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Informations et mesures de sécurité

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

NOTES,

MISES

EN

GARDE

et

AVERTISSEMENTS.

Il est important de faire fonctionner ce

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
meilleur parti du matériel sur le plan
des performances

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

Attire l’attention sur une situation
potentiellement dangereuse pouvant
occasionner des dommages corporels
importants et indique comment
remédier à cette situation

Symboles d’avertissement

Description

ATTENTION

RISQUE
D'ELECTROCUTION

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.

ATTENTION

RISQUE DE BRÛLURES

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.

ATTENTION

RISQUE D'INCENDIE

Risque potentiel d’incendie. Se conformer aux instructions du manuel pour faire
fonctionner le matériel en toute sécurité.

ATTENTION

RISQUE D'EXPLOSION

Risque potentiel d’explosion en raison du type de gaz ou de liquide utilisé.

ATTENTION

SOURCE DE RADIATION

Présence d’une source de radiation ionisante. Se conformer aux instructions du
manuel pour faire fonctionner le matériel en toute sécurité.

ATTENTION

PIECES EN MOUVEMENT

Garder les mains et les doigts hors de portée.

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Summary of Contents for ProStar 340

Page 1: ... 00 Rev 3 ProStar 340 UV Vis Detector Operation Manual 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 ...

Page 2: ......

Page 3: ...ized 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 prom...

Page 4: ...he 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 ...

Page 5: ...moderate injury and or equipment damage and how to avoid these situations Alerts you to potentially hazardous situations that could result in serious injury and how to avoid these situations Warning Symbol Warning Description Hazardous voltages are present inside instrument Disconnect from main power before removing screw attached panels Hazardous chemicals may be present Avoid contact especially ...

Page 6: ... has been used for the analysis of hazardous biological radioactive or toxic samples prior to any instrument service being performed or when an instrument is being returned to the Service Center for repair Electrical Hazards Disconnect the instrument from all power sources before removing protective panels to avoid exposure to potentially dangerous voltages When it is necessary to use a non origin...

Page 7: ...ography The operator should be familiar with the physico chemical 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 f...

Page 8: ...hnical support and training can be provided by qualified personnel on both a contractual or as needed basis Varian Inc Analytical Instruments Sales Offices For Sales or Service assistance and to order Parts and Supplies contact your local Varian office Argentina Buenos Aires Tel 54 11 4 783 5306 Australia Mulgrave Victoria Tel 61 3 9566 1134 Austria Vösendorf bei Wien Tel 43 1 699 9669 Benelux Ber...

Page 9: ...d auf die Vermeidung dieser Situationen hin Warnungssymbol Warnungsbeschreibung WARNUNG ELEKTRISCHER SCHLAG 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 Kon takt besonders beim Auffüllen der Reservoirs Benutzen Sie wirksamen Augen und Hautschutz WA...

Page 10: ...nt 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 ...

Page 11: ...gen 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 ACHTU...

Page 12: ...ützung 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 113...

Page 13: ...ue comment remédier à cette situation Symboles d avertissement Description ATTENTION RISQUE D ELECTROCUTION 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 le...

Page 14: ...es 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...

Page 15: ... opérations de maintenance de routine Ne jamais déconnecter un conduit de solvant ou une vanne sous pression Arrêter préalablement la pompe et laisser la pression descendre à zéro Utiliser des réservoirs incassables à 50 60 psi Laisser l enceinte du réservoir fermée lorsque le réservoir est sous pression Se conformer aux NOTES MISES EN GARDE ET AVERTISSEMENTS du manuel d utilisation Chromatographi...

Page 16: ... du matériel spécifique support technique et service de formation assurés par des chimistes qualifiés sur base contractuelle ou en fonction des besoins spécifiques Points de vente des instruments analytiques Varian Contactez votre point de vente régional Varian pour toute question commerciale ou de service d assistance à la clientèle ou pour passer commande de pièces et de fournitures Argentina Bu...

Page 17: ...NZIONE Descrizione del Pericolo ATTENZIONE Pericolo di folgorazioni Nello strumento sono presenti tensioni pericolose Scollegare il cavo di alimentazione prima di togliere il pannello fissato con le viti Possono essere presenti composti chimici pericolosi Evitare il contatto specialmente quando si riempiono i contenitori Usare protezioni opportune per la pelle e per gli occhi ATTENZIONE Pericolo d...

Page 18: ...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 ...

Page 19: ...ne 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 ATTEN...

Page 20: ... oraria piu il costo delle parti A richiesta si possono avere corsi per operatori sia sotto forma di contratto che a tariffe da concordare 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 Austral...

Page 21: ...peligrosas que pueden causar serios daños y cómo evitar esas situaciones Símbolo Descripción ATENCIÓN PELIGRO DE DESCARGA ELÉCTRICA 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 ATENCIÓN PELIGRO DE QUEM...

Page 22: ...e 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 c...

Page 23: ...nto de rutina Nunca abra una línea ó una válvula bajo presión Apague la bomba antes y deje que la presión baje a cero Utilice depósitos irrompibles que sean capaces de operar a 50 60 psi Mantenga cerrada la junta del depósito cuando se haye bajo presión Lea y cumpla todas las NOTA PRECAUCION y ATENCION del manual Cromatografía Flash El operador debe familiarizarse con las propiedades físico químic...

Page 24: ...bra 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 b...

Page 25: ...Integrator Connections 13 Power Cord 14 Remote Connections 14 Autozero 14 Event 14 Lamp 15 Fluid Connections 15 Operation 17 Introduction 17 Setting Detector Controls 18 Wavelength 18 Range 19 Rise Time 19 Performing a Test Run 19 Shut Down 20 Maintenance and Troubleshooting 21 Changing the Flowcells 21 Flow Cell Maintenance 24 Cleaning the Flowcells 24 Cell Disassembly 24 Flow Cell Reassembly 25 ...

Page 26: ...mp 30 Removing the Tungsten Lamp 31 Installing the Tungsten Lamp 31 Troubleshooting 32 Light Intensity Diagnostics 32 Proper Full Scale Voltage Output 33 Filter Bypass Switch 33 Troubleshooting Guide 34 Appendix 37 Specifications 37 Parts and Accessories 38 ...

Page 27: ...re 1 illustrates the optical system for the detector Only one lamp D2 or tungsten can be mounted at a time Both lamps are continuum lamps that jointly provide consistent intensity across the entire spectrum from 190 to 800 nm Two sets of baffles are used to minimize stray light Wavelength selection is provided by a concave holographic grating actuated by a mechanical wavelength drive LAMP GRATING ...

Page 28: ...ntensity at the photodiode active surfaces see Figure 2 The outputs of the preamplifiers are sent to an analog ratiometer The output of this circuit is a voltage that is directly proportional to the negative logarithm of the ratio of the sample signal to the reference signal This voltage is supplied to the rear panel as the 1V AU integrator output and as the adjusted absorbance full scale recorder...

Page 29: ...u ordered Carefully check the packing list against the contents of the container If anything is missing check the packing materials carefully for the overlooked items If any items are missing contact LC Technical Services at 1 800 FOR HPLC or your local Varian office In addition to the detector you will need the following items for setup and initial operation Strip chart recorder or integrator and...

Page 30: ...flat surface such as a laboratory bench top near the column outlet Allow at least 5 inches of clear space between the rear panel of the unit and any wall or obstruction This gives access to the rear panel connections and provides a free flow of cooling air ...

Page 31: ... Rise Time Selection Switch A four position rotary switch controls the degree of filtering performed by a Second Order Bessel filter Rise times of 0 1 0 3 1 0 and 3 0 seconds can be chosen Typically Rise Time in seconds approximates 2x Time Constant in seconds 3 Range Selection Switch A twelve position rotary switch controls the full scale output range for the rear panel positioned Recorder Output...

Page 32: ... shunted to zero volts Within three seconds a new zero value will be calculated and the Wait Light will turn off The Over Range Light will illuminate when the total absorbance within the flowcell exceeds the capacity of the circuit 7 Over Range Light A green LED indicates a total absorbance in the flowcell which exceeds the autozezro circuit capacity The unit will continue to output voltages propo...

Page 33: ...grator output 11 Reference Light Intensity Switch A momentary switch displays a value which is proportional to the light intensity at the reference photodiode 12 Sample Light Intensity Switch A momentary switch displays a value which is proportional to the light intensity at the sample cell photodiode 13 Visible VIS Lamp Indicator A green LED indicates that a Tungsten lamp is present in the instru...

Page 34: ...remote auto zero function A momentary contact closure or TTL low activates the autozero circuit 5 Remote Event Two terminals provide an event mark with a momentary contact closure or TTL low 6 Remote Lamp Shut Off Two terminals provide a remote means of switching off the lamp Lamps are shut off by providing a continuous contact closure or TTL low Lamps are re ignited by the interruption of a conta...

Page 35: ...r a negative drifting baseline In most cases it need not be used 13 Recorder Offset Switch A two position rocker switch provides a 10 fixed offset to the recorder output This offset is independent of full scale range or full scale voltage This recorder offset does not affect the integrator output 14 Power Switch A two position rocker switch turns the instrument on and off Pressing the top half of ...

Page 36: ... from the D2 lamp can damage skin and eyes Lamps become very hot Use care when handling them to avoid burns 1 Lamp Housing Cover Remove the screw and cover to access the lamp 2 Flowcell Housing Cover Remove to access the flowcell and sample photodiode 3 Flowcell Exit Tubing Connect to a fraction collector back pressure device or waste 4 Flowcell Inlet Line Connect to the column outlet directly if ...

Page 37: ...minimize the total tubing length from this detector outlet to the inlet of the other detector to prevent excessive band broadening The outlet and inlet tubing ID OD and position may vary according to the flowcell in use Consult the flowcell manual for more details Electrical Connections Figure 6 Voltage Selection ...

Page 38: ...or card back into place Ensure that the fuse block is properly oriented for the selected voltage by rotating the block along its longitudinal axis until The long single fuse faces outward for 100 and 120V 1 Amp slow blow The two short fuses face outwards for 200 and 220V 0 5 Amp slow blow Snap the fuse block cover back into place Setting Recorder Full scale Voltage The detector provides a single s...

Page 39: ...nect the positive input of the recorder to the positive screw on the recorder output Connect the input of the recorder to the negative screw on the recorder output 1 2 3 4 5 6 7 INT 1AU V AUTO ZERO EVENT LAMP RECORDER OUTPUT REMOTE Figure 8 Input Output Terminal Integrator Connections The detector also provides a fixed span output 1V AU for use with an integrator or data acquisition system This is...

Page 40: ...positive line is connected to the positive pole and the negative line is connected to the negative pole of the remote Autozero terminal The remote autozero is triggered by shunting across its two input terminals Event The Event connection duplicates the function of the Event Button on the front panel whenever it is connected to a momentary contact closure or TTL low Connect the triggering device s...

Page 41: ... Figure 5 As a general rule the less tubing between the column outlet and the flowcell the better Ideally the column outlet should be connected directly to the detector inlet line If this is not possible you should use a minimum length of narrow bore 0 010 inch ID connecting tubing and a zero dead volume union Because different columns use different fittings the detector is supplied with a bare tu...

Page 42: ...16 03 914783 00 3 ...

Page 43: ...display and the Wait Light will still be lit During this interval the recorder output will be fixed at zero volts while the integrator output will transmit a voltage related to the present flowcell absorbance and last zero value stored in the autozero circuit memory To activate the recorder output press the autozero switch NOTE When the unit is first switched on the display will show random values...

Page 44: ... wavelength selector until the wavelength indicator coincides with the wavelength of maximal absorbance for your sample Wavelength ranges are 190 380 nm for the standard deuterium lamp 380 800 nm for the optional tungsten lamp Rotating this control clockwise decreases wavelength while a counter clockwise rotation will increase wavelength The arrow indicates the direction of rotation for increasing...

Page 45: ...3 1 0 and 3 0 seconds For extremely fast peaks a filter by pass switch is provided on the rear panel Figure 7 Switch 6 NOTE Although the filter may distort peak shape at long rise times peak area is always maintained Integration can be safely performed for the purpose of quantitative analysis from the recorder output Pressing the top portion of this switch turns the circuit on disables the rise ti...

Page 46: ...position The lamp may be shut off remotely with the rear panel located Lamp Shut off terminal This will prolong lamp life while the detector is not in use The lamp is shut off by providing a continuous contact closure or TTL low The lamp is re ignited by interrupting the contact closure or TTL low NOTE After the lamp is remotely re ignited the strip chart recorder output will transmit a voltage re...

Page 47: ... different applications All flowcells are provided premounted in a holder assembly to minimize alignment problems Detailed instructions specific to the various flowcells are included with the flowcells themselves This section of the manual provides general guidelines for maintenance and service of the flowcell and lamp assemblies The flowcell is located in the forward housing on the left side of t...

Page 48: ...de mount 3 Unscrew the two thumbscrews on the photodiode mount and pull the photodiode mount straight back see figure above The connecting cable is long enough to allow the photodiode mount to rest on the bench top 1 Cell Cover 2 Photodiode Retaining Screw 3 Photodiode Mount 4 Tubing Strain Relief Thrumbscrew 5 Cell Retaining Screws 6 Tubing Strain Relief Clamp 7 Cell Body Assembly 8 Cell Holder 9...

Page 49: ...er assembly Installation reverses the removal process 7 Slide the cell holder assembly onto the alignment dowels The inlet line should enter the bottom of the cell in order to provide efficient bubble flushing Securely fasten the cell holder assembly with the two thumbscrews 8 Slip the inlet and outlet tubes into the slots in the strain relief clamp and tighten the thumbscrews holding the clamp in...

Page 50: ...nt the following procedure should be followed for flowcell disassembly see Figure 10 1 Remove the flow cell assembly from the detector as described in the installation section of this manual 2 Remove the two screws which secure the flow cell body to the flow cell mount and free the flow cell from its mount 3 Using a wide flat blade screwdriver remove the window retaining nut 11 4 Remove the retain...

Page 51: ...ing its fitting and pulling the tube straight out Remove the remaining heat conductive epoxy out of the heat exchanger groove which circumscribes the cell body The flow cell body may be cleaned by soaking it in spectroscopic grade methanol For best results an ultrasonic bath should be used Flow Cell Reassembly NOTE For best results the flow cell gaskets should be replaced each time the cell is dis...

Page 52: ...ore it approaches the hole for the heat exchanger restraint To improve heat exchange between the inlet tubing and flow cell body a heat conductive epoxy should be applied into the groove before the tubing is installed After the epoxy has been applied secure the tubing into the heat exchanger groove by replacing the heat exchanger restraining screw 5 and washer 4 Replace the cell outlet tubing by p...

Page 53: ...MAINTENANCE AND TROUBLESHOOTING ProStar 340 UV Vis Detector 27 Figure 10 Flowcell ...

Page 54: ... be mounted in the instrument at a time Consequently moving from the UV to the visible requires the removal of the D2 lamp and installation of the tungsten lamp All lamp assemblies are pre aligned and no further alignment is necessary when changing from one lamp to another Figure 11 Lamp Assemblies A Deuterium B Tungsten Deuterium D2 Lamp The Deuterium Lamp is rated for 1 000 hours of life to 1 2 ...

Page 55: ...layed value is 100 lamp is good 99 50 lamp is marginal 50 replace lamp As a general rule the D2 lamp should produce reference light intensities greater than 50 from 190 380 nm Removing the D2 Lamp 1 Disconnect the power cord from the back panel of the detector 2 Remove the screw and remove the lamp housing the rear housing on the left side of the detector to expose the lamp see Figure 5 UV light c...

Page 56: ...e 11A The lamp leads should emerge from the top of the lamp 2 Use the thumbscrews and aluminum standoffs to attach the lamp assembly to the detector 3 Connect the lamp lead to the upper of the two terminals in the lamp compartment 4 Replace the lamp housing and its retaining screw CAUTION NEVER loosen the screw holding the lamp to the mount and NEVER attempt to rotate or move the lamp up or down i...

Page 57: ...2 than the tungsten lamp from 380 450 nm However this light represents the second order diffraction spectra of the D2 lamp and should not be used To install the tungsten lamp the D2 lamp must first be removed To remove the D2 lamp refer to Removing the D2 Lamp page 29 WARNING BURN HAZARD The tungsten lamp gets very hot Allow sufficient time for it to cool before attempting removal Removing the Tun...

Page 58: ...on troubleshooting detector problems on board diagnostic tips are discussed first Then there is a troubleshooting table organized by symptom cause remedy Light Intensity Diagnostics The detector provides the capability of monitoring relative light intensities at both the sample and reference photodiodes If an unusually noisy baseline is noted relative intensities of reference and sample light shou...

Page 59: ...ltage needs to be increased The instrument is factory configured to 10 mV full scale To change the full scale voltage 1 Press the bottom half of Switch 3 so that it rocks downward to the OFF position see 2 For a 100 mV scale output press the top part of Switch 2 so that it rocks to the ON position upwards 3 For a 1 0 V full scale output press the top portion of Switch 1 so that it rocks to the ON ...

Page 60: ...e Remove systems that consume high power from the line Noisy baseline on recorder random Sample cell windows are contaminated Flush cell with solvents methanol acetone water 6N nitric acid water and check for leaks Sample input line has a leak Check all lines from the output of the column to the input of the sample cell for leaks Bubble trapped in sample cell Increase flow rate and or back pressur...

Page 61: ...nd clean if necessary Solvent from column is changing absorption Column is filled with UV absorbers that are bleeding replace column impure solvent is equilibrating with the column Replace solvent with purer grade switch to a longer wavelength so that background absorption fluctuates less Leakage in the lines from column to flowcell Check lines for leakage Tiny bubble trapped in the sample cell In...

Page 62: ...36 03 914783 00 3 ...

Page 63: ...g 10 full scale offset at each setting Integrator Output 1 0 V AU analog output independent of range control but dependent upon autozero function A switch supplying an additional 10 0mV is provided on the rear of the unit Remote Controls Rear Panel input for autozero Event Mark and Remote Lamp Shut Off Noise 2 x 10 5 AU from 220 280 nm with 1 0 sec rise time static dry flowcell Drift 2 10 4 AU hou...

Page 64: ...um Lamp Assembly R000088516 Pre aligned Tungsten Lamp Assembly FLOWCELLS R000088506 Conventional HPLC 6 mm path 9 µL volume SS R000088507 Microbore HPLC 3 mm path 1 µL volume SS R000088508 Semi Prep glass column 3 mm path 4 5 µL volume SS R000088509 Biocompatible HPLC 6 mm 9 µL volume Kel F rated to 500 psi R000088510 Variable path preparative 0 3 mm path 0 4 6 µL volume SS 1 8 inch fittings rated...

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