ProStar 345 User Manual

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Varian Analytical Instruments
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 This document is provided as a courtesy but is no longer kept current and thus will contain historical references to Varian.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
ProStar 345
©Varian, Inc. 1999 Printed in U.S.A. 03-914784-00:Rev. 2
Operation Manual
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Page 3

Quality Systems At Varian, Inc.

The ISO 9000 series standards were created in Geneva in 1987 to cut through a morass of conflicting quality definitions. These standards define a model for quality assurance systems in product design, development, manufacturing, installation, service, and customer support. They are now the worldwide quality assurance benchmark used to gauge the strength of a company's commitment to quality, and the value of its quality systems.
Various organizations around the world, such as the British Standards Institution (BSI), provide certified, objective auditors to scrutinize quality procedures, product development, manufacturing processes, and customer satisfaction programs. No company can claim ISO 9000 series registration unless it receives a stamp of approval from the demanding quality assessors of BSI or similar accredited examining body. ISO 9000 series registration constitutes an objective third-party report to determine the level of a supplier's commitment to quality.
In 1992, Varian, Inc., Analytical Instruments became registered to the most comprehensive of the ISO 9000 series standards — ISO 9001. ISO 9001 registration means that every stage of our quality system, including product development, manufacturing, final test, shipping, and parts and supplies has been rigorously examined against the most exacting set of internationally recognized standards. It means we live up to a standard of quality that you can count on today, and into the future. Our Quality System has received ISO 9001 certification number FM21797.
The quality systems that earned us ISO 9001 registration have direct benefits for our customers:
We can speed instruments to you faster than ever before. Emergency orders can
be processed even faster.
We fill your orders promptly and completely.
We have implemented a system of continuous feedback from our customers —
we are aware of your needs today and tomorrow.
We have improved your productivity by cutting systems failure rates in half and
speeding service response time.
We have embedded continuous improvement into the fabric of our organization
so that we can achieve even higher levels of quality in the future.
We are embedding GLP requirements into our products and services to help you
meet your regulatory compliance requirements.
ISO 9001 registration is not enough. For us, quality is defined by our customers. We are not satisfied unless you are satisfied. We are striving to understand customer needs, using independent surveys, user groups, customer advisory boards, and our “Hallmark of Quality” response program, in addition to individual face-to-face customer contact. Our products and our processes are configured to meet those needs.
We know that you are seeking more than the most advanced processes and top-notch applications expertise. You want to join forces with a partner committed to delivering world-class quality, reliability, and value — on time, every time.
Our overriding aim is to be that partner.
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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.
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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
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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.
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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.
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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.
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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
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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
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Es besteht eine ionisierende Strahlungsquelle. Beachten Sie die Vorschriften im Handbuch für eine gefahrlose Benutzung.
Bleiben Sie mit Ihren Händen und Fingern weg.
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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.
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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.
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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
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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, MISES EN GARDE et AVERTISSEMENTS. 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
03-914603-82:10 1 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.
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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
GARDE ET 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, MISES EN GARDE ET
AVERTISSEMENTS du manuel d’utilisation.
Chromatographie Flash
L’utilisateur aura la connaissance des propriétés physico-chimiques des constituants de la phase mobile.
Eviter le contact direct des solvants avec les tuyaux en polyuréthane : certains solvants sont susceptibles de provoquer des faiblesses et des fuites avec risques d’explosion.
Tous les constituants du système devront être connectés à une source de courant commune et à une prise de terre commune. Cette prise de terre devra être fixe et non mobile.
Les solvants non-polaires peuvent produire de l’électricité statique lorsqu’ils passent au travers du système. Les bouteilles qui contiennent la phase mobile (incluant les tuyaux et les flacons de collecte de fractions) doivent être mises à la terre pour éliminer l’électricité statique.
Utiliser des appareils de mesure et de décharge d’électricité statique (par exemple des ionisateurs d’air) pour combattre la formation d’électricité statique.
Radiations ultraviolettes
Les détecteurs CPL utilisant une source lumineuse ultraviolette comportent un écran destiné à se prémunir contre les expositions aux rayonnements.
Pour s’assurer une protection permanente:
Vérifier que le couvercle de protection de la lampe
des détecteurs opérant à des longueurs d’onde variables et fixes soit bien en place durant le fonctionnement du matériel.
Ne pas regarder directement les cellules du
détecteur ou la source d’UV. Se protéger systématiquement les yeux lors du contrôle de la source lumineuse ou des cellules, par exemple au moyen de verres borosilicatés ou en polystyrène.
03-914603-82:10 3 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
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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
03-914603-83:10 1 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.
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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.
03-914603-83:10 3 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
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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 ATENCION como 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
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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.
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GC Prácticas de Seguridad
Sistema de Extracción
No se necesita un sistema de extracción para los detectores GC instalados en un laboratorio bien ventilado, excepto cuando se analicen muestras químicas peligrosas. Si instala un sistema de extracción:
Utilice conductos a prueba de fuego. Instale un ventilador al final del sistema. Instale entradas de aire cuya vibración no afecte al
trabajo del detector.
Compruebe periódicamente el correcto
funcionamiento del sistema.
Asegurese de una correcta ventilación del
laboratorio.
Detectores con fuentes radioctivas
Lea con cuidado y cumpla todas las NOTAS,
PRECAUCION, y ATENCION del Manual del
Detector Ni
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
ATENCION del manual.
Cromatografía Flash
El operador debe familiarizarse con las propiedades físico-químicas de los componentes de la fase móvil.
Alejar los disolventes del contacto directo con los tubos de poliuretano ya que ciertos disolventes pueden causar reblandecimiento de los tubos o posibles fugas con riesgo de explosión.
Todos los componentes del sistema deben estar conectados a un enchufe común con toma de tierra común. Esta toma de tierra debe ser una toma de tierra verdadera en lugar de flotante.
Los disolventes no-polares pueden originar carga estática cuando son bombeados por el sistema. Todos los recipientes que contienen fase móvil (incluyendo los tubos y los recipientes de recogida) deben estar conectados a tierra para disipar la electricidad estática.
Utilizar medidores de carga estática y los debidos dispositivos de descarga (por Ej., ionizadores de aire) para salvaguardarse contra la creación de electricidad estática.
Radiación Ultravioleta
Los detectores del Cromatógrafo de Líquidos que utilizan una fuente de luz ultravioleta disponen de protección para prevenir exposiciones radioactivas al personal.
Para una correcta protección:
Asegurese de que las cubiertas de protección de la
lámpara de los detectores está correctamente situada durante su funcionamiento.
No mire directamente a las celdas del detector ó a
la fuente de luz UV. Cuando inspeccione la fuente de luz ó la celda, utilice siempre una protección para los ojos como gafas de borosilicato ó poliestireno.
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Disponibilidad de Recambios
Es Política de Varian disponer de Recambios para cualquier instrumento y la mayoría de los accesorios por un periodo de cinco (5) años después del último instrumento fabricado. Los recambios durante esos cinco años estarán disponibles, pero siempre bajo el sistema “Según disponibilidad”. Los Recambios están definidos como todas aquellas partes individuales mecánicas ó eléctricas que son susceptibles de fallo durante su normal proceso de operación. Por ejemplo, relés, lámparas, sondas de temperatura, elementos del detector, motores, etc. Las planchas de metal, partes de la estructura, placas de circuitos integrados, y otros módulos funcionales son normalmente susceptibles de reparación y por lo tanto sólo estarán disponibles bajos el sistema “Según disponibilidad” después del último instrumento fabricado.
Disponibilidad de Servicio
Varian ofrece una gran variedad de sistemas de Servicio para mantener el soporte a sus usuarios tras el periodo de garantía. El Soporte de Servicio se ofrece a través de atractivos Contratos de Servicio ó bajo un sistema de facturación de mano de obra y materiales. El mantenimiento y el entrenamiento se realiza por ingenieros cualificados bajo Contrato ó petición.
Oficinas de Instrumentación Analítica Varian
Para cualquier consulta sobre Instrumentación Analítica, Servicio Técnico ó Recambios y Accesorios, contacte con su oficina local:
Argentina
Buenos Aires Tel. +54.11.4.783.5306
Australia Mulgrave, Victoria Tel. +61.3.9566.1134
Austria Vösendorf bei Wien Tel. +43.1.699.9669
Benelux Bergen Op Zoom Tel. +31.164.282.800
Brazil and Latin America (S) São Paulo Tel. +55.11.820.0444
Canada Mississauga, Ontario Tel. 800.387.2216
China Beijing Tel. +86.106209.1727
Europe Middelburg, The Netherlands Tel. +31.118.671.000
France Les Ulis Cédex Tel. +33.1.6986.3838
Germany Darmstadt Tel. +49.6151.7030
India Mumbai Tel. +91.22.857.0787/88/89
Italy Torino Tel. +39.011.997.9111
Japan Tokyo Tel. +81.3.5232.1211
Korea Seoul Tel. +82.2.345.22452
Mexico and Latin America (N)
Mexico City Tel. +52.5.523.9465
Russian Federation Moscow Tel. +7.095.937.4280
Spain Madrid Tel. +34.91.472.7612
Sweden Solna Tel. +46.8.445.1620
Switzerland Varian AG Tel. +41.848.803.800
Taiwan Taipei Hsien Tel. +886.2.698.9555
United Kingdom and Ireland
Walton-on-Thames Tel. +44.1932.898000
Venezuela Valencia Tel. +58.41.257.608
United States Walnut Creek, California, USA Tel. +1.800.926.3000 (GC and GC/MS)
Tel. +1.800.367.4752 (LC)
www.varianinc.com
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Table of Contents

Introduction.............................................................................................. 1
Startup Checklist...........................................................................................................1
Manual Conventions .....................................................................................................1
Displays.............................................................................................................................................. 2
Text..................................................................................................................................................... 2
Standard Words.................................................................................................................................. 2
Installation................................................................................................ 5
Unpacking .....................................................................................................................5
Installation.....................................................................................................................5
Voltage Selection..........................................................................................................6
Fuses.............................................................................................................................9
Rear Panel Connections...............................................................................................9
Connecting an Integrator, Workstation, or Recorder..................................................11
Remote Communications Connections ......................................................................11
Flowcell Connections..................................................................................................12
Optional Flowcells.......................................................................................................13
Flowcell Orientation.....................................................................................................14
Re-orienting the Flowcell ............................................................................................15
Using the ProStar 345.................................................................................................16
Finding Your Way Around.................................................................................................................16
Visual Clues...................................................................................................................................... 17
Instrument Control.......................................................................................................18
Menus, Screens, and Messages.................................................................................20
Main Menu........................................................................................................................................20
Status Screen................................................................................................................................... 20
Status Menu......................................................................................................................................21
Messages .........................................................................................................................................21
Basic Operation..................................................................................... 23
A Quick Example.........................................................................................................23
Startup.............................................................................................................................................. 23
Setting Parameters...........................................................................................................................23
Wavelength....................................................................................................................................... 24
Range............................................................................................................................................... 24
Loading the File................................................................................................................................ 25
Practice Run..................................................................................................................................... 26
Adding a Stop Time.......................................................................................................................... 26
Single and Dual Wavelength Operation......................................................................27
Setting Parameters...........................................................................................................................28
File Identification............................................................................................................................... 28
ProStar 345 UV-Vis Detector i
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Wavelength Program........................................................................................................................28
Options ............................................................................................................................................. 29
Loading a File................................................................................................................................... 31
Running The ProStar 345...........................................................................................31
Status Screen................................................................................................................................... 31
Inject Sample....................................................................................................................................31
Starting a Run................................................................................................................................... 32
Stopping a Run.................................................................................................................................32
Changing Run Parameters .........................................................................................33
Status Menu......................................................................................................................................33
Saving the File..................................................................................................................................34
More About Files.........................................................................................................34
Copying Files....................................................................................................................................35
Deleting Files....................................................................................................................................35
Analog Output Operations ..........................................................................................37
Analog Outputs.................................................................................................................................37
Analog Offsets.................................................................................................................................. 38
Advanced Operation.............................................................................. 39
Wavelength Programming ..........................................................................................39
Building the Program........................................................................................................................ 39
Entering Subsequent Time Lines ..................................................................................................... 40
Stop Line...........................................................................................................................................40
Deleting a Line.................................................................................................................................. 40
Running a Program...........................................................................................................................41
Programmed Autozero................................................................................................41
Automatic Lamp Operations .......................................................................................42
Lamps Menu.....................................................................................................................................42
Other Features............................................................................................................45
Status Lock.......................................................................................................................................45
Short Outputs....................................................................................................................................46
Event Mark........................................................................................................................................46
Ready Output....................................................................................................................................47
Display Contrast ...............................................................................................................................47
Cursor Speed....................................................................................................................................47
Shutdown Detector........................................................................................................................... 48
Scanning .....................................................................................................................48
How it Works.....................................................................................................................................48
Selecting the Scan File.....................................................................................................................50
Scan Summary Data Screen............................................................................................................ 53
Stopping the Scan File ..................................................................................................................... 54
Replaying Your Spectra.................................................................................................................... 54
Setting Replay Parameters............................................................................................................... 54
Running Replay................................................................................................................................ 55
Spectral Data Storage ......................................................................................................................56
Viewing Data.....................................................................................................................................56
Develop File ................................................................................................................56
Selecting the Develop File................................................................................................................57
Editing the Develop File.................................................................................................................... 57
Running the Develop File .................................................................................................................58
Repeating the Develop File ..............................................................................................................59
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Sample Queue............................................................................................................59
Queue Menu.....................................................................................................................................59
Setting Up a Queue.......................................................................................................................... 60
Entering a Line..................................................................................................................................60
Adding More Lines............................................................................................................................ 60
Deleting a Line.................................................................................................................................. 60
Loading a Queue.............................................................................................................................. 61
Running a Queue..............................................................................................................................61
Viewing the Progress of a Queue.....................................................................................................61
Loading Other Files .......................................................................................................................... 62
Editing a Queue................................................................................................................................62
Pausing a Queue..............................................................................................................................62
Deleting/Stopping a Queue...............................................................................................................63
K-Factor ......................................................................................................................63
Choosing a Pair of Wavelengths ......................................................................................................65
Calculating the K-Factor................................................................................................................... 66
Using the K-Factor............................................................................................................................ 66
Absorbance Ratios......................................................................................................68
Maintenance and Troubleshooting ...................................................... 71
Flowcells .....................................................................................................................71
Changing the Flowcell ......................................................................................................................71
Flowcell Removal..............................................................................................................................72
Flowcell Installation .......................................................................................................................... 75
Cleaning the Flowcell........................................................................................................................76
Flow Cell Maintenance .....................................................................................................................79
Lamps..........................................................................................................................83
The Deuterium Lamp........................................................................................................................84
The Tungsten Lamp..........................................................................................................................88
Theory of Operation....................................................................................................89
Troubleshooting Table ................................................................................................91
Error Messages...........................................................................................................94
System Errors...................................................................................................................................94
Real-Time Errors .............................................................................................................................. 94
Input Errors.......................................................................................................................................95
Diagnostic Tests..........................................................................................................96
Software Version ..............................................................................................................................97
Light Levels ...................................................................................................................................... 97
Diode Offsets....................................................................................................................................97
λ
Calibration......................................................................................................................................98
Self-Tests..........................................................................................................................................98
Appendix.............................................................................................. 101
Specifications........................................................................................................... 101
Parts and Accessories............................................................................................. 102
Menu Tree................................................................................................................ 103
Menu List.................................................................................................................. 104
Glossary................................................................................................................... 111
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Introduction

Startup Checklist

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.
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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
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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
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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
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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.
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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.
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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.
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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.
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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
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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
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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. Dont 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.
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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
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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
27
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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 dont 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 youre 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 youre using a stop-line in your wavelength program, youll 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 isnt 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 youre 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 youve 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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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 youre 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
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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.
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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, youll 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/.
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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 youre finished setting up the Scan File, youre ready to load it and run. When the Scan File is loaded, youll 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.
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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 werent 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 youve 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 youre 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, youre 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.
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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 youve 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, youre ready to load it and run.

Running the Develop File

When the Develop File is loaded, youll 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
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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 cant 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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Order File:Name #Runs
1 2:THEOPHYL 5
2 3:ABCD 25
3 1:BABITUR 10
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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, youll 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, youll have to pause the queue first.
on page 60. Youre 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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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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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 doesnt. 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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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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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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