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Varian 1200 LC/MS Operator's Manual

Atmospheric pressure chemical ionization (apci)
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Table of Contents
  • Table of Contents
  • Overview of APCI
  • Introduction
  • Basic Principles
  • Positive Ion APCI
  • Negative Ion APCI
  • Applications
  • Installation of APCI Chamber
  • APCI Daily Startup and Shutdown
  • Startup
  • Shutdown
  • Tuning
  • APCI Mobile Phase Selection
  • Optimizing S/N for APCI
  • Typical APCI Operating Parameters
  • APCI Performance Evaluation
  • Operating Conditions for Testing the APCI
  • APCI Sensitivity Test
  • APCI General Maintenance
  • Cleaning
  • Cleaning the Spray Shield
  • Cleaning the Vacuum Capillary
  • Cleaning the Corona Needle
  • Replacing and Aligning the Corona Needle
  • Replacing the Nebulizing Needle
  • Removal
  • Installation
  • Replacing the APCI Quartz Tube
  • Removing the Quartz Tube
  • Installing the Quartz Tube
  • APCI Troubleshooting
  • Comparison of ESI and APCI Parameters
  • APCI Spare Parts

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  • ENGLISH, page 13

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NOTICE: Varian, Inc. was acquired by Agilent
Technologies in May 2010. This document is provided
as a courtesy but is no longer kept current and thus
will contain historical references to Varian. For more
information, go to www.agilent.com/chem.
Atmospheric Pressure Chemical
©Varian, Inc. 2003-2006
1200 LC/MS APCI Option
Ionization (APCI)
Operator's Manual
Printed in U.S.A.
Varian, Inc.
2700 Mitchell Drive
Walnut Creek, CA 94598-1675/usa
03-914981-00:Rev. 3

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  • Page 1 NOTICE: Varian, Inc. was acquired by Agilent Technologies in May 2010. This document is provided as a courtesy but is no longer kept current and thus will contain historical references to Varian. For more Varian, Inc. information, go to www.agilent.com/chem.
  • Page 2 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 2006 All rights reserved.
  • Page 3 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.
  • Page 4 Customer to return the defective workmanship for the periods specified and in accessory or instrument to Varian or to send it to a accordance with the terms on the face of Varian's designated service facility.
  • Page 5 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...
  • Page 6 Garan- garantie wird die Reparatur der Instrumentstörungen tien der Verkäuflichkeit und Eignung für einen be- sein, die sich nach Varian's Ansicht auf Defekte in den sonderen Zweck, Gebrauch oder Anwendung und Originalteilen oder bei der Herstellung zurückführen läßt...
  • Page 7 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...
  • Page 8 Varian diffusera des mises à jour des de Varian au client d'origine. Cependant, lorsque le logiciels, le cas échéant, et si de l'avis de Varian, elles client a acquitté les frais d'installation ou que celle-ci est constituent la mesure corrective la plus appropriée en la inclue dans le prix d'achat, la période de garantie...
  • Page 9 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...
  • Page 10 In assenza d'un contratto di licenza e salvo diverso magnetico, fotomoltiplicatori, filamenti, guarnizioni per accordo scritto tra la Varian e il Cliente, vale il periodo di vuoto, e tutte le parti esposte all'azione dei campioni o garanzia indicato nell'offerta della Varian. La Varian delle fasi mobili.
  • Page 11 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...
  • Page 12 Esta garantía no tendrá efecto en los casos de accidente, Varian, u otro tipo de hardware en el que Varian certifique abuso, alteración, utilización incorrecta, negligencia, que funcionan según lo descrito en Manual de rotura, mantenimiento o uso inadecuados, modificaciones instrucciones, y que esté...
  • Page 13 NOTES CAUTIONS WARNINGS accordance with this instruction manual and any additional information which may be provided by Varian. Address any questions regarding the safe and proper use of your equipment to your local Varian office. NOTE Information to aid you in obtaining...
  • Page 14 It is the responsibility of the Customer to inform Varian Customer Support Representatives if the instrument has been used for the analysis of hazardous biological, radioactive, or toxic samples, prior to any instrument service being performed or when an instrument is being returned to the Service Center for repair.
  • Page 15 Flash Chromatography GC Safety Practices The operator should be familiar with the physico- Exhaust System chemical properties of the components of the mobile No special exhaust ducting is necessary for GC phase. detectors installed in a well-ventilated room except Keep solvents from direct...
  • Page 16 Varian, Inc. Analytical Instruments Sales Offices For Sales or Service assistance and to order Parts and Supplies, contact your local Varian office. Argentina France...
  • Page 17 HINWEIS ACHTUNG WARNUNG, 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. ACHTUNG WARNUNG HINWEIS Eine Information, um einen optimalen Weist auf Situationen, die zu mäßiger...
  • Page 18 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.
  • Page 19 Öffnen Sie niemals eine unter Druck stehende GC Sicherheitspraktiken Lösungsmittelleitung oder ein Ventil. Halten Sie Abgassystem zuerst die Pumpe an und lassen Sie den Druck auf Für GC Detektoren, die in einem gut durchlüfteten Null abfallen. Raum installiert sind, ist keine spezielle Abgasführung Benutzen Sie splittersichere Reservoirs, die für erforderlich, außer wenn die Detektoren zum Testen einen Druck von 3,4 bis 4,1 bar ausgelegt sind.
  • Page 20 Verfügbarkeit von Ersatzteilen Serviceverfügbarkeit Varian bietet seinen Kunden auch Es ist Varian’s Grundsatz, Ersatzteile für alle Instrumente und die wichtig- nach dem Auslaufen der Garantie sten Zubehöre für einen Zeitraum von fünf (5) Jahren nach dem Fertigung- eine Vielfalt von Serviceleistungen sauslauf dieser Geräteserie verfügbar zu haben.
  • Page 21 AVERTISSEMENTS. matériel conformément aux instructions du présent manuel et à toute autre information émanant de Varian. S’adresser au bureau régional Varian pour toute question relative à la sécurité ou à l’utilisation correcte du matériel. NOTE Information destinée à tirer le Attire l’attention sur une situation...
  • Page 22 Le client est tenu d’informer le service Varian d’assistance à la clientèle que son matériel ATTENTION a été utilisé pour l’analyse d’échantillons biologiques dangereux, radioactifs ou toxiques avant que n’en soit effectué...
  • Page 23 Ne jamais déconnecter un conduit de solvant ou Mesures de sécurité en CPG une vanne sous pression. Arrêter préalablement la Système d’échappement pompe et laisser la pression descendre à zéro. Les détecteurs CPG installés dans une pièce bien Utiliser des réservoirs incassables à 50-60 psi. ventilée ne nécessitent pas de conduits spéciaux d’échappement excepté...
  • Page 24 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.
  • Page 25 . E’ importante che lo strumento venga utilizzato rispettando le istruzioni fornite in questo CAUTELA ATTENZIONE 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). ATTENZIONE...
  • Page 26 E’ responsabilità del Cliente informare il Servizio Tecnico Varian, prima di qualsiasi ATTENZIONE intervento di riparazione, se lo strumento è stato utilizzato per l’analisi di campioni biologicamente pericolosi, radioattivi o tossici.
  • Page 27 Procedure di Sicurezza in GC Non smontare mai una linea del solvente od una Scarico dei Gas valvola quando il sistema è sotto pressione. Per i rivelatori GC non è richiesto alcun sistema Fermare prima la pompa ed aspettare che la particolare di scarico dei gas, se lo strumento è...
  • Page 28 Disponibilità delle Parti di Ricambio Servizi Tecnico E’ politica della Varian il fornire le parti di ricambio per lo strumento ed La Varian, alla scadenza del periodo i suoi accessori per un periodo di cinque (5) anni a partire dalla data di di garanzia, è...
  • Page 29 PRECAUCION ATENCION 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. ¡PRECAUCION! ATENCI N Ó...
  • Page 30 Debe ser operado usando gases y/ó disolventes apropiados y con unos niveles máximos de presión, flujos y temperaturas, según se describe en este manual. El Usuario tiene la obligación de informar al Servicio Técnico de Varian cuando el ATENCI N Ó...
  • Page 31 Nunca abra una línea ó una válvula bajo presión. GC Prácticas de Seguridad Apague la bomba antes y deje que la presión baje a Sistema de Extracción cero. No se necesita un sistema de extracción para los Utilice depósitos irrompibles que sean capaces de detectores GC instalados en un laboratorio bien operar a 50-60 psi.
  • Page 32 Disponibilidad de Recambios Disponibilidad de Servicio 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 Varian ofrece una gran variedad de último instrumento fabricado. Los recambios durante esos cinco años sistemas de Servicio para mantener estarán disponibles, pero siempre bajo el sistema “Según disponibilidad”.

  • Page 33: Table Of Contents

    Contents Overview of APCI........................3 Introduction .................................3 Basic Principles ................................3 Positive Ion APCI ..............................4 Negative Ion APCI..............................4 Applications ................................5 Installation of APCI Chamber .............................6 APCI Daily Startup and Shutdown..........................8 Startup..................................8 Shutdown ................................8 Tuning..................................8 APCI Mobile Phase Selection.............................8 Optimizing S/N for APCI .............................9 Typical APCI Operating Parameters ..........................9 APCI Performance Evaluation..........................10 Operating Conditions for Testing the APCI......................10...
  • Page 34 03-914981-00:3...

  • Page 35: Overview Of Apci

    Overview of APCI Introduction For many small molecules, atmospheric pressure chemical ionization (APCI) is an excellent alternative to electrospray ionization (ESI). APCI assumes the analyte molecule has reasonable thermal stability. Thermal degradation in APCI is less likely than in GC/MS, but thermal stability is a fundamental restriction for APCI that is not shared by ESI.

  • Page 36: Positive Ion Apci

    Positive Ion APCI Positive Ion APCI can occur as follows: • + M → (M+H) Proton Transfer: H − Also CH , CH , NH • + M → (M+ NH Adduct Attachment: NH − Also CH , CH • Charge Exchange Negative Ion APCI Negative Ion APCI can occur as follows:...

  • Page 37: Applications

    Sample Inlet Metal Needle Quartz Tube Heater Corona Needle Mass Spec Inlet (to Vacuum Region and API Plug) Cutaway View of APCI Chamber APCI is a soft ionization process that typically produces only singly charged ions with information about the molecular ion. Adduct ions are common, but lower mass fragment ions are not.

  • Page 38: Installation Of Apci Chamber

    Installation of APCI Chamber 1. Remove the Electrospray Ionization (ESI) chamber, if installed. Source parts become hot during operation. Use caution when WARNING: installing or removing the API Source. BURN HAZARD 2. Connect the gas lines to the nebulizer assembly. Nebulizing gas –...
  • Page 39 If this is the first time an APCI chamber is being installed on this instrument, do the following. 1. Change the instrument to APCI mode, by entering APCI on the command line. 2. Before connecting the corona high voltage connector, calibrate the needle current readback.

  • Page 40: Apci Daily Startup And Shutdown

    APCI Daily Startup and Shutdown Startup 1. Set the vaporizer and drying gas temperatures. 2. Click the spray icon to turn on the gases and heaters. 3. When the vaporizer temperature has reached to a minimum of 75% of its set value, start the LC pump.

  • Page 41: Optimizing S/N For Apci

    Optimizing S/N for APCI Do Optimization for each analysis. The detector response varies for each type of analyte and is dependant on the mobile phase composition and flow rate. Typical optimization normally involves flow injection or infusion of analyte into a mobile phase flowing at the analytical flow rate and composition while adjusting N flows and temperatures to achieve maximum signal to noise.

  • Page 42: Apci Performance Evaluation

    APCI Performance Evaluation Operating Conditions for Testing the APCI • Drying Gas: 12 psi at 150 °C • Nebulizing Gas: 60 psi at 550 °C • Auxiliary Gas: 17 psi • Corona Needle Current: 5 μA • Housing Temperature: 50 °C •...

  • Page 43: Apci General Maintenance

    APCI General Maintenance Cleaning Clean the chamber daily with methanol to decrease the accumulation of contamination. If the chamber requires more aggressive cleaning, use slurry of aluminum oxide powder to polish the inside of the housing. Materials used for cleaning can produce hazardous vapors.

  • Page 44: Cleaning The Corona Needle

    Cleaning the Corona Needle Wipe the corona needle with methanol. If the deposits cannot be easily removed, replace the needle as follows. Nebulizer Assembly Vaporizer Tube Compression Fitting Corona Needle Corona Needle Mount Cutaway View of APCI Chamber Replacing and Aligning the Corona Needle Replace the corona needle needs if it is bent, damaged, or cannot be cleaned satisfactorily.

  • Page 45: Replacing The Nebulizing Needle

    Replacing the Nebulizing Needle If the liquid needle becomes plugged, it can be easily replaced. The needle assembly is a length of 0.004 in. ID stainless steel tubing bonded to a length of 0.005 in. ID PEEK™ tubing. Removal Unscrew the fingertight PEEK fitting on top of the nebulizer assembly. Remove the old needle assembly from the top of the nebulizer assembly by pulling the PEEK tubing.

  • Page 46: Removing The Quartz Tube

    Be very careful while handling the quartz tube because it CAUTION is very fragile. Components become very hot and can present a burn WARNING: hazard. Ensure that all parts are cool before beginning BURN HAZARD this procedure. The spray chamber may contain hazardous chemicals. Use appropriate protection when handling.

  • Page 47: Installing The Quartz Tube

    10. Remove the white ceramic insulating washer (03-937323-01) and set both aside. 11. Open the spray chamber. Leave it attached to the instrument by the mounting hinge. 12. Remove corona needle (03-937344-01) from its mount by pulling straight up. Be careful of the sharp point. Set aside. 13.
  • Page 48 5. Open the spray chamber, keeping a finger on the quartz tube through Step 7 so it doesn’t fall out. 6. Place a new polyimide ferrule (03-937339-01) over the exposed end of the quartz tube with the wider side of the ferrule toward the vaporizer assembly. 7.

  • Page 49: Apci Troubleshooting

    If the vaporizer temperature does not increase when turned on, contact your local Varian, Inc. representative for instrument repair and service. Comparison of ESI and APCI Parameters APCI ARAMETER 4L/min @ 350 °...

  • Page 51: Apci Spare Parts

    APCI Spare Parts UMBER ESCRIPTION 03-937327-01 Quartz Vaporizer Tube 03-930109-06 Quartz Vaporizer Tube O-ring 03-937339-01 Quartz Vaporizer Tube Ferrule (Polyimide) 03-937344-01 Corona Needle 28-211542-00 PEEK 2-piece 10-32 Nut and Ferrule 03-937544-03 APCI Liquid Needle Assembly, 0.004 ID 03-937337-01 Spray Shield 27-402529-00 Spray Chamber O-ring 27-402690-00...

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