Varian GC-MS - Saturn 2000 GC-MS Hardware Manual 914978
Varian GC-MS - Saturn 2000 GC-MS Hardware Manual 914978
Varian GC-MS - Saturn 2000 GC-MS Hardware Manual 914978
Hardware Manual
Printed in U.S.A.
03-914978-00:Rev. 1
All rights reserved including the right of reproduction in whole or in part in any form. This document may be electronically reproduced, distributed, or printed in its entirety provided this copyright and statement are attached. Any modification or any other reproduction, distribution, or use of this document or portions hereof is strictly prohibited without the express written permission of Varian, Inc. COPYRIGHT 2001 - 2003. All rights reserved.
Declaration of Conformity
We hereby Declare that the equipment listed below complies with the requirements of: The Low Voltage Directive 73/23/EEC (93/68/EEC) The EMC Directive 89/336/EEC (92/31/EEC and 93/68/EEC)
Applicable Standards
LVD EMC TUV File Number(s): Type of Equipment: EN 61010 EN 50082-1 EN 55011 E9672056 Mass Spectrometer P9672055 Model: Saturn 2000 Series
Manufacturer
Print Name: Martin ODonoghue Signed: Position: General Manager Date: October 16, 2001 Company Name: Varian, Inc. Address: 2700 Mitchell Drive Walnut Creek, California 94598 USA Telephone: 925-939-2400 Fax: 925-945-2168
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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.
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.
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Garantieeinschrnkungen
Diese Garantie erfat nicht vom Kunden bereitgestellte Software, Ausrstungen und Software, die von anderen Herstellern garantiert werden oder den Austausch entbehrlicher Teile und solcher von begrenzter Lebensdauer wie diese, aber nicht darauf beschrnkt: Filter, Glaswaren, Instrument Statuslampen, Lampenquellen, Septen, Sulen, Sicherungen, Schreiberpapier und Tinte, Zerstuber, Fluzellen, Kolben, Dichtungen, Fittings, Ventile, Brenner, Probenrhrchen, Sondeneinstze, Druckkpfe, glasausgekleidetes Rohr, Leitungsund Rohrfittings, Dewars fr variable Temperaturen, Transferleitungen, flexible Disketten, Magnetbandkassetten, elektronische Vervielfacher, Hitzdrhte, Vakuum Gaskets, Sitzflchen und alle Teile, die den Proben und mobilen Phasen ausgesetzt sind. Diese Garantie erlischt bei eingetretenem Unfall, falscher Benutzung, Umbau, Mibrauch, Vernachlssigung, Bruch, falscher Benutzung oder falscher Wartung, unbefugten oder falschen Modifikationen oder Basteleien, Benutzung in ungeeigneter physikalischer Umgebung, Benutzung mit marginaler Stromversorgung oder Benutzung mit anderen ungengenden Einrichtungen oder Versorgungen. Mit vernnftiger Sorgfalt mssen Gefahren vermieden werden. Diese Garantie steht ausdrcklich anstelle von allen anderen angedeuteten Garantien und schliet sie aus, einschlielich, aber nicht beschrnkt auf Garantien der Verkuflichkeit und Eignung fr einen besonderen Zweck, Gebrauch oder Anwendung und allen anderen Verpflichtungen oder Haftungen von Varians Seite, wenn nicht solche Garantien, Verpflichtungen oder Haftungen ausdrcklich schriftlich mit Varian vereinbart wurden.
Softwareprodukte
Wo Software innerhalb des Rahmens eines Lizenzabkommens zwischen dem Kunden und Varian geliefert wird, wird die Garantie genau entsprechend der zeitlichen Abmachung eingehalten. Besteht kein Lizenzabkommen und ist keine alternative Garantiezeit schriftlich zwischen Varian und dem Kunden festgelegt, gilt die Garantiezeit der Allgemei-nen Lieferbedingungen. Varian garantiert fr solche Softwareprodukte, die mit Varians Hardware benutzt und richtig installiert sind oder zur Ausfhrung mit anderer von Varian angegebener Hardware, wie sie in der beigefgten Bedienungsanleitung beschrieben ist, da sie im wesentlichen frei von solchen Defekten sind, die Fehler bei der Ausfhrung der jeweiligen Programmieranweisungen verursachen; Varian garantiert jedoch keine ununterbrochene oder fehlerfreie Arbeitsweise.
Abhilfen
Die einzige und ausschlieliche Abhilfe in der Hardwaregarantie wird die Reparatur der Instrumentstrungen sein, die sich nach Varian's Ansicht auf Defekte in den Originalteilen oder bei der Herstellung zurckfhren lt oder, nach Varian's Wahl, der Austausch der entsprechenden defekten Teile oder die Erstattung eines fairen Teils des Kaufpreises des Instruments oder Zubehrs, vorausgesetzt, da sich Varian alternativ dafr entscheidet. Reparatur oder Austausch unter Garantie verlngert nicht die ursprngliche Garantiezeit.
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Limitation de garantie
Cette garantie ne couvre pas le logiciel fourni par le Client, les quipements ou logiciels garantis par un autre fabricant ni le remplacement des pices consommables ou prsentant une dure de vie limite, notamment : filtres, verres, indicateurs d'tat de l'instrument, lampes source, septa, colonnes, fusibles, papier graphique et encre, nbuliseurs cellules, pistons, joints, raccords, vannes, brleurs, tubes d'chantillonnage, inserts de sonde, ttes d'impression, tubes garniture de verre, dewars, lignes de transfert, disquettes, cassettes magntiques, multiplicateurs d'lectron, filaments, joints hermtiques, isolant et toutes les pices en contact avec des chantillons et des phases mobiles. Ladite garantie est nulle en cas d'accident, de mauvaise utilisation,d'altration, de ngligence, de bris, d'utilisation, maintenance voire de modifications inappropries, d'utilisation dans un environnement inadapt, d'utilisation avec une alimentation marginale ou d'autres installations ou services inappropris. Un certain nombre de prcautions doivent tre prises pour viter tout accident. Ladite garantie se substitue et exclue expressment toute garantie expresse ou tacite, y compris mais ne se limitant pas aux garanties relatives la qualit marchande du programme et la garantie de son aptitude une utilisation ou une application particulire, ainsi que toutes les autres obligations ou engagements de la part de Varian, moins que lesdites garanties,obligations ou engagements aient fait expressment l'objet d'un accord crit deVarian.
Logiciel
Pour tout logiciel faisant l'objet d'un accord de licence conclu entre le client et Varian, la garantie sera strictement limite aux termes dudit accord. En l'absence d'accord de licence et sauf accord crit sur tout autre priode de garantie entre Varian et le client, la priode de garantie est telle que spcifie sur le recto du devis de Varian. Sous rserve de leur installation et de leur utilisation correcte sur le matriel Varian ou tout autre matriel, tel que spcifi, Varian garantie le fonctionnement tel que dcrit dans le manuel d'utilisation fourni avec le matriel et l'absence de dfauts entranant l'impossibilit d'excuter des instructions de programmation respectives. Toutefois, Varian ne garantit pas un fonctionnement sans interruption et sans erreurs.
Recours
Le seul et unique recours relatif la garantie du matriel se limite la rparation suite un mauvais fonctionnement de l'instrument, qui, de l'avis de Varian, est d des dfauts des pices d'origine ou de la fabrication, ou, la discrtion de Varian, au remplacement des pices dfectueuses en question, sous rserve du choix de Varian de rembourser une part raisonnable du prix d'achat de l'instrument ou de l'accessoire. La rpaation ou le remplacement sous garantie n'tend pas la priode de garantie originale. La rparation ou le remplacement, aux termes d'un recours, est laiss l'entire discrtion de Varian, soit par l'envoi d'un technicien de maintenance sur le site du client, soit en autorisant le client retourner l'accessoire ou l'instrument dfectueux Varian, voire l'envoyer un service de maintenance dsign.
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Prodotti software
Se il software viene fornito nell'ambito d'un contratto di licenza stipulato tra la Varian e il Cliente, trovano applicazione in via esclusiva le garanzie previste dal contratto. In assenza d'un contratto di licenza e salvo diverso accordo scritto tra la Varian e il Cliente, vale il periodo di garanzia indicato nell'offerta della Varian. La Varian garantisce che i prodotti software, purch regolarmente utilizzati ed installati su hardware Varian o d'altre marche da essa indicate, hanno le prestazioni descritte nel Manuale d'uso fornito a corredo del software e che sono sostanzialmente esenti da difetti che impediscano l'esecuzione delle rispettive istruzioni di programma. La Varian non garantisce alcun funzionamento ininterrotto o senza errori.
Interventi Tecnici
Gli unici interventi previsti dalla garanzia sull'hardware sono o la riparazione dei malfunzionamenti dello strumento che, a giudizio della Varian, siano dovuti o riconducibili a difetti di costruzione dei materiali originali o, a discrezione della Varian, la sostituzione dei componenti difettosi, fermo restando che la Varian potr, in alternativa, optare per il rimborso di una congrua parte del prezzo d'acquisto dello strumento o dell'accessorio difettosi. La riparazione o la sostituzione in garanzia non valgono a prorogare in alcun modo il periodo di garanzia originariamente previsto.
interventi
delle
Quelli qui contemplati sono gli unici ed esclusivi interventi cui ha diritto il Cliente. In nessun caso la Varian sar responsabile per danni indiretti o consequenziali, mancata disponibilit, perdita di produzione o altre perdite subite.
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Limitacin de garanta
Esta garanta no cubre software provisto por el cliente, equipos y software garantizados por otros fabricantes, consumibles o artculos de duracin de vida limitada, como son, entre otros: filtros, elementos de vidrio, pilotos, lmparas, diafragmas, columnas, fusibles, papel y tinta de grficos, nebulizadores, clulas de flujo, pistones, cierres, juntas, vlvulas, quemadores, tubos de muestras, inserciones de sondas, cabezales de impresin, tubos de vidrio, juntas de tubo, dispositivos de temperatura variable, lneas de transferencia, disquetes, cintas magnticas, multiplicadores de electrones, filamentos, juntas de vaco, soportes y todos los componentes en contacto con muestras y partes mviles. Esta garanta no tendr efecto en los casos de accidente, abuso, alteracin, utilizacin incorrecta, negligencia, rotura, mantenimiento o uso inadecuados, modificaciones inadecuadas o no autorizadas, uso de la fuerza, uso en un entorno inadecuado, funcionamiento con una alimentacin defectuosa o el uso con medios inadecuados. Es necesario tomar las precauciones adecuadas para evitar riesgos. Las garantas de los productos de software de Varian sustituyen y excluyen cualquier otra garanta, implcita o explcita, incluidas pero sin limitacin, las garantas de comerciabilidad, adecuacin a un fin, uso o aplicacin en particular, y todas las dems obligaciones y responsabilidades por parte de Varian, a no ser que estas garantas, obligaciones y responsabilidades sean otorgadas expresamente y por escrito por Varian.
Productos de software
Cuando el software se suministra dentro del marco de una licencia de utilizacin acordada entre Varian y el cliente, cualquier garanta estar estrictamente limitada a los trminos del citado acuerdo. En ausencia de una licencia de utilizacin y a no ser que exista un acuerdo de perodo de garanta por escrito entre Varian y el cliente, el perodo de garanta ser el fijado de acuerdo con los trminos de Varian que se citan. Varian garantiza estos productos de software si se instalan y usan con hardware Varian, u otro tipo de hardware en el que Varian certifique que funcionan segn lo descrito en Manual de instrucciones, y que est libre de defectos que impidan la ejecucin de instrucciones de programacin. Sin embargo, Varian no garantiza la utilizacin ininterrumpida o libre de errores.
Recursos
El nico y exclusivo recurso en cuanto a hardware bajo garanta ser reparar los defectos del aparato, que, en opinin de Varian, sean claramente imputables a defectos de los materiales originales o de fabricacin, o sustituir los componentes defectuosos, pudiendo Varian optar por reembolsar una parte equitativa del precio de compra del aparato o componente. Las reparaciones o sustituciones en perodo de garanta no prolongan el perodo de garanta original.
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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. Alerts you to situations that may cause moderate injury and/or equipment damage, and how to avoid these situations. Warning Description Hazardous voltages are present inside instrument. Disconnect from main power before removing screw-attached panels. Hazardous chemicals may be present. Avoid contact, especially when replenishing reservoirs. Use proper eye and skin protection. Very hot or cryogenically cold surfaces may be exposed. Use proper skin protection. Eye damage could occur either from flying particles, chemicals or UV radiation. Use proper eye and face protection. The potential for fire may be present. Follow manual instructions for safe operation. The potential for explosion may exist because of type of gas or liquid used. Ionizing radiation source is present. Follow manual instructions for safe operation. Keep hands and fingers away. Alerts you to potentially hazardous situations that could result in serious injury, and how to avoid these situations.
Warning Symbol
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T T T T
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
T T T T T
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.
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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: T Use only fireproof ducting. T Install a blower at the duct outlet. T Locate duct intakes such that their vibration or air movement does not effect detector operation. T Check periodically for proper operation of the duct. T Ensure proper ventilation in lab area.
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.
Radioactive Source Detectors T Read carefully and comply with all NOTES,
T T
CAUTIONS, and WARNINGS in the Ni63 ECD manual. Perform the tests for removable radioactive contamination described in the Ni63 ECD manual. Comply with leak test schedules and procedures.
Ultraviolet Radiation
Liquid chromatograph detectors that use an ultraviolet light source have shielding to prevent radiation exposure to personnel. For continued protection:
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.
T T
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.
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.
T T T T T
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.
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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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 asneeded basis.
Argentina Buenos Aires Tel. +54.11.4.783.5306 Australia Mulgrave, Victoria Tel. +61.3.9566.1134 Austria Vsendorf bei Wien Tel. +43.1.699.9669 Benelux Bergen Op Zoom Tel. +31.164.282.800 Brazil and Latin America (S) So 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 Cdex 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
Arbeitsanleitungen
Diese Arbeitsanleitung will Ihnen bei der Aufstellung solcher Arbeitsbedingungen helfen, die einen sicheren und wirkungsvollen Gebrauch Ihrer Gerte ermglichen. Besondere berlegungen und Vorsichtsmanahmen erscheinen in diesem Handbuch in Form von HINWEIS, ACHTUNG und WARNUNG, wie unten beschrieben. Es ist wichtig, da Sie Ihr Gert in bereinstimmung mit dieser Arbeitsanleitung und allen mglichen zustzlichen Informationen von Varian betreiben. Alle Fragen bezglich Sicherheit und Handhabung Ihres Gertes richten Sie an Ihr Varian Bro.
ACHTUNG
Weist auf Situationen, die zu miger Beeintrchtigung und/oder zu Gerteschden fhren und auf die Vermeidung dieser Situationen hin.
WARNUNG
Weist auf mgliche Gefahrensituationen, die zu ernsthaften Verletzungen fhren knnen und auf die Vermeidung dieser Situationen hin.
Warnungssymbol
Warnungsbeschreibung Gefhrliche Spannungen bestehen innerhalb des Instruments. Trennen Sie das Gert vom Netz, bevor Sie abschraubbare Paneele entfernen. Gefhrliche Chemikalien knnen vorhanden sein. Vermeiden Sie jeden Kontakt, besonders beim Auffllen der Reservoirs. Benutzen Sie wirksamen Augen und Hautschutz.
WARNUNG
ELEKTRISCHER SCHLAG
WARNUNG
Herumfliegende Partikel, Chemikalien oder UV-Strahlung knnen Augenschden verursachen. Tragen Sie deshalb einen geeigneten Schutz fr Augen und Gesicht.
WARNUNG
FEUERGEFAHR
Es besteht eine mgliche Feuergefahr. Beachten Sie die Vorschriften im Handbuch fr eine gefahrlose Benutzung. Eine mgliche Explosionsgefahr besteht infolge der benutzten Gas- oder Flssigkeitsart. Es besteht eine ionisierende Strahlungsquelle. Beachten Sie die Vorschriften im Handbuch fr eine gefahrlose Benutzung.
WARNUNG
EXPLOSIONSGEFAHR
WARNUNG
STRAHLUNGSQUELLE
WARNUNG
BEWEGTE TEILE
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Allgemeine Sicherheitsmanahmen
Befolgen Sie diese Sicherheitspraktiken fr eine gefahrlose Gertebenutzung. Prfen Sie regelmig alle Versorgungs und Pneumatikleitungen auf Lecks. Gasleitungen drfen nicht geknickt oder angestochen werden. Verlegen Sie die Leitungen auerhalb von Laufwegen und abseits von extremer Hitze oder Klte. Lagern Sie organische Lsungsmittel in feuerfesten, belfteten und eindeutig bezeichneten Schrnken, damit sie leicht als toxische und/oder brennbare Materialien erkannt werden. Sammeln Sie keine Lsungsmittelabflle. Entsorgen Sie solche Materialien ber ein geregeltes Entsorgungsprogramm und nicht ber die ffentlichen Abwasserleitungen.
HINWEIS:
Dies Instrument wurde nach den zutreffenden Vorschriften der EMC Direktive getestet, die zum Fhren des CE Zeichens der Europischen Union berechtigen. Dieses Gert kann an sich auf Strahlungs-/Strpegel oder Frequenzen auerhalb der getesteten Grenzen reagieren. Dies Instrument ist fr chromatographische Analysen entsprechend prparierter Proben Handbuch spezifizierten maximalen Werte fr Druck, Flsse und Temperaturen betrieben werden. Der Kunde ist vor der Durchfhrung irgendeines Gerteservices verpflichtet den Varian biologischer, radioaktiver oder toxischer Proben benutzt worden ist.
WARNUNG gedacht. Es mu mit geeigneten Gasen und/oder Lsungsmitteln und innerhalb der im
Elektrische Gefahren
Lsen Sie das Instrument von allen Stromquellen, bevor Sie Schutzpaneele entfernen, damit Sie nicht mit potentiell gefhrlichen Spannungen in Berhrung kommen. Wenn ein Nicht-Original Netzkabelstecker benutzt werden mu, mu das Austauschkabel die im Handbuch beschriebene Farbcodierung und Polaritt beibehalten und alle rtlichen Sicherheitsvorschriften erfllen. 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 dafr, da Spannungsquellen und die Netzspannung den gleichen Wert haben, fr den das Instrument verdrahtet ist.
Gasdruckflaschen
Lagern und handhaben Sie komprimierte Gase vorsichtig und in strikter Einhaltung der Sicherheitsvorschriften. Befestigen Sie die Gasflaschen an feststehenden Aufbauten oder an Wnden. Lagern und transportieren Sie Gasflaschen in aufrechter Stellung. Druckregler zuvor abnehmen. Lagern Sie Gasflaschen in gut durchlfteten Rumen, weit genug weg von Heizungen, direktem Sonnenschein, Frosttemperaturen und Entzndungszonen. Kennzeichnen Sie die Flaschen so eindeutig, da kein Zweifel ber deren Inhalt bestehen kann. Benutzen Sie nur geprfte Druckminderer und Verbindungsstcke. Benutzen Sie nur chromatographisch reines Verbindungsrohr (Varian Part Number 03-918326-00), das wesentlich hheren Druck als den hchsten Ausgangsdruck des Druckminderers aushlt.
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GC Sicherheitspraktiken
Abgassystem
Fr GC Detektoren, die in einem gut durchlfteten Raum installiert sind, ist keine spezielle Abgasfhrung erforderlich, auer wenn die Detektoren zum Testen gefhrlicher Chemikalien benutzt werden. Wenn Sie eine Abgasfhrung installieren: Benutzen Sie nur feuerfeste Fhrungen. Installieren Sie ein Geblse am Ausgang. Ordnen Sie die Ansaugffnung so an, da ihre Erschtterungen oder Luftstrmungen nicht die Detektorfunktion beeintrchtigen. Prfen Sie regelmig die einwandfreie Arbeitsweise der Abgasfhrung. Sorgen Sie fr gute Entlftung im Laborbereich.
ffnen Sie niemals eine unter Druck stehende Lsungsmittelleitung oder ein Ventil. Halten Sie zuerst die Pumpe an und lassen Sie den Druck auf Null abfallen. Benutzen Sie splittersichere Reservoirs, die fr 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 Lsungsmittel mit den Zufhrungsleitungen aus Polyurethan, da einige Lsungsmittel das Material der Leitungen schwchen und damit Undichtigkeiten oder Brche hervorrufen knnen. 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 Lsungsmittel knnen sich beim Pumpen durch das System statisch aufladen. Alle Gefe, die mobile Phase enthalten (einschlielich Leitungen und Sammelgefe), mssen zur Ableitung elektrostatischer Aufladungen geerdet sein. Setzen Sie Gerte zur Messung und Ableitung elektrostatischer Aufladungen (z.B. Gerte zur Luftionisierung) als Manahmen gegen den Aufbau statischer Elektrizitt ein.
Radioaktive Detektoren
Lesen Sie sorgfltig und befolgen Sie alle HINWEISE, ACHTUNGEN und WARNUNGEN im Ni63 ECD Handbuch. Fhren Sie die Tests fr zu beseitigende radioaktive Kontamination durch, die im Ni63 ECD Handbuch beschrieben sind. Erfllen Sie die Zeitplne und Verfahren zur Dichtigkeitsprfung.
Verbrennungsgefahr
Beheizte oder tieftemperaturgekhlte Zonen des Gaschromatographen knnen betrchtlich lange hei oder kalt bleiben, nachdem das Instrument bereits abgeschaltet ist. Zur Vermeidung schmerzhafter Verbrennungen mssen Sie darauf achten, da alle beheizten oder gekhlten Zonen auf Raumtemperatur zurckgegangen sind oder Sie mssen ausreichenden Handschutz benutzen, bevor Sie mglicherweise heie oder kalte Oberflchen berhren.
Ultraviolette Strahlung
Detektoren in Liquidchromatographen, die eine ultraviolette Lichtquelle benutzen, besitzen eine Abschirmung, die das Bedienungspersonal gegen Abstrahlungen schtzt. Zum stndigen Schutz: Achten Sie darauf, da die schtzende Lampenabdeckung der Detektoren mit variablen und festen Wellenlngen whrend des Betriebs an ihrem Platz ist. Schauen Sie nicht direkt in die Flssigkeitszellen im Detektor oder in die UV Lampe. Zum Inspizieren der Lichtquelle oder der Flssigkeitszelle benutzen Sie immer einen wirksamen Augenschutz, wie er durch Borsilikatglas oder Polystyrol gewhrleistet wird.
LC Sicherheitspraktiken
Gefahr durch hohen Druck
Wenn eine Leitung bricht, eine Entlftungseinheit sich ffnet oder ein Ventil sich unbeabsichtigt unter Druck ffnet, kann durch die Pumpe mglicherweise ein gefhrlich hoher Flssigkeitsdruck entstehen, der einen Strahl flchtiger und/oder toxischer Flssigkeiten von hoher Stmungsgeschwindigkeit verursacht. Tragen Sie einen Gesichtsschutz, wenn Sie Proben injizieren oder Routinewartungen durchfhren.
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Serviceverfgbarkeit
Varian bietet seinen Kunden auch nach dem Auslaufen der Garantie eine Vielfalt von Serviceleistungen an. Reparaturservice kann zu attraktiven Preisen ber eine Wartungsvereinbarung oder nach Zeit- und Materialaufwand zur Verfgung gestellt werden. Technische Untersttzung und Training bieten wir Ihnen durch qualifizierte Chemiker sowohl auf einer Kontraktbasis als auch nach Ihren Erfordernissen an.
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NOTE
Information destine tirer le meilleur parti du matriel sur le plan des performances Attire lattention sur une situation pouvant occasionner des dommages corporels lgers et/ou des dgts mineurs lappareil et indique comment remdier cette situation Attire lattention sur une situation potentiellement dangereuse pouvant occasionner des dommages corporels importants et indique comment remdier cette situation
Symboles davertissement
Description Exposition des tensions dangereuses. Dbrancher le matriel du secteur avant de dvisser les panneaux protecteurs. Prsence ventuelle de substances chimiques dangereuses. Eviter tout contact, en particulier lors du remplissage des rservoirs. Prendre les mesures de protection adquates pour les yeux et la peau.
ATTENTION
RISQUE D'ELECTROCUTION
ATTENTION
RISQUE DE BRLURES
Exposition des surfaces chaudes ou traites cryogniquement. Prendre les mesures de protection adquates pour la peau. Les dommages causes aux yeux sont de deux natures diffrentes : jet de particules et de produits chimiques ou radiations UV. Utiliser des protections du visage et des yeux appropries.
ATTENTION
RISQUE D'INCENDIE
Risque potentiel dincendie. Se conformer aux instructions du manuel pour faire fonctionner le matriel en toute scurit. Risque potentiel dexplosion en raison du type de gaz ou de liquide utilis. Prsence dune source de radiation ionisante. Se conformer aux instructions du manuel pour faire fonctionner le matriel en toute scurit. Garder les mains et les doigts hors de porte.
ATTENTION
RISQUE D'EXPLOSION
ATTENTION
SOURCE DE RADIATION
ATTENTION
PIECES EN MOUVEMENT
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NOTE:
Ce matriel a t test conformment aux dispositions de la directive CME afin de pouvoir porter le sigle CE de lUnion europenne. Il en rsulte quil peut tre sensible des niveaux de radiation/dinterfrence ou des frquences se situant hors des limites testes. Ce matriel est conu pour effectuer des analyses chromatographiques dchantillons et/ou les solvants adquats et dans les limites des pressions, des dbits et des tempratures maximales spcifies dans le prsent manuel.
ATTENTION prpars selon des mthodes appropries. Il convient de le faire fonctionner avec les gaz
Le client est tenu dinformer le service Varian dassistance la clientle que son matriel
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Ne jamais dconnecter un conduit de solvant ou une vanne sous pression. Arrter pralablement la pompe et laisser la pression descendre zro. Utiliser des rservoirs incassables 50-60 psi. Laisser lenceinte du rservoir ferme lorsque le rservoir est sous pression. Se conformer aux NOTES, MISES EN GARDE ET AVERTISSEMENTS du manuel dutilisation.
Chromatographie Flash
Lutilisateur aura la connaissance des proprits physico-chimiques des constituants de la phase mobile. Eviter le contact direct des solvants avec les tuyaux en polyurthane : certains solvants sont susceptibles de provoquer des faiblesses et des fuites avec risques dexplosion. Tous les constituants du systme devront tre connects une source de courant commune et une prise de terre commune. Cette prise de terre devra tre fixe et non mobile. Les solvants non-polaires peuvent produire de llectricit statique lorsquils passent au travers du systme. Les bouteilles qui contiennent la phase mobile (incluant les tuyaux et les flacons de collecte de fractions) doivent tre mises la terre pour liminer llectricit statique. Utiliser des appareils de mesure et de dcharge dlectricit statique (par exemple des ionisateurs dair) pour combattre la formation dlectricit statique.
Risque de brlures
Les zones des chromatographes gaz chauffes ou traites cryogniquement peuvent rester trs chaudes ou trs froides durant une priode plus ou moins longue aprs la mise hors tension du matriel. Pour viter les brlures, sassurer que ces zones sont revenues temprature ambiante ou utiliser un dispositif adquat de protection des mains avant de les toucher.
Radiations ultraviolettes
Les dtecteurs CPL utilisant une source lumineuse ultraviolette comportent un cran destin se prmunir contre les expositions aux rayonnements. Pour sassurer une protection permanente: Vrifier que le couvercle de protection de la lampe des dtecteurs oprant des longueurs donde variables et fixes soit bien en place durant le fonctionnement du matriel. Ne pas regarder directement les cellules du dtecteur ou la source dUV. Se protger systmatiquement les yeux lors du contrle de la source lumineuse ou des cellules, par exemple au moyen de verres borosilicats ou en polystyrne.
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NOTA
Sono informazioni utili ad ottenere le prestazioni migliori da parte dello strumento.
ATTENZIONE
ATTENZIONE
Allerta loperatore su situazioni che potrebbero causare ferite leggere e danni limitati allo strumento ed il modo di evitarle. Descrizione del Pericolo
Allerta loperatore su situazioni potenzialmente pericolose che possono causare danni molto seri ed il modo di evitarle.
Segnali di ATTENZIONE
ATTENZIONE
Pericolo di folgorazioni
Nello strumento sono presenti tensioni pericolose. Scollegare il cavo di alimentazione prima di togliere il pannello fissato con le viti. Possono essere presenti composti chimici pericolosi. Evitare il contatto, specialmente quando si riempiono i contenitori. Usare protezioni opportune per la pelle e per gli occhi.
ATTENZIONE
Pericolo di scottature
Pericolo di esposizione a superfici molto calde o raffreddate criogenicamente. Usare protezioni opportune per la pelle. Particelle volanti, agenti chimici o radiazioni UV possono danneggiare gli occhi. Vanno quindi utilizzate le opportune protezioni per gli occhi e per il volto.
Pericolo potenziale di incendio. Seguire le istruzioni del manuale per lavorare con una maggiore sicurezza. C pericolo di esplosioni a causa del tipo di gas o liquido utilizzato. E presente una radiazione ionizzante. Seguire le istruzioni del manuale per lavorare con una maggiore sicurezza. Non tenere le mani o le dita vicino.
ATTENZIONE
Pericolo di esplosioni
ATTENZIONE
Pericolo di radiazioni
ATTENZIONE
Parti in movimento
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Norme di Sicurezza
Per lavorare in modo sicuro sullo strumento, Vi consigliamo si adottare le seguenti procedure. Verificare periodicamente che non ci siano perdite sulle linee e sui raccordi pneumatici. Evitare che le linee dei gas vengano piegate o forate. Le linee vanno posizionate in modo tale da non essere calpestate e lontane da sorgenti o troppo calde o troppo fredde. I solventi organici vanno conservati in armadi speciali antiincendio, ventilati e con indicazioni chiare sul contenuto di materiali tossici e/o infiammabili. Non accumulare i solventi utilizzati. Adottare un programma regolare di smaltimento, ma mai nelle acque di scarico.
AVVERTENZA:
Questo strumento stato testato secondo le Direttive EMC allo scopo di poter utilizzare il Marchio CE della Comunit Europea. Questo strumento pu essere suscettibile a radiazioni/interferenze o frequenze che non sono entro i limiti collaudati.
Questo strumento progettato per lanalisi cromatografica di campioni opportunamente ATTENZIONE preparati. Deve essere utilizzato usando gas e solventi adatti a questo scopo ed entro i limiti massimi di pressione, flusso e temperatura riportati in questo manuale. Se lo strumento non viene utilizzato secondo le modalit specificate dal costruttore, le condizioni di sicurezza previste potranno non essere sufficienti. E responsabilit del Cliente informare il Servizio Tecnico Varian, prima di qualsiasi ATTENZIONE intervento di riparazione, se lo strumento stato utilizzato per lanalisi 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 lesposizione 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 polarit 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.
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Procedure di Sicurezza in GC
Scarico dei Gas
Per i rivelatori GC non richiesto alcun sistema particolare di scarico dei gas, se lo strumento installato in una stanza ben ventilata e se non viene utilizzato per lanalisi 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 daria in modo che le vibrazioni e il movimento dellaria non disturbino il rivelatore. Eseguire verifiche periodiche per garantire un funzionamento corretto. Garantire una buona ventilazione nel laboratorio. Non smontare mai una linea del solvente od una valvola quando il sistema 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
Loperatore deve conoscere le propriet fisico-chimiche delle componenti della fase mobile. I solventi non vanno messi in contatto diretto con il tubo di erogazione in poliuretano, dal momento che alcuni solventi possono causare indebolimento e perdite con possibili scoppi. Tutte le componenti del sistema vanno collegate ad una fonte di alimentazione e ad una messa a terra comuni. E meglio che per questultima 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 lelettricit statica. Vanno utilizzati dispositivi di misurazione e scarico (ad esempio ionizzatori daria) per evitare laumento di elettricit statica.
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.
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.
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 sotto pressione, la pompa pu 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.
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Servizi Tecnico
La Varian, alla scadenza del periodo di garanzia, in grado di fornire ai suoi clienti unampia 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.
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Instrucciones de Seguridad
Instrucciones de Operacin
Este Manual de Instrucciones est diseado para ayudarle a establecer las condiciones de operacin que le permitan operar su instrumento de forma segura y eficaz. As mismo, se describen consideraciones especiales precauciones, que aparecen en forma de NOTA, PRECAUCION, y ATENCION como se indica ms abajo.Es importante que utilice el instrumento de acuerdo con este Manual de Operacin y cualquier otra informacin que le proporcione Varian. Remita a la Oficina Local de Varian cualquier cuestin que tenga respecto al correcto uso de su equipo.
NOTA
Informacin para ayudarle a obtener unas prestaciones ptimas de su instrumento.
PRECAUCION!
ATENCIN
Le alerta de situacines que pueden causar daos moderados a la salud al equipo, y cm evitar esas situaciones. Descripcin
Le alerta de potenciales situaciones peligrosas que pueden causar serios daos, y cmo evitar esas situaciones.
Smbolo
ATENCIN
PELIGRO DE DESCARGA ELCTRICA
El instrumento utiliza voltages peligrosos. Desconecte el interruptor general antes de retirar los paneles atornillados. Peligro de productos qumicos. Evite el contacto, especialmente cuando rellene los depsitos. utilice proteccin de ojos y piel.
ATENCIN
PELIGRO DE QUEMADURAS
Superficies posiblemente calientes fras (criognico). Utilice proteccin para la piel. Las partculas voltiles, productos qumicos o radiacin UV pueden causar daos en los ojos. Usar las debidas protecciones para la cara y los ojos.
ATENCIN
PELIGRO DE FUEGO
Peligro potencial de fuego. Siga las instrucciones del Manual de Operacin para su seguro funcionamiento. Peligro potencial de explosin debido al tipo de gas lquido empleado. Peligro por Fuente de radiacin. Siga las instrucciones del Manual de Operacin para su seguro funcionamiento. Mantenga alejados los dedos y las manos.
ATENCIN
PELIGRO DE EXPLOSIN
ATENCIN
PELIGRO DE RADIACIN
ATENCIN
PARTES EN MOVIMIENTO
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NOTA:
Este instrumento ha sido testado bajo las normas de la Directiva EMC segn requerimientos de la Marca CE de la Unin Europea. Por lo tanto, este equipo puede ser sensible a niveles de radiaciones / interferencias frecuencias que no estn incluidas dentro de los lmites testados. Este instrumento est diseado para anlisis cromatogrfico de muestras preparadas apropiadamente. Debe ser operado usando gases y/ disolventes apropiados y con unos niveles mximos de presin, flujos y temperaturas, segn se describe en este manual. El Usuario tiene la obligacin de informar al Servicio Tcnico de Varian cuando el instrumento vaya a ser empleado para anlisis de muestras peligrosas de origen biolgico, radioactivo txico, antes de comenzar a realizar cualquier anlisis.
ATENCIN
ATENCIN
Peligros Elctricos
Desconecte el instrumento de todos las conexiones elctricas a la red antes de retirar los paneles para evitar la posible exposicin a peligrosos voltages. Cuando sea necesario emplear una clavija elctrica no original, asegurese de colocar los cables de acuerdo con el cdigo de colores y polaridades descritos en el manual y los cdigos de seguridad de la red elctrica. Sustituya los fusibles fundidos con fusibles del tipo y tamao estipulados en el panel de fusibles en el manual. Sustituya los cables deteriorados inmediatamente con cables del mismo tipo y graduacin. Asegureses de que los valores de las lneas de electricidad se ajustan a los valores para los que el Instrumento ha sido preparado.
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GC Prcticas de Seguridad
Sistema de Extraccin
No se necesita un sistema de extraccin para los detectores GC instalados en un laboratorio bien ventilado, excepto cuando se analicen muestras qumicas peligrosas. Si instala un sistema de extraccin: Utilice conductos a prueba de fuego. Instale un ventilador al final del sistema. Instale entradas de aire cuya vibracin no afecte al trabajo del detector. Compruebe peridicamente el correcto funcionamiento del sistema. Asegurese de una correcta ventilacin del laboratorio.
Nunca abra una lnea una vlvula bajo presin. Apague la bomba antes y deje que la presin baje a cero. Utilice depsitos irrompibles que sean capaces de operar a 50-60 psi. Mantenga cerrada la junta del depsito cuando se haye bajo presin. Lea y cumpla todas las NOTA, PRECAUCION, y ATENCION del manual.
Cromatografa Flash
El operador debe familiarizarse con las propiedades fsico-qumicas de los componentes de la fase mvil. 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 explosin. Todos los componentes del sistema deben estar conectados a un enchufe comn con toma de tierra comn. Esta toma de tierra debe ser una toma de tierra verdadera en lugar de flotante. Los disolventes no-polares pueden originar carga esttica cuando son bombeados por el sistema. Todos los recipientes que contienen fase mvil (incluyendo los tubos y los recipientes de recogida) deben estar conectados a tierra para disipar la electricidad esttica. Utilizar medidores de carga esttica y los debidos dispositivos de descarga (por Ej., ionizadores de aire) para salvaguardarse contra la creacin de electricidad esttica.
Peligro de Quemaduras
Las zonas de calor fro (criognicas) del Cromatgrafo de Gases pueden permanecer calientes fras durante bastante tiempo despus de apagar el instrumento. Para evitar quemaduras asegureses de que todas las reas que se calienten enfren han vuelto a la temperatura ambiente, protejase adecuadamente las manos, antes de tocar las superficies potencialmente calientes fras.
Radiacin Ultravioleta
Los detectores del Cromatgrafo de Lquidos que utilizan una fuente de luz ultravioleta disponen de proteccin para prevenir exposiciones radioactivas al personal. Para una correcta proteccin: Asegurese de que las cubiertas de proteccin de la lmpara de los detectores est correctamente situada durante su funcionamiento. No mire directamente a las celdas del detector a la fuente de luz UV. Cuando inspeccione la fuente de luz la celda, utilice siempre una proteccin para los ojos como gafas de borosilicato poliestireno.
LC Prcticas de Seguridad
Peligro de Alta Presin
Si se rompe una lnea de presin, se abre una vlvula de seguridad accidentalmente bajo presin, la bomba puede generar lquidos a alta presin potencialmente peligrosos, produciendo un chorro a alta velocidad de lquidos voltiles y/ txicos. Lleve proteccin facial cuando inyecte muestras realice mantenimiento de rutina.
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Disponibilidad de Recambios
Es Poltica de Varian disponer de Recambios para cualquier instrumento y la mayora de los accesorios por un periodo de cinco (5) aos despus del ltimo instrumento fabricado. Los recambios durante esos cinco aos estarn disponibles, pero siempre bajo el sistema Segn disponibilidad. Los Recambios estn definidos como todas aquellas partes individuales mecnicas elctricas que son susceptibles de fallo durante su normal proceso de operacin. Por ejemplo, rels, lmparas, sondas de temperatura, elementos del detector, motores, etc. Las planchas de metal, partes de la estructura, placas de circuitos integrados, y otros mdulos funcionales son normalmente susceptibles de reparacin y por lo tanto slo estarn disponibles bajos el sistema Segn disponibilidad despus del ltimo 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 garanta. El Soporte de Servicio se ofrece a travs de atractivos Contratos de Servicio bajo un sistema de facturacin de mano de obra y materiales. El mantenimiento y el entrenamiento se realiza por ingenieros cualificados bajo Contrato peticin.
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Contents
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Contents
Use Polypropylene Caps to Preserve Liquids in Reservoirs............................................................................. 43 Setting Flows of Vapor from Liquid CI Reagents .............................................................................................. 44 Returning to Gaseous CI Reagent Operation ................................................................................................... 44 Installing and Using the Multiple CI Module............................................................................................................. 45 Pre-Installation Checklist ................................................................................................................................... 46 Installing the Multiple CI Assembly.................................................................................................................... 46 Cable Connections to the GC External Events Board....................................................................................... 51 Adding Liquid CI Reagents to the MCI Module ................................................................................................. 52 Adding Gaseous Reagents to the MCI Module ................................................................................................. 52 Adjusting Flows of CI Reagents ........................................................................................................................ 53 Setting CI/MS Parameters in the MS Method Editor......................................................................................... 57 Adjusting Reagent Flow for Each CI Reagent................................................................................................... 58 Building GC/MS Methods to Use Different CI Reagents................................................................................... 60 Preparing a Standard GC/EI/MS Method .......................................................................................................... 60 Methods for Single CI Reagents ....................................................................................................................... 62 GC/MS SampleList for Alternating EI/MS and CI/MS Acquisitions ................................................................... 63 Multiple CI Reagents in Consecutive Runs ....................................................................................................... 66 Multiple CI Reagents in the Same Run ............................................................................................................. 67 MCI Module Maintenance ........................................................................................................................................ 69 Handling and Storage of CI Liquids in Reservoir Bulbs .................................................................................... 70 Cleaning Reservoir Bulbs .................................................................................................................................. 70 Changing a Channel from Liquid to Gas Operation .......................................................................................... 70 Changing a Channel from Gas to Liquid Operation .......................................................................................... 72 Leak Checking................................................................................................................................................... 73 Cross-Contamination Effects............................................................................................................................. 73 Hints for Successful Operation of the MCI Module ........................................................................................... 74
Contents
Remove the Analyzer Assembly ............................................................................................................................ 102 Replace the Electron Multiplier .............................................................................................................................. 104 Replace the Filament(s)......................................................................................................................................... 105 Remove the Ion Trap Oven.................................................................................................................................... 106 Cleaning the Trap Components ............................................................................................................................. 106 Disassemble the Trap Components ................................................................................................................ 106 Clean the Trap Components ........................................................................................................................... 107 Clean SilChrom Ion Trap Electrodes............................................................................................................... 109 Clean the Two Quartz or Silica Coated Spacers............................................................................................. 109 Reassemble the Trap ...................................................................................................................................... 109 Re-install the Trap Oven ........................................................................................................................................ 110 Reposition the Electron Multiplier .......................................................................................................................... 111 Re-install the Analyzer Assembly .......................................................................................................................... 111 Install the Transfer Line ......................................................................................................................................... 111 Close the Vent........................................................................................................................................................ 112 Turn on the Mass Spectrometer ............................................................................................................................ 112 Bake Out the Trap.................................................................................................................................................. 112 Check Ion Trap Operation...................................................................................................................................... 113 Fill the Calibration Compound Vial......................................................................................................................... 113
GC Maintenance................................................................................................................... 115
Overview ................................................................................................................................................................ 115 General GC Maintenance ...................................................................................................................................... 116 Check and Renew Gas Supplies..................................................................................................................... 116 Leak Check...................................................................................................................................................... 116 Gas Purifier Replacement ............................................................................................................................... 117 Injector Maintenance ....................................................................................................................................... 119 1079 Injector .......................................................................................................................................................... 120 Remove the Glass Insert ................................................................................................................................. 121 Replace the Glass Insert ................................................................................................................................. 122 Clean the Glass Insert ..................................................................................................................................... 123 Deactivate the Glass Insert ............................................................................................................................. 124 How to Remove the Capillary Column from the System ....................................................................................... 125 How to Install a New Capillary Column in the System........................................................................................... 127
Troubleshooting................................................................................................................... 129
How to Isolate a GC or Mass Spectrometer Problem............................................................................................ 129 Checking the Data System .................................................................................................................................... 129 Checking the GC.................................................................................................................................................... 129 Checking the Mass Spectrometer.......................................................................................................................... 129 How to Troubleshoot Problems with Spectra......................................................................................................... 130 What To Do If No Spectrum Appears.............................................................................................................. 130 Check for an Open Filament ........................................................................................................................... 131 Check the Turbomolecular Pump.................................................................................................................... 131 Check the RF Adjustment ............................................................................................................................... 131 Check the Parameter Settings ........................................................................................................................ 131 Check the Assembly of the Trap ..................................................................................................................... 132 Check the Electronics...................................................................................................................................... 132 What To Do If You Experience a Loss of High Mass Peaks ................................................................................. 133 What To Do If Part of the Spectrum is Missing...................................................................................................... 133 Check the RF Adjustment ............................................................................................................................... 133 Check the RF Storage Level ........................................................................................................................... 134 Check the Trap Temperature .......................................................................................................................... 134 What To Do If the Resolution is Poor But the Air and Water Levels are Acceptable ............................................ 134
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Check the Ion Content of the Trap .................................................................................................................. 134 Check the Axial Modulation Setting................................................................................................................. 135 What To Do If There is a High Baseline at High Masses ...................................................................................... 135 What To Do If the Trap Function Calibration Fails After the Calibration Ions Have Been Correctly Identified...... 136 Check the Electron Multiplier Voltage ............................................................................................................. 136 Check the Cal Gas Pressure........................................................................................................................... 136 How to Check for Leaks......................................................................................................................................... 136 How to Establish the Conditions Required to Check for Leaks....................................................................... 136 How to Fix High Water Levels................................................................................................................................ 141 Using a Leak Detection Gas to Troubleshoot for Air Leaks................................................................................... 141 How to Fix a Large Air Leak................................................................................................................................... 142 How To Fix a Small-To-Moderate Air Leak............................................................................................................ 143 Check GC Connections: .................................................................................................................................. 143 How to Troubleshoot the GC ................................................................................................................................. 144 How to Run the COLTEST Sample ....................................................................................................................... 144 Set Up the Injector Conditions......................................................................................................................... 144 Set Up the Column .......................................................................................................................................... 144 Set Up the Transfer-Line and Trap-Temperature Conditions.......................................................................... 145 Set Up the Mass Spectrometer Acquisition Method........................................................................................ 145 How to Troubleshoot Common Chromatographic Problems........................................................................... 146 Correction of Solvent Tailing or Broadening Problems ................................................................................... 147 Correction of Tailing Sample Peaks for Particularly Active Components ....................................................... 147 Correction of Low Response and Severe Tailing with High Boiling Point Compounds .................................. 147 Correction of Leading Sample Peaks (Reverse Tailing) ................................................................................. 148 1 Correction of Poor Resolution ........................................................................................................................ 148 Lack of Reproducibility of Peak Size ............................................................................................................... 148 Correction of Peak Splitting (Particularly for Low Boilers)............................................................................... 149 Correction of Extra, Unexpected Peaks in the Chromatogram ....................................................................... 149 Correction of Retention Time Differences Between Runs............................................................................... 149
Contents
Parts and Supplies ................................................................................................................................................. 161 Kits, Assemblies, Boards, and Cables ............................................................................................................ 161 Trap Components............................................................................................................................................ 162 Pump Spares, Pumps, Pump Conversion Parts ............................................................................................. 162 Diffusion Pump Spares.................................................................................................................................... 163 GC Spares ....................................................................................................................................................... 164 Tools, Test Samples, etc. ................................................................................................................................ 164 Additional Saturn Spares................................................................................................................................. 165 CI Parts/Spares ............................................................................................................................................... 165 Multiple CI Module Parts Lists......................................................................................................................... 165 MCI Module Accessory Kit .............................................................................................................................. 166 Open Split Interface......................................................................................................................................... 166 Calling Varian Service............................................................................................................................................ 167
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Contents
Functional Description
Introduction
The Saturn 2000 GC/MS has four principal components: Gas chromatograph (GC) Mass spectrometer (MS) Data system (DS) AutoSampler (optional)
The following figure is a functional block diagram of the Saturn GC/MS. A short, line-of-sight transfer line connects the GC and mass spectrometer. The AutoSampler sits on top of the GC. A fused silica capillary column in the GC passes through the transfer line directly into the ion trap assembly (see Principal Components of the Saturn GC/MS on page 2). Samples are injected either manually or via the AutoSampler onto the capillary column through the GC injection port. The gas chromatograph then separates the sample molecules. Effluent from the GC passes through the transfer line and into the ion trap. The sample molecules next undergo electron or chemical ionization before being analyzed according to their mass-to-charge ratios. The ions are detected by an electron multiplier, which produces a signal proportional to the number of ions detected. The electron multiplier passes the ion current signal to the system electronics, which in turn amplify the signal, digitize the result, and pass it on to the data system for further processing and display. Refer to the following Functional Block Diagram.
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Functional Description
A Foreline Pump B Transfer Line C GC Oven D Capillary Column E Turbomolecular Pump F Ion Trap Assembly
Principal Components of Saturn GC/MS (Top View)
Functional Description
Technical Specifications
NOTE: Specifications are identical for turbomolecular pump and diffusion pump GC/MS systems unless specified.
Physical Specifications
Saturn GC/MS: Height 21 inches (51 cm) Depth 24 inches (61 cm) Width 38 inches (81 cm) Weight 170 pounds (73 Kg) Installation Requirements: Supplied by Customer Power: Two dedicated Fourplexes, each rated at 115 Vac 15%, 60 Hz, 20A or 230 Vac 15%, 50 Hz, 10-16 A. GASES: Carrier Gas: Ultra high purity helium; purity 99.998% with less than one ppm each of water, oxygen, and total hydrocarbons. CI Reagent Gases: Methane, isobutane, ammonia - purity 99.99%. Environment: Combined GC/MS/DS will average 15,000 Btu/h-1 output when considering air conditioning needs. Combined GC/MS/DS requires 6-12 inches distance from walls. Indoor Use Altitude up to 2500 m Temperatures: Turbomolecular Pump: 59-80 F (15-27 C) Diffusion Pump: 59-95 F (15-35 C). Relative Humidity: 40-80% with no condensation. Installation Category II Pollution Degree: 2
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Functional Description
Mechanical Assemblies
The Saturn mechanical assemblies include the following: Controls and indicators Cooling fans Vacuum system Transfer line Ion trap assembly
In the event of an emergency, shut off of all power to the Saturn GC/MS by placing the main power switch in the OFF position and unplugging the instrument.
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Functional Description
A B C D E F G H I
Main Power Switch (rear panel) Service Switch Transfer Line Heater Trap Heater Manifold Heater LED Pneumatics Manifold CI Cal Gas Adjust Cal Gas Adjust
J K L M N O P Q
Cal Gas Vial Vent Valve RF Coil RF Coil Adjustment Screw Transfer Line Turbomolecular Pump Cooling Fans CI Shutoff Valve
Cooling Fans
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Functional Description
The electronics section fan draws air from the back, and blows it across the SAP/WAVE and power boards in the electronics compartment. Hot air from the GC oven does not affect the MS as long as the system is at least six inches from a wall. The power board supplies power to the electronics compartment fan.
Cooling Zones
Zone 1 is the upper part of the analyzer compartment. Its purpose is to provide forced air-cooling for the Peltier baffles heat sink. It also provides cooling for the manifold electronics. The upper fan on the rear panel pulls air in through the front of the instrument. The air is drawn over the manifold electronics, ducted over the Peltier baffles heat sink, and expelled through the rear of the instrument. The diffusion pump controller monitors operation of this fan. Fan failure will trigger a system shutdown.
CAUTION
The Peltier Baffle ducting must be left in position at all times, or the Peltier baffle will overheat allowing back streaming pump vapor to contaminate the analyzer.
Zone 2 is the electronics compartment, diffusion pump controller, and RF generator board. Its purpose is to cool the majority of the instruments printed circuit boards. The mid level fan on the rear panel pulls air in from two directions. The primary cooling air supply is pulled in through the front of the instrument, over the power board and SAP/Wave board, and expelled through the rear of the instrument. A secondary air supply is pulled in through the left side panel, ducted over the RF generator board, the diffusion pump controller, and then merges with the primary airflow.
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Functional Description
Zone 3 is the diffusion pump compartment. The lower fan on the rear panel pulls air in through carefully positioned vents in the left side panel. Airflow is ducted around the diffusion pumps cooling fins, and expelled through the rear of the instrument.
CAUTION
The left side cover must remain in place whenever the instrument is on. Failure to do so will cause the airflow to bypass the pump, which will overheat and trigger a system shutdown. Fan failure will have the same result. GC side cover must also be in place.
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Functional Description
The vacuum manifold sits atop the RF coil housing. The turbomolecular pump makes an airtight seal with the manifold, to which it is mounted horizontally with a Viton O-ring. The ion trap assembly suspends from the analyzer flange, and extends into the body of the manifold. The manifold makes an airtight seal with the analyzer flange, also via a Viton O-ring. Quick release tabs permit easy removal of the trap in the absence of vacuum. Eight electrical feedthroughs pass through the analyzer flange, i.e., One for the electron gate Three for the filament assembly Two for the axial modulation voltages applied to the filament and multiplier endcap electrodes of the ion trap assembly One for the high voltage to the electron multiplier cathode One for the ion current signal from the electron multiplier anode
Another feedthrough passes through the underside of the manifold to provide radio frequency (RF) voltage to the ring electrode. An ion gauge monitors the pressure inside the manifold by generating and collecting ions from any gas present. The ion gauge also passes through the analyzer flange. Four additional inlets introduce material into the vacuum manifold. These inlets include One for the transfer line One for the CI reagent gas One for introduction of the calibration gas One for venting
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Functional Description
If the speed of the pump is 92% or more of the maximum operating speed, the signal from the controller prompts the power control board to send a TURBOMOLECULAR SPEED OK signal to the SAP/Wave board. The SAP/Wave board uses the signal for enable or disable the filament, electron multiplier voltage, RF generator, CI reagent gas valve, and calibration gas valve by means of an electronic interlock. If the pump speed falls below 92% of its maximum operating speed, the TURBOMOLECULAR SPEED OK signal to the SAP/Wave board turns off. The filament, electron multiplier, RF generator, CI reagent gas valve, and calibration gas valve turns off automatically. This condition probably indicates a major air leak in the system or that the pump is too warm. If this is the case, you will have to locate and fix the leak to make your system fully operational.
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Functional Description
A Manifold B Peltier Baffle C Diffusion Pump D Inlet Seal E Inlet Clamp F Analyzer Assembly G Pneumatics Manifold H RF Coil
Cross Section of the Diffusion Pump Vacuum System
Peltier Baffle
The Peltier baffle is a cooled line of sight baffle that reduces back streaming of vacuum pump vapors into the vacuum manifold. The design consists of a onepiece baffle that is cooled by a thermoelectric cooling element (TEC). The TEC is essentially an electronic heat pump based on the Peltier effect. A voltage is applied to the TEC, causing heat to be pumped from the cold side of the TEC to the hot side. The cold side of the TEC draws heat from the baffle, thereby cooling it, and the hot side of the TEC pushes heat into the heat sink. The heat sink is cooled by forced air convection. The TEC is activated when the system is started, and remains on until it is switched off during the shutdown procedure.
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Functional Description
Diffusion Pump
The ion trap assembly requires a vacuum of approximately 1 x 10 Torr (1.3 x -3 10 Pa) for the generation and detection of ions. The Varian AX65 air-cooled diffusion pump with a pumping speed of 30 l/s for air and 65 l/s for helium provides this. The pump features two safety devices. The first is an over temperature switch that prevents catastrophic pump failure and subsequent ion trap contamination from over heating problems, such as a cooling fan failure or a blocked air inlet. The second feature is a sight glass that allows inspection of the diffusion pump fluid level and condition without breaking vacuum. This reduces periodic maintenance time, and helps prevent the pump being run without fluid.
-5
The diffusion pump controller is activated when the systems main power switch is in the ON position. It will remain activated until the system is switched OFF. Upon activation, the controller will provide power to the TEC, Peltier baffle fan, and diffusion pump fan. It will also check the foreline pressure reading from the thermocouple gauge. If the foreline pressure has reached the diffusion pumps required operational pressure after fifteen minutes, the controller will provide power to the diffusion pump. After another fifteen minutes (thirty minutes total) the diffusion pump will reach operational temperature, and the controller will issue a DIFFUSION PUMP NORMAL signal to the SAP/Wave board, which in turn provides power to the ion trap. During normal running conditions the diffusion pump controller will continue to monitor the TEC, Peltier baffle fan, diffusion pump, and thermocouple gauge. The controller will initiate a system shutdown and send a fault signal to the SAP/Wave board if a power failure is detected on any of these components, or a pump over temperature is detected. The SAP/Wave board will shut off power to the ion trap. The controller will also discontinue power to the diffusion pump, and send a fault signal to the SAP/Wave board if a foreline overpressure is detected. Power to the diffusion pump will be restored, and the fault signal canceled when the overpressure problem no longer exists. The diffusion pump controller also ensures a safe shutdown when the instrument must be switched off for maintenance, repair, or relocation. The controller receives a shut down command from the SAP/Wave board, and immediately discontinues power to the diffusion pump. The controller will wait fifteen minutes before discontinuing power to the TEC. After another fifteen minutes (thirty minutes total) the controller issues a DIFFUSION PUMP OFF signal to the SAP/Wave board, and the shut down procedure may be completed.
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Functional Description
The diffusion pump may be restarted at any time during the shutdown procedure providing no fault condition exists. The controller will restore power to the diffusion pump if it receives a restart command during the first fifteen minutes of the shut down procedure. The diffusion pump will reach operational temperature, and the controller will issue a DIFFUSION PUMP NORMAL signal to the SAP/Wave board after fifteen minutes. A full thirty-minute start up will be initiated if the controller receives a restart command during the second fifteen minutes of the shut down procedure.
Thermocouple Gauge
A thermocouple gauge is a simple, rugged, vacuum gauge that is used to -3 -1 measure vacuum pressures in the 2 Torr (267 Pa) to 1 x 10 Torr (1.3 x 10 Pa) range. The gauges main purpose is to enable the diffusion pump controller to detect gross leaks and foreline pump failure. The thermocouple gauge is active whenever the diffusion pump controller is active. It is monitored during start up to ensure the vacuum system has been pumped down to the diffusion pumps required operational pressure. Once the diffusion pump is operational, the thermocouple gauge is monitored to ensure the operational pressure is maintained.
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Functional Description
Transfer Line
A Spring B Boot C Tie Wrap D Washer E Transfer Line Tip F O-Ring G Heat Exchanger H Nose I E-Ring J Ferrule K Nut A bayonet mount feature secures the transfer line. Before you remove the trap, push gently on the bayonet mount as you twist it counterclockwise and pull the mount out. Make sure the transfer line extends out from the trap. NOTE: Failing to remove the transfer line before removing the trap may damage the trap heater post. The power board supplies power to the cartridge heater via a transfer line heater cable. The heater cable projects out from one end of the transfer line. It then plugs into a soft-shell connector on the top of the power board panel. You set the transfer line temperature from the Instrument Control Page. The maximum temperature that the transfer line can sustain is 350 C; the minimum temperature depends on the GC oven and trap temperatures. In general, you can set the transfer line temperature as much as 30 C below the maximum column operating temperature and not observe adverse chromatographic effects (e.g., retention time shifts or peak broadening).
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Functional Description
A B C D E F G
Heating Cable Boot Nut Ferrule Transfer Line/Alignment Tool Nose Nose Hole
H I J K L M N
O-ring Transfer Line Tip Heating Cable Slot Nose Clip Bayonet Mount Analyzer Assembly Tongue Analyzer Assembly Lock-Down Tabs
The figure below shows the ion trap assembly along with its three electrodes, electron gate, and filament lens. NOTE: The Silica Coated Spacers have a shiny, mirror like finish on the inside surface.
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Functional Description
A B C D E F G
Screw, 6/32, 4 places Clamping Plate Exit End Cap Quartz or Silica Coated Spacer, 2 places RF Ring Electrode Filament End Cap Electron Gate Ion Trap Assembly
H I J K L M
Wave Washer Gate Conductor Trap Oven, T is located this side. Filament Assembly Filament Clip Screw
Trap Oven
The trap oven is a heated anodized aluminum block that maintains a uniform temperature for the trap electrodes. A heater post on the manifold flange generates the heat. A thermal well measures the oven temperature. In addition, the oven holds the ionization filaments, and acts as a lens for focusing the ionizing electrons before they enter the trap.
Filament Assembly
The filament assembly sits in the trap oven. It is connected to three feedthroughs on the manifold flange. The filament assembly consists of two filaments and a repeller plate. The two filaments are mounted side-by-side, with each filament approximately equidistant from the entrance hole of the ovens electron focusing lens. Note that the Saturn GC/MS only uses one filament at any given time; the extra filament is provided as a back up in case the first one burns out.
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Functional Description
Each filament is a rhenium wire. When sufficiently heated by electric current, the filament produces electrons by thermionic emission. The filament emission current refers to the flow of emitted electrons from the filament. The magnitude of the filament emission current is set in the Instrument Control Page. Emission current settings range from 5 to 100 A. NOTE: It is unlikely that two filaments will have the same net flow of electrons into the ion trap. Thus, the signal amplitudes from two different filaments will probably not be the same. A typical difference is 2:1, but it may be as high as 5:1.
Electron Gate
The electron gate is a cylindrical electrode that controls the entry of electrons into the ion trap cavity. When electrons emitted from the heated filament are not needed for ionization, the electron gate is held at a -150 Vdc potential. The electron gate sits inside the trap oven, in front of the lens and behind the endcap electrode. An anodization layer insulates it from the filament endcap. When the ion trap requires electrons, the electron gate potential changes from 150 to +150 Vdc. The gate potential remains positive for a variable length of time, e.g., from 10 sec to 65 ms. During this interval, the electrons are focused into the ion trap cavity with sufficient energy, usually, 50 to 80 eV, to achieve electron ionization of the sample molecules (or of the reagent gas molecules in the case of chemical ionization).
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Functional Description
The filament endcap, exit endcap, and RF-ring electrodes have hyperbolic inner surfaces. Together, these electrodes form a cavity in which ionization, fragmentation, storage, and mass analysis take place. Energetic electrons enter the ion trap cavity through the filament endcap via the electron gate. There are seven holes in the center of the exit endcap electrode. Sample ions produced in the ion trap are ejected through these holes into the electron multiplier. Two identical quartz or silica-coated spacers separate the central ring electrode from the filament and exit endcap. The trap oven and its clamping plate hold the electrodes and spacers in place. A cutout is provided in the quartz spacers and in the exit endcap to allow the transfer line to enter the ion trap. The RF generator assembly provides high voltage RF that is applied to the RF ring electrode. Under the proper RF voltage, the ion trap electrodes create a three-dimensional, hyperbolic electric field. This field is capable of trapping the ions in stable, aperiodic orbits. As the RF voltage increases, however, the ion trajectories become unstable in increasing order of mass per charge. The ion trap ejects the ions and sends them to an electron multiplier for detection. During mass analysis, a supplementary RF voltage of 485 kHz is applied to the filament and exit endcaps. This voltage, termed the axial modulation voltage, improves spectral mass resolution and analytical sensitivity. Other voltages may be applied between the endcaps to implement such options as SECI and MS/MS. For further details, see the Saturn Method Editor for description of scan functions.
Electron Multiplier
The electron multiplier is positioned at the exit endcap electrode. It mounts in a pre-aligned position on a protective metal clip that you can easily remove to replace the multiplier. The multiplier detects positive ions as the ion trap ejects them through the holes in the exit endcap electrode. The continuous-dynode electron multiplier consists of a lead-oxide/glass, funnel-like resistor. A negative voltage of between -800 and -3000V is applied to the front end of the electron multiplier, referred to as the cathode. The back end of the cathode is held at ground potential, and is referred to as the anode.
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Functional Description
A B C D E
Exit End Cap Electron Multiplier Track Multiplier Signal Pin EM Grid Electron Multiplier Mount
F G H I
Multiplier Contacts Multiplier High Voltage Pin Transfer Line Alignment Transfer Line Entrance Hole
The negative voltage applied to the cathode attracts the positive ions ejected from the ion trap cavity. These ions strike the cathode with sufficient velocity to dislodge electrons from the inner curving surface of the cathode. The increasingly positive potential gradient draws the ejected electrons into the electron multiplier, further accelerating them in the process. Because the electron multiplier is curved, the ejected electrons do not travel far before they again strike the inner surface of the multiplier, resulting in the emission of more electrons. This configuration produces a cascade of electrons that are accelerated toward ground potential at the exit end of the cathode. The anode collects the electrons, and passes the resulting ion current signal on to the integrator circuit on the lower manifold board. The ion current signal is proportional to the total number of electrons that the ion trap ejects. Typically, you will adjust the voltage that is applied to the electron multiplier until the gain is 5 about 10 , i.e., until each ion that enters the electron multiplier generates 5 approximately 10 electrons.
Ion Gauge
The optional Saturn GC/MS ion gauge design is based on the Bayard-Alpert gauge tube. The specifications for the gauge are similar to those of commercially available gauges. Fixed pressure readings with nominally identical gauges may exhibit variations of 15%. An accuracy of 25% in mid-range for any one gauge is considered typical.
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Functional Description
In general, the ion gauge exhibits good repeatability. However, the ion gauge response depends on gas composition. A certain pressure of air and water will give a different reading than that of Helium. The Ion Gauge is meant to be a rough indicator of vacuum conditions. It is not a precise quantitative tool. The gauge uses thoria-coated iridium (ThO-Ir) filaments. These filaments are burnout resistant, and therefore exhibit high tolerance to air and water in the vacuum manifold. There is a time delay associated with heating the filament. This delay translates to a delay in determining whether a filament is open. From 15 to 20 seconds are usually required after you turn the filament on to obtain a stable reading. The ion gauge will measure pressures between 10 and 10 Torr. A logarithmic amplifier amplifies the collector current, and the data system interprets this current as measured vacuum.
-6 -2
Foreline Pump
A foreline pump has two purposes. The first is reducing the vacuum system pressure to a level that will allow the operation of high vacuum pumps such as turbomolecular pumps and diffusion pumps. The second is maintaining the vacuum system pressure by removing the high vacuum pumps exhaust gases. The foreline pump is connected to the high vacuum pump by a 2.1m (84 in.) length of 1.9 cm (0.75 in.) ID vacuum tubing. The pump plugs into the rear panel outlet labeled J2 - LINE VOLTAGE - PUMP ONLY on the rear of the MS. Power is supplied through this outlet and is controlled by the power switch on the rear panel. The foreline pump used on the Saturn GC/MS is a two-stage rotary vane pump -3 with a pumping speed of 90 L/min. and a vacuum potential of 1.5 x 10 Torr -1 (2 x 10 Pa).
If you use the Saturn GC/MS to analyze hazardous materials, be sure to affix the foreline pump exhaust to an exhaust system that complies with applicable safety regulations.
Electronic Assemblies
The electronic assemblies consist of the following: Power input subsystem and turbomolecular (or diffusion) pump controller (See Diffusion Pump Controller). Power board Scan acquisition processor/waveform (SAP/Wave) board Manifold electronics assembly RF generator board
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Functional Description
The electronics functions have been distributed throughout the spectrometer to minimize cable lengths between critical components. The SAP/Wave and power boards reside in an electronics enclosure that is separated from the analyzer section by a sheet metal bulkhead. The manifold electronics are enclosed directly above the analyzer. The RF generator attaches to the rear of the RF coil assembly. Below are diagrams of the electronic assemblies used in the Turbomolecular and Diffusion Pump Saturn 2000 GC/MS.
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Functional Description
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Functional Description
electronics service switch allows the vacuum to the maintained in the event that the electronics need to be serviced. The line voltage switches are located on the power board and the turbomolecular controller. These switches are set at the factory. The turbo controller regulates the speed of the turbo pump. The controller provides turbo speed and startup power to the power board.
WARNING:
SHOCK HAZARD
In the event of an emergency, shut off all power to the Saturn GC/MS by placing the main power switch in the OFF position.
Power Board
The power control board supplies power to all electronics components except the turbomolecular controller. It controls the heaters, ion trap and ion gauge filaments and solenoid valves. NOTE: The switching power supply is protected by a 5A, Non-Time-Delay, fuse. The following switching power supplies reside on the board: The +5V dc power supply, which supplies +5V dc voltage to all digital circuits. The -15V and +15V dc power supplies, which supply the voltages to the analog circuits on the power board and the manifold electronics assembly. The +20V and -20V dc power supplies, which supply the voltages to the SAP/Wave and RF generator boards analog circuitry. The +24 Vdc power supply supplies power for the solenoid valves, electronics compartment fan and the electron multiplier power supply. The +55 Vdc power supply, which supplies unregulated +55 Vdc voltage to the RF generator board. The 180-volt power supply that supplies voltage to the ion trap electron gate circuit and the ion gauge.
The following circuits also reside on the board: The trap and ion gauge filament control circuits, which provide current to heat the filament and regulate the emission current from the filament. You set the trap filament emission current between 5 and 100 A via the data system. Three heater control circuits that provide feedback control for the manifold, trap and transfer line heaters. The trap heater uses a proportional integral (PI) control circuit. Because there is an integrator component in this controller, removing power from the circuit will produce a lengthy stabilization time, e.g., up to two hours (dependent on the temperature set point). Three solenoid control circuits, which turn the calibration gas, CI reagent gas, and CI shutoff valve solenoids on and off.
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Functional Description
The electron energy control circuits, which controls the dc bias on both the ion trap and ion gauge filaments. The diagnostic multiplexer circuit, which routes the voltage output of various components, and circuits on the power control board to the SAP/Wave board. You can access these voltage outputs through the diagnostic pages. Mounted on the top edge of the power board are 15 monitor LEDs. When illuminated, these lights indicate that the voltages of the various circuits on the power board are at their proper levels, and that there are no faults. During normal operation all LEDs except the 180 volts should be on. The 180 volts only turns on when the filaments are on.
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Functional Description
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Functional Description
The Scan Acquisition Processor/Waveform Generator Board The scan acquisition processor/waveform generator (SAP/Wave) board is a real-time control and acquisition microcomputer that makes use of an 80C186 microprocessor. The SAP/Wave board communicates with the data system via an IEEE-488 interface board installed in the data system computer bus. The SAP/ Waveboard performs the following functions: Interprets instrument commands from the data system and produces a sequence of analog and digital signals that control operation of circuits on other Saturn GC/MS boards. Collects analog and digital diagnostic data from other subsystems and transmits that information to the data system. Filters, integrates and digitizes the ion current signal and transmits the spectra to the data system. Generates axial modulation waveforms, including waveforms used by SECI, MS/MS and SIS options.
Upon power-up, the 80C186 processor runs a ROM resident program that initializes the board. The program permits the processor to receive information through the IEEE-488 interface. When you start up the Saturn data system, operating information is downloaded to the SAP/Wave boards RAM memory. The SAP/Wave board then performs its operations in response to the commands sent through the IEEE-488 interface. NOTE: The SAP/Wave board is accessed through two connectors on the rear panel of the instrument. J42 is an IEEE connection used for interconnection to the Data System. J43 is a D-shell connector labeled Remote Option and is used for special research applications and the GC start signal. When a mass spectrum is acquired, the data system downloads parameters such as electron multiplier voltage, scan range and time, ionization mode, etc. The SAP/Wave board uses this information to create a scan over the desired mass range. During the scan, ion current data is accumulated and, at the end of the desired scan time, sent to the data system for further processing and display. The waveform generator is capable of generating waveforms over a wide range of frequencies and amplitudes. The data system produces a digital version of the desired time domain waveform, and downloads the resulting binary file RAM. At the appropriate time, the data is clocked out of the RAM into a waveform reconstruction DAC. The DAC output is then filtered to remove undesirable frequencies. The Saturn GC/MS uses the waveform generator in chemicalionization (SECI), MS/MS, or SIS applications; as well as in normal axial modulation. Characteristics of the waveform generator include the following: Dual-port RAM (256 Kbytes) to provide memory for single or multiple digitized waveforms A selectable frequency generation clock (625 KHz, 1.25 MHz, or 2.5 MHz and a 15-bit variable length counter to control timing A 12-bit DAC, low pass filter and amplifier to reconstruct waveforms
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Functional Description
A variable operational frequency range that depends on whether you are using the high frequency transformer (12 to 500 KHz) or low frequency transformer (200 Hz to 1.25 KHz) Application of the waveform output to the endcap electrodes of the ion trap is done via the two transformers located in the manifold electronics assembly.
NOTE: Before you can use any of the waveform options, i.e., SECI, MS/MS, or SIS, the waveform key(s) must be inserted into sockets U5, U6 and/or U7. The key(s) should be installed by the factory, or by a Varian Customer Support Representative.
Computer/Instrument Interface
The computer/instrument interface for the Saturn GC/MS is an IOtech IEEE-488 Interface Board. This board is installed in the computer. The IEEE-488 is a standard computer/instrument communications link for all types of computers. For a complete description of the IEEE-488 Interface Board and its functions, please refer to the documentation provided by the manufacturer.
The Computer
Please refer to your owner's guide for any information about your computer. Also see the Release Notes, which lists compatible computer hardware and software.
The AutoSampler
The optional AutoSamplers available are the Varian 8200, 8400 and 8410 AutoSamplers. For complete installation and operating instructions, please refer to your AutoSampler Operator's Manual.
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Functional Description
Introduction
Chemical ionization (CI) provides mass spectral data that complement electron ionization (EI) data for the analysis of complex compounds. In the standard CI mode of operation, a CI reagent gas is introduced into the ion trap analyzer from an external gas supply cylinder. The reagent gas is ionized by EI to form reagent ions. These reagent ions then ionize sample molecules entering the ion trap with He carrier gas from the capillary column. The operation and adjustment of reagent gases for the standard CI option are described in the first part of this section. NOTE: The CI mode is an option on the Saturn GC/MS. If your system does not have this option, you will not be able to perform CI analyses. Two additional options allow the selection of certain liquids as sources for CI reagent. These are the Liquid CI Inlet (or LCI Inlet) and the Multiple CI Module (or MCI Module). The installation and operation of these options is described later in this section.
Tune the instrument in EI mode Check the Saturn GC/MS system for leaks 33
Isobutane
Ammonia
NOTE: Gases other than methane, isobutane, or ammonia can be used successfully as CI reagent gases with the Saturn GC/MS. For assistance in selecting and using other reagent gases, please contact your Varian Customer Support Representative. The CI reagent gas should contain less than 1 ppm of water. Water in the CI reagent gas may interfere with CI operation. Copper or stainless steel gas lines should be used for methane or isobutane. Stainless steel lines should be used for ammonia. All gas lines should be free of oil (and other contaminants) and preferably flame dried. If possible, use the precleaned copper tubing from the GC Start-Up Kit.
DO NOT flame dry the reagent gas lines with CI reagent gas present.
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CI reagent gases may be hazardous. Use proper protection when installing the reagent gas.
1. Enter the System Control and select the Manual Control tab dialog.
2. Make sure that the electron multiplier, filament, and RF voltage are all off. The Multiplier, Filament, and RF text should be red or black - not green. NOTE: Two solenoid-operated valves control the flow of CI reagent gas into the manifold. The valves are opened and closed by clicking on the CI button on the Instrument Control display. A needle valve controls the amount of reagent gas flowing into the manifold. The needle valve is mounted directly behind the door of the mass spectrometer. The needle valve is adjusted manually by using the knob labeled CI GAS. Turning the knob clockwise increases the flow of reagent gas into the manifold. See Functional Block Diagrams in the Turbomolecular Vacuum Pump or Diffusion Pump Vacuum System. 3. Verify that the CI gas solenoid valves are closed. When these valves are closed, the CI Gas icon to the left of the ion trap symbol is not green. (If the CI icon is green, click on the icon so that it turns to red or black.) 4. Install a two-stage pressure regulator on the reagent gas cylinder or lecture bottle. Tighten the connection securely. NOTE: A two-stage pressure regulator typically consists of the following components: Secondary valve, Pressure adjustment valve, Supply pressure gauge, and Delivery pressure gauge 5. Reagent gas is turned on and off with the Main valve on the cylinder or lecture bottle. The secondary valve on the pressure regulator is next in line. This valve is used for coarse control of the flow of gas from the gas cylinder up to the pressure adjustment valve. The supply pressure gauge is used to monitor the gas pressure in the bottle. The pressure adjustment valve is used to set the head pressure of the gas delivered to the mass spectrometer. 6. Connect one end of the 1/8" OD gas supply line to the pressure regulator.
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7. On the back of the Saturn GC/MS instrument, loosen the two screws that hold the plug in the CI Shutoff Manifold 2 to 3 turns. Remove the plug by pulling straight out and twisting.
A Power Switch B Shutoff Manifold C Plug D 6/32" Screws (2 each) E Vacuum Hose F Fans Connecting CI Gas Supply
8. Use 1/8" OD tubing for the supply line between the gas cylinder and the CI shutoff manifold. No ferrule is required on the mass spectrometer end of this tube. The seal is made with an elastomer O-ring. Inspect the end of the tubing and assure that the surface finish is smooth. If there are scratches, either cut off the damaged part or use 200-600 grit abrasive paper to refinish the sealing end of the tube. 9. Carefully insert the tube into the CI shutoff manifold hole (the one the plug came out of) until it is firmly seated. Be careful not to scratch the tube. Tighten the two screws. 10. Ensure that the secondary valve on the regulator on the gas cylinder is closed. 11. Open the main control valve on the lecture bottle. Next, open the secondary valve and adjust the pressure adjustment valve to approximately 5 psi so that reagent gas flows at a moderate rate through the gas line. 12. Open the mass spectrometer door. Verify that the CI GAS needle valve is turned fully counterclockwise. 13. Next, flush the gas line of air and water vapor as follows. a. If using a diffusion pumped system, monitor the foreline pressure on the diagnostics screen. Do not allow the foreline pressure to exceed 500 mTorr for more than 20 seconds. b. Turn the adjustment valve clockwise to reduce the pressure. c. Open the CI gas solenoid valves by clicking on the CI icon in the Control and Status field of the Manual Control tab dialog in System Control. When the valves are opened, the CI button is green.
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3. To flush excess water from the gas line proceed as follows: a. Ensure that the electron multiplier, filament, and RF voltage are off. b. Open the main valve on the lecture bottle. (The secondary valve on the pressure regulator is already open.) c. Turn the CI needle valve fully counterclockwise. d. Open the CI gas solenoid valves and allow the system to pump down for about 1 hour. e. Close the main valve on the gas cylinder but keep the CI GAS solenoid valves open. Allow the system to pump down for about 15 minutes. f. Recheck the air/water spectrum. If excess water is not present, go to paragraph: Setting Delivery Pressure of the CI Reagent Gas.
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You are now ready to operate the system in the CI mode. If you are a new user, we recommend that you perform the introductory example of CI operation in tuning the Saturn for Chemical Ionization in the Tutorial Manual.
Methane
13 9 45 5000 2000 60 100
Isobutane
19 15 65 5000 2000 60 100
Ammonia
13 9 45 5000 2000 60 100
If you have installed the Liquid CI Inlet or the Multiple CI Module, the following parameters may be used for standard liquid CI reagents.
Acetonitrile d3-Acetonitrile
19 15 65 5000 2000 40 100 19 15 65 5000 2000 20* 100
Methanol
19 15 55 5000 2000 40 100
Use short reaction times for deuterated reagents. Longer reaction times allow more H/D exchange with background water and the resulting spectrum will show + + more [M+H] and less [M+D] .
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Isobutane
Ammonia
Acetonitrile
d3-Acetonitrile
Methanol
In each case, by following these guidelines, the reagent gas pressure in the ion -5 -3 trap will be approximately 1 to 2 x 10 Torr (about 1.3 to 2.6 x 10 Pa). The CI reagent molecules comprise about 1% of the gas pressure in the ion trap. He atoms from column flow are present at 100 times this pressure.
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Note the Diffusion Pump Foreline Pressure reading under the Vacuum System field. The reading should be less than 100 mTorr. Higher readings may indicate problems (i.e., leaks) and the user should refer to the Troubleshooting section for additional information. Click on the Manual Control button, and then click the CI icon to the left of the ion trap symbol (it will turn green when On). Wait one minute for the flow to equilibrate. Click on Diagnostics and note the Diffusion Pump Foreline Pressure reading. The value should be less than 350 mTorr. If necessary, adjust the delivery pressure of the CI reagent gas (using the valve on the pressure regulator) to give a reading below 350 mTorr. If the value exceeds 500 mTorr the diffusion pump will shut down. It will restart when the pressure drops below 500 mTorr.
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d. Loosely attach the Liquid CI Inlet assembly to the back of the instrument via the L-bracket with the screw that was removed. e. Rotate the Liquid CI Inlet assembly out of the way to remove the remaining screw. f. Rotate the Liquid CI Inlet assembly back into position and loosely attach the liquid CI inlet assembly with the remaining long screw (12-22200625).
g. Re-insert the liquid CI restrictor tube through the L-bracket into the back of the instrument. The restrictor tube must be inserted far enough to engage the O-ring in the CI shutoff block.
A B C D
Inlet Block (03-930023-01) Viton O-ring (03-930109-07) O-ring Retainer (03-930025-01) Reservoir Bulb, same as Cal Gas Chamber (03-920270-00)
E F G H
Reservoir Cover (03-93002601) Restrictor (03-930024-01) L-Bracket (03-930027-01) Viton O-Ring (03-930109-04)
3. Replace long restrictor (03-930597-01) with 1/8" OD PEEK tubing (03-93003701). a. With the liquid CI inlet mounting screws still loose, pull out the long restrictor tube from the CI shutoff block. b. Loosen the 4 screws on the top of the pneumatics manifold (at the front of the instrument). c. Pull out the long restrictor tube from the bottom of the pneumatics manifold. Carefully pull the tube out of the front of the instrument. Save this long restrictor for use with pressurized gases such as methane.
d. Feed the PEEK tube (03-930037-01) into position, starting from the front of the instrument (occupies roughly the same space as the long restrictor tube).
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e. Gently install the PEEK tube end into the pneumatics manifold, being careful not to let the retaining plate scratch the tube. f. Do not retighten the 4 screws on the pneumatics manifold yet. g. Insert the other end of the PEEK tube into the CI shut-off block and tighten the 2 screws from the rear of the instrument. 4. Replace the front restrictor. a. Remove the existing short gas restrictor (03-930596-01) from the bottom of the pneumatics manifold. b. Install the front liquid CI restrictor (03-930596-02) into the same location in the pneumatics manifold. Be careful not to let the retaining plate scratch the restrictor tube ends. c. Now retighten the 4 screws on the pneumatics manifold. 5. Replace the top cover. 6. Restart the Saturn system.
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CAUTION
Never force the cap onto the reservoir stem it is glass and can break.
Use safety glasses and protective gloves, especially when attempting to remove a cap from a filled reservoir.
Use a gentle, twisting/pushing motion to install the plastic cap onto the reservoir stem. Use a gentle twisting/pulling motion to remove the plastic cap from reservoir stem.
Be careful not to spill any liquid, especially the few drops which may be in the neck of the bulb.
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1. Loosen the 2 screws that attach the liquid CI inlet L-bracket to the back of the instrument. Also, loosen the 2 screws that attach the L-bracket to the liquid CI inlet block. 2. Remove the liquid CI restrictor end that inserts into the back of the instrument; rotate the restrictor out of the way. 3. Install the long CI gas restrictor (03-930597-01) between the gas supply and the CI shutoff block, through the L-bracket. 4. Tighten all screws. 5. It is not necessary to replace the front liquid CI restrictor (03-930024-01) with the short gas restrictor (03-930596-01). Reduce the gas pressure to 5 psi at the supply to return to normal gas CI operating conditions.
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Pre-Installation Checklist
1. Preparing the Mass Spec a. The Saturn MS should be shut down, vented, and unplugged. 2. Tools Required a. #2 Philips screw driver b. Small tipped straight screw driver c. 5/32 in or 4 mm drill bit d. Electric drill e. Side cutters to cut Tygon tubing
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3. Vent the mass spec. 4. Unplug the power cord from the back of the mass spec. 5. Unpack the Multiple CI kit and place the parts on a table. 6. Open the front door on the mass spec until it presses against the right side panel. 7. Find the register plate (03-930072-01) in the CI kit.
8. Peel off the adhesive strip. 9. Position the register plate 0.25 inches (0.6 cm) from the open front door and 5.25 inches (13.3 cm) from the bottom. Be sure to position the plate parallel to the open front door. Press firmly to adhere the plate to the right side panel. 10. Close the front door and remove the right side panel. 11. Use a 5/32-inch (4 mm) drill bit to drill four holes through the side panel using the register plate as a template.
12. There are two more holes in the register plate. Guide the metal tube through the upper hole and the Tygon tube through the lower hole.
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13. Use two #6 x 0.50 inch long screws to attach the multiple CI manifold to the register plate and side panel. 14. Stand the side panel next to the right side of the mass spec.
15. Guide the two tubes past the power board and through the opening in the chassis halfway up the middle bulkhead, behind the front panel. Leave the tubes protruding out the opening for the mass spec pneumatics. 16. Reattach the side panel with the #8 screws.
17. Loosen the four screws on top of the pneumatics block. 18. Remove the U-shaped tube from the pneumatics block. 19. Remove the single metal tube from the pneumatics block.
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20. There are now three openings in the pneumatics block. 21. Connect the metal tube from the multiple CI assembly to the opening on the left. 22. Connect the previously removed U-shaped tube, to the two right openings in the pneumatics block. 23. Tighten the four screws on top of the pneumatics block. Do not over tighten them.
24. Cut the Tygon tubing, which is running from the pneumatics block to the elbow about 4 inches (10 cm) from the pneumatics block. 25. Install the tee and connect the extra fitting to the Tygon tube from the Multiple CI assembly. 26. Connect the cable to the External Events on your GC.
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3800 GC
If you are installing the MCI Module on a 3400 or 3600 GC, skip to the installation instructions following this section. 1. The Multiple CI solenoid cable plugs into the External Events on the 3800 GC. 2. Remove the GC left side, top cover, and the detector cover. 3. Locate the External Events connector J42. 4. Connect the "A" wires to "1", the "B" wires to "2", and the "C" wires to "3". Hold each wire in the connector, and turn the screw clockwise to lock the wire into place. 5. The 3800 GC must have the External Events configured, or the Workstation software will not be able to activate them. 6. On the GC front panel, press the SETUP button. 7. Press 2 to EDIT Instrument Setup. 8. Press 5 to Edit the Valves. 9. The cursor should be on Valve type number 1. Press the DECR key until "Event A" is displayed. Press the down arrow cursor key. 10. The cursor should be on Valve type number 2. Press the DECR key until "Event B" is displayed. Press the down arrow cursor key. 11. The cursor should be on Valve type number 3. Press the DECR key until "Event C" is displayed. Press the down arrow cursor key. 12. Press the blue key below the display menu box entitled "Save and Exit".
3400/3600 GC
1. Connect the wires as shown to pins 1 and 2 on the Rectifier PWA 03-930346-00. 2. Connect the wires as shown to pins 3 and 4 on the Rectifier PWA. 3. Connect the wires as shown to pins 5 and 6 on the Rectifier PWA. 4. Turn off the GC.
WARNING:
SHOCK HAZARD
Dangerous Voltages Exposed When High Voltage Cover is Removed. Unplug Power Cord. No operator serviceable parts under cover. Refer any questions to high voltage cover to qualified service personnel.
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5. Unplug the power cord. 6. Remove the top covers. 7. Remove the high voltage cover.
8. Connect the Rectifier PWA to pins 3 - 8 on the External Events board in the GC. 9. Tighten all six of the connector screws to ensure good electrical contact. If there are other electrical devices connected to the GC External Events 2, 3, or 4, they will have to be disconnected while Multiple CI is connected. 1. Install the high voltage cover and top covers. 2. Plug in the GC and turn on power. After installation, verify that the MCI Module is leak-tight by performing Air/Water and available pressure checks (depending upon the configuration of your instrument) on the Saturn system. This section describes setup, acquisitions with, and maintenance of the MCI Module.
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Hazardous chemicals may be present. Avoid contact, especially when replenishing reservoirs. Use proper eye and skin protection.
5. Use the 5 mL syringe supplied in the Accessory Kit to fill the bulb halfway with 3 mL of the chosen CI reagent liquid. 6. Carefully reinsert the bulb in the inch inlet port of the channel. 7. Retighten the screws on top of the module. The bulbs will be held firmly by the Oring seals after the screws are tight. 8. Replace the MCI cover and tighten the thumbscrew to hold it in place. 9. After installing CI reagent liquids, and each time a reagent liquid or gas is installed, always use care when first opening the CI valves. 10. If you have a turbo pump system, skip this step. If you have a diffusion pump system, first turn on the relays, then open the needle valves slowly by turning the knobs fully counterclockwise, to clear out the air in the reservoir bulbs. After a few seconds, monitor the foreline pressure. Do not allow the pressure to exceed 500 mTorr for more than twenty seconds or the diffusion pump will shut down. Return the valve settings to open or their previous setting (approximately 7 turns). 11. Do not turn on the filament or multiplier for 2-3 minutes after opening the CI valves. A convenient way to verify that air and water have been removed sufficiently is to check the ion gauge pressure with the CI valves open. Verify that -6 the pressure has returned to less than 35 x 10 Torr before turning on the filament and multiplier.
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Select the section GC Relays under 3400 or 3600 GC Control. You will see the following screen:
If you wish to adjust flows of all three CI reagents in the MCI Module, you will want to save three Methods with Relays turned on for each specific reagent. If Channel A is connected to External Event 1 in the GC, click in the box for Relay 1.
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Now use the menu command FileSave As to save the method with a name such as ChannelA. Check the box for either Relay 2 (Channel B) or Relay 3 (Channel C) and save these methods as ChannelB and ChannelC. You may now open Channels A, B, or C by using the menu command FileActivate (CHANNELx) from the System Control window.
If you have Channel A connected to Valve 1, click in Row 1 under the Valve 1 column. Click on the down-arrow in the combo box and scroll down to find the External Events options for the Valve 1:
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Highlight External Event A and release the mouse button. You will see the following display:
Now, if Channels B and C are connected to Valves 2 and 3, enter the appropriate state by highlighting the first row under Valve 2 and Valve 3. Otherwise, enter External Events A through C under the appropriate Valve column. The display will now show all three External Events with the correct Valve position, but all Valve States are off. In Row 2 under Valve 1, double-click on the Off symbol or use the arrow key on the right side of the cell to toggle the Valve State to On:
Now use the menu command FileSave As to save the method with a name such as ChannelA. Change the Valve States to be On for either External Event B (Valve 2) or External Event C (Valve 3) and save these methods as ChannelB and ChannelC. You may now open Channels A, B, or C by using the menu command FileActivate (CHANNELx) from the System Control window.
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Modify the method to create a single-segment method for CI/Auto acquisition. You may later use this method as a default method for CI acquisition with the MCI Module, so you may wish to adjust method parameters such as Start and End Times and Low and High Mass appropriately for your samples. NOTE: If you do want to use the method for GC/MS acquisitions, remember to assure that there is a Filament/Multiplier delay segment with ionization method = None.
Click on the tab dialog Ionization Mode - CI Auto to choose CI parameters for this MCI Channel. Parameters for the default CI reagent Methane will be shown. Click on the selection arrow in the Reagent Gas field and choose the CI reagent you have selected for Channel A of the MCI Module. In this example we have chosen acetonitrile for Channel A:
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The values of each parameter for acetonitrile CI are identified in the table Default Parameters for Liquid CI Reagents and already entered into the fields on the right side of the table. (If we were setting up for any of the standard gaseous or liquid reagents, their parameters can be entered automatically by clicking on the appropriate Reagent Gas selection. Parameters for other CI reagents may be entered by clicking on the User-Defined selection and entering user-selected parameters.) Once the CI parameters are chosen, click on the Segment Setpoints tab dialog and choose values for other parameters. The default for ARC Target count is 5000 count for all reagents. Values up to 20,000 are commonly used. You may also want to select an Emission Current specific to the Tune File. Generally an emission current of 10-20 A is used in CI acquisitions. When you have finished these steps save the Method for Channel A with the menu command FileSave As ChannelA.mth. Modify this method for the CI reagents in Channels B and C and save the new methods with the menu command FileSave As ChannelB.mth or ChannelC.mth. You may then activate the files from System Control with the menu command FileActivate.
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the Manual Control comes up with the Method tab displayed. Note that the method Name, Mode, and Scan Range are displayed.
5. Click on the Adjustments tab dialog and then choose Acetonitrile as the gas and click on Adjust.
7. If, after a couple of minutes, there is not enough CI gas entering the trap, increase the flow by turning the needle valve for the chosen Channel on the MCI Module clockwise.
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8. While observing the spectrum using Adjust CI Gas, turn the CI needle valve for the selected channel on the MCI Module clockwise to increase (or counterclockwise to decrease) the amount of reagent until the reagent ions abundances meet the requirements outlined for the chosen reagent in the table shown in Ion Intensities for Standard CI Reagents.
Next, choose the Method Directory item Flow/Pressure and verify that the parameters are acceptable. The following method uses a Type 1 EFC and constant pressure programming at 10 psi:
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Now choose the Method Directory item Column Oven and set an appropriate column oven program. The following program requires a 30-minute run:
Choose the Method Directory item Sample Delivery and create a Sample Delivery method with all External Events Off:
Click on the MS Method Editor item under 2000 Mass Spec Control and create a standard EI/MS section with a run time matching that of your EI_GC section.
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Click on the Add button on the right of the window to add another segment and enter 30 under Time so that External Event A will be turned Off again at the end of the run. In the following example, it is assumed that acetonitrile is in Channel A of the MCI Module, which is activated from Valve 1.
NOTE: It is always a good idea to close the chosen Channel of the MCI Module at the end of a run so that the foreline pump is isolated from the CI reagent. Otherwise, the reagent will be pumped continuously from the Channel until it is exhausted.
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If you are planning to use a different CI reagent in each Channel of the MCI Module, save a unique GC/MS Method specific to each Channel of the MCI, each with External Events programming of the correct Event. Under Saturn 2000 Mass Spec Control choose the Method Directory item MS Method Editor to prepare a CI/MS section of the Method.
Several parameters must be examined or selected for an appropriate acquisition with a given CI reagent. In this example, note that the low mass limit for acquisition is 70 and the Background Mass is set to 65 for the acetonitrile CI method. Collecting data below this limit might result in significant interferences from acetonitrile reagent ions. Similar parameters for isobutane CI are advised. Acquisitions with methanol, ammonia, and methane reagents can generally be accomplished effectively with lower starting ranges and background masses. See the tables Default Parameters for Liquid CI Reagents or Default Parameters for Gaseous CI Reagents for suggested background masses. Low mass for acquisition should never be lower than the suggested background mass for a given reagent. Also note that the mode for acquisition must be changed from EI Auto to CI Auto. Save the GC/MS Method with a name indicating the CI reagent chosen - in this case we save the method as ACN_CI.mth If you are planning to use a different CI reagent in each Channel of the MCI Module, save a unique GC/MS Method specific to each Channel of the MCI, each with External Events programming of the correct Event.
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To prepare the Sample List for alternating EI/CI acquisitions, click on the Edit Automation Files button on the Star Toolbar or choose the option StartProgramsSaturn GCMS WorkstationAutomation File Editor. The Automation File Editor Dialog Box will open. Click on the option FileNewSampleList.
Select the name EI_CI for the new Sample List and click on Save.
You will see a dialog to Select SampleList Section Type. Select the 8200 AutoSampler and click OK.
You will now see the new EI_CI SampleList ready for entries.
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Since EI and CI analyses are to be performed on three samples in succession, enter the appropriate names for the data files in each row of the SampleList.
Use the scroll bar at the bottom of the dialog to display fields farther to the right in the SampleList. This will allow you to enter the Method and the 8200 AutoSampler Rack/Vial positions to use for each sample. For this example enter Vial 1 for the first pair of runs and Vials 2 and 3 for the succeeding pairs.
Finally, you need to enter the GC/MS method to be used for each sample. This may be done in the AutoLink section of the SampleList. Click on the AutoLink button in Row 1 of the SampleList. Enter the proposed method for EI/MS
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acquisition in the Command field and click OK. In this example the method is EI_GC.mth.
Since the same EI_GC method will be used later in the list highlight the AutoLink button in the list and click on Fill Down.
The EI_GC method is now selected for all entries in the SampleList. The final step in the process is to click on the AutoLink field for each acetonitrile CI sample and substitute the method ACN_CI. After this has been done, the correct GC/MS methods are specified for all entries in the SampleList.
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Use the AutoLink field to activate the appropriate method for the EI or particular CI reagent required.
Saturn MS Analysis
Similarly, in the Method Directory item 2000 Mass Spec ControlMS Method Editor, the MS Method is split into time segments. The method is set up first for a 30 minute run using the ACN_CI tune file. Segment 1 is a Filament/Multiplier delay until solvent front elutes from the GC column. Segment 2 is for acetonitrile CI acquisition.
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Then, while Segment 2 is highlighted, click the Add twice to create two additional Segments. Segment 2 is left as an acetonitrile CI segment ending at 10 minutes. Segment 3 parameters are changed in the Ionization Mode tab dialog to those for methanol CI and the end time is set for 20 minutes.
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In a complex method such as this, it is always advisable to review the MS Method to assure that the segment times and acquisition parameters have been entered correctly.
k C o u n ts 2 .0
M e th a n o l- m /z
3 3
1 .5
1 .0
0 .5
0 .0 k C o u n ts 2 .0 1 .5 1 .0 0 .5 0 .0 C o u n ts 5 0 0 4 0 0 3 0 0 2 0 0 1 0 0 0
A c e to n itr ile - m /z
4 2
M e th a n e - m /z
1 7 + 2 9
1 0
1 5
2 0
2 5
m in u t e s
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Filling/Refilling the Liquid CI Reservoir Bulb to fill the reservoir bulbs (03-92027000) with liquid. If you wish to replace a liquid reagent with a different liquid, you may use a vial cap (03-949870-04) from the MCI Module Accessory Kit to cap the reservoir and store it in the laboratory refrigerator in the Reservoir Stand (03930073-01) supplied with the Kit. It is a good practice to use a single CI liquid in each channel of the MCI Module. Vapor from the liquid will be absorbed to some extent in the O-rings sealing the vial, restrictors, and solenoids for each channel.
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adapter fitting and the long restrictor (03-930597-01). The long restrictor was connected between the pneumatics manifold and the gas shut off valve before the MCI module was installed. Protect the ends of the restrictors to prevent contamination and plugging, when working on the assembly. The MCI Module must have all of its ports connected for proper operation. If fewer than three reagents are installed, then empty reagent bulbs must be installed in the unused positions. Also, if the restrictors are removed for any reason, their ports must be plugged with the pin plugs (17-783512-00) supplied. 1. Turn off all relays related to the MCI module. 2. If you have a turbo pump system, skip this step. If you have a diffusion pump system: For each channel that will be worked on, close the associated needle valve by turning the knob clockwise. Monitor the foreline pressure. Do not allow it to exceed 500 mTorr for more than 20 seconds. This will reduce the inrush of air into the vacuum system when the channels are reactivated. 3. Remove the MCI cover by loosening the thumbscrew on the front cover. 4. Loosen (but do not remove) the four screws located between the solenoid valves on top of the module. 5. Remove the liquid reagent reservoir by gently rotating and pulling the bulb down and out of the manifold. If there is unused liquid reagent remaining in the bulb, and you wish to save it, cap the bulb with one of the vial caps (03-949870-04) supplied in the accessory kit. You can use the reservoir stand (03-930073-01), also found in the accessory kit, for storage. 6. Remove the lower restrictor (03-930596-02) installed in the two 1/8 inch ports underneath the manifold block. Save the restrictor in a clean, particle free bag, to prevent contamination and plugging. 7. Insert the short lower restrictor (03-930596-01) in these ports. 8. Attach the gas adapter (28-695138-00) to one end of the long restrictor (03 930597-01) with the Teflon ferrules. The gas adapters and Teflon ferrules are found in the accessory kit. Teflon ferrules are used so that the gas adapter fitting can be removed from the long restrictor, so that you may reuse it in its original configuration. Ensure that the connection is tight to prevent leaks. 9. Fully insert the gas adapter into the inch inlet port of the channel and route the long restrictor down and back so that it will clear the cover, when it is reinstalled. 10. Tighten the 4 screws on top of the module. The gas adapters and restrictor lines will be held firmly by the O-ring seal after the screws are tight. 11. Replace the MCI cover and tighten the thumbscrew to hold it in place. Make sure that all of the lines are free and clear of the cover before tightening the thumbscrew. 12. Attach the free end of the long restrictor (03-930597-01) to your pressure regulated gaseous reagent supply, set to 5 psi. 13. After installing CI reagent liquids, and each time a reagent liquid or gas is installed, always use care when first opening the CI needle valves. 14. If you have a turbo pump system, skip this step. If you have a diffusion pump system, first turn on the relays. For each channel worked on, open the needle valve slowly by turning the knob fully counterclockwise to clear out the air in the lines. After a few seconds, return the valve setting to open or their previous setting (approximately 7 turns).
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15. Do not turn on the filament or multiplier for about 2-3 minutes after opening the CI valves. A convenient way to verify that air and water have been removed sufficiently is to check the ion gauge pressure with the CI valves open. Verify -6 that the pressure has returned to less than 35 x 10 Torr before turning on the Filament and Multiplier.
Hazardous chemicals may be present. Avoid contact, especially when replenishing reservoirs. Use proper eye and skin protection.
8. Using the 5 mL syringe supplied in the Accessory Kit, fill a liquid CI reagent reservoir halfway with 3 mL of the chosen CI reagent liquid. 9. Insert the reservoir neck into the inch inlet port of the channel. 10. Tighten the 4 screws on top of the module. The liquid CI reagent reservoir and restrictor lines will be held firmly by the O-ring seal after the screws are tight. 11. Replace the MCI cover and tighten the thumbscrew to hold it in place. Make sure that all of the lines are free and clear of the cover before tightening the thumbscrew. 12. After installing CI reagent liquids, and each time a reagent liquid or gas is installed, always use care when first opening the CI needle valves. 13. If you have a turbo pump system, skip this step. If you have a diffusion pump system, first turn on the relays. For each channel worked on, open the needle valve slowly by turning the knob fully counterclockwise to clear out the air in the lines. Monitor the foreline pressure. Do not allow it to exceed 500 mTorr
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for more than 20 seconds. After a few seconds, return the valve setting to open or their previous setting (approximately 7 turns). 14. Do not turn on the filament or multiplier for about 2-3 minutes after opening the CI valves. A convenient way to verify that air and water have been removed sufficiently is to check the ion gauge pressure with the CI valves open. Verify -6 that the pressure has returned to less than 35 x 10 Torr before turning on the filament and multiplier.
Leak Checking
If a leak in the CI plumbing is suspected, use the general leak-checking procedures found in the Saturn Maintenance and Troubleshooting manual under the heading How to check for leaks. To isolate suspected leaks within the MCI module, replace the liquid vials or gas lines with empty CI reagent vials as outlined in this manual titled Adding Liquid CI Reagents to the MCI Module. After carefully opening the needle valves and relays according to the procedure, allow the air to be pumped from the vials and tubing. Now each Channel can be tested individually by selecting it using the GC relays and with the CI valve open, carefully spraying compressed argon around the fittings while monitoring the spectrum for m/z 40, or you may use tetra-fluoroethane (Dust-Off ) and monitor the spectrum for m/z 69. A leak at one of the O-ring seals may be fixed by cleaning the tubing and O-ring, but usually a new O-ring is required. Extras are provided with the MCI module and also in the accessory kit.
Cross-Contamination Effects
Vapor from liquid CI reagents is absorbed to some extent in the O-ring seals of each Channel used for liquid CI. If the liquid or gas chosen for the Channel is changed, the residual vapor from the previous reagent may create artifact CI reagent ions observable when adjusting the CI gas flow. If these artifact ions comprise more than 10-20% of the total reagent ions observed during CI flow adjustment, they may affect the CI spectra of the analytes. For example, residual soft reagent ions from acetonitrile at m/z 42 and 54 may be observed if one switches the reagent to methanol in a given Channel. These softer reagent ions may lead to an increased proportion of M+1 ions in the methanol CI spectrum compared to the ratios observed without the artifact acetonitrile reagent ions present. Absorbed solvent in Channel seals may be reduced by prolonged vacuum pumping of the Channel: 1. Replace the liquid CI vial or gas line in the Channel with an empty CI reagent vial. 2. Open the Channel from the GC keyboard. See the instructions in Selecting Reagent Channels from the 3800 GC Keyboard. 3. Do not turn on the CI icon in the Saturn software. 4. Open the Needle Valve for the Channel full counterclockwise so that all flow from the Channel is directed to the Foreline Pump. 5. Leave the Channel open overnight or over a weekend. 6. Replace the desired reagent in the Channel position and observe reagent ions during CI gas adjustment.
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Shutdown Page
NOTE: The Diffusion Pump System shutdown sequence takes at least 30 minutes. The Saturn GC/MS heaters are turned OFF. The GC temperature zones should be cooled downed before maintenance is performed. The diffusion pump heater is turned OFF while the Peltier Baffle cooler is kept on. The DIFFUSION PUMP STATUS changes from NORMAL to COOLING. After 15 minutes, at which time there is no longer any pump vapor to contaminate the system, the Peltier Baffle cooler is turned OFF. After another 15 minutes, the cooler has warmed to the point that it wont condense water vapor, and the pump is considered to be off. The DIFFUSION PUMP STATUS changes from COOLING to OFF.
NOTE: If the word FAULT! is displayed in the Vacuum Status box, click on Diagnostics tab for detailed information on fault.
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This represents a group of error messages indicating that the diffusion pump has been shut down. To precisely identify the problem, the USER should go to the Diagnostics tab, check System Test and Run to Completion.. Fault messages may appear on startup or during operation. Turn OFF main power by placing switch at rear of system to OFF (down) position. Manually vent the system for at least 5 minutes using the lever on the front panel.
CAUTION
DO NOT ATTEMPT to VENT SYSTEM by any other method (via transfer line, foreline vacuum clamps, etc.). Rapid, improper venting of the system will cause diffusion pump fluid to back stream into the manifold and ion trap. Maintenance procedures should NOT be attempted until shutdown program has completed!
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NOTE: The Vacuum System status should be periodically checked during Startup for foreline pressure. The pressure should read below 500 mTorr in 5 minutes and < 100 mTorr after 45 minutes. Higher values may indicate a leak. Refer to Troubleshooting.
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Periodic Maintenance
To ensure the Saturn GC/MS peak-performance, you will have to perform periodic maintenance on the vacuum and cooling systems. The following table identifies relevant maintenance intervals. Procedure
Check the foreline pump oil level and condition Purge foreline pump oil Check cooling fans Check diffusion pump fluid and condition Change foreline pump oil Clean diffusion pump
Interval
Weekly Weekly Weekly Monthly Every 6 months Every 6 months
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A B C D E F G H I
Foreline Clamping Ring Seal Inlet Gas Ballast Valve Drain Plug Oil Level Sight Glass Filler Plug Exhaust
Foreline Pump
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CAUTION
Pump weighs 25 kg (55 lb.). Use proper lifting techniques.
6. Place an oil pan beneath the drain port to catch any spillage.
Hazardous chemicals may be present. Avoid contact with skin. Use proper eye and skin protection.
7. Remove the plastic cover and the filler plug on top of the pump. 8. With the container in place to catch the oil, slowly remove the drain plug in the front of the pump.
WARNING
Toxic residues from mass spectrometer samples will build up in used pump oil. Dispose of all used pump oil in accordance with applicable regulations. Place a hazards warning label on the container, if appropriate.
9. Tilt the pump forward and hold until oil flow ceases. 10. Return the pump to the horizontal and refit the plug. 11. Run the pump for approximately ten seconds with the intake port open. This will remove any residual oil from the pumping block.
CAUTION
Avoid breathing oil mist coming from the exhaust port during this operation.
12. Remove the plug, tilt the pump, and drain the oil. 13. Return the pump to the horizontal. 14. Wipe the oil residue from the drainage port, and refit the drain plug.
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15. Fill the pump with fresh oil (88-299517-00) through the filler port until the oil level reaches the maximum level in the sight glass. A funnel may be helpful.
Flushing
The pump should be flushed if the pump oil is particularly dirty. After draining the pump (previous steps 1-13): 1. Remove the inlet filter by removing the inlet ports locking screw with a 4 mm Allen wrench; unscrewing the inlet port with a 30 mm open ended wrench; and pulling the filter up with a pair of tweezers or long nose pliers. 2. Clean the filter in warm soapy water. Rinse and blow-dry with air or nitrogen. 3. Refit the filter. 4. Screw the inlet port back into the pump housing and lock in place with the locking screw. 5. Pour 0.33-Liter l (0.35 US qt) of fresh pump oil in through the inlet port then run the pump.
CAUTION
Avoid breathing oil mist coming from the exhaust port during this operation.
6. Stop the pump, drain the flushing oil, and replace as described previously.
The cooling fans maintain an optimal temperature for the turbomolecular pump and the other electronics modules. Without the cooling fans, the lifetime of the turbomolecular pump and temperature-sensitive PC-board components would be shortened. To ensure proper operation of the cooling system, operate the Saturn GC/MS with its covers in place. In addition, be sure to check the fans at least once each week. The Saturn GC/MS is equipped with two fans on its rear panel. The function of these fans is to pull air into the instrument. To check fan operation, proceed as follows: 1. Make sure that the Saturn main switch and service switch are turned ON. 2. Place a large sheet of paper over one of the fan guards. If the paper is sucked toward the fan guard, the fan is working. If it is not, the fan is broken. Contact your Varian Customer Support Representative to arrange for a replacement.
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Saturn 2000 GC/MS, Front View A B C D E F G H I Main Power Switch (rear panel) Service Switch Transfer Line Heater Trap Heater Manifold Heater LED Pneumatics Manifold CI Cal Gas Adjust Cal Gas Adjust J K L M N O P Q Cal Gas Vial Vent Valve RF Coil RF Coil Adjustment Screw Transfer Line Turbomolecular Pump Cooling Fans CI Shutoff Valve
If the fans are excessively noisy, i.e., if they whine or whir, one of the fans may be about to fail and it should be replaced. To identify which of the two fans is about to fail, proceed as follows: 1. Remove the top cover from the Saturn GC/MS. If the noise continues, proceed to step 3. If the noise stops, proceed to step 2.
2. Turn off the electronics compartment fan via the service switch, and replace the top cover. If the noise returns, it is coming from the turbomolecular pump cooling fan. Proceed to step 4. If the noise does not return, remove the cover and proceed to step 3.
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3. Turn off the electronics compartment fan via the service isolation switch. If the noise continues, it is coming from the turbomolecular pump-cooling fan. If the noise stops, it is coming from the electronics compartment fan.
4. Contact a Varian Customer Support Representative to arrange for replacement of the broken fan.
Turbomolecular Pump Connections A B C Pneumatics Exhaust Tube Transfer Line Clamping Screws (4 places) D E F Turbomolecular Cable Vacuum Hose Vacuum Hose Elbow
11. Loosen each of the four clamping screws about 2 turns with a 3/16-in. hex driver.
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Take care not to completely unscrew the two inner clamping screws. (If you should unscrew them, restart the screws after you have removed the turbomolecular pump from the instrument.)
12. Remove the outside bottom clamping screw. 13. Remove the bottom clamp as you hold the turbomolecular pump in place. 14. Remove the outside top clamping screw (closest to the transfer line). 15. Remove the top clamp as you hold the turbomolecular pump in place. 16. Pull the turbomolecular pump to the rear and lift it clear of the instrument. 17. Remove the large seal from the turbomolecular inlet, and place it on the inlet of the new turbomolecular pump (03-920542-00). The orientation of the seal is not important. On the new turbomolecular pump, leave the red cap over the turbomolecular exhaust port.
18. Carefully slide the new turbomolecular pump and seal into position on the end of the manifold. Make sure the electrical connection (turbomolecular cable) is tilted towards the bulkhead, i.e., toward the left as viewed from the rear of the instrument. Take care not to scratch the sealing surface on the manifold in front of the turbomolecular pump.
19. Insert the top clamp and loosely fasten it into place. 20. Insert the bottom clamp and loosely fasten it into place. 21. Tighten all four clamping screws until snug. 22. Reconnect the turbomolecular cable. Rotate the retaining ring clockwise with downward pressure to lock the cable into position. 23. Remove the red cap over the turbomolecular exhaust port. 24. Place the seal on the turbomolecular pump exhaust port. 25. Reconnect the vacuum hose elbow and clamp. 26. Reconnect the pneumatics exhaust tube. 27. Make sure that the vent valve is closed. 28. Turn on the rear-panel main power switch. 29. Snug up the top and bottom clamp screws. 30. Monitor the turbomolecular pump speed using Diagnostics under Vacuum System Status. 31. Once the pump is running satisfactorily, replace the side panel, top cover, and slide the GC and Saturn GC/MS back together. 32. Discard the old turbomolecular pump. Be sure to comply with all applicable health and safety regulations.
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Cooling fans perform two important functions in the Saturn GC/MS. They prolong the lifetime of temperature sensitive electronic components by maintaining optimal temperatures within the electronics compartments and they provide the airflow required by the air cooled diffusion pump and Peltier baffle. Cooling is divided into three zones. Zone one is the upper part of the analyzer compartment. Its purpose is to provide forced air-cooling for the Peltier baffle, and the manifold electronics. Zone two is the electronics compartment, diffusion pump controller, and RF generator board. Its purpose is to cool the majority of the instruments printed circuit boards. Zone three is the diffusion pump compartment. Its purpose is to cool the diffusion pump. The Saturn GC/MS is equipped with three fans on its rear panel, one for each zone. Each fan pulls air in through the front and/or side of the instrument and expels it through the rear panel. To inspect the cooling system, ensure the Saturn main power switch and service switch are turned ON (refer to the figure showing these zones). Proceed as follows: 1. Zone 1: Upper analyzer compartment. The Zone 1 fan is located in the top left of the rear panel (as viewed from the front of the instrument). Failure of this fan will be detected by the diffusion pump controller, which will initiate a system shutdown. The only components of zone one requiring checking are the Peltier baffle duct and the top cover. To check: 2. Check the front of the instrument is not obstructed. 3. Check the rear of the instrument has at least 250 mm (10") of clearance. 4. Remove the top cover and check the Peltier baffle ducting is in place. 5. Refit the top cover. 6. Zone 2: Electronics compartment, diffusion pump controller, and RF generator board. The Zone 2 fan is located in the middle right hand portion of the rear panel. Zone two may be checked as follows: a. Check the front of the instrument is not obstructed. b. Check the rear of the instrument has at least 250 mm (10") of clearance. c. Check the left side cover is in place and not obstructed (fallen paper, tissues, etc.)
WARNING:
SHOCK HAZARD
Hazardous voltages are present under right side cover. This cover should not be removed.
7. Check the GC and MS are separated by approximately 19 mm (3/4") using the standoffs installed on the MS. 8. Place your finger approximately " away from the fan finger guard to feel if air is coming out of the fan.
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If not, the fan is broken and should be replaced. Contact your Varian Customer Support Representative to arrange for a replacement.
9. Zone 3: Diffusion pump compartment. The Zone 3 fan is located in the lower left corner of the rear panel. Failure of this fan will cause the diffusion pump to overheat. This will be detected by the diffusion pump controller, which will initiate a system shutdown. The only components of zone three requiring checking are the air intake and exhaust. To check: a. Check the left side cover is in place and not obstructed. b. Check the rear of the instrument has at least 250 mm (10") of clearance. c. Check the GC and MS are separated by approximately 19 mm (3/4") using the standoffs installed on the MS.
4. Refit the left side cover and fasten in place with the four screws and two spacers.
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Diffusion Pump Compartment A B C D Thermocouple Gauge Elbow Pneumatics Exhaust Tube Diffusion Pump E F G H Exhaust Clamp Diffusion Pump Controller (behind cover) Inlet Clamp Fan
WARNING:
CAUTION
Do not attempt to vent the MS by any other means. Venting through the foreline connections or transfer line will cause a rapid pressure increase that will coat the ion trap and internal surfaces of the manifold with diffusion pump fluid. A transfer line venting will also cause high mass noise in the trap.
2. Maintenance work may begin once the vacuum system has vented to atmospheric pressure. This takes approximately five minutes. This may be checked by placing a finger over the vent port to feel for suction.
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24. Reinstall the clamp by pushing it onto the joined exhaust flanges. 25. Rotate the clamp 180 and install the screw from the left side. 26. Thread the wing nut onto the screw. 27. Rotate the clamp as far to the left as possible, while still allowing room to turn the wing nut. Otherwise, the wing nut will prevent reinstallation of the side panel. 28. Tighten the wing nut. 29. Refit the vacuum tubing to the elbow and tighten the clamp. 30. Insert the pneumatics exhaust tube into the elbow until the O-ring seats. Screw plastic nut in place using fingers. 31. Reconnect the thermocouple gauge cable to the thermocouple gauge. 32. Push the Peltier baffle duct base over the heat sink and onto the rear panel. Fasten in place using the two screws through the rear panel. 33. Reconnect the Peltier baffle leads to the Peltier baffle. The pins and sockets are differentiated by size. 34. Refit the Peltier baffle ducting by inserting the tabs into the rear panel and pushing the front of the duct down onto the front post. 35. Refit the left side cover and fasten in place with the four screws and two spacers. 36. Bring the MS alongside the GC and refit the transfer line. 37. Reconnect the manifold and trap heater cables. 38. Refit the top cover. 39. Carefully slide the MS up to the GC. 40. Close the vent valve by lowering the vent valve lever. 41. Turn on the MS.
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9. Ensure the new seal and sealing surfaces are clean and free of particles and fibers. 10. Fit the new seal to the Peltier baffle and lower the baffle into position on the manifold. Do not allow the seal to twist. 11. Reconnect the Peltier baffle leads to the Peltier baffle. The pin and sockets are differentiated by size. 12. Close the vent valve by lowering the vent valve lever. 13. Plug in the Saturn power cable. 14. Turn on the MS by switching ON the main power switch on the rear panel. This allows the vacuum to correctly seat and seal the baffle assembly. 15. Refit the retaining nuts and front pillar. These should be snug. 16. Refit the Peltier baffle ducting by inserting the tabs into the rear panel and pushing the front of the duct down onto the front post. 17. Turn the service switch to the OFF position. 18. Reconnect the transfer line, manifold, and trap heater cables. 19. Turn the service switch to the ON position. 20. Refit the top cover. 21. Carefully slide the MS up to the GC. 22. Bring up System Control to download the mass spectrometer software. 23. Bring up the diagnostics page by clicking on the Diagnostics tab. 24. Check the Vacuum Status. This will display a snap shot of the vacuum system status, including any faults. NOTE: The pressure should read below 500 mTorr within the first five minutes, and 100 mTorr within 45 minutes. Higher values may indicate a leak. Refer to Troubleshooting.
CAUTION
Do not immerse the assembly in acetone as it will contaminate porous components, and damage seals.
4. Rinse with isopropyl alcohol. 5. Allow cleaned surfaces to air dry, or bake in the GC oven for 10 min at 100 C. 6. Install the Peltier baffle, using the original seal.
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CAUTION
Be careful not to scratch or damage sealing surfaces.
A B C D
9. Unscrew the wing nut on the diffusion pumps inlet clamp approximately ten turns. 10. Grip the inlet clamp with both hands and push the wing nut into the clamp until the clamp loosens. 11. Hold pump with left hand and remove inlet clamp by moving the wing nut screw to the left, opening clamp and pulling around the flanges and out. 12. Lower the pump onto the base pan. 13. Remove the inlet seal and place on a clean lint free surface for later use.
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14. Grip the pump with your right hand, tilt towards you until the inlet flange clears the manifold flange.
CAUTION
Be careful not to scratch or damage sealing surfaces.
15. Pull the pump out to the full extent of its cable. 16. Disconnect the cable from the diffusion pump controller. 17. Remove the pump and set it on its base.
3. Add fluid until the level is between the mid and maximum mark on the cold arrow. 4. Wipe any spillage from the inlet baffle using a clean lint free cloth. 5. Refit the diffusion pump.
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Diffusion Pump A B C D E F G H I Circlip Inlet Baffle Centering Plate & Spring Jet Assembly Exhaust Baffle & Circlip Sight Glass Assembly Body Retaining Plate Base Plate J K L M N O P Q Heater Assembly Harness Clamp Insulation Disk Insulation Over temperature Switch Inlet Port Exhaust Port Ejector Stage
Hazardous chemicals may be present. Avoid contact with skin. Use proper eye and skin protection.
WARNING
Toxic residues from mass spectrometer samples will build up in used pump fluid. Dispose of all used pump fluid in accordance with applicable regulations. Place a hazards warning label on the container, if appropriate.
To clean the diffusion pump: 1. Layer a number of clean lint free cloths or paper towels on the work surface. 2. Provide a 3" deep x 3" wide x 7" long container filled with acetone to a depth of 2". 3. Remove the pump.
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4. Using a pair of circlip pliers, remove the circlip that holds the exhaust baffle in the exhaust port. Place the circlip on the towels.
CAUTION
Be careful not to scratch or damage sealing surfaces.
5. Withdraw the baffle and place it on the towels. 6. Using a pair of pliers, remove the circlip that holds the inlet baffle in place. Place the circlip on the towels.
CAUTION
Be careful not to scratch or damage sealing surfaces.
7. Withdraw the baffle, centering plate, and spring. Place these items on the towels. 8. Use a towel to wipe excess fluid from the circlip, baffle, centering ring, and spring. Place these items into the container of acetone. 9. Withdraw the jet assembly and place it vertically on the towels. 10. After allowing the excess fluid to drain, wipe down jet assembly and lay it down in the container of acetone. 11. Drain the diffusion pump fluid into a suitable container. 12. Clean the interior of the pump body with acetone and rinse with isopropyl alcohol. Allow to air dry.
CAUTION
Do not submerge the pump body as the solvents will be absorbed into the diffusion pumps insulation, creating a fire risk.
13. Rinse all the other parts washed in acetone with isopropyl alcohol, and air dry. 14. Drop the exhaust baffle into the exhaust port, ensuring the shortest end of the central post is uppermost. 15. Using a pair of circlip pliers, refit the circlip that holds the exhaust baffle in place. Orient the circlip to provide the maximum opening between the baffle and exhaust port wall.
CAUTION
Be careful not to scratch or damage sealing surfaces.
16. Place the jet assembly inside the pump body, ensuring the ejector stage lines up with the exhaust port. When correctly positioned, the jet assembly will locate on a pin in the base of the body. 17. Insert the spring into the counterbore of the jet cap. 18. Place the centering plate on the spring. 19. Lower the baffle onto the centering ring. 20. Using a pair of pliers, refit the circlip that holds the inlet baffle in place.
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CAUTION
Be careful not to scratch or damage sealing surfaces.
21. Pour the diffusion pump fluid (03-930639-01) through one of the holes in the 3 diffusion pumps inlet baffle. Part Number 03-930639-01 contains 40 cm . This is a full charge, plus an allowance for fluid that remains on the walls of the container. NOTE: The fluid is highly viscous and takes five minutes for a full charge to reach the reservoir and show in the sight glass. 22. Add fluid until the level is midway in the Full Cold zone. 23. Wipe any spillage from the inlet baffle using a clean lint free cloth. 24. Refit the diffusion pump.
Hazardous chemicals may be present. Avoid contact with skin. Use proper eye and skin protection.
WARNING
Toxic residues from mass spectrometer samples will build up in used pump fluid. Dispose of all used pump fluid in accordance with applicable regulations. Place a hazards warning label on the container, if appropriate.
3. Remove the two screws holding the over temperature switch in position. 4. Remove the two retaining screws and the base plate. 5. Use an 11/32 socket to unscrew the two nuts. 6. Remove the ground wire, harness clamp, retaining plate and insulating pad. 7. Pull the heater out by its leads, twisting if necessary. 8. If the heater does not come out: a. Apply penetrating oil around the cartridge heater and let it stand for 10 minutes. b. Drive a inch wide flat blade screwdriver approximately 1/8 deep into the center of the heater between the electrical leads. c. Gently turn the screwdriver to break the heater free. d. Pull the heater out by its leads, twisting if necessary.
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e. If the heater does not pull out freely, a second application of penetrating oil may be necessary. 9. Apply the anti-seize compound to the new heater and install it in the base. 10. Refit the insulating pad, retaining plate, harness clamp, ground wire, nuts, base plate, and retaining screws. 11. Install over temperature switch. 12. Pour the diffusion pump fluid (P/N 03-930639-01) through one of the holes in the 3 diffusion pumps inlet baffle. P/N 03-930639-01 contains 40cm . This is a full charge, plus an allowance for fluid that remains on the walls of the container. NOTE: Fluid is highly viscous and takes five minutes for a full charge to reach the reservoir and show in the sight glass. 13. Add fluid until the level is midway in the Full Cold zone. 14. Wipe any spillage from the inlet baffle using a clean lint free cloth. 15. Install the diffusion pump in the MS.
ATTENTION
IMPORTANT NOTE: The new heater will give off an odor during the first thirty minutes of operation. The odor results from the baking of the anti-seize lubricant, and certain compounds used in the manufacture of heaters. This is normal.
CAUTION
Be careful not to scratch or damage sealing surfaces.
3. Inspect the inlet seal. Replace if it is worn or damaged (27-402294-00). 4. Wipe the inlet seal clean with a lint free cloth, rub a thin layer of diffusion pump fluid onto the O-ring, and place the seal onto the inlet port. 5. Lift the pump into position on the manifold flange and hold. 6. From the left side of the pump, feed the inlet clamp plain end first around the inlet flange. 7. Close the clamp and loosely fasten the wing nut. 8. Rotate the pump so the exhaust port is visible through the cut out in the sheet metal. 9. Let go of the pump.
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10. Inspect the exhaust seal. Replace if it is worn or damaged (27-402536-00). 11. Wipe the exhaust seal clean with a lint free cloth, and refit to the exhaust port. 12. Lower the elbow onto the diffusion pump exhaust port.
CAUTION
Take care not to dislodge the seal.
13. Reinstall the exhaust clamp by pushing it onto the joined exhaust flanges. 14. Rotate the clamp 180 and install the screw from the left side. 15. Thread the wing nut onto the screw. 16. Rotate the clamp as far to the left as possible, while still allowing room to turn the wing nut. 17. Rotate the diffusion pump so the elbow lies as close to the manifold as possible. 18. Tighten the wing nut on the exhaust clamp. 19. Rotate the inlet clamp as far inboard as possible. 20. Tighten the wing nut on the inlet clamp. 21. Refit the left side cover and fasten in place with the four screws and two spacers. If the elbow or inlet clamp interfere with the side cover, reposition and refit the side cover. 22. Bring the MS alongside the GC and refit the transfer line. 23. Reconnect the manifold and trap heater cables. 24. Refit the top cover. 25. Carefully slide the MS up to the GC. 26. Close the vent valve by lowering the vent valve lever. 27. Turn on the MS.
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A B C
D E F
Relative positions of the manifold, diffusion pump, elbow and clamps as viewed from above.
NOTE: The manifold and elbow are shown as outlines for clarity.
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WARNING:
5. Remove the nose clip by pulling both sides away from the boot. 6. Pull the nose away from the analyzer until the entire assembly is free of the transfer-line shell. Exercise particular care if the column is still connected to the transfer line.
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A B C D E F G
H I J K L M N
O-ring Transfer Line Tip Heating Cable Slot Nose Clip Bayonet Mount Analyzer Assembly Tongue Analyzer Assembly Lock-Down Tabs
NOTE: Be sure the transfer line is retracted. Otherwise, you will not be able to remove the analyzer assembly without damaging the analyzer. To remove the analyzer assembly, proceed as follows: 1. Remove the top cover of the Saturn GC/MS by grasping both sides and lifting up. 2. Unplug the trap heater harness located near the top of the instrument. 3. On the side of the analyzer assembly (near the transfer line), push out the locking tabs on the power ribbon cable. This releases the cable. 4. Pull the ribbon cable out and move it away from the analyzer. 5. Push down and spread the two analyzer release tabs.
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NOTE: Some Saturn systems have a transfer line removal flap warning that will block the locking tabs. If such a flap is present, tip it out of the way during the procedure and return it to its original position once the analyzer is replaced. 6. Tilt the rear end up carefully to remove the analyzer. 7. Move the analyzer assembly toward the rear to free the front tab. 8. Place the analyzer upside down on a flat surface. NOTE: To prevent contamination when touching parts of the trap or the electron multiplier, wear gloves.
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A B C D E
Exit End Cap Electron Multiplier Track Multiplier Signal Pin EM Grid Electron Multiplier Mount Electron Multiplier
F G H I
Multiplier Contacts Multiplier High Voltage Pin Transfer Line Alignment Transfer Line Entrance Hole
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A B C D E
Belleville Washer Ceramic Filament Assembly Filament Connectors Post Connectors for Filament Screw Filament Assembly
F G H I J
Filament Retainer Analyzer Flange Transfer Line Alignment Tool Center Disk Feeler Disk
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CAUTION
Do not rotate the assembly more than 2 degrees. Otherwise, you may damage the contact springs.
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A B C D E F G
Screw, 6/32, 4 places Clamping Plate Exit End Cap Quartz or Silica Coated Spacer, 2 places RF Ring Electrode Filament End Cap Electron Gate Ion Trap Assembly
H I J K L M
Wave Washer Gate Conductor Trap Oven, T is located this side. Filament Assembly Filament Clip Screw
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2. After you clean a part, hold it under running water and use a clean applicator to remove the last visible traces of aluminum oxide. 3. Immediately place the clean part in a beaker containing a solution of detergent and warm water. NOTE: Do not let the slurry dry on the metal. Dried aluminum oxide is difficult to remove. 4. When you have finished cleaning all of the parts, place the beaker in an ultrasonic cleaner, and subject the beaker and its contents to ultrasound for about 1 minute. 5. Rinse each part with fresh water. 6. Using clean tools, place the parts in a beaker containing de-ionized water, then subject the beaker and its contents to ultrasound for about 1 minute. If the water is cloudy afterwards, replace the deionized water and repeat. 7. Rinse the parts with methanol. 8. Place the parts in a beaker of fresh methanol. Subject the beaker and its contents to ultrasound for about 1 minute. NOTE: Once the ion trap parts are clean, wear clean, lint-free gloves in subsequent handling of the parts to prevent contamination. Do not wear vinyl gloves. 9. Remove the ion trap parts from the beaker, and place them on a clean, lintfree surface. Allow the parts to dry in air. 10. Inspect each part to make sure that all spots and particles have been removed. If you observe any contamination, clean the part again using the procedure described above.
NOTE: You can clean any small stainless steel parts, e.g., the electron gate conductor, the gate, and wavy washer spring, by placing them along with the other stainless steel parts in methanol and subjecting them to ultrasound for 1 minute. NOTE: Check the oven trap near the filament entrance hole for carbon deposits. Carbon buildup may result in lower sensitivity and/or shorter filament lifetime. The carbon stains should be removed only with a cotton swab and methanol. After cleaning, check filament entrance hole for particles and fibers. Area must be cleaned before reassembly.
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DO NOT use Aluminum Oxide or other abrasives because this will remove the silica layer on the trap! DO NOT use harsh laboratory cleaners because this will remove the silica layer on the trap! Use only mild detergent (pH between 6 and 7.5).
NOTE: You will notice that the initial hydrocarbon background is higher than on the standard ion trap. To speed up the bakeout, you may want to bake out the ion trap overnight at 250 C. In the bakeout mode, the manifold is set to 120 C.
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NOTE: The orientation of the trap components is important. Make sure that all parts are free of particles, lint, etc. 1. Replace the gate conductor, tab-down into position. 2. Replace the wavy washer on the gate conductor. The washer orientation is not important. 3. Replace the gate so that the flat, shiny surface faces the washer. 4. Replace the filament (single-hole) electrode in the oven. 5. Replace one of the quartz spacers so that the notch faces the filament (single-hole) electrode. 6. Replace the RF electrode, followed by a quartz spacer. The notch in the quartz spacer should face up towards the exit (seven-hole) electrode. NOTE: Make sure that the notch in the quartz spacer and the notch in the exit end cap are aligned. 7. Replace the exit (seven-hole) electrode so that the notch on this electrode faces the side of the trap labeled with the side-ways T. 8. Slide the clamping plate under the screws on the top of the trap oven assembly. 9. Visually check the transfer line hole, making sure that notches in the quartz spacer and exit endcap electrode are aligned and centered in the trap oven. 10. Tighten the screws.
CAUTION
Do not rotate the assembly more than 2 degrees; otherwise, you may damage the contact springs.
2. To set transfer line hole height to the analyzer flange, place the nub of the center disk into the hole created by the notches in the quartz spacer and the exit (seven-hole) electrode, then 3. Rotate the alignment tool so that the feeler disk touches or almost touches the analyzer flange. Proper alignment is achieved when the feeler disk touches the analyzer flange and the alignment tool is perpendicular to the flange. 4. Replace the Belleville washer so that the crown side is facing upwards. NOTE: When re-installing the trap assembly, make sure that you orient the Belleville washer crownside up. Tighten the nut until the Belleville washer is flat, i.e., until the nut bottoms out.
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5. Replace and tighten the nut until it is snug. 6. Attach filament wires 1, 2, and C to the flange feed-through pins.
NOTE: Take care not to scrape or bang the analyzer parts (e.g., the trap oven assembly, electron multiplier, filament wires, etc.) against the stainless steel manifold flange. 2. With a slight forward downward tilt, check that all cables and hoses are out of the way. Slowly insert the front tongue into the slot. 3. Lower the rear of the analyzer by spreading the release tabs and pushing down gently. You should be able to install the analyzer assembly into the manifold without applying force.
4. Engage the release tabs and make sure that the release tabs are secure in their notches. 5. Connect the trap heater cable. 6. Connect the power ribbon cable and lock it into place. Ensure that the cable is firmly connected and that the locking tabs are fully engaged.
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3. Orient the assembly so that the heating cable fits inside the shell slot. 4. Rotate the nose so that the nose holes line up with the small slots in the shell. These holes will be found at the 4:00 and 10:00 positions. 5. Install the nose clip. 6. Push the nose in, rotating it clockwise to lock it in place. 7. Connect the transfer line heater cable.
6. Briefly press down on the analyzer assembly to ensure a good vacuum seal. 7. Replace the Saturn system cover.
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Overview
NOTE: The Saturn 2000 Maintenance Tutorial on CD-ROM provides viewing maintenance procedures on computer screen. Refer to GC Maintenance Section. It is important for the GC user to learn general maintenance techniques and carry these procedures out on a regular basis. Some common GC maintenance procedures are changing septa and injector inserts, checking for leaks, conditioning columns and changing filters. In this section maintenance information is presented under four headings: general GC maintenance, injector maintenance, and column maintenance. Note that many maintenance procedures, such as repair or replacement of electronic components, should be performed by a qualified Varian service representative. For maintenance problems where mechanical or electrical assemblies need to be repaired or replaced please call your local Varian service center. There are certain maintenance tasks that should be carried out on a routine basis. These regular procedures are done to ensure that the 3800/3900 Gas Chromatograph will continue to operate at optimum performance. The following is a brief summary of some common maintenance tasks and their typical frequency. Additional information on the 3800/3900 GC can be found in the Getting Started and Operators manuals: Maintenance Task
Change septa Check column nuts are tight Condition column Change injector inserts, if necessary Check gas supplies Leak check Change gas cylinders Condition system Replace gas purifiers
Frequency
Typically 50 - 100 injections Daily Daily or as required Weekly Weekly Monthly Quarterly or as required Semiannually Annually or as required
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General GC Maintenance
The common general GC maintenance tasks are checking and changing gas supply cylinders, leak checking, and changing gas purifier filters. These should be performed at the frequency suggested above. The following procedures are critical to the successful long-term operation of a Gas Chromatograph. It is very important to leak check the system on a routine basis and to ensure the quality of gas supplies, particularly the carrier gas.
Leak Check
Leak checking is one of the most important maintenance tasks that is carried out on a Gas Chromatograph. The following information refers to general leak checking procedures for the 3800 Gas Chromatograph. Specific information regarding individual 3800 components will be presented in the relevant part of this maintenance section. Leaks in the GC system can lead to poor chromatographic performance or damage components such as the analytical column. The presence of oxygen in the GC carrier gas at elevated temperatures can lead to permanent column phase degradation. While the use of an oxygen filter on the carrier supply to the instrument can help, leaks downstream of the filter are generally more likely to be the problem. The use of soap-based leak detection fluids is not recommended for a high performance capillary Gas Chromatograph due to the danger of introducing contaminants into the system. If leak detection fluids are being used they should only be used outside the Gas Chromatograph, i.e., to verify there are no leaks in the plumbing to the Gas Chromatograph. If a leak detection fluid is being used inside the Gas Chromatograph, an alcohol such as isopropanol or a 50:50 mixture of isopropanol and water should be used. Use a dropper or syringe to place a few drops of leak detection fluid on the desired fitting and monitor the area for bubble formation. The most important step in leak checking is to verify that the GC system can hold pressure. This is done by removing the column from the injector, sealing all exits from the injector and pressurizing the system. Use the following procedure to leak check 3800 injectors:
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NOTE: When conducting leak check procedures it is important to completely seal all carrier gas exits, including septum purge and split vent outlets. If more than one injector is present, then the outlets of all the injectors must be sealed. The following procedure refers to one injector but should be duplicated for every injector on the 3800. 1. Set the column oven and the injector zone temperatures to 50 C and allow them reach this temperature. This allows safe handling of injector surfaces. 2. Remove injector septum nut and install a new septum. An older septum can often be the source of a substantial leak. 3. Remove the column from the injector. Use the appropriate nut and ferrules to seal the base of the injector. For packed column systems use a 1/4 Swagelok blank off plug (16-000154-00). For capillary systems use a capillary nut (03-949551-00) with a no hole ferrule (28-694590-01). 4. If the injector is a 1079, then the septum purge and split vent outlets must be sealed. The septum purge outlets are located on the top frame surrounding the column oven, behind the column oven door. The split vent outlets are located on the left side panel of the 3800 with manual pneumatics or inside the pneumatics compartment with EFC. Seal the septum purge by removing the outlet fitting from the septum purge valve and replacing it with a blank off plug (16-000154-00). Seal the split vent outlet by installing a Swagelok union on the outlet tube and sealing it with a blank off plug. 5. With all outlet ports plugged, pressurize the system to 20 - 30 psi. This can be accomplished by adjustment of manual pneumatic controls or Electronic Flow Control. For information on setting carrier gas pressure see the Basic Operation section of the 3800 Getting Started manual. 6. Shut off the carrier supply at the source and monitor the displayed pressure at the GC for 15 minutes. The pressure should not drop more than 0.5 psi in 15 minutes. Leak checking ensures that there are no leaks in the GC system up to and including the injector assembly. If the indicated pressure on the GC drops by more than 0.5 psi during the 15-minute test period, this indicates that there is a positive leak in the system. Finding such a leak, particularly if it is a small leak, can be very difficult. In general the best approach is to systematically go through the pneumatic system from the source and tighten each fitting until the leak is eliminated. It is important to note that leaks are often found in the carrier gas supply to the GC. Locate leaks with an electronic leak detector or leak detection fluid. An electronic helium leak detector is available from Varian (01-900153-01). This device can detect helium concentration in the air as low as 2 ppm and is very effective at identifying the precise location of a helium leak from a GC system.
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their lowest possible level. For the MS detector an oxygen filter should be employed as well Varian supplies several types of carrier gas purifiers. These include a combined moisture / hydrocarbon trap, indicating moisture trap, indicating or non-indicating oxygen traps and a combined moisture / hydrocarbon / oxygen trap. While the choice of purifier depends on the individual configuration and performance expectations, the following configuration is recommended for maximum carrier gas purity and protection. The carrier gas should first pass through a hydrocarbon trap, then an indicating moisture filter, then a high capacity oxygen trap and finally through an indicating oxygen trap. As moisture reduces the effectiveness of an oxygen trap, a moisture trap should always be placed in front of an oxygen trap. When the indicating oxygen trap begins to change color, the high capacity oxygen trap should be changed immediately. The moisture trap should also be changed immediately when it changes color to prevent breakthrough of moisture to the oxygen trap. The filters supplies by Varian are mounted either on the rear panel of the instrument or on a filter stand, depending on when the instrument was purchased. Follow one of the two procedures below to replace the filter.
Part Number
03-949770-02 88-501019-00 03-949862-00 01-900007-00
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Part Number
CP17970 CP17971 CP17973
Injector Maintenance
The injector is the component of the Gas Chromatograph that requires the most frequent maintenance. This is due to the fact that the sample is deposited in the injector, thus leading to potential contamination and build up of non-volatile deposits. The most frequent injector maintenance is septum replacement. In addition insert replacement and injector cleaning are very common. As septum replacement is common to all liquid injectors on the 3800 this procedure is presented first, followed by specific maintenance procedures for the individual injectors.
Septum Replacement
The injector septum is an expendable part and must be replaced on a routine basis. The frequency of replacement depends on the number of injections and whether the injections are by hand or with an autosampler. In general the septum should be replaced every 50 - 100 injections or when symptoms of a septum leak are seen. These symptoms include changing retention times, reduced detector response or a drop in column head pressure. The latter symptom is not always valid as some injectors, such as the 1079, are pressure controlled. With a
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pressure-controlled injector, the column head pressure will remain constant even if a leak is present. Use the following procedure to change a septum on any Varian injector: 1. Cool the column oven and injector oven to 50 C. This ensures safe handling of injector parts and protects the column from elevated temperatures while it is exposed to air. 2. Turn off the carrier gas supply to the injector. 3. Remove the injector nut by turning it counterclockwise. 4. Remove the old septum using tweezers or a septum pick (72-000084-00). It is best not to handle any internal parts of the injector. 5. Install the new septum, again using tweezers to avoid contaminating the injector. 6. Replace the injector nut and tighten it finger-tight until you feel resistance from the septum, then tighten an extra 1/4 turn. Turn on the carrier gas supply. On occasion to save time you may want to change a septum while the injector is hot. Use an injector wrench (03-908423-00) to remove and reinstall the injector nut. In all instances the column oven should be cool before removing the injector nut.
1079 Injector
The 1079 is a universal capillary injector that can be operated in several modes. These modes include split, splitless, on-column and large volume injection. Typically, to change from one mode of operation to another involves changing the injector insert. The insert should also be cleaned or replaced on a routine basis. This is especially important when dirty samples are being analyzed. After prolonged use, the 1079 Universal Capillary Injector glass insert may need to be removed either: To clean the current glass insert for reinstallation in the 1079 Injector, or To replace the current glass insert with a new insert.
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Refer to the figure below when removing and/or replacing the glass insert.
1 2 3 4 5 6 7 8 9 Injector Nut Septum Septum Purge Septum Support Graphite Ferrule Carrier Gas Inlet Split Vent Glass Insert Fused Silica Column
10 Capillary Column Nut 11 Vespel Ferrule 12 Point of Injection Tools Required Tweezers or septum pick (72-000084-00) Injector nut wrench (03-908423-00) Flat-blade screwdriver (short handle) Clean laboratory tissue Graphite ferrules (03-925342-02) Insert/ferrule positioning tool (03-925385-00)
WARNING:
BURN HAZARD
The injector nut may be hot. Lower the injector temperature to 50 C and permit the injector nut to cool before proceeding.
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NOTE: If the GC is equipped with an 8200 AutoSampler, to access the injector nut, push the carrousel release button (back left) and swing the carrousel out. 2. With tweezers or septum pick, lift the edge of the septum (Item 2). Remove the septum. NOTE: Replace the injector septum each time the glass insert is replaced. 3. Use a clean flat-blade screwdriver to unscrew the septum support nut (Item 4) until it is loose. 4. Remove the septum support with the tweezers or septum pick. NOTE: Typically, when the septum support is removed, the insert and ferrule remain in the septum support. If the ferrule and insert are in the injector body after the septum support nut is removed, use the tweezers to grasp the top of the insert and lift it from the injector body. 5. Use a laboratory tissue to grasp the glass insert and remove it from the septum support nut. 6. To remove the graphite ferrule from the glass insert, use clean lab tissues to hold the graphite ferrule (Item 5) and the glass insert. Gently turn the glass insert while you pull off the graphite ferrule. NOTE: The glass inserts can be cleaned and reused. Unless the graphite ferrule is obviously damaged, it can be reused as well. However, replace the 5 mm graphite ferrule after the glass insert has been changed three or four times.
Septum Support Insert Ferrule
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2. Position the tool as shown above on a flat, clean surface. Use clean laboratory tissue on the surface. Tighten the septum support finger-tight. Holding the tool with a 5/8 wrench, give the septum support an extra 1/3 to 1/2 turn past finger-tight. Now unscrew the septum support, which now has the ferrule and insert seated in it. If there is any graphite extruded past bottom of the septum support, cut it off with a blade or sharp knife. Carefully wipe off any graphite flakes, which may adhere to the insert or septum support. Gripping the septum support unit with a piece of laboratory tissue, carefully put this unit in the 1079 injector and tighten the septum support 1/6turn past finger-tight. 3. Use tweezers to place a new septum over the septum support. NOTE: If the septum has a Teflon face, place the Teflon face toward the column (down). 4. Place the injector nut on the injector and tighten by hand until you feel some resistance, then tighten an extra 1/4 turn using the injector nut wrench. NOTE: After the injector nut has been replaced, check the split vent and septum purge flow rates to ensure these values have not changed. 5. Condition the insert by setting the 1079 Injector to the split mode and purging with carrier gas for 30 min at 300 C.
WARNING:
BURN HAZARD
Use care when removing inserts from the injector. Inserts can be at high temperatures and are likely hot. Place hot inserts on a clean glass or metal surface only.
2. To clean glass inserts, use one of the following procedures (the choice of cleaning procedure depends upon the nature of samples injected): 3. Rinse the inserts with solvent or soak the inserts in hot acid. 4. Heat them in a glass-annealing oven (to 500 C) or pass the inserts through the flame of a Bunsen burner. 5. Wash in a 1:1:1 mixture of methanol:methylene chloride:hexane in an ultrasonic cleaner for 30-60 min, then dry the inserts in an oven. NOTE: For the 2 mm glass wool packed glass insert, remove the glass wool by blowing compressed gas in the end of the insert. Clean the insert following one of the procedures listed above. Repack the insert with deactivated glass wool (10-20 mg). Leave 1.5 cm of the bottom of the glass insert unpacked. The capillary column will be inserted in this empty space when re-installed in the injector body.
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NOTE: Rinsing the glass inserts with strong acids or bases or heating to a high temperature will remove the deactivation coating on the glass inserts. Rinsing the glass inserts with solvents or mixed solvents will not remove the deactivation coating.
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WARNING:
FIRE HAZARD
Use proper eye and skin protection. Methanol and acetone are toxic and flammable chemicals. Exercise appropriate precautions when these chemicals are used.
4. Remove the injector nut, septum, and septum support, with ferrule and insert attached. 5. Moisten a cotton swab and a stick with methanol and gently swab center of the injector body. 6. Moisten a cotton swab on a stick with iso-octane and gently swab the center of the injector body. 7. Examine the end of the fused silica column to ensure that it has not been damaged. Slide the end of the fused silica column into the opening of the injector. 8. Gently twist the column nut in the opposite direction used to tighten the nut. Place the column nut on the end of the injector and tighten the nut. This procedure minimizes twisting the column. 9. Use the 5/16 open-end wrench and tighten with 1/6-turn to secure the column in place. 10. Replace the septum support, insert, ferrule, septum, and injector nut. 11. To check whether the injector is leak-tight, connect a flow meter to the split vent. Set the Relay to the split mode. If the flow meter indicates a flow less than previously measured, the injector has a leak. 12. Turn the column oven back on by pressing the TURN OVEN ON softkey in the column oven section of the method.
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NOTE: Avoid contamination of the transfer line, injector, and capillary column by using clean tools and wearing clean lint-free Nylon gloves. As you remove parts, place them on a clean, lint-free, unpainted surface. 4. Use the alignment tool and a 5/16-in. wrench to loosen the brass nut on the end of the transfer line. 5. Remove the capillary column from the transfer line. 6. Remove the brass nut, along with the ferrule, from the column. 7. Remove the ferrule from the nut. Discard the ferrule. 8. From inside the GC oven, pull the transfer line end of the column back into the hole in the side of the GC. Leave the free end of the column on the floor of the oven.
To withdraw the transfer line from the vacuum manifold, proceed as follows: 1. Unplug the transfer line heating cable. 2. Grasp the nose of the transfer line, then rotate counterclockwise as you press lightly toward the manifold. Gently slide the transfer line away from the manifold. 3. Remove the nose clip, and then pull the transfer line away from the analyzer. 4. Wrap the transfer line in clean aluminum foil and place it on a clean, dry surface. 5. Cover the analyzer opening with aluminum foil. To remove the capillary column from the GC injector, proceed as follows: 1. Use a 5/16-in. wrench to loosen the capillary column nut that secures the column to the injector. 2. Carefully remove the nut, ferrule, and column from the injector. 3. Slide the column nut, along with the ferrule, off the end of the column. 4. Remove the ferrule from the column nut. Discard the ferrule. 5. Carefully lift the column support cage, along with the column, from the column hanger. Then, remove the support cage and column from the oven. 6. Seal the end of the column or insert the ends of the column into a septum. 7. Store the column and the support cage.
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4. Place a new graphite/Vespel ferrule on the column, with the taper facing the nut. Slide the ferrule, along with the nut, about 30 cm (12 in.) down the column. 5. Carefully insert the tip of the column into the nose end of the transfer line. 6. Slide the column all the way through the transfer line until the tip of the column projects a few inches beyond the transfer line tip. 7. Using a sapphire-, or carbide-tipped scribing tool or ceramic scoring wafer, score the column once lightly about 2 cm (1 in.) from its end. 8. Bend the column slightly to break it at the mark. The column should break cleanly. 9. Using a Kimwipe tissue dipped in methanol, carefully wipe the last 15 cm (6.0 in.) of the column. 10. Be sure to wipe toward the end of the column so that the Kimwipe tissue fibers do not enter the opening at the column end. 11. Position the column in the transfer line as follows. 12. To position the column in the transfer line, proceed as follows: 13. Install the brass nut on the end of the transfer line, but do not tighten the nut completely. 14. Keep an eye on the tip of the column and position it so that about 1 mm (1/32 in.) of the column projects from the transfer line tip. NOTE: As you tighten the nut, the position of the column in the transfer line may change. If this happens, loosen the nut and readjust the column until about 1 mm (1/32 in.) of the column projects from the transfer line tip. 15. Grasping the transfer line securely with the alignment tool, use a 5/16-in. wrench to tighten the brass nut. Tighten the nut until snug, but do not over tighten. 16. Rotate the transfer line so that the heater cable projects downward. 17. To install the transfer line in the manifold, proceed as follows referring to the Transfer Line Exploded View. 18. Position the transfer line in the manifold, and install the clip into the holes and slots.
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19. Gently push the transfer line toward the manifold, and rotate the collar in the clockwise direction until the bayonet lock engages. 20. Reconnect the transfer line heating cable to the mass spectrometer. 21. Gently push the mass spectrometer toward the GC, until the transfer line boot fits snugly over the collar on the side of the GC oven. The capillary column nut should be visible inside the GC column oven. 22. The MS is properly engaged when the bumpers on the left side of the spectrometer achieve full contact with the right side of the GC. 23. Replace the cover on the mass spectrometer.
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Troubleshooting
Checking the GC
The simplest and most effective way of isolating a GC problem is to run a test sample. Running a sample will allow you to check several operational and performance factors, including the carrier gas supply, chromatographic characteristics, and sample-related problems. The test sample that is most frequently run is the COLTEST mixture. This multicomponent mixture is very well suited to troubleshooting injector and column problems. Please see How to Run the COLTEST Sample for a description of the use of this test mixture. To identify the source of a GC electronics problem, press the STATUS key and a CONTROL key (i.e., injector, column oven, etc.) to determine if a fault is present. If a fault is present the message FAULTED appears. You should also consult the 3800 GC manuals for information about fixing GC faults. Make sure that you are thoroughly familiar with all safety issues before you attempt to repair any electronics component.
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Troubleshooting
There are two procedures for isolating problems associated with the Mass Spectrometer. Running the Auto Tune routine from System Control will provide you with information about system performance. Running the diagnostics program will initiate a hardware test. These tests may be used to isolate simple ion trap problems, e.g., air leaks, burned-out filaments, high contamination levels, etc. NOTE: If diagnostics fail, once the problem is corrected, the Reset button must be clicked before further testing. In certain cases, you may need to physically separate the GC and MS to isolate an ion-trap problem. In these cases, remove the column from the injector, and plug its end with a septum. This will minimize the input of air. Maintain the column and transfer line at ambient temperature to prevent degradation of the stationary phase. You do not need to vent the MS vacuum system to complete this procedure. If you wish to further isolate the mass spectrometer, you must remove the column from the ion trap by shutting down the system and capping the transfer line with a no-hole ferrule.
Before you begin troubleshooting, however, be sure that you have baked out Saturn for at least 2 hours. Run Diagnostics to determine if any hardware problems are present. If you have done this, and the missing-spectrum problem persists, continue as follows. These steps apply if either air/water or cal gas peaks are missing.
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3. If you are unsure of appropriate levels, then reset parameters by clicking on the Defaults button in each section. Save your method file as Default. Activate Default file, turn on trap and Cal gas. Check for cal gas spectrum.
4. If the spectrum returns, note which parameter(s) were causing the problem. If no spectrum is present, and the trap was recently disassembled, the assembly of the trap must be checked.
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2. If the axial modulation readback is near zero, there maybe a scratch on the trap oven, which is shorting out one of the endcaps. Shutdown the system, remove the trap oven, and use an ohm meter to check for continuity between the electrodes and ground. Use the screws holding the clamping plate as ground. If this test is done without removing the trap from the electronics assembly, there will be continuity to ground. 3. Check whether there is a problem with the electron multiplier, proceeding as follows: a. Under Monitor States, click on Multiplier. Under Acquisition System check that the electron multiplier voltage is the same or close to the value displayed in the SetPoints box in the Auto Tune section.
b. If the electron multiplier voltage in the Diagnostics is only a few volts, the multiplier is shorted to ground. Shut down the system, and replace the electron multiplier or call a Varian Customer Support Representative.
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NOTE: If, after performing these tests, you are still unable to isolate the cause of the problem, contact your Varian Customer Support Representative.
Before you begin troubleshooting, however, be sure that Saturn has baked out for at least 2 hours, and that the manifold temperature is at or below 50 C. If you have done this, and the problem persists, continue as follows. 1. Check for an air leak in Auto Tune Section. 2. Check RF ramp Adjustment 3. Reduce trap temperature to 150 C. 4. Enter Method editor, check method contains EI AGC ionization mode, and Default values for other parameters. NOTE: If, after performing these tests, you are still unable to isolate the cause of the problem, contact your Varian Customer Support Representative.
Before you begin troubleshooting, however, be sure that Saturn has baked out for at least 2 hours. If you have done this, and the problem persists, continue as follows.
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3. Adjust the RF ramp by turning the RF tuning screw on the front panel. Adjust to minimize the highest reading.
What To Do If the Resolution is Poor But the Air and Water Levels are Acceptable
If the peaks are broader than you would have expected, you should investigate the following possible causes: There are too many ions in the trap (i.e., contamination or high column bleed). The axial modulation value is too high or too low. Axial modulation is not functioning properly.
Before you begin troubleshooting, however, be sure that Saturn has baked out for at least 2 hours. If you have done this, and the problem persists, continue as follows.
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Troubleshooting
If the baseline ramps up, shut down Saturn, then carefully clean the electrode surfaces with a lint-free cloth.
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What To Do If the Trap Function Calibration Fails After the Calibration Ions Have Been Correctly Identified
If the trap function calibration fails after the calibration ions have been correctly identified, you should investigate the following possible causes: The electron multiplier voltage is too low. The cal gas pressure is too low.
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CAUTION
Often, major air leaks are accompanied by a hissing sound. These leaks may be due to extremely loose fittings, improperly seated O-rings, or open valves. If you suspect a major leak, do not turn on the electron multiplier, RF voltage, or filament. Using the Diagnostics section, confirm that the turbomolecular pump is operating at 100% speed or diffusion pump is ready. If it is not, you may be sure there is a major air leak.
4. Enter System Control: Click on Auto Tune Box Click on Air/Water Check Click on Start Auto Tune
If the peaks at masses 32 (O2+), 28 (N2+), and 18 (H2O+) are severely broadened or undifferentiated, your system has a large air leak. Immediately turn off Air/Water Check.
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Troubleshooting
Air/water Spectrum from a System with a Very High Water Vapor Background
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Air/water Spectrum from a System with Excess Water Vapor and a Relatively Small Air Leak
If the ratio of the height of the peak of mass 18 (H2O ) to mass 19 (H3O ) is about 10:1, there is little water vapor in your system. If the ratio of peak height of mass 18 to mass 19 is less than 10:1 but greater than 5:1, additional bakeout maybe necessary. Be aware, however, that if you do not eliminate the water vapor, your systems sensitivity and performance may be less than optimal. If the ratio of the peak height of mass 18 to mass 19 is much less than 10:1, your system contains excess water vapor.
An Air/Water Spectrum Obtained from a System with No Significant Air Leaks and Little Water Vapor as Indicated by:
The peak at mass 18 (H2O ) may be the base (highest) peak. This is dependent on the level of water vapor. The ratio of the peak height at mass 18 (H2O ) to that at mass 19 (H3O ) is greater than or equal to 10:1. The 100% counts value is significantly lower than 500. The ratio of the peak height at mass 28 to that at mass 32 (O2 ) is about 4:1.
+ + +
6. If there are no air or water leaks in your system, you should obtain the following approximate values. Please note that these values are only typical, so the actual values may vary from system to system.
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Troubleshooting
TIC <1000
An Air/Water Spectrum Obtained from a System with a Small Air Leak and Little Water Vapor as Indicated by:
The peak height at mass 28 is noticeably greater than that at mass 18. The ratio of the peak height at mass 28 to that at mass 32 is greater than 4:1. The 100% scale counts value has increased to greater than 500. The ratio of the peak height at mass 18 to that at mass 19 is greater than or equal to 10:1.
An Air/Water Spectrum Obtained from a System with a Moderate Air Leak and Little Water Vapor as Indicated by:
The peak at 28 starts to overload. The 100% counts value may be several thousand counts. The peak height at mass 18 is greater than that at mass 19.
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Troubleshooting
An Air/Water Spectrum Obtained from a System with a Large Air Leak and Little Water Vapor as Indicated by:
The peak at mass 32 is the base (highest) peak. The peaks at masses 18, 19, and 28 are broadened. As a leak increases, all peaks broaden and eventually become undifferentiated.
You will often observe high water backgrounds after venting the system, and especially after cleaning the trap. Several hours of bakeout may be required for the water vapor to desorb from surfaces in the vacuum system, and for the water level to drop to a stable level. Never operate your Saturn if the mass 18 and 19 peaks are the same height (or if the air/water check shows NO). After the system has baked out sufficiently (i.e. overnight), the presence of excess water is due to contamination in the carrier gas tank or an air leak. Saturated filters on the GC may produce an increase in the air/water background. Replace the filters at regular intervals, and whenever moisture or other background from the GC becomes a problem.
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Troubleshooting
be sure to wait until all GC zones are cool before beginning. If the leak is coming from the transfer line connection, you will have to shutdown the GC/MS system and vent the system before fixing it. NOTE: Set the mass range from 35 to 50 if you will be using an argon leakdetection gas, or from 80 to 110 if you will be using a Freon leak-detection gas. Troubleshoot leaks using argon gas as a leak detecting gas. The mass peak of interest for argon is at Mass 40. To reduce the risk of damaging the filaments or multiplier, develop a method file with the following parameters: Set the electron multiplier 100 V below the 10 setting. Turn off AGC and set the ion time to 100 sec. Set the filament emission current to 10 A. Set scan range from m/z of 35 to 50 (or 80 to 110)
5
Enter system control, activate the argon method for troubleshooting and turn the trap ON. NOTE: Do not spray argon indiscriminately around the fittings. Argon diffuses very rapidly from the fitting you are testing toward a true leak. This could lead you to mistakenly identify the fitting that you are testing as the leak source. Check for leaks: Spray a fine stream of argon on the transfer line closest to the analyzer. Examine the monitor for a response. If a peak at mass 40 does not appear, there is no leak. If a peak appears at mass 40, there is a leak. The transfer line O-ring may have particles on its surface. Shut down the system and check the O-ring.
Check the following gaskets and fittings for leaks, one item at a time and in the following order. (Tighten the fittings and/or flanges as needed. Wait a few seconds between subsequent applications of argon.) Calibration gas tube fitting on the pneumatics manifold Vent valve fitting on the manifold Top vacuum manifold flange
The release tabs of the analyzer are not locked into position.
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Troubleshooting
The brass nut on the transfer line is not tight enough, recheck the system. Do not over tighten the fittings. Otherwise, you may generate an even larger leak. If you cannot eliminate the leak, vent the system, and check the O-ring on the manifold and transfer line for particles. Wipe off both O-rings with lint-free paper. The turbomolecular pump will probably fail to achieve its 100% speed if there is a leak or poor seal at the turbo/manifold interface. Never attempt to operate the system under these conditions.
Check GC Connections:
NOTE: Check the GC Maintenance Section for additional information for trouble shooting leaks. To identify and correct a leak at the connections between the capillary column and the injector or transfer line, proceed as follows: Make sure that you are using ferrules of the correct size, i.e., 0.4 mm for 0.25-mm ID columns, and 0.5 mm for 0.32-mm ID columns. Make sure that the ferrule on the transfer line is a graphite/Vespel mixture. Most transfer line connection leaks occur on the high vacuum side (e.g., around the transfer line O-ring).
In the case of a graphite/Vespel ferrule, tighten each ferrule one-half turn beyond finger tightness. In the case of a graphite ferrule, tighten each ferrule threequarters of a turn beyond finger tight. Leaks at the septum may arise from loose injector nuts or overuse of the septum. Regularly change the septum as part of your routine GC preventive maintenance program. To reduce the level of air bleeding into the system and any background from the septum material, use good quality, low bleed septa. Air leaks in the GC pneumatics are the most difficult leaks to detect and eliminate because detection gases are not particularly effective for this purpose. In general, you should tighten all fittings, and then check for such a leak using a solvent such as methanol. Saturated filters on the GC may produce an increase in the air/water background. Replace the filters at regular intervals and whenever moisture or other background from the GC becomes a problem.
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Troubleshooting
If you are using Split/Splitless injection, proceed as follows: 1. Use an isothermal temperature of 260 C. 2. Set up the following external event program conditions: NOTE: Gas saver event, if present, must be ON.
Time 0.00 0.50 Event 1 On Off Injector Mode Splitless Split
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Troubleshooting
The following is a typical chromatogram for this test mixture. Note that 2,6dimethylphenol and 2-ethylhexanoic acid coelute normally on a DB-5 column, depending on column and injector.
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Troubleshooting
The following figure demonstrates the resolving power of Saturn for coeluting compounds.
You can also effectively separate the individual components in the mixture for subsequent data manipulation, e.g., library searches and quantitation. For details about plotting single ion chromatograms for ions specific to a single compound, please refer to the SaturnView help or section in the Software Reference manual.
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Troubleshooting
Solution
Reinstall the column in the injector. Check the column seal with the insert in the SPI/1079 (on-column). Make sure you have a good cut on the column by examining the column under magnification. Check the 1077/1078/1079 injector for insertion depth. Reduce the injection speed for the hot injectors. If possible, reduce the injector temperature. If you are using sandwich injection, reduce the solvent plug to 0.5 L. A typical setting for the SPI is 20 C below the solvent boiling point. The column temperature is set at the solvent boiling point. Hold the column at this temperature until SPI has finished heating (usually about 2 min). Check that the septum purge flow is 0.5 mL/min for a SPI with a 10-psi head pressure, 2 mL/min for a 1077 or 1078 and 3.5-4.5 mL/min for 1079 with a 10-psi head pressure. If necessary, change the septum purge frit or adjust the valve setting (depending on your injector configuration). For a splitless injection, the vent flow should be at least 70 mL/min. The injector should be switched to the split mode 30 to 90 sec after the injection.
Solvent flashing in hot injector (usually 1077, 1078 or 1079) Incorrect temperature control using programmable SPI or 1079. Septum purge line is plugged
Solution
Change or clean the injector insert. If necessary, silanize it. Remove the front 15 cm of the column and reinstall it. If the retention times are changing, or if cutting the column does not fix the problem, replace the column.
Correction of Low Response and Severe Tailing with High Boiling Point Compounds
Symptom
Injector not hot enough to vaporize high boilers High levels of column bleed masking component peaks High levels of silicone or other contamination are coated on the ion trap surfaces Insufficient vaporization of the higher boiling point components Trap temperature is too low
Solution
Increase the temperature of the injector Condition the column at 30 C below its maximum operating temperature (320 C for DB-5). Switch to a high temperature column, (e.g., the SGE HT5), if conditioning does not help. Clean the ion trap as outlined in Maintenance Section. Check Contamination Table for listing of potential contamination. Lower the injector temperature and the injection speed. Check that the graphite ferrule in the 1077 or 1078 is free of cracks, and that the septum support is tight. Increase the trap temperature in increments of 20 C.
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Troubleshooting
Solution
Dilute the sample, or perform a split injection. Change the column. Increase the carrier flow rate.
Solution
Modify the method (e.g., slow the column ramp rate) to improve the separation Decrease the carrier gas linear velocity to improve the resolution. Use a more polar column.
Peaks are not well separated, e.g., 2,6-dimethylphenol and 2-ethylhexanoic acid in the COLTEST mixture.
Solution
Visually check that the syringe is pulling up the sample. Check that the nut is tight. Flush the syringe with solvent. Heating the solvent in a hot injector may help if the syringe is plugged; otherwise, replace the syringe. Replace the septum regularly and ensure that the septum nut is tight. Check the installation of the column in the injector. Tighten the capillary column nut. Change the injector insert. Remove the front 15 cm of the column, or replace the column. Increase the injector temperature (1077,1078 or 1079). Or increase the maximum temperature to which the injector is programmed (SPI or 1079). Confirm that the switch time is chromatographically optimized.
Leak at the septum Improper installation of column in the injector, or a leak at the column inlet Sample is being absorbed by active surfaces in the injector or column Incomplete vaporization of sample in the injector 1077,1078 or 1079 splits too soon
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Troubleshooting
Solution
Lower the injection temperature, or use a SPI/1079 programmed injection. Increase the initial column hold time until SPI/1079 reaches its maximum temperature, (i.e., typically at 2 min.). Re-cut and install the column. Replace the insert and septum.
Solution
Use high-temperature, low-bleed septa. Make sure that the septum purge flow is set to 0.5 mL/min for a SPI injector with a 10-psi head pressure, or 2 mL/min for a 1077 or 1078 injector with a 10-psi head pressure. Confirm that this is indeed the case by running a solvent blank with a new syringe. Use certified sample vials, and keep the samples refrigerated. Check contamination table. Install or replace the carrier gas filters. Remove the column from the injector and bake it out at elevated temperature, (e.g., 350 C) using a purge of at least 20 mL/min. Confirm that this is indeed the case by running a blank or standard. Switch to a new septum type, lower the injection temperature, or reduce the injection volume. Use high purity grade solvents.
Impurities from the carrier gas present Injector or GC pneumatics contaminated Impurities present in the sample Solvents are extracting impurities from the septum. Impurities present in syringe wash solvent
Solution
Check the pneumatics for leaks. If necessary, replace the flow controller/ regulator. Condition or replace the column. Replace the septum at regular intervals. Check that the septum nut and capillary column nut are tight.
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Troubleshooting
150
Troubleshooting
Overview
This section describes symptoms that the user may observe during startup and routine operation.
Shutdown Page
1. Foreline pressure exceeds 5000 mTorr (Large Air Leak) a. Check the GC column is not broken. b. Check the foreline hose between the diffusion pump and foreline pump for cracks or collapsed sections. c. Check all the vacuum seals: diffusion pump, elbow, foreline pump, etc. d. Check for large air leaks. Refer to troubleshooting sections on leaks. e. Check the level and condition of the foreline pump oil. f. Contact Varian Customer Support Representative.
2. Foreline pressure exceeds 500 mTorr (Moderate Air Leak) a. Check the GC column is not broken. b. Check the CI valve is OFF using the Instrument Control Page.
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c.
d. Check the fluid level in the diffusion pump. e. Check the level and condition of foreline pump oil. f. Check the foreline hose between the diffusion pump and foreline pump for cracks or collapsed sections.
g. Check all the vacuum seals: diffusion pump, elbow, foreline pump, etc. h. If a foreline trap is used, replace the pellets. i. j. k. l. Replace the thermocouple gauge. Contact Varian Customer Support Representative. TEC Failure Check cable connections. Connectors and pins are differentiated by size.
m. Contact Varian Customer Support Representative. 3. Peltier Baffle Fan Failure a. Check the fan on the rear panel. b. Contact your Varian Customer Support Representative. 4. Thermocouple Gauge Failure c. Check the cable connections. d. Open filament. Gauge must be replaced. e. Contact Varian Customer Support Representative. 5. Diffusion Pump Overheated a. Check the pump is plugged into the diffusion pump controller. b. Ensure left side cover is in place. Side panel of GC is in place. c. Check the fan. d. Contact Varian Customer Support Representative. 6. Diffusion Pump Heater Failure a. Check pump is plugged into diffusion pump controller. b. Replace heaters to diffusion pump. c. Contact Varian Customer Support Representative.
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d. Check the fluid level and condition of the foreline pump, if its time for maintenance, change the oil. e. If a foreline trap is used, replace the pellets. f. Check all the vacuum seals: diffusion pump, elbow, foreline pump, etc. The diffusion pump seals may leak if the clamp is not tight or because the seals are worn or damage. Worn or damaged seals must be replaced.
g. Contact your Varian Customer Support Representative. 2. CI Gas Settings (must be checked in Diagnostics) a. Pressure Readings should not exceed 350 mTorr. Confirm CI reagent gas head pressure at gas cylinder is set at 5 psi. 3. Diffusion Pump Overheated a. Overheating causes the diffusion pump to turn OFF. Switch the power OFF for 15 minutes. then, switch it ON to reset the diffusion pump. b. Check the ambient temperature of the laboratory does not exceed 35 C. c. Check fluid in the diffusion pump. d. Ensure all baffling is in place. e. Check the fan. f. Check to make sure left side cover is in place. g. Contact Varian Customer Support Representative. 4. High background levels (low ionization time) in the mass spectra may be the result of contamination in the ion trap, GC and/or the diffusion pump. If numerous samples have been analyzed, the high background maybe the result of trap contamination, and the trap components must be cleaned. If the ion trap components have been cleaned and the system has been baked out, the high background levels in the mass spectra maybe the result of contamination in the GC and/or the diffusion pump. Comparison of mass spectra at high and low GC column and injector temperatures may help to identify source. a. Reduce GC column and injector temperature to 100 C or lower and acquire a 2-minute mass spectral data file. b. Increase GC column and injector temperature (~250 C) and acquire 2minute mass spectral data file. c. Identify the most intense mass peaks for both runs, and/or subtract spectra.
d. Use the following table to identify the most likely source(s) of contamination. e. Call your Varian Customer Support Representative.
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Compound
H2O, N2, O2, CO2 PFTBA Methanol Acetone Dimethylpolysiloxane Diffusion Pump Fluid
Possible Source
Air Leak Leaking Calibration Valve Cleaning Solvent Cleaning Solvent Septum or methyl silicone column coating Diffusion Pump Fluid
Vacuum seals damaged by high temperature. Solvent Bottle Contamination Foreline pump oil, fingerprints, saturated trap pellets Pump oil degassing contamination Pump oil degassing contamination
Groups of peaks spaced 14 u apart 77, 141, 169, 204 146, 148, 111
NOTE: Numbers in bold denote masses more useful for identifying contaminants.
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Other Documents
Other documents that you may wish to consult regarding Saturn operation include the following: Software Reference, 03-914979-00 Saturn GC/MS Workstation Tutorials, 03-914988-00 Pre-Installation Instructions, 03-914629-00 Release Notes, 03-914767-00 Upgrade Notes, 03-914768-00
Site Requirements
Site Preparation
The Saturn GC/MS has been designed to operate reliably under carefully controlled environmental conditions. It is the responsibility of the purchaser to provide a suitable location, a power source of acceptable quality, and a suitable operating environment. Operating a system or maintaining it in operational condition outside of the power and operating environment limits listed below could cause failures of many types. The repair of such failures is specifically excluded from the standard warranty and service contract coverage. For additional information, please request specific pre-installation support directly through your local Varian Sales/Service Center.
Power
You are responsible for providing two dedicated fourplex single-phase power sources with earth grounds hard-wired to the main power panel ground. Within North America these power sources must be 20A, 100-130 Vac, 60 Hz 3 Hz, and outside North America they must be 10A, 200-260 Vac, 50 Hz 3 Hz. One of these fourplex power sources is for the mass spectrometer, computer, monitor; and printer the other fourplex power source is for the gas chromatograph and (optional) AutoSampler. If you have additional sample preparation devices or test
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equipment, we recommend a separate dedicated power source for their operation. NOTE: Do not use the free outlet for equipment that draws more than 2 amps.
NOTE: Avoid using power supplies from sources that may be subject to RF interference, such as electric motors and elevators. Care must be taken to ensure that sources of radio frequency interference (RFI) and electromagnetic interference (EMI) are not placed on the same power line, or share the same ground plane, since this can degrade the performance of the GC. Equipment such as motors, solenoids, fluorescent light fixtures, and radio communication transmitters should be isolated from the instrument and connecting cables as much as possible. The power cable from the GC is approximately 2m (6 ft) long and fitted with National Electronics Manufacturers Association (NEMA) 5-20P power plugs. The NEMA 5-20P power plug and corresponding outlet are shown in Figure (a). NEMA 5-20P plugs are rated at 20A and 120 Vac. The power cable from the mass spectrometer is approximately 2.5m (8 ft) long and fitted with US Standard National Electronics Manufacturers Association (NEMA) 5-15P power plugs. The NEMA 5-15P power plug and corresponding outlet are shown in Figure (b). NEMA 5-15P plugs are rated at 15A and 120 Vac. Systems shipped outside the United States and Canada are fitted with CEE 7/7 plugs; these are rated at 16A and 230 Vac. The CEE 7/7 plug and outlet are shown in Figure (c). The power cables for the computer, monitor, and printer are approximately 2m (6 ft) long. They are fitted with NEMA 5-15P plugs. The power cable from the 8200 AutoSampler is about 2m (6 ft) long, and is fitted with a NEMA 5-15P plug rated at 120V.
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NEMA 5-20P, NEMA 5-15P, and CEE 7/7 Power Plugs and Outlets
With a 120V power source, the maximum amperage requirements for each of the Saturn GC/MS components are as follows: Component
Mass Spectrometer Gas Chromatograph Varian 8200 AutoSampler Computer Monitor Laser Printer
Amperes
12 20 0.5 3 2 3-4
NOTE: With a 230V power source, the maximum amperage requirement of each of the above components is one-half of the amperage given above. Never plug the mass spectrometer and the gas chromatograph into the same power source; otherwise, you may overload the fourplex power source. The Interconnect Diagram for Saturn is a diagram for the six power cables from Saturn. Never use the free outlet on each of the power sources for equipment that draws more than 2A.
Quality of Power
The quality of the power supplied to your Saturn is very important. The power must be 100-130 Vac, 60 Hz 3 Hz (200-260 Vac, 50 Hz 3 Hz), and it must be stable. It must be free of fluctuations due to slow changes in the average voltage or to changes resulting from surges, sags, or transients. Slow average changes are gradual, long-term changes in the average root mean square (RMS) voltage level, with typical durations greater than 2 seconds. Sags and surges are sudden changes in average RMS voltage level, with typical durations between 50 sec and 2 seconds.
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Transients (or impulses) are brief voltage excursions of up to several thousand volts with durations of less than 50 sec.
Constant high line voltage or surges in voltage can produce overheating and component failures. Constant low line voltage or sags in voltage may cause the system to function erratically or to even cease functioning. Transients, even of a few microseconds duration, may cause electronic devices to fail catastrophically or degrade sufficiently to significantly shorten their lives. Therefore, it is important to establish the quality of the line power in your laboratory before you install your Saturn.
Operating Environment
It is your responsibility to provide an acceptable operating environment. Attention paid to the operating environment will ensure continued high performance of your Saturn GC/MS. Expenditures for air conditioning will be more than offset by good sample throughput and a reduction in repair costs.
Temperature
The laboratory temperature must be held between 15 and 30 C (59 and 86 F) for the turbomolecular pump system and 15 to 35 C for the diffusion pump system. The optimum operating temperature is between 18 and 21 C (65 and 70 F). NOTE: As the laboratory temperature increases, system reliability decreases. All electronic components generate heat while operating. This heat must be dissipated to the surrounding air if the components are to operate reliably. The turbomolecular pumps temperature cutoff protects the bearing and prolongs its lifetime. If the laboratory temperature is significantly above 30 C (86 C), the pump cutoff temperature could be reached, and this would result in the pump being shutdown. There must be a good flow of air around the system, and the air conditioning must be capable of maintaining a constant temperature (within operational limits) in the immediate vicinity of the system. The average steady-state heat load of the Saturn GC/MS is 6000 BTUs, with a possible short-term heat dissipation of 15000 BTUs during startup. If a 3600 GC is used, heat dissipation increases by about 1200 BTUs.
Humidity
The relative humidity of the operating environment must be between 40 and 80%, with no condensation. Operating a Saturn GC/MS at very low humidity will result in the accumulation and discharge of static electricity; this will shorten the life of electronic components. Operating the system at high humidity will produce condensation and result in short circuits. High humidity will also block the filters on cooling fans and accelerate wear of the heads in the diskette drives. Varian recommends that your laboratory be equipped with a temperature/humidity monitor. This will ensure that your laboratory is always in conformance with temperature and humidity specifications.
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Exhaust System
It is your responsibility to provide an adequate exhaust system. Much of what is introduced into the mass spectrometer will eventually be exhausted from the mechanical pump, along with the small amounts of oil vapor that these pumps characteristically emit. Therefore, the pump outlets should be connected to a fume exhaust system. Consult local regulations for the proper method of exhausting the fumes from your system.
Gas Requirements
Helium - GC Carrier Gas
Minimum 99.998% ultra-high purity, with less than 1.0 ppm each of water, oxygen, and total hydrocarbons. One 257-ft3 tank with Matheson regulator #3104-580, or equivalent tank and regulator. NOTE: The presence of >1 ppm oxygen or water in the carrier gas supply may significantly affect the performance of Saturn, and it damage such components as the capillary column, filaments, and multiplier. Varian recommends that its customers verify that their gas suppliers use controlled tanks; this will ensure that purity standards are maintained. If you purchase pure gases in contaminated tanks, you may end up with a contaminated system requiring costly and time consuming repair.
Cryogenics
Systems equipped with SPI/1079 injectors or column oven cryogenics require one of the following: Liquid CO2 at 850-1000 psig Liquid N2 at 20-50 psig
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If you are not sure which one of these cryogenic options you ordered, check your purchase order.
Other Gases
If you ordered an 8200 AutoSampler or automated valves, an independent supply of air or N2 at 40-60 psig may be required.
160
3. Open the vent valve lever on the front of the mass spectrometer for ten minutes. 4. Keep an eye on the capillary column inside the GC as you gently slide the mass spectrometer away from the GC. Be sure not to bend or kink the capillary column. 5. Use the alignment tool to prevent the transfer line from turning while you loosen the brass capillary nut connecting the column to the transfer line. 6. Cap the transfer line with a capillary nut and no-hole ferrule. 7. Place the capillary column and nut inside the GC oven. This will protect them from damage. 8. Turn off the carrier gas, then disconnect the helium gas line that is connected to the GC filter. 9. Cap the filters with Swagelok plugs or caps. 10. Move the Saturn GC/MS to its new location. Be sure the new location satisfies the power and environmental requirements.
Description
PWA, IEEE INTERFACE, PCI IEEE Cable PWA, POWER BOARD PWA, RF GENERATOR Cable, SAP to PWR 26 pins (Ribbon) Cable, SAP to PWR 64 pins (Ribbon) Replacement Spares Kit Assembly, Analyzer Flange Assembly, Transfer Line (115V) Assembly, Transfer Line (230V) Cable, Transfer Line heater (115V) Cable, Transfer Line heater (230V) Assembly, Vacuum Manifold (115V) Assembly, Vacuum Manifold (230V) Assembly, Ion Gauge Cable, Trap Heater (115V) Cable, Trap Heater (230V)
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Trap Components
NOTE: The Silica Coated Spacers have a shiny, mirror like finish on the inside surface. Part Number
03-930552-01 03-930551-01 14-920009-00 03-930315-01 03-930535-01 03-930108-01 03-930601-91 14-998238-00 03-930657-01 03-930657-02 03-936549-01 03-930591-91 03-930500-01 03-930524-01 03-930535-02 13-122008-00 14-998228-00 03-930539-01 03-930109-04 12-222006-06 03-930109-03 03-930109-14 03-930109-18
Description
Gate Conductor Gate Wavy Washer Assembly, Multiplier Spacer, Quartz Transfer Line Wrench/Analyzer Alignment Tool Assembly, Filament disk with wires Belleville Washer, Small Screw, Long Screw, Short Filament Clip Tip. Transfer Line (Ultra Clean) Trap Oven Clamping Plate Quartz Spacer, Silica Coated Nut, 11/32" Belleville Washer, Large Thermo Well Thermo Well O-ring Trap Oven screw 6-32 X 3/8 O-ring, 1.112 ID Transfer Line Quad-ring, Viton Manifold Quad-ring, Viton Transfer Line
Description
Mechanical Pump, 90 L/min, 115/230V, Varian Screen, Turbo Pump (V-70) Cable, Turbo Controller to turbo Turbo Controller 7 Length Tygon Tubing Turbo Molecular Pump (V-70) Mechanical Vacuum Pump Oil O-ring, Turbo Pump to Manifold
162
Description
Chassis Fan, Electronics Side Chassis Fan, Pump Side Plastic Nut O-ring, Elbow O-ring, Diffusion Pump Inlet O-ring, Diffusion Pump Exhaust O-ring, Peltier Baffle PWA Diffusion Pump Controller Thermocouple Gauge Diffusion Pump AX65 (90V 250W) Includes 40 cc Fluid Diffusion Pump AX65 (165V 250W) Includes 40 cc Fluid Diffusion Pump Heater (90V 250W) Includes 40 cc Fluid Diffusion Pump Heater (165V 250W) Includes 40 cc Fluid Diffusion Pump Fluid - 40cc - Santovac 5 Peltier Baffle Assembly Assembly, Vacuum Manifold DP (120V) Assembly, Vacuum Manifold DP (230V)
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GC Spares
Part Number
03-917742-00 03-925367-31 03-925367-33 03-918332-01 03-949551-00 28-694580-01 28-694581-01 03-920357-02 03-925342-02 03-925350-00 03-918466-00 03-925331-00 03-918464-00 03-926119-27 03-926119-37 03-926119-25 03-926119-38 03-926119-24 03-926116-82 03-925989-02 03-926117-64 03-926119-30
Description
Serial I/O PWA PWA, CPU, IBDH, 3400 SOC PWA, CPU, IBDH, 3600 SOC Insert, SPI, High Performance, Glass Nut, Capillary Injector Ferrule, 0.4 mm ID X 1/16, pkg. 10 Ferrule, 0.5 mm ID X 1/16, pkg. 10 Septa, HT, ThermoGreen 11.5 mm (50/can) 1078/1079 5 mm Glass Insert Ferrule 1078/1079 2 mm ID Packed Insert 1078/1079 2 mm ID Open Insert 1078/1079 0.5 mm ID Open Insert 1078/1079 3.4 mm ID Open Insert 1177 4 mm ID Unpacked Single Gooseneck Insert (5/pk) 1177 4 mm ID Wool Plug Open Insert (5/pk) 1177 4 mm ID Unpacked Open Glass Insert (5/pk) 1177 2 mm ID Wool Plug Open Glass Insert (5/pk) 1177 2 mm ID Unpacked Open Glass Insert (5/pk) 1177 High Temperature Septa (100/pk) 1177 Thermogreen Septa (5/pk) 1177 Viton O-ring Seal (100/pk) 1177 Graphite Seal (100/pk)
Description
FC-43, Reservoir (Cal Gas Bulb) Col Test Sample HCB Sample, 100 pg/L Sensitivity Sample EI/CI HCB, Benzophenone, Tetrachlorobenzene 2,10,500 Aluminum Oxide, 600 Grit Benzophenone Test Sample (50 pg) GC/MS Calibration Compound, FC-43 Fuse, 5 x 20 mm, 0.5A Applicator, Cotton Tipped, pkg. 100
164
Description
Saturn GC/MS Workstation Hardware Maintenance Manual Saturn GC/MS Workstation Software Reference Manual Saturn GC/MS Workstation Tutorials Manual Solenoid, 3-way, Cal Gas Needle Valve, Cal Gas Oil Mist Eliminator ChromatoProbe Kit
CI Parts/Spares
Part Number
03-930102-02 03-930597-01 03-930596-01 03-930101-01 03-930022-91 03-930-106-01
Description
Solenoid, 2-way, CI Restrictor, long, CI Restrictor, short, CI Needle Valve, CI Gas Liquid CI Inlet Kit CI Solenoid, 2-way, Chemrez
Description
Manifold, Multi, CI Inlet Valve, Solenoid, 2 Way, Buna-N Valve, Needle Plate, Clamping, Bottom, Multi CI Plate, Clamping, Top, Multi CI Fitting. Plug Fitting. Tube, Barb Beswick Fitting, Elbow Beswick Fitting, 1/8 inch, Viton Ferrule, Viton Enclosure, Multi CI (cover) View Plate, Enclosure, Multi CI Screw, Captive, 6-32 Reservoir, Bulb Restrictor, Tube, Top Restrictor, Tube, Bottom Screw, 6-32 x 1 1/4, SS
03-914978-00:1
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Part Number
12-222006-08 12-222006-05 28-158923-00 28-849918-00 03-930870-02 03-930109-10 03-930109-17 03-930071-00 03-930068-01 03-930076-01
Description
Screw, 6-32 x 1/2, SS Screw, 6-32 x 5/16 Tubing, Vacuum Fitting, Tee, Barb Cap, Polypro, 1/8 inch O-ring, 2-104 O-ring, 2-108 Cover, Connector, Harness Assembly, Harness, Solenoids, Multi CI Label
Description
Plug, Pin For plugging 1/8 inch ports on MCI when channel not connected to liquid or gas.
03-930109-10 03-930109-17 28-694638-00 28-694639-00 28-695138-00 03-920270-00 03-949870-04 89-988956-00 03-930129-01 03-930073-01
O-ring, 2-104, Buna-N Replacement O-rings for 1/8-inch ports. O-ring, 2-108, Buna-N Replacement O-rings for inch ports. Ferrule, Teflon, rear Replacement ferrules for gas adapter. Ferrule, Teflon, front Gas Tube Adapters To connect gases to MCI module through 1/8-inch ports. Reservoir, Bulb Liquid reagent vials Cap, Plug Vial caps for storage of reagent vials. Syringe, 5 mL, Luer Syringe for adding reagent liquids to reagent vials. Assembly, Luer Teflon needle for syringe Stand, Reservoir For storage, filling of reservoir bulbs.
Description
OSI Restrictor Assembly, OSI, Subassembly Kit, OSI Parts, Field Service Nut, OSI, GC 1/16 X 1.2 mm
166
If you are having problems with the gas chromatograph, please be prepared to provide the following information: GC model AutoSampler model, if any Type of injector you are using Cryogenics Information about your GC column, (i.e., the manufacturer, bonded phase, film thickness, and ID and length)
If you are having problems with your computer and/or software, please be prepared to provide the following information: Computer manufacturer and model Windows version Mouse driver version Printer manufacturer and model Network configuration Printouts of your Autoexec.bat and Config.sys files Saturn software version
In addition, you should observe the following guidelines when describing the problem to the Customer Support Representative: Tell the service representative which part of the software, (e.g., System Control, Manual or Acquisition, you were using when the problem occurred). Tell the service representative which troubleshooting routines you have used.
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