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.
Page 3
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 P9672055
Mass Spectrometer
Model:
Saturn 2000 Series
Authorized Representative in the EU
Print Name: G. A. Wassink
Signed:
Position: Quality Manager
Date: October 16, 2001
Company Name:
Address:
Telephone:
Fax:
Varian B.V.
Herculesweg 8
P.O. Box 8033
4330 EA Middelburg
The Netherlands
+31(0) 118 671 000
+31(0) 118 633 118
Print Name: Martin O’Donoghue
Signed:
Position: General Manager
Date: October 16, 2001
03-914535-12:7
SPEC. 03-914411-00 1:2:3:4n
Manufacturer
Company Name:
Address:
Telephone:
Fax:
Varian, Inc.
2700 Mitchell Drive
Walnut Creek, California 94598
USA
925-939-2400
925-945-2168
Page 4
Quality Systems At Varian, Inc.
The ISO 9000 series standards were created in Geneva in 1987 to cut through a morass of conflicting
quality definitions. These standards define a model for quality assurance systems in product design,
development, manufacturing, installation, service, and customer support. They are now the worldwide quality
assurance benchmark used to gauge the strength of a company's commitment to quality, and the value of its
quality systems.
Various organizations around the world, such as the British Standards Institution (BSI), provide
certified, objective auditors to scrutinize quality procedures, product development, manufacturing processes,
and customer satisfaction programs. No company can claim ISO 9000 series registration unless it receives a
stamp of approval from the demanding quality assessors of BSI or similar accredited examining body. ISO
9000 series registration constitutes an objective third-party report to determine the level of a supplier's
commitment to quality.
In 1992, Varian, Inc., Analytical Instruments became registered to the most comprehensive of the ISO
9000 series standards — ISO 9001. ISO 9001 registration means that every stage of our quality system,
including product development, manufacturing, final test, shipping, and parts and supplies has been
rigorously examined against the most exacting set of internationally recognized standards. It means we live
up to a standard of quality that you can count on today, and into the future. Our Quality System has received
ISO 9001 certification number FM21797.
The quality systems that earned us ISO 9001 registration have direct benefits for our customers:
♦ We can speed instruments to you faster than ever before. Emergency orders can
be processed even faster.
♦ We fill your orders promptly and completely.
♦ We have implemented a system of continuous feedback from our customers —
we are aware of your needs today and tomorrow.
♦ We have improved your productivity by cutting systems failure rates in half and
speeding service response time.
♦ We have embedded continuous improvement into the fabric of our organization
so that we can achieve even higher levels of quality in the future.
♦ We are embedding GLP requirements into our products and services to help you
meet your regulatory compliance requirements.
ISO 9001 registration is not enough. For us, quality is defined by our customers. We are not satisfied
unless you are satisfied. We are striving to understand customer needs, using independent surveys, user
groups, customer advisory boards, and our “Hallmark of Quality” response program, in addition to individual
face-to-face customer contact. Our products and our processes are configured to meet those needs.
We know that you are seeking more than the most advanced processes and top-notch applications expertise.
You want to join forces with a partner committed to delivering world-class quality, reliability, and value —
on time, every time.
Our overriding aim is to be that partner.
03-914451-00:41 of 1
Page 5
Qualitätssysteme bei Varian, Inc.
Die Standards der ISO 9000 Serien wurden 1987 in Genf mit dem Ziel geschaffen, das Durcheinander gegensätzlicher Qualitätsbestimmungen zu entwirren. Diese Standards legen ein Modell für
Qualitätssicherungssysteme hinsichtlich Produktdesign, Entwicklung, Herstellung, Installation, Service
und Kundenbetreuung fest. Sie sind nun die weltweiten Maßstäbe der Qualitätssicherung, die die Anstrengungen eines Unternehmens bezüglich der Qualität und der Bedeutung seiner Qualitätssysteme messen.
Verschiedene Organisationen in der ganzen Welt, wie die British Standards Institution (BSI), stellen ausgebildete, objektive Prüfer zur Begutachtung von Qualitätsmaßnahmen, Produktentwicklung, Herstellungsprozessen und von Programmen zur Erforschung der Kundenzufriedenheit zur Verfügung. Kein
Unternehmen kann die ISO 9000 Registrierung beantragen, ohne die Genehmigung von den beauftragten
Qualitätsgutachtern der BSI oder einer ähnlichen akkreditierten Stelle erhalten zu haben. Die ISO 9000
Registrierung bildet einen objektiven Bericht von dritter Seite, um den Grad der Qualitätsanstrengung
eines Lieferanten zu bestimmen.
1992 wurden die Varian, Inc., Analytical Instruments nach den umfassendsten Standards der ISO
9000 Serie registriert — ISO 9001. Die ISO 9001 Registrierung bedeutet, daß jedes Stadium unseres
Qualitätssystems, einschließlich Produktentwicklung, Herstellung, Endkontrolle, Versand, sowie Teile
und Zubehör rigoros gegen die anspruchsvollste Serie international anerkannter Standards geprüft worden
ist. Das bedeutet, daß wir einen Qualitätsstandard bieten, auf den Sie heute und in Zukunft rechnen können. Unser Qualitätssystem hat die ISO 9001 Zertifikatnummer FM21797 erhalten.
Die Qualitätssysteme der ISO 9001 Registrierung haben für unsere Kunden direkte Vorteile:
♦ Wir können Instrumente schneller denn je zu Ihnen schicken. Eilbestellungen werden
noch schneller durchgeführt.
♦ Wir erfüllen Ihre Bestellungen pünktlich und vollständig.
♦ Wir haben ein System kontinuierlichen Informationsrückflusses von unseren Kunden auf-
gebaut—wir kennen Ihre Anforderungen von heute und von morgen.
♦ Wir haben Ihre Produktivität durch Halbierung der Systemfehlerraten und durch Verkür-
zung unserer Reaktionszeit im Service verbessert.
♦ Wir haben kontinuierliche Verbesserungen in unserer Organisationsstruktur verankert, so
daß wir künftig eine noch höhere Qualität erreichen können.
♦ Wir haben die GLP Anforderungen in unsere Produkte und Dienstleistungen eingeführt,
um Ihnen bei der Erfüllung Ihres behördlichen Abnahmeprotokolls zu helfen.
Die ISO 9001 Registrierung ist nicht genug. Für uns wird Qualität durch unsere Kunden definiert. Wir sind nicht zufrieden, wenn Sie es nicht auch sind. Wir bemühen uns, die Anforderungen unserer Kunden durch unabhängige Untersuchungen, Anwendergruppen, Kundenberatungsgremien und unser Antwortprogramm “Gütesiegel der Qualität” zu verstehen, zusätzlich zu persönlichen Kundenkontakten. Unsere Produkte und unsere Prozesse sind so gestaltet, daß sie diese Anforderungen erfüllen.
Wir wissen, daß Sie mehr als fortschrittliche Prozesse und ausgezeichnetes Anwendungswissen
suchen. Sie suchen einen Partner, der Qualität von Weltklasse, Verläßlichkeit und Nutzen für Sie
liefert— pünktlich und jederzeit.
Unser oberstes Ziel ist, für Sie dieser Partner zu sein.
03-914451-81:4 1 von 1
Page 6
Systèmes de qualité chez Varian, Inc.
Les normes ISO série 9000 ont été créées à Genève, en 1987, pour remédier à la confusion dans la
définition des normes de qualité. Ces normes définissent un modèle de contrôle de qualité dans le domaine de
la conception produit, du développement, de la production, des installations, des services et du support client.
Elles constituent à présent la référence mondiale en matière de contrôle de qualité utilisée aux fins d'évaluation
du niveau d'engagement d'une entreprise dans ce domaine et la valeur de ses systèmes de qualité.
Plusieurs organisations de par le monde, telle la British Standards Institution (BSI) offrent les services
d'auditeurs qualifiés et objectifs, chargés d'examiner les procédures de qualité, le développement de produit,
les procédés de fabrication et les programmes de satisfaction du client.
Aucune société ne peut se prévaloir de l'homologation ISO 9000, sans avoir reçu l'approbation des
évaluateurs rigoureux de la BSI ou d'un organisme accréditif similaire. L'homologation ISO 9000 constitue
une évaluation objective d'un tiers afin de déterminer le niveau d'engagement d'un fournisseur dans le domaine
de la qualité.
En 1992, Varian, Analytical Instruments a reçu l'homologation ISO 9001, normes des plus complètes
de la série IS0 9000. En d'autres termes, chaque étape du processus de qualité, notamment le développement
produit, la fabrication, le test final, l'expédition et les fournitures de pièces a étés oumis à un contrôle
rigoureux par rapport à des normes extrêmement strictes, reconnues au niveau international. Nous sommes
donc à même de vous garantir et de maintenir un niveau de qualité. Lesdites procédures ont reçu
l'homologation ISO 9001 numéro FM21797.
Les systèmes de qualité qui ont reçu l'homologation ISO 9001 présentent des avantages directs pour
nos clients :
♦ Nous sommes en mesure de vous livrer les instruments et de traiter les commandes en urgence
dans des délais record.
♦ Nous répondons pleinement et de manière rapide à vos commandes.
♦ Nous avons mis en place un système de feedback continu de la part de nos clients et sommes
conscients de vos attentes présentes et futures.
♦ Nous avons amélioré votre productivité en réduisant de moitié les Temps de panne et en accélérant
les temps de réponse.
♦ Nous avons apporté des améliorations constantes au sein de notre structure, afin d'atteindre des
niveaux de qualité optima, à l'avenir.
♦ Nos produits et services reflètent les exigences BPL pour vous permettre de répondre aux
impératifs de respect de la règlementation.
Toutefois, nous ne nous contentons pas de l'homologation ISO 9001. Pour nous, la qualité est définie
par nos clients. Nous ne sommes satisfaits que lorsque nos clients le sont. Nous nous efforçons de comprendre
vos besoins, à l'aide d'évaluations externes, de groupes d'utilisateurs, de comités de conseil clients, et de notre
programme “Hallmark of Quality”, outre les contacts directs que nous établissons avec chacun de nos clients.
Nos produits et nos procédés sont conçus pour répondre à vos attentes.
Nous n'ignorons pas que vous recherchez plus que des processus évolués et un savoir-faire d'exception
dans le domaine des applications. Vous souhaitez conjuguer vos forces avec un partenaire s'étant engagé à
offrir une qualité, une fiabilité et une valeur optimales, au moment où il faut et quand il faut.
Notre principal objectif : devenir votre partenaire !
03-914451-82:41 of 1
Page 7
I sistemi di qualità della Varian, Inc.
La serie degli standard ISO 9000 è stata presentata nel 1987 a Ginevra con lo scopo di mettere ordine
in un groviglio di definizioni contrastanti sulla qualità. Tali standard definiscono un modello che assicura la
qualità nella progettazione, nello sviluppo, nella fabbricazione, nell'installazione e nella manutenzione dei
prodotti nonché nel servizio assistenza clienti. Oggi come oggi essi costituiscono il punto di riferimento, a
livello mondiale, ai fini della valutazione dell'impegno delle diverse aziende sul fronte della qualità e della
validità dei sistemi di qualità da esse adottati.
Diverse organizzazioni internazionali, come la British Standard Institution (BSI), dispongono
d'ispettori certificati e imparziali per la valutazione delle procedure di qualità, dello sviluppo dei prodotti, dei
processi di fabbricazione e dei programmi di soddisfazione del cliente. Nessuna azienda può asserire d'essere
in possesso della certificazione ISO 9000 finché non dispone del marchio d'approvazione concesso dai
rigorosi ispettori di qualità della BSI o di altri enti di controllo riconosciuti. La certificazione di conformità
agli standard ISO 9000 costituisce un'attestazione imparziale di terzi del grado d'impegno di una determinata
azienda nei confronti della qualità.
Nel 1992 la Varian, Inc., Analytical Instruments ha ottenuto l'omologazione allo standard più
completo della serie ISO 9000, l'ISO 9001. L'omologazione ISO 9001 significa che ogni singola fase del
nostro sistema di qualità - compresi lo sviluppo del prodotto, la fabbricazione, le prove finali, la spedizione, i
componenti e le forniture - è stata rigorosamente esaminata a fronte della serie più esigente di standard
riconosciuti a livello mondiale, il che significa che rispondiamo pienamente ad uno standard qualitativo sul
quale il cliente può contare oggi come nel futuro. Il nostro Sistema di Qualità ha ottenuto la certificazione ISO
9001 col numero FM21797.
I sistemi di qualità per i quali abbiamo ottenuto l'omologazione ISO 9001 comportano dei vantaggi
diretti per i nostri clienti, ovvero:
♦ Siamo in grado di consegnare gli strumenti più rapidamente rispetto al passato, con la possibilità
di evadere le richieste d'emergenza con una rapidità ancora maggiore.
♦ Gli ordini vengono evasi tempestivamente ed in modo completo.
♦ Abbiamo messo a punto un sistema di riscontro costante con la clientela, in modo da poter essere
sempre perfettamente informati sulle esigenze attuali e future del cliente.
♦ Abbiamo migliorato la produttività del cliente riducendo della metà il tasso di guasti dei sistemi e
velocizzando i tempi d'intervento della manutenzione.
♦ Abbiamo introdotto un costante miglioramento nella nostra struttura organizzativa in modo da
poter conseguire in futuro livelli qualitativi ancor più elevati.
♦ Stiamo adeguando i nostri prodotti e servizi agli standard GLP per poter aiutare i clienti a
soddisfare i requisiti di conformità posti loro dagli enti normativi.
Ma l'omologazione ISO 9001 non è tutto. Per quanto ci riguarda, la qualità viene definita dai nostri
clienti: noi siamo soddisfatti solo se lo è il cliente. Ci adoperiamo al massimo per comprendere le esigenze del
cliente, ricorrendo ad indagini di società private, gruppi di utenti, associazioni di consumatori e con il nostro
programma di risposta Hallmark of Quality - il marchio di garanzia di qualità - oltre che col contatto diretto
coi singoli clienti. I nostri prodotti ed i nostri processi sono configurati per rispondere a tali esigenze.
Sappiamo che a Voi i processi più avanzati e l'esperienza delle applicazioni di prim'ordine non
bastano. Sappiamo che intendete unire le vostre forze con quelle d'un partner impegnato a fornire livelli
qualitativi internazionali, affidabilità e valore, in modo tempestivo e costante.
Quel partner vogliamo essere noi.
03-914451-83:41 of 1
Page 8
Sistemas de calidad en Varian, Inc.
Las normas ISO 9000 fueron creadas en Ginebra en 1987 para acabar con una multitud de
definiciones de calidad contradictorias. Estas normas constituyen un modelo de sistemas de garantía de
calidad en el diseño, desarrollo, fabricación, instalación, mantenimiento y asistencia técnica de productos. Se
han convertido en el banco de pruebas de garantía de calidad a nivel mundial y miden el grado de
compromiso de una empresa con la calidad, así como el alcance de sus sistemas de calidad.
Diversas organizaciones mundiales, como la British Standards Institution (BSI), proporcionan
expertos titulados de probada objetividad para investigar procedimientos de calidad, desarrollo de productos,
procesos de fabricación y programas de servicio al cliente.
Varian, Inc., Analytical Instruments fue registrada en 1992 con la norma más exhaustiva de la serie
ISO 9000: la ISO 9001. La certificación por la norma ISO 9001 significa que todas las etapas de nuestro
sistema de calidad, como el desarrollo del producto, la fabricación, las pruebas finales, la expedición, así
como los suministros y recambios, han sido examinados rigurosamente respecto a las normas más exigentes
reconocidas internacionalmente. Significa que nos comprometemos a mantener un nivel de calidad con el que
podrá siempre contar, hoy y en el futuro. Il nostro Sistema di Qualità ha ottenuto la certificazione ISO 9001
col numero FM21797.
Los sistemas de calidad que nos valieron la certificación ISO 9001 representan beneficios directos
para nuestros clientes:
♦ haremos llegar nuestros aparatos más rápidamente que nunca. Podemos cumplir con pedidos
urgentes aún más deprisa.
♦ Atenderemos sus pedidos de forma rápida y completa.
♦ Aplicamos un sistema de retorno de información permanente con nuestros clientes: siempre
somos conscientes de sus necesidades, actuales o futuras.
♦ Hemos mejorado la productividad de nuestros clientes, disminuyendo el índice de defectos a la
mitad y acortando el tiempo de respuesta del servicio de mantenimiento.
♦ Hemos integrado sistemas de mejora continuada en nuestra organización, de forma que podremos
obtener niveles de calidad aún superiores en un futuro.
♦ Estamos integrando los requerimientos GLP en nuestros productos y servicios para ayudarle a
cumplir con requerimientos de conformidad obligatorios.
La conformidad con ISO 9001 no nos basta. Para nosotros, los criterios de calidad los definen
nuestros clientes. No estaremos satisfechos hasta que usted lo esté. Intentamos comprender las necesidades de
nuestros clientes, a través de entidades independientes, grupos de usuarios, oficinas de asesoramiento a
usuarios y nuestro programa de respuesta “Hallmark of Quality”, además de los contactos directos con
nuestros clientes. Nuestros productos y procedimientos están diseñados para poder corresponder a sus
necesidades.
Sabemos que nuestros clientes buscan más que experiencia en procesos avanzados y aplicaciones
punteras. Se trata de unir fuerzas con un socio que se compromete a entregar calidad reconocida a nivel
mundial, fiabilidad y valor, a tiempo, siempre.
Nuestra meta principal es ser ese socio.
03-914451-84:41 of 1
Page 9
Varian, Inc. Analytical Instrument Warranty
Hardware Products
All analytical instruments sold by Varian, Inc. are
warranted to be free from defects in material and
workmanship for the periods specified and in
accordance with the terms on the face of Varian's
quotation or as otherwise agreed upon in writing
between Varian and the Customer. The warranty
period begins on the date of shipment from Varian to
the original Customer. However, where installation is
paid for by the Customer or included in the purchase
price, the warranty period begins upon completion of
installation. If the Customer schedules installation to
start later than 30 days after delivery or if such delay
is caused through the Customer's inability to provide
adequate facilities or utilities or through failure to
comply with Varian's reasonable pre-installation
instructions or through other omissions by Customer,
then the warranty period starts on the 31st day from
date of shipment. Moreover Varian will charge the
Customer for labor and other expenses involved in
making multiple or follow-up installation service calls.
Software Products
Where software is provided within the frame of a
license agreement concluded between the Customer
and Varian, any warranty shall be strictly in
accordance with the terms of such agreement.
In the absence of a license agreement and unless an
alternate warranty period is agreed upon in writing
between Varian and the Customer, the warranty
period is as specified on the face of Varian's
quotation. Varian warrants such software products, if
used with and properly installed on Varian hardware
or other hardware as specified by Varian to perform
as described in the accompanying Operator's Manual
and to be substantially free of those defects which
cause failure to execute respective programming
instructions; however, Varian does not warrant
uninterrupted or error-free operation.
Remedies
The sole and exclusive remedy under hardware
warranty shall be repair of instrument malfunctions
which in Varian's opinion are due or traceable to
defects in original materials or workmanship or, at
Varian's option, replacement of the respective
defective parts, provided that Varian may as an
alternative elect to refund an equitable portion of the
purchase price of the instrument or accessory.
Repair or replacement under warranty does not
extend the original warranty period.
Repair or replacement under warranty claims shall be
made in Varian's sole discretion either by sending a
Customer Support Representative to the site or by
authorizing the Customer to return the defective
accessory or instrument to Varian or to send it to a
designated service facility. The Customer shall be
responsible for loss or damage in transit and shall
prepay shipping cost. Varian will return the accessory
or instrument to the Customer prepaid and insured.
Claims for loss or damage in transit shall be filed by
the Customer. To correct software operation
anomalies, Varian will issue software revisions where
such revisions exist and where, in Varian's opinion,
this is the most efficient remedy.
Limitation of Warranty
This warranty does not cover software supplied by
the Customer, equipment and software warranted by
another manufacturer or replacement of expendable
items and those of limited life, such as but not limited
to: Filters, glassware, instrument status lamps, source
lamps, septa, columns, fuses, chart paper and ink,
nebulizers, flow cells, pistons, seals, fittings, valves,
burners, sample tubes, probe inserts, print heads,
glass lined tubing, pipe and tube fittings, variable
temperature dewars, transfer lines, flexible discs,
magnetic tape cassettes, electron multipliers,
filaments, vacuum gaskets, seats and all parts
exposed to samples and mobile phases.
This warranty shall be void in the event of accident,
abuse, alteration, misuse, neglect, breakage,
improper operation or maintenance, unauthorized or
improper modifications or tampering, use in an
unsuitable physical environment, use with a marginal
power supply or use with other inadequate facilities or
utilities. Reasonable care must be used to avoid
hazards.
This warranty is expressly in lieu of and excludes
all other express or implied warranties, including
but not limited to warranties of merchantability
and of fitness for particular purpose, use or
application, and all other obligations or liabilities
on the part of Varian, unless such other
warranties, obligations or liabilities are expressly
agreed to in writing by Varian.
Limitation of Remedies and Liability
The remedies provided herein are the sole and
exclusive remedies of the Customer. In no case
will Varian be liable for incidental or
consequential damages, loss of use, loss of
production or any other loss incurred.
03-914412-00:2
1 of 1
Page 10
Varian, Inc. Analytical Instrument Garantie
Hardwareprodukte
Es wird garantiert, daß alle von Varian, Inc. verkauften
analytischen Instrumente für die angegebene Zeitdauer
und in Übereinstimmung mit den „Allgemeinen Lieferbedingungen“ oder anderen schriftlichen Zusagen
zwischen Varian und dem Kunden frei von Material- und
Herstellungsfehlern sind. Die Garantiezeit beginnt mit
dem Versanddatum von Varian zum Originalkunden.
Wenn die Installation vom Kunden bezahlt oder im Verkaufspreis eingeschlossen ist, beginnt die Garantiezeit
nach der abgeschlossenen Installation. Wenn der
Kunde den Installationsbeginn später als 30 Tage
nach erfolgter Lieferung ansetzt, oder wenn die
Verzögerung dadurch verursacht wird, daß der Kunde
nicht den ausreichenden Platz oder die Versorgungseinrichtungen beschafft oder Varian's
berechtigte Anweisungen zur Installationsvorbereitung
nicht einhält oder andere Versäumnisse des Kunden
vorliegen, dann beginnt die Garantiezeit am 31. Tag
nach dem Versanddatum. Darüber hinaus wird Varian
dem Kunden den Arbeitsaufwand und andere Unkosten
durch mehrfache oder fortgesetzte Installationsanforderungen berechnen.
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 für solche Softwareprodukte, die mit Varian’s Hardware benutzt und
richtig installiert sind oder zur Ausführung mit anderer
von Varian angegebener Hardware, wie sie in der beigefügten Bedienungsanleitung beschrieben ist, daß sie im
wesentlichen frei von solchen Defekten sind, die Fehler
bei der Ausführung der jeweiligen Programmieranweisungen verursachen; Varian garantiert jedoch keine
ununterbrochene oder fehlerfreie Arbeitsweise.
Abhilfen
Die einzige und ausschließliche Abhilfe in der Hardwaregarantie wird die Reparatur der Instrumentstörungen
sein, die sich nach Varian's Ansicht auf Defekte in den
Originalteilen oder bei der Herstellung zurückführen läßt
oder, nach Varian's Wahl, der Austausch der entsprechenden defekten Teile oder die Erstattung eines fairen
Teils des Kaufpreises des Instruments oder Zubehörs,
vorausgesetzt, daß sich Varian alternativ dafür entscheidet.
Reparatur oder Austausch unter Garantie verlängert
nicht die ursprüngliche Garantiezeit.
Reparatur oder Austausch unter Garantieansprüchen
soll in Varian's ausschließlichem Ermessen entweder
durch einen Serviceingenieur beim Kunden oder durch
Ermächtigung des Kunden zum Einschicken des defekten Zubehörs oder Instruments an Varian oder einen
Servicestützpunkt erfolgen. Der Kunde übernimmt die
Verantwortung für Verlust oder Beschädigung im Transit
und hat die Versandkosten im voraus zu bezahlen. Varian wird das Zubehör oder Instrument vorausbezahlt und
versichert zum Kunden zurückschicken. Ansprüche für
Verlust oder Beschädigung im Transit hat der Kunde zu
erheben. Zur Korrektur von Anomalien des Softwarebetriebs wird Varian Software-Neuausgaben ausgeben, sofern Revisionen existieren und dies die beste
Abhilfe ist.
Garantieeinschränkungen
Diese Garantie erfaßt nicht vom Kunden bereitgestellte
Software, Ausrüstungen und Software, die von anderen
Herstellern garantiert werden oder den Austausch entbehrlicher Teile und solcher von begrenzter Lebensdauer wie diese, aber nicht darauf beschränkt: Filter,
Glaswaren, Instrument Statuslampen, Lampenquellen,
Septen, Säulen, Sicherungen, Schreiberpapier und
Tinte, Zerstäuber, Flußzellen, Kolben, Dichtungen, Fittings, Ventile, Brenner, Probenröhrchen, Sondeneinsätze, Druckköpfe, glasausgekleidetes Rohr, Leitungsund Rohrfittings, Dewars für variable Temperaturen,
Transferleitungen, flexible Disketten, Magnetbandkassetten, elektronische Vervielfacher, Hitzdrähte, Vakuum
Gaskets, Sitzflächen und alle Teile, die den Proben und
mobilen Phasen ausgesetzt sind.
Diese Garantie erlischt bei eingetretenem Unfall, falscher Benutzung, Umbau, Mißbrauch, Vernachlässigung, 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 ungenügenden Einrichtungen oder Versorgungen. Mit vernünftiger Sorgfalt
müssen Gefahren vermieden werden.
Diese Garantie steht ausdrücklich anstelle von allen
anderen angedeuteten Garantien und schließt sie
aus, einschließlich, aber nicht beschränkt auf Garantien der Verkäuflichkeit und Eignung für einen besonderen Zweck, Gebrauch oder Anwendung und
allen anderen Verpflichtungen oder Haftungen von
Varian’s Seite, wenn nicht solche Garantien,
Verpflichtungen oder Haftungen ausdrücklich
schriftlich mit Varian vereinbart wurden.
Beschränkung der Hilfen und Haftung
Die hier gegebenen Hilfen sind einzig und allein Sache des Kunden. In keinem Fall wird Varian für
versehentliche oder sich ergebende Schäden wie
Nutzungsverlust, Produktionsverlust oder jeden anderen Verlust haften.
03-914412-81:2
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Page 11
Garantie des instruments d'analyse Varian, Inc.
Matériel
Les instruments d'analyse vendus par Varian, Inc. sont
garantis exempts de défauts de matière et de
fabrication, pour les périodes spécifiées et
conformément aux conditions mentionnées sur le recto
du devis ou aux termes de tout autre accord écrit
intervenu entre Varian et le client. La période de
garantie commence à compter de la date de livraison
de Varian au client d'origine. Cependant, lorsque le
client a acquitté les frais d'installation ou que celle-ci est
inclue dans le prix d'achat, la période de garantie
commence à compter de l'achèvement de l'installation.
Si le client prévoit le début de l'installation au-delà de
30 jours après la livraison ou si ledit retard est dû à
l'inaptitude du client à mettre à disposition les
installations ou services ou au non respect des
instructions de pré-installation de Varian ou à la suite
desdites négligences du client, la période de garantie
commence le 31ème jour à compter de la date de
livraison. De plus, Varian fera supporter au client tout
frais de main d'oeuvre et autres coûts résultant de
multiples appels téléphoniques aux fins de suivi de
l'installation.
Logiciel
Pour tout logiciel faisant l'objet d'un accord de licence
conclu entre le client et Varian, la garantie sera
strictement limitée aux termes dudit accord.
En l'absence d'accord de licence et sauf accord écrit
sur tout autre période de garantie entre Varian et le
client, la période de garantie est telle que spécifiée sur
le recto du devis de Varian. Sous réserve de leur
installation et de leur utilisation correcte sur le matériel
Varian ou tout autre matériel, tel que spécifié, Varian
garantie le fonctionnement tel que décrit dans le manuel
d'utilisation fourni avec le matériel et l'absence de
défauts entraînant l'impossibilité d'exécuter des
instructions de programmation respectives. Toutefois,
Varian ne garantit pas un fonctionnement sans
interruption et sans erreurs.
Recours
Le seul et unique recours relatif à la garantie du
matériel se limite à la réparation suite à un mauvais
fonctionnement de l'instrument, qui, de l'avis de Varian,
est dû à des défauts des pièces d'origine ou de la
fabrication, ou, à la discrétion de Varian, au
remplacement des pièces défectueuses en question,
sous réserve du choix de Varian de rembourser une
part raisonnable du prix d'achat de l'instrument ou de
l'accessoire.
La répaation ou le remplacement sous garantie n'étend
pas la période de garantie originale.
La réparation ou le remplacement, aux termes d'un
recours, est laissé à l'entière discrétion de Varian, soit
par l'envoi d'un technicien de maintenance sur le site du
client, soit en autorisant le client à retourner l'accessoire
ou l'instrument défectueux à Varian, voire à l'envoyer à
un service de maintenance désigné.
Le client assumera la responsabilité de toute perte ou
sinistre lors du transport et règlera à l'avance les frais
de transport. Varian renverra l'accessoire ou
l'instrument au client en port payé et assuré. Toute
réclamation résultant d'une perte ou d'un sinistre
intervenu lors du transport devra être faite par le client.
Aux fins de correction des anomalies de fonctionnement
du logiciel, Varian diffusera des mises à jour des
logiciels, le cas échéant, et si de l'avis de Varian, elles
constituent la mesure corrective la plus appropriée en la
matière.
Limitation de garantie
Cette garantie ne couvre pas le logiciel fourni par le
Client, les équipements ou logiciels garantis par un
autre fabricant ni le remplacement des pièces
consommables ou présentant une durée de vie limitée,
notamment : filtres, verres, indicateurs d'état de
l'instrument, lampes source, septa, colonnes, fusibles,
papier graphique et encre, nébuliseurs cellules, pistons,
joints, raccords, vannes, brûleurs, tubes
d'échantillonnage, inserts de sonde, têtes d'impression,
tubes à garniture de verre, dewars, lignes de transfert,
disquettes, cassettes magnétiques, multiplicateurs
d'électron, filaments, joints hermétiques, isolant et
toutes les pièces en contact avec des échantillons et
des phases mobiles.
Ladite garantie est nulle en cas d'accident, de
mauvaise utilisation,d'altération, de négligence, de bris,
d'utilisation, maintenance voire de modifications
inappropriées, d'utilisation dans un environnement
inadapté, d'utilisation avec une alimentation marginale
ou d'autres installations ou services inappropriés. Un
certain nombre de précautions doivent être prises pour
éviter tout accident.
Ladite garantie se substitue et exclue expressément
toute garantie expresse ou tacite, y compris mais
ne se limitant pas aux garanties relatives à la
qualité marchande du programme et la garantie de
son aptitude à une utilisation ou une application
particulière, ainsi que toutes les autres obligations
ou engagements de la part de Varian, à moins que
lesdites garanties,obligations ou engagements
aient fait expressément l'objet d'un accord écrit
deVarian.
Limitations de garantie et de la
responsabilité :
Les recours exclusifs du client sont expressément
énoncés aux présentes. En aucun cas, Varian ne
sera tenu pour responsable de tout dommage
provenant de l'utilisation ou en découlant, de toute
impossibilité d'utilisation ou de déficit de
production ou de tout autre perte y afférent.
03-914412-82:21 of 1
Page 12
Garanzia sugli strumenti analitici Varian, Inc.
Prodotti hardware
Tutti gli strumenti analitici commercializzati dalla Varian,
Inc. sono garantiti da eventuali difetti di materiali e di
costruzione per i periodi ed alle condizioni indicati
sull'offerta Varian o comunque concordati per iscritto tra
la Varian ed il Cliente. Il periodo di garanzia decorre
dalla data di spedizione dalla Varian al Cliente. Se
l'installazione è a carico del Cliente o compresa nel
prezzo d'acquisto, il periodo di garanzia decorre dalla
fine dell'installazione. Se il Cliente prevede di procedere
all'installazione oltre i 30 giorni dalla consegna o se tale
ritardo è imputabile alla mancata messa a disposizione,
da parte del Cliente, di locali o strumenti idonei o al
mancato rispetto delle ragionevoli istruzioni di
preinstallazione della Varian o comunque a fatti
imputabili al Cliente, il periodo di garanzia decorre dal
31° giorno dalla data di spedizione. Inoltre, la Varian
addebiterà al Cliente le spese di manodopera e d'altro
tipo sostenute per interventi d'installazione multipli o di
verifica.
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, purché 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
potrà, 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.
Le riparazioni o le sostituzioni in garanzia verranno
effettuate, ad esclusiva discrezione della Varian,
inviando sul posto un tecnico o autorizzando la resa
dello strumento o dell'accessorio difettoso alla Varian o
al centro d'assistenza indicato dalla Varian. Il Cliente
sarà responsabile di eventuali danni o perdite subiti
durante il trasporto dallo strumento o dall'accessorio
reso e dovrà pagare le spese di spedizione in via
anticipata. La Varian restituirà al Cliente lo strumento o
l'accessorio in porto franco con assicurazione a proprio
carico. Sono a cura del Cliente gli eventuali reclami per
perdite o danni di trasporto. Per eliminare eventuali
anomalie di funzionamento del software, la Varian
fornirà le eventuali revisioni del software disponibili
qualora a suo giudizio siano il rimedio migliore.
Limitazioni della garanzia
La presente garanzia non copre il software fornito dal
Cliente, le attrezzature e il software garantiti da altre
case né la sostituzione del materiale di consumo o di
durata limitata, quali, senza intento limitativo, filtri,
provette, spie di stato dello strumento, voltmetri, setti,
colonne, fusibili, carta ed inchiosto , nebulizzatori, celle
a flusso, pistoni, guarnizioni, pezzi speciali, valvole,
bruciatori, tubi di campionamento, inserti per sonde,
testine di stampa, tubazioni rivestite in vetro, raccordi
per tubi, dewars a temperatura variabile, linee di
trasferimento, dischi flessibili, cassette a nastro
magnetico, fotomoltiplicatori, filamenti, guarnizioni per
vuoto, e tutte le parti esposte all'azione dei campioni o
delle fasi mobili.
La presente garanzia decade in caso d'incidente, abuso,
modifica, uso improprio, incuria, rottura, funzionamento
o manutenzione impropri, modifiche non autorizzate od
improprie o manomissioni, impiego in ambiente fisico
non idoneo, impiego con alimentazione ai limiti o con
altri mezzi o dispositivi inadeguati. Devono inoltre
essere adottate tutte le misure ragionevoli atte ad
evitare ogni e qualsiasi rischio.
La presente garanzia sostituisce ed esclude
espressamente ogni altra garanzia espressa o
implicita, comprese - senz'intento limitativo - le
garanzie di commerciabilità ed idoneità a scopi,
impieghi od applicazioni specifici nonché tutti gli
altri obblighi o responsabilità della Varian, a meno
che le altre garanzie, obblighi o responsabilità in
parola non siano stati accettati per iscritto dalla
Varian.
Limitazione degli interventi e delle
responsabilità
Quelli qui contemplati sono gli unici ed esclusivi
interventi cui ha diritto il Cliente. In nessun caso la
Varian sarà responsabile per danni indiretti o
consequenziali, mancata disponibilità, perdita di
produzione o altre perdite subite.
03-914412-83:2
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Page 13
Instrumentos analíticos Varian, Inc. Garantía
Productos hardware
Todos los instrumentos analíticos vendidos por Varian,
Inc. están garantizados contra defectos de materiales y
de fabricación por la duración especificada y de acuerdo
con los términos establecidos en las ofertas de Varian, o
según lo especificado en el acuerdo escrito entre Varian
y el cliente. El plazo de garantía comienza a partir de la
fecha de envío del material de Varian al cliente original.
Sin embargo, si la instalación ha sido pagada por el
cliente o incluida en el precio de compra, el plazo de
garantía comenzará a partir de la fecha de conclusión de
la instalación. Si el cliente especifica que la instalación
comenzará 30 días después de la entrega, o si este plazo
se genera por la imposibilidad por parte del cliente de
proveer los medios necesarios o la falta de cumplimiento
de las directrices de preinstalación de Varian, o cualquier
otra omisión por parte del cliente, el plazo de garantía
comenzará el trigésimoprimer día a partir del envío.
Además, Varian cobrará al cliente por trabajos y otros
gastos relacionados con intervenciones de servicio de
instalación múltiples o tardías.
Productos de software
Cuando el software se suministra dentro del marco de
una licencia de utilización acordada entre Varian y el
cliente, cualquier garantía estará estrictamente limitada a
los términos del citado acuerdo. En ausencia de una
licencia de utilización y a no ser que exista un acuerdo de
período de garantía por escrito entre Varian y el cliente,
el período de garantía será el fijado de acuerdo con los
términos 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 según lo descrito en Manual de
instrucciones, y que esté libre de defectos que impidan la
ejecución de instrucciones de programación. Sin
embargo, Varian no garantiza la utilización ininterrumpida
o libre de errores.
Recursos
El único y exclusivo recurso en cuanto a hardware bajo
garantía será reparar los defectos del aparato, que, en
opinión de Varian, sean claramente imputables a
defectos de los materiales originales o de fabricación, 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 período de garantía
no prolongan el período de garantía original.
Las reparaciones o sustituciones en período de garantía
se efectuarán, a criterio exclusivo de Varian, enviando un
representante de servicio posventa a la instalación, o
autorizando al cliente a reexpedir el componente o
aparato defectuoso a Varian o a un servicio de
reparación designado. El cliente será responsable sobre
pérdidas o daños de transporte, y pagará los costes de
dicho transporte. Varian reexpedirá el componente o
aparato a portes pagados y con seguro de transporte.
Las demandas por daños o pérdidas deberán ser
gestionadas por el cliente. Para corregir anomalías de
funcionamiento de software, Varian editará revisiones de
software, siempre y cuando éstas estén disponibles, y
cuando, en opinión de Varian, este sea el remedio mas
eficaz.
Limitación de garantía
Esta garantía no cubre software provisto por el cliente,
equipos y software garantizados por otros fabricantes,
consumibles o artículos de duración de vida limitada,
como son, entre otros: filtros, elementos de vidrio, pilotos,
lámparas, diafragmas, columnas, fusibles, papel y tinta
de gráficos, nebulizadores, células de flujo, pistones,
cierres, juntas, válvulas, quemadores, tubos de muestras,
inserciones de sondas, cabezales de impresión, tubos de
vidrio, juntas de tubo, dispositivos de temperatura
variable, líneas de transferencia, disquetes, cintas
magnéticas, multiplicadores de electrones, filamentos,
juntas de vacío, soportes y todos los componentes en
contacto con muestras y partes móviles.
Esta garantía no tendrá efecto en los casos de accidente,
abuso, alteración, utilización incorrecta, negligencia,
rotura, mantenimiento o uso inadecuados, modificaciones
inadecuadas o no autorizadas, uso de la fuerza, uso en
un entorno inadecuado, funcionamiento con una
alimentación defectuosa o el uso con medios
inadecuados. Es necesario tomar las precauciones
adecuadas para evitar riesgos.
Las garantías de los productos de software de Varian
sustituyen y excluyen cualquier otra garantía,
implícita o explícita, incluidas pero sin limitación, las
garantías de comerciabilidad, adecuación a un fin,
uso o aplicación en particular, y todas las demás
obligaciones y responsabilidades por parte de
Varian, a no ser que estas garantías, obligaciones y
responsabilidades sean otorgadas expresamente y
por escrito por Varian.
Limitaciones de recursos y
responsabilidades
Los recursos provistos en lo citado son única y
exclusivamente los del cliente. Varian no podrá ser
responsable en ningún caso por daños imprevistos o
consecuencias, pérdida de uso, pérdida de
producción o cualquier otra pérdida incurrida.
03-914412-84:21 of 1
Page 14
y
r
r
r
d
r
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 d escribed in the manual, wh ich appear in the form
of
NOTES, CAUTIONS
accordance with this instruction manual an d any additional information which may be provided by Varian. Address
any questions rega rding the safe and proper use o f your equipment to your local Varian office.
, and
WARNINGS
as described below. It is important that you operate your equipment in
NOTE
Information to aid you in obtaining
optimal performance from your
instrument.
Warning Symbol Warning Description
Alerts you to situations that may
cause moderate injury and/or
equipment damage, and how to
avoid these situations.
Hazardous voltages are present inside instru ment. Disconnect from
main power before removing screw-attached panels.
Hazardous chemicals may be present. Avoid contact, especiall
when replenishing reservoirs. Use proper eye and skin protection.
Very hot or cryogenically cold surfaces may be exposed. Use prope
skin protection.
Eye damage could occur either from flying particles, chemicals o
UV radiation. Use proper eye and face protection.
The potential for fire may be present. Follow manual instructions fo
safe operation.
Alerts you to potentially hazardous
situations that could result in
serious injury, and how to avoid
these situations.
03-914603-00:10
The potential for explosion may exist because of type of gas or liqui
used.
Follow these safety practices to ensure safe equipment operation.
T
Perform periodic leak checks on all supply lines and pneumatic plumbing .
T
Do not allow gas lines to become kinked or punctured. Place lines away from fo ot traffic
and extreme heat or cold.
T
Store organic solvents in fireproof, vented and clearly labeled cabinets so they are easily
identified as toxic and/or flammable materials.
T
Do not accumulate waste solvents. Dispose of such materials through a regulated disposal
program and not through municipa l sewage lines .
NOTICE
This instrument has been tested per applicable requirements of EMC Directive as required t
carry the European Union CE Mark. As such, this equipment may be susceptible t
radiation/interference levels or frequencies which are not within the tested limits.
This instrument is d esigned for chromatographic analysis of appropriately prepared samples. I
must be operated using appropriate gases and/or solvents and within specified maximum range
for pressure, flows, and temperatures as described in this manual. If the equipment is used in
manner not specified by the manufacturer, the protection provided by the equipment may b
impaired.
It is the responsibility of the Customer to inform Varian Customer Support Representatives i
the instrument has been used for the analysis of hazardous biological, radioactive, or toxi
samples, prior to any instrument service being performed or when an instrument is bein
returned to the Service Center for repair.
Electrical Hazards
T
Disconnect the instrument f rom all po wer sources before re moving pr otective panels to avoid
exposure to potentially dangerous vo ltages.
T
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.
T
Replace blown fuses with fuses of the size and rating stipulated on the fuse panel or in the manual.
T
Replace faulty or frayed power cords immediately with the same type and rating.
T
Make sure that voltage sources and line voltage match the value for which the instrument is wired.
Compressed Gas Cylin ders
T
Store and handle compressed gases carefully and in strict adherence to safety codes.
T
Secure cylinders to an immovable structure or wall.
T
Store and move cylinders in an upright, vertical position. Before transport, remove regulators
and install cylinder cap.
T
Store cylinders in a well-ventilated area away from heat, direct sunshine, freezing
temperatures, and ignition sources.
T
Mark cylinders clearly so there is no doubt as to their contents.
T
Use only approved regulators and connections.
T
Use only connec tor tubing that is chromatogra phically clean (Varian Part Num ber 03-918326-00)
and has a pressure rating significantly greater than the highest outlet pressure from the regulator.
2 of 4
03-914603-00:10
Page 16
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.
Radioactive Source Detectors
T
Read carefully and comply with all NOTES,
CAUTIONS, and WARNI NGS in the Ni
63
ECD
manual.
T
Perform the tests for removable radioactive
contami nation described in the Ni
T
Comply with leak test schedules and procedures.
63
ECD manual.
Burn Hazard
Heated or cryogenically cooled zones of gas
chromatographs can remain hot or cold for a
considerable time after instrument power is turned off.
To prevent painful burns, ensure that all heated or
cooled areas have retu rn ed to room temperature or wear
adequate hand protection before you touch potentially
hot or cold surfaces.
LC Safety Practices
High Pressure Hazard
If a line ruptures, a relief device opens, or a valve opens
accidentally under pressure, potentially hazardous high
liquid pressures can be generated by the pump causing
a high velocity stream of volatile and/or toxic liquids.
T
Wear face protection when you inject samples or
perform routine maintenance.
T
Never open a solvent li ne or valv e under pressure.
Stop the pump first and let the pressure drop to
zero.
T
Use shatter-proof reservoirs capable of operating at
50-60 psi.
T
Keep the reservoir enclosure closed when the
reservoir is under pressure.
T
Read and adhere to all NOTES, CAUTIONS, and
WARNI NGS in the manual.
Flash Chromatography
The operator should be familiar with the physicochemical properties of the components of the mobile
phase.
Keep solvents from direct contact with the polyurethane
supply tubing as certain solvents will cause weakening
and leaks with possible bursting.
All components of the system should be connected to a
common power supply and common ground. This
ground must be a true ground rather than a floating
ground.
Non-polar solvents can develop a static charge when
pumped through the system. All vessels that contain
mobile phase (including tubing and collection vessels)
must be grounded to dissipate st atic electricity.
Employ static measuring and static discharge devices
(e.g., air ionizers) to safeguard against the buildup of
static electricity.
Ultraviolet Radiation
Liquid chromatograph detectors that use an ultraviolet
light source have shielding to prevent radiation
exposure to personnel .
For continued protection:
T
Ensure that protective lamp covers of variable and
fixed wavelength detectors are in place during
operation.
T
Do not look directly into detector fluid cells or at
the UV light source. When inspecting the light
source or fluid cell, always use protective eye
covering such as borosilicate glass or polystyrene.
The following is a Federal Communications
Commission advisory:
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 desi gned to provide reasonable
protection against harmful interference when the
equipment is operated in a commercial environment.
This equipm ent generates, uses, and can radi ate radi o
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 interfer ence at his
own expense.
This equipment has been
03-914603-00:10
3 of 4
Page 17
Spare Parts Availability
It is the policy of Varian to provide operational spare parts for any
instrument and major accessory for a period of five (5) years after
shipment of the final production run of that instrument. Spare parts will
be available after this five (5) year period but on an as available basis.
Operational spare parts are defined as those individual electrical or
mechanical parts that are susceptible to failure during their normal
operation. Examples includ e relays, lamps, temperature probes, detector
elements, motors, etc. Sheet metal parts, structural members or
assemblies and castings, printed circuit boards, and functional modules
Service Availability
Varian provides a variety of services
to support its customers after warranty
expiration. Repair service can be
provided by attractively priced service
contracts or on a time and material
basis. Technical support and training
can be provided by qualified
personnel on both a contractual or as-
needed basis.
are normally capable of being rebuilt to like-new condition throughout
their useful life and therefore will be supplied only on an as available
basis after the final production run of the instrument.
Varian Analytical Instr u ments Sales Offices
For Sales or Service assistance and to order Parts and Supplies, contact your local Varian office.
Argentina
Buenos Aires
Tel. +54.11.4.783.5306
Australia
Mulgrave, Victoria
Tel. +61.3.9566.1134
Austria
Vösendorf bei Wien
Tel. +43.1.699.9669
Benelux
Bergen Op Zoom
Tel. +31.164.282.800
Brazil and Latin America (S)
São Paulo
Tel. +55.11.820.0444
Canada
Mississauga, Ontario
Tel. 800.387.2216
China
Beijing
Tel. +86.106209.1727
Europe
Middelburg, The Netherlands
Tel. +31.118.671.000
France
Les Ulis Cédex
Tel. +33.1.6986.3838
Germany
Darmstadt
Tel. +49.6151.7030
India
Mumbai
Tel. +91.22.857.0787/88/89
Italy
Torino
Tel. +39.011.997.9111
Japan
Tokyo
Tel. +81.3.5232.1211
Korea
Seoul
Tel. +82.2.345.22452
Mexico and Latin America (N)
Mexico City
Tel. +52.5.523.9465
Russian Federation
Moscow
Tel. +7.095.937.4280
Spain
Madrid
Tel. +34.91.472.7612
Sweden
Solna
Tel. +46.8.445.1620
Switzerland
Varian AG
Tel. +41.848.803.800
Taiwan
Taipei Hsien
Tel. +886.2.698.9555
United Kingdom and
Ireland
Walton-on-Thames
Tel. +44.1932.898000
Venezuela
Valencia
Tel. +58.41.257.608
United States
Walnut Creek, California,
USA
Tel. +1.800.926.3000
(GC and GC/MS)
Tel. +1.800.367.4752
(LC)
www.varianinc.com
4 of 4
03-914603-00:10
Page 18
Sicherheitsinformationen
G
S
C
G
R
E
Arbeitsanleitungen
Diese Arbeitsanleitung will Ihnen bei der Aufstellung solcher Arbeitsbedingungen helfen, die einen sicheren und
wirkungsvollen Gebrauch Ihrer Geräte ermöglichen. Besondere Überlegungen und Vorsichtsmaßnahmen erscheinen
in diesem Handbuch in Form von
Sie Ihr Gerät in Übereinstimmung mit dieser Arbeitsanleitung und allen möglichen zusätzlichen Informationen von
Varian betreiben. Alle Fragen bezüglich Sicherheit und Handhabung Ihres Gerätes richten Sie an Ihr Varian Büro.
HINWEIS, ACHTUNG und WARNUNG, wie unten beschrieben. Es ist wichtig, daß
HINWEIS
Eine Information, um einen optimalen
Wirkungsgrad Ihres Instruments zu
erzielen.
Weist auf Situationen, die zu mäßiger
Beeinträchtigung und/oder zu
Geräteschäden führen und auf die
Vermeidung dieser Situationen hin.
ACHTUN
Weist auf mögliche Gefahrensituationen,
die zu ernsthaften Verletzungen führen
können und auf die Vermeidung dieser
Situationen hin.
Warnungssymbol Warnungsbeschreibung
WARNUNG
ELEKTRISCHER
HLA
Gefährliche Spannungen bestehen innerhalb des Instruments. Trennen Sie das
Gerät vom Netz, bevor Sie abschraubbare Paneele entfernen.
Gefährliche Chemikalien können vorhanden sein. Vermeiden Sie jeden Kontakt, besonders beim Auffüllen der Reservoirs. Benutzen Sie wirksamen
Augen und Hautschutz.
WARNUNG
VERBRENNUNGSGEF AHR
Sehr heiße oder tiefstgekühlte Oberflächen können freigelegt sein. Benutzen
Sie einen wirksamen Hautschutz.
Herumfliegende Partikel, Chemikalien oder UV-Strahlung können
Augenschäden verursachen. Tragen Sie deshalb einen geeigneten Schutz für
Augen und Gesicht.
WARNUNG
W ARNUNG
FEUERGEFAHR
WARNUNG
EXPLOSIONSGEFAH
WARNUNG
STRAHLUNGSQUELLE
WARNUNG
BEWEGTE TEIL
03-914603-81:101 of 4
Es besteht eine mögliche Feuergefahr. Beachten Sie die Vorschriften im
Handbuch für eine gefahrlose Benutzung.
Eine mögliche Explosionsgefahr besteht infolge der benutzten Gas- oder
Flüssigkeitsart.
Es besteht eine ionisierende Strahlungsquelle. Beachten Sie die Vorschriften
im Handbuch für eine gefahrlose Benutzung.
Bleiben Sie mit Ihren Händen und Fingern weg.
Page 19
Allgemeine Sicherheitsmaßnahmen
Befolgen Sie diese Sicherheitspraktiken für eine gefahrlose Gerätebenutzung.
Prüfen Sie regelmäßig alle Versorgungs und Pneumatikleitungen auf Lecks.
Gasleitungen dürfen nicht geknickt oder angestochen werden. Verlegen Sie die Leitungen
außerhalb von Laufwegen und abseits von extremer Hitze oder Kälte.
Lagern Sie organische Lösungsmittel in feuerfesten, belüfteten und eindeutig bezeichneten
Schränken, damit sie leicht als toxische und/oder brennbare Materialien erkannt werden.
Sammeln Sie keine Lösungsmittelabfälle. Entsorgen Sie solche Materialien über ein geregeltes
Entsorgungsprogramm und nicht über die öffentlichen Abwasserleitungen.
HINWEIS:
Dies Instrument wurde nach den zutreffenden Vorschriften der EMC Direktive getestet, die
zum Führen des CE Zeichens der Europäischen Union berechtigen. Dieses Gerät kann an sich
auf Strahlungs-/Störpegel oder Frequenzen außerhalb der getesteten Grenzen reagieren.
Dies Instrument ist für chromatographische Analysen entsprechend präparierter Proben
WARNUNG
gedacht. Es muß mit geeigneten Gasen und/oder Lösungsmitteln und innerhalb der im
Handbuch spezifizierten maximalen Werte für Druck, Flüsse und Temperaturen betrieben
werden.
Der Kunde ist vor der Durchführung irgendeines Geräteservices verpflichtet den Varian
WARNUNG
Kundendienstvertreter zu informieren, wenn das Instrument für Analysen gefährlicher
biologischer, radioaktiver oder toxischer Proben benutzt worden ist.
Elektrische Gefahren
Lösen Sie das Instrument von allen Stromquellen, bevor Sie Schutzpaneele entfernen, damit Sie nicht mit
potentiell gefährlichen Spannungen in Berührung kommen.
Wenn ein Nicht-Original Netzkabelstecker benutzt werden muß, muß das Austauschkabel die im Handbuch
beschriebene Farbcodierung und Polarität beibehalten und alle örtlichen Sicherheitsvorschriften erfüllen.
Ersetzen Sie durchgebrannte Sicherungen nur mit Sicherungen der Werte, die am Sicherungspaneel oder im
Handbuch angegeben sind.
Ersetzen Sie fehlerhafte oder durchgescheuerte Netzkabel sofort durch Kabel gleicher Art.
Sorgen Sie dafür, daß Spannungsquellen und die Netzspannung den gleichen Wert haben, für den das
Instrument verdrahtet ist.
Gasdruckflaschen
Lagern und handhaben Sie komprimierte Gase vorsichtig und in strikter Einhaltung der
Sicherheitsvorschriften.
Befestigen Sie die Gasflaschen an feststehenden Aufbauten oder an Wänden.
Lagern und transportieren Sie Gasflaschen in aufrechter Stellung. Druckregler zuvor abnehmen.
Lagern Sie Gasflaschen in gut durchlüfteten Räumen, weit genug weg von Heizungen, direktem
Sonnenschein, Frosttemperaturen und Entzündungszonen.
Kennzeichnen Sie die Flaschen so eindeutig, daß kein Zweifel über deren Inhalt bestehen kann.
Benutzen Sie nur geprüfte Druckminderer und Verbindungsstücke.
Benutzen Sie nur chromatographisch reines Verbindungsrohr (Varian Part Number 03-918326-00), das
wesentlich höheren Druck als den höchsten Ausgangsdruck des Druckminderers aushält.
2 of 4 03-914603-81:10
Page 20
GC Sicherheitspraktiken
Abgassystem
Für GC Detektoren, die in einem gut durchlüfteten
Raum installiert sind, ist keine spezielle Abgasführung
erforderlich, außer wenn die Detektoren zum Testen
gefährlicher Chemikalien benutzt werden. Wenn Sie
eine Abgasführung installieren:
Benutzen Sie nur feuerfeste Führungen.
Installieren Sie ein Gebläse am Ausgang.
Ordnen Sie die Ansaugöffnung so an, daß ihre Er-
schütterungen oder Luftströmungen nicht die Detektorfunktion beeinträchtigen.
Prüfen Sie regelmäßig die einwandfreie Arbeits-
weise der Abgasführung.
Sorgen Sie für gute Entlüftung im Laborbereich.
Radioaktive Detektoren
Lesen Sie sorgfältig und befolgen Sie alle
HINWEISE, ACHTUNGEN und WARNUNGEN im
63
ECD Handbuch.
Ni
Führen Sie die Tests für zu beseitigende radioak-
tive Kontamination durch, die im Ni
buch beschrieben sind.
Erfüllen Sie die Zeitpläne und Verfahren zur Di-
chtigkeitsprüfung.
63
ECD Hand-
Verbrennungsgefahr
Beheizte oder tieftemperaturgekühlte Zonen des Gaschromatographen können beträchtlich lange heiß oder
kalt bleiben, nachdem das Instrument bereits abgeschaltet ist. Zur Vermeidung schmerzhafter Verbrennungen
müssen Sie darauf achten, daß alle beheizten oder
gekühlten Zonen auf Raumtemperatur zurückgegangen
sind oder Sie müssen ausreichenden Handschutz benutzen, bevor Sie möglicherweise heiße oder kalte
Oberflächen berühren.
LC Sicherheitspraktiken
Gefahr durch hohen Druck
Wenn eine Leitung bricht, eine Entlüftungseinheit sich
öffnet oder ein Ventil sich unbeabsichtigt unter Druck
öffnet, kann durch die Pumpe möglicherweise ein gefährlich hoher Flüssigkeitsdruck entstehen, der einen
Strahl flüchtiger und/oder toxischer Flüssigkeiten von
hoher Stömungsgeschwindigkeit verursacht.
Tragen Sie einen Gesichtsschutz, wenn Sie Proben
injizieren oder Routinewartungen durchführen.
Öffnen Sie niemals eine unter Druck stehende
Lösungsmittelleitung oder ein Ventil. Halten Sie
zuerst die Pumpe an und lassen Sie den Druck auf
Null abfallen.
Benutzen Sie splittersichere Reservoirs, die für
einen Druck von 3,4 bis 4,1 bar ausgelegt sind.
Halten Sie die Reservoirverkleidung geschlossen,
wenn die Reservoirs unter Druck stehen.
Lesen Sie und befolgen Sie alle HINWEISE,
ACHTUNGEN und WARNUNGEN im Handbuch.
Blitzlicht-Chromatographie
Der Bediener sollte mit den physikalisch-chemischen
Eigenschaften der Komponenten vertraut sein, aus
denen sich die mobile Phase zusammensetzt.
Vermeiden Sie direkten Kontakt der Lösungsmittel mit
den Zuführungsleitungen aus Polyurethan, da einige
Lösungsmittel das Material der Leitungen schwächen
und damit Undichtigkeiten oder Brüche hervorrufen
können.
Alle Systemkomponenten sollten an der gleichen
Netzstromquelle und einer gemeinsamen Erdung
angeschlossen sein. Dabei muss es sich um eine echte,
nicht um eine schwebende Erdung handeln.
Nicht-polare Lösungsmittel können sich beim Pumpen
durch das System statisch aufladen. Alle Gefäße, die
mobile Phase enthalten (einschließlich Leitungen und
Sammelgefäße), müssen zur Ableitung elektrostatischer Aufladungen geerdet sein.
Setzen Sie Geräte zur Messung und Ableitung
elektrostatischer Aufladungen (z.B. Geräte zur
Luftionisierung) als Maßnahmen gegen den Aufbau
statischer Elektrizität ein.
Ultraviolette Strahlung
Detektoren in Liquidchromatographen, die eine
ultraviolette Lichtquelle benutzen, besitzen eine
Abschirmung, die das Bedienungspersonal gegen
Abstrahlungen schützt. Zum ständigen Schutz:
Achten Sie darauf, daß die schützende Lampenab-
deckung der Detektoren mit variablen und festen
Wellenlängen während des Betriebs an ihrem Platz
ist.
Schauen Sie nicht direkt in die Flüssigkeitszellen
im Detektor oder in die UV Lampe. Zum Inspizieren der Lichtquelle oder der Flüssigkeitszelle
benutzen Sie immer einen wirksamen Augenschutz,
wie er durch Borsilikatglas oder Polystyrol gewährleistet wird.
03-914603-81:103 of 4
Page 21
Verfügbarkeit von Ersatzteilen
Es ist Varian’s Grundsatz, Ersatzteile für alle Instrumente und die wichtigsten Zubehöre für einen Zeitraum von fünf (5) Jahren nach dem Fertigungsauslauf dieser Geräteserie verfügbar zu haben. Nach diesem Zeitraum von
fünf (5) Jahren können Ersatzteile auf der Basis solange vorhanden bezogen werden. Als Ersatzteil werden hier solche elektrischen und mechanischen Einzelteile verstanden, die unter normalen Bedingungen ausfallen
können. Beispiele sind Relais, Lampen, Temperaturfühler, Detektorelemente, Motore usw. Metallbleche, Formteile oder Baugruppen und
Gußteile, PC Boards und Funktionsmodule können normalerweise neuwertähnlich für eine brauchbare Lebensdauer instandgesetzt werden und
werden deshalb nur auf der Basis solange vorhanden nach dem Produktionsauslauf des Instruments geliefert werden.
Serviceverfügbarkeit
Varian bietet seinen Kunden auch
nach dem Auslaufen der Garantie
eine Vielfalt von Serviceleistungen
an. Reparaturservice kann zu attraktiven Preisen über eine Wartungsvereinbarung oder nach Zeit- und
Materialaufwand zur Verfügung
gestellt werden. Technische Unterstützung und Training bieten wir
Ihnen durch qualifizierte Chemiker
sowohl auf einer Kontraktbasis als
auch nach Ihren Erfordernissen an.
Varian Analytical Instruments Verkaufsbüros
Für Verkaufs oder Servicehilfe und zum Bestellen von Teilen und Zubehören setzen Sie sich bitte mit Ihrem
Varian Büro in Verbindung.
Argentina
Buenos Aires
Tel. +54.11.4.783.5306
Australia
Mulgrave, Victoria
Tel. +61.3.9566.1134
Austria
Vösendorf bei Wien
Tel. +43.1.699.9669
Benelux
Bergen Op Zoom
Tel. +31.164.282.800
Brazil and Latin America (S)
São Paulo
Tel. +55.11.820.0444
Canada
Mississauga, Ontario
Tel. 800.387.2216
China
Beijing
Tel. +86.106209.1727
Europe
Middelburg, The Netherlands
Tel. +31.118.671.000
France
Les Ulis Cédex
Tel. +33.1.6986.3838
Germany
Darmstadt
Tel. +49.6151.7030
India
Mumbai
Tel. +91.22.857.0787/88/89
Italy
Torino
Tel. +39.011.997.9111
Japan
Tokyo
Tel. +81.3.5232.1211
Korea
Seoul
Tel. +82.2.345.22452
Mexico and Latin America (N)
Mexico City
Tel. +52.5.523.9465
Russian Federation
Moscow
Tel. +7.095.937.4280
Spain
Madrid
Tel. +34.91.472.7612
Sweden
Solna
Tel. +46.8.445.1620
Switzerland
Varian AG
Tel. +41.848.803.800
Taiwan
Taipei Hsien
Tel. +886.2.698.9555
United Kingdom and
Ireland
Walton-on-Thames
Tel. +44.1932.898000
Venezuela
Valencia
Tel. +58.41.257.608
United States
Walnut Creek, California, USA
Tel. +1.800.926.3000
(GC and GC/MS)
Tel. +1.800.367.4752
(LC)
www.varianinc.com
4 of 4 03-914603-81:10
Page 22
Informations et mesures de sécurité
CTROCUTIO
S
E
T
Instructions de fonctionnement
Ce manuel d’instruction est conçu pour aider l’utilisateur à créer des conditions opératoires lui permettant de faire
fonctionner le matériel efficacement et en toute sécurité. Il contient entre autres certaines observations spéciales
présentées sous forme de
matériel conformément aux instructions du présent manuel et à toute autre information émanant de Varian. S’adresser
au bureau régional Varian pour toute question relative à la sécurité ou à l’utilisation correcte du matériel.
NOTES,MISESENGARDEetAVERTISSEMENTS.Il est important de faire fonctionner ce
NOTE
Information destinée à tirer le
meilleur parti du matériel sur le plan
des performances
Symboles d’avertissement Description
ATTENTION
RISQUE
D'ELE
N
ATTENTION
RISQUE DE BRÛLURE
Attire l’attention sur une situation
pouvant occasionner des dommages
corporels légers et/ou des dégâts
mineurs à l’appareil et indique
comment remédier à cette situation
Exposition à des tensions dangereuses. Débrancher le matériel du secteur avant de
dévisser les panneaux protecteurs.
Présence éventuelle de substances chimiques dangereuses. Eviter tout contact, en
particulier lors du remplissage des réservoirs. Prendre les mesures de protection
adéquates pour les yeux et la peau.
Exposition à des surfaces chaudes ou traitées cryogéniquement. Prendre les
mesures de protection adéquates pour la peau.
Les dommages causées aux yeux sont de deux natures différentes : jet de
particules et de produits chimiques ou radiations UV. Utiliser des protections du
visage et des yeux appropriées.
Attire l’attention sur une situation
potentiellement dangereuse pouvant
occasionner des dommages corporels
importants et indique comment
remédier à cette situation
ATTENTION
RISQUE D'INCENDI
ATTENTION
RISQUE D'EXPLOSION
ATTENTION
SOURCE DE RADIATION
ATTENTION
PIECES EN MOUVEMEN
Risque potentiel d’incendie. Se conformer aux instructions du manuel pour faire
fonctionner le matériel en toute sécurité.
Risque potentiel d’explosion en raison du type de gaz ou de liquide utilisé.
Présence d’une source de radiation ionisante. Se conformer aux instructions du
manuel pour faire fonctionner le matériel en toute sécurité.
Garder les mains et les doigts hors de portée.
03-914603-82:101 of 4
Page 23
Précautions générales en matière de sécurité
N
N
Les pratiques suivantes garantissent une utilisation sans risques du matériel:
Effectuer régulièrement des essais d’étanchéité de tous les conduits d’alimentation et de tous les tuyaux du
système pneumatique.
Ne pas travailler avec des conduits de gaz déformés ou percés. Installer les conduits de gaz à l’écart des allées
et venues et à l’abri du chaud ou du froid.
Conserver les solvants organiques dans des récipients à l’épreuve du feu, bien ventilés et portant mention de la
nature de leur contenu, en particulier lorsque lesdits solvants sont toxiques et/ou inflammables.
Ne pas accumuler les solvants de rebut. Les éliminer conformément à un programme agréé d’élimination des
déchets et non via les égouts municipaux.
NOTE:
Ce matériel a été testé conformément aux dispositions de la directive CME afin de
pouvoir porter le sigle CE de l’Union européenne. Il en résulte qu’il peut être sensible à
des niveaux de radiation/d’interférence ou à des fréquences se situant hors des limites
testées.
Ce matériel est conçu pour effectuer des analyses chromatographiques d’échantillons
ATTENTIO
préparés selon des méthodes appropriées. Il convient de le faire fonctionner avec les gaz
et/ou les solvants adéquats et dans les limites des pressions, des débits et des températures
maximales spécifiées dans le présent manuel.
Le client est tenu d’informer le service Varian d’assistance à la clientèle que son matériel
ATTENTIO
a été utilisé pour l’analyse d’échantillons biologiques dangereux, radioactifs ou toxiques
avant que n’en soit effectué la maintenance.
Risques de chocs électriques
Déconnecter le matériel de toute source d’alimentation avant d’en démonter les panneaux de protection, sous
peine de s’exposer à des tensions dangereuses.
En cas d’utilisation d’un cordon d’alimentation n’étant pas d’origine, s’assurer que celui-ci soit conforme à la
polarité et au codage des couleurs décrits dans le manuel d’utilisation ainsi qu’à toutes les normes régionales
de sécurité régissant le secteur de la construction.
Remplacer les fusibles sautés par des fusibles de même type que ceux stipulés sur le panneau des fusibles ou
dans le manuel d’utilisation.
Remplacer les cordons d’alimentation défectueux ou dénudés par des cordons d’alimentation de même type.
S’assurer que les sources de tension et la tension de secteur correspondent à la tension de fonctionnement du
matériel.
Bouteilles à gaz comprimé
Ranger et manipuler les bouteilles à gaz comprimé avec précaution et conformément aux normes de sécurité.
Fixer les bouteilles à gaz comprimé à un mur ou à une structure inamovible.
Ranger et déplacer les bouteilles à gaz comprimé en position verticale. Avant de transporter les bouteilles à
gaz comprimé, retirer leur régulateur.
Ranger les bouteilles dans un endroit bien ventilé et à l’abri de la chaleur, des rayons directs du soleil, du gel
ou des sources d’allumage.
Marquer les bouteilles de manière à n’avoir aucun doute quant à leur contenu.
N’utiliser que des connexions et régulateurs agréés.
N’utiliser que des tuyaux de raccordement propres sur le plan chromatographique (Varian P/N 03-918326-00)et
pouvant supporter des pressions sensiblement plus élevées que la plus haute pression de sortie du régulateur.
2 of 4 03-914603-82:10
Page 24
Mesures de sécurité en CPG
Système d’échappement
Les détecteurs CPG installés dans une pièce bien
ventilée ne nécessitent pas de conduits spéciaux
d’échappement excepté lorsqu’ils sont destinés à
analyser des substances chimiques dangereuses. Lors
de l’installation de tels conduits:
N’utiliser que des conduits à l’épreuve du feu
Installer un ventilateur à la sortie du conduit.
Placer les orifices d’aspiration de manière à ce que
les vibrations ou les mouvements d’air n’affectent
pas le fonctionnement du détecteur.
Ne jamais déconnecter un conduit de solvant ou
une vanne sous pression. Arrêter préalablement la
pompe et laisser la pression descendre à zéro.
Utiliser des réservoirs incassables à 50-60 psi.
Laisser l’enceinte du réservoir fermée lorsque le
réservoir est sous pression.
Se conformer aux NOTES, MISESENGARDEET
AVERTISSEMENTSdumanuel d’utilisation.
Chromatographie Flash
L’utilisateur aura la connaissance des propriétés
physico-chimiques des constituants de la phase mobile.
Vérifier périodiquement l’état du conduit.
S’assurer que le laboratoire est correctement
ventilé.
Détecteurs à source radioactive
Se conformer au manuel d’utilisation de l’ECD
63
Ni
, en particulier à ses NOTES, MISES EN
GARDEET AVERTISSEMENTS.
Effectuer les tests de décontamination radioactive
décrits dans le manuel d’utilisation de l’ECD Ni
Se conformer aux procédures et au calendrier des
63
.
essais d’étanchéité.
Risque de brûlures
Les zones des chromatographes à gaz chauffées ou
traitées cryogéniquement peuvent rester très chaudes ou
très froides durant une période plus ou moins longue
après la mise hors tension du matériel. Pour éviter les
brûlures, s’assurer que ces zones sont revenues à
température ambiante ou utiliser un dispositif adéquat
de protection des mains avant de les toucher.
Eviter le contact direct des solvants avec les tuyaux en
polyuréthane : certains solvants sont susceptibles de
provoquer des faiblesses et des fuites avec risques
d’explosion.
Tous les constituants du système devront être connectés
à une source de courant commune et à une prise de
terre commune. Cette prise de terre devra être fixe et
non mobile.
Les solvants non-polaires peuvent produire de
l’électricité statique lorsqu’ils passent au travers du
système. Les bouteilles qui contiennent la phase mobile
(incluant les tuyaux et les flacons de collecte de
fractions) doivent être mises à la terre pour éliminer
l’électricité statique.
Utiliser des appareils de mesure et de décharge
d’électricité statique (par exemple des ionisateurs d’air)
pour combattre la formation d’électricité statique.
Radiations ultraviolettes
Les détecteurs CPL utilisant une source lumineuse
ultraviolette comportent un écran destiné à se prémunir
contre les expositions aux rayonnements.
Pour s’assurer une protection permanente:
Mesures de sécurité en CPL
Risques liés aux hautes pressions
En cas de rupture d’un tuyau ou en cas d’ouverture
accidentelle d’une vanne alors que le système est sous
pression, la pompe peut occasionner des dommages en
expulsant à grande vitesse des jets de liquides volatiles
et/ou toxiques.
Mettre un masque de protection lors de l’injection
des échantillons ou en effectuant les opérations de
maintenance de routine.
03-914603-82:103 of 4
Vérifier que le couvercle de protection de la lampe
des détecteurs opérant à des longueurs d’onde
variables et fixes soit bien en place durant le
fonctionnement du matériel.
Ne pas regarder directement les cellules du
détecteur ou la source d’UV. Se protéger
systématiquement les yeux lors du contrôle de la
source lumineuse ou des cellules, par exemple au
moyen de verres borosilicatés ou en polystyrène.
Page 25
Disponibilité des pièces de rechange
La politique de Varian consiste à fournir des pièces de rechange pour
tous les appareils et accessoires majeurs durant une période de cinq (5)
ans après livraison de leur production finale. Les pièces de rechange ne
sont fournies au terme de cette période de cinq (5) ans que suivant les
disponibilités. Il faut entendre par pièces de rechange les pièces
individuelles électriques ou mécaniques susceptibles de défaillance au
cours de leur utilisation normale. Par exemple, les relais, les lampes, les
sondes thermiques, les éléments de détecteur, les moteurs, etc. Les
parties en tôles, les éléments ou assemblages structurels et les pièces de
fonderie, les cartes à circuits imprimés et les modules fonctionnels sont
normalement susceptibles d’être remis à l’état neuf pendant toute la
durée de leur vie utile et ne sont dès lors fournies, au terme de la
Service d’assistance à
la clientèle
Varian fournit divers services
destinés à aider sa clientèle après
expiration de la garantie: service de
réparation sur base de contrats de
maintenance à prix attractifs ou sur
base d’accords à durée limitée
portant sur du matériel spécifique;
support technique et service de
formation assurés par des chimistes
qualifiés sur base contractuelle ou
en fonction des besoins spécifiques.
production finale des appareils, que suivant les disponibilités.
Points de vente des instruments analytiques Varian
Contactez votre point de vente régional Varian pour toute question commerciale ou de service d’assistance à
la clientèle ou pour passer commande de pièces et de fournitures.
Argentina
Buenos Aires
Tel. +54.11.4.783.5306
Australia
Mulgrave, Victoria
Tel. +61.3.9566.1134
Austria
Vösendorf bei Wien
Tel. +43.1.699.9669
Benelux
Bergen Op Zoom
Tel. +31.164.282.800
Brazil and Latin America (S)
São Paulo
Tel. +55.11.820.0444
Canada
Mississauga, Ontario
Tel. 800.387.2216
China
Beijing
Tel. +86.106209.1727
Europe
Middelburg, The Netherlands
Tel. +31.118.671.000
France
Les Ulis Cédex
Tel. +33.1.6986.3838
Germany
Darmstadt
Tel. +49.6151.7030
India
Mumbai
Tel. +91.22.857.0787/88/89
Italy
Torino
Tel. +39.011.997.9111
Japan
Tokyo
Tel. +81.3.5232.1211
Korea
Seoul
Tel. +82.2.345.22452
Mexico and Latin America (N)
Mexico City
Tel. +52.5.523.9465
Russian Federation
Moscow
Tel. +7.095.937.4280
Spain
Madrid
Tel. +34.91.472.7612
Sweden
Solna
Tel. +46.8.445.1620
Switzerland
Varian AG
Tel. +41.848.803.800
Taiwan
Taipei Hsien
Tel. +886.2.698.9555
United Kingdom and
Ireland
Walton-on-Thames
Tel. +44.1932.898000
Venezuela
Valencia
Tel. +58.41.257.608
United States
Walnut Creek, California, USA
Tel. +1.800.926.3000
(GC and GC/MS)
Tel. +1.800.367.4752
(LC)
www.varianinc.com
4 of 4 03-914603-82:10
Page 26
Informazioni sulla Sicurezza
E
E
i
o
i
i
Instruzioni per l’Uso
Questo manuale ha lo scopo di aiutare l’operatore ad utilizzare lo strumento in modo sicuro ed efficiente. Le
considerazioni e le precauzioni speciali vengono presentate in questo manuale sotto forma di avvisi di
CAUTELA e ATTENZIONE. E’ importante che lo strumento venga utilizzato rispettando le istruzioni fornite in questo
manuale o che verranno fornite successivamente dalla Varian. Per ogni eventuale chiarimento sull’uso o sulla
sicurezza, si prega di contattare la Varian di Leinì (TO).
NOTA,
NOTA
Sono informazioni utili ad ottenere
le prestazioni migliori da parte
dello strumento.
Segnali di ATTENZIONE Descrizione del Pericolo
ATTENZIONE
Pericolo di folgorazion
ATTENZIONE
Pericolo di scottature
ATTENZIONE
Pericolo di incendi
Allerta l’operatore su situazioni che
potrebbero causare ferite leggere e
danni limitati allo strumento ed il
modo di evitarle.
Nello strumento sono presenti tensioni pericolose. Scollegare il cavo
di alimentazione prima di togliere il pannello fissato con le viti.
Possono essere presenti composti chimici pericolosi. Evitare il
contatto, specialmente quando si riempiono i contenitori. Usare
protezioni opportune per la pelle e per gli occhi.
Pericolo di esposizione a superfici molto calde o raffreddate
criogenicamente. Usare protezioni opportune per la pelle.
Particelle volanti, agenti chimici o radiazioni UV possono
danneggiare gli occhi. Vanno quindi utilizzate le opportune
protezioni per gli occhi e per il volto.
Pericolo potenziale di incendio. Seguire le istruzioni del manuale per
lavorare con una maggiore sicurezza.
ATTENZION
Allerta l’operatore su situazioni
potenzialmente pericolose che
possono causare danni molto seri ed
il modo di evitarle.
ATTENZION
ATTENZIONE
Pericolo di esplosion
ATTENZIONE
Pericolo di radiazion
C’è 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.
ATTENZIONE
Parti in movimento
03-914603-83:101 of 4
Non tenere le mani o le dita vicino.
Page 27
Norme di Sicurezza
E
E
Per lavorare in modo sicuro sullo strumento, Vi consigliamo si adottare le seguenti procedure.
Verificare periodicamente che non ci siano perdite sulle linee e sui raccordi pneumatici.
Evitare che le linee dei gas vengano piegate o forate. Le linee vanno posizionate in modo tale
da non essere calpestate e lontane da sorgenti o troppo calde o troppo fredde.
I solventi organici vanno conservati in armadi speciali antiincendio, ventilati e con indicazioni
chiare sul contenuto di materiali tossici e/o infiammabili.
Non accumulare i solventi utilizzati. Adottare un programma regolare di smaltimento, ma mai
nelle acque di scarico.
AVVERTENZA:
ATTENZION
ATTENZION
Questo strumento è stato testato secondo le Direttive EMC allo scopo di poter utilizzare il
Marchio CE della Comunità Europea. Questo strumento può essere suscettibile a
radiazioni/interferenze o frequenze che non sono entro i limiti collaudati.
Questo strumento è progettato per l’analisi cromatografica di campioni opportunamente
preparati. Deve essere utilizzato usando gas e solventi adatti a questo scopo ed entro i limiti
massimi di pressione, flusso e temperatura riportati in questo manuale. Se lo strumento non
viene utilizzato secondo le modalità specificate dal costruttore, le condizioni di sicurezza
previste potranno non essere sufficienti.
E’ responsabilità del Cliente informare il Servizio Tecnico Varian, prima di qualsiasi
intervento di riparazione, se lo strumento è stato utilizzato per l’analisi di campioni
biologicamente pericolosi, radioattivi o tossici.
Pericoli Elettrici
Prima di togliere i pannelli di protezione, scollegare lo strumento da tutte le alimentazioni
elettriche in modo da evitare l’esposizione a voltaggi potenzialmente pericolosi.
Quando si rende necessario sostituire il cavo di alimentazione, assicurarsi che il nuovo cavo
rispetti sia le codifiche di colore e di polarità riportate nel manuale di istruzioni che quelle
stabilite dalle norme di sicurezza del laboratorio.
Sostituire i fusibili bruciati solo con fusibili che abbiano le stesse caratteristiche; queste ultime sono
riportate sul pannello dei fusibili e/o nel manuale di istruzioni.
Sostituire immediatamente i cavi di alimentazione difettosi o consumati con cavi dello stesso
tipo e con le stesse caratteristiche.
Assicurarsi che il voltaggio del pannello di alimentazione corrisponda a quello dello
strumento da collegare.
Bombole dei Gas
Occorre prestare molta attenzione quando si spostano bombole di gas compressi. Rispettare tutte le
norme di sicurezza.
Assicurare le bombole ad una parete o ad una struttura fissa.
Spostare e conservare le bombole sempre in posizione verticale. Togliere i manometri prima di
spostare le bombole.
Conservare le bombole in un’area ben ventilata, non infiammabile, lontana da sorgenti di calore,
non esposta a temperature troppo fredde o alla luce diretta del sole.
Evidenziare in modo chiaro e che non lasci dubbi il contenuto di ogni bombola.
Usare solo manometri e raccordi di qualità.
Usare solo tubazioni cromatograficamente pulite (Numero di Parte Varian 03-918326-00) e calibrate
per pressioni superiori a quella massima di uscita dal manometro.
2 of 4 03-914603-83:10
Page 28
Procedure di Sicurezza in GC
Scarico dei Gas
Per i rivelatori GC non è richiesto alcun sistema
particolare di scarico dei gas, se lo strumento è
installato in una stanza ben ventilata e se non viene
utilizzato per l’analisi di sostanze chimiche pericolose.
Se si deve installare un sistema di scarico dei gas:
Usare condutture non infiammabili
Installare un aspiratore in uscita
Posizionare la presa d’aria in modo che le
vibrazioni e il movimento dell’aria non disturbino
il rivelatore.
Eseguire verifiche periodiche per garantire un
funzionamento corretto.
Garantire una buona ventilazione nel laboratorio.
Rivelatori a Sorgente Radioattiva
Leggere e rispettare tutte gli avvisi di NOTA,
CAUTELA e ATTENZIONE riportati nel manuale
del rivelatore ECD al Ni
Eseguire tutti i test di contaminazione radioattiva
rimovibile descritti nel manuale dell’ECD al Ni
Rispettare tutte le procedure e le scadenze di
verifica per eventuali perdite.
63
.
63
.
Pericolo di Scottature
Le zone calde o raffreddate criogenicamente del
gascromatografo possono mantenere la loro
temperatura per parecchio tempo, dopo aver spento lo
strumento. Per evitare scottature, assicurarsi che le
zone riscaldate o raffreddate siano a temperatura
ambiente oppure indossare delle protezioni adeguate
prima di toccare tali superfici.
Procedure di Sicurezza in LC
Pericolo di Alte Pressioni
In caso di rottura di una linea o di apertura accidentale
di una valvola, quando il sistema è sotto pressione, la
pompa può liberare liquidi tossici e/o volatili molto
pericolosi.
E’ opportuno adottare un sistema di protezione del
viso quando si inietta il campione o si esegue una
manutenzione routinaria del sistema.
Non smontare mai una linea del solvente od una
valvola quando il sistema è sotto pressione.
Fermare prima la pompa ed aspettare che la
pressione scenda a zero.
Usare dei contenitori per solventi infrangibili ed in
grado di lavorare a 50-60 psi.
Quando i contenitori sono sotto pressione, usare
una protezione esterna.
Leggere e rispettare tutti gli avvisi di NOTA,
CAUTELA e ATTENZIONE.
Cromatografia Flash
L’operatore deve conoscere le proprietà fisico-chimiche
delle componenti della fase mobile.
I solventi non vanno messi in contatto diretto con il
tubo di erogazione in poliuretano, dal momento che
alcuni solventi possono causare indebolimento e perdite
con possibili scoppi.
Tutte le componenti del sistema vanno collegate ad una
fonte di alimentazione e ad una messa a terra comuni.
E’ meglio che per quest’ultima venga utilizzata una
spina con polo di terra.
I solventi non-polari possono sviluppare una carica
statica quando vengono pompati attraverso il sistema.
Tutti i recipienti che contengono la fase mobile (inclusi
i tubi e i recipienti di raccolta) devono avere una messa
a terra per disperdere l’elettricità statica.
Vanno utilizzati dispositivi di misurazione e scarico (ad
esempio ionizzatori d’aria) per evitare l’aumento di
elettricità statica.
Radiazioni Ultraviolette
I rivelatori di cromatografia liquida che usano sorgenti
a luce ultravioletta montano degli schermi di protezione
per evitare che gli operatori siano esposti a radiazioni
pericolose.
Per una protezione sicura:
Assicurarsi che i coperchi delle lampade dei
rivelatori a lunghezza fissa e variabile siano sempre
al loro posto, quando si lavora.
Non guardare mai direttamente dentro le celle o
alla sorgente di luce UV. Quando si vuole
ispezionare la lampada o le celle, usare sempre
delle protezioni adatte per gli occhi, quali vetro in
borosilicato e polistirolo.
03-914603-83:103 of 4
Page 29
Disponibilità delle Parti di Ricambio
E’ politica della Varian il fornire le parti di ricambio per lo strumento ed
i suoi accessori per un periodo di cinque (5) anni a partire dalla data di
produzione dell’ultima unità della serie. Le parti di ricambio saranno
disponibili anche dopo questo periodo di cinque (5) anni ma solo in base
alla disponibilità delle stesse. Per parti di ricambio si intendono i
componenti elettrici e meccanici soggetti ad usura durante l’uso, in
condizioni normali, dello strumento. Come esempio, citiamo i relay, le
lampade, i probe di temperatura , i componenti del rivelatore, i motorini,
ecc. Le parti strutturali o da fusione, le schede elettroniche ed i moduli
funzionali possono essere ricostruiti e rimessi a nuovo durante tutto il
loro periodo di vita e perciò sarà possibile acquistarli, dopo la
Servizi Tecnico
La Varian, alla scadenza del periodo
di garanzia, è in grado di fornire ai
suoi clienti un’ampia scelta di
opzioni. Le riparazioni possono
essere effettuate sulla base di
contratti di manutenzione particolarmente vantaggiosi od in base ad una
tariffa oraria piu’ il costo delle parti.
A richiesta, si possono avere corsi
per operatori sia sotto forma di
contratto che a tariffe da concordare.
produzione dell’ultima unità delle serie, solo in base alla loro
disponibilità.
Uffici Vendite della Divisione Strumenti Analitici della Varian
Per informazioni relative alla Vendita, al Servizio Tecnico o all’acquisto di Parti di ricambio, si prega di
contattare l’ufficio Varian piu’ vicino.
Argentina
Buenos Aires
Tel. +54.11.4.783.5306
Australia
Mulgrave, Victoria
Tel. +61.3.9566.1134
Austria
Vösendorf bei Wien
Tel. +43.1.699.9669
Benelux
Bergen Op Zoom
Tel. +31.164.282.800
Brazil and Latin America (S)
São Paulo
Tel. +55.11.820.0444
Canada
Mississauga, Ontario
Tel. 800.387.2216
China
Beijing
Tel. +86.106209.1727
Europe
Middelburg, The Netherlands
Tel. +31.118.671.000
France
Les Ulis Cédex
Tel. +33.1.6986.3838
Germany
Darmstadt
Tel. +49.6151.7030
India
Mumbai
Tel. +91.22.857.0787/88/89
Italy
Torino
Tel. +39.011.997.9111
Japan
Tokyo
Tel. +81.3.5232.1211
Korea
Seoul
Tel. +82.2.345.22452
Mexico and Latin America (N)
Mexico City
Tel. +52.5.523.9465
Russian Federation
Moscow
Tel. +7.095.937.4280
Spain
Madrid
Tel. +34.91.472.7612
Sweden
Solna
Tel. +46.8.445.1620
Switzerland
Varian AG
Tel. +41.848.803.800
Taiwan
Taipei Hsien
Tel. +886.2.698.9555
United Kingdom and
Ireland
Walton-on-Thames
Tel. +44.1932.898000
Venezuela
Valencia
Tel. +58.41.257.608
United States
Walnut Creek, California, USA
Tel. +1.800.926.3000
(GC and GC/MS)
Tel. +1.800.367.4752
(LC)
www.varianinc.com
4 of 4 03-914603-83:10
Page 30
Instrucciones de
S
CARG
C
A
S
O
O
Seguridad
Instrucciones de Operación
Este Manual de Instrucciones está diseñado para ayudarle a establecer las condiciones de operación que le permitan
operar su instrumento de forma segura y eficaz. Así mismo, se describen consideraciones especiales ó precauciones,
que aparecen en forma de
instrumento de acuerdo con este Manual de Operación y cualquier otra información que le proporcione Varian.
Remita a la Oficina Local de Varian cualquier cuestión que tenga respecto al correcto uso de su equipo.
NOTA, PRECAUCION, y ATENCIONcomo se indica más abajo.Es importante que utilice el
NOTA
Información para ayudarle a
obtener unas prestaciones óptimas
de su instrumento.
Símbolo Descripción
ATENCIÓN
PELIGRO DE
DE
AELÉCTRI
ATENCIÓN
PELIGRO DE
QUEMADURA
ATENCIÓN
PELIGRO DE FUEG
Le alerta de situaciónes que pueden
causar daños moderados a la salud
ó al equipo, y cóm evitar esas
situaciones.
El instrumento utiliza voltages peligrosos. Desconecte el interruptor
general antes de retirar los paneles atornillados.
Peligro de productos químicos. Evite el contacto, especialmente cuando
rellene los depósitos. utilice protección de ojos y piel.
Superficies posiblemente calientes ó frías (criogénico). Utilice
protección para la piel.
Las partículas volátiles, productos químicos o radiación UV pueden
causar daños en los ojos. Usar las debidas protecciones para la cara y los
ojos.
Peligro potencial de fuego. Siga las instrucciones del Manual de
Operación para su seguro funcionamiento.
¡PRECAUCION!
Le alerta de potenciales situaciones
peligrosas que pueden causar serios
daños, y cómo evitar esas
situaciones.
ATENCINÓ
ATENCIÓN
PELIGRO DE EXPLOSIÓN
ATENCIÓN
PELIGRO DE RADIACIÓN
Peligro potencial de explosión debido al tipo de gas ó líquido empleado.
Peligro por Fuente de radiación. Siga las instrucciones del Manual de
Operación para su seguro funcionamiento.
ATENCIÓN
PARTES EN MOVIMIENT
03-914603-84:101 of 4
Mantenga alejados los dedos y las manos.
Page 31
Precauciones Generales de Seguridad
Siga estas indicaciones de seguridad para una correcta operación del equipo.
Realice verificaciones periódicas de fugas en todas las líneas de suministro y tuberías.
No permita que las líneas de gas se doblen ó pinchen. Manténgalas alejadas de zonas de
paso y del calor ó frío excesivo.
Guarde los disolventes orgánicos en cabinas ventiladas, a prueba de fuego, y etiquetadas
para que puedan ser fácilmente identificadas como material tóxico y/ó inflamable.
No acumule disolventes inservibles. Deseche todo el material inservible a través de un
programa especial de desechos y no a través del sistema convencional.
NOTA:
Este instrumento ha sido testado bajo las normas de la Directiva EMC según requerimientos
de la Marca CE de la Unión Europea. Por lo tanto, este equipo puede ser sensible a niveles de
radiaciones / interferencias ó frecuencias que no estén incluidas dentro de los límites
testados.
ATENCINÓ
Este instrumento está diseñado para análisis cromatográfico de muestras preparadas
apropiadamente. Debe ser operado usando gases y/ó disolventes apropiados y con unos
niveles máximos de presión, flujos y temperaturas, según se describe en este manual.
ATENCINÓ
El Usuario tiene la obligación de informar al Servicio Técnico de Varian cuando el
instrumento vaya a ser empleado para análisis de muestras peligrosas de origen biológico,
radioactivo ó tóxico, antes de comenzar a realizar cualquier análisis.
Peligros Eléctricos
Desconecte el instrumento de todos las conexiones eléctricas a la red antes de retirar los
paneles para evitar la posible exposición a peligrosos voltages.
Cuando sea necesario emplear una clavija eléctrica no original, asegurese de colocar los
cables de acuerdo con el código de colores y polaridades descritos en el manual y los
códigos de seguridad de la red eléctrica.
Sustituya los fusibles fundidos con fusibles del tipo y tamaño estipulados en el panel de fusibles
ó en el manual.
Sustituya los cables deteriorados inmediatamente con cables del mismo tipo y
graduación.
Asegureses de que los valores de las líneas de electricidad se ajustan a los valores para
los que el Instrumento ha sido preparado.
Botellas de Gas Comprimido
Guarde y maneje las botellas de gas con cuidado y de acuerdo con las normas de seguridad.
Asegure las botellas a una estructura inmovil ó a la pared.
Guarde y mueva las botellas en posición vertical. Retire los reguladores antes de
transportarlas.
Guarde las botellas en un área ventilada, lejos de fuentes de calor, de luz solar directa y de
temperaturas extremadamente bajas.
Identifique las botellas claramente para evitar cualquier duda sobre su contenido.
Utilice sólamente reguladores y conexiones aprobadas.
Utilice sólo tubos de conexión cromatográficamente límpios (Varian p/n 03-918326-00) y que
tengan una graduación de presión significativamente mayor que la mayor presión del regulador.
2 of 403-914603-84:10
Page 32
GC Prácticas de Seguridad
Sistema de Extracción
No se necesita un sistema de extracción para los
detectores GC instalados en un laboratorio bien
ventilado, excepto cuando se analicen muestras
químicas peligrosas. Si instala un sistema de
extracción:
Nunca abra una línea ó una válvula bajo presión.
Apague la bomba antes y deje que la presión baje a
cero.
Utilice depósitos irrompibles que sean capaces de
operar a 50-60 psi.
Mantenga cerrada la junta del depósito cuando se
haye bajo presión.
Utilice conductos a prueba de fuego.
Instale un ventilador al final del sistema.
Instale entradas de aire cuya vibración no afecte al
trabajo del detector.
Compruebe periódicamente el correcto
funcionamiento del sistema.
Asegurese de una correcta ventilación del
laboratorio.
Detectores con fuentes radioctivas
Lea con cuidado y cumpla todas las NOTAS,
PRECAUCION, y ATENCIONdel Manual del
Detector Ni
Realice los test de contaminación radioactiva
descritos en el Manual del Detector Ni
Cumpla con los plazos y procedimientos de test de
63
ECD.
63
ECD.
fugas.
Peligro de Quemaduras
Las zonas de calor ó frío (criogénicas) del
Cromatógrafo de Gases pueden permanecer calientes ó
frías durante bastante tiempo después de apagar el
instrumento. Para evitar quemaduras asegureses de que
todas las áreas que se calienten ó enfríen han vuelto a la
temperatura ambiente, ó protejase adecuadamente las
manos, antes de tocar las superficies potencialmente
calientes ó frías.
Lea y cumpla todas las NOTA, PRECAUCION, y
ATENCIONdel manual.
Cromatografía Flash
El operador debe familiarizarse con las propiedades
físico-químicas de los componentes de la fase móvil.
Alejar los disolventes del contacto directo con los tubos
de poliuretano ya que ciertos disolventes pueden causar
reblandecimiento de los tubos o posibles fugas con
riesgo de explosión.
Todos los componentes del sistema deben estar
conectados a un enchufe común con toma de tierra
común. Esta toma de tierra debe ser una toma de tierra
verdadera en lugar de flotante.
Los disolventes no-polares pueden originar carga
estática cuando son bombeados por el sistema. Todos
los recipientes que contienen fase móvil (incluyendo
los tubos y los recipientes de recogida) deben estar
conectados a tierra para disipar la electricidad estática.
Utilizar medidores de carga estática y los debidos
dispositivos de descarga (por Ej., ionizadores de aire)
para salvaguardarse contra la creación de electricidad
estática.
Radiación Ultravioleta
Los detectores del Cromatógrafo de Líquidos que
utilizan una fuente de luz ultravioleta disponen de
protección para prevenir exposiciones radioactivas al
personal.
LC Prácticas de Seguridad
Peligro de Alta Presión
Si se rompe una línea de presión, ó se abre una válvula
de seguridad accidentalmente bajo presión, la bomba
puede generar líquidos a alta presión potencialmente
peligrosos, produciendo un chorro a alta velocidad de
líquidos volátiles y/ó tóxicos.
Lleve protección facial cuando inyecte muestras ó
realice mantenimiento de rutina.
Para una correcta protección:
Asegurese de que las cubiertas de protección de la
lámpara de los detectores está correctamente
situada durante su funcionamiento.
No mire directamente a las celdas del detector ó a
la fuente de luz UV. Cuando inspeccione la fuente
de luz ó la celda, utilice siempre una protección
para los ojos como gafas de borosilicato ó
poliestireno.
03-914603-84:103 of 4
Page 33
Disponibilidad de Recambios
Es Política de Varian disponer de Recambios para cualquier instrumento y
la mayoría de los accesorios por un periodo de cinco (5) años después del
último instrumento fabricado. Los recambios durante esos cinco años
estarán disponibles, pero siempre bajo el sistema “Según disponibilidad”.
Los Recambios están definidos como todas aquellas partes individuales
mecánicas ó eléctricas que son susceptibles de fallo durante su normal
proceso de operación. Por ejemplo, relés, lámparas, sondas de temperatura,
elementos del detector, motores, etc. Las planchas de metal, partes de la
estructura, placas de circuitos integrados, y otros módulos funcionales son
normalmente susceptibles de reparación y por lo tanto sólo estarán
disponibles bajos el sistema “Según disponibilidad” después del último
instrumento fabricado.
Disponibilidad de
Servicio
Varian ofrece una gran variedad de
sistemas de Servicio para mantener
el soporte a sus usuarios tras el
periodo de garantía. El Soporte de
Servicio se ofrece a través de
atractivos Contratos de Servicio ó
bajo un sistema de facturación de
mano de obra y materiales. El
mantenimiento y el entrenamiento
se realiza por ingenieros
cualificados bajo Contrato ó
petición.
Oficinas de Instrumentación Analítica Varian
Para cualquier consulta sobre Instrumentación Analítica, Servicio Técnico ó Recambios y Accesorios,
contacte con su oficina local:
Argentina
Buenos Aires
Tel. +54.11.4.783.5306
Australia
Mulgrave, Victoria
Tel. +61.3.9566.1134
Austria
Vösendorf bei Wien
Tel. +43.1.699.9669
Benelux
Bergen Op Zoom
Tel. +31.164.282.800
Brazil and Latin America (S)
São Paulo
Tel. +55.11.820.0444
Canada
Mississauga, Ontario
Tel. 800.387.2216
China
Beijing
Tel. +86.106209.1727
Europe
Middelburg, The Netherlands
Tel. +31.118.671.000
France
Les Ulis Cédex
Tel. +33.1.6986.3838
Germany
Darmstadt
Tel. +49.6151.7030
India
Mumbai
Tel. +91.22.857.0787/88/89
Italy
Torino
Tel. +39.011.997.9111
Japan
Tokyo
Tel. +81.3.5232.1211
Korea
Seoul
Tel. +82.2.345.22452
Mexico and Latin America (N)
Mexico City
Tel. +52.5.523.9465
Russian Federation
Moscow
Tel. +7.095.937.4280
Spain
Madrid
Tel. +34.91.472.7612
Sweden
Solna
Tel. +46.8.445.1620
Switzerland
Varian AG
Tel. +41.848.803.800
Taiwan
Taipei Hsien
Tel. +886.2.698.9555
United Kingdom and
Ireland
Walton-on-Thames
Tel. +44.1932.898000
Venezuela
Valencia
Tel. +58.41.257.608
United States
Walnut Creek, California, USA
Tel. +1.800.926.3000
(GC and GC/MS)
The Gas Chromatograph ........................................................................................................................................... 9
The Mass Spectrometer........................................................................................................................................... 10
Controls and Indicators...................................................................................................................................... 10
The Pneumatics Manifold.................................................................................................................................. 18
The Transfer Line .............................................................................................................................................. 19
Ion Trap Assembly............................................................................................................................................. 20
Ion Gauge .......................................................................................................................................................... 24
The Power Input Subsystem and Turbomolecular Pump Controller ................................................................. 27
Main Power Circuit ............................................................................................................................................ 27
Power Board...................................................................................................................................................... 28
The RF Generator Assembly............................................................................................................................. 29
The Manifold Electronics Assembly .................................................................................................................. 30
The Data System ..................................................................................................................................................... 32
The Computer .......................................................................................................................................................... 32
The AutoSampler ..................................................................................................................................................... 32
Chemical Ionization Options................................................................................................. 33
Installing CI Reagent Gas ........................................................................................................................................ 33
CI Reagent Gas Requirements ......................................................................................................................... 34
Setting Up the CI Reagent Gas Supply............................................................................................................. 34
Checking the Reagent Gas Plumbing for Leaks ............................................................................................... 37
Setting Flows of CI Reagents .................................................................................................................................. 37
Default Parameters for Gaseous CI Reagents.................................................................................................. 38
Default Parameters for Liquid CI Reagents....................................................................................................... 38
Ion Intensities for Standard CI Reagents .......................................................................................................... 39
Setting CI Gas Pressure in a Diffusion Pump System ...................................................................................... 39
The Liquid CI Inlet Option ........................................................................................................................................ 40
Installation of the Liquid CI Inlet ........................................................................................................................ 40
Filling/Refilling the Liquid CI Reservoir Bulb ..................................................................................................... 43
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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
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
Check Cooling Fans Turbomolecular Pump System ............................................................................................... 82
How to Replace the Turbomolecular Pump ............................................................................................................. 84
Check Cooling Fans Diffusion Pump System .......................................................................................................... 86
Checking the Diffusion Pump Fluid Level and Condition......................................................................................... 87
Turning Off the Diffusion Pumped Mass Spectrometer ........................................................................................... 88
Replacing the Diffusion Pump Thermocouple Gauge.............................................................................................. 89
Replacing the Diffusion Pump Peltier Baffle ............................................................................................................ 90
Cleaning the Diffusion Pump Peltier Baffle .............................................................................................................. 91
Removing the Diffusion Pump ................................................................................................................................. 92
Topping Off the Diffusion Pump Fluid Level ............................................................................................................ 93
Cleaning the Diffusion Pump ................................................................................................................................... 94
Changing the Diffusion Pump Heater ...................................................................................................................... 96
Reinstalling the Diffusion Pump ............................................................................................................................... 97
Turning on the Mass Spectrometer.......................................................................................................................... 99
How to Service the Ion Trap .................................................................................................................................. 100
Turn off the Mass Spectrometer ............................................................................................................................ 101
Retract/Remove the Transfer Line......................................................................................................................... 101
2000 MS Hardware Maintenance
2
Contents
Page 36
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
General GC Maintenance ...................................................................................................................................... 116
Check and Renew Gas Supplies..................................................................................................................... 116
Gas Purifier Replacement ............................................................................................................................... 117
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
03-914978-00:1
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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
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
Correction of Poor Resolution1........................................................................................................................ 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
Troubleshooting of Diffusion Pump System ..................................................................... 151
Problems During Startup........................................................................................................................................ 151
Problems During Routine Operation...................................................................................................................... 152
Miscellaneous Procedures and Instructions..................................................................... 155
Other Documents ................................................................................................................................................... 155
Site Requirements ................................................................................................................................................. 155
Site Preparation ............................................................................................................................................... 155
Quality of Power .............................................................................................................................................. 157
Temperature .................................................................................................................................................... 158
Gas Requirements ................................................................................................................................................. 159
Helium - GC Carrier Gas ................................................................................................................................. 159
Methane, Isobutane - CI Reagent Gases (with CI option only)....................................................................... 159
Ammonia - CI Reagent Gas (with CI option only) ........................................................................................... 159
Other Gases .................................................................................................................................................... 160
How to Install Saturn .............................................................................................................................................. 160
How to Move Saturn .............................................................................................................................................. 160
2000 MS Hardware Maintenance
4
Contents
Page 38
Parts and Supplies ................................................................................................................................................. 161
Kits, Assemblies, Boards, and Cables ............................................................................................................ 161
Tools, Test Samples, etc................................................................................................................................. 164
CI Parts/Spares ............................................................................................................................................... 165
Multiple CI Module Parts Lists ......................................................................................................................... 165
Open Split Interface......................................................................................................................................... 166
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.
03-914978-00:1
Functional Description
7
Page 41
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)
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8
Functional Description
Page 42
Technical Specifications
NOTE: Specifications are identical for turbomolecular pump and diffusion pump
GC/MS systems unless specified.
Saturn 2000 GC/MS System Performance
Specifications
Ionization Mode:
MS/MS:
consistency and wide dynamic range. Patented non-Resonant dissociation provides
spectral consistency and wide dynamic range, as well as additional spectral information
via cascading.
10 to 650 u. Scan range time programmable throughout the analysis.
Two dedicated Fourplexes,
Ultra high purity helium;
Electron Ionization standard, Chemical Ionization optional.
Up to 10 Hz, depending upon mass range selected.
CI Reagent Gases:
ammonia - purity 99.99%.
Environment:
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
Methane, isobutane,
Combined GC/MS/DS will
The Gas Chromatograph
The Saturn GC/MS employs the high performance Varian Model 3800 or 3900
Gas Chromatograph. The gas chromatograph comes with a 1079 or 1177
Universal Capillary Injector which provides five modes of injection - isothermal
split and splitless, temperature-ramped splitless, on-column and large volume.
For further details about the GC, please see the Varian 3800 Gas
Chromatograph Getting Started Manual (03-914647-00) and the 3800 GC
Operator's Manual (03-914648-00).
03-914978-00:1
Functional Description
9
Page 43
The Mass Spectrometer
The Saturn GC/MS employs an ultra trace ion trap mass spectrometer. The
mass spectrometer consists of the mechanical and electronic assemblies. The
following sections describe these assemblies.
The instrument is separated into the electronics and analyzer compartments.
The electronics compartment includes the
The Saturn mechanical assemblies include the following:
•
Controls and indicators
•
Cooling fans
•
Vacuum system
•
Transfer line
•
Ion trap assembly
Controls and Indicators
The main power switch for the Saturn GC/MS, located on the rear panel, controls
power to the vacuum system and to the electronics.
When the main power switch is turned on, the light-emitting diode (LED) on the
Saturn GC/MS front panel is illuminated.
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.
2000 MS Hardware Maintenance
10
Functional Description
Page 44
A Main Power Switch (rear
panel)
B Service Switch K Vent Valve
C Transfer Line Heater L RF Coil
D Trap Heater M RF Coil Adjustment Screw
E Manifold Heater N Transfer Line
F LED O Turbomolecular Pump
G Pneumatics Manifold P Cooling Fans
H CI Cal Gas Adjust Q CI Shutoff Valve
I Cal Gas Adjust
Saturn 2000 GC/MS Mass Spectrometer
J Cal Gas Vial
Cooling Fans
To prevent overheating, do not block air intakes.
03-914978-00:1
Turbomolecular Pump System
Two fans mounted on the rear of the spectrometer cool the unit. The analyzer
compartment fan draws air from the back, blowing it directly on the bearing end
of the turbomolecular pump in the analyzer compartment. The air then flows past
the manifold electronics and out the front of the instrument. The turbomolecular
pump controller supplies power to the analyzer compartment fan.
Functional Description
11
Page 45
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.
Diffusion Pump System
The GC/MS Diffusion pump system has three cooling zones, each with its own
fan mounted in the rear of the instrument.
Cooling Zones
Zone 1
is the upper part of the analyzer compartment. Its purpose is to provide
forced air-cooling for the Peltier baffle’s 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 baffle’s 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 instrument’s 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.
2000 MS Hardware Maintenance
12
Functional Description
Page 46
Zone 3
air in through carefully positioned vents in the left side panel. Airflow is ducted
around the diffusion pump’s cooling fins, and expelled through the rear of the
instrument.
is the diffusion pump compartment. The lower fan on the rear panel pulls
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.
Turbomolecular Pump Vacuum System
The turbomolecular vacuum system evacuates excess water vapor, air, and
carrier gas from the mass spectrometer ion trap assembly. Principal
turbomolecular vacuum system components include
•
Vacuum manifold
•
Turbomolecular pump
•
Foreline pump
•
Vent valve
•
Calibration gas valve
•
CI reagent gas valves
Below is a diagram of the vacuum system.
03-914978-00:1
The Saturn Turbomolecular Vacuum System
Turbomolecular Pump Vacuum Manifold
The vacuum manifold, which can be heated for bake out, encloses the ion trap
assembly. The vacuum manifold is a stainless-steel tube, which houses the
analyzer. The turbomolecular vacuum pump, which evacuates the manifold,
discharges into a foreline pump. (Also see Diffusion Pump Vacuum System
section for additional vacuum manifold information for the diffusion pump
system.)
Functional Description
13
Page 47
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
Turbomolecular Vacuum Pump
A turbomolecular vacuum pump provides the high vacuum for the Saturn GC/MS.
Under normal operating conditions, this pump supplies a vacuum of
approximately 10
assembly. The pump is rated at 70 liters/second and operates at 60 liters/
second; it is air cooled and thermostatically protected. If the temperature of the
pump housing near the bearing exceeds 60 °C, the pump speed will
automatically shut down.
A turbomolecular-pump controller regulates and supplies power to the pump.
The controller sits below the pump in the analyzer compartment of the
spectrometer. Turning off the main power switch on the rear panel of the mass
spectrometer shuts off power to the turbomolecular-pump controller and thus to
the pump.
NOTE: The electronics service switch does not control the vacuum pumps.
-5
Torr (1.33x10
-3
Pa) in the manifold region outside the ion trap
2000 MS Hardware Maintenance
The turbomolecular-pump controller monitors the pump’s rotational speed. The
controller sends a signal proportional to the pump speed to the SAP/Wave board
via the power board. You can monitor the turbomolecular pump speed from the
Instrument Control Page.
14
Functional Description
Page 48
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.
Diffusion Pump Vacuum System
The diffusion pump is an alternative vacuum pump to the turbomolecular pump.
It is less costly to replace, has a longer life span, and can be operated in ambient
temperatures up to 35 °C. However, servicing the instrument does take slightly
longer because the diffusion pump must be fully cooled and the Peltier baffle
warmed up to room temperature before breaking vacuum.
The diffusion pump vacuum system removes air, carrier gas, adsorbed water
vapor, and analytes from the mass spectrometer ion trap assembly. Principal
diffusion pump components are shown, and include:
•
Vacuum manifold
•
Peltier baffle
•
Diffusion pump
•
Thermocouple gauge
•
Foreline pump
•
Vent valve
•
Calibration gas valve
•
CI reagent gas valves (optional)
Saturn Diffusion Pump Vacuum System
03-914978-00:1
Functional Description
15
Page 49
Diffusion Pump Vacuum Manifold
The vacuum manifold is a stainless steel tube that maintains the ion trap
assembly in a vacuum. Carrier gas is fed into the ion trap via the transfer line,
and calibration gas and Chemical Ionization gases are fed into the ion trap via
the pneumatics assembly. The vacuum manifold is evacuated and maintained at
vacuum of approximately 1 x 10
Peltier baffle is incorporated in the manifold to minimize background
contamination caused by the back streaming of pump vapors.
The vacuum manifold, analyzer assembly, pneumatics assembly, Peltier baffle,
and diffusion pump, are shown.
-5
Torr (1.3 x 10-3 Pa) by a diffusion pump. A
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.
2000 MS Hardware Maintenance
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Functional Description
Page 50
Diffusion Pump
The ion trap assembly requires a vacuum of approximately 1 x 10-5 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.
Diffusion Pump Controller
The diffusion pump controller controls and provides power to the following
vacuum components:
•
TEC in the Peltier Baffle
•
Peltier baffle fan
•
Diffusion pump
•
Diffusion pump fan
•
Thermocouple gauge
The diffusion pump controller is activated when the system’s 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 pump’s
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.
03-914978-00:1
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.
Functional Description
17
Page 51
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
measure vacuum pressures in the 2 Torr (267 Pa) to 1 x 10
-3
Torr (1.3 x 10-1 Pa)
range. The gauge’s 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 pump’s required operational pressure. Once the
diffusion pump is operational, the thermocouple gauge is monitored to ensure the
operational pressure is maintained.
The Pneumatics Manifold
The pneumatics manifold is an aluminum block mounted to the front of the
vacuum manifold. It is equipped with two solenoid and needle valves for the cal
gas and CI, the glass cal gas vial, and vent valve.
The vent valve is a manually operated valve that connects to atmosphere via the
pneumatics manifold. You open and close the vent valve via a toggle arm, which
is accessible from the front of the instrument.
The calibration-gas-valve assembly consists of a metering needle valve, an
ON/OFF solenoid-operated valve, and a glass vial containing the calibration
liquid. The assembly sits directly behind the instrument’s door. The needle valve
controls calibration gas flow into the vacuum manifold through the solenoid valve.
The calibration compound is perfluorotributylamine (PFTBA) or C
known as fluorocarbon-43 (FC-43). A small glass vial attached to the valve
assembly holds the compound. You set the flow of calibration gas into the
manifold manually via a needle valve. The data system controls the opening and
closing of the solenoid-operated valve.
12F27
N, also
2000 MS Hardware Maintenance
Two solenoid valves control the flow of CI reagent gas into the manifold. First,
the shutoff valve near the rear panel opens to permit reagent gas flow into the
instrument through a fitting. When this valve is open, the foreline pump removes
a portion of the CI gas to prevent CI gas surges (pressure pulses) in the ion trap.
The gas then flows through the shutoff valve through metering and solenoidoperated valves before entering the vacuum manifold. With the CI gas solenoid
open, the CI needle valve determines the split ratio of the reagent flow between
the manifold and foreline pump.
You turn the CI reagent gas valve on and off via the data system from the
Instrument Control Page or Acquisition, you adjust the flow rate of the reagent
gas into the manifold by means of a metering valve.
18
Functional Description
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The Transfer Line
A stainless-steel-tube transfer line directly couples the GC to the mass
spectrometer. The transfer line keeps the GC column warm as the column
enters the mass spectrometer. The transfer line is 12 cm (5 in.) long, and has a
diameter of 4.1 cm (1.6 in.). One end enters a hole in the right side of the GC
before passing into the GC oven. The other end enters the vacuum manifold
with the transfer-line tip inserted into the ion trap.
The body of the transfer line consists of a stainless-steel weldment fitted with a
center tube, a heat exchanger, and a boot. The heat exchanger is an aluminum
cylinder that contains a cartridge heater and a thermocouple as the temperature
sensor. The temperature sensor measures the temperature of the tube. The
cartridge heater heats the cylinder, which in turn distributes heat evenly
throughout the length of the transfer line tube. The boot of the transfer line,
which mates to the GC, prevents hot air leakage from the GC Oven.
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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A Heating Cable H O-ring
B Boot I Transfer Line Tip
C Nut J Heating Cable Slot
D Ferrule K Nose Clip
E Transfer Line/Alignment
Tool
F Nose M Analyzer Assembly Tongue
G Nose Hole N Analyzer Assembly Lock-Down Tabs
Transfer Line Exploded View
L Bayonet Mount
Ion Trap Assembly
The ion trap assembly consists of
•
Trap oven
•
Filament assembly
•
Electron gate
•
Ion trap electrodes (3)
2000 MS Hardware Maintenance
•
Quartz rings
•
Electron multiplier assembly
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.
20
Functional Description
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A Screw, 6/32, 4 places H Wave Washer
B Clamping Plate I Gate Conductor
C Exit End Cap J Trap Oven, “T” is located this side.
D Quartz or Silica Coated Spacer, 2 places K Filament Assembly
E RF Ring Electrode L Filament Clip
F Filament End Cap M Screw
G Electron Gate
Ion Trap Assembly
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 oven’s 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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Filament Assembly Shown with Ion Trap
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 µA.
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 µsec 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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Ion Trap Electrodes
The ion trap assembly contains three stainless steel electrodes:
•
Filament endcap electrode
•
Exit endcap electrode
•
RF ring electrode
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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A Exit End Cap F Multiplier Contacts
B Electron Multiplier Track G Multiplier High Voltage Pin
C Multiplier Signal Pin H Transfer Line Alignment
D EM Grid I Transfer Line Entrance Hole
E Electron Multiplier Mount
Position of the Electron Multiplier Relative to the Ion Trap
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
about 10
approximately 10
5
, i.e., until each ion that enters the electron multiplier generates
5
electrons.
2000 MS Hardware Maintenance
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
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Foreline Pump
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
amplifier amplifies the collector current, and the data system interprets this
current as measured vacuum.
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 pump’s 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.
-6
and 10-2 Torr. A logarithmic
The foreline pump used on the Saturn GC/MS is a two-stage rotary vane pump
with a pumping speed of 90 µL/min. and a vacuum potential of 1.5 x 10
(2 x 10
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.
-1
Pa).
Electronic Assemblies
The electronic assemblies consist of the following:
•
Power input subsystem and turbomolecular (or diffusion) pump controller
(See Diffusion Pump Controller).
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.
2000 MS Hardware Maintenance
The Saturn 2000 GC/MS Turbomolecular Pump Electronic Assemblies
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Functional Description
Page 60
The Saturn 2000 GC/MS Diffusion Pump Electronic Assemblies
The Power Input Subsystem and Turbomolecular
Pump Controller
The power input subsystem contains the following circuits and switches:
•
Main power switch
•
SERVICE switch
•
Line voltage switches
Main Power Circuit
Line power of 115 Vac ±15%, 60 Hz ±3 Hz (or 230 ±15 Vac, 50 Hz ±3 Hz) first
enters the rear panel of the mass spectrometer, through J1, then passes through
the line filter and the circuit breaker. After the circuit breaker, power is split in two
directions. One path supplies the turbomolecular pump controller and foreline
pump via J2. The second path goes to the electronics service switch, which
controls power going to the power board and the rest of the electronics. The
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electronics service switch allows the vacuum to the maintained in the event that
D
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 HAZAR
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 board’s 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 µA 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).
2000 MS Hardware Maintenance
•
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
Page 62
•
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.
The RF Generator Assembly
The RF generator assembly consists of an RF generator circuit board, an RF
detector circuit board, and the RF coil. A shielded housing beneath the vacuum
manifold encloses the coil and RF detector circuit board. The RF generator
circuit board is attached to the back of the shielded housing.
The RF generator circuit board receives an analog signal from the SAP/Wave
circuit board that is proportional to the current mass position in the scan, which is
in turn proportional to the desired RF voltage applied to the ion trap. The RF
detector circuit board sends a signal proportional to the actual amount of RF
voltage applied to the ion trap to the RF generator board. The RF generator
board compares the desired and actual amount of the RF voltage and adjusts the
gain of an RF amplifier to cause the actual RF voltage to equal the desired RF
voltage. Since the high voltage required at the ion trap exceeds the capabilities
of conventional electronic amplifiers, a resonant LC circuit consisting of the RF
coil and the ion trap capacitance is used. At resonance, the RF voltage at the ion
trap end of the coil is about 100 times that at the RF generator circuit end of the
coil.
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Functional Description
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The Ion Trap Assembly
The Manifold Electronics Assembly
Two boards reside in the enclosure directly atop the Analyzer flange. The
following circuitry, which is critical to the functioning of the ion trap or that must
be in close proximity to the trap, resides on these boards.
•
The electron multiplier power supply, which supplies high voltage (-800
to -3000 Vdc) to the cathode of the electron multiplier.
•
The integrator circuit, which receives the amplified ion current from the
anode of the electron multiplier, converts the current into voltage, e.g.,
-7
10
A into 1.0V, and passes the voltage on to the SAP/Waveboard.
•
The trap filament selection relay.
•
The electron gate control that controls the gate polarity.
•
The axial-modulation low and high frequency transformers.
•
The ion gauge support circuitry, which includes filament On/Off and
selection relays and a log amplifier for gauge read-back signal
conditioning.
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Functional Description
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•
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 board’s 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
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•
A 12-bit DAC, low pass filter and amplifier to reconstruct waveforms
Functional Description
31
Page 65
The Data System
•
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.
The data system (DS) has both hardware and software components. The
hardware includes a computer/instrument interface, personal computer, video
display monitor, and optionally, a printer.
The software stored on the fixed disk drive includes programs to control the
Saturn GC/MS, to automatically set Saturn system parameters, and to oversee
scan-control, data-acquisition, and data-processing programs. For a complete
description of Saturn software, refer to the
Saturn Software Reference Manual
.
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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Chemical Ionization Options
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.
Installing CI Reagent Gas
Before evacuation, new gas lines will contain a significant amount of adsorbed
water vapor. The longer the gas line, the greater the amount of adsorbed water
and the greater the pumping time required to evacuate water from the line. To
minimize the pumping time required to evacuate the gas line, we recommend
that the line be as short as possible. Make sure, however, that the gas line is
long enough to run to the rear of the Saturn GC/MS and to accommodate the
movement of the mass spectrometer 9 inches (23 cm) to the right (for access to
the transfer line and turbomolecular pump).
Gas cylinders or lecture bottles should not be stored where they can damage
cables or gas lines, and they should be secured in accordance with standard
safety practices. Lecture bottles have rounded ends and will require some
means of support (e.g., Matheson Model 505 Non-Tip Stand).
Before installing the CI reagent gas supply, you should complete the following
procedures:
•
Tune the instrument in EI mode
•
Check the Saturn GC/MS system for leaks
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CI Reagent Gas Requirements
These paragraphs give the requirements for the reagent gases used for CI
operation with Saturn GC/MS. The following reagent gases are recommended:
methane, isobutane, and ammonia. Other reagent gases can also be used
successfully with the Saturn GC/MS.
We recommend that you use a high-purity reagent gas for maximum sensitivity
and good spectral quality. Impurities in the reagent gas may limit the number of
sample ions that can be formed, thus reducing spectral sensitivity. In addition,
impurities may react with sample ions, thereby creating confusing mass spectral
data.
The amount of reagent gas consumed during CI operation is very low (typically 1
to 2 mL/minute). We recommend that you use a K size gas cylinder of the
selected reagent gas.
The requirements for the recommended gases are as follows:
Methane Methane should have a purity of 99.99% or better. Use a
gas cylinder with a two-stage pressure regulator that has a
stainless steel diaphragm and maximum inlet pressure of
15 psi (1 bar).
Isobutane Isobutane should have a purity of 99.99% or better. Use a
gas cylinder with a two-stage pressure regulator that has a
stainless steel diaphragm and maximum inlet pressure of
15 psi (1 bar).
Ammonia Ammonia should have a purity of at least 99.99% and be
anhydrous grade. Use a gas cylinder with a two-stage
pressure regulator that has a stainless steel diaphragm and
maximum inlet pressure of 15 psi (1 bar).
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.
Setting Up the CI Reagent Gas Supply
Use the following procedure to set up the CI reagent gas supply.
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Chemical Ionization Options
Page 68
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
Vacuum Pump
Diffusion Pump Vacuum System
or
Turbomolecular
.
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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.
2000 MS Hardware Maintenance
d. Evacuate the CI reagent supply line for about 30 minutes.
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Checking the Reagent Gas Plumbing for Leaks
To check for air leaks in the reagent gas line connections and the presence of
water vapor in the gas line, follow the procedure using a Leak Detection Gas to
Troubleshoot for Air Leaks in the Troubleshooting Section. Depending upon the
results you obtain, you may need to modify the procedure as follows:
If a large air leak exists, check the CI GAS fitting on the rear of the instrument
and the fitting on the pressure regulator for tightness. Then recheck the air/water
spectrum; or
If excess water vapor is indicated by a high 19/18 ratio, there may be water in the
gas line and/or an atmospheric air leak in the reagent gas plumbing. Proceed as
follows:
1. Shut off the flow of reagent gas into the manifold by closing the CI solenoid
valves. If necessary, click on the CI icon in the Control and Status field of the
Manual Control tab dialog in System Control. When the valves are closed,
the CI button is black or red - not green.
2. Recheck the air/water spectrum. If the peak at mass 19 (for water)
decreases, then water is present in the gas line. In this case, go to step 3. If
the peak at mass 19 does not decrease significantly, little water is present in
the gas line. In this case, the MS system probably has an air leak. You will
need to fix the leak as described in the Troubleshooting Section. Be sure to
check for leaks around:
•
The CI GAS port on the rear of the mass spectrometer
•
The fitting that connects the reagent gas line to the pressure regulator
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.
Setting Flows of CI Reagents
After any leaks have been located and fixed, set the delivery pressure of the CI
reagent gas as follows:
1. Ensure that the CI gas solenoid valves are closed. If necessary, click on the
CI icon in the Control and Status field of the Manual Control tab dialog in
System Control. When the valves are closed, the CI button is black or red not green.
03-914978-00:1
2. Open the main valve on the lecture bottle. Using the pressure adjustment
valve on the regulator set the head pressure to about 5 psi (34 kPa).
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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.
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]+.
65 65 55
2000 2000 2000
40 20* 40
100 100 100
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Ion Intensities for Standard CI Reagents
The CI Adjust function gives recommendations of an acceptable level of CI
reagent ions for each of the five standard CI reagents. The general principles
used in implementing these tests are:
Methane Adjust the reagent gas pressure so that the peak
heights at m/z 17 (CH
equal. The ratio of the ions at m/z 17 to m/z 16 should
be about 10:1. The ion at m/z 41 (C
visible.
Isobutane Adjust the reagent gas pressure so that the peak
heights at m/z 57 [(CH3)3C+] and m/z 43 [(CH3)2CH+] are
about equal. There may also be an intense reagent ion
at m/z 41 (C
3H5
Ammonia Adjust the gas pressure so that the ratio of the peak
heights at m/z 18 [(NH3)H+] to m/z 17 (NH
10:1.
Acetonitrile Adjust the reagent gas pressure so that the ion at m/z
42 [CH3CNH+] is about 10 times higher than at m/z 41.
The valley between the 41/42 ions should reach a
minimum at less than half the height of the m/z 41 ion.
The m/z 54 ion [CH
15% the height of m/z 42. Too much acetonitrile in the
trap can cause early filament failures.
d3-Acetonitrile Adjust the reagent gas pressure so that the ion at m/z
46 [CD3CND+] is about 10 times higher than at m/z 44.
The m/z 58 ion [CD3CDCND+] will be present at 10 15% the height of m/z 46.
Methanol The ion at m/z 33 [(CH3OH)H+] will dominate the
spectrum. No ion is observed at m/z 32, but a small
peak is observed at m/z 31 and m/z 47.
+
) and 29 (C2H
5
+
).
CHCNH+] will be present at 10 -
3
+
) are about
5
+
) should be
3H5
+
) is about
3
03-914978-00:1
In each case, by following these guidelines, the reagent gas pressure in the ion
trap will be approximately 1 to 2 x 10
-5
Torr (about 1.3 to 2.6 x 10-3 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.
Setting CI Gas Pressure in a Diffusion Pump System
For the diffusion pump system, the CI Reagent Gas delivery pressure should be
set to only 5 psi as indicated on the pressure regulator. The foreline pressure
should then be checked:
•
Start System Control and click on the Diagnostics tab.
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•
Note the
System field. The reading should be less than 100 mTorr. Higher
readings may indicate problems (i.e., leaks) and the user should refer to
Troubleshooting
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
Pressure
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.
The Liquid CI Inlet Option
You may review the installation and use of the Liquid CI Inlet on the Saturn 2000
Maintenance Tutorial CD. Alternatively, you may read the instructions that follow
in this section.
Installation of the Liquid CI Inlet
1. Before beginning, shut down and vent the Saturn system. If you are not
disassembling the trap, it is not necessary to wait for the trap electrodes to
cool down before installing the Liquid CI Inlet assembly.
Diffusion Pump Foreline Pressure
section for additional information. Click on the
reading. The value should be less than 350 mTorr. If
reading under the Vacuum
Diffusion Pump Foreline
2000 MS Hardware Maintenance
2. Remove the top cover. Attach the Liquid CI Inlet assembly to the back of the
instrument using the following instructions. Refer to the drawings below to
more easily identify the parts discussed.
a. From the back of the instrument, remove one of the two screws that hold
the CI shutoff block intact. Replace it, loosely, with a long screw
supplied with the kit (12-222006-25).
b. Remove the remaining screw.
c. Gently pull the free end of the liquid CI restrictor tube (03-930024-01)
from the L-bracket where it attaches to the back of the instrument, while
leaving the other end of the restrictor tube attached to the Liquid CI Inlet
block.
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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 (12-222006-
25).
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 Inlet Block (03-930023-01) E Reservoir Cover (03-930026-
01)
B Viton O-ring (03-930109-07) F Restrictor (03-930024-01)
C O-ring Retainer (03-930025-01) G L-Bracket (03-930027-01)
D Reservoir Bulb, same as Cal
Gas Chamber (03-920270-00)
H Viton O-Ring (03-930109-04)
3. Replace long restrictor (03-930597-01) with 1/8" OD PEEK tubing (03-930037-
01).
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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Filling/Refilling the Liquid CI Reservoir Bulb
1. Be sure the CI valves are closed. Disengage the 4 screws that retain the
liquid CI reservoir cover. They may remain in the block.
2. Remove the reservoir cover.
3. Gently pull the bulb down to remove it from the block. The O-ring and O-ring
retainer may stay attached to the bulb.
4. Use the reservoir cover as a stand for filling; place the bulb into the reservoir
cover. Place O-ring retainer over the bulb stem. Place the O-ring over the
bulb stem.
5. Use a pipette or syringe to fill the bulb halfway with liquid CI reagent. This
requires about 3 mL of reagent.
6. Pick up the reservoir cover with the bulb, retainer and O-ring, and insert the
bulb stem into the block.
7. Orient the cover so that the 4 screws can engage the cover. Tighten the 4 screws, being careful not to strip the threads in the plastic cover.
8. After installing liquid CI, and each time the reservoir bulb is refilled with liquid, always use care when first opening the CI valves. Do not turn on the filament or multiplier for about 2-3 minutes after opening the CI valves from the Instrument Page. 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 the pressure has returned to less than 35 x 10Filament and Multiplier. For diffusion pumped systems monitor the foreline pressure. Adjust the CI valve to prevent the foreline pressure from exceeding 500 mTorr. Turn the valve clockwise to reduce the pressure.
-6
Torr before turning on the
Use Polypropylene Caps to Preserve Liquids in
Reservoirs
Yellow polypropylene caps have been provided to seal reservoirs containing
liquid CI reagents when they are not installed on the instrument.
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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Setting Flows of Vapor from Liquid CI Reagents
1. Connect a liquid reagent reservoir containing the chosen liquid to the liquid
reagent inlet block.
2. Open the CI needle valve 6-7 turns counterclockwise.
3. Open the CI solenoids by clicking on the CI button on the Manual Control
page and allow the vapor flow from the reservoir to equilibrate. If, after
several minutes, there is not enough CI gas entering the trap, increase the
flow by turning the needle valve clockwise.
4. While observing the spectrum using Adjust CI Gas, turn the CI needle valve
to increase or decrease the amount of reagent entering the trap until the
resolution between M and M+1 just starts to degrade. For best results when
using acetonitrile, use a filament emission current of at least 20 µA and
maintain at least 50% valley between m/z 41 and m/z 42. A convenient way
to examine the valley is to click on the top of the m/z 41 peak and drag it to
the top of the display using the cursor. See below for a properly adjusted
acetonitrile spectrum and for a properly adjusted methanol spectrum.
Properly Adjusted Acetonitrile Reagent Spectrum
Properly Adjusted Methanol Reagent
Returning to Gaseous CI Reagent Operation
To switch from the Liquid CI Inlet back to a pressurized CI gas (such as
methane), the CI gas line may be re-installed without removing the liquid CI inlet
assembly.
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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.
Installing and Using the Multiple CI Module
The MCI Module operates essentially as a triplicate of the Standard CI option in
the Saturn
diagram of the module. A liquid (or optional gas) sample is chosen for Channel A.
Two solenoid valves intervene between the liquid sample and the main gas line
to the Saturn MS on the right of the diagram. These valves are always controlled
together — both ON or both OFF. The control of the Valve States is from the
External Events (Valve States) section of the GC. The valves may be turned ON
and OFF either from the GC front panel or from the GC section of the GC/MS
Method. The restrictors between the two solenoid valves for each Channel have
been chosen to provide an adequate and adjustable flow of acetonitrile,
methanol, methane, or isobutane flow when the MCI Module is set up according
to instructions. A third, adjustable, restrictor is the Needle Valve in the line
connected to the foreline Pump.
The guiding principle in the design of CI flow is to provide an adequate flow of
reagent vapor, which is adjustably split toward the foreline pump and the ion trap.
Closing the 15-turn needle valve clockwise (CW) directs more flow to the ion
trap; counterclockwise adjustment sends a higher proportion of the flow to the
foreline pump. This two-directional flow pattern allows the foreline pump to
rapidly clear residual CI reagent from the MCI Module when the Main CI Solenoid
in the Saturn 2000 (lower right of the schematic) is turned off in Manual Control.
It also allows rapid changeover of flows from one Channel to another.
®
2000. Examine the Channel A section of the following schematic
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Schematic Diagram of the MCI Module
Multiple CI Module (shown with and without cover)
Pre-Installation Checklist
1. Preparing the Mass Spec
a. The Saturn MS should be shut down, vented, and unplugged.
2. Tools Required
2000 MS Hardware Maintenance
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
Installing the Multiple CI Assembly
1. Run the Saturn Software.
2. Select Shutdown and wait for the system to shut down.
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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.
2000 MS Hardware Maintenance
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.
03-914978-00:1
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
D
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
C
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.
A
B
WARNING:
SHOCK HAZAR
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.
Cable Connections to the GC External Events Board
A cable to the External Events board of the GC connects each Channel of the
MCI Module. Upon installation of the MCI Module, make these connections and
identify the External Events connected to each Channel of the MCI Module. For
3800 GCs which have seven External Events, the most likely scenario is that
External Events 1, 2, and 3 will be connected to Channels A, B, and C on the
MCI Module. For 3400/3600 GCs, which have four External Events, the most
likely scenario is that External Event 1 will be used to control split and splitless
modes in a 1078 injector. Then Events 2, 3, and 4 will be connected to Channels
A, B, and C on the MCI Module. Assure that you are aware of the connection
pattern for your system.
For easiest reference in the future, we suggest that you use an erasable marking
pen to write the number of the External Event along with the installed reagent on
the label for each Channel of the MCI Module.
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Adding Liquid CI Reagents to the MCI Module
The addition of liquid reagents to the MCI Module is accomplished in much the
same manner as addition of liquid reagent to the single Liquid CI option (LCI).
The LCI liquid filling process is shown in detail on the Saturn Maintenance
Tutorial CD under the heading
In the MCI Module, this sequence is followed:
1. Turn off all relays related to the MCI module.
MS Maintenance … CI Installation
.
2. If you have a
system:
valve by turning the knob clockwise. This will reduce the inrush of air into the vacuum system when 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 MCI Manifold. Any of the liquid CI reservoirs may now be removed by rotating the bulb and pulling down, away from the manifold. Be careful not to break the fragile necks of the bulbs. Be sure to keep bulbs installed in all positions of the MCI Manifold, whether they contain a liquid reagent or are empty.
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 ¼ 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.
turbo pump system
For each channel that will be worked on, close the associated needle
, skip this step. If you have a
diffusion pump
2000 MS Hardware Maintenance
10. If you have a
system
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 ½ 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
the pressure has returned to less than 35 x 10
filament and multiplier.
turbo pump system
, first turn on the relays, then open the needle valves slowly by turning
, skip this step. If you have a
-6
Torr before turning on the
diffusion pump
Adding Gaseous Reagents to the MCI Module
To change a channel from liquid operation mode to gaseous, follow the
procedure given in the MCI Module Maintenance section.
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Adjusting Flows of CI Reagents
There are two ways to turn Channels of the MCI Module On and Off. The
simplest way, which you may want to use when you are adjusting CI flows, is
from the keyboard of the GC. The second way is to program a GC/MS Method in
the Saturn GCMS Workstation software and download the method to the GC. To
select reagent Channels, first identify which External Event is connected to
Channel A, B, or C. If you have a 3800 GC, make sure that these External
Events are configured from the GC keyboard.
Selecting Reagent Channels from the 3400/3600 GC Keyboard
To program reagent Channels from the 3400/3600 GC keyboard, select the
External Event (or Relay) for the chosen Channel by using the command
Program…Relays
display will read, “Initial Relays -1-2-3-4”. If you are activating Channel A
connected to External Event 2, press 2 and Enter on the numeric keyboard. The
display will change to reflect that Relay 2 is On. You may check the status of the
relays at any time from the GC keyboard by pressing Status … Relays. In this
example, you would then see the display “Relays On: 2”. You can adjust each of
the CI reagents installed in the MCI Module by turning on the appropriate relay
from the GC keyboard, then using the procedures in
in the MS Method Editor
to adjust CI reagent flows.
Selecting Reagent Channels from the 3800 GC Keyboard
from the keyboard. If no relays are currently active, the
Setting CI/MS Parameters
and in
Adjusting Reagent Flow for Each CI Reagent
To program reagent Channels from the GC keyboard, select the External Event
(or Valve) for the chosen Channel by using the command
Delivery…Valve States
display will show all Valves in the - State (Off). If you are activating Channel A
connected to Valve 1, use the arrow keys to highlight Valve 1 and the Inc. or
Dec. key to toggle the State to +. The display will change to reflect that Valve 1 is
On (+). You may check the status of the relays at any time from the GC keyboard
by pressing
reagents installed in the MCI Module by turning on the appropriate Valve from
the GC keyboard, then using the procedures in
the MS Method Editor
adjust CI reagent flows.
Sample Delivery…Valve States
from the keyboard. If no relays are currently active, the
. You can adjust each of the CI
Setting CI/MS Parameters in
and in
Adjusting Reagent Flow for Each CI Reagent
Sample
to
Setting up the Method for 3400/3600 GCs
You may adjust the flows of CI reagents from the Manual Control screen of the
Saturn System Control Module. However, for the correct Channel of the MCI
Module to be selected for adjustments, the GC/MS method should have the
correct Channel selected in the GC Relays section of the Method.
Using the Star Toolbar or the
menu, open the Method Builder application. The Method Directory is shown on
the left side of the window, as shown below. Only the relevant sections for 3400
GC and Saturn 2000 control are shown in this example. (Relays in 3600 GC
Control are adjusted in the same way as in the 3400 GC).
Start…Programs…Saturn GCMS Workstation
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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
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
File…Activate…
(CHANNELx) from the System Control window.
File…Save As
to save the method with a name
Setting Valve States for 3800 GCs
You may adjust the flows of CI reagents from the Manual Control screen of the
Saturn System Control Module. However, for the correct Channel of the MCI
Module to be selected for adjustments, the GC/MS method should have the
correct Channel selected in the GC Sample Delivery section of the Method.
Using the Star Toolbar or the
menu, open the Method Builder application. The Method Directory is shown on
the left side of the window, as shown in the following Figure. Only the relevant
sections for 3800 GC and Saturn 2000 control are shown in this example.
Select the section Sample Delivery under 3800 GC Control.
You will see the screen below:
Start…Programs…Saturn GC/MS Workstation
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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:
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Now use the menu command
File…Save 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
File…Activate…
(CHANNELx) from the System Control window.
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Setting CI/MS Parameters in the MS Method Editor
To adjust CI reagent flows for a given CI gas and to use the appropriate
parameters in a CI/MS acquisition, you will need to modify the GC/MS Method for
each reagent Channel so that CI/MS parameters for each reagent are
appropriate. Open the Method ChannelA (or its equivalent) that you created in
Selecting Reagent Channels in the GC/MS Method
the
Directory select the entry MS Method Editor under 2000 Mass Spec Control. The
MS Method Editor dialog will appear.
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.
. From the Method
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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
Parameters for Liquid CI Reagents
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 µA is used in CI acquisitions.
When you have finished these steps save the Method for Channel A with the
menu command
Modify this method for the CI reagents in Channels B and C and save the new
methods with the menu command
ChannelC.mth. You may then activate the files from System Control with the
menu command
File…Save As
File…Activate
and already entered into the fields on the
ChannelA.mth.
File…Save As
.
ChannelB.mth or
Default
Adjusting Reagent Flow for Each CI Reagent
1. Connect a liquid reagent reservoir containing the chosen liquid or connect a
selected gas supply to Channel A, B, or C in the MCI Module inlet block. Use
the procedures in
Adding Gaseous Reagents to the MCI Module
Adding Liquid CI Reagents to the MCI Module
.
or
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2. Open the CI needle valve for the chosen Channel 6-7 turns counterclockwise.
3. Open the CI solenoids for the chosen Channel either from the GC keyboard or by activating a method for that reagent (ChannelA.mth, ChannelB.mth, or ChannelC.mth with the System Control menu command In this case, the method ChannelA.mth is activated.
4. Enter the Manual Control dialog of Saturn System Control. Click on the CI button in the Saturn icon on the upper left of the screen and allow a few seconds for the vapor flow from the reservoir to equilibrate. The set of tab dialogs in the center of
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File…Activate Method
.
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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.
6. The adjustment process will begin, as shown.
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
.
Building GC/MS Methods to Use Different CI
Reagents
The MCI Module may be used in several different ways to acquire data on a
sample for qualitative identification. In general it is advisable to develop a
standard GC and EI Method for data acquisition; then to modify the existing
method to acquire data in each selected CI mode.
NOTE: Acquisition with each CI reagent using the MCI Module requires a unique
GC/MS method. The GC section of the method MUST contain External Events programming to select the CI reagent in Channel A, B, or C. The MS section of
the method MUST have CI mode selected with the appropriate CI Tune File.
Preparing a Standard GC/EI/MS Method
Whether you are going to run methods development on single samples or on a
series of samples, it is generally advisable to prepare GC and MS methods for
EI/MS acquisitions first.
This example shows GC method development for the 3800 GC. The
development of the method for 3400/3600 GCs is similar. In the Saturn Windows
Workstation, open a GC/MS method for editing and save it as EI_GC.mth. In the
Methods Directory, choose the item GC Injector. Enter 260 as an isothermal
injector temperature. (It is assumed that you are using a 1079 injector.)
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:
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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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Save the GC/MS Method.
Methods for Single CI Reagents
Open the standard GC/MS Method you have created and saved (e.g.,
EI_GC.mth) in the Saturn GC/MS Workstation. Before proceeding use the
Method Editor menu command
specific to the first CI reagent you want to use (e.g. ACN_CI for acetonitrile CI).
Then choose the Method Directory item Sample Delivery to turn on the External
Event for that CI gas:
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.
File… Save As
to save the file with a name
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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
Gaseous CI Reagents
acquisition should never be lower than the suggested background mass for a
given reagent.
for suggested background masses. Low mass for
Default Parameters for
or
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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.
GC/MS SampleList for Alternating EI/MS and CI/MS
Acquisitions
In this example, a set of three samples has been placed in the 8200
AutoSampler in positions 1, 2, and 3 of the sample carousel. When the
AutoSampler run is started, each sample will first be run in EI mode using the
method EI_GC.mth, then in CI mode with acetonitrile as the CI reagent using the
method ACN_CI.mth. Note that care must be taken to use the correct GC/MS
method for each entry in the table. The data can now be acquired in automation
by preparing appropriate SampleList for the 8200 AutoSampler, the 3800 GC and
the Saturn MS.
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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
. The
Automation File Editor Dialog Box will open. Click on the option
File…New…SampleList.
Select the name EI_CI for the new Sample List and click on Save.
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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.
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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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Multiple CI Reagents in Consecutive Runs
If unique GC and MS methods for all three reagents have been set up, it is
possible to acquire data either in EI mode or with any of the CI reagents by
simply selecting the right GC/MS method for each run. In the following example,
a single sample in Rack 1, Vial 1 of the 8200 AutoSampler is used to acquire
data in EI, acetonitrile CI, methanol CI, and methane CI modes. Use the
procedure outlined above for
CI/MS Acquisitions
to create a SampleList as shown.
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GC/MS SampleList for Alternating EI/MS and
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Use the AutoLink field to activate the appropriate method for the EI or particular
CI reagent required.
Multiple CI Reagents in the Same Run
In some demanding applications, it may be desirable to change CI reagents
within a single chromatographic acquisition. This is done by time programming
the GC/MS Method so that the correct External Events are opened during the
corresponding MS acquisition time for each CI reagent. In this example, a
GC/MS method named TRI_CI is created to use acetonitrile CI (Event A,
Channel A) for the first ten minutes of the run, then methanol CI (Event B,
Channel B) and methane CI (Event C, Channel C) in the succeeding ten-minute
segments. To develop this method, open the Method Builder and choose to edit
ACN_CI.mth. After opening the method use the menu command
to save the method as TRI_CI.mth.
3800 GC Method Section
Create an External Events program in the GC Sample Delivery section to open
different channels of the MCI Module as desired during the GC/MS run:
File…Save As
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Saturn MS Analysis
Similarly, in the Method Directory item 2000 Mass Spec Control…MS 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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