Varian ProStar 400 Operation Manual

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Varian, Inc.
2700 Mitchell Drive
Walnut Creek, CA 94598-1675/usa
ProStar 400
AutoSampler
Operation Manual
©Varian, Inc. 2000 - 2004
Printed in U.S.A.
03-914786-00:Rev. 3

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Summary of Contents for Varian ProStar 400

  • Page 1 Varian, Inc. 2700 Mitchell Drive Walnut Creek, CA 94598-1675/usa ProStar 400 AutoSampler Operation Manual ©Varian, Inc. 2000 - 2004 Printed in U.S.A. 03-914786-00:Rev. 3...
  • 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. The Customer shall be...
  • Page 5 It is important that you operate your equipment in accordance with this instruction manual and any additional information which may be provided by Varian. Address any questions regarding the safe and proper use of your equipment to your local Varian office.
  • Page 6 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 7 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 when the detectors are used to test hazardous Keep solvents from...
  • Page 8 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 9 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 10 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 11 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 12 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 13 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 14 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 15 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 16 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 17 . 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 18 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 19 Non smontare mai una linea del solvente od una Procedure di Sicurezza in GC valvola quando il sistema è sotto pressione. Scarico dei Gas Fermare prima la pompa ed aspettare che la Per i rivelatori GC non è richiesto alcun sistema pressione scenda a zero.
  • Page 20 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 21 PRECAUCION ATENCION el instrumento de acuerdo con este Manual de Operación y cualquier otra información que le proporcione Varian. Remita a la Oficina Local de Varian cualquier cuestión que tenga respecto al correcto uso de su equipo. ¡PRECAUCION! ATENCI N Ó...
  • Page 22 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 23 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 24 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 25: Table Of Contents

    Loading the Sample Tray ....................10 Positioning of vials....................10 Needle wash vials....................11 Large Volume Samples .....................11 Description ........................11 Installation ........................12 Instrument Description ................. 13 General Description......................13 Injection Principle ......................14 Dispenser-controlled Injection..................14 Pressure-controlled Injections..................15 Digital Dispenser System (DDS).................16 Operating Principle ....................16 ProStar 400 AutoSampler...
  • Page 26 RUN Parameters......................22 Cooling Control (optional) ...................23 RUN ...........................23 HOLD ..........................24 Priority Sample......................25 Remote Control........................25 PC Workstation Interface....................26 Varian 4400 Integrator Interface..................27 Special Display Messages....................27 After Use..........................28 Maintenance/Service ................29 Needle Penetration Depth ....................30 Needle Pair Replacement....................30 Sample Needle......................30 Air Needle ........................32 Dispenser Pump Tubing ....................32...
  • Page 27: Introduction

    The ProStar 400 therefore makes use of flushed loop injection, with reproducibility of injection better than 0.5%. ProStar 400 AutoSampler...
  • Page 28 03-914786-00:3...
  • Page 29: Installation

    4 Cooling fan, only in case of tray cooling 5 Standard RS232 connector 6 Connector vial number output 7 Connector control I/O 8 Optional communication connector 9 Serial Number Label Figure 1 ProStar 400 AutoSampler Rear Panel ProStar 400 AutoSampler...
  • Page 30: Power Connections

    Two 2.5 amp T-type (slo-blo) 55-500344-00 Communication Connectors For connection to Varian ProStar and Star LC modules, use Cable Kit Part Number 03-909126-90. Follow the Installation Instructions included with that cable. Information in the following paragraphs is provided for users who wish to develop custom interfaces to other devices.
  • Page 31: Control I/O Connector

    Next injection input (active low, pulled up, TTL) This input triggers a next injection when the ProStar 400 AutoSampler is in REMOTE CONTROL mode. It can also be used as a START input when the ProStar 400 is not in REMOTE CONTROL mode.
  • Page 32: Vial Number Output Connector

    Bit 7 units x 80 Ground Inject marker (TTL, active low) RS485 Connector The ProStar 400 can be controlled by a PC using the RS485 interface. Fluid Connections The instrument has been tested with isopropanol. Make sure that the mobile phase of your HPLC system is miscible with isopropanol.
  • Page 33: Sample Loop

    Figure 2 Keyboard Cover Removal Sample Loop The ProStar 400 is factory-equipped with a 20 µL sample loop. If a different volume is to be injected, the sample loop must be replaced. Please note that to fill the loop quantitatively, three times the loop volume is withdrawn from the sample vial for loops smaller than 100 µL and twice the loop volume for loops...
  • Page 34: Sample Drain For Loopfilling By Headspace Pressure

    Sample Drain for Loopfilling by Headspace Pressure Time-based loopfilling by sample headspace pressure can be selected (see Operation on page 17) to shorten loopfill time for larger loop volumes (see Injection Principle on page 14). To allow time-based loopfilling and to prevent hydrostatic sample loss, the special sample drain for headspace pressure loopfill must be connected at the injection valve, replacing the dispenser connection at the valve.
  • Page 35: Injection Volume

    Due to the reduced solvent velocity near the wall of the tubing (loop), it takes more than the nominal loopvolume to fill the loop reproducibly. For flushed loop injections the ProStar 400 takes twice the loop volume from the sample vial for a sample loop equal to or larger than 100 µL and three times the loop volume...
  • Page 36: Filling And Sealing The Vials

    Use the STEP key (see Operation on page 17) to rotate the tray (functioning only when the ProStar 400 is in READY status). CAUTION Do not rotate the tray manually; you may damage the tray drive mechanism.
  • Page 37: Needle Wash Vials

    Large Volume Samples Description The large volume sample tray is an option of the ProStar 400 AutoSampler. This option allows the user to inject large volumes of sample with the DDS or by headspace pressure. The option consists of: •...
  • Page 38: Installation

    Installation Install the LSV option according to the following procedure: • Replace the standard installed tubing and needles with the tubing and needles of the LSV option. Follow the procedure described in Maintenance/Service, page 29. • Replace the standard tray by the LSV tray. •...
  • Page 39: Instrument Description

    Instrument Description General Description Figure 3 ProStar 400 1 Sample tray, consisting of 4 removable segments 2 Keyboard 3 Display 4 Removable cover 5 Needle arm with sample needle 6 Injection valve with sample loop 7 Dispenser cassette screw 8 Dispenser...
  • Page 40: Injection Principle

    Injection Principle A six-port high pressure switching valve can perform the injections based on the flushed loop principle. Loopfilling can be done on a volume basis, controlled by the digital dispenser system, or on a time basis by headspace pressure on the sample to shorten filling time for larger loop volumes.
  • Page 41: Pressure-Controlled Injections

    HPLC mobile phase flow path: sample is transported to the column. Analysis time starts. NOTE: A special sample drain that prevents siphoning must be connected to the injection valve (replacing the dispenser connection). Refer to Installation on page 3. ProStar 400 AutoSampler...
  • Page 42: Digital Dispenser System (Dds)

    If one injection is to be made out of each sample vial, the needle pair withdraws after the analysis time is complete and sequence steps 1-2 starts for the next vial. If more than one injection is to be made out of the same sample vial, the needles remain in the vial.
  • Page 43: Operation

    Operation Operating the ProStar 400 AutoSampler is easy. After programming the system SETTINGS, only a few parameters need to be programmed for regular automatic processing of a series of samples. All parameter values are saved in memory when power is switched off or during power failure, except the tray temperature setting, if the tray cooling option is installed.
  • Page 44: Ready Status

    READY Status • READY status is the “ground state” of the ProStar 400 AutoSampler which is initiated automatically after power UP. Every mode can be entered from READY status, except PRIORITY mode, which can be entered only when the ProStar 400 AutoSampler is in RUN mode.
  • Page 45: Function Codes

    PERATION Function Codes The following table shows all the possible modes of the ProStar 400 AutoSampler. Function code Selected mode Selects SYSTEM SETTINGS mode. Selects COOLING CONTROL mode (only if cooling option is installed) Selects PRIORITY mode (only accessible during sample run).
  • Page 46: Programming Chart

    Programming Chart to step. 1. FIRST VIAL (1—>48/92/96) to step. TRAY COOLING (ON / OFF) 2. LAST VIAL (1—>48/92/96) 3. NO OF INJ'S/VIAL (1—>9) 1. LOOPVOLUME (0->999µL) 4. PREFLUSH VOLUME (30—>999µL) 2. SAMPLE VOLUME (STD/LSV) FLUSH TIME (1—> 999 SEC) 3.
  • Page 47: Programming

    COOLING CONTROL mode to program the tray cooling, if installed. System Settings With the ProStar 400 in READY status, key in F,9 to select SYSTEM SETTINGS mode. Press PROG/END to enable programming of the following parameters (use STEP key to go to...
  • Page 48: Run Parameters

    Parameters will appear in the RUN PARAMETER mode. Enter 0 if no auxiliaries are to be used. RUN Parameters With the ProStar 400 in READY status, press PROG/END to select RUN PARAMETER mode and to enable programming at the same time.
  • Page 49: Cooling Control (Optional)

    Cooling Control (optional) Sample tray temperature control is switched ON/OFF in the COOLING CONTROL mode. With the ProStar 400 in READY status, key in F,7 to select COOLING CONTROL mode. Press PROG/END to switch ON or OFF the cooling control.
  • Page 50: Hold

    The first character of the second line will be a blinking R if the ProStar 400 is under remote control or a blinking p if a priority sample is programmed. It is possible to reprogram RUN PARAMETERS during RUN;...
  • Page 51: Priority Sample

    See the installation instructions enclosed with the cable for details of these modes of operation. When the ProStar 400 is in REMOTE CONTROL mode it can only be controlled using the “next injection” and “next vial” inputs.
  • Page 52: Pc Workstation Interface

    A “next injection” input signal will start the RUN. A blinking R (first position of the lower display line) indicates that the ProStar 400 is under remote control. All other relevant RUN information will be displayed as usual. When all programmed vials have been processed, the display...
  • Page 53: Varian 4400 Integrator Interface

    Figure 7 Star Workstation Communication for Single ProStar 400 AutoSampler Varian 4400 Integrator Interface The ProStar 400 outputs the vial location number through a BCD port. Varian Cable Kit Part Number 03-919938-90 provides a cable to connect the BCD output to the Varian 4400 Integrator.
  • Page 54: After Use

    Enter correct value. After Use If the ProStar 400 AutoSampler is not to be used for more than two days, flush needle and valve with water and isopropanol (can be placed as last vials of a sample series) and loosen pump tubing cassette screw one turn.
  • Page 55: Maintenance/Service

    15 Air inlet hole in connector to prevent emptying of sample vial by hydrostatic suction. 16 Needle connection nut 17 Ferrule (PTFE) 18 Sample needle connection hub Figure 8 Injection System 19 Air seal ProStar 400 AutoSampler...
  • Page 56: Needle Penetration Depth

    Needle Penetration Depth To keep rest volume small, the sample needle should stop close to the bottom of the sample vial. If penetration depth requires adjustment, proceed as follows (see Figure 8): Remove keyboard cover. • Place an uncapped vial in the tray. •...
  • Page 57 Connect loose end of needle connection tubing to port 2 of injection valve (use a Rheodyne ferrule ). Do not tighten excessively; it may close the tubing. • Check needle penetration depth and adjust if necessary. • Connect main power supply. • CLOSE KEYBOARD COVER. ProStar 400 AutoSampler...
  • Page 58: Air Needle

    Air Needle To replace air needle, proceed as follows: • Remove sample needle. • Unscrew air needle and install new air needle. • Reinstall sample needle. Dispenser Pump Tubing • Loosen fitting that connects PTFE inlet tubing of dispenser to injection valve.
  • Page 59: Appendix

    Switching time injection valve Electrically <100 msec PERFORMANCE Reproducibility Flushed loop injections: RSD ≤ 0.5 % Memory effect Better than 0.2 % ELECTRICAL Power requirements 115 Vac; ±10%; 50/60 Hz; 100 VA 230 Vac; ±10%; 50/60 Hz; 100 VA ProStar 400 AutoSampler...
  • Page 60 COMMUNICATION OUTPUTS Inject marker (Relays & TTL) Stop I/O (TTL) Vial number BCD output (TTL) Auxiliary 1 (open collector) Auxiliary 1 inverted (open collector) Auxiliary 2 (open collector) Auxiliary 2 inverted (open collector) INPUTS Next injection input (TTL) Next vial input (TTL) Freeze runtime (TTL)
  • Page 61: Accessories

    Includes: PEEK Tubing (10ft. x 0.01" ID), Package of 10 fingertight fittings and 2 mL Sample Vials (3 x 144) 0391968900 ProStar 400 Large Volume Option Allows injection volumes up to 4 mL. 48 Sample Vial Capacity Includes: Racks for 4 mL Vials, Serum Needle, Air Serum Needle, 500 µL sample loop, and PTFE tubing.
  • Page 62 Part Number Description 2000 µL SS Loop for Valco Valve 0392611014 5000 µL SS Loop for Valco Valve 0392611015 0392611016 10 mL SS Loop for Valco Valve 20 µL PEEK Loop for Valco Valve 0392611017 50 µL PEEK Loop for Valco Valve 0392611018 100 µL PEEK Loop for Valco Valve 0190018208...
  • Page 63 FOR LARGE VOLUME SAMPLE TRAYS 0190000839 4 mL Vials 0190000840 Caps for 4 mL Vials 0190000841 Septa for 4 mL Vials NOTE: The use of Eppendorf microcentrifuge tubes may cause malfunctioning of the ProStar 400 vial sensor. ProStar 400 AutoSampler...

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