings form the Status Menu, each change
is effective as soon as you leave the field. You will also see that
the File identification on the first line of the Status Menu now
reads “File N:xxxx changed” (where N:xxxx is the file number
and name) and that the words “Save File” now appear below
Range 2.
To save the changed file, press [ENTER]. The confirmation
message below will appear briefly.
** File Saved **
If you wish to keep the original file without saving the changes,
do not press the ENTER key. Instead, reload the unaltered file
by using the Files Menu as follows:
1. Press [MENU].
2. Select /FILES/.
3. Select /Load/.
4. The words “Load File N: (filename)” will appear on the
screen. Enter the desired file number and press [ENTER].
The confirmation message will appear for one second. You are
then returned to the Status Screen, where all settings will contain
their original values.
More About Files
How to edit and load files from the Files Menu was described
earlier. The Files Menu also allows you to copy and delete files
in a few easy steps as shown in the following section. The
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section also describes how to protect files from being edited,
copied to, or deleted.
Copying Files
To copy a file:
1. Press [MENU].
2. Select /FILES/ to display the Files Menu.
Edit Load
Copy Delete
3. Select /Copy/. The Copy Menu will appear on the screen.
Copy File 1: (filename 1)
To File 2: (filename 2)
4. Enter the identification number for the file you wish to copy
in the Copy File field.
ASIC OPERATION
5. Enter the number of the file to which you wish to copy to in
6. Press [ENTER]. The message shown below appears briefly,
** File Copied **
If you attempt to copy to a protected file (see the section below,
titled
a file isn’t protected, make sure it is empty or unwanted before
you copy to it, as it will be overwritten.
** Protected File **
Cannot Be Copied To
Deleting Files
1. Press [MENU].
2. Select /FILES/ to display the Files Menu .
ProStar 345 UV-Vis Detector
the To File field.
and you’re returned to the Files Menu.
Protecting Files
), you will see the message shown below. If
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3. Select /Delete/. The words “Delete File N:(filename)” will
appear on the screen.
4. Enter the identification number of the file you wish to delete.
When you press [ENTER], the message shown below
appears briefly, and the display returns to the Files Menu.
(The parameters in the file you’ve just deleted return to their
default values.)
** File Deleted **
If you attempt to delete a protected file (see the next section,
Protecting Files
** Protected File **
Cannot Be Deleted
), the message below will be displayed.
The ProStar 345 allows you to protect files from being edited,
copied to, or deleted. To access the file protection operation,
follow these steps:
1. Press [MENU].
2. Select /OPTIONS/. The Options Menu appears.
Lamps
Analog Outputs
More
3. Select /More/ to display the More Menu.
Zero on λ change Yes
Cursor Speed Medium
---------------------------------------
Status Lock Off
READY Output Active Hi
File Name Protect
1: Off
2: Off
3: Off
4: Off
4. Scroll down to the table containing the fields /File Name/
and /Protect/. To protect a file from being edited, copied to,
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B
or deleted, select On in the Protect field that corresponds to
the appropriate file number. To remove the file protection,
select Off.
Analog Output Operations
The ProStar 345 has two outputs, Analog Output 1 and Analog
Output 2. Labeled CH1 and CH2 on the rear panel, these
outputs are useful for monitoring analyses at two different
sensitivity settings simultaneously. For example, analog outputs
allow you optimally to detect very small peaks and very large
peaks in the same sample run.
Analog Outputs
ANALOG OUTPUT 1 By default, Analog Output 1 is either the
absorbance reading for single-wavelength
operation, or the absorbance reading of
wavelength one (λ1) for dual-wavelength
operation.
ASIC OPERATION
ANALOG OUTPUT 2 Analog Output 2 is selectable (AU, AU1-
1. Press [MENU].
2. Select /OPTIONS/.
3. Select /Analog Outputs/. The menu shown appears:
Analog 1 Offset % 0
Analog 2 Offset % 0
----------------------------------------
Analog 2 AU
K Factor 1.000
4. Scroll down to Analog 2. The selections are:
ProStar 345 UV-Vis Detector
K*AU2, and AU1/AU2), and so can be used to
monitor several different outputs. To access
these options:
which is either the same absorbance reading you got
AU:
from Analog Output 1 in single-wavelength operation, or the
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absorbance reading of Wavelength Two (λ2) for dualwavelength operation.
Analog Offsets
AU1-K*AU2:
using the K-Factor technique. See page 63 for further
details.
AU1/AU2:
wavelength. This ratio is sometimes used to check peak
purity. See Absorbance Ratios on page 68 for more details.
Both analog outputs 1 and 2 can be offset. Analog offsets may
be used in cases where there is a high background absorbance
reading, or when there is considerable baseline drift from your
chromatographic system and you’re unable to keep your
integrator (recorder) signal on-scale.
Because integrators have very limited capacity for handling
negative signals, you may wish to set a small positive offset (1%)
when using an integrator.
Negative offsets are available for use with recorders, where you
may wish to set the pen at either side of the strip-chart.
The offset options are selectable from the Analog Outputs Menu.
which is the readout of the suppressed signal
which is the ratio of absorbances for dual-
NOTE: We recommend a 1% offset setting for use with your data system or
integrator.
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Advanced Operation
This section describes using the ProStar 345 more advanced
capabilities, such as wavelength programming, automatic
zeroing, scanning, and queues. You should be familiar with
Basic Operation
Wavelength Programming
Your detector can change wavelength as a function of time:
Wavelength Programming. This feature gives you maximum
detection sensitivity for each component in a mixture without
making multiple injections of the sample.
, before you begin.
Building the Program
In wavelength programming, time lines are entered into a
“Wavelength Program.” Each time line specifies the time at
which you want a wavelength change to occur.
You can build a wavelength program in either the Status Menu
or the Files Menu using the procedure outlined in this section.
The following instructions are for single-wavelength operation,
but you can build a dual-wavelength program in the same way.
Display the Wavelength Program in either the Status Menu or
the Files Menu.
Time Wavelength
0.00 254
The initial time entry is 0.00. Move the cursor to the wavelength
field(s), and enter the initial wavelength(s) for your analysis.
ProStar 345 UV-Vis Detector 39
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Entering Subsequent Time Lines
To add a second time line, scroll down to the first blank line and
press [+]. The second line automatically will have a time setting
of 1.00 and the same wavelength settings as the first. Change
the Time and corresponding wavelength field(s) to the desired
values.
A wavelength program may contain as many as ten lines for a
single run. You can cross between the UV and visible ranges (in
single-wavelength mode only).
If you enter time lines out of sequence, the detector will
automatically sort the lines and place them in chronological
order.
Stop Line
The last line of the program (the stop-line) lists the time at which
the detector automatically will end the run and return to initial
conditions. Since wavelengths are not important in the stop-line,
they can be set to any value(s).
NOTE: Remember, the last line of the program is always the detector signal to
end a run; it is not a programmed wavelength change.
Deleting a Line
To delete an entire time line, place the cursor in the Time field
and press [-] repeatedly until the value goes blank. When you
leave the line, it will be deleted. The display below shows a
completed wavelength program.
Time Wavelength
0.00 254
----------------------------------------
5.00 280
7.00 265
10.00 265
In our example, the initial detection wavelength is 254 nm. At
5.00 minutes into the run, the wavelength changes to 280 nm. At
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7.00 minutes, it changes to 265 nm. The run ends at 10.00
minutes, and the detector returns to its initial wavelength of 254
nm and to its READY state.
Running a Program
After you set the rest of your parameters, the detector is ready to
run. It is good practice to zero the detector at the beginning of
every run and at each wavelength change. See the next section,
titled
Programmed Autozero
Once you start the run, you may edit any timed event
(wavelength change, autozero, or stop-time) that has not yet
taken place. These changes can be made only from the Status
Menu. Each edit is entered immediately into the detector
operating wavelength program.
, for details.
For example, for the program displayed as in
stop time is 10.0 minutes. If, at 7.00 minutes into the run, you
determine that the run should be 9.00 minutes long, you can edit
the last line of the program and the current run will stop at 9.00
minutes.
Programmed Autozero
The ProStar 345 can be programmed to perform an automatic
zero with each wavelength change during a run using the Zero
on λ Change field. To access this feature:
1. Press [MENU] and select /OPTIONS/ to access the Options
Menu.
Lamps
Analog Outputs
-------------------------------------
More
3. Select /More/ to display the More Menu.
4. Place the cursor on the Zero on λ Change field. This field
appears on the first line of the More Menu.
Deleting a Line
the
ProStar 345 UV-Vis Detector
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5. Select Yes, to zero the detector response automatically with
each wavelength change during a run, or No, to turn this
feature off.
You can also use this automatic zero feature to add autozeros
into your wavelength program without changing the detector
wavelength settings. To do this, simply add additional time lines.
Adding autozeros in this way is convenient in cases such as
solvent programming, where the detector baseline may drift due
to changes in solvent background.
Time Wavelength
0.00 254
----------------------------------------
2.00 254
5.00 280
7.00 280
10.00 280
With the Zero on λ Change field set to Yes, the detector will
autozero at 2.00, 5.00 and 7.00 minutes into the run. The
wavelength will only change once (at 2.00 minutes into the run).
Automatic Lamp Operations
The Lamps Menu allows you to select lamps, track lamp life, and
turn the lamps on and off automatically. It contains the fields
described below.
Lamps Menu
To access the Lamps Menu:
1. Press [MENU] and select /OPTIONS/.
2. Select /Lamps/.
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Lamp D2 (190-365)
D2 Lamp Hours 0
----------------------------------------
W Lamp Hours 0
Current Time 0:00
Startup Manual
Startup Time 0:00
Shutdown Manual
Shutdown Time 0:00
Time from READY 1:00
DVANCED OPERATION
Lamp
The Lamp field allows you to select from the following:
• D2 (190-365), for deuterium
• W (366-800), for tungsten
• D2 + W (190-800), for dual-lamp operation
• or OFF, to shut the lamp(s) off.
In actuality, the wavelength setting in the loaded file selects the
appropriate lamp for you automatically. In fact, the wavelength
setting you choose in your file has priority over any selection you
make here in the Lamp field.
For example, if the loaded file designates a wavelength in the
UV range, but you selected W (366-800) in the Lamp field
manually, the detector display will read NRDY (not ready) for the
deuterium lamp.
Lamp Hours (W and D2 fields)
These fields track automatically the number of hours each lamp
has been in operation. For the value to be accurate, you have to
set the appropriate Lamp Hours field to zero each time you
install a new lamp.
ProStar 345 UV-Vis Detector
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NOTE: If you change lamps before they are burned out (with the intention of
using them again at a later date), keep a record of how many hours they
have been in operation and remember to recalibrate the detector
immediately following each lamp change.
Startup and Shutdown
When you set the Startup and Shutdown fields to “Manual”, the
lamp designated in the Lamp field turns on and off when the
detector power is switched on and off.
Startup and Shutdown Times
When you set the Startup and Shutdown fields to “Time” (see
above), the designated lamp will turn on and off automatically at
the local time set in the Startup Time and Shutdown Time fields,
respectively.
NOTE: For the detector to perform automatic lamp startup and shutdown
correctly, the detector 24-hour clock must be set to your local time. Set
the clock in the Current Time field.
Time from READY
If you prefer, you can use the Time from READY feature to
program the detector to shut the lamp off after a series of
automated runs. Time from READY is a preset time interval that
begins automatically each time the detector returns to its READY
state. If the Time from READY interval elapses without a run
signal being received from either the keypad or the detector Run
(Input) terminal, the detector lamp turns itself off. To use the
Time from READY feature:
1. Select Time from READY in the Shutdown field.
2. In the Time from READY field, enter the length of time
during which a run signal must be received by the detector
before the lamp turns off.
For example, the chromatographic system is set up for an
automated run and the autosampler signals the detector to run
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after each injection. With the detector settings shown in the
display below the lamp will turn off 10 hours after the last run is
completed.
Shutdown Time from READY
Shutdown time 00:00
---------------------------------------
Time from READY 10:00
You can also program the lamps to turn off at the end of a queue
by selecting End of Queue in the Shutdown field. For more
information on the Queue feature, see page 59
Other Features
Additional features include the abilities to lock the Status Screen,
to short the detector outputs, to place an event mark on the
chromatogram, and to send a ready signal to external devices.
You can also control the display contrast and cursor speed, and
make a quick shutdown of the detector lamps and motors.
Status Lock
You can lock the detector display using the Status Lock field.
This feature lets you prevent accidental changes to a file
currently being run. You can move the cursor down from the
Status Screen as far as the Status Menu File Name field.
However, you’ll still be able to access the Main Menu and the
rest of the menu structure using [MENU} .
To access Status Lock:
1. Press [MENU].
2. Select /OPTIONS/.
3. Select /More/.
4. Scroll down to /Status Lock/. Select On or Off to turn the
5. Press [STATUS].
ProStar 345 UV-Vis Detector
lock on or off, respectively.
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Short Outputs
When zeroing a readout device such as an integrator or
recorder, it is convenient to be able to short the detector outputs.
You can do this using the Short Outputs feature as follows:
To access Short Outputs:
1. Press [MENU].
2. Select /COMMANDS/. The Commands Menu appears.
Event Mark
Short Outputs
----------------------------------------
Shutdown Detector
When you select Short Outputs, the detector analog outputs are
shorted together (zero volts) and the field name changes to
“Unshort Outputs.” To return the outputs to their normal
(unshorted) operating state, select Unshort Outputs, and the field
changes back, now reading “Short Outputs.” (When you leave
this screen, the field returns to Short Outputs automatically.)
Event Mark
Using the event mark feature, you can place an event mark on
your chromatogram to note various occurrences, such as the
turning of a sampling valve. The event mark is a spike (15% of
full-scale for one second) in both detector output signals.
To access Event Mark:
1. Press [MENU].
2. Select / COMMANDS/. The Commands Menu appears.
3. Place the cursor on Event Mark. Press [ENTER] each time
you wish to place an event mark on your chromatogram.
NOTE: You may not want to use event marks if your data will be analyzed by an
integrator. Integrators can misinterpret event marks as peaks.
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Ready Output
Using the NOT READY terminal on the detector back panel, the
detector can send a signal to other devices each time it goes to
its READY state. This feature is used frequently with
autosamplers to signal that the detector is ready for the next
injection.
To access the READY Output field:
1. Press [MENU]
2. Select /OPTIONS/.
3. Select/More/.
4. Scroll down to the READY Output field. Select Active Hi or
Active Lo, depending on which signal you wish to send.
NOTE: Refer to the appropriate reference manual for the instrument being
connected.
For details on interfacing the detector NOT READY terminal with
other devices.
Display Contrast
You can vary the display contrast to make it easier to read. To
change the display contrast, first press [STATUS] to access the
Status Screen. Then press the [] key and the [+] key
simultaneously to increase the contrast, or the [] key and the [-]
key to reduce the contrast.
Cursor Speed
You can control the display cursor speed to make it easier to
use. To access Cursor Speed:
1. Press [MENU].
2. Select /OPTIONS/.
ProStar 345 UV-Vis Detector
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Shutdown Detector
3. Select /More/.
4. Scroll down to Cursor Speed and select Fast, Medium, or
Slow.
This feature offers a quick shutdown, and subsequent startup, of
the detector lamps and motors. The electronics stay on to
maintain the detector memory. To shut down the detector:
1. Press [MENU]
2. Select /COMMANDS/.
3. Scroll down to the Shutdown Detector field.
4. Press [ENTER]. The confirmation message appears on the
display.
** Detector Shutdown **
To restart the detector, press any key on the keypad. The
detector will restart under the same conditions present when the
Shutdown Detector command was activated.
Scanning
The detector can perform a spectral scan on eluting peaks
without stopping the eluant flow. This unique feature simplifies
greatly the determination of wavelength maxima for individual
compounds in your sample during method development work.
How it Works
When a scan in initiated, the monochromator moves from the
run-wavelength to the scan start-wavelength. The detector scans
by stepping through a defined spectral range at specified
wavelength increments. Individual absorbances are read at each
increment until the monochromator has reached the last
wavelength.
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The detector can collect and store in its memory as many as ten
spectra from a single chromatographic run. The actual number
of spectra is determined by the number of data points in each
scan. Since the number of data points varies with the
wavelength interval and the scanning range, first calculate the
number of data points using Equation 1, then use either
Equation 2 or Equation 3 to determine the number of spectra
you’ll be able to collect.
Equation 1. Use this equation to calculate the number of data
points for any scan between 1 (the lower wavelength), and 2
(the higher wavelength):
# of data points
=
λ
interval
λλ
1
+=
−
12
Equation 2. Use this equation to calculate the number of spectra
you can collect when using wavelength intervals of 2 nm or
greater. Round the resulting number down to the nearest
integer.
# of spectra
=
−
)*pointsdataof(#,
120005
14 4)* points data of(#
+
Equation 3. Use this equation to calculate the number of spectra
you can collect when using wavelength intervals of 1 nm. Round
the resulting number down to the nearest integer.
# of spectra
=
−
* points data of(#
40005
)*pointsdataof(#,
+
144
)
NOTE: To approximate the scan time (in seconds) for a given run, divide the
number of data points by twenty.
For example, if you want to scan from 190 to 564 nm in 2-nm
steps, there would be 188 data points and the ProStar 345 would
be able to store up to 3 spectra.
# of spectra
ProStar 345 UV-Vis Detector
=
−
121880005
) *(,
2744
766
144188
++
) *(
3583
.
===
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Each scan is corrected for baseline absorbance before being played
back either as individual data points, or a smoothed, continuous
spectrum.
Selecting the Scan File
To select spectral scanning, follow these step-by-step
instructions.
1. Press [MENU]. Select /FILES/.
2. Select /Edit/.
3. Use the [+] key to increment the Edit File field until an “S” is
displayed. The File Name field is named SCAN
automatically. (You cannot edit the Scan File name.)
Edit File 5
File Name SCAN
---------------------------------------
Scan
Replay
6. Select/Setup/ to set up your spectral scanning parameters.
The Scan File Setup Menu is shown in the display below.
Start λ 220
End λ 365
------------------------------------
λ Interval 5
Run λ 250
Rise Time 1.0
Scan Zero Time 0.00
Range 1 1.0
Range 2 1.0
1. In the Start λ field, enter the wavelength at which each scan
should start.
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2. In the End λ field, enter the wavelength at which each scan
should end.
3. In /λ Interval/, enter the wavelength interval to be used. To
perform a scan, the ProStar 345 takes individual
absorbance readings at wavelengths incremented by this
interval.
NOTE: Five nanometers is an excellent wavelength interval for most
applications. At this interval you get very rapid scans and you can still
display the Max to 1 nm accuracy.
4. In /Run /, enter the wavelength at which the
chromatographic run will be monitored.
5. In /Scan Zero Time/, enter the runtime at which you wish the
detector to perform an automatic baseline scan. If you use
an automatic baseline scan, make sure no peaks are eluting
during the designated scan time.
6. Fill in entries for Rise Time, Range 1, and Range 2 as for
When you’re finished setting up the Scan File, you’re ready to
load it and run. When the Scan File is loaded, you’ll notice the
fields /Zero/ and /Scan/ in the Status Screen.
Status λ AU Scan
READY 250 0.0001 Zero
Zero
/Zero/ is used to perform baseline scans of the solvent
background absorbance. With the detector baseline stabilized
and the cursor on the Zero field, press [ENTER]. The ProStar
345 performs and stores a baseline scan using the parameters
you set in the Scan File. While the detector is performing a
baseline scan, the Status field displays SCAN 0.
Baseline scans may be taken at any time during the run, as long
as no peak is eluting at that time. Subsequent sample scans are
corrected using the last baseline scan taken. This is especially
ProStar 345 UV-Vis Detector
any chromatographic run.
51
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advantageous for gradient elution, where the background
absorbance of the eluant may be changing constantly.
For example, let us say you perform a baseline scan before you
initiate a run, and then again at 5.00 minutes into the run. You
also perform sample scans of you eluting peaks at 2.4 minutes
will be corrected using the baseline scan taken before the run
began. The sample scan taken at 5.6 minutes will be corrected
using the baseline scan taken at 5.0 minutes.
Scan
Once you begin the run, the cursor will move from /Zero/ to
/Scan/ in the Status Screen. Each time you wish to perform a
sample scan, press [ENTER].
NOTE: There is a one-second delay from the time the detector takes its
absorbance readings to the time you see the same reading on the
analog readout. Keep this in mind when choosing you scan times.
Each time you perform a sample scan, the detector
monochromator moves from the run wavelength to the start
wavelength. The detector performs each scan (from the start
wavelength to the end wavelength) by taking individual
absorbance readings at wavelengths incremented by the interval
you set in the Scan File. When the scan is finished, the
monochromator returns to the run wavelength.
For example, using the default Scan File Setup Menu the
detector would monitor the run at 250 nm. Each scan would
include absorbance readings for wavelength settings of 220,
225, 230, 235, and so on, up to 350 nm.
NOTE: If you chose starting and ending wavelengths that weren’t an exact
multiple of your wavelength interval, the ending spike (event mark) on
your chromatogram would be placed at the last multiple of the
wavelength interval that falls within the scanning range. For example,
with a starting wavelength of 200 nm, an ending wavelength of 365 nm,
and a wavelength interval of ten, the end spike on your chromatogram
would be at 360 nm, the last full wavelength multiple within the range.
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While the detector is scanning, the Status field displays SCAN.
CAUTION
During scanning, the output signal will hold at the last absorbance value taken before
the scan was initiated until the scan is finished. For this reason, quantitative analysis
should never be performed when scanning.
Scan Summary Data Screen
When the Scan File is loaded, the normal Status Menu no longer
appears below the Status Screen. Instead, several new lines that
we call the “Scan Summary Data Screen” appear. The Scan
Summary Data Screen is useful in setting up the parameters to
replay your stored spectra.
An example of the Scan Summary Data screen as it appears
after two sample scans.
File S: SCAN
---------------------------------------
Time λMax λMaxAU λMin
10.50 280 1.6668 230
11.66 255 0.7768 220
The Scan Summary Data Screen has four fields:
1. /Time/, which is the run time at which the scan was initiated
2. /λ Max/, which is the scan wavelength where the maximum
3. /λ Max AU/, which is the maximum absorbance
4. / λ Min/, which is the scan wavelength where the minimum
If no maximum was found, the λMax and λMaxAU fields show
zero. The summary information is updated as each sample scan
is completed.
ProStar 345 UV-Vis Detector
absorbance occurred
absorbance occurred
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NOTE: The ProStar 345 uses a second derivative to find the “local” Max.
In our example above scans were taken at 10.50 and 11.66
minutes into the run. The scan taken at 10.50 minutes has a
maximum absorbance of 1.6668 AU at 280 nm. The minimum
absorbance occurred at 230 nm. To replay your 10.50-minute
scan, you would use a range of 2.0 AUFS to keep the
absorbance values on-scale.
Stopping the Scan File
There is no programmed stop in the Scan mode. The run will
continue until it reaches 99.99 minutes, or until you press
[STOP].
Replaying Your Spectra
When you’ve completed your run, you can retrieve your stored
sample spectra using the Replay Menu.
To access the Replay Menu:
1. Press [MENU]. Select /FILES/.
2. Select /Edit/ to display the Scan File Edit Menu.
Select /Replay/.
Range 1 1.0
Range 2 1.0
---------------------------------------
Replay Rate (nm/sec) 5
Spectra Time 10.50
Replay Spectra
Display AU, λ
Setting Replay Parameters
To set the parameters for replay:
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1. Set /Range 1/ and /Range 2/ for Analog Output 1 and
Analog Output 2. If you’re using only one output, disregard
the appropriate range.
2. Enter the Replay Rate (nm/sec). This is the rate at which the
detector will read out the spectral data to your chart. You’ll
use this value and an appropriate chart speed to calculate
wavelength increments on your printed sample spectrum.
For example, if your sample scan were taken between 190
and 340 nm (a span of 150 nm), a replay rate of 5 nm/sec
would print the spectrum in 30 seconds. A chart speed of 30
cm/min would give you a scan of 15 centimeters in
increments of 10 nm/cm.
3. Select the spectrum you want to replay by selecting its start
time in the Spectra Time field. Each spectrum taken during
the run is identified individually by the run time at which it
was initiated.
When you finish setting your replay parameters, you’re ready to
send the spectral data to your chart using the Replay Spectra
command.
Running Replay
To initiate the Replay Spectra command in the Replay Menu,
press [ENTER]. While the replay is occurring, the screen shown
below appears on the display.
Replay λ AU
10.50 220 0.00001
The screen Replay field displays the start time of the spectrum
being replayed. The λ and AU fields display the individual data
points being plotted.
The ProStar 345 uses advanced curve-fitting algorithms to
present a smooth, continuous plotted spectrum. The spectrum is
replayed in 1-nm steps regardless of the wavelength interval
selected. To change the appearance of replayed spectra from 1nm stepped curves to smooth curves (or vice versa), vary the
recording device replay rate and response time.
ProStar 345 UV-Vis Detector
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If no spectra are stored in memory when you activate the Replay
Spectra command, the message shown below will appear on the
display. when the replay in finished, the display returns to the
Replay Menu.
** No Scans Stored **
You may stop a replay at any time by pressing [STOP].
Spectral Data Storage
Spectral data are stored in the ProStar 345 memory until a new
file or queue is loaded or the detector is turned off.
Viewing Data
You can display the individual data points of your stored spectra
by selecting the Display AU, λ field in the Replay Menu. A
screen similar to that shown will appear on the display.
Display λ AU
10.50 220 0.00001
NOTE: Only actual data points (separated by the proper wavelength interval)
can be displayed.
The Display AU, λ screen shows the time at which the scan was
initiated, along with each wavelength and absorbance reading
collected. You can move the cursor through the data using [+]
and [-]. To return to the Replay Menu, press .
Develop File
The Develop File is unique to the ProStar 345. It allows you to
perform sequential sample injections at different wavelengths
automatically. This automation makes method development
much easier because you can use an automated run to
determine the optimum detection wavelength for each
component in your sample. You can also use the Develop File to
troubleshoot chromatographic problems, or to confirm method
transfer from laboratory to laboratory.
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Selecting the Develop File
1. Press [MENU]. Select /FILES/.
2. Press [+] to increment the Edit File field until a “D” is
displayed. The File Name field will read DEVELOP. (You
cannot edit the Develop File name.)
Editing the Develop File
1. Once you’ve selected the Develop File as described above,
press either [ ENTER] or [] to access the Develop File Edit
Menu.
Edit File D
File Name DEVELOP
----------------------------------------
Start λ 220
End λ 350
λ Interval 5
Run Time 10.00
Runs per λ 2
Rise Time 1.0
Autozero Time 0.00
Range 1 1.0
Range 2 1.0
2. In /Start λ/, enter the wavelength at which the 1st
3. In /End λ/, enter the wavelength at which the last
4. In /λ Interval/, enter the wavelength increment that the
5. In /Run Time/, enter the length of each run.
6. In/Runs per λ/, enter the number of injections to be made at
ProStar 345 UV-Vis Detector
chromatogram is to be monitored.
chromatogram is to be monitored.
detector monochromator should use for each wavelength
change.
each wavelength setting.
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7. Enter Rise Time, Autozero Time, Range 1, and Range 2 as
you would for a typical run. Range 1 and Range 2 are the
corresponding ranges for Analog Outputs 1 and 2.
As an example, the Develop File shown above is used. The
ProStar 345 would make its first two ten-minute runs at 220 nm.
The monochromator would then change to 225 nm, and the
detector would make two runs at this wavelength. This pattern
would continue in five-nanometer increments until the detector
has made two runs at the last wavelength, 350 nm.
After setting up your Develop File, you’re ready to load it and
run.
Running the Develop File
When the Develop File is loaded, you’ll notice an additional field
in the Status Screen, /#Runs/.
Status λ AU #Runs
READY 220 +0.0001 1/3
#Runs
The #Runs field in the Status Screen shows the current run
number, followed by a forward slash and the total number of
injections for the wavelength specified in the l field. The field is
updated with each injection. For example, if the file is set up to
make three injections per wavelength, and the detector is in the
second run for the 250-nm setting, the # Runs field would appear
as 2/3.
The Status Menu looks the same for a Develop File as it does for
a typical chromatographic file.
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File D DEVELOP
----------------------------------------
Time Wavelength
0.00 250
10.00 250
Rise Time 1.0
Autozero Time 0.00
Range 1 1.0
Range 2 1.0
DVANCED OPERATION
NOTE: You can change any of the parameters in the Status Menu while the
detector is running, but the changes will be effective only until the next
wavelength is loaded.
Repeating the Develop File
After the last wavelength is run, the detector is reset
automatically to the starting wavelength in the Develop File. The
file can be run as many additional times as you wish, as long as
the detector continues to receive run signals.
Sample Queue
Sometimes it is convenient to group samples together under
different detector conditions in an automated run. For these
occasions, the Model 205 offers a queuing feature. Using a
queue, you can program the detector to load and run a specified
file automatically for your first group of samples, then load a
second file to run your next group of samples. The queue feature
allows you to run as many as ten groups in a singe queue.
Queue Menu
1. Press [MENU].
2. Select /QUEUE/.
When no queue is loaded, the Queue Menu appears as shown
below.
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Edit Load
Delete
Setting Up a Queue
To setup a queue, select /Edit/ from the Queue Menu. For an
empty queue, the display appears as shown below.
Order File:Name #Runs
1
Entering a Line
A “1” is placed automatically in the Order field of the first file to
be run. You can’t change that, so the cursor appears under the
first editable field, /File:Name/. Scroll through the available files
and press [ENTER] when your choice appears.
NOTE: You may only select numbered files. The Scan and Develop files aren’t
available in the Queue mode.
Enter the number of injections to be made in the # RUNS field
and press [ENTER]. You can have as many as 999 injections
per file.
Adding More Lines
After completing the first line, a second line appears
automatically. The Order field reads 2, and the rest of the line is
blank. Select the proper file and the number of injections to be
made for that file. You can have as many as ten groups in the
queue.
Deleting a Line
To delete a line, press [-] while in the File:Name field until the
field is blank. When you leave the line, it is deleted and the
queue is resorted automatically.
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A
Order File:Name #Runs
1 2:THEOPHYL 5
2 3:ABCD 25
3 1:BABITUR 10
DVANCED OPERATION
In our example, we have programmed the detector to run File 2
off the first five injections, File 3 for the next 25 injections, and
File 1 for the last 10 injections.
Loading a Queue
To load a queue, select/Load/ in the Queue Menu. When the
words “Load Queue” appear, press [ENTER]. The confirmation
message in the display below appears for one second.
** Queue Loaded **
When a queue is loaded, the letter “Q” appears at the extreme
left of the Status Screen shown below.
Status λ AU
Q READY 250 +0.0001
If you attempt to load a queue when no queue exists, the
message shown below appears on the display.
** No Queue Available **
Running a Queue
When the detector receives its first start signal, it loads and runs
the file designated in Order 1. It will continue to run this file each
time it receives a start signal until the file has run the number of
times specified in the #Runs field. The detector will then load
and run the file designated in Order 2 and run it the number of
times specified in that line, and so on, until the entire queue has
run.
Viewing the Progress of a Queue
1. Press [MENU].
2. Select /QUEUE/. Note that when a queue is loaded, the
Queue Menu looks different. The Load field has been
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Loading Other Files
replaced by “Pause.” See below for more information on the
Pause selection.
Edit Pause
Delete
3. Select /Edit/to display the queue.
While the queue is running, the # Runs field decreases by one
automatically with each injection. When a last injection of a
particular file is made, the queue is resorted automatically. In
other words, the information for Order 2 is now moved up to
Order 1, the information for Order 3 is moved up to Order 2, and
so forth. This process continues until the queue becomes empty,
is paused, or is deleted.
When a queue is loaded or running, you may not load any other
file from the Files Menu without first pausing or deleting the
queue. If you forget to pause or delete the queue and attempt to
load a different file, you’ll get the message shown below. You
are then returned to the Files Menu.
** Queue Loaded **
Can’t Load File
Editing a Queue
To edit an existing queue, follow the procedures outlined in
Setting Up a Queue
Queue while it is running, but if you want to edit anything in
Order 1, you’ll have to pause the queue first.
on page 60. You’re allowed to edit the
Pausing a Queue
1. Select /Pause/ from the Queue Menu.
2. When the words “Pause Queue” appear, press [ENTER]. If
a file is running, the run continues until it is completed, at
which point the detector returns to its READY state. The
letter Q will then no longer appear in the Status Menu.
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DVANCED OPERATION
When you wish to continue, you must reload the queue. When
the detector receives a start signal, the queue will resume
operation at the point where it left off.
Deleting/Stopping a Queue
1. Display the Queue Menu.
2. Select/Delete/.
3. When the words “Delete Queue” appear, press [ENTER]. If
a file is running, the run continues until it is completed. A
confirmation message appears for one second and you’re
returned to the Queue Menu.
You may delete or stop a queue at any time, but remember that
the queue will be erased from memory. It is good practice to
delete an existing queue prior to creating a new one.
K-Factor
The K-factor calculates a factored response that can be used to
eliminate, add, or subtract absorbance. This technique is useful
for suppressing peaks when there are two coeluting, or poorly
resolved, peaks in your chromatogram. It is also useful in
applications where you want to add or subtract absorbances at
two different wavelengths in real-time.
For example, if you want to quantitate a peak without
interference from another peak, you would use the K-factor to
calculate a response of zero.
More specifically, let us say you want to analyze for Compound
A in the presence of Compound B. If both absorb at the
monitoring wavelength, λ1, but only Compound B absorbs at a
second wavelength, λ2, you can calculate a K-factor for
Compound B using its absorbances at λ1 and λ2. You can then
use the K-factor to calculate the absorbance due to only
Compound A at the monitoring wavelength (λ1), by subtracting
the Compound B contribution from the total absorbance. The
ProStar 345 uses the algorithm:
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Absorbance due to A at λ1 = TAbs(λ1) - K x TAbs(λ2)
where TAbs(λ1) is the sum of the absorbances of A and B at the
monitoring wavelength, K is the K-factor, and TAbs(λ2) is the
total absorbance obtained at λ2.
Figure 9 shows a chromatogram of a mixture of toluene and
butyl paraben where the two compound peaks overlap. Toluene
(Peak A) is the compound of interest. Butyl paraben (Peak B) is
the peak we want to suppress.
We will use this example throughout the following steps for
determining and using the K-factor.
Figure 9 A Chromatogram of Two Unresolved Peaks: toluene (A) and butyl paraben (B)
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DVANCED OPERATION
Choosing a Pair of Wavelengths
The first step in determining the K-factor is to choose a pair of
wavelengths for your analysis.
1. Take an absorbance spectrum of each compound. You can
do this by injecting samples of compound A and compound
B alone, separately, under the same chromatographic
conditions as your analysis, and using the ProStar 345
scanning feature. (See
Scanning
on page 48).
Figure 10 Spectra of Individual Compounds
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2. Label the wavelength maximum for your peak of interest as
λ1.
3. From the spectra, pick a wavelength for which compound B
absorbs and compound A doesn’t. This wavelength is
labeled λ2. For our example, we have chosen 254 nm as λ1
and 280 nm as λ2.
Calculating the K-Factor
Use the ProStar 345 Display AU, λ screen to obtain the
individual absorbance value data from your scan of compound B.
Calculate the K-factor using the following equation:
K = AU1/AU2
where AU1 and AU2 are the absorbance values for compound B
at λ1 and λ2, respectively.
For our example, the absorbance values are 0.0144 and 0.0032
(for 254 and 280 nm respectively), so our K-factor is 4.5
calculated as follows:
K= 0.0144/0.0032 = 4.5
Using the K-Factor
To use the K-factor, set the parameters in the Analog Outputs
Menu, inject your sample, and monitor the results as follows:
1. The menu below will appear. Press [MENU]
2. Select /OPTIONS/.
3. Select /Analog Outputs/.
Analog 1 Offset (%) 0
Analog 2 Offset (%) 0
----------------------------------------
Analog 2 AU
K Factor 1.000
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DVANCED OPERATION
4. Scroll down to Analog 2 and select AU1-K*AU2.
5. Scroll down to K-factor and enter your calculated value (4.5,
for our example).
6. Inject your sample.
NOTE: Make sure your file was set to dual-wavelength mode as described in
Basic Operations
. Also remember that in this example, AU1 (λ1) is 254
nm and AU2 (λ2) is 280 nm.
7. Use Analog Output 2 (CH 2 on the detector rear panel) to
monitor the chromatograms for your peak of interest.
Figure 11 Chromatogram of Toluene with Butyl Paraben Suppressed
Our example chromatogram would now appear, as shown in the
figure above, with a slightly lowered response for toluene and no
absorbance contribution from butyl paraben. Using the K-factor
in this way, we can quantitate toluene in the presence of butyl
paraben without altering the chromatography.
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Absorbance Ratios
Ratioing the detector outputs from two different wavelengths can
be a useful way of confirming peak purity. When a peak is pure,
the ratio of the absorbances should remain constant. Thus the
ratio for a pure compound produces a relatively square wave,
while the ratio for an impure compound produces a distorted
wave (see the plots at 1.57 and 0.97 minutes, respectively, in the
figure below).
Figure 12 Using Absorbance Ratios to Determine the Purity of Two
Peaks in a chromatogram
To use absorbance ratioing, you need to select AU1/AU2 for the
Analog 2 Output field in the Analog Outputs Menu. You also
need to select the two wavelengths you want to ratio.
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DVANCED OPERATION
To select the most appropriate wavelengths, use the ProStar
345 Scan File to collect a spectrum across a range of
wavelengths. Then select/Display AU, λ/from the Replay Menu
and examine the collected data.
Display λ AU
1.50 250 0.00001
-----------------------------------------
1.50 250 1.66681
1.50 280 0.28831
Ratioing only occurs when the absorbance value for each
wavelength exceeds 12.5% of the corresponding range value.
So, in our example, if Ranges 1 and 2 were set to 1.0 in the
/FILES/, /Edit/, Options Menu, the 250 and 280 nm wavelengths
could be rationed. Twelve-and-a-half percent of 1.0 (the range)
is 0.125. Absorbance values less than 0.125 are too low for
ratioing. No ratio output is produced when the absorbance
values fall below 7.5% of the range values.
Generally, good wavelengths to choose are:
• the lambda max of the main peak (AU1)
• a wavelength with an absorbance value less than the
lambda max but greater than 12.5% of the corresponding
range (AU2)
NOTE: A good rule of thumb is to select a second wavelength that is either half
the height of the lambda max or more than ten nanometers removed
from the lambda max.
Whichever wavelengths you choose, do not select a wavelength
that has a low absorbance value. Low absorbance values
decrease the signal-to-noise ratio, thus making the absorbance
ratios less meaningful. Similarly, a small fluctuation in AU2
results in a big difference in the absorbance ratio if AU2 is very
small. Fortunately, by relying on the preset range values, the
ProStar 345 has a built-in safeguard that prevents the ratioing of
low absorbance values.
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Maintenance and Troubleshooting
Routine maintenance is necessary to ensure peak performance,
performance can only be guaranteed if you follow proper care
and maintenance procedures.
This section explains how to clean and replace your detector
flowcell and lamps.
Flowcells
This section describes the changing and general cleaning of
your detector flowcell For other flowcell problems, such as a
cracked window or leaks that occur in locations other than at the
inlet/outlet fittings, contact LC Technical Services at 1-800-FORHPLC or your local Varian Office.
NOTE: Flowcells are factory-assembled units that should not be disassembled
by a novice under any circumstances.
Changing the Flowcell
The flowcell must be removed whenever you need to replace a
broken cell, change between specialized applications, or clean
the cell with nitric acid. For a list of available flowcells, see Parts
and Accessories, page 102. All flowcells are shipped premounted in a holder for easier installation and alignment.
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Figure 13 Left-side View of Detector Chassis. Front housing contains
flowcell; rear housing contains lamps
Flowcell Removal
To access the flowcell, remove the front enclosure of the two
enclosures on the detector left side (as you face the detector
from the front). The flowcell assembly is located inside the
enclosure (Figure 13). Once the enclosure is removed, the
flowcell is easily identified by the tubing that extends from the
fittings at its top and bottom,
1. Disconnect the power cord from the detector rear panel and
turn the power switch off.
2. Loosen the knurled thumbscrew that holds the flowcell
enclosure in place, and remove and set aside both the
thumbscrew and the housing.
3. Disconnect the flowcell inlet tube from the chromatograph
and free the flowcell outlet tubing from the waste reservoir.
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DT-Z063E\DG
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